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BACKGROUND OF THE INVENTION
1. Field of the Invention
A coin control mechanism for use in combination with a dispensing device. The mechanism includes a totalizer having three possible positions to allow the dispensing device to open when any one of three different cumulative values of coins are inserted therein.
2. Description of the Prior Art
The specifications and drawings of U.S. Pat. No. 4,037,701 ('701) are incorporated herein by reference, including the description of the prior art therein.
SUMMARY OF THE INVENTION
It is an object of this invention to allow for three different price combinations to be quickly and easily changed from outside the coin control mechanism. The coin control mechanism includes three adjustable price setters to allow for coins of a variety of denominations to actuate a release mechanism when any one of three preset denomination totals are inserted into the mechanism.
It is a further object of this invention to provide a bypass that allows a third price setting between a high price setting and a low price setting on a totalizer means to calculate the cumulative total of coins inserted into the coin control mechanism.
It is a further object of this invention to provide a slug rejecter means that will intercept a ferromagnetic slug before such slug reaches the totalizer means.
The specifications and drawings of the '701 patent are incorporated herein by reference, with the part numbers and terminology of that application carried into this application's specifications and drawings for clarity and ease of understanding. Structure that is added to the '701 patent begins with number four hundred and is even numbered. Structure that is inherent or disclosed in the '701 patent but not numbered therein but numbered in this application will start with number four hundred and one and be odd numbered.
The '701 patent discloses coin control mechanism 52 which comprises a totalizer means and a coin chute means arranged so that as coins pass through the coin chute means they activate the totalizer means to advance it in response to the denomination of the coin. For example, a quarter will advance the totalizer means more than a nickel. The locking means of the dispensing device is released on the registering of a predetermined price total on the totalizer means.
The latch control means of the '701 patent controls release of the access door. An adjustable price setter means sets the price or value of the coins necessary to operate the coin control mechanism at a predetermined price setting.
The adjustable price setter means of the '701 patent comprises an adjustable limit means to permit rapid changing of the price selected between an upper and a lower limit by the vendor. This is particularly useful in the case of newspaper vending machines because the price may vary between a daily edition to the Sunday paper.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a side view of the coin control mechanism with the coin chute means removed.
FIG. 1A is a perspective of the bypass removed from the coin control mechanism.
FIG. 2 is a side view of the coin control mechanism.
FIG. 3 is a partial cutaway of the top view of the coin control mechanism.
FIG. 4 is a side view of the bypass within the coin control mechanism.
FIGS. 5A, 5B and 5C are a front side view with the front plate of the coin control mechanism removed, illustrating the three positions of the bypass and associated structure.
FIG. 6 is a perspective view from within the coin control mechanism of the limit stop.
FIG. 7 is a left side view of the coin chute means mounting plate with the slug reject means mounted thereon.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
Structurally, this invention adds to the '701 patent bypass 400, illustrated in FIG. 1A apart from coin control mechanism 52. The function of bypass 400 is to permit a third price setting limit means for coin control mechanism 52. Frequently, periodical dispensing device 10 will carry papers of different prices at different times. For example, the daily edition of a newspaper may be one price, the Saturday edition a second price, and the Sunday edition, "Special" or "Extra" editions a third price. By using bypass 400 and the structure operatively associated therewith, as more fully set forth below, three different price setting limits are available to the vendor.
Bypass 400 is illustrated in FIG. lA. It includes interact member 416 and curved portion 408. The paragraphs below will set forth additional structure and the general mode of operation. The section entitled "Operation of Bypass" will specifically describe its function.
The position of bypass 400 and its structural relationship to other elements is shown in FIGS. 1, 3, 4, 5A, 5B, and 5C. Spring 402 biases interact member 416 of bypass 400 against linkage 282. Price setter control means 48 is connected to linkage 282. Bypass 400 is actuated by rotating key means in price setter control means 48, causing rotation of linkage 282. This interaction between linkage 282 and bypass 400 is more clearly set forth in FIGS. 4, 5A, 5B and 5C. This rotation of linkage 282 by rotation of the key in price setter control means 48 will cause bypass 400 to pivot on pin 404.
Generally, this pivoting of bypass 400 raises and lowers adjustable limit means 406 where it contacts curved portion 408 of bypass 400. FIG. 3 illustrates the location of spring 412 that biases adjustable limit means 406 towards a lowered position through apertures 410 and against curved portion 408. As can be seen in FIG. 4, prong 418 of adjustable limit means 406 passes slidably through plate 70 at apertures 410 therein, in much the same manner as adjustable limit means 98 and 100 pass through apertures 111 of the '701 mechanism. A series of apertures 410 is seen in FIG. 2. Adjustable limit means 406 may be manually raised so prong 418 is withdrawn from one aperture 410 and reinserted into a different aperture 410. This change would change the total denomination of coins required to activate coin oontrol mechanism 52, in the same manner that a change in position of limit means 98 or 100 as disclosed in the '701 patent effects such a change.
OPERATION OF BYPASS
Bypass 400 operates in the following manner. Price setter control means 48 may be rotated to one of three positions by use of the key means. Each of the three positions corresponds to one of three different price settings as determined by the position of adjustable limit means 98 and 100 in apertures 111 and adjustable limit means 406 in apertures 410. These three different positions are illustrated in FIG. 2 as 280a, 280b and 280c. Rotation of price setter control means 48 causes linkage 282 to rotate which in turn moves limit stop 280 to one of the three positions set by limit means 98, 100, and 406 illustrated in FIG. 2 as 280a, 280b and 280c. Each of these positions corresponds to a different position of totalizer register means 268. For example, position 280a, 280b and 280c may correspond to $0.50, $1.00, and $1.25, respectively, in total coinage required to activate coin control mechanism.
FIG. 2 illustrates the positional relationship of limit means 98, 100 and 406. To describe such positions, limit means 98 will alternately be referred to as upper limit means 98, as its position determines, denominationally, the greatest total coinage required to activate coin control mechanism 52. Limit means 100 will alternately be referred to as lower limit means 100, as its position determines, denominationally, the lowest coinage required to activate coin control mechanism 52. Limit means 406 will alternately be referred to as middle limit means 406 as its position determines, denominationally, the coinage required to activate coin control mechanism 52 when such coinage is intermediate between the upper and lower coinage totals.
Middle limit means 406 may be set in any of the stop positions determined by apertures 410, as long as such a stop position is between the position of upper limit means 98 and lower limit means 100.
The positions of limit stop 280, denoted 280a, 280b and 280c in FIG. 2, correspond to (arbitrarily) a 0°, 90° and 180° position of the key means which operates price setter control means 48. The corresponding position of bypass 400, middle limit means 406 and linkage 282 corresponding to each position of limit stop 280 shown in FIG. 2 as 280a, 280b and 280c is illustrated in FIGS. 5A, 5B and 5C, respectively.
Linkage 282 may be rotated to one of three positions by the key means attached to price setter control means 48. Linkage 282 has wall member 403 and articulates at pin 405. The three different positions of the key means correspond to FIGS. 5A, 5B, and 5C, each figure illustrating the corresponding position of linkage 282 and integral wall member 403. For the sake of illustration, the position indicated 280a will correspond to a 0° position of key means. In this position bypass spring 402 is "loaded" and biasing interact member 416 of bypass 400 against wall member 403 of linkage 282 as illustrated in FIG. 5A. In this position, limit means 406 is elevated sufficiently to allow limit stop 280 to pass beneath it. Position 280a reflects the position of totalizer register means 268, which position determines how far totalizer means must rotate before disengaging the locking means of the dispenser and thereby allowing access to the dispenser.
The rotation of the key means from 0° to 90° results in position of limit stop 280 as set forth in FIG. 2 as 280b and FIG. 5B. When the position of bypass 400 is in the position as illustrated in FIG. 5B, limit means 406 is urged against curved portion 408 by spring 412, allowing limit means 406 to move to its lowered position from its elevated position. Limit means 406 catches limit stop 280 in notch 420, as limit stop 280 moves toward limit means 98 under the urging of the key means against spring 290 (which normally maintains limit stop 280 at position 280a). Limit means 406 catches limit stop 280 before the key means and linkage 282 reaches 90°. The key means must be turned with greater torque after the catch as linkage 288 is stationary (because limit stop 280 is stationary against limit means 406) and the continued rotation of the key means up to the 90° position forces an extension of spring 401. At the 90° position, limit stop 280 is being urged against limit means 406 by spring 401. Simultaneous with the rotation from 0° to 90°, wheels 268 and 272 (which are biased to rotate around stud 276) "follow" limit stop 280. Wheels 268 and 272 move as a unit and are biased, pressing limit plate 281 which is integral with wheel 272 against stop tab 279 projecting from and integral with limit stop 280, as seen in FIG. 6. In other words, as the key is rotated from 0° to 90°, three actions are taking place: limit means 406 is lowering and getting closer to plate 70 at the same time that limit stop 280 is rotating towards limit means 406, and such rotation is allowing wheels 268 and 272 of totalizer register means 268 to "follow along," or rotate therewith.
After the key means is rotated from a 0° (280a) position to a 90° (280b) position, limit stop 280 has come to rest in notch 420 of middle limit means 406. The 90° position of linkage 282, interact member 416 and limit means 406 is as illustrated in FIG. 5B. Wheels 268 and 272 of totalizer register means 268 have "followed along" in the manner described above. An intermediate coinage total is now required to activate the dispenser and allow access to the periodicals contained therein.
When the key means is moved from the 90° position to the 180° position, limit stop 280 comes to a rest against limit means 98. Rotation of key to the 180° position moves limit stop 280 to the position indicated by 280c in FIG. 2. The movement of limit stop 280 to 280c is initiated and effected in the same manner and through the same linkage as the movement to position 280b. In this 180° position, the position of linkage 282, interact member 416 and limit means 406 is as illustrated in FIG. 5C, and limit means 406 is being held in an elevated position.
As can be seen in FIGS. 5A, 5B and 5C the raising and lowering of limit means 406 in response to the turning of the key means is sufficient to allow enough clearance for limit stop 280 to pass therebeneath when limit means 406 is in the raised position and is low enough to catch limit stop 280 when in its lowered position.
Furthermore, during the rotation from 90° to 180°, wheels 268 and 272 rotate in the same manner as set forth above. The rotation of limit stop 280 from 280b to position 280c occurs when linkage 286 shifts from the position as illustrated in FIG. 5B, where spring 401 is biasing limit stop 280 against limit stop means 406, to a position as illustrated in FIG. 5C where spring 401 is still biasing limit stop 280 in clockwise direction but limit stop is now flush against limit stop means 98. The raising of limit means 406 allows the movement of limit stop 280 thereunder and up to limit stop means 98. The force required to urge such biasing and maintain pressure originates at spring 401 and is transmitted through elements 288 and 278 to limit stop 280.
At the 180° position of the key means and linkages 282 and 296, limit stop 280 rests against limit stop means 98. The movement of wheels 268 and 272 of totalizer register means 268 has changed the position of notch portion 274 with respect to element 218. In other words, as the key means is rotated from 90° to 180°, three actions are taking place. Limit means 406 is raising, limit stop 280 is then released and moves towards limit means 98, while, simultaneously, wheels 268 and 272 are rotating and changing position of totalizer register means 268.
For limit stop 280 to return from 180° (280c) to 0° (280a), the key means is rotated back to the 0° position. This rotation results in the following actions. First, it allows limit means 406 to lower as wall member 403 rotates away from interact member 416 and permits springs 412 and 402 to compress. This catches limit stop 280 against the back side of limit means 406 (opposite notch 420). Then, as the 0° position is being approached, wall member 403 contacts interact member 416, rotates bypass 400 and raises limit means 406, allowing limit stop 280 to freely rotate back to the 0° (280a) position.
Thus, it is seen how the use of bypass 400, a three-position key means, limit means 406, and the related structure set forth herein allows a rapid change of the coin control mechanism to one of three different coin denominational totals to activate the dispenser.
A further improvement of coin control mechanism 52 is the addition of slug reject means 500 illustrated in FIG. 7. Slug reject means 500 is a ferromagnetic mass that is attached to coin control mechanism 52 adjacent to the coin chute means in order to intercept a ferromagnetic slug before such slug reaches the totalizer means. Slug reject means 500 may be mounted on and extend through plates 292, 294 or 342. In the preferred embodiment, slug reject means 500 is mounted on plate 342 by bracket 502. It passes through plates 342 and 292 so that a flat surface thereof lies in the plane of plate 392 facing the coin chute.
In operation, slug reject means 500 will magnetically intercept a ferromagnetic slug in the slug's passage through the coin chute. This will prevent the slug from activating the totalizer means, and will also jam the coin chute. However, depressing coin return actuator bar 64 will allow the slug to fall into coin return opening 62. This occurs because the depressing of coin return actuator bar 64 rotates plates 292 and 292 away from plate 342 (as set forth in the '701 patent) and therefore removes the slug from the grip of the magnetic field generated by slug reject means 500.
Although the invention has been described with reference to a specific embodiment, this description is not meant to be construed in a limiting sense. Various modifications of the disclosed embodiments will become apparent to those skilled in the art upon reference to the description of the invention. It is therefore contemplated that the appended claims will cover such modifications that fall within the true scope of the invention.
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A coin control mechanism for use with a dispensing machine and containing a three-way adjustable price setter and a mechanical linkage to quickly change the coin control mechanism among any one of three preset prices, thus allowing for different price settings on different days. Three adjustable legs control the preinsertion position of a totalizer which calculates the cumulative total of coins inserted into the coin chute of the coin control mechanism. A three-position keyway and linkage allows an operator to quickly change the preinsertion position of the totalizer from outside of the coin control mechanism.
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FIELD AND BACKGROUND OF THE INVENTION
The invention relates to circular knitting machines, especially machines for manufacturing hosiery or the like, that are provided with latch needles mounted in a needle cylinder. In operation, the needles are lowered and lifted by means of swinging sinkers which are provided with two guiding butts alternately engageable with cam channels. Alternatively, the butts can be provided immediately on the needles, or on guiding sinkers of double-head needles.
Circular knitting machines provided with swinging sinkers having two guiding butts are well known. These machines are adapted for reverse knitting operations, such as knitting heels and toes of hosiery, and particularly in a single feed system. The system is usually provided with a right and left sinking cam as well as with heel cam which is designed for displacing the needles onto the level of the sinking cams, i.e. in both knitting directions. Due to such an arrangement, the cam channels for the butts of the needles or for the needle guiding sinkers cross each other. Below the heel cam there is provided a compensating cam which is designed for positioning the needles and for preventing the needles form assuming, owing to the knitting speed, a position which is lower than the position which is necessary for laying thread into the needles. Consequently, the needle races are broken, and the guiding butts are exposed to many shocks which causes paths to lose their curvilinear course. The motion, especially with double-cylinder machines, is ensured within a section, by the lower butts of the guiding sinkers so that even the race continuity is impaired. Therefore, any increase in knitting speed is difficult.
SUMMARY OF THE INVENTION
It is an object of the present invention to eliminate the drawbacks of the prior art devices as referred to above and to provide an improved circular knitting machine for manufacturing hosiery having latch needles which are mounted in a lower needle cylinder. When operated, the latch needles are lowered and lifted by swinging sinkers provided with two guiding butts, i.e. a first guiding butt and a second guiding butt, which are alternately engageable with cam channels and which can be provided either directly on the needles, or on the swinging sinkers when received in vertical tricks of the lower needle cylinder.
According to the present invention, at least one first sinking cam, is provided in the cam channel for the first guiding butts which provides a rotational knitting direction. Second guiding butts in the cam channel have at least one second sinking cam or at least one third sinking cam for providing a reverse knitting direction. In the cam channel of the second guiding butts, there are provided cam means for transferring the needles from knitting paths into and out of an elevated heel path. The cam means comprises three shaped grooves which have at their ends chamferings for forcing the second guiding butts into the vertical tricks of the needle cylinder. Above the starting point of each groove, there is proved a swinging push-button. While in the cam channel for the first guiding butts, there are provided means for reducing and adding needles when in the reverse knitting operation. The means comprising a shaped through groove having at its end a chamfering for forcing the first guiding butts into the vertical tricks of the needle cylinder, and a radially movable push-button being provided above the starting point of said shaped through groove. The cam channels for guiding the first and the second guiding butts are separate from each other for both knitting directions.
BRIEF DESCRIPTION OF THE DRAWINGS
In the drawings:
FIG. 1 is a partial view of cam section arrangement according to the present invention;
FIG. 2 is a sectional view of a lower needle cylinder having guiding butts and swinging butts;
FIG. 3 is a sectional view of a cam block and a swinging sinker together with a push-button; and
FIG. 4 is a view showing a swinging push-button in operation according to the present invention.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
As illustrated in FIG. 2, the present invention pertains to a double-cylinder circular knitting machine designed for manufacturing ribbed goods and hosiery, and comprises an upper needle cylinder (not shown) and a lower needle cylinder 1 having vertical tricks 2. Vertical tricks 2 of said lower needle cylinder 1 receive guiding sinkers 3 of needles 4'. The needles 4' are of a double-head latch type which allows for the transfer to the upper needle cylinder for knitting link-to-link stitches. By means of a joint 31, each guiding sinker 3 carries a swinging sinker 4 having one first and one second guiding butt 41 and 42, respectively, as well as pattern butts 43. The cam system of the lower needle cylinder 1 consists of five cam sections 5, 6, 7, 8 and 9. In the cam section 6, there is mounted, for vertical motion, a first sinking cam 10 for engaging the needle 4' in a rotational knitting direction S. In cam section 8, a second vertically movable sinking cam 11 is provided for engaging needles 4' in the rotational knitting direction S. Finally, in the cam section 9 there is disposed a third sinking cam 12 for engaging needles 4' in a reverse knitting direction S'.
The cam sections 5 and 6, when assembled together, form a channel 13 for first guiding butts 41 of the swinging sinkers 4. The channel 13 forms the work race for needles 4' of the first knitting system for forming stitches in the rotational knitting direction S. A shaped through groove 14' serves for guiding the first guiding butts 41 in the reverse knitting direction S' and terminates in a chamfering 141' for forcing the first guiding butts 41 into the vertical tricks 2 of the lower needle cylinder 1. In the cam section 7, there are provided three shaped through grooves 71, 72 and 73 in the path of the second guiding butts 42. The groove 71 is designed for transferring the needles 4' from the knitting position into a heel forming position during the reverse direction S' of rotation. A starting point of the groove 71 corresponds to a clearing position of the needle 4', and the end portion to the heel position. At its end, the groove 71 has a chamfering 711 for forcing the second guiding butts 42 into the vertical tricks 2 of the needle cylinder 1. The shaped through groove 72 serves for transferring the needles 4' back from the heel position into the knitting position during the reverse knitting direction S'. The starting point of the groove 72 corresponds to the heel position of the needle 4' while the end portion corresponds to the clearing position. The end portion of the groove 72 has a chamfering 722 for forcing the second guiding butts 42. Finally, the third shaped through groove 73 forms a mirror image of the groove 72 and serves the same purpose as groove 72. At the end of the groove 73 there is also a chamfering 733 for forcing the second guiding butts 42.
The cam sections 8, 9 and 7 form a channel 15 for guiding the second guiding butts 42 as to a height corresponding to that of the guiding sinkers 3 when the points of the sinkers 3 open the latches of the upper needles 4'; alternatively, the channel 15 can serve for transferring the needles 4' between the upper and lower needle cylinders.
The cam sections 8 and 9 form a channel 16 within the path of the second guiding butts 42 for the stitch-forming motion of needles 4' in a second knitting system. During the rotational knitting direction S, a portion of the channel 16 is in the cam section 9. There is also a shaped through groove 91, constituting a mirror image of the groove 71 and having, a chamfering 911, for reducing the number of needles for the rotational knitting direction S. Further, in the cam section 9, there is formed, within the path of the second guiding butts 42, a shaped through groove 92 which provides the needles 4' with a stitch-forming motion in the reverse knitting direction S', and partially in the knitting direction S. The groove 92 terminates at its ends by chamferings 921 and 922 designed for forcing the second guiding butts 42. In the transfer point there is provided in the cam section 9 a through groove for the push-button 17.
In a choice point V of the needles 4' (indicated by dot-and-dash line) there is provided in the cam section 7 a vertical groove 18 designed for being engaged by swinging levers of a known selecting means (not shown), in which levers, in inoperative positions, enter the space between pattern butts 43. While in their operative positions, they engage the paths of butts 43. Upstream of the choice point V, there is provided in the path of the first butts 41, a radially movable push-button 19 which, enters, in an operative position, the channel 14. Downstream of the choice point V, there is provided radially movable push-button 24'. Above the starting point of the channel 16 there is further provided within the path of the first guiding butts 41, in the channel 14, a radially movable push-button 19'. Above the starting points of the shaped through grooves, there are provided, at the height of the channel 13 or the channel 14, respectively, four swinging push-buttons 20, 21, 22, 23. Each of the push-buttons 20, 21, 22, and 23 consist of a swinging presser lever 24 (FIG. 3) which is spring-loaded by a torsion spring provided about its pivot. The swinging presser lever 24 is arranged on a carrier 25 fixedly supporting a permanent magnet 26 together with a coil 27 connected to a controlling computer (not shown). The carrier 25 is arranged radially movable to the needle cylinder 1.
In operation, during the rotational knitting, the swinging push-buttons 20, 21, 22, 23 and 24' are removed from the needle cylinder into non-operative positions and radially movable push-button 19 and 19 are situated within the path of the first guiding butts 41 in the channel 14 so that they cause engagement of the guiding butts 41 in front of the choice point V. The guiding levers of the guiding means (according to a program) causes a pressure to the pattern butts 43 so that the swinging sinkers 4 follow, by their first guiding butts 41', the path of the channel 14 so that the guiding sinkers 3 and the corresponding needles 4' form face stitches in the fabric. By the radially movable or approaching push-button 19', the first guiding butts 41 are forced into the lower needle cylinder 1 while the second guiding butts 42 are swung into the channel 16. The needles 4' form face stitches in the second knitting system or on the second sinking cam 11 whereupon the guiding sinkers 3 are displaced again to the position in front of the choice point V or the radially movable push-button 19. The swinging sinkers 4, whose pattern butts 43 have not been forced into the needle cylinder 1, are guided, by means of their second guiding butts 42, in the channel 15. By the push-button 17, the guiding sinkers 3 together with the needles 4' are disengaged so that the needles 4' are transferred between the two needle cylinders, provided the needles in the upper needle cylinder are also brought into the transfer position. The empty guiding sinkers 3 pass by means of the first guiding butts 41 through the channel 15 up to the choice point V. The needles 4', once transferred onto the upper needle cylinder, form back stitches.
The heel or the toe of a hose, by the reverse motion of the needle cylinders, is formed in the following way listed below.
The needles 4' are separated in the lower needle cylinder into operating and non-operating needles as follows. By the selecting device all of the pattern butts 43 are pressed in. The radially movable push-button 24' is brought to the lower needle cylinder 1 in that section only which corresponds to the heel-forming needles 4'. The radially movable push-button 24' will press in the first guiding butts 41 so that the second guiding butts 42 get into the shaped through groove 91 where they are raised and pressed in again by the chamfering 911. The first guiding butts 41 are received by the channel 13, and the corresponding guiding sinkers 3 or needles 4', respectively, assume an elevated heel position with stitches on the needle stems below the needle latches. The other needles 4' knit in the first knitting regime or system while the radially movable or approaching push-buttons 19 and 19' are removed from the lower needle cylinder whereby the second knitting system is set out of operation. Meanwhile the machine is given reverse motion, and the swinging push-buttons 20 and 21 are brought to the lower needle cylinder 1. The operating needles 4' are in the clearing position, which means that the first guiding butts 41 are in the channel 14. Prior to changing the rotational knitting direction S into the reverse knitting direction S', there is effected the first stitch reducing or narrowing phase by means of the swinging push-button 21 which can force only one first guiding butt 41. The swinging push-button 21 or 20, operate in such way that the first guiding butt 41, owing to friction, carries along the swinging presser lever 24 which swings into a space between the adjacent lever 24 which swing into a space between the adjacent first guiding butts 41 so that the next first guiding butt 41 swings up to the permanent magnet 26 by attraction whereas the other first guiding butts 41 are allowed to pass and are pressed in the further narrowing phases. In this phase, the swinging presser lever 24 of the swinging push-button 21 is held by the permanent magnet 26. By pressing the first guiding butt 41, the corresponding second guiding butt 42 is pressed out into the shaped through groove 91 while, during the further rotation, it strikes the chamfering 911 whereby the first guiding butt 41 is tilted out backward into the channel 13, i.e. into an inoperative height or position. Thus the corresponding guiding sinker 3 and the needle 4' are displaced into the heel-forming position. During this rotation direction, the swinging presser lever 24 of the swinging push-button 20 is held by the permanent magnet 26. When changing the rotational directions to the reverse direction S', the first guiding butts 41 are led through the channel 14 up to the shaped through groove 14' where they are pressed in by the chamfering 141'. The second guiding butts 42 of the swinging sinkers 4 are titled out into the shaped through groove 92, and the corresponding needles 4' form stitches in the first knitting system in the reverse knitting direction S' on the third sinking cam 12. After the stitch formation, the needles 4' are raised into the clearing position while the chamfering 921 will press in the second guiding butts 42 into the vertical tricks 2, and the first guiding butts 41 enter the channel 14. The group of operating needles 4' is then led by means of the channel 14 up to the dead point, i.e. the point where the swinging sinker stops before turning in the opposite direction for reverse knitting, while before the latter, the needle 4' or the guiding sinker 3, respectively, is eliminated from this group into the heel-forming position by the swinging push-button 20, and particularly in the same way as described with the swinging push-button 21, which means by the shaped through groove 71 and the chamfering 711. A part of the first guiding butts 41 belonging to the corresponding operating needles 4', upstream of the dead point, is led again through the shaped through groove 4' and is pressed in by the chamfering 141', and further on the guiding sinkers 3 are led up to the dead point by the second guiding butts 42 in the shaped through groove 2. Downstream of the dead point, during the rotational knitting direction S, the second guiding butts 42 are pressed in by the chamfering 922, and the guiding sinkers 3 are led by means of the first guiding butts 41. After the winding of coil 27 has been supplied with current, the permanent magnet 26 will release the swinging presser lever 24 of swinging push-button 21 which, due to the force of torsion spring, reassumes its initial position whereupon the next removal of the needle 4' can be affected as hereinabove described. After the reduction of the predetermined number of needles 4' has ended, the knitting of the second heel portion is effected in the following way while the heel-forming needles 4' are being added again.
The swinging push-buttons 22 and 23 are set in operation; these, however, are shaped so that their swinging presser levers have a larger working front whereby they gradually press in the two first guiding butts 41. Otherwise, their function remains the same. These swinging butts 22 and 23 alternately press in the first guiding butts 41 from both sides of the group of swinging sinkers 4 belonging to the guiding sinkers 3 or to the needles 4', respectively, in the elevated heel-forming position. In this way, the second guiding butts 42 are titled out into the shaped through grooves 72 or 73, respectively, and are pressed in again by the chamferings 722 and 733 so that their first guiding butts 41 are tilted out again into the channel 14, and the needles 4' are transferred in this way back to the knitting position. Simultaneously, however, the swinging push-buttons 20 and 21 are in operation, which results again in adding only one needle 4' in each of the two knitting directions. After the needle adding has ended, the swinging push-button 20, 21, 22 and 23 are displaced away from the lower needle cylinder 1, and the knitting machine continues its rotational operation as described above.
Within the scope of the present invention, it is possible to provide the swinging sinkers 4 immediately on the needle stems for single-cylinder knitting machines manufacturing hosiery with reverse heel or toe, respectively, or with single-cylinder machines for creating the so-called, intarsia designs on calf, by means of reverse knitting, without effecting the subject matter of the invention.
Needless to say, the invention can be applied to a machine with a plurality of knitting systems operating either in the reverse or rotational regime. The sinking cams of the knitting systems in the rotational operation can be provided only within the path of one type of guiding butts, which is preferable with single-cylinder machines, or in the paths of both guiding butt types, depending on the knitting technologies applied to the machine. However, for the reverse operation, the sinking cams for the rotational and the reverse direction of knitting S and S', respectively, are always disposed in the grooves of the first and the second guiding butts 41 and 42, respectively.
Further, in lieu of the swinging push-buttons, it is possible to use only radially movable push-buttons or any other means for pressing in the corresponding guiding butts, such as a well-known electric motor with reverse rotation so that the swing extent can be controlled by means of a microcomputer. Such means for pressing in the guiding butts would be, in the reverse regime, fixedly attached whereas the butts would be approached by said electric motor.
For controlling the guiding butts it is possible to use stationary cam means instead of shaped through grooves 71, 72, 73, 91 and 92, and the corresponding chamferings for pressing them in. Thus, the independence of the means is maintained, which means that the paths of the butts are separate from one another.
LIST OF REFERENCE NUMBERS USED
1 lower needle cylinder
2 vertical trick
3 guiding sinker
4 swinging sinker
4' needle
5,6,7,8,9 cam sections
10 first sinking cam
11 second sinking cam
12 third sinking cam
13,14 channel for butts
14' shaped through groove
15,16 channeled for butts
17 push-button
18 vertical groove
19, 19',24' radially approaching push-button
24 swinging presser lever
25 carrier
26 permanent magnet
27 coil
31 joint
41 first guiding butt
42 second guiding butt
43 pattern butt
71,72,73,91,92 shaped through grooves
141' chamferings with grooves 71, 72, 73
911,922,923 chamferings with grooves 91 and 92
V choice point
S direction of knitting rotation
S' reverse knitting direction
20,21,22,23 swinging push-buttons
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A circular knitting machine for manufacturing hosiery comprises a lower needle cylinder (1) having a cam section arrangement (5, 6, 7, 8, 9) and a verticle trick (2) grooved on the needle cylinder (1) near the arrangement (5, 6, 7, 8, 9). The cam section arrangement (5, 6, 7, 8, 9) defines a plurality of channels (13, 14, 15, 16). A sinker arrangement (3, 4) is disposed in the verticle trick (2) for verticle movement and has guiding butts (41, 42) alternately engageable with the channels (13, 14, 15, 16). The guiding butts (41, 42) are movable in the channels (13, 14, 15, 16) in a knitting direction (S) and a reverse knitting direction (S'). A plurality of needles (4') are engaged with the sinker arrangement (3, 4). Stitch cams (10, 11) are mounted to the cam section arrangement (5, 6, 7, 8, 9) for engaging the needle (4') when the needles (4') are moved in the knitting direction (S). A reverse stitch cam (12) is mounted to the cam section arrangement (5, 6, 7, 8, 9) for engaging the needles (4') when the needles (4') are moved in the reverse knitting direction (S').
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BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates generally to optical unit actuators for information recording/reproducing apparatus, and more particularly to an actuator for driving an optical unit including an objective lens for recording and reproducing information on an optical recording medium such as an optical disk.
2. Description of the Prior Art
With the spread use of optical disk drive units as an external storage for computers, the demand for a compact and high-speed unit has increased.
More specifically, there have been a demand for high speed rotation of an optical disk for the purpose of realizing a high data transfer rate, and a demand for a compact and flat structure resulting from the tendency toward an optical disk of a smaller diameter.
The speeding-up and compacting of the optical disk unit involves several problems to be solved. A main problem is the maintenance of control characteristics of an optical disk, an optical head and a control circuit for the optical head.
An optical unit actuator of a conventional information recording/reproducing apparatus will be described below with reference to FIGS. 6 and 7 of the accompanying drawings, in which FIG. 6 is an exploded perspective view of a main portion of the optical unit actuator, and FIG. 7 is a cross-sectional view taken along line VII--VII of FIG. 6.
As shown in FIG. 6, the actuator includes an objective lens holder 1 to which an objective lens 2, two opposed tracking coils 3 and a focusing coil 4 are secured by bonding. The objective lens holder 1 has a pair of aligned central cylindrical projections (not designated) which are fitted in the central holes of two opposed plate springs 6 and bonded to the plate springs 6. The outer peripheral portions of the respective plate springs 6 are secured by bonding to a carriage 5, so that the objective lens holder 1 is mounted in the carriage 5. The objective lens holder 1 is displaceable relative to an optical disk 7 both in a focusing direction and in a tracking direction. In order to move the carriage 5 in the radial direction of the optical disk 7, two opposed linear motor coils 8, 9 are wound around bobbins 10, 11 which are secured by bonding to opposite sides of the carriage 5. A fixed optical base 12 generates a light beam used for recording/reproducing information on the optical disk 7. The light beam is projected on a mirror 13 fixed on the bobbin 11 and then is reflected by this mirror 13 toward the objective lens 2. A magnetic circuit which constitutes a fixed unit or member as against the displacement of the objective lens 2 is composed of two opposed back yokes 14, 14, magnets 15, 15 secured by bonding to the respective back yokes 14, 14, two confronting yokes 16, 16 facing the corresponding magnets 15, 15 and two opposed side yokes 17, 18 for completing a closed magnetic circuit. The components of the magnetic circuit are assembled together by a rigid connection in terms of vibration. The carriage 5 is assembled with the magnetic circuit such that parts of the tracking coils 3, focusing coil 4 and linear motor coils 8, 9 are disposed in magnetic gas defined between the magnets 15 and the confronting yokes 16. The magnetic circuit is common to the tracking coils 3, focusing coil 4, and linear motor coils 8, 9. A pair of shafts 19 extends between the side yokes 17, 18 and resiliently retained on the side yokes 17, 18 by means of plate springs 20. The shafts 19 are slidably received in a pair of plain bearings 5a, 5a, respectively, of the carriage 5 so that the carriage 5 is slidable along the shaft 19 in the radial direction of the optical disk 7. The fixed optical base 12 includes a semiconductor laser for generating a light beam for recording and reproducing information on the optical disk 7, optical components, a photoelectric transducer, etc. and is secured to the side yoke 17. The optical disk 7 is rotated at a predetermined speed by a spindle motor 22 secured to the side yoke 18.
The conventional optical unit actuator of the foregoing construction involves problems in maintaining the control characteristics of the optical disk, optical head and control circuit for the optical head when an attempt is made to speed up the rotation of the optical disk for the purpose of increasing the data transfer rate and to minimize the overall size of the unit to conform to the tendency toward a small-diameter optical disk.
The problems associated with the conventional optical unit actuator will be described below with reference to FIG. 8. FIG. 8 shows amplitude-to-vibration performance curves of various components of the actuator obtained when the focusing coil 4 is excited to move the objective lens holder 1 in the focusing direction of the optical disk 7. In this Figure, the solid line indicated by a shows the vibrational characteristic of the objective lens holder 1, and the chain line indicated by b.c shows the vibrational characteristic of the magnets 15 and the back yokes 14.
To insure a reliable recording/reproducing of information on an optical disk 7, it is desired that the objective lens holder 1 does not induce parasitic oscillation even at a high frequency, as indicated by the solid line a, but generates an acceleration which is capable of following a dynamic radial runout and an axial deflection of the optical disk 7.
The acceleration of the objective lens holder 1 means that the magnet 15 and the back yoke 14 are caused to vibrate, as indicated by the chain line b.c, by a reaction force resulting from acceleration of the objective lens holder 1. In this instance, the magnet 15 and the corresponding back yoke 14 are integral with each other and hence vibrate at the same amplitude of vibration. The difference in amplitude between the objective lens holder 1 and the magnet 15 or between the objective lens holder 1 and the back yoke 14 is determined by the ratio of a mass of the objective lens holder 1 to a mass of the magnetic circuit which constitutes a fixed unit or member as against the displacement of the movable objective lens holder 1.
The vibrational energy which vibrates the magnet 15 and the back yoke 14 is transmitted to the fixed optical base 12 via the side yoke 17. Since the side yoke 17 is joined with the magnet 15 and the back yoke 14 in rigid connection in terms of vibration, the fixed optical base 12 is vibrated.
When optical disk 7 is rotating at a high speed in the range of 2400-3600 rpm so as to provide a high data transfer rate, a great acceleration is produced due to the dynamic radial runout and the axial deflection of the rotating optical disk 7. To enable the objective lens 2 to accurately follow the thus rotating optical disk 7 during the recording/reproducing operation, the objective lens holder 1 is highly accelerated. A very large acceleration thus produced creates a considerably large vibrational energy which is in turn transmitted to the fixed optical base 12.
The fixed optical base 12 is thus vibrating under the influence of the vibrational energy. During that time, various optical components, a photoelectric transducer, etc. which are disposed in an optical path extending between the fixed optical base 12 and the optical disk 7 are vibrated. As a result, a control system used for controlling the objective lens 2 to follow the optical disk 7 is in the oscillated condition. Under such condition, the objective lens 2 is no longer possible to accurately follow the movement of a recording surface of the optical disk 7. Thus, an accurate recording/reproducing operation is difficult to achieve.
An optical information recording/reproducing apparatus for use with a small-diameter optical disk must be compact in size and low in profile. Consequently, the optical disk per se is as thin as possible. To this end, an optical disk of a single plate structure is used. The optical disk of the single plate structure is low in rigidity and hence is likely to induce resonance vibration when subjected to a reaction force resulting from the acceleration of the objective lens holder 1 which is transmitted via the spindle motor 22. When the optical disk 7 undergoes resonance vibration, the control system used for controlling the objective lens 2 to follow the recording surface of the optical disk 7 is caused to oscillate. Thus, an accurate recording/reproducing of information on the optical disk is no longer possible.
SUMMARY OF THE INVENTION
With the foregoing difficulties of the prior art in view, it is an object of the present invention to provide an optical unit actuator for information recording/reproducing apparatus which is capable of speeding up the data transfer rate of the apparatus and minimizing the overall size of the apparatus without deteriorating the control characteristics of an optical disk, an optical head and a control circuit for the optical head.
An optical unit actuator of this invention includes an optical unit including an objective lens and displaceable in a predetermined direction relative to a recording medium, a fixed unit which is immovable as against the movable optical unit, and an electromagnetic drive mechanism including at least one coil and a magnet cooperative with the coil to drive the optical unit in the predetermined direction relative to the recording medium. One of the coil and the magnet is fixed to the optical unit and the other of the coil and the magnet is held on the fixed unit with an elastic support means disposed therebetween.
With this construction, when the optical unit including the objective lens is displaced in a direction to access the recording medium, a reaction force acting between the coil and the magnet is produced as a result of acceleration of the optical unit. The reaction force is, however, substantially dampened or taken up by the elastic support means before it is transmitted to the fixed unit. The optical components, a photoelectric transducer, etc. disposed on the fixed unit may vibrate only at a low level and do not induce resonance vibration. The control system for achieving follow-up control of the objective lens relative to the optical disk is protected from oscillation. Thus, recording/reading operation can be performed reliably and accurately.
The above and other objects, features and advantages of the present invention will become more apparent from the following description when making reference to the detailed description and the accompanying sheets of drawings in which preferred structural embodiments incorporating the principles of the present invention are shown by way of illustrative example.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is an exploded perspective view of an optical unit actuator for information recording/reproducing apparatus according to a first embodiment of this invention;
FIG. 2 is a cross-sectional view taken along line II--II of FIG. 1;
FIG. 3 is an exploded perspective view of a main portion of an optical unit actuator according to a second embodiment of this invention;
FIG. 4 is a graph showing the vibrational characteristics of the optical unit actuator shown in FIG. 1;
FIG. 5 is a graph showing the vibrational characteristics of the optical unit actuator shown in FIG. 3;
FIG. 6 is an exploded perspective view of an optical unit actuator of a conventional information recording/reproducing apparatus;
FIG. 7 is a cross-sectional view taken along line VII--VII of FIG. 6; and
FIG. 8 is a graph showing the vibrational characteristics of the optical unit actuator shown in FIG. 6.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
FIGS. 1 and 2 shows an actuator for an optical unit of an information recording/reproducing apparatus according to a first embodiment of this invention.
The optical unit actuator includes an objective lens holder 1 to which an objective lens 2, tracking coils 3 and a focusing coil 4 are secured by bonding. The objective lens holder 1 has a pair of aligned central projections (not designated) which are bonded to central holes of two opposed plate springs 6. The outer peripheral portions of the respective plate springs 6 are secured by bonding to opposite sides of a rectangular hollow carriage 5, so that the objective lens holder 1 is mounted in the carriage 5. The thus mounted objective lens holder 1 is displaceable relative to an optical disk 7 both in a focusing direction and in a tracking direction. In order to move the carriage 5 in the radial direction of the optical disk 7, two opposed linear motor coils 8, 9 are wound around bobbins 10, 11 which are secured by bonding to opposite sides of the carriage 5. A fixed optical base 12 generates a light beam for recording/reproducing information on the optical disk 7. The light beam emitted from the fixed optical base 12 is projected on a mirror 13 fixed on the bobbin 11 and subsequently it is reflected by this mirror 13 toward the objective lens 2.
A magnetic circuit which constitutes a fixed unit or member as against the displacement of the objective lens 2 is composed of two opposed back yokes 14, 14, magnets 15, 15 held on the respective back yokes 14, 14 with elastic support members 21 disposed therebetween, two confronting yokes 16, 16 facing the corresponding magnets 15, 15, and two opposed side yokes 17, 18 interconnecting opposite ends of the back yokes 14, the magnets 15 and the confronting yokes 16 to complete a closed magnetic circuit. The components of the magnetic circuit are assembled together by a rigid connection in terms of vibration. The carriage 5 is assembled with the magnetic circuit in such a manner that parts of the tracking coils 3, focusing coil 4 and linear motor coils 8, 9 are disposed in magnetic gaps defined between the magnets 15 and the confronting yokes 16. The magnetic circuit is common to the tracking coils 3, focusing coil 4, and linear motor coils 8, 9. A pair of shafts 19 extends between the side yokes 17, 18 and resiliently retained on the side yokes 17, 18 by means of plate springs 20. The shafts 19 are slidably received in a pair of plain bearings 5a, 5a, respectively, of the carriage 5 so that the carriage 5 is slidable along the shaft 19 in the radial direction of the optical disk 7.
The fixed optical base 12 includes a semiconductor laser (not shown) for generating a light beam used for recording and reproducing information on the optical disk 7, optical components (not shown), a photoelectric transducer (not shown) for receiving the reflected light returning from the optical disk 7, etc. The fixed optical base 12 is secured to the side yoke 17. A spindle motor 22 for rotating the optical disk 7 at a predetermined speed is secured to the side yoke 18.
The optical head of the foregoing embodiment is a separate type optical head in which the fixed optical base 12 is always disposed in a given position regardless of the position of the objective lens 2 in the radial direction of the optical disk 7.
FIG. 3 shows a main portion of an optical unit actuator according to a second embodiment of this invention. The optical unit actuator includes a rectangular objective lens holder 31 to which an objective lens 32, two opposed tracking coils 33 and two opposed focusing coils 34 are secured by bonding. The objective lens holder 31 has a vertical plain bearing 30 slidably fitted over a support shaft 36 upstanding from a central portion of a rectangular actuator base 35. The objective lens holder 31 is displaceable relative to the actuator base 35 in the focusing direction and the tracking direction of the optical disk 7. Two opposed tracking magnets 37 for supplying magnetic flux to the tracking coils 33 are held on the actuator base 35 with elastic support members 39 such as rubber sheets disposed between the corresponding tracking magnets 37 and the actuator base 35. The actuator base 35 constitutes a fixed unit or member as against the displacement of the movable objective lens holder 31. Likewise, two opposed focusing magnets 38 for supplying magnetic flux to the focusing coils 34 are held on the actuator base 35 with elastic support members 40 such as rubber sheets disposed between the corresponding focusing magnets 38 and the actuator base 35. The tracking and focusing magnets 37, 38 are magnetized in the manner illustrated in FIG. 3, so that magnetic flux flowing between two adjacent poles of each respective magnet is substantially perpendicular to the direction of a current flowing through the corresponding coil.
A rectangular optical base 42 carries thereon a semiconductor laser 43 for generating a light beam during the infomation recording/reproducing operation, optical components (not shown), a photoelectric transducer 44, etc. The actuator base 35 is secured by a plurality of screws 41 to the optical base 42. The optical base 42 has two linear motor coils 45 on and along its opposite side edges for movement in the radial direction of the optical disk 7. Two parallel spaced guide shafts 47 extend across a rectangular opening in a rectangular drive base 46 and guide the optical base 42 as the optical base 42 moves in the radial direction of the optical disk 7. A pair of elongate magnets 48 for supplying magnetic flux to the respective linear motor coils 45 are secured by bonding to a pair of back yokes 49, respectively. Each magnet 48 and the corresponding back yoke 49 are held on the drive base 46 with an elastic support member 50 such as a rubber sheet disposed therebetween. The drive base 46 constitutes a fixed unit or member as against the displacement of the movable optical base 42 in the radial direction of the optical disk 7. A spindle motor 51 is secured by a pair of screws 52 to the drive base 46 for rotating the optical disk 7 at a predetermined speed.
The optical head of the second embodiment is an integral type optical head in which the objective lens 32 and the optical base 42 are movable, as a single unit, in the radial direction of the optical disk 7.
The principle of operation of the optical unit actuator shown in FIG. 1 will be described below with reference to FIG. 4. FIG. 4 shows amplitude-to-vibration performance curves of various components of this actuator which are obtained when the focusing coil 4 is excited to move the objective lens holder 1 in the focusing direction of the optical disk 7. In this Figure, the solid line designated by a indicates the vibrational characteristic of the objective lens holder 1, the chain line designated by b indicates the vibrational characteristic of each magnet 15, and the broken line designated by c indicates the vibrational characteristic of each back yoke 14.
As is apparent from FIG. 4, the vibrational characteristic of the objective lens 1 is the same as the vibrational characteristic of the objective lens 1 of the conventional actuator shown in FIG. 8. The vibrational characteristics of the magnet 15 and the back yoke 14 are, however, different from the vibrational characteristics of the magnet 15 and the back yoke 14 of the conventional actuator shown in FIG. 8.
Since the magnet 15 is held on the back yoke 14 with the elastic support member 21 disposed therebetween, the magnet 15, as it is vibrating under a reaction force resulting from the accelerated objective lens holder 1, undergoes resonance vibration as indicated by the solid line b in FIG. 4. The frequency f of resonance vibration is determined by the mass of the magnet 15 and the spring constant of the resilient support member 21. In a frequency range exceeding the resonance frequency f, the vibration of the magnet 15 changes to follow the characteristic of a secondary system in the same manner as the vibration of the objective lens holder 1.
On the other hand, when the objective lens holder 1 is accelerated, the back yoke 14 is caused to vibrate under a reaction force applied through the elastic support member 21. In this instance, vibration of the back yoke 14 changes to follow the characteristic of the secondary system until the resonance frequency f is reached and thereafter changes to follow the characteristic of a quaternary system.
As obvious from the vibrational characteristics of the respective components of the actuator described above, the elastic support members 21 serve as a mechanical filter (or damper) which substantially dampens or takes up a reaction force resulting from an acceleration of the objective lens holder 1 before it is transmitted to the components disposed downstream of the back yoke 14, such as the side yoke 17 and the fixed optical base 12. As a consequence, the optical components and the photoelectric transducer, which are disposed in an optical path extending between the fixed optical base 12 and the optical disk 7, are unlikely to vibrate at a high frequency beyond the resonance frequency f. The control system used to perform the follow-up control of the objective lens 2 relative to the optical disk 7 is, therefore, protected from oscillation and, hence, an accurate recording/reproducing of information on the optical disk 7 is possible.
Furthermore, owing to the filter effect (or damper effect) of the elastic support member 21, vibration is unlikely to transmit to the spindle motor 22. The optical disk 7 is free from vibration and enables the objective lens 2 to access to a desired point on the recording surface of the optical disk 7. Thus, information can accurately be recorded on, or reproduced from, the optical disk 7.
Obviously, the elastic support members 21 also provide the same filter effect when the tracking coils 3 are excited.
It is preferable that the resonance frequency f, i.e. the cutoff frequency of the filter provided by the elastic support members 21 is set at a frequency level below the node of a servo gain of the objective lens 2.
In general, the node of the servo gain is set at a frequency in the range of 1-4 KHz. In this frequency range, however, the optical components of the fixed optical base 12 and the components of the magnetic circuit are susceptible to resonance vibration. A sufficient filter effect against such resonance vibration is obtained when the cutoff frequency f is set in the range of 100-700 Hz.
The optical unit actuator of the second embodiment shown in FIG. 3 operates in the same principle as the actuator of the first embodiment. FIG. 5 shows amplitude-to-vibration performance curves of various components of the actuator of the second embodiment which are obtained when the tracking coils 33 are excited to move the objective lens holder 31 in the tracking direction of the optical disk 7. In this Figure, the solid line designated by a indicates the vibrational characteristic of the objective lens holder 31, the chain line designated by b indicates the vibrational characteristic of each tracking magnet 15, and the broken line designated by c indicates the vibrational characteristic of the actuator base 35.
When the objective lens holder 31 is driven in the tracking direction, a reaction force is produced as a result of acceleration of the objective lens holder 31. The reaction force subsequently generates vibration, however, the thus generated vibration is substantially absorbed or taken up by the elastic support members 39 before it is transmitted to the actuator base 35 and the optical base 42. The elastic support members 39 serve as a mechanical filter. The elastic support members 40 also provide a filter effect when the focusing coils 34 are excited. The elastic support members 39, 40 have a cutoff frequency which is determined in the same manner as the cutoff frequency of the elastic support members 21 described above.
In the actuator of the second embodiment, the elastic support members 50 are provided on the corresponding magnets 48 which are provided for supplying magnetic flux to the linear motor coils 45 so as to move the optical base 42 in the radial direction of the optical disk 7. The elastic support members 50 thus provided serve to lower the level of vibration caused by a reaction force which acts on the magnets 48 as a result of acceleration of the optical base 42 while the optical base 42 is moving in the radial direction of the optical disk 7. The drive base 46 and the spindle motor 51 are, therefore, subjected to vibration of a very low level which is no longer effective to induce resonance vibration of the optical disk 7. The node of a gain of the linear motor is set at a relatively low frequency level as compared to the gain node of the objective lens 32, so that the cutoff frequency c of the elastic support members 50 must be set within an appropriate frequency range to conform to the gain node of the linear motor.
As described above, the optical unit actuators of the foregoing embodiments, as against the conventional actuator, includes an elastic support member associated with a magnet which supplies magnetic flux to a coil for driving an optical unit and an objective lens mounted thereon.
With this construction, even when the magnet is vibrating at a relatively large amplitude such as several hundred μm due to resonance vibration of the associated elastic support member, vibration of the magnet does not exert negative influence at all on the vibrational characteristic of the optical unit including the objective lens which is driven by the coil disposed in a parallel magnetic field produced by the magnet.
The actuators of the first and second embodiments described above are of the moving coil type. The present invention is also applicable to a moving magnet type actuator which comprises an optical unit including a magnet and movable in a predetermined direction relative to the optical disk, and a fixed unit including a coil supported thereon by an elastic support member. The elastic support member may be a metal plate spring, a plastic plate spring or the like so long as it possesses the same filter effect.
The optical unit actuator for information recording/reproducing apparatus according to this invention includes a coil secured to a movable optical unit having an objective lens, and a magnet held by an elastic support member on a fixed unit which is stationary as against the displacement of the movable optical unit. The elastic support member is simple in construction and possesses a filter effect which is capable of substantially dampening or taking up vibration caused by a reaction force as a result of an acceleration produced when the optical unit is driven. Thus, the optical components of the fixed unit and the optical disk do not cause resonance vibration and the control characteristics of the optical disk, the optical head and the control circuit for the optical head can, therefore, be maintained. As a result, information is accurately recorded on, or reproduced from, the optical disk.
Obviously various minor changes and modifications of the present invention are possible in the light of the above teaching. It is therefore to be understood that within the scope of the appended claims the invention may be practiced otherwise than as specifically described.
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An optical unit actuator for an optical information recording/reproducing apparatus includes an electromagnetic drive mechanism composed of a coil and a magnet cooperative to drive an objective lens mounted on an optical unit. One of the coil and the magnet is secured to the optical unit. The other of the coil and the magnet is held on a fixed unit with an elastic support member disposed therebetween, the fixed unit being immovable as against the movable optical unit. The elastic support member substantially dampens or takes up vibration caused by a reaction force creased as a result of acceleration of the objective lens when the objective lens is driven to follow a dynamic radial runout and an axial deflection of an optical disk. With the elastic support member thus provided, an optical component, a photo-electric transducer or the optical disk which is disposed on the side of the fixed unit is isolated from vibration. The control characteristics of a system including an optical head, the optical disk and a control circuit for the optical head can, therefore, be improved.
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FIELD OF THE INVENTION
The present invention relates to a plunger lift apparatus for the lifting of formation liquids in a hydrocarbon well. More specifically, the plunger comprises an internal nozzle apparatus that operates to propel one or more jets of gas through an internal aperture and into a liquid load, transferring gas into the liquid load and causing an aeration of the liquid load during lift.
BACKGROUND OF THE INVENTION
A plunger lift is an apparatus that is used to increase the productivity of oil and gas wells. Nearly all wells produce liquids. In the early stages of a well's life, liquid loading is usually not a problem. When rates are high, the well liquids are carried out of the well tubing by the high velocity gas. As a well declines, a critical velocity is reached below which the heavier liquids do not make it to the surface and start to fall back to the bottom, exerting back pressure on the formation and loading up the well. A plunger system is a method of unloading gas in high ratio oil wells without interrupting production. In operation, the plunger travels to the bottom of the well where the loading fluid is picked up by the plunger and is brought to the surface removing all liquids in the tubing. The plunger also helps keep the tubing free of paraffin, salt or scale build-up.
A plunger lift system works by cycling a well open and closed. During the open time, a plunger interfaces between a liquid slug and gas. The gas below the plunger will push the plunger and liquid to the surface. This removal of the liquid from the tubing bore allows an additional volume of gas to flow from a producing well. A plunger lift requires sufficient gas presence within the well to be functional in driving the system. Oil wells making no gas are thus not plunger lift candidates.
A typical installation plunger lift system 100 can be seen in FIG. 1 . Lubricator assembly 10 is one of the most important components of plunger system 100 . Lubricator assembly 10 includes cap 1 , integral top bumper spring 2 , striking pad 3 , and extracting rod 4 . Extracting rod 4 can be employed depending on the plunger type. Within lubricator assembly 10 is plunger auto catching device 5 and plunger sensing device 6 .
Sensing device 6 sends a signal to surface controller 15 upon plunger 200 arrival at the well top. Plunger 200 can be the plunger of the present invention or other prior art plungers. Sensing the plunger is used as a programming input to achieve the desired well production, flow times and wellhead operating pressures.
Master valve 7 should be sized correctly for the tubing 9 and plunger 200 . An incorrectly sized master valve 7 will not allow plunger 200 to pass through. Master valve 7 should incorporate a full bore opening equal to the tubing 9 size. An oversized valve will allow gas to bypass the plunger causing it to stall in the valve.
If the plunger is to be used in a well with relatively high formation pressures, care must be taken to balance tubing 9 size with the casing 8 size. The bottom of a well is typically equipped with a seating nipple/tubing stop 12 . Spring standing valve/bottom hole bumper assembly 11 is located near the tubing bottom. The bumper spring is located above the standing valve and can be manufactured as an integral part of the standing valve or as a separate component of the plunger system. The bumper spring typically protects the tubing from plunger impact in the absence of fluid. Fluid accumulating on top of plunger 200 may be carried to the well top by plunger 200 .
Surface control equipment usually consists of motor valve(s) 14 , sensors 6 , pressure recorders 16 , etc., and an electronic controller 15 which opens and closes the well at the surface. Well flow ‘F’ proceeds downstream when surface controller 15 opens well head flow valves. Controllers operate on time and/or pressure to open or close the surface valves based on operator-determined requirements for production. Additional features include: battery life extension through solar panel recharging, computer memory program retention in the event of battery failure and built-in lightning protection. For complex operating conditions, controllers can be purchased that have multiple valve capability to fully automate the production process.
FIGS. 2 , 2 A, 2 B and 2 C are side views of various plunger mandrel embodiments. Although an internal mandrel orifice 44 may or may not be present in prior art plungers, such an orifice can define a passageway for the internal nozzle of the present device. Each mandrel shown comprises a male end sleeve 41 . Threaded male area 42 can be used to attach various top and bottom ends as described below in FIGS. 3 , 3 A, 3 B and 3 C.
A. As shown in FIG. 2B , plunger mandrel 20 is shown with solid ring 22 sidewall geometry. Solid sidewall rings 22 can be made of various materials such as steel, poly materials, Teflon®, stainless steel, etc. Inner cut grooves 30 allow sidewall debris to accumulate when a plunger is rising or falling. B. As shown in FIG. 2C , plunger mandrel 80 is shown with shifting ring 81 sidewall geometry. Shifting rings 81 allow for continuous contact against the tubing to produce an effective seal with wiping action to ensure that most scale, salt or paraffin is removed from the tubing wall. Shifting rings 81 are individually separated at each upper surface and lower surface by air gap 82 . C. As shown in FIG. 2 , plunger mandrel 60 has spring-loaded interlocking pads 61 in one or more sections. Interlocking pads 61 expand and contract to compensate for any irregularities in the tubing, thus creating a tight friction seal. D. As shown in FIG. 2A , plunger mandrel 70 incorporates a spiral-wound, flexible nylon brush 71 surface to create a seal and allow the plunger to travel despite the presence of sand, coal fines, tubing irregularities, etc. E. Flexible plungers (not shown) are flexible for coiled tubing and directional holes, and can be used in straight standard tubing as well.
FIGS. 3 , 3 A, 3 B and 3 C are side views of fully assembled plungers each comprising a fishing neck ‘A’. Each plunger comprises a bottom striker 46 suited for hitting the well bottom.
Recent practices toward slim-hole wells that utilize coiled tubing also lend themselves to plunger systems. With the small tubing diameters, a relatively small amount of liquid may cause a well to load-up, or a relatively small amount of paraffin may plug the tubing.
Plungers use the volume of gas stored in the casing and the formation during the shut-in time to push the liquid load and plunger to the surface when the motor valve opens the well to the sales line or to the atmosphere. To operate a plunger installation, only the pressure and gas volume in the tubing/casing annulus is usually considered as the source of energy for bringing the liquid load and plunger to the surface.
The major forces acting on the cross-sectional area of the bottom of the plunger are:
The pressure of the gas in the casing pushes up on the liquid load and the plunger. The sales line operating pressure and atmospheric pressure push down on the plunger. The weight of the liquid and the plunger weight push down on the plunger. Once the plunger begins moving to the surface, friction between the tubing and the liquid load acts to oppose the plunger. In addition, friction between the gas and tubing acts to slow the expansion of the gas.
In some cases, a large liquid loading can cause the plunger lift to operate at a slowed rate. A well's productivity can be impacted by the lift rate. Thus a heavy liquid load can be a major factor on a well's productivity.
SUMMARY OF THE INVENTION
The present apparatus provides a plunger lift apparatus that can more effectively lift a heavy liquid. In short, a heavy liquid load can be brought to the surface at a higher rise velocity.
One or more internal orifices allow for a transfer of gas from the well bottom into the liquid load during plunger lift. This jetting of the gas causes an aeration to occur so the plunger may carry a heavy liquid load to the well top in an improved manner. In addition, a liquid load can rise at a higher velocity. The apparatus can increase the production of liquid allowing for a faster rise velocity with a fixed liquid load.
One aspect of the present invention is to provide a plunger apparatus that can have an extended capacity in carrying a liquid load to the well top.
Another aspect of the present invention is to increase lift velocity of the plunger and liquid load when rising to the well top.
Another aspect of the present invention is to provide a means for transferring momentum from gas at the well bottom through a gas jet and onto a liquid load to assist with overall plunger lift load.
Another aspect of the present invention is to provide a plunger that can be used with any existing plunger sidewall geometry.
Other aspects of this invention will appear from the following description and appended claims, reference being made to the accompanying drawings forming a part of this specification wherein like reference characters designate corresponding parts in the several views.
The present invention comprises a plunger lift apparatus having a top section with an inner longitudinal orifice and one or more nozzle exit apertures (orifices) at or near its upper surface. The top section can comprise a standard American Petroleum Institute (API) fishing neck, if desired, but other designs are possible. A mandrel mid section allowing for the various sidewall geometries comprises an internal orifice throughout its length. A lower section also comprises an internal longitudinal orifice. The sections can be assembled to form the liquid aeration plunger of the present invention. Gas passes through an internal plunger conduit (orifice), up through an internal nozzle, and out through one or more apertures thereby transferring momentum from a gas to a liquid load providing a lift assist and causing gaseous aeration of the liquid load.
When the surface valves open to start the lift process, down hole pressure will result in gas being forced through the plunger nozzles, exiting one or more apertures into the liquid load transferring momentum from the jetting gas onto the liquid load. The gas transfer causes aeration and results in a liquid lift assist. The plunger may carry a heavier liquid load to the well top because the aeration effectively lightens the load. The present apparatus can carry a fixed liquid load at an improved velocity as compared to a non-aerated liquid load. Applying a soapy mixture down to the well bottom between the well casing and tubing can assist the aeration process by allowing a higher surface tension in the gaseous bubbles formed within the liquid load.
An additional embodiment incorporates a nozzle type aerator in a bypass plunger design, employing the same basic concept of momentum transfer and gaseous aeration of the liquid load.
The present apparatus allows for improved productivity in wells that have large levels of loaded liquid. The disclosed plunger allows for a more efficient lift of high liquid loads both increasing the lift capacity and also the lift velocity by aerating the liquid load during plunger lift. The liquid aeration plunger is easy to manufacture, and easily incorporates into the design into existing plunger geometries.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 (prior art) is an overview depiction of a typical plunger lift system installation.
FIGS. 2 , 2 A, 2 B and 2 C (prior art) are side views of plunger mandrels with various plunger sidewall geometries.
FIGS. 3 , 3 A, 3 B and 3 C (prior art) are side views of fully assembled plungers each shown with a fishing neck top and utilizing various plunger sidewall geometries.
FIG. 4 is a cross-sectional view of an upper section embodiment of a liquid aeration plunger showing an internal orifice, nozzles, and nozzle exit apertures.
FIG. 5 is an isometric cut away view of a liquid aeration plunger embodiment.
FIG. 6 is an isometric cut away view of a liquid aeration plunger embodiment during a plunger lift.
FIGS. 7 , 7 A, 7 B and 7 C (prior art) show side views of variable orifice bypass valves and plunger mandrels with various sidewall geometries.
FIG. 8A (prior art) is a side cross-sectional view of a variable orifice bypass valve assembly with the actuator rod shown in the open (or bypass) position.
FIG. 8B (prior art) is a side cross-sectional view of a variable orifice bypass valve assembly and similar to FIG. 8A but with the actuator rod shown in its closed (no bypass) position.
FIG. 9 is a top view of a grooved actuator rod.
FIGS. 9A , 9 B show cross sectional views of possible modifications of an actuator rod for a bypass valve assembly to allow for gas entry in a closed position.
FIG. 9C is a cross sectional view of FIG. 9 along line 9 C- 9 C.
FIGS. 10 , 10 A, 10 B are side cross-sectional views of the embodiments shown in FIGS. 9C , 9 A and 9 B respectively.
Before explaining the disclosed embodiments of the present invention in detail, it is to be understood that the invention is not limited in its application to the details of the particular arrangement shown, since the invention is capable of other embodiments. Also, the terminology used herein is for the purpose of description and not of limitation.
DETAILED DESCRIPTION OF THE INVENTION
Referring now to the drawings, the present invention is a liquid aeration plunger 2000 apparatus ( FIG. 5 ) having an upper section 200 (FIGS. 4 , 5 ) with an inner longitudinal orifice and one or more nozzle exit apertures at or near its upper end. The top section can comprise a standard American Petroleum Institute (API) fishing neck, if desired, but other designs are possible. The plunger has a mandrel mid section that can accommodate various sidewall geometries, an internal orifice throughout its length and a lower section 46 A ( FIG. 5 ) with an internal longitudinal orifice.
All the sections can be connected together to allow the gaseous aeration of the liquid load by the plunger of the present invention. When the surface valves open to start the lift process, gas is forced through the plunger nozzles. As the gas exits from the apertures into the liquid load, transferring momentum from the gas to the liquid, a turbulent and gaseous aeration of the liquid occurs. This action results in a more efficient lift of the liquid to the well top.
FIG. 4 is a cross-sectional view of upper section 200 of the liquid aeration plunger shown in FIG. 5 . The upper external end is a prior art fishing neck ‘A’ design. Upper section 200 is shown with four nozzle exit apertures 52 dispersed evenly around its upper surface, with each exiting at about 45° to the liquid load boundary. Upper section 200 can easily connect to any mandrel such as that shown in FIGS. 2 , 2 A, 2 B and 2 C. Internal female sleeve orifice 58 mates with the male end sleeve 41 and threaded internal female sleeve orifice 56 mates with threaded male area 42 . Upper section internal through-orifice 54 can communicate with each nozzle exit orifice 53 . It should be noted that the nozzle quantity, location, size and designs are offered by way of example and not limitation. For example, four nozzle orifices 53 and four aperture exits 52 are shown, each at about a 45° cut angle into upper section orifice 54 . However, the present invention is not limited to the design shown. Other nozzle designs could easily be incorporated to encompass one or more exit nozzle apertures, various size nozzle holes, various angles, etc.
The upper end has at least one exit orifice that has a total cross sectional area in the range of about 0.25% to 10% of the maximum plunger cross sectional area. Typically, the smallest range of the cross sectional area of either the lower end apertures or the upper end apertures or the internal longitudinal orifice is about 3.22 mm 2 (about 0.005 inch 2 ) to about 32.3 mm 2 (about 0.05 inch 2 ). In FIG. 4 , the four nozzle orifices are each typically about 2.36 mm (about 0.093 inch) in diameter, combining to about 17.4 mm 2 (about 0.027 inch 2 ) of area as compared to the outside diameter of a typical plunger of about 47 mm (about 1.85 inch) or about 1735 mm 2 (about 2.69 inch 2 ).
FIG. 5 is an isometric cut side view of liquid aeration plunger 2000 . In this embodiment, upper section 200 , solid wall plunger mandrel 20 , and lower section 46 A, are shown having interconnected internal orifices. Lower section 46 A is modified from present art by providing lower section internal orifice 44 A. Lower section 46 A can be attached to a mandrel by mating male end sleeves 41 and threaded male areas 42 , previously shown in FIGS. 2 , 2 A, 2 B and 2 C.
Liquid aeration plunger 2000 functions to allow gas to pass into lower section 46 A at lower entry aperture 48 , up through lower section internal orifice 44 A, through internal mandrel orifice 44 , then up through upper section internal through-orifice 54 , through nozzle exit orifices 53 and finally exiting out of apertures 52 . It should also be noted that the size of nozzle exit orifices 53 and apertures 52 control the amount of gas jetting. The depicted embodiment design is shown by way of example and not limitation. It should be noted that although the mandrel shown is solid wall plunger mandrel 20 , any other sidewall geometry can be utilized including all aforementioned sidewall geometries. Lower section internal orifice 44 A, internal mandrel orifice 44 , and upper section internal through-orifice 54 can be manufactured in various internal dimensions.
FIG. 6 shows liquid aeration plunger 2000 during a plunger lift. When the surface valves open to start the lift process, gas G enters the plunger lower entry aperture 48 , passes up through all internal orifices ( 44 A, 44 , 54 , 53 ), exits apertures 52 in directions E, and jets into the liquid load L to form bubbles B in a turbulent fashion. This action results in a transfer of momentum from the jetting gas into the liquid load. The gaseous jetting, turbulence and aeration of the liquid is a result of the momentum transfer. The plunger may carry a heavier than average liquid load to the well top, thereby increasing the load capacity and/or allowing for a faster rise velocity of a given liquid load. The result is an increase in well productivity for wells with high liquid loads.
Injecting a soapy mixture S down to the well bottom between the aforementioned well casing 8 and tubing 9 can assist the aeration process by allowing a higher surface tension in the gaseous bubbles B formed within the liquid load L. Liquid aeration plunger 2000 can easily be manufactured with any existing plunger sidewall geometry.
Another embodiment of the present invention incorporates a nozzle type aerator in a bypass plunger design, employing the same basic concept of momentum transfer and gaseous aeration of the liquid load. Bypass plungers typically have an actuator that is in a ‘open’ position during plunger descent to the well bottom and is in a ‘closed’ position during a plunger rise to the well top. Modifications to the actuator rod, to the bypass valve, or mandrel housing at the closed interface can be made to accommodate an orifice or an aperture for gas jetting. In an embodiment modifying a typical bypass valve, one or more small apertures or orifices within the actuator rod provide for gas jetting into the liquid load during the ‘closed’ position of the actuator rod. Thus when in a ‘closed’ position, the bypass plunger will function via the transfer of momentum and gas jetting causing aeration of the liquid load.
FIGS. 7 , 7 A, 7 B and 7 C show side views of variable orifice bypass valves (VOBV) 300 . Pad plunger mandrel section 60 A, brush plunger mandrel section 70 A, solid ring plunger mandrel section 20 A, and shifting ring plunger mandrel section 80 A can each be mounted to a VOBV 300 by mating female threaded end 64 and male threaded end 66 . Each plunger 61 , 71 , 21 and 81 is shown in an unassembled state. A standard American Petroleum Institute (API) internal fishing neck can also be used. Each mandrel section also has hollowed out core 67 . Each depicted bottom section is a VOBV 300 shown in its full open (or full bypass) set position. The bypass function allows fluid to flow through during the return trip to the bumper spring with the bypass closing when the plunger reaches the well bottom. The bypass feature optimizes plunger travel time in high liquid wells. The present invention is not limited by the specific design of bypass valve and VOBV is shown only as an example.
FIG. 8A is a side cross-sectional view of a prior art VOBV assembly 300 with actuator rod 25 shown in the open (or bypass) position. VOBV assembly 300 threaded interface 64 joins to a mandrel section via mandrel threads 66 (See FIGS. 7 , 7 A, 7 B and 7 C). When VOBV assembly 300 arrives at the well top, the aforementioned striker rod within the lubricator hits actuator rod 25 at rod top end 37 moving actuator rod 25 in direction P to its open position. In its open position, the top end of actuator rod 25 rests against variable control cylinder 26 internal surface. Brake clutch 21 will hold actuator rod 25 in its open position allowing well loading (gas/fluids, etc.) to enter the open orifice and move up through the hollowed out section of bypass plunger during plunger descent. This feature optimizes its descent to the well bottom as a function of the bypass setting. Access hole 29 is for making adjustments to the bypass setting via variable orifice opening 31 . In other words, the amount of gas allowed to enter the bypass valve can be adjusted.
FIG. 8B is a side cross-sectional view of a prior art VOBV assembly 300 and similar to FIG. 8A but with actuator rod 25 depicted in its closed (no bypass) position. When bottom bumper spring striker end 34 hits the well bottom, the actuator rod 25 moves in direction C to a closed position. In the closed position, rod top end 37 with its slant surface 36 closes against threaded top section end 66 and is held in the closed position by brake clutch 21 thus allowing VOBV 300 to be set in a closed bypass condition to enable itself to rise back to the well top.
FIGS. 9A , 9 B show possible modifications of actuator rod 25 which are described in more detail below. When actuator rod 25 is in a closed position, there is a seal along slant surface 36 , which prevents gas flow through the VOBV. The modifications of the embodiment of the present invention will allow for small gas exit aperture(s) when modified actuator rods are in a closed position ( FIG. 8B ). Allowing a portion of gas to exit when in a closed position will cause the aforementioned momentum transfer from the gas into the liquid load within central hollowed out core 67 (see FIGS. 10 , 10 A, 10 B) and will result in a liquid lift assist in a bypass plunger. The modifications are shown by way of example and not limitation of the present invention.
FIGS. 9 , 9 C are views of grooved actuator rod 25 A comprising four grooves 94 cut partially into actuator rod top surface 37 , into slant surface 36 and down top side surface 39 . The number and the type of grooves are shown by way of example and not limitation. For example, grooves also could be cut into the mating sidewall of VOBV/mandrel (not shown). In the embodiment shown, section A-A defines a cross section of grooved actuator rod 25 A. Gas would pass into the liquid residing within each mandrel section hollowed out core 67 via grooves 94 . Also shown in dotted line format is an alternate design comprising top slant holes 96 which could be drilled from top surface 37 to just below side surface 39 . Slant holes 96 could replace the aforementioned grooves 94 . Equivalent designs could include a metal burr acting to keep one rod slightly open in the closed position.
FIG. 9A is a side cross-sectional view of split orifice actuator rod 25 B comprising central orifice 74 , and four connected orifices 76 positioned about 45° from each other. Gas enters at gas entry aperture 86 located at actuator rod bottom surface 34 . The gas moves up through central orifice 74 , then through nozzle orifices 76 , and exits into the liquid load from apertures 78 located along actuator rod top surface 37 .
FIG. 9B is a side cross-sectional view of center orifice actuator rod 25 C comprising central through orifice 84 . Gas enters aperture 86 along actuator rod bottom surface 34 and gas exits aperture 88 at actuator rod top surface 37 .
FIGS. 10 , 10 A, 10 B are side cross-sectional views of the embodiments shown in FIGS. 9C , 9 A and 9 B, respectively. Each design is shown by way of example and not limitation. In each case a limited amount of gas is allowed to exit the seal area of the VOBV when the actuator is in a closed position and when the down hole pressure allows gas to be jetted through the valve.
FIG. 10 shows VOVB assembly 300 A in a closed position. When down hole pressure is released, gas enters variable orifice opening 31 and/or access hole 29 (see FIG. 8 A) and jets through grooves 94 , transferring gas in direction GE to liquid load L. Also shown are the top slant holes 96 which could be drilled from top surface 37 to below the side surface. Slant holes 96 could replace grooves 94 .
FIG. 10A is a side cross-sectional view showing split orifice actuator rod 25 B in a closed position within VOBV assembly 300 B. Split orifice actuator rod 25 B is modified to comprise central orifice 74 and four connected orifices 76 positioned about 45° from each other. Gas G enters at gas entry aperture 86 located at actuator rod bottom surface 34 . The gas moves up through central orifice 74 , through nozzle orifices 76 , and exits in direction GE into the liquid load L from apertures 78 located along actuator rod top surface 37 .
FIG. 10B is a side cross-sectional view showing center orifice actuator rod 25 B in a closed position within VOBV assembly 300 C. Center orifice actuator rod 25 B comprises central through orifice 84 . Gas G enters aperture 86 along actuator rod bottom surface 34 and exits out gas exit aperture 88 in direction GE and into the liquid load L.
An actuator rod or side escape of the actuator rod or seal area has at least one exit orifice with a total cross sectional area in the range of about 0.25% to about 10% of the maximum plunger cross sectional area. Typically, the smallest range of the cross sectional area of the apertures (or escape area), which exit gas into hollowed out core 67 , is about 3.22 mm 2 (about 0.005 inch 2 ) to about 32.3 mm 2 (about 0.05 inch 2 ). As an example, and not a limitation, in FIG. 10A the four nozzle orifices are each typically about 2.36 mm (about 0.093 inch) in diameter, combining to about 17.4 mm 2 (about 0.027 inch 2 ) of area as compared to the outside diameter of a typical plunger of about 47 mm (about 1.85 inch) or about 1735 mm 2 (about 2.69 inch 2 ).
Examples shown above in FIGS. 9 , 9 A, 9 B, 10 , 10 A and 10 B are shown by way of example and not limitation for variable type bypass valve embodiments. Modifications to fixed bypass valves, although not specifically shown, can also provide for the gas jetting in a similar manner as described above.
The liquid turbulence and aeration caused by the energy transfer allows for improved efficiency and productivity in wells that have high levels of liquid. The gas jetting allows for a more efficient lift of large liquid loads by increasing the plunger lift capacity of a liquid load and/or increasing the lift velocity of a given load. The liquid aeration plunger is easy to manufacture, and can easily be incorporated into the design of existing plunger geometries. As previously described, applying a soapy mixture down to the well bottom between the well casing and tubing can assist the aeration process by allowing a higher surface tension in the gaseous bubbles formed within the liquid load.
It should be noted that although the hardware aspects of the of the present invention have been described with reference to the depicted embodiment above, other alternate embodiments of the present invention could be easily employed by one skilled in the art to accomplish the gas momentum aspect of the present invention. For example, it will be understood that additions, deletions, and changes may be made to the orifices, apertures, or other interfaces of the plunger with respect to design other than those described herein.
Although the present invention has been described with reference to the depicted embodiments, numerous modifications and variations can be made and still the result will come within the scope of the invention. No limitation with respect to the specific embodiments disclosed herein is intended or should be inferred.
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A plunger apparatus operates to propel one or more jets of gas through one or more internal orifices and/or nozzles out through an aperture and into a liquid load whereby a transfer of the gas into the liquid load causes turbulent aeration to the liquid load during a plunger rise. This action can boost the carrying capacity of a plunger lift system resulting in improved well production.
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CROSS REFERENCE TO RELATED APPLICATION(S)
The present invention is a Continuation-in-Part Application of co-pending, commonly assigned U.S. patent application Ser. No. 12/195,670, filed Aug. 21, 2008; U.S. patent application Ser. No. 12/204,958, filed Sep. 5, 2008; and U.S. patent application Ser. No. 12/353,764, filed Jan. 14, 2009, all of which are incorporated herein in their entirety.
FIELD OF THE INVENTION
The present invention relates to a multilayer modular energy harvesting apparatus, system for using said apparatus and method for implementation said apparatus.
BACKGROUND OF THE INVENTION
Piezoelectricity is the ability of certain crystalline materials to develop an electrical charge proportional to an applied mechanical stress. The converse effect can also be seen in these materials where strain is developed proportional to an applied electrical field. The Curie's originally discovered it in the 1880's. Today, piezoelectric materials for industrial applications are lead based ceramics available in a wide range of properties. Piezoelectric materials are the most well known active material typically used for transducers as well as in adaptive structures.
Mechanical compression or tension on a poled piezoelectric ceramic element changes the dipole moment, creating a voltage. Compression along the direction of polarization, or tension perpendicular to the direction of polarization, generates voltage of the same polarity as the poling voltage. Tension along the direction of polarization, or compression perpendicular to the direction of polarization, generates a voltage with polarity opposite that of the poling voltage. These actions are generator actions—the ceramic element converts the mechanical energy of compression or tension into electrical energy. This behavior is used in fuel-igniting devices, solid state batteries, force-sensing devices, and other products. Values for compressive stress and the voltage (or field strength) generated by applying stress to a piezoelectric ceramic element are linearly proportional up to a material-specific stress. The same is true for applied voltage and generated strain.
The review article “Advances In Energy Harvesting Using Low Profile Piezoelectric Transducers” by Shashank Priya, published in J Electroceram (2007) 19:165-182 provides a comprehensive coverage of the recent developments in the area of piezoelectric energy harvesting using low profile transducers and provides the results for various energy harvesting prototype devices. A brief discussion is also presented on the selection of the piezoelectric materials for on and off resonance applications.
The paper “On Low-Frequency Electric Power Generation With PZT Ceramics” by Stephen R. Platt, Shane Farritor, and Hani Haider, published in IEEE/ASME Transactions On Mechatronics, VOL. 10, NO. 2, April 2005 discusses the potential application of PZT based generators for some remote applications such as in vivo sensors, embedded MEMS devices, and distributed networking. The paper points out that developing piezoelectric generators is challenging because of their poor source characteristics (high voltage, low current, high impedance) and relatively low power output.
The article “Energy Scavenging for Mobile and Wireless Electronics” by Joseph A. Paradiso and Thad Starner, published by the IEEE CS and IEEE ComSoc, 1536-1268/05 reviews the field of energy harvesting for powering ubiquitously deployed sensor networks and mobile electronics and describers systems that can scavenge power from human activity or derive limited energy from ambient heat, light, radio, or vibrations.
In the review paper “A Review of Power Harvesting from Vibration using Piezoelectric Materials” by Henry A. Sodano, Daniel J. Inman and Gyuhae Park published in The Shock and Vibration Digest, Vol. 36, No. 3, May 2004 197-205, Sage Publications discuses the process of acquiring the energy surrounding a system and converting it into usable electrical energy—termed power harvesting. The paper discuss the research that has been performed in the area of power harvesting and the future goals that must be achieved for power harvesting systems to find their way into everyday use.
Intl. Patent Application WO/07/038157A2 entitled “Energy Harvesting Using Frequency Rectification” to Carman Gregory P. and Lee Dong G.; filed: Sep. 21, 2006 discloses an energy harvesting apparatus for use in electrical system, having inverse frequency rectifier structured to receive mechanical energy at frequency, where force causes transducer to be subjected to another frequency.
U.S. Pat. No. 5,265,481 to Sonderegger, Hans C., et al. entitled “Force sensor systems especially for determining dynamically the axle load, speed, wheelbase and gross weight of vehicles” discloses sensor system incorporated in road surface—has modular configuration for matching different road widths.
SUMMARY OF THE INVENTION
The present invention relates to a multilayer modular energy harvesting apparatus, system for using said apparatus and method for implementation said apparatus.
According to an exemplary embodiment of the invention, a multilayer generator is provided comprising: a box having a top cover; a bottom electrode placed above the bottom of said box; a top electrode placed below said top cover; and a multilayer electricity generating structure positioned between said bottom electrode and top electrode, each layer of said multilayer electricity generating structure comprising a plurality of piezoelectric rods held in place by a matrix layers, wherein: thickness of said matrix layer is smaller than length of said plurality of piezoelectric rods in the corresponding layer, said piezoelectric rods are oppositely poled in alternating layers, adjacent layers are separated by a central electrode.
In some embodiments, said box and said matrix layers are substantially cylindrical.
In some embodiments, said box constructed of a round top cover, a round bottom cover and a cylindrical mid section.
In some embodiments, said round top cover and said round bottom cover are substantially identical.
In some embodiments, said matrix layers are shaped and sized to snugly fit inside said box.
In some embodiments, said matrix layers are configured to withstand sheer stresses in said plurality of piezoelectric rods due to pressure applied on said cover.
In some embodiments, said matrix layers are made of a non-conductive material selected from the group comprising: glass; PLEXIGLAS (Extruded Acrylic Plexiglass); thermoplastics; reinforced resin and concrete.
In some embodiments, said cover is further configured such when pressure is applied to said cover, said applied pressure causes mechanical and electrical contact between ends of said piezoelectric rods and the nearest electrodes.
In some embodiments, said rods in each layer are poled in the same direction, and are electrically connected in parallel by two of said electrodes such that the charge generated by said layer is the sum of the charges generated by all the rods in said layer.
In some embodiments, said alternating electrode layers are joined such that the voltage generated by said entire multilayer generator is substantially equal to the voltage generated by one rod, and the charge generated by said entire multilayer generator is substantially equal to the sum of charges generated by all said rods.
In some embodiments, said generator further comprising fasteners, wherein said fasteners are configured to apply preloading force on said cover.
In some embodiments, said cover is stiff and is configured to substantially evenly spread force applied to said cover among said piezoelectric rods.
In some embodiments, said generator further comprising a load spreading layer situated between said cover and said top electrode, said load spreading layer configured to receive force applied to said cover and to substantially evenly spread force among said piezoelectric rods.
In some embodiments, said at least one of said box and said cover is made of concrete.
In some embodiments, said box and said matrix layers are shaped as polygons.
In some embodiments, said generator further comprising a seal situated between said box and said cover.
According to another exemplary embodiment of the invention, a multilayer super-module generator is provided comprising: a box having a plurality of chambers; and at least one top cover, wherein in each chamber: a bottom electrode placed above the bottom of said chamber; a top electrode placed below said top cover; and a multilayer electricity generating structure positioned between said bottom electrode and top electrode, each layer of said multilayer electricity generating structure comprising a plurality of piezoelectric rods held in place by a matrix layers, wherein: thickness of said matrix layer is smaller than length of said plurality of piezoelectric rods in the corresponding layer, said piezoelectric rods are oppositely poled in alternating layers, adjacent layers are separated by a central electrode.
In some embodiments, each chamber has a separate top cover.
In some embodiments, all the chambers are covered by same top cover.
In some embodiments, said rods in each layer in each chamber are poled in the same direction, and are electrically connected in parallel by two of said electrodes, alternating electrode layers in each chamber are joined such that the voltage generated by said entire multilayer generator in each chamber is substantially equal to the voltage generated by one rod, and the charge generated by said entire multilayer generator is substantially equal to the sum of charges generated by all said rods, and said generators in said chambers are electrically joined in parallel.
According to another exemplary embodiment of the invention, a method of installing an energy harvesting system in a road comprising the steps of: drilling an array of circular holes in said road; cutting slots in said road, joining said circular holes; placing a round piezoelectric energy generator in each of said drilled holes; placing connecting cables in said cut slots; and covering said connecting cables in said cut slots.
In some embodiments, said method further comprising covering said round piezoelectric energy generators placed in said drilled holes.
In some embodiments, said round piezoelectric energy generators are placed in said drilled holes such that upper surface of said round piezoelectric energy generators are flush with the surface of said road.
In some embodiments, the step of drilling an array of circular holes in said road comprises using cup drill.
In some embodiments, said method further comprising pouring a reinforcing layer at the bottom of said drilled hole before placing a round piezoelectric energy generator in each of said drilled holes.
According to another exemplary embodiment of the invention, a method of installing an energy harvesting system in a railroad comprising the steps of: providing a sleeper having a cavity under the track mount; placing in said cavity a multilayer generator comprising: a bottom electrode placed above the bottom of cavity; a top electrode placed below said mount; and a multilayer electricity generating structure positioned between said bottom electrode and top electrode, each layer of said multilayer electricity generating structure comprising a plurality of piezoelectric rods held in place by a matrix layers, wherein: thickness of said matrix layer is smaller than length of said plurality of piezoelectric rods in the corresponding layer, said piezoelectric rods are oppositely poled in alternating layers, and adjacent layers are separated by a central electrode, alternating electrode layers are joined such that said rods are electrically connected in parallel; and attaching said mount and said track to said sleeper such that force applied by a train traveling over said track causes generation of electric energy in said piezoelectric rods.
Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. Although methods and materials similar or equivalent to those described herein can be used in the practice or testing of the present invention, suitable methods and materials are described below. In case of conflict, the patent specification, including definitions, will control. In addition, the materials, methods, and examples are illustrative only and not intended to be limiting.
BRIEF DESCRIPTION OF THE DRAWINGS
The invention is herein described, by way of example only, with reference to the accompanying drawings. With specific reference now to the drawings in detail, it is stressed that the particulars shown are by way of example and for purposes of illustrative discussion of the preferred embodiments of the present invention only, and are presented in the cause of providing what is believed to be the most useful and readily understood description of the principles and conceptual aspects of the invention. In this regard, no attempt is made to show structural details of the invention in more detail than is necessary for a fundamental understanding of the invention, the description taken with the drawings making apparent to those skilled in the art how the several forms of the invention may be embodied in practice.
The invention is capable of other embodiments or of being practiced or carried out in various ways. Also, it is to be understood that the phraseology and terminology employed herein is for the purpose of description and should not be regarded as limiting.
In discussion of the various figures described herein below, like numbers refer to like parts.
The drawings are generally not to scale. For clarity, non-essential elements were omitted from some of the drawings.
In the drawings:
FIG. 1( a ) depicts piezoelectric rods as used in the art.
FIG. 1( b ) depicts piezoelectric rods as used in the art.
FIG. 1( c ) depicts a multilayer piezoelectric stack according to an exemplary embodiment of the current invention.
FIG. 2( a ) schematically depicts an isometric view of a multilayer modular generator according to an exemplary embodiment of the current invention.
FIG. 2( b ) schematically depicts a cross-sectional view of a multilayer modular generator according to an exemplary embodiment of the current invention.
FIG. 3 schematically depicts an exploded view of the internal elements of a multilayer modular generator according to an exemplary embodiment of the current invention.
FIG. 4( a ) schematically depicts an isometric view of a round multilayer modular generator according to another exemplary embodiment of the current invention.
FIG. 4( b ) schematically depicts a cross-sectional view of a round multilayer modular generator according to another exemplary embodiment of the current invention.
FIG. 4( c ) schematically depicts a top view of a matrix layer used in a round multilayer modular generator according to another exemplary embodiment of the current invention.
FIG. 5( a ) illustrates a cross section of a road with round multilayer modular generators embedded in it and vehicle over it, according to another exemplary embodiment of the current invention.
FIG. 5( b ) schematically depicts the stress distribution caused by a passing vehicle on a round multilayer modular generator according to another exemplary embodiment of the current invention.
FIG. 5( c ) schematically depicts a graph of the stress distribution caused by a passing vehicle according to another exemplary embodiment of the current invention.
FIG. 6 schematically depicts a system for energy harvesting implemented in a road and using a plurality of round multilayer modular generators according to another exemplary embodiment of the current invention.
FIGS. 7( a - f ) schematically depict steps of constructing an energy harvesting system by embedding a plurality of round multilayer modular generators according to an exemplary embodiment of the current invention.
FIG. 7( a ) schematically depicts drilling, in a road, holes for embedding round multilayer modular generators, preferably using a cup drill.
FIG. 7( b ) schematically depicts drilling, in a road, holes for embedding round multilayer modular generators, preferably using a cup drill.
FIG. 7( c ) schematically depicts cutting, in a road, slits for embedding connecting cable, preferably using a disk saw.
FIG. 7( d ) schematically depicts optional stage of pouring reinforcing layer, preferably made of concrete at the bottom of the drilled hole.
FIG. 7( e ) schematically depicts the stage of laying the round multilayer modular generators and the connecting cables in the drilled holes and the cut slits respectively; and
FIG. 7( f ) schematically depicts the stage of refilling the drilled holes and the cut slits, preferably with asphalt.
FIG. 8 schematically depicts a cross section of a railway sleeper with a modular multilayer generator according to yet another exemplary embodiment of the current invention.
FIG. 9( a ) schematically depicts an isometric view of a multilayer super-module generator according to yet another exemplary embodiment of the current invention.
FIG. 9( b ) schematically depicts a system for energy harvesting, implemented in a road and using a plurality of multilayer super-module generators according to yet another exemplary embodiment of the current invention.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
The present invention relates to a modular energy harvesting apparatus, system for using said apparatus and method for implementation said apparatus.
Before explaining at least one embodiment of the invention in detail, it is to be understood that the invention is not limited in its application to the details of construction and the arrangement of the components set forth in the following description or illustrated in the drawings. The invention is capable of other embodiments or of being practiced or carried out in various ways.
FIG. 1 schematically depicts piezoelectric elements.
FIG. 1( a ) and FIG. 1( b ) depict piezoelectric rods used in the art, while FIG. 1( c ) depicts a multilayer piezoelectric stack according to an exemplary embodiment of the current invention.
FIG. 1( a ) shows a single layer piezoelectric rod used in the art for energy generation. When rod 100 , made of an elongated piezoelectric material 101 , is subjected to longitudinal force, high voltage is generated between the positive end electrode 102 and negative end electrode 104 , which are bonded to the elongated piezoelectric material 101 . It should be noted that while the generated voltage is high, the electric current that can be harvested is small. It was found that controlling a generated electrical signal having high voltage and low current is difficult. Converting such a signal to useful electrical power that can be transported, used and stored may be expensive and inefficient due to the high voltage generated.
FIG. 1( b ) schematically depicts a multilayer integrated piezoelectric rod 110 as used in the art. Integrated rod 110 comprises a plurality of layers 111 , each made of piezoelectric material, where adjacent layers are oppositely poled (three such layers are seen, but number of layer may be larger). The layers 111 are separated by electrodes, for example positive central electrode 113 and negative central electrode 115 . Central electrodes as well as end electrodes are bonded to their adjacent layer, thus creating a single monolithic, multi-layer stack. All positive electrodes (in this case positive central electrode 113 and positive end electrode 119 ) are connected together to the positive terminal 112 . Similarly, all negative electrodes (in this case negative central electrode 115 and negative end electrode 118 ) are connected together to the negative terminal 114 .
When rod 110 , is subjected to longitudinal force, a relatively voltage is generated between the positive terminal 112 and negative terminal 114 . Compared to the signal generated by single layer rod 100 , the signal generated by monolithic multilayer rod 110 is N times smaller while the generated charge (or current for the close-loop circuit) is N times larger (wherein N is the number of layers).
It should be noted that the process of bonding the electrodes and creating a monolithic multilayer stack might be expensive.
FIG. 1( c ) schematically depicts a multilayer piezoelectric stack 120 according to an exemplary embodiment of the current invention. Multilayer piezoelectric stack 120 comprises a plurality of separate piezoelectric rods 121 , each made of piezoelectric material, where adjacent layers are oppositely poled (three such layers are seen, but number of layer may be larger). The rods 121 are separated by electrodes, for example positive central electrode 123 and negative central electrode 125 . Central electrodes as well as end electrodes are not bonded to their adjacent layers, but instead make mechanical and electrical contact with the layer when the stack is under pressure. All positive electrodes (in this case positive central electrode 123 and positive end electrode 129 ) are connected together to the positive terminal 122 . Similarly, all negative electrodes (in this case negative central electrode 125 and negative end electrode 128 ) are connected together to the negative terminal 124 .
When rod 120 , is subjected to longitudinal force, voltage is generated between the positive terminal 122 and negative terminal 124 . Compared to the signal generated by single layer rod 100 , the voltage output generated by multilayer stack 120 is N times smaller while the generated charge (or current) is N times larger (wherein N is the number of layers).
As multilayer stack 120 is not bonded, it is preferably supported by an external support structure which will be seen in the following figures. Assembling the multilayer stack 120 is easy and cheap as it requires only stacking the layers and the electrodes within the supporting structure. Additionally, the support structure may be configured to prevent the multilayer stack 120 from bucking under pressure by resisting shear forces that may developed as the stack tries to bend. Thus, it may be possible to apply larger forces on a supported multilayer stack 120 than to the monolithic rod 100 .
It should be noted that piezoelectric rods 121 are appears as having cylindrical shape in FIG. 1( c ) as exemplary embodiment. Other shapes may be used. For example, rods may have square rectangular, hexagonal, oval or any other cross-section. Length of the rods may vary, wherein for the same stress, shorter rods yields lower voltage than longer rods. Shorter rods enable situating more rods along the same length of multilayer stack 120 , thus generating larger charge for the same applied longitudinal force.
FIG. 2( a ) schematically depicts an isometric view of a multilayer modular generator according to an exemplary embodiment of the current invention.
Multilayer modular generator 200 comprises a box 210 and a cover 212 . An electric cable 221 , preferably comprising a positive lead and a negative lead, transfers electrical signal generated by a plurality of supported multilayer stacks 120 within box 210 in response to pressure applied to cover 212 .
FIG. 2( b ) schematically depicts a cross-sectional view of a multilayer modular generator according to an exemplary embodiment of the current invention.
Multilayer modular generator 200 comprises a box 210 and a cover 212 . An electric cable 221 , preferably comprising a positive lead 221 a and a negative lead 221 b , transfers electrical signal generated by a plurality of supported multilayer stacks within box 210 in response to pressure applied to cover 212 . Preferably, a flexible seal 214 may be used to prevent moisture and dirt from entering the box, while allowing small relative motion of the cover in response to force applied to it.
Piezoelectric stacks within box 210 comprises of plurality of individual piezoelectric elements 201 , arranged in layers. Elements 201 in each layer are held in place by a matrix layer 231 (tree such matrix layers: 231 a , 231 b and 231 c are seen, but number of layers may be two or larger than three). Piezoelectric elements in adjacent layers are oppositely poled and are separated by central electrode layers (two such electrode layers are seen, positive central electrode layer 224 a and negative central electrode layer 224 c ). Top surfaces of piezoelectric elements in top layer make contact with top electrode layer (in the example depicted here—positive end electrode layer 224 d ). Similarly, bottom surfaces of piezoelectric elements in bottom layer make contact with bottom electrode layer (in the example depicted here—negative end electrode layer 224 a ).
All positive electrodes (in this case positive central electrode 224 b and positive end electrode 224 d ) are connected together to the positive terminal 221 a . Similarly, all negative electrodes (in this case negative central electrode 224 c and negative end electrode 224 a ) are connected together to the negative terminal 221 a.
FIG. 3 schematically depicts an exploded view of the internal elements of a multilayer modular generator 200 according to an exemplary embodiment of the current invention.
In this figure, the arrangement of piezoelectric elements 201 in a layers and columns can be seen. In each layer the piezoelectric elements 201 are arranged in a substantially identical two-dimensional array and held in place in holes 232 in the corresponding matrix layer 231 . For clarity, only few of the piezoelectric elements 201 were presented.
In the exemplary embodiment, a 3×3 array of piezoelectric elements 201 is depicted for clarity. However larger array are typically used. The array need not be square or symmetrical. Preferably, the shape of the matrix layer, the box and the cover is such that it can tile a surface (triangle, rectangular, square, or hexagonal). Similarly, any shape may be selected, such as oval, round, etc, within the general scope of the current invention.
Number of Matrix layers 231 is preferably equal to the number of layers of piezoelectric elements 201 . In the exemplary embodiment, three layers of piezoelectric elements 201 are depicted for clarity (held in place by matrix layers 231 a , 231 b and 231 c ). However any number of layers may be used.
Matrix layers 231 are preferably made of strong, nonconductive material so it can support piezoelectric elements 201 against shear stresses while electrically insulating them and the electrode layers. In a preferred embodiment of the invention, matrix layers 231 are made of glass sheets having holes 232 drilled in them. Optionally, the glass sheets are tempered or thermally treated to reduce internal stress or increase strength after holes 232 were drilled. Alternatively, glass sheet are casted. Using glass to manufacture the matrix layers is advantageous due to the mechanical and electrical properties of glass. Additionally, glass is cheap, nontoxic, easily processed, and easily disposable or recyclable. Alternatively, molded plastic is used. It should be noted that matrix layers may also be patterned with holes other than holes 232 for reducing cost and weight.
Central electrodes 224 b and 224 c as well as end electrodes 224 a and 224 d are preferably patterned having contact pads 223 electrically connected by connecting lines 2621 . Electrode layers are preferably made of a thin conductive material, for example copper or copper alloy. This pattern reduces the amount of metal used for the electrode layer, thus reducing the cost. However, electrodes may be a full or perforated sheet or differently patterned.
Although elements 201 and holes 232 are depicted cylindrical, other shapes may be used. For example, Elements 201 (or holes 232 ) may be shaped as rectangular boxes or bars.
FIG. 4( a ) schematically depicts an isometric view of a round multilayer modular generator 400 according to a preferred embodiment of the current invention.
In contrast to the rectangular shape of multilayer modular generator 200 , round multilayer modular generator 400 is shaped as a wide cylinder. Positive lead 421 a and negative lead 421 b exit the casing of the round multilayer modular generator.
In the non-limiting exemplary embodiment of FIG. 4 , casing of round multilayer modular generator 400 comprises a top cover 405 , a bottom cover 407 and mid section 406 . Preferably, a flexible seal (not seen in these figures for clarity) may be used to prevent moisture and dirt from entering the box, while allowing small relative motion of the covers in response to force applied to them.
Fasteners, such as screws 410 (three are seen, but different number of fasteners may be used), holds the casing together. Preferably, fasteners 410 apply some pressure on the layered structure within the casing, pre-loading the piezoelectric elements and ensuring mechanical and electrical contact between the piezoelectric elements and the electrode. Preloading the piezoelectric elements increases the energy yield of the generator and prevents energy loss for making contact in loose structure every time pressure is applied. Optionally, fasteners 410 comprise elastic elements that maintain the proper preloading force. Optionally, fasteners 410 are screws that are tightened with predetermined torque. It should be noted that mechanical and/or electrical contact between rods and electrodes may exist without preloading the screws, for example due to tightly fitting the internal elements of the generator into the box, or due to weight of the cover and/or the internal elements, or elastic properties of the internal elements or the box.
FIG. 4( b ) schematically depicts a cross-sectional view of a round multilayer modular generator according to another exemplary embodiment of the current invention.
The layered structure of round multilayer modular generator is depicted, showing matrix layers 431 a to 431 c , electrode layers 424 a to 424 d and piezoelectric elements 401 .
In the depicted exemplary embodiment, top and bottom covers are similar or substantially identical to reduce design and production costs. In this design, the number of layers can easily be changed by changing the length of midsection casing part 406 and inserting a different number of layers into the case.
FIG. 4( c ) schematically depicts a top view of round matrix layer 424 used in a round multilayer modular generator 400 according to another exemplary embodiment of the current invention.
Round matrix layer 424 comprises holes 432 for piezoelectric elements 401 and holes 417 for fasteners 411 .
FIG. 5 demonstrates an advantage of a round multilayer modular generator according to another exemplary embodiment of the current invention.
FIG. 5( a ) shows a cross section of a road with round multilayer modular generators embedded in it and vehicle over it, according to another exemplary embodiment of the current invention. When a vehicle (only axle 529 is seen for clarity), passes over a road 519 , the wheels 530 slightly are distorted 539 and make a substantially rectangular contact with the road. The asphalt layer 520 of the road, which is placed over the foundation 510 slightly, distorts 540 due to the pressure applied by wheels 530 and the strain is transferred to generators 400 embedded within asphalt layer 520 . For clarity, road distortion 540 was exaggerated.
FIG. 5( b ) schematically depicts the stress distribution caused by a passing vehicle on a round multilayer modular generator 400 according to another exemplary embodiment of the current invention. As stress spreads deeper and latterly within the asphalt layer 520 , zones of high stress 540 and zones of low stress 511 develop. By placing round multilayer modular generators 400 such that the majority of their volume is within the zones of high stress 540 , efficient use of the available energy is possible.
FIG. 5( c ) schematically depicts a graph of the stress distribution caused by a passing vehicle according to another exemplary embodiment of the current invention.
The zone of high stress 540 and zones of low stress 511 can be seen in this figure.
FIG. 6 schematically depicts a system 600 for energy harvesting implemented in a road and using a plurality of round multilayer modular generators 400 according to another exemplary embodiment of the current invention.
In the depicted example, two lanes road 650 having curbs 651 is embedded with a plurality of round multilayer modular generators 400 , preferably placed at locations were wheels of traveling vehicles are most likely to pass. Connecting cables 614 and 612 , transfer generated electrical energy to a control unit 610 for storage or for delivery to energy user such as electrical main grid vial cable 690 .
Preferably, Connecting cables 614 and 612 are also embedded beneath the surface of road 650 .
FIG. 7 schematically depicts steps of constructing an energy harvesting system 600 by embedding a plurality of round multilayer modular generators according to another exemplary embodiment of the current invention.
FIG. 7( a ) and FIG. 7( b ) schematically depict drilling, in a road, holes for embedding round multilayer modular generators, preferably using a cup drill.
Drilling circular holes in a road is easier than cutting rectangular holes. Drilling hole 710 in asphalt layer 520 having an upper surface 519 and deposited over a foundation layer 510 , may be done using standard roadwork equipment, for example cup drill 701 may be used to remove a cylindrical core from the road leaving a cylindrical hole 710 .
FIG. 7( c ) schematically depicts cutting in a road's asphalt layer 520 , slits 720 for embedding connecting cable 614 , preferably using a disk saw 711 (seen in FIG. 7( b )).
Optionally, slits 720 and holes 710 are made only part way into asphalt layer 520 . However any of slits 720 and holes 710 may be made all the way to or into foundation layer 510 .
FIG. 7( d ) schematically depicts optional stage of pouring a reinforcing layer 730 , preferably made of concrete at the bottom of the drilled hole 710 . The optional reinforcement layer 730 acts ad sturdy foundation for the round multilayer modular generator 400 to be placed in hole 710 and may be used to ensure desired depth of hole 710 which may not be easily drilled to the required accuracy.
FIG. 7( e ) schematically depicts the stage of laying the round multilayer modular generator 400 in drilled hole 710 over optional reinforcement 730 , and placing the connecting cables 614 in the cut slit 720 .
FIG. 7( f ) schematically depicts the stage of refilling the drilled holes and the cut slits, preferably with asphalt or bitumen 750 , thus embedding round multilayer modular generator 400 and cables 614 of system 600 below the surface 519 of the road.
FIG. 8 schematically depicts a cross section of a part of railway sleeper 810 with a modular multilayer generator 200 according to yet another exemplary embodiment of the current invention.
In this cross section, multilayer modular generator 800 is seen placed in a recess in sleeper 810 . Preferably multilayer modular generator 800 is multilayer modular generator 200 as depicted in FIG. 2 , but other types of multilayer modular generators may be used. For example round multilayer modular generator 400 . Optionally, internal elements depicted in FIG. 3 or 4 ( b ) are placed in a recess in sleeper 810 such that the internal recess acts as a box and mount 840 and elastomeric layer 850 acts as cover.
When a train traverses along rail 830 , stress caused by the train's weight it transferred via rail 830 , mount 840 and elastomeric layer 850 and presses on multilayer modular generator 200 , causing charge to be generated in said generator. Depth of recess for multilayer modular generator 800 in sleeper 810 is limited by metal reinforcement cables or bars 820 in sleeper 810 . This depth limits the number of layers in multilayer modular generator 200 . However, Sleeper 810 may be redesigned to allow deeper recesses. Similarly, width of for multilayer modular generator 800 in sleeper 810 is limited by the distance between screws 825 which hold mount 840 to sleeper 810 ; however, sleeper 810 may be redesigned to allow wider or narrower recesses.
It should be noted that rods 201 multilayer modular generator 200 ( 401 for round multilayer modular generator 400 ) are at least slightly longer than the corresponding matrix layer 231 ( 431 ), thus, when pressure is applied between the top and the bottom of the multilayer modular generator 200 ( 400 ), a physical and electrical contact is formed between the edges of rods 201 ( 401 ) and electrodes 224 ( 424 ). Electrode layers 224 ( 424 ) electrically connect rods 201 ( 401 ) in parallel. Pressure may be applied using fasteners 410 (not seen in FIGS. 2( a ) and 2 ( b ), but shown in FIGS. 4( a ) and 4 ( b )). Alternatively or additionally, pressure may be applied by the weight of cover 212 ( 405 ), which may be made of heavy material for example concrete or metal. Optionally, the entire box is made of concrete. Alternatively or additionally, pressure may be applied by encapsulation of the entire multilayer modular generator in elastic encapsulation. Encapsulation may also provide added protection against moisture, in addition to seal 214 (seen in FIG. 2( b ), but may be implemented in round modular generator 400 as well). Alternatively or additionally, pressure may be applied by the weight of embedding material used for covering the multilayer modular generator, for example asphalt or bitumen layer 750 seen in FIG. 7( f ) for the case of round multilayer modular generator 400 , but similarly applies when embedding multilayer modular generator 200 . When a multilayer modular generator is embedded in railroad sleeper (FIG. 8 ), the weight of the track 830 , and pressure applied to hold track 830 in place causes physical and electrical contact between the edges of rods and the electrodes.
Optionally, a pressure spreading layer (not shown for clarity) may be inserted between cover 212 ( 405 ) and top electrode layer 224 d ( 424 d ). In this case, the cover 212 ( 405 ) may be relatively thin and mechanical forces applied to the cover is transferred to said pressure spreading layer and spread among the plurality of rods 201 ( 401 ). Similarly, optionally, a pressure spreading layer (not shown for clarity) is inserted between the bottom of box 210 ( 407 ) and bottom electrode layer 224 a ( 424 a ) to spread the forces. Alternatively, optionally or additionally covers 212 ( 405 ) are stiff and acts as force spreading member.
FIG. 9( a ) schematically depicts an isometric view of a multilayer super-module generator 900 according to yet another exemplary embodiment of the current invention.
Super-module generator 900 preferably comprises a container 910 within which a plurality of multilayer modular generator 200 is placed. Optionally container 910 is divided to chambers by dividers 930 .
Alternatively, internal parts of multilayer modular generator 200 , as depicted in FIG. 3 are placed in each chamber of container 910 and covered with individual or a common cover (not seen in this figure). Leads 921 from each multilayer modular generator are united into electrical cable 912 .
It should be noted that the array of 2×3 multilayer modular generators 200 in a super-module generator 900 is exemplary, and other shapes, number and orientations of multilayer modular generators is possible.
Multilayer modular generator 200 , round generator 400 , and super-module generator 900 may be embedded in a road, airport runway, indoor floor or street pavement to harvest energy from vehicles or pedestrians.
FIG. 9( b ) schematically depicts a top view of a system for energy harvesting 960 , implemented in a road 650 and using a plurality of multilayer super-module generators 900 , according to yet another exemplary embodiment of the current invention.
In this figure, system for energy harvesting 960 comprises a plurality of multilayer super-module generators 900 and connecting cables 912 , embedded below the surface of a road or a highway 650 .
In the depicted example, two lanes road 650 having curbs 651 is embedded with a plurality super-module generators 900 , preferably placed at locations were wheels of traveling vehicles are most likely to pass. Connecting cables 912 , transfer generated electrical energy to a control unit 918 for storage or for delivery to energy user such as electrical main grid vial cable 990 .
For simplicity, only one lane of road 650 is seen fitted with super-module generators 900 , however, few or all lanes may be fitted with super-module generators 900 .
In the depicted example, super-module generators 900 are seen placed to form a single row. However, super-module generators 900 may be placed in two rows per lane, each where a wheel of a traveling care is likely to pass. Optionally, super-module generators 900 may be placed in a two dimensional array to tile a large area.
It should be noted the novel modular multilayer construction of multilayer modular generator 200 , round multilayer modular generator 400 and super-module generators 900 enables flexible fitting of a piezoelectric generator to its specific application, preferably with minimal redesign of few mechanical parts such as box 210 , mid section 406 or container 910 .
It should be noted that modular generator 200 , round modular generator 400 and super-module generator 900 may be embedded under the surface 519 of the road, or alternatively, modular generator 200 , round modular generator 400 and super-module generator 900 may be placed such that their upper surface is flush with the surface 519 of the road so that mechanical pressure is directly transferred to their covers. In this later case, asphalt or bitumen layer 750 seen in FIG. 7( f ) is missing.
It is appreciated that certain features of the invention, which are, for clarity, described in the context of separate embodiments, may also be provided in combination in a single embodiment. Conversely, various features of the invention, which are, for brevity, described in the context of a single embodiment, may also be provided separately or in any suitable sub combination.
Although the invention has been described in conjunction with specific embodiments thereof, it is evident that many alternatives, modifications and variations will be apparent to those skilled in the art. Accordingly, it is intended to embrace all such alternatives, modifications and variations that fall within the spirit and broad scope of the appended claims. All publications, patents and patent applications mentioned in this specification are herein incorporated in their entirety by reference into the specification, to the same extent as if each individual publication, patent or patent application was specifically and individually indicated to be incorporated herein by reference. In addition, citation or identification of any reference in this application shall not be construed as an admission that such reference is available as prior art to the present invention.
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A multilayer piezoelectric generator is disclosed comprising a round, rectangular or other shaped box having a cover. In the box are top and bottom electrodes and a plurality of electricity generating layers. Each Layer comprises a plurality of piezoelectric rods held in place by a matrix layer that fits snugly in the box and configured to accept shear strains developed in the rods when pressure is applied to the cover. The layers are separated by central electrode layers. The structure is configures such that pressure is evenly spreads among all the rods and causes the rods to make contacts with the electrodes. Rods in adjacent layers are oppositely poled, and the electrodes are configured and wired such that all the rods are connected parallel such that their generated charge is summed. Adaptation of the generator to its application is done by changing the number and thickness of the layers.
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CROSS-REFERENCE TO RELATED APPLICATION
[0001] This application claims the benefit of the filing date of U.S. Provisional Application Ser. No. 61/074,246, entitled “APORPHINE DERIVATIVES, APORPHINE DERIVATIVES SALTS AND THEIR PHARMACEUTICAL USES” filed Jun. 20, 2008 under 35 USC & 119(e)(1).
BACKGROUND OF THE INVENTION
[0002] 1. Field of the Invention
[0003] The present invention relates to some novel salts of aporphine compounds and methods for preparing the same and, more particularly, to pharmaceutically acceptable salts of aporphine compounds and carboxyl-group containing agents and methods for preparing the same.
[0004] 2. Description of Related Art
[0005] A multitude of studies in experimental animals, together with clinical data, provide evidence that increased production of ROS (reactive oxygen species) are involved in the development and progression of cardiovascular disease including atherogenesis. In particular, the paper demonstrates various steps where oxidative stress could be involved in atherogenesis ( Chen J et al., Indian Heart J 2004; 56: 163-173). Atherosclerosis is the buildup of fatty deposits called plaque on the inside walls of arteries. Arteries are blood vessels that carry oxygen and blood to the heart, brain, and other parts of the body. As plaque builds up in an artery, the artery gradually narrows and can become clogged. As an artery becomes more and more narrowed, less blood can flow through.
[0006] Oxidative stress refers to the physico-chemical, chemical, biochemical and toxicological behavior of the Reactive Oxygen Species (ROS). Oxidative stress plays a significant role in the pathogenesis of atherosclerosis and its complications. Oxidative stress mediates cell damage, in part, via reactive oxygen species (ROS). Oxidative stress has been identified throughout the process of atherogenesis. As the process of atherogenesis proceeds, inflammatory cells, as well as other constituents of the atherosclerotic plaque release large amounts of ROS, which further facilitate atherogenesis. In general, increased production of ROS may affect four fundamental mechanisms that contribute to atherosclerosis: endothelial cell dysfunction, vascular smooth muscle cells (VSMC) growth, monocyte migration and oxidation of low density lipoproteins (LDLs) (Alexander R W, Hypertension 1995; 25(2): 155-161; Berliner J A et al., Free Radic Biol Med 1996, 20: 707-727). A number of studies suggest that ROS oxidatively modified LDL is a more potent proatherosclerotic mediator than the native unmodified LDL (Heinecke J W., Atherosclerosis 1998, 141: 1-15). An important characteristic of endothelial dysfunction is impaired synthesis, release, and activity of endothelium-derived Nitric Oxide (NO). Nitric Oxide Synthase (NOS) converts Arginine into NO, the molecule that resists plaque formation, vasospasm, and abnormal clotting. Several studies have demonstrated that endothelial NO inhibits several processes involved in atherogenesis. For example, it mediates vascular relaxation and inhibits platelet aggregation, vascular SMC proliferation, and endothelium-leukocyte interactions. Inactivation of NO by superoxide anion limits the bioavailability of NO and leads to nitrate tolerance, vasoconstriction, and hypertension as well as atherosclerosis. Accordingly, if you can make and maintain Nitric Oxide then you will not develop cardiovascular disease. If the Nitric Oxide system can be successfully rebooted, then the cardiovascular disease can be stabilized.
[0007] ROS are involved in intracellular signalling. However, when ROS production is enhanced, dysregulation of physiological processes occurs. O 2 − and other radicals may react with NO causing endothelial dysfunction. The reaction of O 2 − with NO leads to production of peroxynitrite. Peroxynitrite is itself a potent oxidant which can induce oxidation of proteins, lipids and DNA. In addition, ROS can stimulate vascular smooth muscle cell hypertrophy and hyperplasia. Furthermore, elevations in levels of ROS may, via a variety of mechanisms, initiate development of a vascular pro-inflammatory state. This pro-inflammatory state may be promoted via activation of redox-sensitive transcription factors, such as nuclear factor B and the leucocyte adhesion molecule vascular cell adhesion molecule 1, by reduction in levels of NO or by Angiotension-II-dependent pathways. Besides, risk factors for atherosclerosis, such as hypertension and hyperlipidemia, are also associated with increased generation of ROS (Patterson C et al., Circ. Res. 2000; 87(12): 1074-1076).
[0008] Oxidative stress alters many functions of the endothelium. As known in the art, oxidative stress is involved in the pathogenesis of a group of many diseases, such as cardiovascular diseases, including hypercholesterolemia, atherosclerosis, hypertension, diabetes, and heart failure etc. (Cai H et al., Circ Res. 2000; 87: 840-844), and ischemic cerebral diseases, including ischemic cerebral thrombosis, ischemic cerebral embolism, hypoxic ischemic encephalopathy etc. Department of Physiological Science, University of California also published that oxidative stress is thought to play a major role in the pathogenesis of a variety of human diseases, including atherosclerosis, diabetes, hypertension, aging, Alzheimer's disease, kidney disease and cancer (Roberts C K et al., Life Sci. Mar. 9, 2009). In addition, a role of the free-radical processes and disturbances of oxidative-restorative blood homeostasis and nervous tissue in the pathogenesis of brain ischemic pathology and other diseases was published (Solov'eva EIu et al., Zh Nevrol Psikhiatr Im SS Korsakova. 2008; 108(6): 37-42).
[0009] As ROS appear to have a critical role in many diseases, there has been considerable interest in identifying the enzyme systems involved and in developing strategies to reduce oxidative stress. Superoxide dismutase mimetics, thiols, xanthine oxidase and NAD(P)H (nicotinamide adenine dinucleotide phosphate reduced form) oxidase inhibitors are currently receiving much interest, while animal studies using gene therapy show promise, but are still at an early stage. Of the drugs in common clinical use, there is evidence that ACE (angiotensin-converting enzyme) inhibitors and AT 1 (angiotensin II type 1) receptor blockers have beneficial effects on oxidative stress above their antihypertensive properties, whereas statins, in addition to improving lipid profiles, may also lower oxidative stress (Hamilton C A et al., Clinical Science 2004; 106. 219-234).
[0010] Meanwhile, for some aporphine derivatives, the effect on oxidative stress has been investigated. Hereafter, some known aporphine derivatives (e.g. thaliporphine, glaucine, N-[2-(2-methoxyphenoxy)ethyl]norglaucine) will be introduced.
[0011] Thaliporphine is an aporphine derivative, which is a phenolic alkaloid isolated from the plants of Neolitsea konishii K (Teng C M et al., Eur J Pharmacol. 1993, 233(1). 7-12). It has been disclosed that thaliporphine is a positive inotropic agent with a negative chronotropic action. This compound has antiarrhythmic action. (Su M J et al., Eur. J Pharmacol. 1994; 254: 141-150).
[0012] In ischemia or ischemia-reperfusion (I/R), nitric oxide (NO) can potentially exert several beneficial effects. Thaliporphine increased NO levels and exerted cardioprotective action in ischemic or I/R rats. Thaliporphine treatment significantly increased NO and decreased lactate dehydrogenase (LDH) levels in the blood during the end period of ischemia or I/R. These changes in NO and LDH levels by thaliporphine were associated with a reduction in the incidence and duration of ventricular tachycardia (VT) and ventricular fibrillation (VF) during ischemic or I/R period. Thaliporphine, acting via NO-dependent or NO-independent mechanisms, reduces ischemia or I/R-induced cardiac injury.
[0013] Thaliporphine could be a novel agent for attenuating endotoxin-induced circulatory failure and multiple organ injury and may increase the survival rate. These beneficial effects of thaliporphine may be attributed to the suppression of TNF-alpha (Tumor necrosis factor alpha), NO and superoxide anion (O 2 − ) (Chiao C W et al., Naunyn Schmiedebergs Arch Pharmacol. 2005; 371(1): 34-43).
[0014] The vasorelaxant effect of glaucine was studied. Glaucine has an intracellular effect and also acts on the cell membrane by blocking voltage-dependent and receptor-operated calcium channels (Loza I, Planta Med. 1993, 59(3): 229-231). The scavenging and iron-reducing properties of a series of benzylisoquinolines of natural and synthetic origin have been studied. Boldine and glaucine acted as scavengers of hydroxyl radical in the deoxyribose degradation by Fe 3+ -EDTA +H 2 0 2 (Fenton's reagent) (Ubeda A et al., Free Radic Biol Med. 1993; 15(2): 159-167).
[0015] The antihyperglycemic actions of some aporphines and their derivatives in normal Wistar, streptozotocin (STZ)-induced diabetic (IDDM, Insulin-dependent diabetes mellitus) and nicotinamide-STZ induced diabetic (NIDDM, Non-insulin-dependent diabetes mellitus) rats were investigated. These compounds included thaliporphine, glaucine, boldine, and the derivatives, N-[2-(2-methoxyphenoxy)ethyl]norglaucine and diacetyl-N-allylsecoboldine. Thaliporphine exerts an antihyoperglycemic action through insulin-dependent and insulin-independent mechanisms. Glaucine and boldine exerted less potent hypoglycemic action in STZ-diabetic rats, both compounds may lower the plasma glucose mainly through an insulin-dependent mechanism. N-methyllaurotetanine and predicentrine produce their antihyperglycemic effect through an insulin-independent mechanism (Chi T C et al. Planta Med. 2006; 72(13): 1175-1180).
[0016] U.S. Pat. No. 6,313,134 discloses thaliporphine and its derivatives for the treatment and/or prophylaxis of cardiac diseases, including cardiac arrhythmia, myocardial ischemia or myocardial infarction, and sudden death caused by cardiac arrhythmia or acute myocardial infarction.
[0017] U.S. Pat. No. 7,057,044 provides aporphine and oxoaporphine compounds that have endothelial nitric oxide synthase (eNOS) maintaining or enhancing activities and may be used to manufacture a medicaments for preventing or treating ischemic diseases in human and mammal, and the ischemic diseases may include ischemic cerebral apoplexy, ischemic cerebral thrombosis, ischemic cerebral embolism, hypoxic ischemic encephalopathy, ischemic cardiac disease or ischemic enteropathy etc.
[0018] Aporphine and thaliporphine derivatives have the antihyperglycemic activities. Aporphine and thaliporphine derivatives may be used to prevent or treat hyperglycemic disease in human and mammal.
[0019] In addition to aporphine derivatives, some known carboxyl group-containing agents having effects on oxidative stress were disclosed as follows.
[Statins]
(a) Cardioprotective Actions of Statins
[0020] Statins increase NO bioavailability through PI3K/Akt (Phosphatidylinositol 3-kinase/Akt) and Rho-mediated signaling. NO can then mediate cytoprotection in the setting of myocardial ischemia and reperfusion through effects on the coronary vasculature and at the level of the mitochondria within cardiac myocytes. The vascular effects of increased NO bioavailability include the attenuation of both platelet and leukocyte adhesion and plugging within the coronary microcirculation and coronary vasodilatation. Statin-mediated generation of NO can also result in protection of the mitochondria through the activation of mitochondrial K ATP (mK ATP ) channels. The opening of these channels serves to depolarize the mitochondrial membrane, maintain the integrity of the mitochondrial matrix and decrease ROS generation by the mitochondria following ischemia and reperfusion. With statins, a class of compounds is intended, comprising as main components fluvastatin, pravastatin, atorvastatin, cerivastatin, rosuvastatin, pitavastatin, lovastatin acid and simvastatin acid.
(b) Statins and Their Role in Vascular Protection
[0021] The statins reduce cholesterol synthesis through inhibition of HMG-CoA (3-hydroxy-3-methylglutaryl-CoA) reductase and are widely prescribed for hyperlipidaemia to reduce the risk of atherosclerotic complications. The beneficial effect of lipid lowering by statins in the treatment of coronary heart disease has been demonstrated in large clinical trials. However, statins appear to have additional benefits on vascular function above and beyond their lipid lowering effects. Through inhibition of L-mevalonate synthesis, statins also prevent the synthesis of isoprenoid intermediates, including farnesylpyrophosphate and geranylgeranylpyrophosphate. Isoprenylation is important in the post-translational modification of a variety of proteins, including the small GTPases Rho, Rac and Ras, and hence plays an integral role in cellular signalling. Moreover, interference with isoprenylation underlies many of the beneficial actions of the statins on vascular endothelium, which include increased endothelial nitric oxide synthase expression, pro-angiogenic effects, increased fibrinolytic activity, immunomodulatory and anti-inflammatory actions, including increased resistance to complement. (Mason J C., Clinical Science 2003, 105: 251-266).
(c) Statins and Their Role in NO:
[0022] NO plays a central role in the maintenance of normal endothelial function and is generated in response to laminar shear stress. Endothelial NO is a vasodilator, inhibits smooth muscle proliferation, platelet aggregation, endothelial adhesion molecule expression and leucocyte-EC interactions. The demonstration that statins are able to enhance local NO generation in ECs, by increasing the half-life of eNOS (endothelial NO synthase) mRNA, was fundamental to the acceptance of the emerging evidence for lipid-independent effects]. Statins retain their ability to increase eNOS in the presence of oxidized LDL and under hypoxic conditions. In addition, statins exert further beneficial effects on the endothelium through their inhibition of the expression of the potent vasoconstrictor endothelin-1. These actions have now been demonstrated for a number of different statins, including simvastatin, lovastatin, atorvastatin, pravastatin and fluvastatin in in vivo and in vitro studies (Mason J C., Clinical Science 2003; 105. 251-266).
[0023] Atherosclerosis induced an endothelial [NO]/[ONOO − ] balance indicative of endothelial dysfunction. Statins showed anti-atherosclerotic effects mediated by HO −1 /eNOS, restoring the [NO]/[ONO O − ] imbalance and reducing lipid peroxidation.
[Angiotensin II Receptor Blockers]
(a) Application of Angiotensin II Receptor Blockers
[0024] Angiotensin II receptor blockers (ARBs) can be employed for treating high blood pressure, and may be useful in the treatment of other cardiac diseases such as stroke, heart attack and congestive heart failure, and also seem to have a beneficial effect on the kidney, particularly the kidneys of people with diabetes.
[0025] Hypertension is an important risk factor in atherogenesis. There is activation of renin angiotensin system (RAS) in many hypertensive patients. Activation of RAS with the formation of angiotensin II (Ang II) and subsequent activation of Ang II receptors, mainly type I receptors (AT1R), has been implicated in atherogenesis. Ang II can exert multiple pro-atherogenic effects on vascular endothelial cells and smooth muscle cells(SMCs) by activating AT1R. Ang II enhances the uptake of ox-LDL and the biosynthesis of cholesterol in macrophages, leading to formation of foam cells; Ang II upregulates LOX-1 (lectin-like oxidized low-density lipoprotein receptor-1) gene and protein expression in cultured human coronary artery endothelial cells, and enhances the noxious effects of ox-LDL, both via AT1R activation. Ang II induces apoptosis of human coronary artery endothelial cells.
[0026] With angiotensin II receptor blockers (ARBs), a class of compounds is intended, comprising as main components losartan, valsartan, irbesartan, candesartan, telmisartan and olmesartan. Valsartan, candesartan and telmisartan are containing a carboxylic acid side chain. The pharmaceutical compositions containing them and their use as blood pressure-reducing drugs and use to treat and/or prevent stroke, heart attack and congestive heart failure and other cardiac diseases as cardiac arrhythmia, myocardial ischemia or myocardial infarction.
(b) Angiotensin II Receptor Blockers (ARBs) and Their Role in Oxidative Stress and Cardiovascular Diseases
[0027] Ang II plays a crucial role in the induction of oxidative stress and the pathogenesis of cardiovascular and renal diseases, and the beneficial mechanisms of ARBs are multifactorial. (Shao J et al., J Hypertens. 2007; 25(8): 1643-1649.)
[0028] Telmisartan attenuated the oxidative stress induced by hydrogen peroxide in both cells, suggesting that it acted via a receptor-independent antioxidant effect. Telmisartan did not change expression levels of antioxidative enzymes such as catalase or glutathione peroxidase. Telmisartan inhibits intracellular oxidative stress, at least in part, in a receptor-independent manner, possibly owing to its lipophilic and antioxidant structure.
[0029] Several enzymatic sources of reactive oxygen species (ROS) were described as potential reasons of eNOS uncoupling in diabetes mellitus. Telmisartan inhibits activation of superoxide sources like NADPH oxidase, mitochondria, and xanthine oxidase. These effects may explain the beneficial effects of telmisartan on endothelial dysfunction in diabetes. (Wenzel P et al., Free Radic Biol Med. 2008, 45(5): 619-626.)
[0030] Cardioprotective mechanism of telmisartan is via PPAR-gamma-eNOS pathway in dahl salt-sensitive hypertensive rats. (Kobayashi N et al., Am J Hypertens. 2008; 21(5): 576-581) Telmisartan is a partial agonist of the peroxisome proliferator-activated receptor-gamma (PPAR-gamma). The cardioprotective mechanism of telmisartan may be partly due to improvement of endothelial function associated with PPAR-gamma-eNOS, oxidative stress, and Rho-kinase pathway.
[Angiotensin I Converting Enzyme Inhibitors]
(a) Application of Angiotensin I Converting Enzyme Inhibitors (ACEIs)
[0031] ACEIs are useful in the treatment of cardiovascular disorders, especially hypertension and congestive heart failure as well as for achieving other therapeutic effects by inhibiting the conversion of angiotensin I to angiotensin II.
[0032] With angiotensin I converting enzyme inhibitors, a class of compounds is intended, comprising as main components captopril, perindopri, ramipril, enalapril, fosinopril, quinapril, lisinopril, benazepril. The pharmaceutical compositions containing them are used for controlling blood pressure, treating heart failure and preventing kidney damage in people with hypertension or diabetes. They also benefit patients who have had heart attacks.
(b) Angiotensin I Converting Enzyme Inhibitors (ACEIs) and Their Role in Oxidative Stress and Cardiovascular Diseases
[0033] ACEI improve the vasoconstrictive/vasodilatory balance by blocking the formation of angiotensin II and preventing the degradation of bradykinin. In vitro, animal and human experimental studies have shown that ACEI have several properties: promote vasodilation, limit neurohormonal activation and vasoconstriction during ischemia, improve endothelial function by reducing oxidative stress, and slow down the development of atherosclerosis. Previous trials have shown that ACEI reduced cardiovascular events in patients with heart failure or ventricular dysfunction. In PROGRESS (n=6105), a perindopril-based regimen reduced recurrent stroke by 28% and substantially reduced cardiac outcomes among individuals with cerebrovascular disease. In HOPE (n=9297), ramipril reduced the composite outcome (cardiovascular death, myocardial infarction and cerebrovascular accident) by 22% in patients with high cardiovascular risk. (Bertrand M E., Curr Med Res Opin. 2004; 20(10):1559-69.)
[0034] Captopril has protective effects against damages of vascular endothelium induced by homocysteine and lysophosphatidylcholine. Captopril can prevent the inhibition of endothelium-dependent relaxation induced by homocysteine in isolated rat aorta, which may be related to scavenging oxygen free radicals and enhancing NO production (Fu Y F et al., J Cardiovasc Pharmacol. 2003, 42(4): 566-5 72).
[0035] The mechanisms of endothelial dysfunction induced by homocysteine thiolactone (HTL) may include the decrease of NO and the generation of oxygen free radicals and that captopril can restore the inhibition of endothelium-dependent relaxation (EDR) induced by HTL in isolated rat aorta, which may be related to scavenging oxygen free radicals and may be sulfhydryl-dependent (Liu Y H et al., J Cardiovasc Pharmacol. 2007; 50(2): 155-161).
[0036] Formation of homocysteine (Hcy) is the constitutive process of gene methylation. The accumulation of homocysteine (Hcy) leads to increased cellular oxidative stress in which mitochondrial thioredoxin, and peroxiredoxin are decreased and NADH oxidase activity is increased.
[0037] Hyperhomocysteinaemia is an independent risk factor for atherosclerosis, including cardiovascular (CV) disease, cerebrovascular disease and peripheral vascular disease in the general population. The homocysteine theory of atherosclerosis was first suggested by McCully in 1969, following his observation that children with homocysteinuria and markedly elevated plasma homocysteine levels (>100 μmol/L) had severe premature arterial disease. Since then, many clinical and epidemiological studies have demonstrated that a mild or moderate increase in plasma homocysteine is a risk factor for vascular disease.
[0038] The adverse effects of homocysteine on endothelial function may be mediated by reduced production and bioavailability of nitric oxide due to oxidative stress. Hyperhomocysteinaemia could cause oxidative stress via a number of mechanisms. In vitro studies using cultured endothelial cells have demonstrated auto-oxidation of homocysteine to form reactive oxygen species, including superoxide anion and hydrogen peroxide, increased lipid peroxidation and impaired production of the antioxidant glutathione peroxidase.
[Fibric Acids]
[0039] (a)Application of Fibric Acids
[0040] Coronary heart disease patients with low high-density lipoprotein cholesterol (HDL-C) levels, high triglyceride levels, or both are at an increased risk of cardiovascular events.
[0041] Fibric acid derivatives effectively lower triglycerides and raise high-density lipoprotein (HDL) cholesterol, but their effect on low-density lipoprotein (LDL) cholesterol is weakly beneficial (small decreases) to adverse (small increases) and varies according to the triglyceride level. With fibric acid, a class of compounds is intended, comprising as main components bezafibrate, clofibric acid, fenofibric acid and gemfibrozil.
[0000] (b) Fibric cids and Their Role in Oxidative Stress and Cardiovascular Diseases
[0042] The Bezafibrate Infarction Prevention (BIP) study was another randomized, placebo-controlled trial studying the effects of bezafibrate among men and women with coronary heart disease (CHD) ( Circulation 2000; 102: 21-27). Bezafibrate therapy demonstrated significant reductions in triglyceride and LDL concentrations and fibrinogen while elevating HDL levels. When the study was completed, bezafibrate was associated with a 9% reduction (p=0.26) in fatal and nonfatal myocardial infarction and sudden death. Overall mortality rates and frequency of newly diagnosed cancer were similar among the groups, showing bezafibrate to be safe agent among adults with CHD, but it had no significant effect on the frequency of major coronary events.
[0043] Although there is evidence that hyperlipidemia and predominance of small dense low density lipoproteins (LDLs) are associated with increased oxidative stress, the oxidation status in patients with hypertriglyceridemia (HTG) has not been studied in detail. Bezafibrate reversed the oxidation resistance to the normal range. In conclusion, these results indicate the following: (1) Hypertriglyceridemia is associated with normal in vivo oxidative stress and enhanced ex vivo resistance of lipoproteins to oxidation. (2) Bezafibrate reduces the resistance of lipoproteins to copper-induced oxidation and enhances oxidative stress in hypertriglyceridemia patients ( Arteriosclerosis, Thrombosis, and Vascular Biology. 2000, 20: 2434-2440).
[Meglitinides]
(a) Application of Meglitinides
[0044] In type 2 diabetes mellitus, impairment of insulin secretion is an important component of the disease. The meglitinide analogues (“meglitinides”) are a class of oral antidiabetic agents that increase insulin secretion in the pancreas. The properties of this class of drug suggest that they have the potential to produce a rapid, short-lived insulin output. With meglitinide, a class of compounds is intended, comprising as main components repaglinide, nateglinide and mitiglinide. Two analogues are currently available for clinical use: repaglinide and nateglinide ( Cochrane Database Syst Rev. 2007; 18(2): CD004654).
(b) Meglitinides and Their Role in Cardiovascular Protection
[0045] Glinides (meglitinides) represent a chemically heterogeneous new class of insulin-secreting agents characterized by a rapid onset and short duration of action. They act by closure of the ATP-dependant K channel. Repaglinide has an equivalent HbA1c lowering effect to conventional sulfonylureas but reduces predominantly postprandial glucose levels. Nateglinide has an even shorter duration of action and has almost no effect on fasting plasma glucose levels. Several experimental data suggest that glinides could preserve B cell function over time better than hypoglycaemic sulfonylureas, and that the improvement of post-prandial glucose levels could exert a long term protective cardiovascular effect ( Diabetes Metab. 2006; 32(2): 113-120).
[Other Carboxyl Group-Containing Agents]
Other Carboxyl Group-Containing Agents and Their Role in Oxidative Stress and Induced Diseases
[0046] Atherosclerosis is a major cause of death in elderly individuals. Endothelial dysfunction is recognized as a key early event in atherogenesis. Administration of essential amino acids may improve brachial reactivity in elderly persons and may also protect against the development of atherosclerosis via the rise in plasma-free IGF-1 levels. (Manzella D et al., Am J Hypertens. 2005; 18(6): 858-863.)
[0047] The antioxidant supplement, n-acetyl cysteine, is a sulfur-based amino acid needed to make glutathione, a natural antioxidant enzyme produced in the body to fight free-radical activity. Without glutathione, your body immune system would be greatly compromised, and left with little defense against toxins and disease.
[0048] N-acetyl cysteine may be effective in the prevention and/or treatment of cancer, heavy metal poisoning, smoker cough, bronchitis, heart disease, cystic fibrosis, acetaminophen poisoning, and septic shock. Its detoxifying effects may also help enhance the benefits of regular exercise by protecting the body from oxidative stress.
[0049] Acetylcysteine is a precursor in the formation of the antioxidant glutathione in the body. The thiol (sulfhydryl) group confers antioxidant effects and is able to reduce free radicals. Recent studies suggest that high-dose N-acetylcysteine provides better protection from contrast-induced nephropathy, and the antioxidant properties of N-acetylcysteine may also provide cardiac protection. N-acetylcysteine-enhanced contrast medium reduces MI size and protects renal function in a pig model of ischemia and reperfusion. Thrombolysis after acute myocardial infarction may lead to a number of adverse effects (reperfusion injury) such as myocardial stunning, arrhythmias and even myocardial damage and extension of the infarct size. Some recent clinical studies have demonstrated that the intravenous infusion of N-acetylcysteine during thrombolysis was associated with a decrease in infarct size and better preservation of left ventricular function, probably due to antioxidant and free radical scavenger properties of N-acetylcysteine.
[0050] Methionine and cysteine enhance force of contraction by N-methylation of membrane phospholipids of the sarcolemma and sarcoplasmic reticulum. Methionine and, to a lesser extent, cysteine may reduce myocardial damage by oxygen radical species. (Pisarenko O I., Clin Exp Pharmacol Physiol. 1996; 23(8): 627-633.)
[0051] Amino acids (e.g. glutamate, aspartate), or keto acids (e.g. pyruvic acid, 2-ketoglutaric acid) have myocardial protective properties. Cardioplegic solutions rich in the hydrophilic, basic amino acids, glutamate and aspartate, or keto acids have enhanced myocardial preservation and left ventricular function. Several biochemical mechanisms exist by which certain amino acids may attenuate ischemic or reperfusion injury. Glutamate and aspartate may become preferred myocardial fuels in the setting of ischemia. They may also reduce myocardial ammonia production and reduce cytoplasmic lactate levels, thereby deinhibiting glycolysis. Some amino acids may become substrate for the citric acid cycle. Glutamate and aspartate also move reducing equivalents from cytoplasm to mitochondria where they are necessary for oxidative phosphorylation and energy generation. A rationale exists for the use of an amino acid-rich cardioplegia-like solution in myocardial infarction. ( Clin Cardiol. 1998; 21(9): 620-624.) Pyruvate cardioplegia solution may be used in any surgery where the heart must be arrested, but it is particularly useful in cardiopulmonary bypass surgery. Because the solution relies primarily upon pyruvate to protect the heart from damage during and immediately after arrest, other additives are not as necessary as with current cardioplegia solutions or are not necessary at all. (US Patent Appl. 20030124503) Taurine (2-aminoethanesulphonic acid), a sulphur-containing amino acid, is found in most mammalian tissues. Taurine was found to exhibit diverse biological actions, including protection against ischemia-reperfusion injury, modulation of intracellular calcium concentration, and antioxidant, antiatherogenic and blood pressure-lowering effects. There is a wealth of experimental information and some clinical evidence available in the literature suggesting that taurine could be of benefit in cardiovascular disease of different etiologies. ( Exp Clin Cardiol. 2008;13(2): 57-65.) Taurine reduces iron-mediated myocardial oxidative stress, preserves cardiovascular function, and improves survival in iron-overloaded mice. The role of taurine in protecting reduced glutathione levels provides an important mechanism by which oxidative stress-induced myocardial damage can be curtailed. (Oudit G Y et al., Circulation. 2004; 109(15): 1877-1885.)
[0052] L-Arginine, the substrate of nitric oxide synthase, is known to exert favorable effects in the prevention and treatment of cardiovascular diseases. In several conditions, including atherosclerosis and ischemia/reperfusion, where oxygen metabolites are thought to mediate endothelial and myocardial injury, L-arginine has protective effects. (Lass A et al., Mol Pharmacol. 2002, 61: 1081-1088.) Nitric oxide (NO) plays a fundamental role in the vasculature because of its diverse influence in vascular protection, including its well-reported antiproliferative, anti-inflammatory, antithrombotic and vasodilator effects. In many vascular disease states, NO production is reduced as a result of endothelial dysfunction, in part caused by a decrease in substrate (L-arginine) availability. L-Arginine supplementation in patients with vascular disease is well reported to benefit patients therapeutically because of its effect on both NO-dependent and -independent mechanisms. The role of L-methionine and homocystine and their effect on NO also play an influential role in the body. (Huynh N N et al., Clin Exp Pharmacol Physiol. 2006, 33(1-2): 1-8)
[0053] The ability of carnosine to suppress significantly the development of ischemic reperfusion contracture and to support the restoration of the contractile force during reperfusion were shown. At the same time, a decrease of myoglobin and nucleoside release from myocytes was observed, this indicating a membrane-protecting effect of carnosine. Heart muscle protection by acetylated derivatives of carnosine and anserine under ischemia correlates with the preferential localization of these compounds in high quantities in the myocardium. (Alabovsky V V et al., Biochemistry (Mosc). 1997; 62(1): 77-87.)
[0054] Accumulating chemical, biochemical, clinical and epidemiological evidence supports the chemoprotective effects of phenolic antioxidants against oxidative stress-mediated disorders. The pharmacological actions of phenolic antioxidants stem mainly from their free radical scavenging and metal chelating properties as well as their effects on cell signaling pathways and on gene expression. (Soobrattee M A et al., Mutat Res. 2005; 579(1-2): 200-213.)
[0055] Scientific research has gradually verified the antidiabetic effects of ginger (Zingiber officinale Roscoe). Especially gingerols, which are the major components of ginger, are known to improve diabetes including the effect of enhancement against insulin-sensitivity. Aldose reductase inhibitors have considerable potential for the treatment of diabetes, without increased risk of hypoglycemia. The assay for aldose reductase inhibitors in ginger led to the isolation of five active compounds. 2-(4-hydroxy-3-methoxyphenyl)ethanoic acid, one carboxyl group-containing phenolic compound of the five active compounds, was a good inhibitor of recombinant human aldose reductase. These results suggested that it would contribute to the protection against or improvement of diabetic complications for a dietary supplement of ginger or its extract containing aldose reductase inhibitors. (Kato A et al., J Agric. Food Chem. 2006; 54(18): 6640-6644.)
[0056] Chromocarbe diethylamine is more effective than vitamin C against exercise-induced oxidative stress. Chromocarbe diethylamine was more effective than vitamin C in the prevention of glutathione oxidation in blood. Furthermore, chromocarbe diethylamine partially prevented muscle damage. Chromocarbe diethylamine was the most effective compound in the prevention of exercise-induced lipid peroxidation in plasma. ( Pharmacol Toxicol. 2001; 89(5): 255-258.)
SUMMARY OF THE INVENTION
[0057] The object of the present invention is to provide a novel pharmaceutically acceptable compound, i.e. a salt of an aporphine derivative and a carboxyl group-containing agent, in which the aporphine derivative and the carboxyl group-containing agent have effects on oxidative stress.
[0058] To achieve the object, the present invention provides a pharmaceutically acceptable compound, which is a 1:1 salt of a basic group-containing compound represented by the following formula (I) and a carboxyl group-containing agent,
[0000]
[0059] wherein,
[0060] each of R 1 , R 2 , R 3 and R 4 , independently, is hydrogen, C 1-6 alkyl, or —C(O)R 5 ;
[0061] R is hydrogen, C 1-6 alkyl, —C(O)R 5 , or C 1-6 alkyl substituted by the following group: —C(O)OR 6 , —C(O)NR 6 R 7 , —OR 6 , —NR 6 R 7 , C 4-9 heteroaryl containing at least one heteroatom selected from the group consisting of N, O and S, C 4-9 heterocyclyl containing at least one heteroatom selected from the group consisting of N, O and S, or C 6-10 aryl unsubstituted or substituted by at least one selected from the group consisting of halogen, hydroxyl, C 1-6 alkoxy and C 1-6 alkyl;
[0062] R 5 is C 4-9 heteroaryl containing at least one heteroatom selected from the group consisting of N, O and S, or C 1-6 alkyl substituted by —NR 6 R 7 or C 4-9 heterocyclyl containing at least one heteroatom selected from the group consisting of N, O and S;
[0063] each of R 6 and R 7 , independently, is hydrogen, C 1-6 alkyl, C 4-9 heteroaryl containing at least one heteroatom selected from the group consisting of N, O and S, C 4-9 heterocyclyl containing at least one heteroatom selected from the group consisting of N, O and S , or C 6-10 aryl unsubstituted or substituted by at least one selected from the group consisting of halogen, hydroxyl, C 1-6 alkoxy and C 1-6 alkyl; and
[0064] the carboxyl group-containing agent is selected from the group consisting of a statin, an angiotensin II receptor blocker, an angiotensin I converting enzyme inhibitor, a fibric acid, a meglitinide, and a specific acid.
[0065] Accordingly, since the pharmaceutically acceptable compound according to the present invention contains two kinds of active agents (i.e. an aporphine derivative and a carboxyl group-containing agent), the pharmaceutically acceptable compound according to the present invention can exhibit synergistic pharmacological activities of the aporphine derivative and the carboxyl group-containing agent so as to achieve a better combined therapeutic effects.
[0066] With regard to the pharmaceutically acceptable compound of the present invention, since the aporphine derivative functions as a base and the carboxyl group-containing agent functions as an acid, the aporphine derivative and the carboxyl group-containing agent can react with each other to form a 1:1 salt (e.g. a statin salt of aporphine compound, an angiotensin II receptor blocker salt of aporphine compound, an angiotensin I converting enzyme inhibitor salt of aporphine compound, a fibric acid salt of aporphine compound, and a meglitinide salt of aporphine compound), which has unique characteristics distinguishable from either carboxyl group-containing agent alone or aporphine derivative alone, based on the testing results in Fourier-Transformed Infrared Spectroscopy (FTIR), LC/MS and NMR analyses. Additionally, the pharmaceutically acceptable compound of the present invention may be converted into the carboxyl group-containing agent and the aporphine compound in the body after administration.
[0067] Referring to Formula (I), preferably, each of R 1 , R 2 , R 3 and R 4 , independently, is hydrogen or C 1-6 alkyl, and R is hydrogen, C 1-6 alkyl, —C(O)R 5 , or C 1-6 alkyl substituted by —C(O)OR 6 , —C(O)NR 6 R 7 , —OR 6 or C 4-9 heteroaryl containing at least one heteroatom selected from the group consisting of N, O and S.
[0068] Referring to Formula (I), more preferably, each of R 1 , R 2 , R 3 and R 4 , independently, is hydrogen or C 1-6 alkyl, and R is hydrogen, C 1-6 alkyl, —C(O)R 5 , or C 1-6 alkyl substituted by —C(O)OR 6 , —C(O)NR 6 R 7 , C 4-9 heteroaryl containing at least one heteroatom selected from the group consisting of N, O and S, one —OR 6 , or both of hydroxyl and —O—C 6-10 aryl unsubstituted or substituted by at least one selected from the group consisting of halogen, hydroxyl, C 1-6 alkoxy and C 1-6 alkyl.
[0069] Referring to Formula (I), most preferably, each of R 1 , R 2 , R 3 and R 4 , independently, is hydrogen or C 1-6 alkyl, and R is hydrogen, C 1-6 alkyl, —C(O)R 5 , or C 1-6 alkyl substituted by C(O)NR 6 R 7 , C 4-9 heteroaryl containing at least one heteroatom selected from the group consisting of N, O and S, one —OR 6 , or both of hydroxyl and —O—C 6-10 aryl unsubstituted or substituted by at least one selected from the group consisting of halogen, hydroxyl, C 1-6 alkoxy and C 1-6 alkyl. Herein, preferably, R 6 is C 4-9 heteroaryl containing at least one heteroatom selected from the group consisting of N, O and S, C 4-9 heterocyclyl containing at least one heteroatom selected from the group consisting of N, O and S, or C 6-10 aryl unsubstituted or substituted by at least one selected from the group consisting of halogen, hydroxyl, C 1-6 alkoxy and C 1-6 alkyl, and R 7 is hydrogen.
[0070] Referring to Formula (I), specifically, R may be hydrogen, C 1-6 alkyl,
[0000]
[0000] n being an integer from 0 to 5, and R′ independently being halogen, hydroxyl, C 1-6 alkoxy or C 1-6 alkyl.
[0071] Exemplary compounds of the formula (I) are shown below.
[0000]
Com-
pound
No.
Structure
1
2
3
4
5
6
7
8
9
10
11
[0072] In the present invention, the term “alkyl” refers to a straight or branched hydrocarbon. Examples of alkyl include, but are not limited to, methyl, ethyl, n-propyl, i-propyl, n-butyl, i-butyl, and t-butyl.
[0073] In the present invention, the term “aryl” refers to a 6-carbon monocyclic, 10-carbon bicyclic aromatic ring system wherein each ring may have 1 to 4 substituents. Examples of aryl groups include, but are not limited to, phenyl and naphthyl.
[0074] In the present invention, the term “alkoxy” refers to an —O-alkyl radical. Examples of alkoxy include, but are not limited to, methoxy, ethoxy, n-propoxy, isopropoxy, n-butoxy, iso-butoxy, sec-butoxy, and tert-butoxy.
[0075] In the present invention, the term “heteroaryl” refers to a hydrocarbon ring system (mono-cyclic or bi-cyclic) having at least one aromatic ring which contains at least one heteroatom such as O, N, or S as part of the ring system and the reminder being carbon. Examples of heteroaryl moieties include, but are not limited to, furyl, pyrrolyl, thienyl, oxazolyl, imidazolyl, thiazolyl, pyridinyl, pyrimidinyl, benzimidazolyl, benzothiazolyl, coumarinyl, quinazolinyl, and indolyl. In the present invention, the term “heterocyclyl” refers to a nonaromatic ring system having at least one heteroatoms (such as O, N, or S). Examples of heterocyclyl groups include, but are not limited to, piperidinyl, piperazinyl, pyrrolidinyl, dioxanyl, morpholinyl, and tetrahydrofuranyl.
[0076] According to the pharmaceutically acceptable compound of the present invention, preferably, the statin is selected from the group consisting of fluvastatin, pravastatin, atorvastatin, cerivastatin, rosuvastatin, pitavastatin, lovastatin acid and simvasatin acid. Until the present invention described herein, there was no report of a statin salt of aporphine compound. The statin salt of aporphine compound may achieve synergistic pharmacological activities. Statins can increase endothelial nitric oxide synthase expression on vascular endothelium. Aporphine compounds can inhibit lipid peroxidase, exert the free radical scavenging activities and protect vascular smooth muscle cells. The parts of the synergistic effects from aporphine compounds are lipid peroxidase inhibition, free radical scavenging activities, and vascular smooth muscle cells protection; and the other parts from statins are lowering-lipid effect, antioxidative effect, vascular protection and increase endothelial nitric oxide synthase expression. The above may make the statin salt of aporphine compound having better combined therapeutic effects in the preventing progression of atherosclerosis, cardiovascular protection and the prevention and treatment of coronary heart disease (CHD) events.
[0077] According to the pharmaceutically acceptable compound of the present invention, preferably, the angiotensin II receptor blocker is selected from the group consisting of valsartan, candesartan and telmisartan. Until the invention described herein, there was no report of angiotensin II receptor blocker (ARB) salt of aporphine compound. Angiotensin II receptor blocker salt of thaliporphine may achieve synergistic pharmacological activities. Angiotensin II receptor blockers can attenuate the oxidative stress and improve vascular function. Aporphine compounds can inhibit lipid peroxidase, exert the free radical scavenging activities and protect vascular smooth muscle cells. The parts of the synergistic effects from aporphine compounds are lipid peroxidase inhibition, free radical scavenging activities, and vascular smooth muscle cells protection; and the other parts from angiotensin II receptor blockers are antioxidative effect, lowering-hypertension effect, oxidative stress inhibition effect, endothelial nitric oxide synthase (eNOS) enhancing effect, and vascular function improvement. The above may make the angiotensin II receptor blocker salt of aporphine compound having better combined therapeutic effects in the preventing progression of atherosclerosis, cardiovascular protection and the prevention and treatment of coronary heart disease (CHD) events.
[0078] According to the pharmaceutically acceptable compound of the present invention, preferably, the angiotensin I converting enzyme inhibitor is selected from the group consisting of captopril, perindopril, ramipril, enalapril, fosinopril, quinapril, lisinopril and benazepril. Until the invention described herein, there was no report of Angiotensin I converting enzyme inhibitor (ACEI) salt of aporphine compound. Angiotensin I converting enzyme inhibitor salt of thaliporphine may achieve synergistic pharmacological activities. Angiotensin I converting enzyme inhibitors can protect against damages of vascular endothelium induced by homocysteine and scavenge oxygen free radicals. Aporphine compounds can inhibit lipid peroxidase, exert the free radical scavenging activities and protect vascular smooth muscle cells. The parts of the synergistic effects from aporphine compounds are lipid peroxidase inhibition, free radical scavenging activities, and vascular smooth muscle cells protection; and the other parts from angiotensin I converting enzyme inhibitors are antioxidative effect, lowering-hypertension effect, endothelial nitric oxide synthase (eNOS) enhancing effect, homocysteine inhibition effect and protection against damages of vascular endothelium. The above may make the angiotensin I converting enzyme inhibitor salt of aporphine compound having better combined therapeutic effects in the preventing progression of atherosclerosis, cardiovascular protection and the prevention and treatment of coronary heart disease (CHD) events.
[0079] According to the pharmaceutically acceptable compound of the present invention, preferably, the fibric acid is selected from the group consisting of bezafibrate, clofibric acid, fenofibric acid and gemfibrozil. Until the invention described herein, there was no report of fibric acid salt of aporphine compound. Fibric acid salt of aporphine compound may achieve synergistic pharmacological activities. Fibric acids can effectively lower triglycerides and reverse the oxidative stress. Aporphine compounds can inhibit lipid peroxidase, exert the free radical scavenging activities and protect vascular smooth muscle cells. The parts of the synergistic effects from aporphine compounds are lipid peroxidase inhibition, free radical scavenging activities, and vascular smooth muscle cells protection; and the other parts from fibric acids are antioxidative effect, lowering-triglyceride effect, endothelial nitric oxide synthase (eNOS) enhancing effect, and oxidative stress inhibition. The above may make the fibric acid salt of aporphine compound having better combined therapeutic effects in the preventing progression of atherosclerosis, cardiovascular protection and the prevention and treatment of coronary heart disease (CHD) events.
[0080] According to the pharmaceutically acceptable compound of the present invention, preferably, the meglitinide is selected from the group consisting of repaglinide, nateglinide and mitiglinide. Until the invention described herein, there was no report of meglitinide salt of aporphine compound. Meglitinide salt of aporphine may achieve synergistic pharmacological activities. Meglitinide can improvement of post-prandial glucose levels. Aporphine compounds can also produce antihyperglycemic effect. The parts of the synergistic effects from aporphine compounds are lipid peroxidase inhibition, free radical scavenging activities, and vascular smooth muscle cells protection; and the other part from meglitinides is antihyperglycemic effect. The above may make the meglitinide salt of aporphine compound having better combined therapeutic effects in the preventing or treating hyperglycemic disease in human and mammal and cardiovascular protection.
[0081] According to the pharmaceutically acceptable compound of the present invention, preferably, the specific acid is selected from the group consisting of an amino acid, a phenolic acid, a chromocarb, an ozagrel, a capobenic acid, a pyruvic acid, a 2-ketoglutaric acid, a phosphocreatine, a thioctic acid, an acipimox, an ambrisentan, a tirofiban, an active metabolite of clopidogrel and an active metabolite of ticlopidine. Herein, the amino acid is one selected from the group consisting of a cysteine, an acetyl cysteine, a thioproline, a carnosine, a carnitine, a phosphoserine, a tiopronin, a methionine, a glutamine, a glutathione, a pyridoxal 5-phosphate, a nicotinic acid, a mono-arginine oxoglurate, a taurine and an orotic acid, and the phenolic acid is one selected from the group consisting of an acetyl salicylic acid, a salsalate, a caffeic acid, a ferulic acid, a p-hydroxyphenylacetic acid, a 4-hydroxy-3-methoxyphenylacetic acid, a p-coumaric acid, and a sinapic acid. For specific acid salt of aporphine, the parts of the synergistic effects from aporphine compounds are lipid peroxidase inhibition, free radical scavenging activities, and vascular smooth muscle cells protection; and parts from specific acids are antioxidative effect and endothelial nitric oxide synthase (eNOS) enhancing effect. The above may make the specific acid salt of aporphine having better combined therapeutic effects in the myocardial protection and the prevention and treatment of coronary heart disease (CHD) events.
[0082] Accordingly, the novel aporphine compound salts may be employed for treating and/or preventing hyperglycemic disease and several oxidative stress related diseases, such as coronary syndromes, neurodegenerative disorders, reducing cholesterol levels as well as may achieve other therapeutic effects, including treatment and/or prophylaxis of cardiac diseases, including cardiac arrhythmia, myocardial ischemia or myocardial infarction, and sudden death caused by cardiac arrhythmia or acute myocardial infarction and treatment of cardiovascular disorders, especially hypertension and congestive heart failure and preventing progression of coronary atherosclerosis, and treatment and/or prophylaxis of ischemic diseases, especially ischemic cerebral apoplexy, ischemic cerebral thrombosis, ischemic cerebral embolism, hypoxic ischemic encephalopathy, ischemic cardiac disease or ischemic enteropathy.
[0083] In the present invention, the pharmaceutically acceptable compound of the present invention can be administered by any suitable route including transnasal, topical, rectal, buccal, oral or parenteral. The pharmaceutically acceptable compound may be liquid or solid for topical, oral or parenteral administration in form of tablets, capsules and pills eventually with enteric coating, powders, granules, pellets, emulsions solutions, suspensions, syrups, elixir, ointments, creams, injectable forms or liposomes.
[0084] The present invention further provide a method for preparing the above-mentioned pharmaceutically acceptable compound, including the following steps: dissolving the basic group-containing compound of the formula (I) in a free base form or in a salt form and the carboxyl group-containing agent in a free acid form or in a salt form in a first solvent to form a solution; and removing the first solvent from the solution or mixing the solution with a second solvent to obtain the pharmaceutically acceptable compound.
[0085] In the method for preparing the pharmaceutically acceptable compound according to the present invention, the first solvent used might be any solvent in which the basic group-containing compound of the formula (I) and the carboxyl group-containing agent can be well dissolved, such as water, C 1-8 straight or branched alcohols, acetone, methyl ethyl ketone, methyl isobutyl ketone, dichloromethane, diethyl ether, diisopropyl ether, dimethyl sulfoxide, N,N′-dimethylformamide, N,N′-dimethylacetamide, and a mixture of the above-mentioned thereof. Additionally, the second solvent used might be any solvent, which is miscible with the first solvent and can cause the precipitation of the pharmaceutically acceptable compound, such as acetonitrile, ethanol, acetone, methyl ethyl ketone, dichloromethane, diethyl ether, diisopropyl ether, or the combination thereof.
[0086] In the method for preparing the pharmaceutically acceptable compound according to the present invention, any conventional methods that can be used to remove the solvent can be used for removing the solvent from the mixture. The preferred methods for removing the solvent include, but are not limited to, concentrated and crystallized by natural evaporation, vacuum concentration, or drying under nitrogen.
[0087] The present invention further provide another method for preparing the above-mentioned pharmaceutically acceptable compound, including the following steps: mixing the basic group-containing compound of the formula (I) in a free base form or in a salt form and the carboxyl group-containing agent in a base form or in a salt form to form a mixture; and pulverizing the mixture by a physical-mechanical means to form the pharmaceutically acceptable compound. Herein, an example of the physical-mechanical means is pulverizing the mixture in a motar with a pestle.
[0088] Additionally, the obtained pharmaceutically acceptable salt can be further purified by dissolving the salt in a suitable solvent, concentrated and recrystallized by evaporating the solvent by natural evaporation, vacuum concentration, or drying under nitrogen.
[0089] The present invention also provides a pharmaceutical formulation which comprises the above-mentioned pharmaceutically acceptable compound and a pharmaceutically acceptable carrier. The pharmaceutical formulation is suitable for use in transnasal, transdermal, rectal, oral treatment or parenteral injection.
[0090] These pharmaceutically acceptable salts may be used to manufacture medicaments for treating and/or preventing hyperglycemic disease and treatment and/or prophylaxis of cardiac diseases, including cardiac arrhythmia, myocardial ischemia or myocardial infarction, and sudden death caused by cardiac arrhythmia or acute myocardial infarction, or to manufacture medicaments for preventing or treating ischemic diseases, and the ischemic diseases may include ischemic cerebral apoplexy, ischemic cerebral thrombosis, ischemic cerebral embolism, hypoxic ischemic encephlopathy, ischemic cardiac disease or ischemic enteropathy etc.
[0091] Also within the scope of this invention is a method for treating oxidative stress induced diseases by administering to a subject in need thereof an effective amount of the above-mentioned pharmaceutically acceptable compound.
[0092] Other objects, advantages, and novel features of the invention will become more apparent from the following detailed description when taken in conjunction with the accompanying drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
[0093] FIG. 1 shows a diagram of absorbance of DPPH versus the concentration of Compounds 1 and 2 (—▪— for Compound 1, —∘— for Compound 2).
[0094] FIG. 2 shows a diagram of absorbance of DPPH versus the concentration of thaliporphine, atorvastatin and atorvastatin salt of thaliporphine (—— for thaliporphine, —∘— for atorvastatin, —▾— for atorvastatin salt of thaliporphine).
[0095] FIG. 3 shows a diagram of absorbance of DPPH versus the concentration of thaliporphine, telmisartan and telmisartan salt of thaliporphine (—— for thaliporphine, —∘— for telmisartan, —▾— for telmisartan salt of thaliporphine).
[0096] FIG. 4 shows a diagram of absorbance of DPPH versus the concentration of thaliporphine, captopril and captopril salt of thaliporphine (—— for thaliporphine, —∘— for captopril, —▾— for captopril salt of thaliporphine).
[0097] FIG. 5 shows a diagram of absorbance of DPPH versus the concentration of thaliporphine, bezafibrate and bezafibrate salt of thaliporphine (—— for thaliporphine, —∘— for bezafibrate, —▾— for bezafibrate salt of thaliporphine).
[0098] FIG. 6 shows a diagram of absorbance of DPPH versus the concentration of thaliporphine, nateglinide and nateglinide salt of thaliporphine (—— for thaliporphine, —∘— for nateglinide, —▾— for nateglinide salt of thaliporphine).
[0099] FIG. 7 shows a diagram of absorbance of DPPH versus the concentration of thaliporphine, acetylcysteine and acetylcysteine salt of thaliporphine (—— for thaliporphine, —∘— for acetylcysteine, —▾— for acetylcysteine salt of thaliporphine).
[0100] FIG. 8 shows a diagram of absorbance of DPPH versus the concentration of thaliporphine, salsalate and salsalate salt of thaliporphine (—— for thaliporphine, —∘— for salsalate, —▾— for salsalate salt of thaliporphine).
[0101] FIG. 9 shows a fluorescence decay dynamics of β-phycoerythin (—for 0.1% DMSO as a control group, - -- - for Compound 1 of 5×10 −6 M, --- for Compound 2 of 5×10 −6 M).
[0102] FIG. 10 shows a fluorescence decay dynamics of fluorescenin (—for 0.1% DMSO as a control group, . . . for thaliporphine of 10 −6 M, —for atorvastatin of 10 −6 M, - -- - for atorvastatin salt of thaliporphine of 10 −6 M).
[0103] FIG. 11 shows a fluorescence decay dynamics of fluorescenin (—for 0.1% DMSO as a control group, . . . for thaliporphine of 10 −6 M, --- for captopril of 10 −6 M, - -- - for captopril salt of thaliporphine of 10 −6 M).
[0104] FIG. 12 shows a fluorescence decay dynamics of fluorescenin (—for 0.1% DMSO as a control group, . . . for thal iporphine of 10 −6 M, --- for bezafibrate of 10 −6 M, - -- - for bezafibrate salt of thaliporphine of 10 −6 M).
[0105] FIG. 13 shows a fluorescence decay dynamics of fluorescenin (—for 0.1% DMSO as a control group, . . . for thaliporphine of 10 −6 M, --- for nateglinide of 10 −6 M, - -- - for nateglinide salt of thaliporphine of 10 −6 M).
[0106] FIG. 14 shows a fluorescence decay dynamics of fluorescenin (—for 0.1% DMSO as a control group, . . . for thaliporphine of 10 −6 M, --- for acetylcysteine of 10 −6 M, - -- - for acetylcysteine salt of thaliporphine of 10 −6 M).
[0107] FIG. 15 shows a fluorescence decay dynamics of fluorescenin (—for 0.1% DMSO as a control group, . . . for thaliporphine of 10 −6 M, --- for salsalate of 10 −6 M, - -- - for salsalate salt of thaliporphine of 10 −6 M).
[0108] FIG. 16 shows a fluorescence decay dynamics of fluorescenin (—for 0.1% DMSO as a control group, . . . for glaucine of 10 −6 M, --- for ozagrel of 10 −6 M, - -- - for ozagrel salt of glaucine of 10 −6 M).
[0109] FIG. 17 shows a diagram of cell viability versus the concentration of Compounds 1 and 2 (▭ for a control group, for H 2 O 2 of 200 μM, for Compound 1+H 2 O 2 of 200 μM, for Compound 2+H 2 O 2 of 200 μM).
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
[0110] According to the present invention, the pharmaceutically acceptable salts may be formed by (1) the interaction of the acid (i.e. the carboxyl group-containing agent) with the base (i.e. the aporphine compound); and (2) the solvent dissolution-removal or pulverization method employed in the present invention which further enhances the salt forming process. The pharmaceutically acceptable salts may be readily filtered and easily dried, and, if necessary, can be easily re-purified by re-dissolving the salt in a suitable solvent followed by drying to remove the solvent, or followed by mixing the resulting solution with another suitable solvent to precipitate the pharmaceutically acceptable compound.
[0111] For example, the pharmaceutically acceptable salts may be prepared in accordance with the following procedure.
[0112] To a round bottom flask equipped with a magnetic stirrer was charged an aporphine compound, a chosen carboxyl group-containing agent, and an appropriate solvent system. The resulting reaction mixture was allowed to agitate at a certain temperature for a certain period of time until it was dissolved completely. The resulting solution was concentrated via reduced pressure distillation, or the resulting solution was mixed with another suitable solvent, and the desired aporphine compound-carboxylic acid salt was thus obtained.
[0113] In addition, with regard to aporphine compounds included in pharmaceutically acceptable salts, some aporphine derivatives (e.g. thaliporphine, norglaucine, N-[2-(2-methoxyphenoxy)ethyl]norglaucine) are known, while some aporphine derivatives are novel and cannot be commercially provided (such as theses above-mentioned exemplary compounds 1-7). Thereby the present invention provides methods for preparing novel aporphine derivatives.
[0114] Northaliporphine can be found within the U.S. Pat. No.4,202,980, norglaucine can be found within the U.S. Pat. No.4,120,964, boldine, thaliporphine, glaucine, laurolitsine, can be employed as the starting material to generate the aporphine derivatives of the general formula (I). The boldine is available from the market, the thaliporphine and the glaucine can be synthesized according to U.S. Pat. No.6,313,134 B1, and the norglaucine, the northaliporphine and the laurolitsine can be synthesized according to U.S. Pat. No. 7,294,715 B2.
[0115] An acylation or alkylation reaction may be involved in the preparation of the aporphine derivatives. These various aporphine derivatives can be achieved by various approaches (eg. Acylation by acyl halide, acyl anhydride, or mixed anhydride; alkylation from a suitable alkylating agent, reductive amination from a suitable aldehyde and hydrogenation from a suitable imine, etc.). By using the above preparation processes, the general formula (I) can be synthesized.
[0116] Accordingly, theses above-mentioned exemplary compounds 1-7 can be obtained by the following synthesis schemes 1-7, respectively.
[0117] The following examples are illustrative, but not limiting the scope of the present invention. Reasonable variations, such as those occur to reasonable artisan, can be made herein without departing from the scope of the present invention.
PREPARATION EXAMPLE 1
Preparation of Compound 1
[0118]
[0119] Northaliporphine (380 mg, 1.16 mmol), methanol (MeOH, 10 mL) and 2-[(2-methoxy-phenox)methyl]oxirane (167 mg, 0.92 mmol) were added into a 50 mL round bottom flask and stirred at 70° C. for 16 hours. The mixture was evaporated to dryness. The residue was purified by chromatography (silica gel: 70-230 mesh 30 g, mobile phase: 2% MeOH/CH 2 Cl 2 , v/v) to obtain Compound 1, R f 0.15 (2% MeOH/CH 2 Cl 2 , v/v); Physical data were as follows: mp: 63-68° C. (CH 2 Cl 2 ); IR(KBr)v max : 3500, 2931, 1605, 1506, 1464, 1253, 1112 cm −1 ; 1 H NMR (CDCl 3 , 500 MHz):δ 8.00 (s, 1H), 6.98-6.88 (m, 4H), 6.75 and 6.73 (s, 1H), 6.53 (s, 1H), 6.12 (brs, 1H), 4.24-4.07 (m, 3H), 3.90 (s, 3H), 3.88 (s, 3H), 3.85 (s, 3H), 3.79 (s, 3H), 3.39-2.53 (m, 9H); EIMS (70 eV): m/z (%) 507 [M] + , 339 (100).
PREPARATION EXAMPLE 2
Preparation of Compound 2
[0120]
[0121] Northaliporphine (260 mg, 0.794 mmol), MeOH (10 mL) and 2-chloro-N-(2,6-dimethyl-phenyl)acetamide (187 mg, 0.946 mmol) were added into a 50 mL two-necked round bottom flask. Then triethylamine (Et 3 N, 0.5 mL, 3.55 mmol) was dropped into the mixture, and the reaction was allowed to proceed at 60° C. for two days. The mixture was evaporated to dryness. The residue was partitioned with water (50 mL) and dichloromethane (50 mL×3), and the organic layers were collected. The organic layer was dried with anhydrous MgSO 4 and then filtered. The filtrate was evaporated to dryness. The residue was purified by chromatography (silica gel: 70-230 mesh 30 g, mobile phase: 2% MeOH/CH 2 Cl 2 , v/v) to obtain Compound 2, R f 0.58 (2% MeOH/CH 2 Cl 2 , v/v); Physical data were as follows: mp: 205-207° C. (CH 2 Cl 2 ); IR(KBr)v max : 3312, 2945, 1663,1 604, 1511, 1477, 1258, 1087 cm −1 ; 1 H NMR(CDCl 3 , 500 MHz):δ 8.99 (s, 1H), 8.02 (s, 1H), 7.10 (s, 3H), 6.76 (s, 1H), 6.56 (s, 1H), 6.12 (s, 1H), 3.91 (s, 9H), 3.77-3.11 (m, 5H), 2.98-2.86 (m, 2H), 2.75-2.69 (m, 2H), 2.25 (s, 6H); EIMS (70 eV): m/z (%) 488 [M] + , 326 (100).
PREPARATION EXAMPLE 3
Preparation of Compound 3
[0122]
[0123] Norglaucine (300 mg, 0.88 mmol), MgSO 4 (1 g), MeOH (7 mL), 2-thiophenecarboxaldehyde (0.14 mL, 1.5 mmol) and AcOH (0.5 mL, 8.88 mmol) were added into a 100 mL two-necked round bottom flask and stirred at room temperature. Sodium cyanoborohydride (NaBH 3 CN, 100 mg, 1.58 mmol) was added into the mixture after 1 hour, and the reaction was allowed to proceed at 70° C. for 4 hours. The mixture was evaporated to dryness. The residue was partitioned with water (50 mL) and dichloromethane (50 mL×2), and the organic layers were collected. The organic layer was dried with anhydrous MgSO 4 and then filtered. The filtrate was evaporated to dryness. The residue was purified by chromatography (silica gel: 230-400 mesh 30 g, mobile phase: EA/Hex=1/2, v/v) to obtain Compound 3, R f 0.77 (EA/Hex=1/1, v/v); Physical data were as follows: mp: 143-148° C. (CH 2 Cl 2 ); IR(KBr)v max : 2958, 1578, 1514, 1466, 1110 cm −1 ; 1 H NMR(CDCl 3 , 400 MHz):δ 8.05 (s, 1H), 7.22-7.20 (m, 1H), 6.96-6.95 (m, 2H), 6.77 (s, 1H), 6.57 (s, 1H), 4.35 (d, J=14.6 Hz, 1H), 3.92 (s, 3H), 3.88 (s, 3H), 3.86 (s, 3H), 3.85 (d, J=14.6 Hz, 1H), 3.62 (s, 3H), 3.36-3.33 (m, 1H), 3.15-3.09 (m, 2H), 3.05-3.02 (m, 1H), 2.71-2.60 (m, 2H), 2.51-2.44 (m, 1H); EIMS (70 eV): m/z (%) 437 [M] + , 97 (100).
PREPARATION EXAMPLE 4
Preparation of Compound 4
[0124]
[0125] 2-Aminopyridine (2 g, 21.3 mmol), chloroacetyl chloride (2.5 mL, 31.4 mmol) and Et 3 N (4.4 mL, 31.8 mmol) were dissolved in dichloromethane (CH 2 Cl 2 , 100 mL). The reaction mixture was stirred at room temperature for 17 hours, after which the organic phase was washed with an aqueous solution of NaHCO 3 (10%, w/v). The organic layer was dried with anhydrous MgSO 4 and then filtered. The filtrate was evaporated to dryness. The residue was purified using flash chromatography (CH 2 Cl 2 ), yielding 2.46 g (68%) of 2-(chloroacetyl)amidopyridine.
[0126] Norglaucine (0.3 g, 0.88 mmol), 2-(chloroacetyl)amidopyridine (0.15 g, 0.88 mmol) and potassium carbonate (K 2 CO 3 , 0.3 g, 1.8 mmol) in acetonitrile (CH 3 CN, 7 mL) was stirred at 80° C. for 16 hours. The mixture was evaporated to dryness. The residue was partitioned with water (50 mL) and dichloromethane (50 mL×2). The organic layer was dried with anhydrous MgSO 4 and then filtered. The filtrate was evaporated to dryness. The residue was purified by chromatography (silica gel: 230-400 mesh 30 g, mobile phase: EA/Hex=1:1, v/v) to obtain Compound 4, R f 0.75 (100% EA); Physical data were as follows: mp: 43-46° C. (CH 2 Cl 2 ); IR(KBr)v max : 3300, 2933, 1693, 1578, 1513, 1434, 1257, 1091 cm −1 ; 1 H NMR (CDCl 3 , 400 MHz):δ 9.87 (s, 1H), 8.29-8.24 (m, 2H), 8.04 (s, 1H), 7.73-7.69 (m, 1H), 7.04-7.01 (m, 1H), 6.70 (s, 1H), 6.61 (s, 1H), 3.89 (s, 3H), 3.87 (s, 6H), 3.63 (s, 3H), 3.61 (d, J=17.2 Hz, 1H), 3.46-3.42 (m, 1H), 3.30-3.23 (m, 2H), 3.13-3.08 (m, 1H), 2.92-2.68 (m, 4H); ESI-MS (30 V): m/z (%) 476 [M+H] + (100).
PREPARATION EXAMPLE 5
Preparation of Compound 5
[0127]
[0128] Norglaucine (500 mg, 1.47 mmol), chloroacetyl chloride (0.35 mL, 4.4 mmol) and CH 2 Cl 2 (7 mL) were added into a 100 mL round bottom flask. Then 0.6 mL of Et 3 N was dropped into a round bottom flask at room temperature for 1 hour. The reaction solution was poured into 50 mL water, and the mixture was stirred and adjusted with ammonia water to pH 8.0. The mixture was extracted two times with dichloromethane, and the organic layers were collected. The organic layer was dried with anhydrous MgSO 4 and then filtered. The filtrate was evaporated to dryness. The residue was purified by chromatography (silica gel: 230-400 mesh 30 g, mobile phase: EA/Hex=1/1, v/v) to obtain chloroacetamide A, R f 0.46 (EA/Hex=1/1, v/v).
[0129] Chloroacetamide A (300 mg, 0.719 mmol) and piperidine (0.5 mL) in CH 3 CN (7 mL) was stirred at 80° C. for 16 hours and the reaction progress was monitored by silica TLC. The mixture was evaporated to dryness. The residue was partitioned with water (50 mL) and dichloromethane (50 mL×2), and the organic layers were collected. The organic layer was dried with anhydrous MgSO 4 and then filtered. The filtrate was evaporated to dryness. The residue was purified by chromatography (silica gel: 230-400 mesh 20 g, mobile phase: EA/Hex=1:1, v/v) to obtain Compound 5, R f 0.33 (100% EA); Physical data were as follows: mp: 108-110° C. (CH 2 Cl 2 ); IR(KBr)v max : 2934, 1640, 1514, 1451, 1254, 1102 cm −1 ; 1 H NMR(CDCl 3 ,400MHz):δ 8.12 (s, 1H), 6.76 (s, 1H), 6.62 (s, 1H), 5.00-4.00 (m, 2H), 3.89 (s, 3H), 3.88 (s, 6H), 3.65 (s, 3H), 3.33-2.66 (m, 7H), 2.43 (m, 4H), 1.57-1.56 (m, 4H), 1.42 (m, 2H); EIMS (70 eV): m/z (%) 466 [M] + , 381 (100).
PREPARATION EXAMPLE 6
Preparation of Compound 6
[0130]
[0131] Nicotinic acid (0.1 g, 0.86 mmol) was heated under reflux with thionyl chloride (1.0 mL, 12.4 mmol) for 1 hour. The solvent was evaporated under reduced pressure. An off-white solid was formed and the product was used immediately for the next step.
[0132] Norglaucine (0.2 g, 0.58 mmol) and Et 3 N (0.23 mL, 1.56 mmol) were dissolved in CH 3 CN (1 mL). The mixture was reacted with nicotinoyl chloride in CH 3 CN (1 mL) by adding it drop by drop at room temperature. The mixture was stirred at room temperature for 1 hour, and the solvent was evaporated under reduced pressure. The residue was partitioned with water (10 mL) and dichloromethane (10 mL), and the organic layer was evaporated under reduced pressure. The residue was purified by chromatography (silica gel: 230-400 mesh 15 g, mobile phase: EA/Hex=1:1, v/v) to obtain Compound 6, R f 0.3 (100% EA); Physical data were as follows: mp: 178-181° C. (CH 2 Cl 2 ); IR(KBr)v max : 2947, 1632, 1514, 1466, 1265, 1099 cm −1 ; 1 H NMR (CDCl 3 , 400 MHz):δ 8.70 (s, 1H), 8.67 (brd, J=4.1 Hz, 1H), 8.14 (s, 1H), 7.78 (brd, J=7.7 Hz, 1H), 7.39-7.36 (m, 1H), 6.78 (s, 1H), 6.62 (s, 1H), 3.90 (s, 6H), 3.88 (s, 3H), 3.66 (s, 3H), 3.72-2.64 (m, 6H); EIMS (70 eV): m/z (%) 446 [M] + (100).
PREPARATION EXAMPLE 7
Preparation of Compound 7
[0133]
[0134] Nicotinic acid (865 mg, 7 mmol) was heated under reflux with thionyl chloride (3.5 mL, 48.5 mmol) for 1 hour. The solvent was evaporated under reduced pressure. An off-white solid was formed and the product was used immediately for the next step.
[0135] Boldine (1 g, 3.1 mmol), nicotinoyl chloride (1 g, 7.1 mmol), Et 3 N (1.3 mL, 9.3 mmol) and toluene (12 mL) were added into a 100 ML round bottom flask. The mixture was stirred at 80° C. for 17 hours and the reaction progress was monitored by silica TLC. After removing the salt by filtration, the filtrate was evaporated to dryness. The residue was partitioned with water (75 mL) and dichloromethane (75 mL×3), and the organic layers were collected. The organic layer was dried with anhydrous MgSO 4 and then filtered. The filtrate was evaporated to dryness. The residue was purified by chromatography (silica gel: 230-400 mesh 50 g, mobile phase: MeOH/CH 2 Cl 2 =1/8, v/v) to obtain Compound 7, R f 0.58 (MeOH/CH 2 Cl 2 =1/6, v/v); Physical data were as follows: mp: 110-113° C. (MeOH); IR(KBr)v max : 2955, 1744, 1589, 1421, 1273, 1096 cm −1 ; −1 H NMR (CD 3 OD, 400 MHz):δ 9.25 (d, J=2.0 Hz, 1H), 9.19 (d, J=2.0 Hz, 1H), 8.77 (dd, J=5.1, 1.4 Hz, 1H), 8.74 (dd, J=5.0, 1.4 Hz, 1H), 8.53-8.50 (m, 1H), 8.47-8.45 (m, 1H), 8.05 (s, 1H), 7.60-7.54 (m, 1H), 7.14 (s, 1H), 6.99 (s, 1H), 3.73 (s, 3H), 3.52 (s, 3H), 2.50 (s, 3H), 3.15-2.46 (m, 7H); ESI-MS (30 V): m/z (%) 538 [M+H] + , 106 (100).
[0136] In the following examples, a prepared salt of an aporphine derivative and a carboxyl group-containing agent are characterized by their distinctive physical and chemical properties, which are different from either the carboxyl group-containing agent alone or the aporphine derivative alone, as demonstrated by the FTIR, MS, and NMR analyses.
[0137] Infrared spectroscopy (IR) has long been used in the evaluation of chemical compounds. Fourier Transform Infrared Spectroscopy (FT-IR) has been used to identify and evaluate organic and inorganic materials or compounds. Using FTIR, spectral data is collected and converted from an interference pattern to a spectrum. The system provides for subtractive elimination of background spectra, such that particular chemical compounds can be identified by a molecular “fingerprint”.
[0138] Electro-spray Ionization Mass Spectroscopy (ESI-MS) can be used to determine the molecular weights and the chemical structures of the pharmaceutically acceptable salts.
[0139] Nuclear magnetic resonance solutions provide useful data regarding the type, quantity and arrangement of different atoms in chemical systems, liquids and solids.
EXAMPLE 1
Preparation of an Atorvastatin salt of the Thaliporphine by Thaliporphine Free Base and Atorvastatin Free Acid
[0140] Thaliporphine free base (0.0741 g, 0.217 mmol) and Atorvastatin free acid (0.1262 g, 0.226 mmol) were thoroughly mixed and then added to 5 mL of methanol. The resultant mixture was then stirred until the mixture was dissolved. The Atorvastatin salt of Thaliporphine was obtained as removing the methanol by reduced-pressure or vacuum concentration, or drying under nitrogen until the sample was completely dried.
[Thaliporphine]
[0000]
IR(KBr)v max : 3272, 1602, 1517, 1465, 1255, 1112, 1083 cm −1
Molecular Weight: 341
[Atorvastatin]
[0000]
IR(KBr)v max : 3380, 1717, 1640, 1508 cm −1
Molecular Weight: 558
[Atorvastatin Salt of Thaliporphine]
[0000]
IR(KBr)v max : 3402, 2959, 1663, 1596, 1510, 1465, 1253, 1107 cm −1
Molecular Weight: 899
ESI-MS (30V): m/z (%) 900 [M+H] + , 342 (100)
[0148] 1 H NMR (CD 3 OD, 500 MHz):δ 8.14 (s, 1H), 7.29-7.28 (m, 2H), 7.23-7.19 (m, 4H), 7.13-7.00 (m, 8H), 6.89 (s, 1H), 6.67 (s, 1H), 4.06-3.90 (m, 2H), 3.88 (s, 3H), 3.85 (s, 3H), 3.83 (s, 3H), 3.66-3.58 (m, 2H), 3.39-3.35 (m, 2H), 3.19-3.16 (m, 2H), 2.99-2.93 (m, 1H), 2.82-2.78 (m, 5H), 2.65 (t, J=14.0 Hz, 1H), 2.35-2.24 (m, 2H), 1.71-1.65 (m, 2H), 1.53-1.48 (m, 2H), 1.46 (d, J=7.0 Hz, 6H).
EXAMPLE 2
Preparation of a Telmisartan salt of the Thaliporphine by Thaliporphine Free Base and Telmisartan Free Acid
[0149] Thaliporphine free base (0.12 g, 0.351 mmol) and Telmisartan free acid (0.18 g, 0.351 mmol) were thoroughly mixed and then added to 5 mL of methanol. The resultant mixture was then stirred until the mixture was dissolved. The Telmisartan salt of Thaliporphine was obtained as removing the methanol by reduced-pressure or vacuum concentration, or drying under nitrogen until the sample was completely dried.
[Thaliporphine]
[0000]
IR(KBr)v max : 3272, 1602, 1517, 1465, 1255, 1112, 1083 cm −1
Molecular Weight: 341
[Telmisartan]
[0000]
IR(KBr)v max : 3431, 3059, 2963, 1696, 1461, 1267, 742 cm −1
Molecular Weight: 514
[Telmisartan Salt of Thaliporphine]
[0000]
IR(KBr)v max : 3392, 2957, 1601, 1516, 1461, 1253, 1106 cm −1
Molecular Weight: 855
ESI-MS (30V): m/z (%) 856 [M+H] + , 279 (100)
[0157] 1 H NMR (CD 3 OD, 500 MHz):δ 8.12 (s, 1H), 7.63 (d, J=6.5 Hz, 2H), 7.47-7.46 (m, 2H), 7.40 (t, J=7.5 Hz, 2H), 7.29-7.22 (m, 6H), 7.03 (d, J=7.0 Hz, 2H), 6.82 (s, 1H), 6.60 (s, 1H), 5.45-5.37 (m, 2H), 3.84 (s, 3H), 3.81 (s, 9H), 3.69 (s, 3H), 3.60-3.58 (m, 2H), 3.17-2.95 (m, 5H), 2.67 (s, 3H), 2.51-2.45 (m, 2H), 1.82-1.81 (m, 2H), 1.02 (t, J=7.5 Hz, 3H).
EXAMPLE 3
Preparation of a Captopril Salt of the Thaliporphine by Thaliporphine Free Base and Captopril Free Acid
[0158] Thaliporphine free base (0.1222 g, 0.356 mmol) and Captopril free acid (0.078 g, 0.359 mmol) were thoroughly mixed and then added to 2 mL of methanol. The resultant mixture was then stirred until the mixture was dissolved. The Captopril salt of Thaliporphine was obtained as removing the methanol by reduced-pressure or vacuum concentration, or drying under nitrogen until the sample was completely dried.
[Thaliporphine]
[0000]
IR(KBr)v max : 3272, 1602, 1517, 1465, 1255, 1112, 1083 cm −1
Molecular Weight: 341
[Captopril]
[0000]
IR(KBr)v max : 2980, 2566, 1748, 1589 cm −1
Molecular Weight: 217
[Captopril Salt of Thaliporphine]
[0000]
IR(KBr)v max : 3421, 2966, 1607, 1517, 1464, 1396, 1255, 1106 cm −1
Molecular Weight: 558
ESI-MS (30V): m/z (%) 559 [M+H] + , 342 (100)
[0166] 1 H NMR (CD 3 OD, 500 MHz):δ 8.14 (s, 1H), 6.90 (s, 1H), 6.70 (s, 1H), 4.39-4.36 (m, 1H), 3.89 (s, 3H), 3.86 (s, 3H), 3.83 (s, 3H), 3.69-3.53 (m, 4H), 3.28-3.15 (m, 3H), 2.94 (s, 3H), 2.86-2.66 (m, 4H), 2.44-2.33 (m, 1H), 2.21-2.11 (m, 2H), 2.01-1.91 (m, 2H), 1.13 (d, J=7 Hz, 3H).
EXAMPLE 4
Preparation of a Bezafibrate Salt of the N-[2-(2-methoxyphenoxy)ethyl]norglaucine by N-[2-(2-methoxyphenoxy) ethyl]norglaucine Free Base and Bezafibrate Free Acid
[0167] N-[2-(2-methoxyphenoxy)ethyl]norglaucine free base (0.128 g, 0.26 mmol) and Bezafibrate free acid (0.094 g, 0.26 mmol) were thoroughly mixed and then added to 5 mL of methanol. The resultant mixture was then stirred until the mixture was dissolved. The Bezafibrate salt of N-[2-(2-methoxyphenoxy)ethyl]norglaucine was obtained as removing the methanol by reduced-pressure or vacuum concentration, or drying under nitrogen until the sample was completely dried.
[N-[2-(2-methoxyphenoxy)ethyl]norglaucine]
[0000]
IR(KBr)v max : 2933, 1593, 1506, 1463, 1253, 1113, 1095, 1025 cm −1
Molecular Weight: 491
[Bezafibrate]
[0000]
IR(KBr)v max : 3358, 2886, 1718, 1610, 1549, 1147 cm −1
Molecular Weight: 361
[Bezafibrate salt of N-[2-(2-methoxyphenoxy)ethyl]norglaucine]
[0000]
IR(KBr)v max : 3402, 2935, 1595, 1508, 1465, 1253, 1110 cm −1
Molecular Weight: 852
ESI-MS (30V): m/z (%) 853 [M+H] + , 492 (100)
[0175] 1 H NMR (CD 3 OD, 500 MHz):δ 8.00 (s, 1H), 7.72 (d, J=7.5 Hz, 2H), 7.43 (d, J=7.5 Hz, 2H), 7.07 (d, J=8.0 Hz, 2H), 7.01 (d, J=8.0 Hz, 1H), 6.95-6.90 (m, 4H), 6.82 (d, J=8.0 Hz, 2H), 6.77 (s, 1H), 4.37-4.33 (m, 2H), 3.86 (s, 6H), 3.85 (s, 3H), 3.70 (s, 3H), 3.64 (s, 3H), 3.51 (t, J=7.0 Hz, 2H), 3.49-2.87 (m, 8H), 2.81 (t, J=7.0 Hz, 2H), 1.50 (s, 6H).
EXAMPLE 5
Preparation of a Repaglinide Salt of the Glaucine by Glaucine Free Base and Repaglinide Free Acid
[0176] Glaucine free base (0.2 g, 0.563 mmol) and Repaglinide free acid (0.255 g, 0.563 mmol) were thoroughly mixed and then added to 5 mL of methanol. The resultant mixture was then stirred until the mixture was dissolved. The Repaglinide salt of Glaucine was obtained as removing the methanol by reduced-pressure or vacuum concentration, or drying under nitrogen until the sample was completely dried.
[Glaucine]
[0000]
IR(KBr)v max : 2962, 1597, 1516, 1463, 1251, 1113, 1091 cm −1
Molecular Weight: 355
[Repaglinide]
[0000]
IR(KBr)v max : 3308, 2935, 1687, 1637, 1217 cm −1
Molecular Weight: 452
[Repaglinide Salt of Glaucine]
[0000]
IR(KBr)v max : 3292, 2934, 1653, 1609, 1516, 1464, 1110 cm −1
Molecular Weight: 807
ESI-MS (30V): m/z (%) 808 [M+H] + ,162 (100)
[0184] 1 H NMR (CD 3 OD, 500 MHz):δ 7.92 (s, 1H), 7.46 (d, J=7.7 Hz, 1H), 7.17 (brd, J=7.3 Hz, 1H), 7.10-7.03 (m, 2H), 6.97-6.93 (m, 1H), 6.85 (s, 2H), 6.79 (brd, J=7.3 Hz, 1H), 6.68 (s, 1H), 5.53-5.50 (m, 1H), 3.93 (q, J=6.9 Hz, 2H), 3.79 (s, 3H), 3.78 (s, 3H), 3.77 (s, 3H), 3.56 (s, 3H), 3.45 (s, 2H), 3.45-3.39 (m, 2H), 3.12-3.08 (m, 2H), 2.97 (brm, 2H), 2.85-2.71 (m, 3H), 2.69 (s, 3H), 2.57 (t, J=13.8 Hz, 2H), 1.67 (brm, 2H), 1.56-1.36 (m, 7H), 1.27 (t, J=6.9 Hz, 3H), 0.87 (d, J=6.1 Hz, 3H), 0.85 (d, J=6.1 Hz, 3H).
EXAMPLE 6
Preparation of a Acetylcysteine Salt of the Thaliporphine Derivative by Thaliporphine Free Base and Acetylcysteine Free Acid
[0185] Thaliporphine free base (0.1353 g, 0.396 mmol) and Acetylcysteine free acid (0.0647 g, 0.396 mmol) were thoroughly mixed and then added to 5 mL of methanol. The resultant mixture was then stirred until the mixture was dissolved. The Acetylcysteine salt of Thaliporphine was obtained as removing the methanol by reduced-pressure or vacuum concentration, or drying under nitrogen until the sample was completely dried.
[Thaliporphine]
[0000]
IR(KBr)v max : 3272, 1602, 1517, 1465, 1255, 1112, 1083 cm −1
Molecular Weight: 341
[Acetylcysteine]
[0000]
IR(KBr)v max : 3374, 2547, 1718, 1534 cm −1
Molecular Weight: 163
[Acetylcysteine Salt of Thaliporphine]
[0000]
IR(KBr)v max : 3381, 2938, 2558, 1605, 1480, 1254, 1105 cm −1
Molecular Weight: 504
ESI-MS (30V): m/z (%) 505 [M+H] + , 342 (100)
[0193] 1 H NMR (CD 3 OD, 500 MHz):δ 8.14 (s, 1H), 6.91 (s, 1H), 6.71 (s, 1H), 4.43 (brs, 1H), 4.00-3.98 (m, 1H), 3.89 (s, 3H), 3.85 (s, 3H), 3.83 (s, 3H), 3.50-3.48 (m, 3H), 3.18-3.15 (m, 2H), 2.91 (brs, 3H), 2.85-2.82 (m, 1H), 2.79-2.76 (m, 2H), 1.99 (s, 3H).
EXAMPLE 7
Preparation of a Chromocarb Salt of the Thaliporphine by Thaliporphine Free Base and Chromocarb Free Acid
[0194] Thaliporphine free base (0.1285 g, 0.376 mmol) and Chromocarb free acid (0.0715 g, 0.376 mmol) were thoroughly mixed and then added to 2 mL of methanol. The resultant mixture was then stirred until the mixture was dissolved. The Chromocarb salt of Thaliporphine was obtained as removing the methanol by reduced-pressure or vacuum concentration, or drying under nitrogen until the sample was completely dried.
[Thaliporphine]
[0000]
IR(KBr)v max : 3272, 1602, 1517, 1465, 1255, 1112, 1083 cm −1
Molecular Weight: 341
[Chromocarb]
[0000]
IR(KBr)v max : 3080, 1737, 1631, 1239 cm −1
Molecular Weight: 190
[Chromocarb Salt of Thaliporphine]
[0000]
IR(KBr)v max : 3402, 1632, 1613, 1518, 1465, 1254, 1105 cm −1
Molecular Weight: 531
ESI-MS (30V): m/z (%) 532 [M+H] + , 342 (100)
[0202] 1 H NMR (CD 3 OD, 500 MHz):δ 8.09 (s, 1H), 8.07-8.05 (m, 1H), 7.77-7.73 (m, 1H), 7.62-7.61 (m, 1H), 7.44-7.42 (m, 1H), 6.90 (s, 1H), 6.89 (s, 1H), 6.68 (s, 1H), 4.19-4.17 (m, 1H), 3.87 (s, 3H), 3.84 (s, 3H), 3.82 (s, 3H), 3.76-3.26 (m, 4H), 3.12 (s, 3H), 2.98-2.81 (m, 2H).
EXAMPLE 8
Preparation of a Atorvastatin Salt of the Compound 1 by Compound 1 Free Base and Atorvastatin Free Acid
[0203] Compound 1 free base (0.05 g, 0.099 mmol) and Atorvastatin free acid (0.055 g, 0.099 mmol) were thoroughly mixed and then added to 5 mL of methanol. The resultant mixture was then stirred until the mixture was dissolved. The Atorvastatin salt of Compound 1 was obtained as removing the methanol by reduced-pressure or vacuum concentration, or drying under nitrogen until the sample was completely dried.
[Compound 1]
[0000]
IR(KBr)v max : 3500, 2931, 1605, 1506, 1464, 1253, 1112 cm −1
[0205] Molecular Weight: 507
[Atorvastatin]
[0000]
IR(KBr)v max : 3380, 1717, 1640, 1508 cm −1
Molecular Weight: 558
[Atorvastatin Salt of Compound 1]
[0000]
IR(KBr)v max : 3402, 2936, 1655, 1595, 1508, 1438, 1254, 1106 cm −1
Molecular Weight: 1065
ESI-MS (30V): m/z (%) 1066 [M+H] + , 279 (100)
[0211] 1 H NMR (CD 3 OD, 400 MHz):δ 8.04 and 8.03 (s, 1H), 7.21-7.10 (m, 4H), 7.05-6.88 (m, 14H), 6.75 and 6.73 (s, 1H), 6.59 and 6.57 (s, 1H), 4.24-4.22 (m, 1H), 4.00-3.72 (m, 7H), 3.80 (s, 3H), 3.74 (s, 9H), 3.29-2.50 (m, 8H), 2.24-2.20 (m, 2H), 1.62-1.42 (m, 4H), 1.38 (d, J=7.1 Hz, 6H).
EXAMPLE 9
Preparation of a Bezafibrate Salt of the Compound 1 by Compound 1 Free Base and Bezafibrate Free Acid
[0212] Compound 1 free base (0.04 g, 0.079 mmol) and Bezafibrate free acid (0.028 g, 0.079 mmol) were thoroughly mixed and then added to 5 mL of methanol. The resultant mixture was then stirred until the mixture was dissolved. The Bezafibrate salt of Compound 1 was obtained as removing the methanol by reduced-pressure or vacuum concentration, or drying under nitrogen until the sample was completely dried.
[Compound 1]
[0000]
IR(KBr)v max : 3500, 2931, 1605, 1506, 1464, 1253, 1112 cm −1
Molecular Weight: 507
[Bezafibrate]
[0000]
IR(KBr)v max : 3358, 2886, 1718, 1610, 1549, 1147 cm −1
Molecular Weight: 361
[Bezafibrate Salt of Compound 1]
[0000]
IR(KBr)v max : 3418, 2938, 1640, 1596, 1508, 1465, 1258, 1106 cm −1
Molecular Weight: 868
ESI-MS (30V): m/z (%) 869 [M+H] + , 508 (100)
[0220] 1 H NMR (CD 3 OD, 400 MHz):δ 8.03 (s, 1H), 7.61 (d, J=6.7 Hz, 2H), 7.31 (d, J=6.7 Hz, 2H), 6.95-6.70 (m, 9H), 6.60 and 6.58 (s, 1H), 4.34-4.30 (m, 1H), 4.03-3.93 (m, 3H), 3.79-3.65 (m, 12H), 3.41-2.65 (m, 12H), 1.39 (s, 6H).
TEST EXAMPLE 1
Evaluation of Antioxidizing Activity in Free Radical Scavenging of 1,1-diphenyl-2-picryl-hydrazyl (DPPH)
[0221] An ethanolic solution of the stable nitrogen centered free radical 1,1-Diphenyl-2-picrylhydrazyl (DPPH, 100 μM) was incubated with the test compounds (10 −8 -10 −4 M or 1-100 μM) in 94-well plates, and then mixed thoroughly in a light-proof environment at room temperature. After 30 min, the absorbance (O.D.) was monitored spectrophotometrically at 517 nm. The activity in inhibiting free radical DPPH results in the decrease of absorbance.
[0222] FIG. 1 shows that the test compounds 1-2 exhibit activity in free radical scavenging of DPPH at a concentration larger than about 10 −5 M. Accordingly, it can be confirmed that the compounds 1-2 and the salts thereof exhibit the activity in inhibiting free radical DPPH.
[0223] FIG. 2 shows that the atorvastatin salt of thaliporphine exhibits more efficient activity in free radical scavenging of DPPH, in comparison with atorvastatin alone and thaliporphine alone.
[0224] FIG. 3 shows that the telmisartan salt of thaliporphine exhibits more efficient activity in free radical scavenging of DPPH, in comparison with telmisartan alone and thaliporphine alone.
[0225] FIG. 4 shows that the captopril salt of thaliporphine exhibits more efficient activity in free radical scavenging of DPPH, in comparison with captopril alone and thaliporphine alone.
[0226] FIG. 5 shows that the bezafibrate salt of thaliporphine exhibits more efficient activity in free radical scavenging of DPPH, in comparison with bezafibrate alone and thaliporphine alone.
[0227] FIG. 6 shows that the nateglinide salt of thaliporphine exhibits more efficient activity in free radical scavenging of DPPH, in comparison with nateglinide alone.
[0228] FIG. 7 shows that the acetylcysteine salt of thaliporphine exhibits more efficient activity in free radical scavenging of DPPH, in comparison with acetylcysteine alone and thaliporphine alone.
[0229] FIG. 8 shows that the salsalate salt of thaliporphine exhibits more efficient activity in free radical scavenging of DPPH, in comparison with salsalate alone and thaliporphine alone.
[0230] Thereby, it can be confirmed that these novel salts of aporphine derivatives exhibit more efficient activity in comparison with carboxyl group-containing agent alone and aporphine derivative alone.
TEST EXAMPLE 2
Evaluation of Protecting Activity from Peroxy Radical-Induced Damage
[Method A]
[0231] In order to evaluate the effect of test compounds in scavenging hydrophilic peroxy radical, the experiment was executed with reference to the method described by Tsuchiya et al. (Methods Enzymol 1992, 213: 460-472). In the experiment, peroxides will react with fluorescent substances and thus inflect observed fluorescence intensity. Thereby, the effect of test compounds in free radical scavenging can be evaluated by measuring the variation of the fluorescence intensity after the addition of test compounds.
[0232] First, to a silicate tube was added a phosphate solution (2 ml, pH 7.4), followed by the addition of β-phycoerythrin (5 nM) to increase relative fluorescence intensity. After 5 minutes, 2,2′-azobis (2-amidinopropane)dihydrochloride (25 mM, AAPH) was added therein. Subsequently, through a fluorescent spectrometry (Shimadzu RF-5301PC, Japan), the fluorescence intensity of β-phycoerythrin was measured by excitation at 540 nm and emission at 570 nm. Then, the test compounds (5×10 −6 M) was further added therein to observe the variation of the fluorescence intensity, in which 0.1% DMSO was taken as a control group.
[0233] FIG. 9 shows that the test compounds 1-2 can protect β-phycoerythin from peroxy radical AAPH—induced damage, and thus delay β-phycoerythin fluorescence degradation. Thereby, it can be confirmed that the test compounds 1-2 and the salts thereof exhibit activity in free radical scavenging of APPH.
[Method B]
[0234] In order to evaluate the oxygen radical absorbing capacity of test compounds. The automated assay was carried out as described in a previous report by Gillespie and co-workers (Gillespie et al., 2007). The experiment was conducted at 37° C. under pH 7.4 condition with a blank sample in parallel. Briefly, 2,2′-azobis (2-amidinopropane) dihydrochloride (AAPH) was used as a peroxyl generator. The final reaction mixture for each black microplat in a 96-well microplate assay contained 0.06 μM fluorescenin, 18.75 mM AAPH and appropriate test substance (1 μM) in 75 mM phosphate buffer. Test substance was directly dissolved in DMSO and diluted with 75 mM potassium phosphate buffer (pH 7.4) for analysis. The analyzer was programmed to record the fluorescence of fluorescenin every minute after the addition of AAPH. All fluorescent measurements are expressed relative to the initial reading (excitation at 485 nm and emission at 530 nm) on a FLUOstar Galaxy plate reader (Roche Diagnostic System Inc., Branchburg, N.J.). Raw data were exported from the Fluostar Galaxy software to an Excel (Microsoft, Roselle, Ill.) sheet for further calculations. All the reaction mixtures were prepared in duplicate, and at least three independent assays were performed for each sample. (Gillespie, K M et al., Nature Protocols 2007; 2: 867-870.)
[0235] FIG. 10 shows that the atorvastatin salt of thaliporphine exhibits more efficient activity in free radical scavenging of APPH, in comparison with atorvastatin alone and thaliporphine alone.
[0236] FIG. 11 shows that the captopril salt of thaliporphine exhibits more efficient activity in free radical scavenging of APPH, in comparison with captopril alone and thaliporphine alone.
[0237] FIG. 12 shows that the bezafibrate salt of thaliporphine exhibits more efficient activity in free radical scavenging of APPH, in comparison with bezafibrate alone and thaliporphine alone.
[0238] FIG. 13 shows that the nateglinide salt of thaliporphine exhibits more efficient activity in free radical scavenging of APPH, in comparison with nateglinide alone and thaliporphine alone.
[0239] FIG. 14 shows that the acetylcysteine salt of thaliporphine exhibits more efficient activity in free radical scavenging of APPH, in comparison with acetylcysteine alone and thaliporphine alone.
[0240] FIG. 15 shows that the salsalate salt of thaliporphine exhibits more efficient activity in free radical scavenging of APPH, in comparison with salsalate alone and thaliporphine alone.
[0241] FIG. 16 shows that the ozagrel salt of glaucine exhibits more efficient activity in free radical scavenging of APPH, in comparison with ozagrel alone and glaucine alone.
[0242] Thereby, it can be confirmed that these novel salts of aporphine derivatives exhibit more efficient activity in comparison with carboxyl group-containing agent alone and aporphine derivative alone.
TEST EXAMPLE 3
Evaluation of Activity in Inhibiting Lipid Peroxidase
[0243] The assay was executed with reference to the method described in Biochem Biophys Res Commun. Mar. 28, 1986; 135(3): 1015-21. The assay conditions are shown as follows, and the results are shown in Table 1.
Assay Conditions:
[0000]
(a) Source: Dunkin Hartley Guinea pig liver microsomes
(b) Substrate: Polyunsaturated fatty acid
(c) Vehicle: 1% DMSO
(d) Pre-Incubation Time/Temp: 15 minutes/37° C.
(e) Incubation Time/Temp: 20 minutes/37° C.
(f) Incubation Buffer: 0.25 M Potassium Phosphate, pH 7.4, 0.1 mM EDTA
(g) Quantitation Method: Spectrophotometric quantitation of Malondialdehyde
[0000]
TABLE 1
Compound No.
Species
Concentration
Inhibition (%)
1
guinea pig
10 μM
64
2
guinea pig
10 μM
70
[0251] In view of the experimental results shown in Table 1, it can be confirmed that the test compounds 1-2 and the slats thereof exhibit activity in inhibiting lipid peroxidase.
TEST EXAMPLE 4
Evaluation of Protecting Activity in Vascular Smooth Muscle Cells
Procedure
[0252] The vascular smooth muscle cells of rats (2×10 4 cells/mL×1 mL) were quantitatively seeded in 24-well plates, and cultured in Dulbecco's modified Eagle medium (DMEM) with 10% fetal bovine serum (FBS) for 24 hours to achieve cell adhesion. After cell adhesion, the DMEM medium with 10% fetal bovine serum was replaced with a fresh DMEM medium with 0.1% fetal bovine serum to perform cell culture for 48 hours.
[0253] Next, the test compounds were added in the cultures (final concentration: 0.1, 1, 10 μM). After 30 minutes, H 2 O 2 (200 μM) was added therein to perform reaction for 24 hours in an incubator. Subsequently, in a light-proof environment, MTT (100 μL) was added into each well to perform reaction at 37° C. for 3 hours. The supernatant liquor was removed and then isopropanol (500 μL) was added, followed by shaking for 10 minutes. After standing for 10 minutes, supernatant liquor (200 μL) was transferred into 96-well plates. Finally, the absorbance values (O.D.) were monitored at 540 nm (OD540) and 630 nm (OD630). Based on the measured absorbance values (OD540-OD630), the effect of these test compounds on cell growth can be evaluated, as shown in FIG. 3 .
Experimental Results
[0254] After H 2 O 2 of various concentration and vascular smooth muscle cells of rats were maintained in the incubator to perform reaction for 24 hours at 37° C., concentration-dependent cytotoxicity by H 2 O 2 was observed, in which H 2 O 2 of a concentration larger than 100 μM resulted in cell death.
[0255] After these test compounds of various concentration (Compounds 1 and 2) reacted with vascular smooth muscle cells of rats for 30 minutes followed by adding H 2 O 2 (200 μM) to perform reaction for 24 hours, it can be found that H 2 O 2 (200 μM) significantly caused the decrease of cell number (#P<0.05), the test compound 2 (10 μM) can slightly inhibit H 2 O 2 to damage vascular smooth muscle cells and the test compound 1 (10 μM) can significantly inhibit H 2 O 2 to damage vascular smooth muscle cells and thereby increase cells survival rate (**P<0.01), as shown in FIG. 17 .
[0256] In view of the results of Test Examples 1-4, it can be confirmed that the pharmaceutically acceptable salts provided by the present invention are effective in inhibiting lipid peroxidase, exerting the free radical scavenging activities and protecting blood vessel smooth muscle cells and thus can reduce the oxidative stress.
[0257] Although the present invention has been explained in relation to its preferred embodiment, it is to be understood that many other possible modifications and variations can be made without departing from the scope of the invention as hereinafter claimed.
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The present invention discloses novel pharmaceutically acceptable salts of aporphine compounds and carboxyl-group containing agents. Also, the present invention discloses methods for preparing the pharmaceutically acceptable salts. These pharmaceutically acceptable salts are suitable for use in treating and/or preventing hyperglycemic disease and/or several oxidative stress related diseases.
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This application is the national phase filing of International application PCT/EP96/03605, filed Aug. 14, 1996, which designated the U.S. and claims priority based on GB 95307332.7, filed in Great Britain on Oct. 16, 1995.
The invention relates to new bispecific or bivalent antibody fragment analogues, a process for preparing such antibody fragment analogues and various uses of such antibody fragment analogues.
BACKGROUND OF THE INVENTION AND PRIOR ART
1. Antibody Structure
Antibody molecules typically are Y-shaped molecules whose basic unit consist of four polypeptides, two identical heavy chains and two identical light chains, which are covalently linked together by disulfide bonds. Each of these chains is folded in discrete domains. The C-terminal regions of both heavy and light chains are conserved in sequence and are called the constant regions, also known as C-domains. The N-terminal regions, also known as V-domains, are variable in sequence and are responsible for the antibody specificity. The antibody specifically recognizes and binds to an antigen mainly through six short complementarity-determining regions located in their V-domains (see FIG. 1).
In this specification abbreviations are used having the following meaning.
C-domain: Constant domain
V-domain: Variable domain
V.sub. : Variable domain of the light chain
V H : Variable domain of the heavy chain
Fv: dual chain antibody fragment containing both a V H and a V L
scFv: single-chain Fv (V H and V L genetically linked either directly or via a peptide linker)
CDR: Complementarity-determining region
ELISA: Enzyme Linked Immuno Sorbent Assay
PCR: Polymerase Chain Reaction
IPTG: IsoPropyl-β-ThioGalactopyranoside
PBS: Phosphate Buffered Saline
PBST: Phosphate Buffered Saline with 0.15% Tween
TMB: 3,3',5,5'-TetraMethylBenzidine
It is generally known that proteolytic digestion of an antibody with papain yields three fragments. The fragment containing the CH 2 and CH 3 domains of the two heavy chains connected by the complete hinge (see FIG. 1) crystallises very easily and was therefore called Fc fragment. The two other fragments are identical and were called Fab fragments, as they contained the antigen-binding site. Digestion with pepsin is such that the two Fab's remain connected via the hinge, forming only two fragments: Fc' and Fab 2 .
The Fv is the smallest unit of an antibody which still contains the complete binding site (see FIG. 1) and full antigen binding activity. It consists of only the V-domains of the heavy and light chains thus forming a small, heterodimeric variable fragment or Fv. Fv's have a molecular weight of about 25 kD, which is only one sixth of the parent whole antibody (in the case of an IgG). Previously Fv's were only available by proteolysis in a select number of cases (Givol, 1991). The production of Fv's can now be achieved more routinely using genetic engineering methods through cloning and expressing DNA encoding only the V-domains of the antibody of interest. Smaller fragments, such as individual V-domains (Domain Antibodies or dABs, Ward et al., 1989), and even individual CDR's (Williams et al., 1989; Taub et al., 1989) were shown to retain the binding characteristics of the parent antibody. However, this is not achievable on a routine basis: most naturally occurring antibodies need both a V H and a V L to retain full immunoreactivity. For example, in the case of V H D1.3 (Ward et al., 1989), although it still binds hen egg lysozyme (HEL) with an affinity close to that of the parent antibody, it was shown that loss of specificity was observed in that it can no longer distinguish turkey lysozyme from HEL, whereas the Fv can (Berry and Davies, 1992). Although murine dABs can be obtained more routinely from spleen libraries (Ward et al., 1989), the approach is unsustainable because of the many problems associated with their production and physical behaviour: expression is extremely poor, affinity tends to be low, stability and solubility in water is low, and non-specific binding is usually very high. According to the literature a possible explanation of these undesirable characteristics is the exposure of the hydrophobic residues which are normally buried in the V H -V L interface. The exposed hydrophobic patches are thought to contribute to aggregation of the protein inside the cells and/or in the culture medium, leading to poor expression and/or poor solubility (Anthony et al., 1992; Ward et al., 1989). The hydrophobic patches can also explain the high non-specific binding described by Berry and Davies, 1992. These problems clearly limit the usefulness of these molecules. Most of the Camelid antibodies appear to be an exception to this rule in that they only need one V-domain, namely V H , to specifically and effectively bind an antigen (Hamers-Castermans et al., 1993). In addition, preliminary data indicate that they seem not to suffer from the disadvantages of mouse dABs, as these camelid antibodies or fragments thereof are soluble and have been shown to express well in yeast and Aspergillus moulds. These observations can have important consequences for the production and exploitation of antibody-based products, see patent application WO 94/25591 (UNILEVER et al., first priority date Apr. 29, 1993).
2. Production of Antibody Fragments
Several microbial expression systems have already been developed for producing active antibody fragments, e.g. the production of Fab in various hosts, such as E. coli (Better et al., 1988, Skerra and Pluckthun, 1988, Carter et al., 1992), yeast (Horwitz et al., 1988), and the filamentous fungus Trichoderma reesei (Nyyssonen et al., 1993) has been described. The recombinant protein yields in these alternative systems can be relatively high (1-2 g/l for Fab secreted to the periplasmic space of E. coli in high cell density fermentation, see Carter et al., 1992), or at a lower level, e.g. about 0.1 mg/l for Fab in yeast in fermenters (Horwitz et al., 1988), and 150 mg/l for a fusion protein CBHI-Fab and 1 mg/l for Fab in Trichoderma in fermenters (Nyyssonen et al., 1993) and such production is very cheap compared to whole antibody production in mammalian cells (hybridoma, myeloma, CHO). Although the latter can give yields of the order of 1 g/l in high cell density fermentation, it is a time-consuming and very expensive manufacturing method resulting in a cost price of about 1000 .English Pound./gram of antibody. It was further demonstrated that plants can be used as hosts for the production of both whole antibodies (Hiatt et al., 1989) and scFv's (Owen et al., 1992, Firek et al., 1993), whereby yields of up to 0.5% of the total soluble protein content in tobacco leaves were mentioned.
The fragments can be produced as Fab's or as Fv's, but additionally it has been shown that a V H and a V L can be genetically linked in either order by a flexible polypeptide linker, which combination is known as an scFv (Bird et al. (1988), Huston et al. (1988), and granted patent EP-B-0281604 (GENEX/ENZON LABS INC.; first priority date Sep. 2, 1986).
3. Bivalent and Bispecific Antibodies and Antibody Fragments
The antibody fragments Fab, Fv and scFv differ from whole antibodies in that the antibody fragments carry only a single antigen-binding site. Recombinant fragments with two binding sites have been made in several ways, for example, by chemical cross-linking of cysteine residues introduced at the C-terminus of the V H of an Fv (Cumber et al., 1992), or at the C-terminus of the V L of an scFv (Pack and Pluckthun, 1992), or through the hinge cysteine residues of Fab's (Carter et al., 1992). Another approach to produce bivalent antibody fragments is described by Kostelny et al. (1992) and Pack and Pluckthun (1992) and is based on the inclusion of a C-terminal peptide that promotes dimerization.
When two different specificities are desired, one can generate bispecific antibody fragments. The traditional approach to generate bispecific whole antibodies was to fuse two hybridoma cell lines each producing an antibody having the desired specificity. Because of the random association of immunoglobulin heavy and light chains, these hybrid hybridomas produce a mixture of up to 10 different heavy and light chain combinations, only one of which is the bispecific antibody (Milstein and Cuello, 1983). Therefore, these bispecific antibodies have to be purified with cumbersome procedures, which considerably decrease the yield of the desired product.
Alternative approaches include in-vitro linking of two antigen specificities by chemical cross-linking of cysteine residues either in the hinge or via a genetically introduced C-terminal Cys as described above. An improvement of such in vitro assembly was achieved by using recombinant fusions of Fab's with peptides that promote formation of heterodimers (Kostelny et al., 1992). However, the yield of bispecific product in these methods is far less than 100%.
A more efficient approach to produce bivalent or bispecific antibody fragments, not involving in vitro chemical assembly steps, was described by Holliger et al. (1993). This approach takes advantage of the observation that scFv's secreted from bacteria are often present as both monomers and dimers. This observation suggested that the V H and V L of different chains can pair, thus forming dimers and larger complexes. The dimeric antibody fragments, also named "diabodies" by Hollinger et al., in fact are small bivalent antibody fragments that assembled in vivo. By linking the V H and V L of two different antibodies 1 and 2, to form "cross-over" chains V H 1V L 2 and V H 2-V L 1 (see FIG. 2B), the dimerisation process was shown to reassemble both antigen-binding sites. The affinity of the two binding sites was shown to be equal to the starting scFv's, or even to be 10-fold increased when the polypeptide linker covalently linking V H and V L was removed, thus generating two proteins each consisting of a V H directly and covalently linked to a V L not pairing with the V H (see FIG. 2C). This strategy of producing bispecific antibody fragments was also described in several patent applications. Patent application WO 94/09131 (SCOTGEN LTD; priority date Oct. 15, 1992) relates to a bispecific binding protein in which the binding domains are derived from both a V H and a V L region either present at two chains or linked in an scFv, whereas other fused antibody domains, e.g. C-terminal constant domains, are used to stabilise the dimeric constructs. Patent application WO 94/13804 (CAMBRIDGE ANTIBODY TECHNOLOGY/MEDICAL RESEARCH COUNCIL; first priority date Dec. 4, 1992) relates to a polypeptide containing a V H and a V L which are incapable of associating with each other, whereby the V-domains can be connected with or without a linker.
Mallender and Voss, 1994 (also described in patent application WO 94/13806; DOW CHEMICAL CO; priority date Dec. 11, 1992) reported the in vivo production of a single-chain bispecific antibody fragment in E. coli. The bispecificity of the bivalent protein was based on two previously produced monovalent scFv molecules possessing distinct specificities, being linked together at the genetic level by a flexible polypeptide linker. The thus formed V H 1-linker-V L 1-linker-V H 2-linker-V L 2 fragment (see FIG. 2A) was shown to contain both antigen binding specificities 1 and 2. (1=anti-fluorescein, 2=anti-single-stranded DNA). Traditionally, whenever single-chain antibody fragments are referred to, a single molecule consisting of one heavy chain linked to one (corresponding) light chain in the presence or absence of a polypeptide linker is implicated. When making bivalent or bispecific antibody fragments through the `diabody` approach (Holliger et al., (1993) and patent application WO 94/09131) or by the `double scFv` approach (Mallender and Voss, 1994 and patent application WO 94/13806), again the V H is linked to a (the corresponding) V L .
It is realised that claims 32 and 33 of patent application WO 93/11161 (ENZON INC.; priority date Nov. 25, 1991) and the corresponding passages in that specification on page 22, lines 1-10 may read on a polypeptide comprising two V L 's fused together via a flexible polypeptide linker, and on a polypeptide comprising two V H 's fused together via a flexible polypeptide linker, respectively. However, no examples were given to substantiate this approach, thus it was in fact a hypothetical possibility instead of an actually produced compound.
A skilled person would not have expected that such approach would be viable for at least three reasons. Firstly, it is widely recognised that immunoglobulin heavy chains (excluding the above described camel immunoglobulins) have very limited solubility and spontaneously precipitate out of aqueous solution when isolated from their light chain partners. Secondly, several groups have shown (Ward et al., 1989, Berry and Davies, 1992, and Anthony et al., 1992) that expression of V H 's in the absence of V L 's is hampered by extremely poor yields of unstable product with many undesirable properties, e.g. non-specific binding. Thirdly in patent application WO 94/13804 it was described on page 31 lines 10-12, that in computer modelling experiments they could not model as heterodimers V H --V H and V L --V L given the constraints of short linkers.
Thus the simple suggestion given in patent application WO 93/11161 is not an enabling disclosure leading a skilled person to try with a reasonable expectation of success whether such suggestion would work; therefore, that patent application should not be considered as relevant prior art for the present invention.
SUMMARY OF THE INVENTION
The present invention provides a bispecific or bivalent antibody fragment analogue, which comprises a binding complex containing two polypeptide chains, one of which comprises two times a variable domain of a heavy chain (V H ) in series and the other comprises two times a variable domain of a light chain (V L ) in series.
In one aspect of the invention one chain of the antibody fragment analogue comprises a first V H (V H -A) connected to a second V H (V H -B) and the other chain comprises a first V L (V L -A) connected to a second V L (V L -B). In a preferred embodiment of this aspect one chain comprises a first V H (V H -A) followed by a second V H (V H -B), thus [V H -A * V H -B], and the other chain comprises a first V L (V L -A) preceded by a second V L (V L -B), thus [V L -B * V L -A]. For some embodiments of this aspect the two V H 's are directly connected to each other, but for other embodiments of this aspect of the invention the two V L 's are directly connected to each other. According to another embodiment of this aspect of the invention the two V H 's are connected to each other by a linker and also the two V L 's are connected to each other by a linker. Such a linker usually comprises at least one amino acid residue.
According to a special embodiment of this aspect of the invention one chain comprises a first V H (V H -A) followed by a second V H (V H -B), thus [V H -A * V H -B], and the other chain comprises a first V L (V L -A) followed by a second V L (V L -B), thus [V L -A * V L -B], and in which the two V H 's are connected to each other by a linker and also the two V L 's are connected to each other by a linker, whereas each linker comprises at least 10 amino acid residues.
According to the above aspect of the invention with A being different from B there are provided bispecific antibody fragment analogues.
According to another aspect of the invention the specificities A and B are the same resulting in a bivalent antibody fragment.
According to a further aspect of the invention the bispecific or bivalent antibody fragment analogues can be used in a diagnostic technique or for immunoassays, in a purification method, for therapy, or in other methods in which immunoglobulins or fragments thereof are used. Such uses are well-known in the art.
The invention also provides a process for producing the antibody fragments of the invention in that a host is transformed by incorporating into that host a DNA encoding the two V H 's with or without a connecting linker and a DNA encoding the two V L 's with or without a connecting linker. Preferably the two DNA's are placed in a dicistronic arrangement.
It is also possible that the two linked V H 's and the two linked V L 's are produced separately by different hosts, after which the linked V H 's produced by one host can be combined with the linked V L 's produced by the other host. The hosts can be selected from the group consisting of prokaryotic bacteria of which examples are Gram-negative bacteria, e.g. E. coli, and Gram-positive bacteria, e.g. B. subtilis or lactic acid bacteria, lower eukaryotes examples of which are yeasts, e.g. belonging to the genera Saccharomyces, Kluyveromyces, or Trichoderma, moulds, e.g. belonging to the genera Aspergillus and Neurospora, and higher eukaryotes, examples of which are plants, e.g. tobacco, and animal cells, examples of which are myeloma cells and CHO cells. The techniques to transform a host by genetic engineering methods in order to have a desirable polypeptide produced by such host are well-known to persons skilled in the art as is evident from the literature mentioned above under the heading "Background of the invention and prior art".
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 depicts in schematic form the structure of a typical antibody (immunoglobulin) molecule.
FIG. 2 shows a schematic representation of published arrangements of heavy and light chain V-domain gene fragments that have been proven to produce bispecific antibody fragments.
FIG. 3 shows in diagrammatic form the suggested arrangement of the V-domains of a double head antibody fragment according to the invention with the V-domains in the following order: V H A-V H B+V L B-V L A.
FIG. 4 shows the nucleotide sequence of the EcoRI-HindIII insert of pUR.4124 containing DNA (see SEQ ID NO: 1) encoding V L Lys-Linker-V H Lys (see SEQ ID NO: 2).
FIG. 5 shows the nucleotide sequence of the HindIII-EcoRI insert of plasmid Fv.3418 (see SEQ ID NO: 3) containing DNA encoding pelB leader-V H 3418 (see SEQ ID NO: 4) and DNA encoding pelB leader-V L 3418 (see SEQ ID NO: 5).
FIG. 6 shows the nucleotide sequence of the HindIII-EcoRI insert of plasmid Fv.4715-myc (see SEQ ID NO: 6) containing DNA encoding pelB leader-V H 4715 (see SEQ ID NO: 7) and DNA encoding pelB leader-V L 4715-Myc tag (see SEQ ID NO: 8).
FIG. 7 shows the nucleotide sequence of the HindIII-EcoRI insert of scFv.4715-myc containing DNA (see SEQ ID NO: 9) encoding pelB leader-V H 4715-Linker-V L 4715-Myc tag (see SEQ ID NO: 10).
FIGS. 8A and 8B show the nucleotide sequence of the HindIII-EcoRI insert of pGOSA.E (see SEQ ID NO: 11) containing DNA encoding pelB leader-V H 4715-Linker-V L 3418 (see SEQ ID NO: 12) and DNA encoding pelB leader-V L 3418-Linker-V H 4715 (see SEQ ID NO: 13).
FIG. 9 gives an overview of the oligonucleotides and their positions in pGOSA.E that can be used to replace V-domain gene fragments.
FIG. 10 illustrates the amino acid sequence of the V H--V H and V L --V L domain junctions in fusion polypeptides GOSA.E (see amino acids 114-145 in SEQ ID NO: 12 and amino acids 102-128 in SEQ ID NO: 13), GOSA.V (see SEQ ID NO: 30 and amino acids 102-128 in SEQ ID NO: 13), GOSA.S (see amino acids 114-145 in SEQ ID NO: 12 and SEQ ID NO: 31) and GOSA.T (see SEQ ID NO: 30 and SEQ ID NO: 31).
FIG. 11 shows the specificity of Streptococcus binding of scFv.4715-myc.
FIG. 12 shows the specificity of glucose oxidase targeting onto the surface of various Streptococcus strains by GOSA.E.
FIG. 13 shows the specificity of glucose oxidase targeting onto the surface of various Streptococcus strains by GOSA.V.
FIG. 14 shows the specificity of glucose oxidase targeting onto the surface of various Streptococcus strains by GOSA.S.
FIG. 15 shows the specificity of glucose oxidase targeting onto the surface of various Streptococcus strains by GOSA.T.
FIG. 16 shows the results of an ELISA. Individual fractions of a gelfiltration experiment using partially purified GOSA.E as feedstock were tested for glucose oxidase and Streptococcus sanguis bispecific binding activity.
FIG. 17 shows the results of an ELISA. Individual fractions of a gelfiltration experiment using partially purified GOSA.V as feedstock were tested for glucose oxidase and Streptococcus sanguis bispecific binding activity.
FIG. 18 shows the results of an ELISA. Individual fractions of a gelfiltration experiment using partially purified GOSA.T as feedstock were tested for glucose oxidase and Streptococcus sanguis bispecific binding activity.
FIG. 19 shows the source of fragment PCR.I BstEII/SacI.
FIG. 20 shows the source of fragment PCR.II SfiI/EcoRI.
FIG. 21 shows the source of fragment PCR.III NheI/SacI.
FIG. 22 shows the source of fragment PCR.IV XhoI/EcoRI.
FIG. 23 shows the source of fragment PCR.V SalI/EcoRI.
FIG. 24 shows the source of fragment PCR.VI SfiI/NheI.
FIG. 25 shows the source of fragment PCR.VII BstEII/NheI.
FIG. 26 shows the source of fragment PCR.VIII XhoI/EcoRI.
FIG. 27 shows the source of fragment PCR.IX BstEII/NheI.
FIG. 28 shows the source of fragment PCR.X PstI/EcoRI.
FIG. 29 shows the construction of plasmid pGOSA.A.
FIG. 30 shows the construction of plasmid pGOSA.B.
FIG. 31 shows the construction of plasmid PGOSA.C.
FIG. 32 shows the construction of plasmid pGOSA.D.
FIG. 33 shows the construction of plasmid pGOSA.E.
FIG. 34 shows the construction of plasmid pGOSA.V.
FIG. 35 shows the construction of plasmid pGOSA.S.
FIG. 36 shows the construction of plasmid PGOSA.T.
FIGS. 37A and 37B show the construction of plasmid pGOSA.G.
FIG. 38 shows the construction of plasmid pGOSA.J.
FIG. 39 shows the construction of plasmid pGOSA.Z.
FIG. 40 shows the construction of plasmid pGOSA.AA.
FIG. 41 shows the construction of plasmid pGOSA.AB.
FIG. 42 shows the construction of plasmid PGOSA.L.
FIG. 43 shows the construction of plasmid PGOSA.Y.
FIG. 44 shows the construction of plasmid pGOSA.X.
FIG. 45 shows the construction of plasmid pGOSA.AC.
FIG. 46 shows the construction of plasmid pGOSA.AD.
Table 1 shows the nucleotide sequence of the oligonucleotides used to produce the constructs described in this specification. Restriction sites encoded by these primers are underlined.
Table 2 gives an overview of all GOSA constructs described in this specification.
Table 2A describes intermediate constructs that were not further tested.
Table 2B describes the dicistronic constructs.
Table 2C describes the monocistronic constructs.
DETAILED DESCRIPTION OF THE INVENTION
In this specification the construction of an antibody fragment analogue consisting of a two chain protein complex is described, in which one of the chains consists of two heavy chain V-domains and the other chain consists of the two corresponding light chain V-domains in either order. The variable domains are linked either directly or through a polypeptide linker. Subsequent molecular modelling of this combination suggested that the protein chains could fold such that both binding sites are fully accessible, provided that the connecting linkers are kept long enough to span 30 to 35 Å.
Whereas in patent application WO 93/11161 it is explicitly described that for the above described bispecific complexes two flexible polypeptide linkers in the self assembling complex are required, the present invention illustrated here describes in particular the construction of a two chain protein complex containing only one linker or no linkers at all. The latter antibody fragment analogue thus consists of a two chain protein complex containing one polypeptide chain comprising heavy chain V-domains fused directly together and another polypeptide chain comprising the corresponding light chain V-domains fused together, both fusions in the absence of linkers. But also two chain protein complexes in which each chain comprises a linker between the two variable domains can be used as antibody fragment analogues according to the invention as described below with construct pGOSA.E. However, the two chain complexes containing only one linker or no linker at all are preferred. The abbreviation GOSA used in this specification relates to a combination of glucose oxidase and Streptococcus sanguis.
In this specification evidence is provided that these antibody fragment analogues ("double heads") contain both antigen binding specificities of the Fv's used to generate these bispecific antibody fragments. It is exemplified that these type of constructs according to the invention can be used to target the enzyme glucose oxidase to whole bacteria, using antibody fragments derived from hybridomas expressing antibodies directed against these antigens.
The present invention is now described by reference to some specific examples, which are included for purposes of illustration only and are not intended to limit the scope of the invention.
EXAMPLES
General Experimental
Strains, Plasmids and Media
All cloning steps were performed in E. coli JM109 (endA1, recA1, gyrA96, thi, hsdR17(r K , m K + ), relA1, supE44, Δ(lac-proAB), [F', traD36, proAB, lacI q ZΔM15]. E. coli cultures were grown in 2×TY medium (16 g tryptone, 10 g yeast extract, 5 g NaCl per liter H 2 O), where indicated supplemented with 2% glucose and/or 100 μg/ml ampicillin. Transformations were plated out on SOBAG plates (20 g tryptone, 5 g yeast extract, 15 g agar, 0.5 g NaCl per liter H 2 O plus 10 mM MgCl 2 , 2% glucose, 100 μg/ml ampicillin) The expression vectors used are derivatives of pUC19. The oligonucleotide primers used in the PCR reactions were synthesized on an Applied Biosystems 381A DNA Synthesiser by the phosphoramidite method.
Expression of GOSA Constructs
Colonies from freshly transformed JM109 plated onto SOBAG plates were used to inoculate 2×TY medium supplemented with 100 μg/ml ampicillin, 2% glucose. Cultures were shaken at 37° C. to an OD 600 in the range of 0.5 to 1.0. Cells were pelleted by centrifugation and the supernatant was removed. The pelleted cells were resuspended in 2×TY medium with 100 μg/ml ampicillin, 1 mM IPTG, and grown for a further 18 hours at 25° C. Cells were pelleted by centrifugation and the supernatant, containing the secreted chains, used directly in an ELISA. The proteins in the periplasm of the pelleted cells were extracted by resuspending the cell pellet in 1/20 of the original culture volume of lysis buffer (20% sucrose, 200 mM Tris-HCl pH 7.5, 1 mM EDTA, 500 μg/ml lysozyme). After incubation at 25° C. for 20 minutes an equal volume of H 2 O was added and the incubation was continued for another 20 minutes. The suspension was spun at 10.000 g for 15 minutes and the supernatant containing the periplasmic proteins was used directly in an ELISA.
ELISA
96 well ELISA plates (Greiner HC plates) were activated overnight at 37° C. with 200 μl/well of an 1/10 dilution of an over night culture of Streptococcus cells in 0.05 M sodium carbonate buffer at pH=9.5. Following one wash with PBST, the antigen sensitised plates were pre-blocked for 1 hour at 37° C. with 200 μl/well blocking buffer (2% BSA, 0.15% Tween in PBS). Samples containing 50 μl blocking buffer plus 50 μl culture supernatants or periplasmic cell extracts (neat or diluted with PBS) were added to the Streptococcus sensitised plate and incubated for 2 hours at 37° C. Following 4 washes with PBS-T, 100 μl of blocking buffer containing glucose oxidase (50 μg/ml) was added to every well. After incubation at 37° C. for 1 hour unbound glucose oxidase was removed by 4 washes with PBS-T. Bound glucose oxidase was detected by adding 100 μl substrate to each well (70 mM Na-citrate, 320 mM Na-phosphate, 27 mg/ml glucose, 0.5 μg/ml HRP, 100 μg/ml TMB). The colour reaction was stopped after 1 hour by the addition of 35 μl 2 M HCl and the A450 was measured (compare FIGS. 11/15).
Affinity Purification of GOSA Antibody Fragments
GOSA.E, GOSA.V, GOSA.S and GOSA.T were partially purified by affinity chromatography. 100 ml periplasmic extract of each of these constructs was loaded onto a Glucose-oxidase-Sepharose column (CNBr-Sepharose, Pharmacia) prepared according to the manufacturer's instructions. After extensive washes with PBS the bound GOSA antibody fragments were eluted in 0.1M glycine buffer at pH=2.8. The fractions were neutralised with Tris and analysed by polyacrylamide gel electrophoresis followed by silver staining and tested for the presence of double head activity.
EXAMPLE 1
Construction of the pGOSA Double Head Expression Vectors
In this Example the construction of a two chain protein complex is described, in which one of the chains consists of two heavy chain V-domains and the other chain consists of the two corresponding light chain V-domains. The variable domains are linked either directly or through a polypeptide linker. The expression vectors used are derivatives of a pUC19 derived plasmid containing a HindIII-EcoRI fragment that in the case of plasmid scFv.4715-myc contains a DNA fragment encoding one pelB signal sequence fused to the N-terminus of the V H that is directly linked to the corresponding V L of the antibody through a connecting flexible peptide linker, (Gly 4 Ser) 3 (present in SEQ ID NO: 2 as amino acids 109-123 and in SEQ ID NO: 10 as amino acids 121-135), thus generating a single-chain molecule (see FIG. 7).
In the dual-chain Fv and the pGOSA expression vectors, the DNA fragments encoding both the V H and V L of the antibody are preceded by a ribosome binding site and a DNA sequence encoding the pelB signal sequence in an artificial dicistronic operon under the control of a single inducible promoter (see FIGS. 5, 6 and 8A and 8B). Expression of these constructs is driven by the inducible lacZ promoter. The nucleotide sequence of the HindIII-EcoRI inserts of the plasmids pUR.4124, Fv.3418, Fv.4715-myc and scFv.4715-myc constructs used for the generation of the bispecific antibody fragments are given in FIGS. 4-7, respectively. Moreover, a culture of E. coli cells harbouring plasmid scFv.4715-myc and a culture of E. coli cells harbouring plasmid Fv.3418 were deposited under the Budapest Treaty at the National Collection of Type Cultures (Central Public Health Laboratory) in London (United Kingdom) with deposition numbers NCTC 12916 and NCTC 12915, respectively. In agreement with Rule 28 (4) EPC, or a similar arrangement for a State not being a Contracting State of the EPC, it is hereby requested that a sample of such deposit, when requested, will be submitted to an expert only. The construction of PGOSA.E (see FIGS. 8A and 8B for the HindIll-EcoRI insert of pUC19) involved several cloning steps. The appropriate restriction sites in the various domains were introduced by PCR directed mutagenesis using the oligonucleotides listed in Table 1 below. The PGOSA.E derivatives pGOSA.V, pGOSA.S and PGOSA.T with only one or no linker sequence are derived from the pGOSA.E construct by removing the linker sequences by means of PCR directed mutagenesis with oligonucleotides listed in Table 1 below.
TABLE 1__________________________________________________________________________DBL.15'-CAC CAT CTC CAG AGA CAA TGG CAA G-3' (= SEQ ID NO: 14)DBL.25'-GAG CGC GAG CTC GGC CGA ACC GGC C.sup.1 GA TCC GCC (= SEQ ID NO: 15)ACC GCC AGA GCC-3'DBL.35'-CAG GAT CCG GCC GGT TCG GCC.sup.1 CAG GTC CAG CTG (= SEQ ID NO: 16)CAA CAG TCA GGA-3'DBL.45'-CTA CAT GAA TTC.sup.2 GCT AGC.sup.3 TTA TTA TGA GGA GAC (= SEQ ID NO: 17)GGT GAC GGT GGT CCC TTG GC-3'DBL.55'-TAA TAA GCT AGC.sup.3 GGA GCT GCA TGC AAA TTC TAT (= SEQ ID NO: 18)TTC-3'DBL.65'-ACC AAG CTC GAG.sup.4 ATC AAA CGG GG-3' (= SEQ ID NO: 19)DBL.75'-AAT GTC GAA TTC.sup.2 GTC GAC.sup.5 TCC GCC ACC GCC AGA (= SEQ ID NO: 20)GCC-3'DBL.85'-ATT GGA GTC GAC.sup.5 ATC GAA CTC ACT CAG TCT CCA (= SEQ ID NO: 21)TTC TCC-3'DBL.95'-TGA AGT GAA TTC.sup.2 GCG GCC GC.sup.6 T TAT TAC CGT TTG (= SEQ ID NO: 22)ATT TCG AGC TTG GTC CC-3'DBL.105'-CGA ATT CGG TCA CC.sup.8 G TCT CCT CAC AGG TCC AGT (= SEQ ID NO: 23)TGC AAC AG-3'DBL.115'-CGA ATT CTC GAG.sup.4 ATC AAA CGG GAC ATC GAA CTC (= SEQ ID NO: 24)ACT CAG TCT CC-3'DBL.125'-CGA ATT CGG TCA CC.sup.8 G TCT CCT CAC AGG TGC AGT (= SEQ ID NO: 25)TGC AGG AG-3'PCR.515'-AGG T(C/G)(A/C) A(C/A)C TGC AG.sup.7 (C/G) AGT C(A/T)G (= SEQ ID NO: 26)G-3'PCR.895'-TGA GGA GAC GGT GAC C.sup.8 GT GGT CCC TTG GCC CC-3' (= SEQ ID NO: 27)PCR.905'-GAC ATT GAG CTC.sup.9 ACC CAG TCT CCA-3' (= SEQ ID NO: 28)PCR.1165'-GTT AGA TCT CGA G.sup.4 CT TGG TCC C-3' (= SEQ ID NO: 29)__________________________________________________________________________ 1=SfiI, 2=EcoRI, 3=NheI, 4=XhoI, 5=SalI, 6=NotI, 7=PstI, 8=BstEII, 9=SacI
These three constructs lack some of the restriction sites at the new joining points. The V H A-V H B gene fragment without a linker lacks the 5' V H B SfiI site. The V L B-V L A gene fragment without a linker lacks the 5' V L A SalI site. The position of the oligonucleotides in the PGOSA constructs given in Table 1 are shown in FIG. 9. The pGOSA expression vectors and the oligonucleotides in Table 1 have been designed to enable most specificities to be cloned into the pGOSA constructs. FIG. 10 shows the amino acid sequence of the junctions between the V H A-V H B and V L B-V L A fragments encoded by DNA present in pGOSA.E, pGOSA.V, pGOSA.S and pGOSA.T. A more detailed description of the preparation of pGOSA.E, pGOSA.V, PGOSA.S and pGOSA.T is given in Example 5.
EXAMPLE 2
Bifunctional Binding Activity of GOSA Double Heads
In this Example we provide evidence that the above described molecules ("double heads"), i.e. the two chain protein complexes, contain both antigen binding specificities of the Fv's used to generate these multi-functional antibody fragment analogues. FIG. 12-15 show that GOSA.E, GOSA.V, GOSA.S and GOSA.T can be used to specifically target the enzyme glucose oxidase to several Streptococcus sanguis strains using antibody fragments derived from hybridoma's expressing antibodies directed against these antigens.
Comparison of the binding specificity of the GOSA constructs (see FIGS. 12-15) and the binding specificity of the scFv.4715-myc (see FIG. 11) shows that the fine specificity of the anti-Streptococcus sanguis scFv.4715 is preserved in the GOSA "double heads".
EXAMPLE 3
FPLC Analysis of GOSA Double Heads
Partially purified GOSA.E, GOSA.V, GOSA.S and GOSA.T samples (estimated to be 50-80% pure by polyacrylamide gel electrophoresis) were analysed on a Pharmacia FPLC Superose 12 column. The analysis was performed using PBS at a flow rate of 0.3 ml/minute. Eluate was monitored at 280 nm and 0.3 ml fractions were collected and analysed by ELISA. Usually GOSA.E, GOSA.V, GOSA.S and GOSA.T samples only gave one GOSA double head activity peak as determined by ELISA (see FIGS. 16-18). The position of this peak in the elution pattern indicated that the molecular weight of the GOSA double head is 40-50 kD. Since this molecular weight corresponds to the expected molecular weight of the V H 2+V L 2 double head dimer, the conclusion is justified that GOSA.E, GOSA.V, GOSA.S and GOSA.T are primarily produced as dimeric molecules. Occasionally an activity peak with an apparent molecular weight of ≈200 kD was observed (see FIG. 16). The presence of Glucose Oxidase activity in these fractions (data not shown) indicate that these fractions contain GOSA double head complexed with glucose oxidase that was eluted with the GOSA sample from the glucose oxidase-sepharose affinity matrix.
EXAMPLE 4
Production of Other Double Heads
The methods described in the previous Examples were used to produce other double heads, which also appeared to be active against the antigens for which they were developed. These other double heads had the following specificities:
anti-S. sanguis/anti-beta-HCG,
anti-S. sanguis/anti-urease,
anti-S. sanguis/anti-hen-egg-lysozyme,
anti-beta-HCG/anti-hen-egg-lysozyme,
anti-hen-egg-lysozyme/anti-glucose oxidase,
anti-huIgG/anti-glucose oxidase,
anti-urease/anti-glucose oxidase,
anti-lacto-peroxidase/anti-glucose oxidase,
anti-alpha-HCG/anti-glucose oxidase, and
anti-reactive-Red-6/anti-glucose oxidase.
EXAMPLE 5
Detailed Description of the Preparation of Intermediate Constructs pGOSA.A, pGOSA.B pGOSA.C and pGOSA.D and Their Use for the Preparation of Plasmid pGOSA.E and Its Derivatives PGOSA.V, PGOSA.S and PGOSA.T
Oligonucleotides and PCR
The primary structures of the oligonucleotide primers used in the construction of the bispecific `pGOSA` constructs are shown in Table 1 above. Reaction mixture used for amplification of DNA fragments were 10 mM Tris-HCl, pH 8.3, 2.5 mM MgCl 2 , 50 mM KCl, 0.01% gelatin (w/v), 0.1% Triton X-100, 400 mM of each dNTP, 5.0 units of Vent DNA polymerase (New England Biolabs), 100 ng of template DNA, and 500 ng of each primer (for 100 μl reactions). Reaction conditions were: 94° C. for 4 minutes, followed by 33 cycles of each 1 minute at 94° C., 1 minute at 55° C., and 1 minute 72° C.
Plasmid DNA\Vector\Insert Preparation and Ligation\Transformation
Plasmid DNA was prepared using the `Qiagen P-100 Midi-DNA Preparation` system. Vectors and inserts were prepared by digestion of 10 μg (for vector preparation) or 20 μg (for insert preparation) with the specified restriction endonucleases under appropriate conditions (buffers and temperatures as specified by suppliers). Modification of the DNA ends with Klenow DNA polymerase and dephosphorylation with Calf Intestine Phosphorylase were performed according to the manufacturers instructions. Vector DNAs and inserts were separated through agarose gel electrophoresis and purified with DEAE-membranes NA45 (Schleicher & Schuell) as described by Maniatis et al. Ligations were performed in 20 μl volumes containing 30 mM Tris-HCl pH 7.8, 10 mM MgCl 2 , 10 mM DTT, 1 mM ATP, 300-400 ng vector DNA, 100-200 ng insert DNA and 1 Weiss unit T 4 DNA ligase. After ligation for 2-4 h at room temperature, CaCl 2 competent E. coli JM109 (Maniatis) were transformed using 7.5 μl ligation reaction. The transformation mixtures were plated onto SOBAG plates and grown overnight at 37° C. Correct clones were identified by restriction analysis and verified by automated dideoxy sequencing (Applied Biosystems).
Restriction Digestion of PCR Products
Following amplification each reaction was checked for the presence of a band of the appropriate size by agarose gel electrophoresis. One or two 100 μl PCR reaction mixtures of each of the PCR reactions PCR.I-PCR.X (FIG. 20-29), together containing approximately 2-4 μg DNA product were subjected to phenol-chloroform extraction, chloroform extraction and ethanol precipitation. The DNA pellets were washed twice with 70% ethanol and allowed to dry. Next, the PCR products were digested overnight (18 h) in the presence of excess restriction enzyme in the following mixes at the specified temperatures and volumes.
PCR.I
50 mM Tris-HCl pH 8.0, 10 mM MgCl 2 , 50 mM NaCl, 4 mM spermidine, 0.4 μg/ml BSA, 4 μl (=40 U) SacI, 4 μl (=40 U) BstEII, in 100 μl total volume at 37° C.
PCR.II
10 mM Tris-Acetate pH 7.5, 10 mM MgAc 2 , 50 mM KAc (1x "One-Phor-All" buffer ex Pharmacia), 4 μl (=48 U) SfiI, in 50 μl total volume at 50° C. under mineral oil. After overnight digestion, PCR.II-SfiI was digested with EcoRI (overnight at 37° C.) by the addition of 16 μl H 2 O, 30 μl 10x "One-Phor-All" buffer (Phanmacia) (100 mM Tris-Acetate pH 7.5, 100 mM MgAc 2 , 500 mM KAc) and 4 μl (=40 U) EcoRI.
PCR. III
10 mM Tris-Acetate pH 7.5, 10 mM MgAc 2 , 50 mM KAc (1x "One-Phor-All" buffer {Pharmacia}), 4 μl (=40 U) NheI, 4 μl (=40 U) SacI, in 100 μl total volume at 37° C.
PCR.IV
20 mM Tris-Acetate pH 7.5, 20 mM MgAc 2 , 100 mM KAc (2x "One-Phor-All" buffer {Pharmacia}), 4μl (=40 U) XhoI, 4 μl (=40 U) EcoRI, in 100 μl total volume at 37° C.
PCR.V
20 nM Tris-Acetate pH 7.5, 20 mM MgAc 2 , 100 mM KAc (2x "One-Phor-All" buffer {Pharmacia}), 4 μl (=40 U) SalI, 4 μl (=40 U) EcoRI, in 100 μl total volume at 37° C.
PCR.VI
10 mM Tris-Acetate pH 7.5, 10 mM MgAc 2 , 50 mM KAc (1x "One-Phor-All" buffer {Pharmacia}), 4 μl (=48 U) SfiI, in 50 μl total volume at 50° C. under mineral oil. After overnight digestion, PCR.VI-SfiI was digested with NheI (overnight at 37° C.) by the addition of 41 μl H 2 O, 5 μl 10x "One-Phor-All" buffer (Pharmacia) (100 mM Tris-Acetate pH 7.5, 100 mM MgAc 2 , 500 mM KAc) and 4 μl (=40 U) NheI.
PCR.VII
50 mM Tris-HCl, pH 8.0, 10 mM MgCl 2 , 50 mM NaCl, 4 mM spermidine, 0.4 μg/ml BSA, 4 μl (=40 U) NheI, 4 μl (=40 U) BstEII, in 100 μl total volume at 37° C.
PCR.VIII
20 mM Tris-Acetate pH 7.5, 20 mM MgAc 2 , 100 mM KAc (2x "One-Phor-All" buffer {Pharmacia}), 4 μl (=40 U) EcoRI, in 50 μl total volume at 37° C. After overnight digestion, PCR.VIII-EcoRI was digested with XhoI (overnight at 37° ) by the addition of 46 μl H 2 O and 4 μl (=40 U) XhoI.
PCR.IX
25 mM Tris-Acetate, pH 7.8, 100 mM KAc, 10 mM MgAc, 1 mM DTT (1x "Multi-Core" buffer {Promega}), 4 mM spermidine, 0.4 μg/ml BSA, 4 μl (=40 U) NheI, 4 μl (=40 U) BstEII, in 100 μl total volume at 37° C.
PCR.X
50 mM Tris-HCl, pH 8.0, 10 mM MgCl 2 , 50 mM NaCl, 4 mM permidine, 0.4 μg/ml BSA, 4 μl (=40 U) PstI, 4 μl (=40 U) EcoRI, in 100 μl total volume at 37° C.
______________________________________The digested PCR fragments______________________________________PCR.I-SacI/BstEII, PCR.II-SfiI/EcoRI,PCR.III-NheI/SacI, PCR.IV-XhoI/EcoRI,PCR.V-SalI/EcoRI, PCR.VI-SfiI/NheI,PCR.VII-BstEII/NheI, PCR.VIII-XhoI/EcoRI,PCR.IX-BstEII/NheI, and PCR.X-PstI/EcoRI______________________________________
were purified on an 1.2% agarose gel using DEAE-membranes NA45 (Schleicher & Schuell) as described by Maniatis et al. The purified fragments were dissolved in H 2 O at a concentration of 100-150 ng/μl.
Construction of the pGOSA Double Head Expression Vectors
The construction of pGOSA.E (see FIGS. 8A and 8B) involved several cloning steps that produced 4 intermediate constructs PGOSA.A to pGOSA.D (see FIG. 29-33). The final expression vector pGOSA.E and the oligonucleotides in Table 1 above have been designed to enable most specificities to be cloned into the final pGOSA.E construct (FIG. 9). The upstream V H domain can be replaced by any PstI-BstEII V H gene fragment obtained with oligonucleotides PCR.51 and PCR.89 (see Table 1 above). The oligonucleotides DBL.3 and DBL.4 (see Table 1 above) were designed to introduce SfiI and NheI restriction sites in the V H gene fragments thus allowing cloning of those V H gene fragments into the Sfil-NheI sites as the downstream V H domain. All V L gene fragments obtained with oligonucleotides PCR.116 and PCR.90 (see Table 1 above) can be cloned into the position of the V L .3418 gene fragment as a SacI-XhoI fragment. A complication here however is the presence of an internal SacI site in the V H .3418 gene fragment. Oligonucleotides DBL.8 and DBL.9 (see Table 1 above) are designed to allow cloning of V L gene fragments into the position of the V L .4715 gene fragment-as a SalI-NotI fragment. The pGOSA.E derivatives PGOSA.V, pGOSA.S and PGOSA.T with only one or no linker sequences contain some aberrant restriction sites at the new joining points. The V H A-V H B construct without a linker lacks the 5' V H B SfiI site. The V H B fragment is cloned into these constructs as a BstEII/NheI fragment using oligonucleotides DBL.10 or DBL.11 and DBL.4 (see Table 1 above). The V L B-V L A construct without a linker lacks the 5' V L A SalI site. The V L A fragment is cloned into these constructs as a XhoI/EcoRI fragment using oligonucleotides DBL.11 and DBL.9 (see Table 1 above).
In the following part of the description the following linkers are mentioned which are also present in the sequence listing:
the (Gly 4 Ser) 3 linker, present in SEQ ID NO: 2 as amino acids 109-123 and SEQ ID NO: 10 as amino acids 121-135,
the (Gly 4 Ser) 3 AlaGlySerAla linker (=linkerA), present in SEQ ID NO: 12 as amino acids 121-139, and
the (Gly 4 Ser) 2 Gly 4 Val linker (=linkerV), present in SEQ ID NO: 13 as amino acids 108-122.
pGOSA.A
This plasmid is derived from both the Fv.4715-myc construct and the scFv.4715-myc construct.
An SfiI restriction site was introduced between the DNA sequence encoding the (Gly 4 Ser) 3 linker and the gene fragment encoding the V L of the scFv.4715-myc construct (see FIG. 30). This was achieved by replacing the BstEII-SacI fragment of the latter construct by the fragment PCR-I BstEII/SacI (FIG. 19) that contains an SfiI site between the DNA encoding the (Gly 4 Ser) 3 linker and the V L .4715 gene fragment. The introduction of the SfiI site also introduced 4 additional amino acids (AlaGlySerAla) between the (Gly 4 Ser) 3 linker and V L .4715 resulting in a (Gly 4 Ser) 3 AlaGlySerAla linker (linkerA). The oligonucleotides used to produce PCR-I (DBL.1 and DBL.2, see Table 1 above) were designed to match the sequence of the framework-3 region of V H .4715 and to prime at the junction of the DNA encoding the (Gly 4 Ser) 3 linker and the V L .4715 gene fragment, respectively. Thus PGOSA.A can be indicated as: pelB-V H 4715-linkerA- (SfiI) -V L 4715-myc.
pGOSA.B
This plasmid is derived from plasmid Fv.3418 (see FIG. 31). The XhoI-EcoRI fragment of plasmid Fv.3418 comprising the 3' end of DNA encoding framework-4 of the V L including the stop codon was removed and replaced by the fragment PCR-IV XhoI/EcoRI (FIG. 22). The oligonucleotides used to produce PCR-IV (DBL.6 and DBL.7, see Table 1 above) were designed to match the sequence at the junction of the V L and the (Gly 4 Ser) 3 linker perfectly (DBL.6), and to be able to prime at the junction of the (Gly 4 Ser) 3 linker and the V H in pUR.4124 (DBL.7). DBL.7 removed the PstI site in the V H (silent mutation) and introduced a SalI restriction site at the junction of the (Gly 4 Ser) 3 linker and the V H , thereby replacing the last Ser of the linker by a Val residue resulting in a (Gly 4 Ser) 2 Gly 4 Val linker (linkerV). Thus pGOSA.B can be indicated as:
pelB-V H 3418+pelB-V L 3418-linkerV- (SalI-EcoRI)
pGOSA.C
This plasmid contains DNA encoding V H .4715 linked by the (Gly 4 Ser) 3 AlaGlySerAla linker to V H .3418 (see FIG. 31), thus: pelB-V H 4715-linkerA-V H 3418.
This construct was obtained by replacing the SfiI-EcoRI fragment from pGOSA.A encoding V L .4715 by the fragment PCR-II SfiI/EcoRI containing the V H .3418 gene (see FIG. 20). The oligonucleotides used to produce PCR-II (DBL.3 and DBL.4, see Table 1 above) hybridize in the framework-1 and framework-4 region of the gene encoding V H .3418, respectively. DBL.3 was designed to remove the PstI restriction site (silent mutation) and to introduce an SfiI restriction site upstream of the V H gene. DBL.4 destroys the BstEII restriction site in the framework-4 region and introduces an NheI restriction site downstream of the stopcodon.
pGOSA.D
This plasmid contains a dicistronic operon comprising the V H .3418 gene and DNA encoding V L .3418 linked by the (Gly 4 Ser) 2 Gly 4 Val linker to V L .4715 (see FIG. 32), thus:
pelB-V H 3418+pelB-V L 3418-linkerV-V L 4715.
This construct was obtained by digesting plasmid pGOSA.B with SalI-EcoRI and inserting the fragment PCR-V SalI/EcoRI (FIG. 23) containing the V L .4715 gene. The oligonucleotides used to obtain PCR-V (DBL.8 and DBL.9, see Table 1 above) were designed to match the nucleotide sequence of the framework-1 and framework-4 regions of the V L .4715 gene, respectively. DBL.8 removed the SacI site from the framework-1 region (silent mutation) and introduced a SalI restriction site upstream of the V L .4715 gene. DBL.9 destroyed the XhoI restriction site in the framework-4 region of the V L .4715 gene (silent mutation) and introduced a NotI and an EcoRI restriction site downstream of the stop codon.
PGOSA.E
This plasmid contains a dicistronic operon comprising DNA encoding V H .4715 linked by the (Gly4Ser) 3 AlaGlySerAla linker to V H .3418 plus DNA encoding V L .3418 linked by the (Gly 4 Ser) 2 Gly 4 Val linker to V L .4715 (see FIG. 33), thus:
pelB-V H 4715-linkerA-V H 3418+pelB-V L 3418-linkerV-V L 4715.
Both translational units are preceded by a ribosome binding site and DNA encoding a pelB leader sequence. This plasmid was obtained by a three-point ligation by mixing the vector resulting from pGOSA.D after removal of the V H 3418-encoding PstI-SacI insert with the PstI-NheI pGOSA.C insert containing V H .4715 linked to V H .3418 and the PCR-III NheI/SacI fragment (see FIG. 21). The remaining PstI-SacI pGOSA.D vector contains the 5' end of the framework-1 region of V H 3418 up to the PstI restriction site and V L .3418 linked by the (Gly 4 Ser) 2 Gly 4 Val linker to V L .4715 starting from the SacI restriction site in V L .3418. The PstI-NheI PGOSA.C insert contains V H .4715 linked by the (Gly 4 Ser) 3 -AlaGlySerAla linker to V H .3418, starting from the PstI restriction site in the framework-1 region in V H .4715. The NheI-SacI PCR-III fragment provides the ribosome binding site and DNA encoding the pelB leader sequence for the V L .3418-(Gly 4 Ser) 2 Gly 4 Val-V L .4715 construct. The oligo-nucleotides DBL.5 and PCR.116 (see Table 1 above) used to generate PCR-III were designed to match the sequence upstream of the ribosome binding site of V L .4715 in Fv.4715 and to introduce an NheI restriction site (DBL.5), and to match the framework-4 region of V L .3418 (PCR.116).
pGOSA.V
This plasmid is derived from PGOSA.E (see FIG. 35) from which the BstEII/NheI fragment containing DNA encoding linkerA-V H .3418 was excised and replaced by the fragment PCR-VII BstEII/NheI containing the V H .3418 gene (see FIG. 25). The resulting plasmid pGOSA.V contains V H .3418 linked directly to the framework-4 region of V H .4715, plus V L .4715 linked by the (Gly 4 Ser) 2 Gly 4 Val linker to the framework-4 region of V L .3418, thus:
pelB-V H 4715*V H 3418+pelB-V L 3418-linkerV-V L 4715.
pGOSA.S
This plasmid is derived from pGOSA.E (see FIG. 35) from which the (Gly 4 Ser) 2 Gly 4 Val-V L 4715 XhoI/EcoRI fragment was excised and replaced by the fragment PCR-VIII XhoI/EcoRI which contains V L .4715 (see FIG. 26). The resulting plasmid pGOSA.S contains V H .4715 linked by the (Gly 4 Ser) 3 -AlaGlySerAla linker to V H .3418 plus V L .3418 linked directly to the 5' end of the framework-1 region of V L .4715, thus:
pelB-V H .4715-linkerA-V H .3418+pelB-V L .3418*V L .4715.
pGOSA.T
This plasmid contains a dicistronic operon consisting of V H .3418 directly to the framework-4 region of V H .4715 plus V L .3418 linked directly to the 5' end of the framework-1 region of V L .4715 (see FIG. 36). Both transcriptional units are preceded by a ribosome binding site and a pelB leader sequence, thus:
pelB-V H .4715*V H .3418+pelB-V L .3418*V L .4715.
This construct was obtained by inserting the NheI/EcoRI fragment of pGOSA.S which contains V L .3418 linked directly to the 5' end of the framework-1 region of V L .4715, into the vector pGOSA.V from which the NheI/EcoRI fragment containing V L .3418 linked by the (Gly 4 Ser) 2 Gly 4 Val linker to V L .4715 was removed.
EXAMPLE 6
Detailed Description of the Preparation of Other Dicistronic Constructs pGOSA.G, and pGOSA.J, pGOSA.Z, PGOSA.AA and PGOSA.AB
pGOSA.G
This plasmid is an intermediate for the synthesis of pGOSA.J. It is derived from pGOSA.E from which the V H 4715 PstI/BstEII fragment has been excised and replaced by the V H 3418 PstI/BstEII fragment (excised from Fv.3418). The resulting plasmid pGOSA.G (see FIGS. 37A and 37B) contains two copies of V H .3418 linked by the (Gly 4 Ser) 3 AlaGlySerAla linker, plus V L .4715 linked by the (Gly 4 Ser) 2 Gly 4 Val linker to the framework-4 region of V L .3418, thus:
pelB-V H .3418-linkerA-V H .3418+pelB-V L .3418-linkerV-V L .47
pGOSA.J
This plasmid contains a dicistronic operon consisting of V H .3418 linked by the (Gly 4 Ser) 3 AlaGlySerAla linker to V H .4715 plus V L .3418 linked by the (Gly 4 Ser) 2 Gly 4 Val linker to V L .4715. Both transcriptional units are preceded by a ribosome binding site-and a pelB leader sequence (see FIG. 39), thus:
pelB-V H .3418-linkerA-V H .4715+pelB-V L .3418-linkerV-V L .47
This construct was obtained by inserting the fragment PCR-VI SfiI/NheI which contains V H 4715 (FIG. 24), into the vector pGOSA.G from which the SfiI/NheI V H 3418 fragment was removed.
pGOSA.Z
This plasmid is derived from PGOSA.G from which the (Gly 4 Ser) 3 AlaGlySerAla linker-V H 3418 BstEII/NheI fragment was excised and replaced by the fragment PCR-IX BstEII/NheI which contains V H .4715 (FIG. 27). The resulting plasmid pGOSA.Z (see FIG. 39) contains V H .3418 linked directly to the framework-1 region of V H .4715, plus V L .4715 linked by the (Gly 4 Ser) 2 Gly 4 Val linker to the framework-4 region of V L .3418, thus:
pelB-V H .3418*V H .4715+pelB-V L .3418-linkerV-V L .4715
PGOSA.AA
This plasmid contains a dicistronic operon consisting of the V H .3418 linked directly to the 5' end of the framework-1 region of V H .4715 plus V L .3418 linked directly to the 5' end of the framework-1 region of V L .4715. Both transcriptional units are preceded by a ribosome binding site and a pelB leader sequence (see FIG. 40). This construct was obtained by inserting the NheI/EcoRI fragment of PGOSA.T which contains V L .3418 linked directly to the 5' end of the framework-1 region of V L .4715, into the vector pGOSA.Z from which the NheI/EcoRI fragment containing V L .3418 linked by the (Gly 4 Ser) 2 Gly 4 Val linker to V L .4715 was removed, thus:
pelB-V H .3418*V H .4715+pelB-V L .3418*V L .4715
pGOSA.AB
This plasmid is derived from pGOSA.J by a three point ligation reaction (see FIG. 41). The SacI/EcoRI insert, containing part of V H .3418 and the full (Gly4Ser) 3 AlaGlySerAla linker-V H .4715 and the V L .3418-(Gly 4 Ser) 2 Gly 4 Val-V L .4715 encoding sequences, was removed and replaced by the SacI/SacI pGOSA.J fragment containing the same part of V H .3418 and the full (Gly 4 Ser) 3 AlaGlySerAla linker-V H .4715 and the SacI/EcoRI PGOSA.T fragment containing V L .3418 linked directly to the framework-1 region of V L .4715 (see FIG. 36). The resulting plasmid contains V H .3418 linked by the (Gly 4 Ser) 3 AlaGlySerAla linker to the 5' end of the framework-1 region of V H .4715 plus V L .3418 linked directly to the 5' end of the framework-1 region of V L .4715, thus:
pelB-V H .3418-linkerA-V H .4715+pelB-V L .3418*V L .4715
EXAMPLE 7
Detailed Description of the Preparation of Monocistronic Constructs pGOSA.L and pGOSA.Y, and pGOSA.C, pGOSA.X. pGOSA.AC and pGOSA.AD
pGOSA.L
This plasmid is derived from pGOSA.E from which the HindlIl/NheI fragment containing DNA encoding V H .4715-(Gly 4 Ser) 3 AlaGlySerAla-V H .3418 was removed (see FIG. 42). The DNA ends of the vector were made blunt-end using Klenow DNA polymerase and ligated. The resulting plasmid pGOSA.L contains V L .3418 linked by the (Gly 4 Ser) 2 Gly 4 Val linker to the 5' end of the framework-1 region of V L .4715, thus:
pelB-V L .3418-linkerV-V L .4715.
pGOSA.Y
This plasmid is derived from pGOSA.T from which the HindIII/NheI fragment containing DNA encoding V H .4715-V H .3418 was removed (see FIG. 43). The DNA ends of the vector were made blunt-end using Klenow DNA polymerase and ligated. The resulting plasmid pGOSA.Y contains V L .3418 linked directly to 5' end of the framework-1 region of V L .4715, thus:
pelB-V L .3418*V L .4715.
The preparation of pGOSA.C was given in Example 5 above; it can be indicated with: pelB-V H .4715-linkerA-V H .3418.
pGOSA.X
This plasmid is derived from pGOSA.T from which the RheI/EcoRI fragment containing DNA encoding V L .3418-V L .4715 was removed. The DNA ends of the vector were made blunt-end using Klenow DNA polymerase and ligated. The resulting plasmid pGOSA.X (see FIG. 44) contains V H .4715 linked directly to 5' end of the framework-1 region of V H .3418, thus: pelB-V H .4715*V H .3418.
pGOSA.AC
This plasmid is derived from pGOSA.Z from which the NheI/EcoRI fragment containing DNA encoding V L .3418-(Gly 4 Ser) 2 Gly 4 Val-V L .4715 was removed (see FIG. 45). The DNA ends of the vector were made blunt-end using Klenow DNA polymerase and ligated. The resulting plasmid pGOSA.AC contains V H .3418 linked directly to 5' end of the framework-1 region of V H .4715, thus:
pelB-V H .3418*V H .4715.
pGOSA.AD
This plasmid was obtained by inserting the PstI/EcoRI PCR.X. fragment containing DNA encoding V H .3418- (Gly 4 Ser) 3 AlaGly-SerAla-V H .4715 (see FIG. 28) into the Fv.4715-myc vector from which the PstI/EcoRI Fv.4715-myc insert was removed (see FIG. 46), thus: pelB-V H .3418-linkerA-V H .4715.
These monocistronic constructs can be used to transform the same host with two different plasmids or to transform two different hosts, so that the two V H 's in series can be produced separately from the two V L 's in series.
Evaluation of the Results Obtained
Bifunctional binding activity of GOSA double heads
In this specification the construction of a two chain protein complex is described, in which one of the chains consists of two heavy chain V-domains and the other chain consists of the two corresponding light chain V-domains. The variable domains are linked either directly or through a polypeptide linker. In this specification evidence is provided that these type of molecules ("double heads") contain both antigen binding specificities of the Fv's used to generate these multi-functional antibody fragments. FIG. 12 shows that GOSA.E can be used to specifically target the enzyme glucose oxidase to several Streptococcus sanguis strains, using antibody fragments derived from hybridomas expressing antibodies directed against these antigens. FIG. 12 further shows that the fine specificity of the anti-Streptococcus sanguis scFv 4715 is preserved in the GOSA.E double head.
Effect of Linkers and Relative Position of V-domains on Double Head Activity
After it was shown that the "cross-over double-head" approach (V H A-V H B+V L B-V L A) yields active bispecific molecules, the importance of the relative position of the V-domains in these constructs was investigated. Both possible positional orientations (GOSA.E=V H A-LinkerA-V H B+V L B-LinkerV-V L A and GOSA.J=V H B-LinkerA-V H A+V L B-LinkerV-V L A) were constructed and tested for bispecific activity, despite the suggestion obtained by molecular modelling that the binding site formed by the second (downstream/C-terminal) V-domains in the configuration V H B-V H A+V L B-V L A (GOSA.J) was in an unfavourable position for binding to large protein antigens on the surface of cells. Surprisingly however, it was found experimentally that the downstream binding site is in fact accessible. Although the relative position of the heavy chains and the light chains was found to have an effect on the observed reactivity both tested combinations show bispecific activity with the "cross-over" combination (GOSA.E=V H A-V H B+V L B-V L A) exhibiting a higher level of reactivity compared to the combination V H B-V L A+V L B-V L (=GOSA.J) as demonstrated for A=anti-Strep and B=anti-Gox.
Molecular modelling of the V H B-V H A+V L B-V L A (=GOSA.J) configuration further suggested that, only when the connecting linkers are kept long enough (to span 30 to 35 Å), the protein chains could fold such that both binding sites are fully accessible.
The "cross-over" configuration: V H A-V H B+V L B-V L A (GOSA.E) wherein linker length was not critical, was predicted to result in a complex with both binding sites facing in opposite directions, without the restraints suggested for the configuration V H B-V H A+V L B-V L A (GOSA.J). Removing the flexible polypeptide linker from the V H A-V H B chain only had a minimal effect on the ability of the double head in the "cross-over" configuration (GOSA.V=V H A*V H B+V L B-V L A) to bind both S. sanguis and Glucose oxidase. However, removing the flexible polypeptide linker from the V H B-V H A chain from the molecule in the V H B-V H A+V L B-V L A configuration (GOSA.Z =V H B*V H A+V L B-V L A) resulted in a dramatic reduction of its ability to bind both S. sanguis and Glucose oxidase.
In contrast with the double head in the "cross-over" configuration without the flexible polypeptide linker between the two heavy chain domains (GOSA.V), where molecular modelling predicted the resulting molecule to be active, removal of the flexible linker from the V L B-V L A chain could not be modelled such that both binding sites were fully accessible. ELISA results confirm that the double head in the V H B-V H A+V L B-V L A configuration without a linker between the two light chain domains (GOSA.AB) exhibits only minimal S. sanguis and glucose oxidase binding activity. Surprisingly, deletion of the flexible linker from the V L B-V L A chain from the double head in the "cross-over" configuration (GOSA.S) only had a small effect on the bispecific activity of the resulting molecule. As expected from the molecular modelling results from the double heads without a flexible linker between the two light chain domains, removal of both the flexible polypeptide linkers from the double head molecules, could not be modelled such that both binding sites were fully accessible. In agreement with the ELISA results obtained with the GOSA.AB construct, the double head in the V H B-V H A+V L B-V L A configuration without any linkers (GOSA.AA) only exhibits minimal if any S. sanguis and glucose oxidase binding activity. Surprisingly, the double head in the "cross-over" configuration without any linkers (GOSA.T=V H A*V H B+V L B*V L A) still exhibited 25-50% of S. sanguis and glucose oxidase bispecific binding activity when compared to the activity of the double head in the "cross-over" configuration with two linkers (GOSA.E).
Thus the conclusion of this work is that modelling can give some indications, but that the computer programmes cannot predict what is possible and what not. Several deviations from the modelling expectations were found. With a paraphrase on an old saying: theories are nice but the experiment is the ultimate proof.
Sensitivity of GOSA Double Heads
Using an ELISA format it was shown that the sensitivity of the GOSA.E double head is as least as a sensitive as an IgG-glucose oxidase conjugate, as determined by the lowest concentration of Streptococcus sanguis antigen immobilised on a solid phase that is still detectable.
GOSA Double Heads Are Produced as Dimers
FPLC analysis of partially affinity-purified GOSA.E, GOSA.V, GOSA.S and GOSA.T samples usually gave only one GOSA double head activity peak as determined by ELISA (FIGS. 16-18). The position of this peak in the elution pattern indicated that the molecular weight of the GOSA double head is 40-50 kD. Since this molecular weight corresponds to the expected molecular weight of the V H 2+V L 2 double head dimer, it was concluded that GOSA.E, GOSA.V, GOSA.S and GOSA.T are primarily produced as dimeric molecules. Occasionally an activity peak with an apparent molecular weight of ≈200 kD was observed (FIG. 16). The presence of glucose oxidase activity in these fractions indicate that these fractions contain GOSA double head complexed with glucose oxidase.
In Vitro Assembly of GOSA Double Heads
It was shown that bifunctionally active dimeric GOSA molecules together in one cell can be produced by translation from one dicistronic messenger (GOSA.E, GOSA.S, GOSA.T, GOSA.V, GOSA.J, GOSA.AB, GOSA.AA and GOSA.Z). In addition high levels of S. sanguis and glucose oxidase bispecific binding activity is formed when supernatants of cultures producing the separate GOSA subunits are mixed (see Example 7). The effects of linkers and the relative position of the individual V H -domains on the S. sanquis and glucose oxidase bispecific binding activity observed in these mixing experiments are comparable to the dicistronic constructs.
The constructs described above are summarised in Table 2 below.
Table 2A describes intermediate constructs that were not further tested.
Table 2B describes the dicistronic constructs.
Table 2C describes the monocistronic constructs.
(LiA) stands for the V H --V H linker (Gly 4 Ser) 3 AlaGlySerAla (=linkerA)
(LiV) stands for the V L --V L linker (Gly 4 Ser) 2 Gly 4 Val (=linkerV)
TABLE 2______________________________________Table 2AGOSA.A: V.sub.H.4715-LiA-(SfiI)-V.sub.L.4715-mycGOSA.B: V.sub.H.3418-LiV-V.sub.L.3418-(SalI/EcoRI)GOSA.D: V.sub.H.3418 + V.sub.L.3418-LiV-V.sub.L.4715GOSA.G: V.sub.H.3418-LiA-V.sub.H.3418 + V.sub.L.3418-LiV-V.sub.L.4715Table 2BGOSA.E: V.sub.H.4715-LiA-V.sub.H.3418 + V.sub.L.3418-LiV-V.sub.L.4715GOSA.S: V.sub.H.4715-LiA-V.sub.H.3418 + V.sub.L.3418*V.sub.L.4715GOSA.T: V.sub.H.4715*V.sub.H.3418 + V.sub.L.3418*V.sub.L.4715GOSA.V: V.sub.H.4715*V.sub.H.3418 + V.sub.L.3418-LiV-V.sub.L.4715GOSA.J: V.sub.H.3418-LiA-V.sub.H.4715 + V.sub.L.3418-LiV-V.sub.L.4715GOSA.AB: V.sub.H.3418-LiA-V.sub.H.4715 + V.sub.L.3418*V.sub.L.4715GOSA.AA: V.sub.H.3418*V.sub.H.4715 + V.sub.L.3418*V.sub.L.4715GOSA.Z: V.sub.H.3418*V.sub.H.4715 + V.sub.L.3418-LiV-V.sub.L.4715Table 2CGOSA.L: V.sub.L.3418-LiV-V.sub.L.4715GOSA.Y: V.sub.L.3418*V.sub.L.4715GOSA.AD: V.sub.H.3418-LiA-V.sub.H.4715GOSA.AC: V.sub.H.3418*V.sub.H.4715GOSA.C: V.sub.H.4715-LiA-V.sub.H.3418GOSA.X: V.sub.H.4715*V.sub.H.3418______________________________________ (*) indicates that the two heavy chain domains or the two light chain domains are fused together without a connecting linker.
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__________________________________________________________________________# SEQUENCE LISTING- (1) GENERAL INFORMATION:- (iii) NUMBER OF SEQUENCES: 31- (2) INFORMATION FOR SEQ ID NO: 1:- (i) SEQUENCE CHARACTERISTICS:#pairs (A) LENGTH: 737 base (B) TYPE: nucleic acid (C) STRANDEDNESS: double (D) TOPOLOGY: linear- (ii) MOLECULE TYPE: other nucleic acid#= "cDNA domains with syntheticc linker(s)"- (vii) IMMEDIATE SOURCE:#insert of pUR4124E: EcoRI-HindIII- (ix) FEATURE: (A) NAME/KEY: CDS (B) LOCATION:11..730 (D) OTHER INFORMATION:/pro - #duct= "VLlys-GS-VHlys"- (ix) FEATURE: (A) NAME/KEY: mat.sub.-- - #peptide (B) LOCATION:11..334 (D) OTHER INFORMATION:/pro - #duct= "VLlys"- (ix) FEATURE: (A) NAME/KEY: misc.sub.-- - #RNA (B) LOCATION:335..379 (D) OTHER INFORMATION:/pro - #duct= "(Gly4Ser)3 linker"- (ix) FEATURE: (A) NAME/KEY: mat.sub.-- - #peptide (B) LOCATION:380..727 (D) OTHER INFORMATION:/pro - #duct= "VHlys"#1: (xi) SEQUENCE DESCRIPTION: SEQ ID NO:- GAATTCGGCC GAC ATC GAG CTC ACC CAG TCT CCA GC - #C TCC CTT TCT GCG 49#Thr Gln Ser Pro Ala Ser Leu Ser Ala# 10- TCT GTG GGA GAA ACT GTC ACC ATC ACA TGT CG - #A GCA AGT GGG AAT ATT 97Ser Val Gly Glu Thr Val Thr Ile Thr Cys Ar - #g Ala Ser Gly Asn Ile# 25- CAC AAT TAT TTA GCA TGG TAT CAG CAG AAA CA - #G GGA AAA TCT CCT CAG 145His Asn Tyr Leu Ala Trp Tyr Gln Gln Lys Gl - #n Gly Lys Ser Pro Gln#45- CTC CTG GTC TAT TAT ACA ACA ACC TTA GCA GA - #T GGT GTG CCA TCA AGG 193Leu Leu Val Tyr Tyr Thr Thr Thr Leu Ala As - #p Gly Val Pro Ser Arg# 60- TTC AGT GGC AGT GGA TCA GGA ACA CAA TAT TC - #T CTC AAG ATC AAC AGC 241Phe Ser Gly Ser Gly Ser Gly Thr Gln Tyr Se - #r Leu Lys Ile Asn Ser# 75- CTG CAA CCT GAA GAT TTT GGG AGT TAT TAC TG - #T CAA CAT TTT TGG AGT 289Leu Gln Pro Glu Asp Phe Gly Ser Tyr Tyr Cy - #s Gln His Phe Trp Ser# 90- ACT CCT CGG ACG TTC GGT GGA GGG ACC AAG CT - #C GAG ATC AAA CGG GGT 337Thr Pro Arg Thr Phe Gly Gly Gly Thr Lys Le - #u Glu Ile Lys Arg Gly# 105- GGA GGC GGT TCA GGC GGA GGT GGC TCT GGC GG - #T GGC GGA TCG CAG GTG 385Gly Gly Gly Ser Gly Gly Gly Gly Ser Gly Gl - #y Gly Gly Ser Gln Val110 1 - #15 1 - #20 1 -#25- CAG CTG CAG GAG TCA GGA CCT GGC CTG GTG GC - #G CCC TCA CAG AGC CTG 433Gln Leu Gln Glu Ser Gly Pro Gly Leu Val Al - #a Pro Ser Gln Ser Leu# 140- TCC ATC ACA TGC ACC GTC TCA GGG TTC TCA TT - #A ACC GGC TAT GGT GTA 481Ser Ile Thr Cys Thr Val Ser Gly Phe Ser Le - #u Thr Gly Tyr Gly Val# 155- AAC TGG GTT CGC CAG CCT CCA GGA AAG GGT CT - #G GAG TGG CTG GGA ATG 529Asn Trp Val Arg Gln Pro Pro Gly Lys Gly Le - #u Glu Trp Leu Gly Met# 170- ATT TGG GGT GAT GGA AAC ACA GAC TAT AAT TC - #A GCT CTC AAA TCC AGA 577Ile Trp Gly Asp Gly Asn Thr Asp Tyr Asn Se - #r Ala Leu Lys Ser Arg# 185- CTG AGC ATC AGC AAG GAC AAC TCC AAG AGC CA - #A GTT TTC TTA AAA ATG 625Leu Ser Ile Ser Lys Asp Asn Ser Lys Ser Gl - #n Val Phe Leu Lys Met190 1 - #95 2 - #00 2 -#05- AAC AGT CTG CAC ACT GAT GAC ACA GCC AGG TA - #C TAC TGT GCC AGA GAG 673Asn Ser Leu His Thr Asp Asp Thr Ala Arg Ty - #r Tyr Cys Ala Arg Glu# 220- AGA GAT TAT AGG CTT GAC TAC TGG GGC CAA GG - #G ACC ACG GTC ACC GTC 721Arg Asp Tyr Arg Leu Asp Tyr Trp Gly Gln Gl - #y Thr Thr Val Thr Val# 235# 737 TTSer Ser- (2) INFORMATION FOR SEQ ID NO: 2:- (i) SEQUENCE CHARACTERISTICS:#acids (A) LENGTH: 239 amino (B) TYPE: amino acid (D) TOPOLOGY: linear- (ii) MOLECULE TYPE: protein#2: (xi) SEQUENCE DESCRIPTION: SEQ ID NO:- Asp Ile Glu Leu Thr Gln Ser Pro Ala Ser Le - #u Ser Ala Ser Val Gly# 15- Glu Thr Val Thr Ile Thr Cys Arg Ala Ser Gl - #y Asn Ile His Asn Tyr# 30- Leu Ala Trp Tyr Gln Gln Lys Gln Gly Lys Se - #r Pro Gln Leu Leu Val# 45- Tyr Tyr Thr Thr Thr Leu Ala Asp Gly Val Pr - #o Ser Arg Phe Ser Gly# 60- Ser Gly Ser Gly Thr Gln Tyr Ser Leu Lys Il - #e Asn Ser Leu Gln Pro#80- Glu Asp Phe Gly Ser Tyr Tyr Cys Gln His Ph - #e Trp Ser Thr Pro Arg# 95- Thr Phe Gly Gly Gly Thr Lys Leu Glu Ile Ly - #s Arg Gly Gly Gly Gly# 110- Ser Gly Gly Gly Gly Ser Gly Gly Gly Gly Se - #r Gln Val Gln Leu Gln# 125- Glu Ser Gly Pro Gly Leu Val Ala Pro Ser Gl - #n Ser Leu Ser Ile Thr# 140- Cys Thr Val Ser Gly Phe Ser Leu Thr Gly Ty - #r Gly Val Asn Trp Val145 1 - #50 1 - #55 1 -#60- Arg Gln Pro Pro Gly Lys Gly Leu Glu Trp Le - #u Gly Met Ile Trp Gly# 175- Asp Gly Asn Thr Asp Tyr Asn Ser Ala Leu Ly - #s Ser Arg Leu Ser Ile# 190- Ser Lys Asp Asn Ser Lys Ser Gln Val Phe Le - #u Lys Met Asn Ser Leu# 205- His Thr Asp Asp Thr Ala Arg Tyr Tyr Cys Al - #a Arg Glu Arg Asp Tyr# 220- Arg Leu Asp Tyr Trp Gly Gln Gly Thr Thr Va - #l Thr Val Ser Ser225 2 - #30 2 - #35- (2) INFORMATION FOR SEQ ID NO: 3:- (i) SEQUENCE CHARACTERISTICS:#pairs (A) LENGTH: 920 base (B) TYPE: nucleic acid (C) STRANDEDNESS: double (D) TOPOLOGY: linear- (ii) MOLECULE TYPE: other nucleic acid#= "cDNA domains with syntheticc linker(s)"- (vii) IMMEDIATE SOURCE:#insert Fv.3418LONE: HindIII-EcoRI- (ix) FEATURE: (A) NAME/KEY: CDS (B) LOCATION:36..443 (D) OTHER INFORMATION:/pro - #duct= "pelB-VH3418"- (ix) FEATURE: (A) NAME/KEY: sig.sub.-- - #peptide (B) LOCATION:36..101 (D) OTHER INFORMATION:/pro - #duct= "pectate lyase"- (ix) FEATURE: (A) NAME/KEY: mat.sub.-- - #peptide (B) LOCATION:102..440 (D) OTHER INFORMATION:/pro - #duct= "VH3418"- (ix) FEATURE: (A) NAME/KEY: CDS (B) LOCATION:495..884 (D) OTHER INFORMATION:/pro - #duct= "pelB-VL4318"- (ix) FEATURE: (A) NAME/KEY: sig.sub.-- - #peptide (B) LOCATION:495..560#/product= "pectate lyase"ATION:- (ix) FEATURE: (A) NAME/KEY: mat.sub.-- - #peptide (B) LOCATION:561..881 (D) OTHER INFORMATION:/pro - #duct= "VL3418"#3: (xi) SEQUENCE DESCRIPTION: SEQ ID NO:#CTA TTG CCT 53C AAGGAGACAG TCATA ATG AAA TAC# Met Lys Tyr Leu Leu Pro20- ACG GCA GCC GCT GGA TTG TTA TTA CTC GCT GC - #C CAA CCA GCG ATG GCC 101Thr Ala Ala Ala Gly Leu Leu Leu Leu Ala Al - #a Gln Pro Ala Met Ala- CAG GTG CAG CTG CAG CAG TCA GGA CCT GAG CT - #G GTA AAG CCT GGG GCT 149Gln Val Gln Leu Gln Gln Ser Gly Pro Glu Le - #u Val Lys Pro Gly Ala# 15- TCA GTG AAG ATG TCC TGC AAG GCT TCT GGA TA - #C ACA TTC ACT AGC TAT 197Ser Val Lys Met Ser Cys Lys Ala Ser Gly Ty - #r Thr Phe Thr Ser Tyr# 30- GTT ATG CAC TGG GTG AAA CAG AAG CCT GGG CA - #G GGC CTT GAG TGG ATT 245Val Met His Trp Val Lys Gln Lys Pro Gly Gl - #n Gly Leu Glu Trp Ile# 45- GGA TAT ATT TAT CCT TAC AAT GAT GGT ACT AA - #G TAC AAT GAG AAG TTC 293Gly Tyr Ile Tyr Pro Tyr Asn Asp Gly Thr Ly - #s Tyr Asn Glu Lys Phe# 60- AAA GGC AAG GCC ACA CTG ACT TCA GAC AAA TC - #C TCC AGC ACA GCC TAC 341Lys Gly Lys Ala Thr Leu Thr Ser Asp Lys Se - #r Ser Ser Thr Ala Tyr#80- ATG GAG CTC AGC AGC CTG ACC TCT GAG GAC TC - #T GCG GTC TAT TAC TGT 389Met Glu Leu Ser Ser Leu Thr Ser Glu Asp Se - #r Ala Val Tyr Tyr Cys# 95- TCA AGA CGC TTT GAC TAC TGG GGC CAA GGG AC - #C ACG GTC ACC GTC TCC 437Ser Arg Arg Phe Asp Tyr Trp Gly Gln Gly Th - #r Thr Val Thr Val Ser# 110- TCA TAA TAAGAGCTAT GGGAGCTTGC ATGCAAATTC TATTTCAAGG AG - #ACAGTCAT 493Ser#GGA TTG TTA TTA CTC 539 GCA GCC GCT Met Lys Tyr Leu Leu Pro Thr Ala Ala A - #la Gly Leu Leu Leu Leu10- GCT GCC CAA CCA GCG ATG GCC GAC ATC GAG CT - #C ACC CAG TCT CCA TCT 587Ala Ala Gln Pro Ala Met Ala Asp Ile Glu Le - #u Thr Gln Ser Pro Ser# 5 1- TCC ATG TAT GCA TCT CTA GGA GAG AGA ATC AC - #T ATC ACT TGC AAG GCG 635Ser Met Tyr Ala Ser Leu Gly Glu Arg Ile Th - #r Ile Thr Cys Lys Ala#25- AGT CAG GAC ATT AAT ACC TAT TTA ACC TGG TT - #C CAG CAG AAA CCA GGG 683Ser Gln Asp Ile Asn Thr Tyr Leu Thr Trp Ph - #e Gln Gln Lys Pro Gly# 40- AAA TCT CCC AAG ACC CTG ATC TAT CGT GCA AA - #C AGA TTG CTA GAT GGG 731Lys Ser Pro Lys Thr Leu Ile Tyr Arg Ala As - #n Arg Leu Leu Asp Gly# 55- GTC CCA TCA AGG TTC AGT GGC AGT GGA TCT GG - #G CAA GAT TAT TCT CTC 779Val Pro Ser Arg Phe Ser Gly Ser Gly Ser Gl - #y Gln Asp Tyr Ser Leu# 70- ACC ATC AGC AGC CTG GAC TAT GAA GAT ATG GG - #A ATT TAT TAT TGT CTA 827Thr Ile Ser Ser Leu Asp Tyr Glu Asp Met Gl - #y Ile Tyr Tyr Cys Leu# 85- CAA TAT GAT GAG TTG TAC ACG TTC GGA GGG GG - #G ACC AAG CTC GAG ATC 875Gln Tyr Asp Glu Leu Tyr Thr Phe Gly Gly Gl - #y Thr Lys Leu Glu Ile#105# 920CAA ACGGTATAAG GATCCAGCTC GAATTCLys Arg- (2) INFORMATION FOR SEQ ID NO: 4:- (i) SEQUENCE CHARACTERISTICS:#acids (A) LENGTH: 135 amino (B) TYPE: amino acid (D) TOPOLOGY: linear- (ii) MOLECULE TYPE: protein#4: (xi) SEQUENCE DESCRIPTION: SEQ ID NO:- Met Lys Tyr Leu Leu Pro Thr Ala Ala Ala Gl - #y Leu Leu Leu Leu Ala10- Ala Gln Pro Ala Met Ala Gln Val Gln Leu Gl - #n Gln Ser Gly Pro Glu# 10- Leu Val Lys Pro Gly Ala Ser Val Lys Met Se - #r Cys Lys Ala Ser Gly# 25- Tyr Thr Phe Thr Ser Tyr Val Met His Trp Va - #l Lys Gln Lys Pro Gly# 40- Gln Gly Leu Glu Trp Ile Gly Tyr Ile Tyr Pr - #o Tyr Asn Asp Gly Thr# 55- Lys Tyr Asn Glu Lys Phe Lys Gly Lys Ala Th - #r Leu Thr Ser Asp Lys# 70- Ser Ser Ser Thr Ala Tyr Met Glu Leu Ser Se - #r Leu Thr Ser Glu Asp#90- Ser Ala Val Tyr Tyr Cys Ser Arg Arg Phe As - #p Tyr Trp Gly Gln Gly# 105- Thr Thr Val Thr Val Ser Ser 110- (2) INFORMATION FOR SEQ ID NO: 5:- (i) SEQUENCE CHARACTERISTICS:#acids (A) LENGTH: 129 amino (B) TYPE: amino acid (D) TOPOLOGY: linear- (ii) MOLECULE TYPE: protein#5: (xi) SEQUENCE DESCRIPTION: SEQ ID NO:- Met Lys Tyr Leu Leu Pro Thr Ala Ala Ala Gl - #y Leu Leu Leu Leu Ala10- Ala Gln Pro Ala Met Ala Asp Ile Glu Leu Th - #r Gln Ser Pro Ser Ser# 10- Met Tyr Ala Ser Leu Gly Glu Arg Ile Thr Il - #e Thr Cys Lys Ala Ser# 25- Gln Asp Ile Asn Thr Tyr Leu Thr Trp Phe Gl - #n Gln Lys Pro Gly Lys# 40- Ser Pro Lys Thr Leu Ile Tyr Arg Ala Asn Ar - #g Leu Leu Asp Gly Val# 55- Pro Ser Arg Phe Ser Gly Ser Gly Ser Gly Gl - #n Asp Tyr Ser Leu Thr# 70- Ile Ser Ser Leu Asp Tyr Glu Asp Met Gly Il - #e Tyr Tyr Cys Leu Gln#90- Tyr Asp Glu Leu Tyr Thr Phe Gly Gly Gly Th - #r Lys Leu Glu Ile Lys# 105- Arg- (2) INFORMATION FOR SEQ ID NO: 6:- (i) SEQUENCE CHARACTERISTICS:#pairs (A) LENGTH: 999 base (B) TYPE: nucleic acid (C) STRANDEDNESS: double (D) TOPOLOGY: linear- (ii) MOLECULE TYPE: other nucleic acid#= "cDNA domains with syntheticc linker(s)"- (vii) IMMEDIATE SOURCE:#insert of Fv.4715-mycindIII-EcoRI- (ix) FEATURE: (A) NAME/KEY: CDS (B) LOCATION:40..468 (D) OTHER INFORMATION:/pro - #duct= "pelB-VH4715"- (ix) FEATURE: (A) NAME/KEY: sig.sub.-- - #peptide (B) LOCATION:40..105 (D) OTHER INFORMATION:/pro - #duct= "pectate lyase"- (ix) FEATURE: (A) NAME/KEY: mat.sub.-- - #peptide (B) LOCATION:106..465 (D) OTHER INFORMATION:/pro - #duct= "VH4715"- (ix) FEATURE: (A) NAME/KEY: CDS (B) LOCATION:520..963 (D) OTHER INFORMATION:/pro - #duct= "pelB-VL4715-myc"- (ix) FEATURE: (A) NAME/KEY: sig.sub.-- - #peptide (B) LOCATION:520..585 (D) OTHER INFORMATION:/pro - #duct= "pectate lyase"- (ix) FEATURE: (A) NAME/KEY: mat.sub.-- - #peptide (B) LOCATION:586..927 (D) OTHER INFORMATION:/pro - #duct= "VL4715"- (ix) FEATURE: (A) NAME/KEY: misc RNA (B) LOCATION:928..960 (D) OTHER INFORMATION:/pro - #duct= "myc-tag"#6: (xi) SEQUENCE DESCRIPTION: SEQ ID NO:- AAGCTTGCAT GCAAATTCTA TTTCAAGGAG ACAGTCATA ATG AAA TAC - # CTA TTG 54# Met Lys Tyr Leu Leu20- CCT ACG GCA GCC GCT GGA TTG TTA TTA CTC GC - #T GCC CAA CCA GCG ATG 102Pro Thr Ala Ala Ala Gly Leu Leu Leu Leu Al - #a Ala Gln Pro Ala Met5- GCC CAG GTG CAG CTG CAG GAG TCA GGG GGA GA - #C TTA GTG AAG CCT GGA 150Ala Gln Val Gln Leu Gln Glu Ser Gly Gly As - #p Leu Val Lys Pro Gly# 15- GGG TCC CTG ACA CTC TCC TGT GCA ACC TCT GG - #A TTC ACT TTC AGT AGT 198Gly Ser Leu Thr Leu Ser Cys Ala Thr Ser Gl - #y Phe Thr Phe Ser Ser# 30- TAT GCC TTT TCT TGG GTC CGC CAG ACC TCA GA - #C AAG AGT CTG GAG TGG 246Tyr Ala Phe Ser Trp Val Arg Gln Thr Ser As - #p Lys Ser Leu Glu Trp# 45- GTC GCA ACC ATC AGT AGT ACT GAT ACT TAT AC - #C TAT TAT TCA GAC AAT 294Val Ala Thr Ile Ser Ser Thr Asp Thr Tyr Th - #r Tyr Tyr Ser Asp Asn# 60- GTG AAG GGG CGC TTC ACC ATC TCC AGA GAC AA - #T GGC AAG AAC ACC CTG 342Val Lys Gly Arg Phe Thr Ile Ser Arg Asp As - #n Gly Lys Asn Thr Leu# 75- TAC CTG CAA ATG AGC AGT CTG AAG TCT GAG GA - #C ACA GCC GTG TAT TAC 390Tyr Leu Gln Met Ser Ser Leu Lys Ser Glu As - #p Thr Ala Val Tyr Tyr#95- TGT GCA AGA CAT GGG TAC TAT GGT AAA GGC TA - #T TTT GAC TAC TGG GGC 438Cys Ala Arg His Gly Tyr Tyr Gly Lys Gly Ty - #r Phe Asp Tyr Trp Gly# 110- CAA GGG ACC ACG GTC ACC GTC TCC TCA TAA TA - #AGAGCTAT GGGAGCTTGC 488Gln Gly Thr Thr Val Thr Val Ser Ser# 120#TTG CCT ACG 540G AGACAGTCAT A ATG AAA TAC CTA# Met - # Lys Tyr Leu Leu Pro Thr20 - #- GCA GCC GCT GGA TTG TTA TTA CTC GCT GCC CA - #A CCA GCG ATG GCC GAC 588Ala Ala Ala Gly Leu Leu Leu Leu Ala Ala Gl - #n Pro Ala Met Ala Asp#1#5- ATC GAG CTC ACT CAG TCT CCA TTC TCC CTG AC - #T GTG ACA GCA GGA GAG 636Ile Glu Leu Thr Gln Ser Pro Phe Ser Leu Th - #r Val Thr Ala Gly Glu# 15- AAG GTC ACT ATG AAT TGC AAG TCC GGT CAG AG - #T CTG TTA AAC AGT GTA 684Lys Val Thr Met Asn Cys Lys Ser Gly Gln Se - #r Leu Leu Asn Ser Val# 30- AAT CAG AGG AAC TAC TTG ACC TGG TAC CAG CA - #G AAG CCA GGG CAG CCT 732Asn Gln Arg Asn Tyr Leu Thr Trp Tyr Gln Gl - #n Lys Pro Gly Gln Pro# 45- CCT AAA CTG TTG ATC TAC TGG GCA TCC ACT AG - #G GAA TCT GGA GTC CCT 780Pro Lys Leu Leu Ile Tyr Trp Ala Ser Thr Ar - #g Glu Ser Gly Val Pro#65- GAT CGC TTC ACA GCC AGT GGA TCT GGA ACA GA - #T TTC ACT CTC ACC ATC 828Asp Arg Phe Thr Ala Ser Gly Ser Gly Thr As - #p Phe Thr Leu Thr Ile# 80- AGC AGT GTG CAG GCT GAA GAC CTG GCA GTT TA - #T TAC TGT CAG AAT GAT 876Ser Ser Val Gln Ala Glu Asp Leu Ala Val Ty - #r Tyr Cys Gln Asn Asp# 95- TAT ACT TAT CCG TTC ACG TTC GGA GGG GGG AC - #C AAG CTC GAG ATC AAA 924Tyr Thr Tyr Pro Phe Thr Phe Gly Gly Gly Th - #r Lys Leu Glu Ile Lys# 110- CGG GAA CAA AAA CTC ATC TCA GAA GAG GAT CT - #G AAT TAA TAAGATCAAA 973Arg Glu Gln Lys Leu Ile Ser Glu Glu Asp Le - #u Asn# 125# 999 GCTC GAATTC- (2) INFORMATION FOR SEQ ID NO: 7:- (i) SEQUENCE CHARACTERISTICS:#acids (A) LENGTH: 142 amino (B) TYPE: amino acid (D) TOPOLOGY: linear- (ii) MOLECULE TYPE: protein#7: (xi) SEQUENCE DESCRIPTION: SEQ ID NO:- Met Lys Tyr Leu Leu Pro Thr Ala Ala Ala Gl - #y Leu Leu Leu Leu Ala10- Ala Gln Pro Ala Met Ala Gln Val Gln Leu Gl - #n Glu Ser Gly Gly Asp# 10- Leu Val Lys Pro Gly Gly Ser Leu Thr Leu Se - #r Cys Ala Thr Ser Gly# 25- Phe Thr Phe Ser Ser Tyr Ala Phe Ser Trp Va - #l Arg Gln Thr Ser Asp# 40- Lys Ser Leu Glu Trp Val Ala Thr Ile Ser Se - #r Thr Asp Thr Tyr Thr# 55- Tyr Tyr Ser Asp Asn Val Lys Gly Arg Phe Th - #r Ile Ser Arg Asp Asn# 70- Gly Lys Asn Thr Leu Tyr Leu Gln Met Ser Se - #r Leu Lys Ser Glu Asp#90- Thr Ala Val Tyr Tyr Cys Ala Arg His Gly Ty - #r Tyr Gly Lys Gly Tyr# 105- Phe Asp Tyr Trp Gly Gln Gly Thr Thr Val Th - #r Val Ser Ser# 120- (2) INFORMATION FOR SEQ ID NO: 8:- (i) SEQUENCE CHARACTERISTICS:#acids (A) LENGTH: 147 amino (B) TYPE: amino acid (D) TOPOLOGY: linear- (ii) MOLECULE TYPE: protein#8: (xi) SEQUENCE DESCRIPTION: SEQ ID NO:- Met Lys Tyr Leu Leu Pro Thr Ala Ala Ala Gl - #y Leu Leu Leu Leu Ala10- Ala Gln Pro Ala Met Ala Asp Ile Glu Leu Th - #r Gln Ser Pro Phe Ser# 10- Leu Thr Val Thr Ala Gly Glu Lys Val Thr Me - #t Asn Cys Lys Ser Gly# 25- Gln Ser Leu Leu Asn Ser Val Asn Gln Arg As - #n Tyr Leu Thr Trp Tyr# 40- Gln Gln Lys Pro Gly Gln Pro Pro Lys Leu Le - #u Ile Tyr Trp Ala Ser# 55- Thr Arg Glu Ser Gly Val Pro Asp Arg Phe Th - #r Ala Ser Gly Ser Gly# 70- Thr Asp Phe Thr Leu Thr Ile Ser Ser Val Gl - #n Ala Glu Asp Leu Ala#90- Val Tyr Tyr Cys Gln Asn Asp Tyr Thr Tyr Pr - #o Phe Thr Phe Gly Gly# 105- Gly Thr Lys Leu Glu Ile Lys Arg Glu Gln Ly - #s Leu Ile Ser Glu Glu# 120- Asp Leu Asn 125- (2) INFORMATION FOR SEQ ID NO: 9:- (i) SEQUENCE CHARACTERISTICS:#pairs (A) LENGTH: 924 base (B) TYPE: nucleic acid (C) STRANDEDNESS: double (D) TOPOLOGY: linear- (ii) MOLECULE TYPE: other nucleic acid#= "cDNA domains with syntheticc linker(s)"- (vii) IMMEDIATE SOURCE:#insert of scFv.4715-mycdIII-EcoRI- (ix) FEATURE: (A) NAME/KEY: sig.sub.-- - #peptide (B) LOCATION:40..105 (D) OTHER INFORMATION:/pro - #duct= "pectate lyase"- (ix) FEATURE: (A) NAME/KEY: mat.sub.-- - #peptide (B) LOCATION:106..465 (D) OTHER INFORMATION:/pro - #duct= "VH4715"- (ix) FEATURE: (A) NAME/KEY: misc.sub.-- - #RNA (B) LOCATION:466..510 (D) OTHER INFORMATION:/pro - #duct= "(Gly4Ser)3-linker"- (ix) FEATURE: (A) NAME/KEY: mat.sub.-- - #peptide (B) LOCATION:511..852 (D) OTHER INFORMATION:/pro - #duct= "VL4715"- (ix) FEATURE: (A) NAME/KEY: misc.sub.-- - #RNA (B) LOCATION:853..885 (D) OTHER INFORMATION:/pro - #duct= "myc-tag"- (ix) FEATURE: (A) NAME/KEY: CDS (B) LOCATION:40..888 (D) OTHER INFORMATION:/pro - #duct= "pelB-VH4715-(Gly4Ser)3- VL4715-myc"#9: (xi) SEQUENCE DESCRIPTION: SEQ ID NO:- AAGCTTGCAT GCAAATTCTA TTTCAAGGAG ACAGTCATA ATG AAA TAC - # CTA TTG 54# Met Lys Tyr Leu Leu20- CCT ACG GCA GCC GCT GGA TTG TTA TTA CTC GC - #T GCC CAA CCA GCG ATG 102Pro Thr Ala Ala Ala Gly Leu Leu Leu Leu Al - #a Ala Gln Pro Ala Met5- GCC CAG GTG CAG CTG CAG GAG TCA GGG GGA GA - #C TTA GTG AAG CCT GGA 150Ala Gln Val Gln Leu Gln Glu Ser Gly Gly As - #p Leu Val Lys Pro Gly# 15- GGG TCC CTG ACA CTC TCC TGT GCA ACC TCT GG - #A TTC ACT TTC AGT AGT 198Gly Ser Leu Thr Leu Ser Cys Ala Thr Ser Gl - #y Phe Thr Phe Ser Ser# 30- TAT GCC TTT TCT TGG GTC CGC CAG ACC TCA GA - #C AAG AGT CTG GAG TGG 246Tyr Ala Phe Ser Trp Val Arg Gln Thr Ser As - #p Lys Ser Leu Glu Trp# 45- GTC GCA ACC ATC AGT AGT ACT GAT ACT TAT AC - #C TAT TAT TCA GAC AAT 294Val Ala Thr Ile Ser Ser Thr Asp Thr Tyr Th - #r Tyr Tyr Ser Asp Asn# 60- GTG AAG GGG CGC TTC ACC ATC TCC AGA GAC AA - #T GGC AAG AAC ACC CTG 342Val Lys Gly Arg Phe Thr Ile Ser Arg Asp As - #n Gly Lys Asn Thr Leu# 75- TAC CTG CAA ATG AGC AGT CTG AAG TCT GAG GA - #C ACA GCC GTG TAT TAC 390Tyr Leu Gln Met Ser Ser Leu Lys Ser Glu As - #p Thr Ala Val Tyr Tyr#95- TGT GCA AGA CAT GGG TAC TAT GGT AAA GGC TA - #T TTT GAC TAC TGG GGC 438Cys Ala Arg His Gly Tyr Tyr Gly Lys Gly Ty - #r Phe Asp Tyr Trp Gly# 110- CAA GGG ACC ACG GTC ACC GTC TCC TCA GGT GG - #A GGC GGT TCA GGC GGA 486Gln Gly Thr Thr Val Thr Val Ser Ser Gly Gl - #y Gly Gly Ser Gly Gly# 125- GGT GGC TCT GGC GGT GGC GGA TCG GAC ATC GA - #G CTC ACT CAG TCT CCA 534Gly Gly Ser Gly Gly Gly Gly Ser Asp Ile Gl - #u Leu Thr Gln Ser Pro# 140- TTC TCC CTG ACT GTG ACA GCA GGA GAG AAG GT - #C ACT ATG AAT TGC AAG 582Phe Ser Leu Thr Val Thr Ala Gly Glu Lys Va - #l Thr Met Asn Cys Lys# 155- TCC GGT CAG AGT CTG TTA AAC AGT GTA AAT CA - #G AGG AAC TAC TTG ACC 630Ser Gly Gln Ser Leu Leu Asn Ser Val Asn Gl - #n Arg Asn Tyr Leu Thr160 1 - #65 1 - #70 1 -#75- TGG TAC CAG CAG AAG CCA GGG CAG CCT CCT AA - #A CTG TTG ATC TAC TGG 678Trp Tyr Gln Gln Lys Pro Gly Gln Pro Pro Ly - #s Leu Leu Ile Tyr Trp# 190- GCA TCC ACT AGG GAA TCT GGA GTC CCT GAT CG - #C TTC ACA GCC AGT GGA 726Ala Ser Thr Arg Glu Ser Gly Val Pro Asp Ar - #g Phe Thr Ala Ser Gly# 205- TCT GGA ACA GAT TTC ACT CTC ACC ATC AGC AG - #T GTG CAG GCT GAA GAC 774Ser Gly Thr Asp Phe Thr Leu Thr Ile Ser Se - #r Val Gln Ala Glu Asp# 220- CTG GCA GTT TAT TAC TGT CAG AAT GAT TAT AC - #T TAT CCG TTC ACG TTC 822Leu Ala Val Tyr Tyr Cys Gln Asn Asp Tyr Th - #r Tyr Pro Phe Thr Phe# 235- GGA GGG GGG ACC AAG CTC GAG ATC AAA CGG GA - #A CAA AAA CTC ATC TCA 870Gly Gly Gly Thr Lys Leu Glu Ile Lys Arg Gl - #u Gln Lys Leu Ile Ser240 2 - #45 2 - #50 2 -#55- GAA GAG GAT CTG AAT TAA TAAGATCAAA CGGTAATAAG GA - #TCCAGCTC GAATTC 924Glu Glu Asp Leu Asn 260- (2) INFORMATION FOR SEQ ID NO: 10:- (i) SEQUENCE CHARACTERISTICS:#acids (A) LENGTH: 282 amino (B) TYPE: amino acid (D) TOPOLOGY: linear- (ii) MOLECULE TYPE: protein#10: (xi) SEQUENCE DESCRIPTION: SEQ ID NO:- Met Lys Tyr Leu Leu Pro Thr Ala Ala Ala Gl - #y Leu Leu Leu Leu Ala10- Ala Gln Pro Ala Met Ala Gln Val Gln Leu Gl - #n Glu Ser Gly Gly Asp# 10- Leu Val Lys Pro Gly Gly Ser Leu Thr Leu Se - #r Cys Ala Thr Ser Gly# 25- Phe Thr Phe Ser Ser Tyr Ala Phe Ser Trp Va - #l Arg Gln Thr Ser Asp# 40- Lys Ser Leu Glu Trp Val Ala Thr Ile Ser Se - #r Thr Asp Thr Tyr Thr# 55- Tyr Tyr Ser Asp Asn Val Lys Gly Arg Phe Th - #r Ile Ser Arg Asp Asn# 70- Gly Lys Asn Thr Leu Tyr Leu Gln Met Ser Se - #r Leu Lys Ser Glu Asp#90- Thr Ala Val Tyr Tyr Cys Ala Arg His Gly Ty - #r Tyr Gly Lys Gly Tyr# 105- Phe Asp Tyr Trp Gly Gln Gly Thr Thr Val Th - #r Val Ser Ser Gly Gly# 120- Gly Gly Ser Gly Gly Gly Gly Ser Gly Gly Gl - #y Gly Ser Asp Ile Glu# 135- Leu Thr Gln Ser Pro Phe Ser Leu Thr Val Th - #r Ala Gly Glu Lys Val# 150- Thr Met Asn Cys Lys Ser Gly Gln Ser Leu Le - #u Asn Ser Val Asn Gln155 1 - #60 1 - #65 1 -#70- Arg Asn Tyr Leu Thr Trp Tyr Gln Gln Lys Pr - #o Gly Gln Pro Pro Lys# 185- Leu Leu Ile Tyr Trp Ala Ser Thr Arg Glu Se - #r Gly Val Pro Asp Arg# 200- Phe Thr Ala Ser Gly Ser Gly Thr Asp Phe Th - #r Leu Thr Ile Ser Ser# 215- Val Gln Ala Glu Asp Leu Ala Val Tyr Tyr Cy - #s Gln Asn Asp Tyr Thr# 230- Tyr Pro Phe Thr Phe Gly Gly Gly Thr Lys Le - #u Glu Ile Lys Arg Glu235 2 - #40 2 - #45 2 -#50- Gln Lys Leu Ile Ser Glu Glu Asp Leu Asn# 260- (2) INFORMATION FOR SEQ ID NO: 11:- (i) SEQUENCE CHARACTERISTICS:#pairs (A) LENGTH: 1706 base (B) TYPE: nucleic acid (C) STRANDEDNESS: double (D) TOPOLOGY: linear- (ii) MOLECULE TYPE: other nucleic acid#= "cDNA domains with syntheticc linker(s)"- (vii) IMMEDIATE SOURCE:#insert of pGOSA.EE: HindIII-EcoRI- (ix) FEATURE: (A) NAME/KEY: CDS (B) LOCATION:40..864 (D) OTHER INFORMATION:/pro - #duct= "pelB-VH4715-LiA-VH3418"- (ix) FEATURE: (A) NAME/KEY: sig.sub.-- - #peptide (B) LOCATION:40..105 (D) OTHER INFORMATION:/pro - #duct= "pectate lyase"- (ix) FEATURE: (A) NAME/KEY: mat.sub.-- - #peptide (B) LOCATION:106..465 (D) OTHER INFORMATION:/pro - #duct= "VH4715"- (ix) FEATURE: (A) NAME/KEY: misc.sub.-- - #RNA (B) LOCATION:466..522 (D) OTHER INFORMATION:/pro - #duct= "linkerA (Gly4Ser) 3AlaGlySerAl - #a"- (ix) FEATURE: (A) NAME/KEY: mat.sub.-- - #peptide (B) LOCATION:523..861 (D) OTHER INFORMATION:/pro - #duct= "VH3418"- (ix) FEATURE: (A) NAME/KEY: CDS (B) LOCATION:913..1689 (D) OTHER INFORMATION:/pro - #duct= "pelB-VL3418-LiV-VL4715"- (ix) FEATURE: (A) NAME/KEY: sig.sub.-- - #peptide (B) LOCATION:913..978 (D) OTHER INFORMATION:/pro - #duct= "pectate lyase"- (ix) FEATURE: (A) NAME/KEY: mat.sub.-- - #peptide (B) LOCATION:979..1299 (D) OTHER INFORMATION:/pro - #duct= "VL3418"- (ix) FEATURE: (A) NAME/KEY: misc.sub.-- - #RNA (B) LOCATION:1300..1344 (D) OTHER INFORMATION:/pro - #duct= "linker V (Gly4Ser)2Gly4Val"- (ix) FEATURE: (A) NAME/KEY: mat.sub.-- - #peptide (B) LOCATION:1345..1686 (D) OTHER INFORMATION:/pro - #duct= "VL4715"#11: (xi) SEQUENCE DESCRIPTION: SEQ ID NO:- AAGCTTGCAT GGAAATTCTA TTTCAAGGAG ACAGTCATA ATG AAA TAC - # CTA TTG 54# Met Lys Tyr Leu Leu20- CCT ACG GCA GCC GCT GGA TTG TTA TTA CTC GC - #T GCC CAA CCA GCG ATG 102Pro Thr Ala Ala Ala Gly Leu Leu Leu Leu Al - #a Ala Gln Pro Ala Met5- GCC CAG GTG CAG CTG CAG GAG TCA GGG GGA GA - #C TTA GTG AAG CCT GGA 150Ala Gln Val Gln Leu Gln Glu Ser Gly Gly As - #p Leu Val Lys Pro Gly# 15- GGG TCC CTG ACA CTC TCC TGT GCA ACC TCT GG - #A TTC ACT TTC AGT AGT 198Gly Ser Leu Thr Leu Ser Cys Ala Thr Ser Gl - #y Phe Thr Phe Ser Ser# 30- TAT GCC TTT TCT TGG GTC CGC CAG ACC TCA GA - #C AAG AGT CTG GAG TGG 246Tyr Ala Phe Ser Trp Val Arg Gln Thr Ser As - #p Lys Ser Leu Glu Trp# 45- GTC GCA ACC ATC AGT AGT ACT GAT ACT TAT AC - #C TAT TAT TCA GAC AAT 294Val Ala Thr Ile Ser Ser Thr Asp Thr Tyr Th - #r Tyr Tyr Ser Asp Asn# 60- GTG AAG GGG CGC TTC ACC ATC TCC AGA GAC AA - #T GGC AAG AAC ACC CTG 342Val Lys Gly Arg Phe Thr Ile Ser Arg Asp As - #n Gly Lys Asn Thr Leu# 75- TAC CTG CAA ATG AGC AGT CTG AAG TCT GAG GA - #C ACA GCC GTG TAT TAC 390Tyr Leu Gln Met Ser Ser Leu Lys Ser Glu As - #p Thr Ala Val Tyr Tyr#95- TGT GCA AGA CAT GGG TAC TAT GGT AAA GGC TA - #T TTT GAC TAC TGG GGC 438Cys Ala Arg His Gly Tyr Tyr Gly Lys Gly Ty - #r Phe Asp Tyr Trp Gly# 110- CAA GGG ACC ACG GTC ACC GTC TCC TCA GGT GG - #A GGC GGT TCA GGC GGA 486Gln Gly Thr Thr Val Thr Val Ser Ser Gly Gl - #y Gly Gly Ser Gly Gly# 125- GGT GGC TCT GGC GGT GGC GGA TCG GCC GGT TC - #G GCC CAG GTC CAG CTG 534Gly Gly Ser Gly Gly Gly Gly Ser Ala Gly Se - #r Ala Gln Val Gln Leu# 140- CAA CAG TCA GGA CCT GAG CTG GTA AAG CCT GG - #G GCT TCA GTG AAG ATG 582Gln Gln Ser Gly Pro Glu Leu Val Lys Pro Gl - #y Ala Ser Val Lys Met# 155- TCC TGC AAG GCT TCT GGA TAC ACA TTC ACT AG - #C TAT GTT ATG CAC TGG 630Ser Cys Lys Ala Ser Gly Tyr Thr Phe Thr Se - #r Tyr Val Met His Trp160 1 - #65 1 - #70 1 -#75- GTG AAA CAG AAG CCT GGG CAG GGC CTT GAG TG - #G ATT GGA TAT ATT TAT 678Val Lys Gln Lys Pro Gly Gln Gly Leu Glu Tr - #p Ile Gly Tyr Ile Tyr# 190- CCT TAC AAT GAT GGT ACT AAG TAC AAT GAG AA - #G TTC AAA GGC AAG GCC 726Pro Tyr Asn Asp Gly Thr Lys Tyr Asn Glu Ly - #s Phe Lys Gly Lys Ala# 205- ACA CTG ACT TCA GAC AAA TCC TCC AGC ACA GC - #C TAC ATG GAG CTC AGC 774Thr Leu Thr Ser Asp Lys Ser Ser Ser Thr Al - #a Tyr Met Glu Leu Ser# 220- AGC CTG ACC TCT GAG GAC TCT GCG GTC TAT TA - #C TGT TCA AGA CGC TTT 822Ser Leu Thr Ser Glu Asp Ser Ala Val Tyr Ty - #r Cys Ser Arg Arg Phe# 235- GAC TAC TGG GGC CAA GGG ACC ACC GTC ACC GT - #C TCC TCA TAA# 864Asp Tyr Trp Gly Gln Gly Thr Thr Val Thr Va - #l Ser Ser240 2 - #45 2 - #50#AAA TAC 921CTGCATG CAAATTCTAT TTCAAGGAGA CAGTCATA ATG# Met - # Lys Tyr20 - #- CTA TTG CCT ACG GCA GCC GCT GGA TTG TTA TT - #A CTC GCT GCC CAA CCA 969Leu Leu Pro Thr Ala Ala Ala Gly Leu Leu Le - #u Leu Ala Ala Gln Pro5- GCG ATG GCC GAC ATC GAG CTC ACC CAG TCT CC - #A TCT TCC ATG TAT GCA1017Ala Met Ala Asp Ile Glu Leu Thr Gln Ser Pr - #o Ser Ser Met Tyr Ala# 10- TCT CTA GGA GAG AGA ATC ACT ATC ACT TGC AA - #G GCG AGT CAG GAC ATT1065Ser Leu Gly Glu Arg Ile Thr Ile Thr Cys Ly - #s Ala Ser Gln Asp Ile# 25- AAT ACC TAT TTA ACC TGG TTC CAG CAG AAA CC - #A GGG AAA TCT CCC AAG1113Asn Thr Tyr Leu Thr Trp Phe Gln Gln Lys Pr - #o Gly Lys Ser Pro Lys#45- ACC CTG ATC TAT CGT GCA AAC AGA TTG CTA GA - #T GGG GTC CCA TCA AGG1161Thr Leu Ile Tyr Arg Ala Asn Arg Leu Leu As - #p Gly Val Pro Ser Arg# 60- TTC AGT GGC AGT GGA TCT GGG CAA GAT TAT TC - #T CTC ACC ATC AGC AGC1209Phe Ser Gly Ser Gly Ser Gly Gln Asp Tyr Se - #r Leu Thr Ile Ser Ser# 75- CTG GAC TAT GAA GAT ATG GGA ATT TAT TAT TG - #T CTA CAA TAT GAT GAG1257Leu Asp Tyr Glu Asp Met Gly Ile Tyr Tyr Cy - #s Leu Gln Tyr Asp Glu# 90- TTG TAC ACG TTC GGA GGG GGG ACC AAG CTC GA - #G ATC AAA CGG GGT GGA1305Leu Tyr Thr Phe Gly Gly Gly Thr Lys Leu Gl - #u Ile Lys Arg Gly Gly# 105- GGC GGT TCA GGC GGA GGT GGC TCT GGC GGT GG - #C GGA GTC GAC ATC GAA1353Gly Gly Ser Gly Gly Gly Gly Ser Gly Gly Gl - #y Gly Val Asp Ile Glu110 1 - #15 1 - #20 1 -#25- CTC ACT CAG TCT CCA TTC TCC CTG ACT GTG AC - #A GCA GGA GAG AAG GTC1401Leu Thr Gln Ser Pro Phe Ser Leu Thr Val Th - #r Ala Gly Glu Lys Val# 140- ACT ATG AAT TGC AAG TCC GGT CAG AGT CTG TT - #A AAC AGT GTA AAT CAG1449Thr Met Asn Cys Lys Ser Gly Gln Ser Leu Le - #u Asn Ser Val Asn Gln# 155- AGG AAC TAC TTG ACC TGG TAC CAG CAG AAG CC - #A GGG CAG CCT CCT AAA1497Arg Asn Tyr Leu Thr Trp Tyr Gln Gln Lys Pr - #o Gly Gln Pro Pro Lys# 170- CTG TTG ATC TAC TGG GCA TCC ACT AGG GAA TC - #T GGA GTC CCT GAT CGC1545Leu Leu Ile Tyr Trp Ala Ser Thr Arg Glu Se - #r Gly Val Pro Asp Arg# 185- TTC ACA GCC AGT GGA TCT GGA ACA GAT TTC AC - #T CTC ACC ATC AGC AGT1593Phe Thr Ala Ser Gly Ser Gly Thr Asp Phe Th - #r Leu Thr Ile Ser Ser190 1 - #95 2 - #00 2 -#05- GTG CAG GCT GAA GAC CTG GCA GTT TAT TAC TG - #T CAG AAT GAT TAT ACT1641Val Gln Ala Glu Asp Leu Ala Val Tyr Tyr Cy - #s Gln Asn Asp Tyr Thr# 220- TAT CCG TTC ACG TTC GGA GGG GGG ACC AAG CT - #C GAA ATC AAA CGG TAA1689Tyr Pro Phe Thr Phe Gly Gly Gly Thr Lys Le - #u Glu Ile Lys Arg# 235# 1706 C- (2) INFORMATION FOR SEQ ID NO: 12:- (i) SEQUENCE CHARACTERISTICS:#acids (A) LENGTH: 274 amino (B) TYPE: amino acid (D) TOPOLOGY: linear- (ii) MOLECULE TYPE: protein#12: (xi) SEQUENCE DESCRIPTION: SEQ ID NO:- Met Lys Tyr Leu Leu Pro Thr Ala Ala Ala Gl - #y Leu Leu Leu Leu Ala10- Ala Gln Pro Ala Met Ala Gln Val Gln Leu Gl - #n Glu Ser Gly Gly Asp# 10- Leu Val Lys Pro Gly Gly Ser Leu Thr Leu Se - #r Cys Ala Thr Ser Gly# 25- Phe Thr Phe Ser Ser Tyr Ala Phe Ser Trp Va - #l Arg Gln Thr Ser Asp# 40- Lys Ser Leu Glu Trp Val Ala Thr Ile Ser Se - #r Thr Asp Thr Tyr Thr# 55- Tyr Tyr Ser Asp Asn Val Lys Gly Arg Phe Th - #r Ile Ser Arg Asp Asn# 70- Gly Lys Asn Thr Leu Tyr Leu Gln Met Ser Se - #r Leu Lys Ser Glu Asp#90- Thr Ala Val Tyr Tyr Cys Ala Arg His Gly Ty - #r Tyr Gly Lys Gly Tyr# 105- Phe Asp Tyr Trp Gly Gln Gly Thr Thr Val Th - #r Val Ser Ser Gly Gly# 120- Gly Gly Ser Gly Gly Gly Gly Ser Gly Gly Gl - #y Gly Ser Ala Gly Ser# 135- Ala Gln Val Gln Leu Gln Gln Ser Gly Pro Gl - #u Leu Val Lys Pro Gly# 150- Ala Ser Val Lys Met Ser Cys Lys Ala Ser Gl - #y Tyr Thr Phe Thr Ser155 1 - #60 1 - #65 1 -#70- Tyr Val Met His Trp Val Lys Gln Lys Pro Gl - #y Gln Gly Leu Glu Trp# 185- Ile Gly Tyr Ile Tyr Pro Tyr Asn Asp Gly Th - #r Lys Tyr Asn Glu Lys# 200- Phe Lys Gly Lys Ala Thr Leu Thr Ser Asp Ly - #s Ser Ser Ser Thr Ala# 215- Tyr Met Glu Leu Ser Ser Leu Thr Ser Glu As - #p Ser Ala Val Tyr Tyr# 230- Cys Ser Arg Arg Phe Asp Tyr Trp Gly Gln Gl - #y Thr Thr Val Thr Val235 2 - #40 2 - #45 2 -#50- Ser Ser- (2) INFORMATION FOR SEQ ID NO: 13:- (i) SEQUENCE CHARACTERISTICS:#acids (A) LENGTH: 258 amino (B) TYPE: amino acid (D) TOPOLOGY: linear- (ii) MOLECULE TYPE: protein#13: (xi) SEQUENCE DESCRIPTION: SEQ ID NO:- Met Lys Tyr Leu Leu Pro Thr Ala Ala Ala Gl - #y Leu Leu Leu Leu Ala10- Ala Gln Pro Ala Met Ala Asp Ile Glu Leu Th - #r Gln Ser Pro Ser Ser# 10- Met Tyr Ala Ser Leu Gly Glu Arg Ile Thr Il - #e Thr Cys Lys Ala Ser# 25- Gln Asp Ile Asn Thr Tyr Leu Thr Trp Phe Gl - #n Gln Lys Pro Gly Lys# 40- Ser Pro Lys Thr Leu Ile Tyr Arg Ala Asn Ar - #g Leu Leu Asp Gly Val# 55- Pro Ser Arg Phe Ser Gly Ser Gly Ser Gly Gl - #n Asp Tyr Ser Leu Thr# 70- Ile Ser Ser Leu Asp Tyr Glu Asp Met Gly Il - #e Tyr Tyr Cys Leu Gln#90- Tyr Asp Glu Leu Tyr Thr Phe Gly Gly Gly Th - #r Lys Leu Glu Ile Lys# 105- Arg Gly Gly Gly Gly Ser Gly Gly Gly Gly Se - #r Gly Gly Gly Gly Val# 120- Asp Ile Glu Leu Thr Gln Ser Pro Phe Ser Le - #u Thr Val Thr Ala Gly# 135- Glu Lys Val Thr Met Asn Cys Lys Ser Gly Gl - #n Ser Leu Leu Asn Ser# 150- Val Asn Gln Arg Asn Tyr Leu Thr Trp Tyr Gl - #n Gln Lys Pro Gly Gln155 1 - #60 1 - #65 1 -#70- Pro Pro Lys Leu Leu Ile Tyr Trp Ala Ser Th - #r Arg Glu Ser Gly Val# 185- Pro Asp Arg Phe Thr Ala Ser Gly Ser Gly Th - #r Asp Phe Thr Leu Thr# 200- Ile Ser Ser Val Gln Ala Glu Asp Leu Ala Va - #l Tyr Tyr Cys Gln Asn# 215- Asp Tyr Thr Tyr Pro Phe Thr Phe Gly Gly Gl - #y Thr Lys Leu Glu Ile# 230- Lys Arg235- (2) INFORMATION FOR SEQ ID NO: 14:- (i) SEQUENCE CHARACTERISTICS:#pairs (A) LENGTH: 25 base (B) TYPE: nucleic acid (C) STRANDEDNESS: single (D) TOPOLOGY: linear- (ii) MOLECULE TYPE: other nucleic acid#= "synthetic DNA"RIPTION: /desc- (vii) IMMEDIATE SOURCE: (B) CLONE: primer DBL.1#14: (xi) SEQUENCE DESCRIPTION: SEQ ID NO:# 25 AATG GCAAG- (2) INFORMATION FOR SEQ ID NO: 15:- (i) SEQUENCE CHARACTERISTICS:#pairs (A) LENGTH: 45 base (B) TYPE: nucleic acid (C) STRANDEDNESS: single (D) TOPOLOGY: linear- (ii) MOLECULE TYPE: other nucleic acid#= "synthetic DNA"RIPTION: /desc- (vii) IMMEDIATE SOURCE: (B) CLONE: primer DBL.2#15: (xi) SEQUENCE DESCRIPTION: SEQ ID NO:#45 GAAC CGGCCGATCC GCCACCGCCA GAGCC- (2) INFORMATION FOR SEQ ID NO: 16:- (i) SEQUENCE CHARACTERISTICS:#pairs (A) LENGTH: 45 base (B) TYPE: nucleic acid (C) STRANDEDNESS: single (D) TOPOLOGY: linear- (ii) MOLECULE TYPE: other nucleic acid#= "synthetic DNA"RIPTION: /desc- (vii) IMMEDIATE SOURCE: (B) CLONE: primer DBL.3#16: (xi) SEQUENCE DESCRIPTION: SEQ ID NO:#45 CGGC CCAGGTCCAG CTGCAACAGT CAGGA- (2) INFORMATION FOR SEQ ID NO: 17:- (i) SEQUENCE CHARACTERISTICS:#pairs (A) LENGTH: 53 base (B) TYPE: nucleic acid (C) STRANDEDNESS: single (D) TOPOLOGY: linear- (ii) MOLECULE TYPE: other nucleic acid#= "synthetic DNA"RIPTION: /desc- (vii) IMMEDIATE SOURCE: (B) CLONE: primer DBL.4#17: (xi) SEQUENCE DESCRIPTION: SEQ ID NO:- CTACATGAAT TCGCTAGCTT ATTATGAGGA GACGGTGACG GTGGTCCCTT GG - #C 53- (2) INFORMATION FOR SEQ ID NO: 18:- (i) SEQUENCE CHARACTERISTICS:#pairs (A) LENGTH: 36 base (B) TYPE: nucleic acid (C) STRANDEDNESS: single (D) TOPOLOGY: linear- (ii) MOLECULE TYPE: other nucleic acid#= "synthetic DNA"RIPTION: /desc- (vii) IMMEDIATE SOURCE: (B) CLONE: primer DBL.5#18: (xi) SEQUENCE DESCRIPTION: SEQ ID NO:# 36 CTGC ATGCAAATTC TATTTC- (2) INFORMATION FOR SEQ ID NO: 19:- (i) SEQUENCE CHARACTERISTICS:#pairs (A) LENGTH: 23 base (B) TYPE: nucleic acid (C) STRANDEDNESS: single (D) TOPOLOGY: linear- (ii) MOLECULE TYPE: other nucleic acid#= "synthetic DNA"RIPTION: /desc- (vii) IMMEDIATE SOURCE: (B) CLONE: primer DBL.6#19: (xi) SEQUENCE DESCRIPTION: SEQ ID NO:# 23AACG GGG- (2) INFORMATION FOR SEQ ID NO: 20:- (i) SEQUENCE CHARACTERISTICS:#pairs (A) LENGTH: 36 base (B) TYPE: nucleic acid (C) STRANDEDNESS: single (D) TOPOLOGY: linear- (ii) MOLECULE TYPE: other nucleic acid#= "synthetic DNA"RIPTION: /desc- (vii) IMMEDIATE SOURCE: (B) CLONE: primer DBL.7#20: (xi) SEQUENCE DESCRIPTION: SEQ ID NO:# 36 ACTC CGCCACCGCC AGAGCC- (2) INFORMATION FOR SEQ ID NO: 21:- (i) SEQUENCE CHARACTERISTICS:#pairs (A) LENGTH: 39 base (B) TYPE: nucleic acid (C) STRANDEDNESS: single (D) TOPOLOGY: linear- (ii) MOLECULE TYPE: other nucleic acid#= synthetic DNA"CRIPTION: /desc- (vii) IMMEDIATE SOURCE: (B) CLONE: primer DBL.8#21: (xi) SEQUENCE DESCRIPTION: SEQ ID NO:# 39 AACT CACTCAGTCT CCATTCTCC- (2) INFORMATION FOR SEQ ID NO: 22:- (i) SEQUENCE CHARACTERISTICS:#pairs (A) LENGTH: 50 base (B) TYPE: nucleic acid (C) STRANDEDNESS: single (D) TOPOLOGY: linear- (ii) MOLECULE TYPE: other nucleic acid#= "synthetic DNA"RIPTION: /desc- (vii) IMMEDIATE SOURCE: (B) CLONE: primer DBL.9#22: (xi) SEQUENCE DESCRIPTION: SEQ ID NO:# 50GGCCGC TTATTACCGT TTGATTTCGA GCTTGGTCCC- (2) INFORMATION FOR SEQ ID NO: 23:- (i) SEQUENCE CHARACTERISTICS:#pairs (A) LENGTH: 41 base (B) TYPE: nucleic acid (C) STRANDEDNESS: single (D) TOPOLOGY: linear- (ii) MOLECULE TYPE: other nucleic acid#= "synthetic DNA"RIPTION: /desc- (vii) IMMEDIATE SOURCE: (B) CLONE: primer DBL.1 - #0#23: (xi) SEQUENCE DESCRIPTION: SEQ ID NO:# 41 CTCC TCACAGGTCC AGTTGCAACA G- (2) INFORMATION FOR SEQ ID NO: 24:- (i) SEQUENCE CHARACTERISTICS:#pairs (A) LENGTH: 44 base (B) TYPE: nucleic acid (C) STRANDEDNESS: single (D) TOPOLOGY: linear- (ii) MOLECULE TYPE: other nucleic acid#= "synthetic DNA"RIPTION: /desc- (vii) IMMEDIATE SOURCE: (B) CLONE: primer DBL.1 - #1#24: (xi) SEQUENCE DESCRIPTION: SEQ ID NO:# 44 AACG GGACATCGAA CTCACTCAGT CTCC- (2) INFORMATION FOR SEQ ID NO: 25:- (i) SEQUENCE CHARACTERISTICS:#pairs (A) LENGTH: 41 base (B) TYPE: nucleic acid (C) STRANDEDNESS: single (D) TOPOLOGY: linear- (ii) MOLECULE TYPE: other nucleic acid#= "synthetic DNA"RIPTION: /desc- (vii) IMMEDIATE SOURCE: (B) CLONE: primer DBL.1 - #2#25: (xi) SEQUENCE DESCRIPTION: SEQ ID NO:# 41 CTCC TCACAGGTGC AGTTGCAGGA G- (2) INFORMATION FOR SEQ ID NO: 26:- (i) SEQUENCE CHARACTERISTICS:#pairs (A) LENGTH: 22 base (B) TYPE: nucleic acid (C) STRANDEDNESS: single (D) TOPOLOGY: linear- (ii) MOLECULE TYPE: other nucleic acid#= "synthetic DNA"RIPTION: /desc- (vii) IMMEDIATE SOURCE: (B) CLONE: primer PCR.5 - #1#26: (xi) SEQUENCE DESCRIPTION: SEQ ID NO:# 22TCW GG- (2) INFORMATION FOR SEQ ID NO: 27:- (i) SEQUENCE CHARACTERISTICS:#pairs (A) LENGTH: 32 base (B) TYPE: nucleic acid (C) STRANDEDNESS: single (D) TOPOLOGY: linear- (ii) MOLECULE TYPE: other nucleic acid#= "synthetic DNA"RIPTION: /desc- (vii) IMMEDIATE SOURCE: (B) CLONE: primer PCR.8 - #9#27: (xi) SEQUENCE DESCRIPTION: SEQ ID NO:# 32 GTGG TCCCTTGGCC CC- (2) INFORMATION FOR SEQ ID NO: 28:- (i) SEQUENCE CHARACTERISTICS:#pairs (A) LENGTH: 24 base (B) TYPE: nucleic acid (C) STRANDEDNESS: single (D) TOPOLOGY: linear- (ii) MOLECULE TYPE: other nucleic acid#= "synthetic DNA"RIPTION: /desc- (vii) IMMEDIATE SOURCE: (B) CLONE: primer PCR.9 - #0#28: (xi) SEQUENCE DESCRIPTION: SEQ ID NO:# 24AGTC TCCA- (2) INFORMATION FOR SEQ ID NO: 29:- (i) SEQUENCE CHARACTERISTICS:#pairs (A) LENGTH: 22 base (B) TYPE: nucleic acid (C) STRANDEDNESS: single (D) TOPOLOGY: linear- (ii) MOLECULE TYPE: other nucleic acid#= "synthetic DNA"RIPTION: /desc- (vii) IMMEDIATE SOURCE: (B) CLONE: primer PCR.1 - #16#29: (xi) SEQUENCE DESCRIPTION: SEQ ID NO:# 22GTC CC- (2) INFORMATION FOR SEQ ID NO: 30:- (i) SEQUENCE CHARACTERISTICS:#acids (A) LENGTH: 13 amino (B) TYPE: amino acid (D) TOPOLOGY: linear- (ii) MOLECULE TYPE: protein#30: (xi) SEQUENCE DESCRIPTION: SEQ ID NO:- Thr Thr Val Thr Val Ser Ser Gln Val Gln Le - #u Gln Gln# 10- (2) INFORMATION FOR SEQ ID NO: 31:- (i) SEQUENCE CHARACTERISTICS:#acids (A) LENGTH: 12 amino (B) TYPE: amino acid (D) TOPOLOGY: linear- (ii) MOLECULE TYPE: protein#31: (xi) SEQUENCE DESCRIPTION: SEQ ID NO:- Lys Leu Glu Ile Lys Arg Asp Ile Glu Leu Th - #r Gln# 10__________________________________________________________________________
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A bispecific or bivalent double head antibody fragment, which is composed of a binding complex containing two polypeptide chains, whereby one polypeptide chain has two times a variable domain of a heavy chain (V H ) in series and the other polypeptide chain has two times a variable domain of a light chain (V L ) in series, and the binding complex contains two pairs of variable domains (V H -A//V L -A and V H -B//V L -B), wherein said double head antibody fragments have binfunctional antigen binding activity. A process for producing such an antibody fragment is disclosed. An immunoassay is also provided for, wherein the improvement is the inclusion of a bispecific or bivalent double head antibody fragment, which is composed of a binding complex containing two polypeptide chains, whereby one polypeptide chain has two times a variable domain of a heavy chain (V H ) in series and the other polypeptide chain has two times a variable domain of a light chain (V L ) in series, as a binding means.
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BACKGROUND
[0001] The present invention relates in general to pulse generators. More specifically, the present invention relates to bipolar pulse generators that provide a high power/energy pulse on a load.
[0002] Recent trends in the development of pulse power microwave sources for a variety of applications have been directed to increasing power, efficiency and energy on the load. Transmission line pulse generators with different kinds of fast switches, including light activated photoconductors, can achieve some of the best results in generating high power short duration pulses. For a given limited charging voltage of transmission lines defined by high-current switches, high powered and high energy density transmission lines imply low characteristic impedances. This low range of characteristic impedances, however, frequently causes problems for coupling with typically used load impedances, 50 ohm or higher, for example, radiating impedances, which introduces a problem with efficient high ratio impedance transformation.
[0003] Bipolar pulse generators very often have significant advantages compared to unipolar pulse generators, with just one example being UWB radiation. Further, there are many potential applications of bipolar pulse generators, for example in industry, physics and medicine, where very often bipolar pulse generators with time separation between positive and negative sub-pulses are preferable or required. Today, however, there are only various types of high power and high energy unipolar pulse generators (Marx generator and stacked Blumlein generator in various modifications).
[0004] For example, a high energy Marx generator with coaxial cable to provide rectangular unipolar pulse is known and described in “A PFN Marx Generator Based on High-Voltage Transmission Lines”, by S. M. Turnbull et al. presented in Meas. Sci. Technol. 11 (2000) N 51 -N 55 . Further, a stacked Blumlein generator with a single switch has been proposed in U.S. Pat. No. 2,769,101 issued to R. D. Drosd. This type of generator has been designed and presented in various publications including, for example, “Modeling of Wound Coaxial Blumlein Pulsers”, by Jose O. Rossi et al:, published in IEEE Transactions on Plasma Science”, Vol. 34, No. 5, October 2006, “Design of a 150 kV, 300A, 100 Hz Blumlein Coaxial Pulser for Long Pulse Operation”, presented in IEEE Transactions on Plasma Science”, Vol. 30, No. 5, October 2002. Still further, some modifications of stacked (cascade) Blumlein generators are presented in “A Combined High-Voltage, High-Energy Pulse Generator”, by S. J. MacGregor et al. published in “Meas. Sci. Technol” 5 (1994), pp. 1580-1582, and “A Novel HV Double Pulse Modulator”, published in “Meas. Sci. Technol” 5 (1994), pp. 1407-1408. Finally, another type of high-power generator, namely, a “Multi-Stage Blumlein” is proposed by J. Yampolsky in US Patent Application 2005/0174715 A1, 2005. The content of each of the above-reference documents is incorporated herein by reference. All of the above-referenced generators produce only a unipolar pulse and do not provide voltage (impedance) transformation, with the exception of the proposed multi-stage Blumlein disclosed in US Patent Application 2005/0174715A1, which provides moderate transformation but requires a substantial number of switching devices.
[0005] A transmission line “High-Voltage Pulses Generator” has also been described in U.S. Pat. No. 1,098,502 A1 issued to Bosamykin V. S. et al, 1996, which provides bipolar pulse by a single switch. However, the power/energy on load is much less compared to that provided by the above-mentioned unipolar generators. In addition, impedance transformation in the device is low.
[0006] The applicant has also previously described a transmission line in U.S. Patent Application 2007/0165839 A1 entitled “Bipolar Pulse Generators With Voltage Multiplication”, which provides a device with a single switch with all of the required voltage/impedance transformation. However, in a stacked configuration with several switches, the energy provided by this type of generator is less compared to the above mentioned Blumlein-based stacked unipolar generators with less number of switches.
[0007] Accordingly, there remains a need for a bipolar pulse generator solution based on voltage charged transmission lines, which provides high power and high energy. Further, there remains a need for high power/energy bipolar pulse generator, which can provide voltage/impedance transformation. Still further, there remains a need for a high power/energy bipolar pulse generator with pulse separation between positive and negative sub-pulses.
[0008] It would be desirable to provide a bipolar pulse generator that could meet all of the above needs while being implemented in a simple structure, preferably with a single switch, and preferably in a high efficiency design that has a relatively low total size, while still allowing simple access by fibers to a closing photoconductive switch that actuates the bipolar pulse generator.
SUMMARY OF THE INVENTION
[0009] The present invention provides a bipolar pulse generator that can be implemented in a simple structure while providing a high efficiency design having a relatively low total size and still allowing access by fibers used to control a photoconductive switch that activates the generator.
[0010] In a preferred embodiment of the invention, a bipolar pulse generator includes a stacked Blumlein generator structure with an additional transmission line connected to a load at its near end and short-circuited at its distal end. An extra transmission line is positioned between the Blumlein generator's structure and the load provides specified limited gap between positive and negative sub-pulses.
[0011] According to a further preferred embodiment of the present invention, the bipolar pulse generator further includes a bended Blumlein generator structure, in which an existing intrinsic “stray” transmission line is used to provide the bipolar pulse.
[0012] According to a still another embodiment of the present invention, the bipolar pulse generator consists of stepped transmission line with additional switches positioned between steps, which are charged by different voltages.
[0013] The bipolar pulse generator according to the invention generates high power/energy pulses in a compact design with access to fibers for activating photoconductor switches. Bipolar pulse generators according to the invention are useful for HPM generation, in particle accelerators and in other high voltage physical, industrial, medical and test instruments.
[0014] Other features, uses, advantages, embodiments, etc. of the invention will become apparent to those skilled in the art from the following detailed description of the preferred embodiments of the invention.
BRIEF DESCRIPTION OF THE DRAWINGS
[0015] The invention will be described with reference to certain preferred embodiments thereof along with the accompanying figures, wherein:
[0016] FIG. 1 depicts a schematic of classic n-stacked Blumlein pulse generator according to the prior art;
[0017] FIG. 2 depicts a schematic of double stacked bipolar pulse generator according to the prior art;
[0018] FIG. 3 depicts a schematic of two-step bipolar pulse generator as an expansion of the generator in FIG. 2 for impedance transformation according to the prior art;
[0019] FIG. 4 depicts a schematic of double Blumlein pulse generator according to the prior art;
[0020] FIG. 5 depicts a schematic of two series connected double Blumlein pulse generators according to the prior art;
[0021] FIG. 6 depicts a schematic of bipolar pulse generator with two switches positioned in first two successive steps according to the prior art;
[0022] FIG. 7 a depicts a schematic of transmission line Marx-based bipolar pulse generator according to an embodiment of the present invention;
[0023] FIG. 7 b depicts a pulse shape on the load of generator shown on FIG. 7 a;
[0024] FIG. 8 a depicts a schematic of an n-stacked Blumlein based bipolar pulse generator according to an embodiment of the present invention;
[0025] FIG. 8 b depicts a pulse shape on the load of generator shown on FIG. 8 a;
[0026] FIG. 9 depicts a schematic of a three-step, two-stacked Blumlein based bipolar pulse generator according to an embodiment of the present invention;
[0027] FIG. 10 depicts a table of normalized element's values of an N-step, two-stacked Blumlein-based bipolar pulse generators according to an embodiment of the present invention;
[0028] FIG. 11 a depicts a schematic of a double Blumlein-based bipolar pulse generator according to an embodiment of the present invention;
[0029] FIG. 11 b depicts a pulse form on the load for generator according to FIG. 11 a;
[0030] FIG. 12 a depicts a schematic of a double Blumlein-based bipolar pulse generator with their intrinsic transmission lines according to an embodiment of the present invention;
[0031] FIG. 12 b depicts a pulse form on the load for generator according to FIG. 12 a;
[0032] FIG. 13 a depicts a schematic of two series connected double Blumlein based bipolar pulse generators with their intrinsic transmission lines according to an embodiment of the present invention;
[0033] FIG. 13 b depicts a schematic of two series connected double Blumlein based bipolar pulse generators in case of neglecting of intrinsic transmission lines according to an embodiment of the present invention;
[0034] FIG. 14 depicts a schematic of a series connected N double Blumlein based bipolar pulse generators with their intrinsic transmission lines according to an embodiment of the present invention;
[0035] FIG. 15 a depicts a schematic of double single-stage bipolar pulse generator with their intrinsic transmission lines that provides a bipolar pulse without a gap between sub-pulses according to an embodiment of the present invention;
[0036] FIG. 15 b illustrates the pulse form on load for generator according to FIG. 15 a;
[0037] FIG. 16 depicts a schematic of series connected two single-stage double bipolar pulse generators with their intrinsic transmission lines according to an embodiment of the present invention;
[0038] FIG. 17 depicts a schematic of series connected two single-stage, double bipolar pulse generators without (neglecting) their intrinsic transmission lines according to an embodiment of the present invention;
[0039] FIG. 18 a depicts a schematic of two-step, double bipolar pulse generators with their intrinsic transmission lines according to an embodiment of the present invention;
[0040] FIG. 18 b illustrates the pulse form on the load provided by the generator according to FIG. 18 a;
[0041] FIG. 19 depicts a schematic of three-step bipolar pulse generator with two switches in first two successive steps and with the gap between sub-pulses equal to the length of sub-pulse as an embodiment of the present invention;
[0042] FIG. 20 illustrate the table of multi-steps bipolar pulse generators with two switches in first two successive steps and with the gap between sub-pulses equal to the length of sub-pulse according to an embodiment of the present invention;
[0043] FIG. 21 a depicts a totally folded design of N-step bipolar pulse generator with two switches in first two successive steps and with the gap between sub-pulses equal to the length of sub-pulse according to an embodiment of the present invention; and
[0044] FIG. 21 b depicts a partial-folded design of N-step bipolar pulse generator with two switches in first two successive steps and with the gap between sub-pulses equal to the length of sub-pulse according to an embodiment of the present invention
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0045] FIG. 1 depicts a well-known stacked Blumlein pulse Generator that provides a high-energy unipolar pulse on a matched load. FIG. 2 depicts a schematic of a prior art double stacked bipolar pulse generator of the type described in US Patent Application 2007/0165839 A1. The stored energy and the energy on the load, however, is 75% of the energy provided by double stacked (n=2) unipolar generator presented on FIG. 1 . FIG. 3 depicts a schematic of a prior art bipolar pulse generator, which is an extended type of generator shown in FIG. 2 with and additional impedance transformation step. FIG. 4 depicts a schematic of a prior art unipolar pulse generator, which is a double Blumlein pulse generator (with interconnected open-circuited charged transmission lines) presented by S. J. MacGregor et al. discussed above. FIG. 5 depicts a schematic of a prior art unipolar pulse generator, which is two series connected double Blumlein pulse generators (with interconnected open-circuited charged transmission lines) presented by S. J. MacGregor et al. discussed above. FIG. 6 depicts a schematic of a prior art bipolar pulse generator with two switches in first two successive steps presented in US 2007/0165839 A1. The power/energy of the generating pulse is not a maximum that could be achieved in similar structure with two switches positioned in first two successive steps. The invention will be described in part with reference to prior art structures such as those discussed above.
[0046] FIG. 7 a is a schematic of Marx-based transmission line bipolar pulse generator according to an embodiment of the present invention. The generator may consist of any number (n) of identically charged transmission lines 10 . Each transmission line 10 is connected to a corresponding individual switch 11 and to a corresponding individual charging element 12 (resistor R or inductance L). Instead of typical direct connection to the load 15 , the load 15 is connected through an additional transmission line 13 of a specified length. In addition, a transmission line 14 is connected to the load 15 at its near end and is short-circuited at its distal end. The electrical length of the transmission line 14 is equal to the sum of length of each charged line 10 and the length of line 13 . The described arrangement provides a specified gap between positive and negative sub-pulses that is equal double the transit time of transmission line 13 .
[0047] In operation, all of the charged transmission lines 10 are charged by their individual charging element 12 . Once all the charged transmission lines 10 are fully charged, all of the switches 11 are closed at the same moment of time, thereby causing the charged transmission lines 10 to operate as n series connected generators. As a result, a bipolar pulse with a predicted time space or gap between positive and negative sub-pulses is realized on the load 15 as is illustrated in FIG. 7 b.
[0048] FIG. 8 a is a schematic of a stacked Blumlein-based bipolar pulse generator according to an embodiment of the present invention. The generator consists of a charging structure 30 with any number n of identically first charged transmission lines 31 with switches at their near ends, and n oppositely charged second transmission lines 32 with the same length and characteristic impedances as for the first transmission lines 31 . The output of this stacked Blumlein structure 30 is connected to the near end of an additional non-charged transmission line 33 with a specified electrical length t 1 and characteristic impedance equal to 2 n Z 0 , where Z 0 is a characteristic impedance of each charged first transmission lines 31 and the second transmission lines 32 . The load 34 is connected to the distal end of the transmission line 33 . In addition, another transmission line 35 is provided, which is connected to the load 34 at its near end and is short-circuited at its distal end. The load impedance is equal to nZ 0 , while the characteristic impedance of transmission line 35 is the same as for transmission line 33 . The electrical length of the transmission line 35 is equal 2 t +t 1 , where t is electrical length of each of the first transmission lines 31 and the second transmission lines 32 .
[0049] During operation, all the transmission lines 31 and the transmission lines 32 are charged by a voltage supply V 0 . All of the n switches are then closed simultaneously and a wave propagation process occurs. Identical waves propagate on all of the charged transmission lines 31 and the same is true for all of the charged transmission lines 32 . The resulting pulse on the load is illustrated on FIG. 8 b and minimum separation between sub-pulses is equal 2 t.
[0050] Referring to FIG. 9 , a schematic of a three-step two stacked Blumlein based bipolar pulse generator according to an embodiment of the invention is illustrated. The generator starts from a generator according to FIG. 8 a for particular case n=2 (transmission lines 41 and transmission lines 42 ) and t 1 =0. Extra step transmission lines 43 and 44 are provided as well as a transmission line 45 with specific characteristic impedances, obtained by impedance transformation procedure applied to initial circuit ( FIG. 8 a for n=2 and t 1 =0). This provides additional impedance/voltage transformation. The charged structure 40 of this generator consists of transmission lines 41 , 42 , 43 , 44 and 45 . Load 46 is positioned between charged transmission line structure 40 and a transmission line 47 that is connected to the load 46 and short-circuited at its distal end. The bipolar pulse is initiated by simultaneously closing two switches 48 .
[0051] FIG. 10 is a table of normalized characteristic impedances of transmission lines as well as load impedances for odd numbers of steps 1 , 3 , 5 . . . 19 . The table illustrates the rate of increasing impedance transformation by increasing the number of steps. The pulse form is independent on the number of steps. Only the magnitude of pulse is increased from step to step.
[0052] FIG. 11 a is a schematic of a double Blumlein based bipolar pulse generator according to an embodiment of the present invention. This generator consists of a known double Blumlein unipolar pulse generator structure (transmission lines 60 , 61 , 62 and switch 63 ) with additional transmission lines 64 and 65 . A transmission line 64 with time delay t 1 is connected between the output of the double Blumlein unipolar pulse generator structure and a load 66 . Transmission line 65 is connected to the load 66 at its near end and is short-circuited at its distal end. A characteristic impedance of the transmission lines 64 , 65 is twice the impedance of the load 66 and four times more then the impedance of each of the transmission lines 60 , 61 or 62 . The electrical length of the transmission line 65 is twice the length of transmission lines 60 or 61 and is equal to the length of transmission line 62 . Line 62 could also be separated in the middle by two identical length transmission lines without any change in operation and in pulse form on the load 66 .
[0053] Ideal operation of this generator is similar to that for generator according to FIG. 8 a when the number of switches equal two (n=2). The resulting pulse form on the load 66 is illustrated on FIG. 11 b . The ideal operation of the generator according to FIG. 11 a assumes that there are no inductances by outer conductors, or more correctly, no transmission lines associated by outer conductors of transmission lines 60 and 61 , i.e. between nodes a 1 and a 2 , as well as between nodes a 1 and b 1 by outer conductors of transmission line 62 . However, between these nodes, there always exists intrinsic (stray) transmission lines short-circuited at their distant ends in practice. These transmission lines with specific characteristic impedances and electrical length could be used instead of transmission line 65 (or in addition to transmission line 65 with increased characteristic impedance) to provide a bipolar pulse. However, it is valid only for the case t 1 =0 and illustrated on FIG. 12 a.
[0054] Referring to FIG. 12 a , which is a schematic of double Blumlein-based Bipolar Pulse generator as an embodiment of the present invention. This generator consists of known double Blumlein unipolar pulse generator structure with transmission lines 70 , 71 , 72 and switch 73 . This structure is similar to the structure with transmission lines 60 , 61 , 62 and switch 63 of FIG. 11 a . However, instead of using transmission line 65 with time delay 2 t (t 1 =0), which is short-circuited at its distal end, there are two intrinsic transmission lines 74 and 75 formed by outer conductors of transmission lines 70 , 71 and by a folded outer conductor of transmission line 72 . Transmission lines 74 and 75 are connected in series relative to load 76 with resulting characteristic impedance equal to 4 Z and operate in the same manner as the transmission line 64 of FIG. 11 a . The electrical length of each of these lines should also be equal to 2 t.
[0055] It should be noted that combined design of FIG. 11 a for t 1 =0 and FIG. 12 a is also possible. Accordingly, in addition to the two intrinsic transmission lines 74 and 75 of FIG. 12 a (with impedances more then 2 Z each), the transmission line 65 of FIG. 11 a with characteristic impedance more then 4 Z could be used.
[0056] FIG. 13 a is a schematic of a series connected two double Blumlein based bipolar pulse generators according to an embodiment of the present invention. This generator consists of a double Blumlein-based bipolar pulse generator's structure (transmission lines 80 , 81 , 84 , 86 and 88 ), which is the same as the generator on FIG. 12 a and it is connected in series with exactly the same generator's structure (transmission lines 82 , 83 , 85 , 87 and 89 ). Both switches 91 and 92 should be closed simultaneously. These two switches could be replaced by a single switch or by any number of simultaneously closed switches. It should be noted that intrinsic transmission lines 86 , 87 , 88 and 89 (if they are neglected) could be replaced by a single (or two) transmission line(s) as shown in FIG. 13 b (transmission line 95 or transmission lines 94 and 95 if t 1 >0). In the case of two lines, transmission line 94 with time delay t 1 provides an additional 2 t 1 separation between sub-pulses, i.e. total time separation 2 ( t +t 1 ) could be implemented. Any negative effect by the intrinsic transmission lines can be minimized by proper design.
[0057] FIG. 14 is a schematic of series connected N double Blumlein based bipolar pulse generator according to an embodiment of the present invention. This generator consists of double Blumlein-based bipolar pulse generator structure (transmission lines 100 , 101 , 106 , 109 and 112 ), which is the same as generator in FIG. 12 a and is connected in series with exactly the same generator structure (transmission lines 102 , 103 , 107 , 110 and 113 ). This second double Blumlein-based bipolar pulse generator structure is also connected in series with the next the same generator structure and finally with the last N-th generator structure (lines 104 , 105 , 108 , 111 and 114 ). All simultaneously closed N switches 116 , 117 . . . 118 could be replaced by a single switch or by any number of switches. The load 115 is a result of series connection matched loads of individual double Blumlein-based Bipolar Pulse Generators with their summarized impedance 2 NZ.
[0058] By analogy with the generators shown in FIG. 13 a and FIG. 13 b , all of the intrinsic transmission lines 109 , 110 , . . . 111 and 112 , 113 , . . . 114 could be replaced by a single line connected to the load 115 at its near end and short-circuited at its distal end, which is similar to transmission line 95 ( FIG. 13 b ) when t 1 =0. For an extended gap between sub-pulses (t 1 >0), an additional transmission line as transmission line 94 in FIG. 13 b should be used. If various combined solutions for short-circuited at their distal end transmission line and intrinsic lines as discussed above with respect to FIGS. 11 a , 12 a and FIG. 13 a , could be used depending on specific designs issues. It should be noted for all generators shown in FIGS. 11 a , 12 a , 13 a and 14 , various positions of ground connections can be used including single ground or no connections to ground.
[0059] FIG. 15 a is a schematic of double single-stage bipolar pulse generator according to an embodiment of the present invention. By analogy with the double Blumlein-based bipolar pulse generators according to FIG. 12 a , this generator is obtained by interconnection of two bipolar pulse generators. However, in this case there is no gap between positive and negative sub-pulses. Two switched transmission lines 120 and 121 are combined with a single switch 126 and a single non-switched transmission line 122 is provided with double length 2 t . Two intrinsic equal-length transmission lines 123 and 124 with impedances Z 2 and Z 1 , respectively, are provided. For this generator, no connections to ground or different ground connections, including shown on FIG. 15 a , could be used. Independent on connections to ground, different combinations of characteristic impedances Z 1 and Z 2 without deterioration of the generating pulse are acceptable. Assuming Z=1 (normalization) some of these combinations are presented in Table 1 below.
[0000]
TABLE 1
Z1 (Z2)
8
7
6
5
4
3
2.5
2
Z2 (Z1)
8
9.2
11
14
20
38
74
∞
[0060] FIG. 15 b illustrates pulse shape on the load 125 independent on values Z 1 and Z 2 . In the case when Z 1 and Z 2 are very high (Z 1 , Z 2 >>Z, i.e. intrinsic lines 123 and 124 are neglected), the bipolar pulse according to FIG. 15 b could be achieved by using a transmission line connected to the load 125 at its near end and short-circuited at its distal end, as was shown on FIG. 11 a and FIG. 13 b . To provide separation between sub-pulses an extra transmission line like transmission line 64 in FIG. 11 a or transmission line 94 in FIG. 13 b should be used.
[0061] Referring to FIG. 16 , which is a schematic of generator, which consists of two series connected double single-stage bipolar pulse generators shown on FIG. 15 a as an embodiment of the present invention. This generator consists of double single-stage bipolar pulse generator structure (lines 130 , 131 , 134 , 136 and 138 ), which is the same as generator structure on FIG. 15 a and it is connected in series with exactly the same generator structure (transmission lines 132 , 133 , 135 , 137 and 139 ). Both switches 141 and 142 should be closed simultaneously. These two switches could be replaced by a single switch or by any number of simultaneously closed switches.
[0062] In the case when impedances Z 1 and Z 2 of intrinsic transmission lines 136 , 137 , 138 and 139 are much more compared to Z (and 3 Z) the structure FIG. 13 b is valid with specific values of load impedance 140 , which should be equal to 32 Z/3 as shown on FIG. 17 . Characteristic impedance of transmission line 143 should be equal to 32 Z and their electrical length is equal t. Separation between sub-pulses will be also equal zero.
[0063] FIG. 18 a is a schematic of bipolar pulse generator as an embodiment of the present invention. This generator consists of two-step, double single-stage bipolar pulse generator structure with intrinsic transmission lines that provides bipolar pulse. This generator operates, in principle, as generator according to FIG. 7 a in mentioned above US Patent Application 2007/0165839 A1. First step with transmission lines 150 and 152 is connected to the second step with transmission lines 151 and 153 , while transmission line 154 with double electrical length 2 t play the same role as two transmission lines 340 in mentioned above generator according to FIG. 7 a . Intrinsic lines 155 and 156 connected in series play the same role as transmission line 385 in mentioned above generator according to FIG. 7 a . FIG. 18 b illustrates the pulse form on the load provided by generator according to FIG. 18 a.
[0064] FIG. 19 is a schematic of bipolar pulse generator with two switches in first two successive steps as an embodiment of the present invention. This generator provides bipolar pulse with gap between sub-pulses equal to the length of sub-pulse. The charging voltage 2V of second and third steps is twice the charging voltage V of the first step. In this case voltages on both switches 164 and 165 are identical and equal V. Mostly because of characteristic impedance of the second step line 161 is about twice the characteristic impedance of the first step line 160 the total energy stored in this generator, i.e. in lines 160 , 161 , 162 and 163 is much higher compared to single-switch stepped-line generator, as well as two-switches generator according to FIG. 20 in US Patent Application 2007/0165839 A1.
[0065] During operation if switch 164 is turned ON (closed) at time t 0 , the second switch 165 should be turned ON (closed) at time t 0 +t, i.e., at time slightly less than t after t 0 to prevent overvoltage on switch 165 . However, in the case of switch 165 is a spark-gap it will be turned ON automatically due to overvoltage. The impedance transformation (ZL/Z) as a ratio of load impedance 167 to the lowest impedance Z of the first step 160 and ratio of inductive stub 166 to the load impedance will be increased by increasing the number of steps without deterioration the pulse shape. FIG. 20 shows a table of normalized element's values for N-step (N=3, 5, 7 . . . 23) bipolar pulse generator according to FIG. 19 and illustrate the increasing transformation ratios.
[0066] FIGS. 21 a and 21 b illustrates folded and partly folded designs of bipolar pulse generator according to FIG. 19 , as an embodiment of the present invention. Both switches 164 and 165 are positioned outside structure that is preferable for practical implementation.
[0067] The invention has been described with reference to certain preferred embodiments thereof. It will be understood by those skilled in the art that modifications and variations are possible with the scope of the appended claims.
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A bipolar pulse generator is implemented in a simple structure while providing a high efficiency design having a relatively low total size, while still allowing access by fibers used to control a photoconductive switch that activates the generator. The bipolar pulse generator includes a stacked Blumlein generator structure with an additional transmission line connected to a load at its near end and short-circuited at its distal end. An extra transmission line is positioned between the Blumlein generator's structure and the load provides specified limited gap between positive and negative sub-pulses. The bipolar pulse generator further includes a bended Blumlein generator structure, in which an existing intrinsic “stray” transmission line is used to provide the bipolar pulse. Still further, bipolar pulse generator includes stepped transmission lines, with additional switches positioned between steps, which are charged by different voltages.
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[0001] This application claims priority from U.S. Provisional Application No. 61/231,744 filed Aug. 6, 2009, which is hereby incorporated by reference.
FIELD
[0002] This application generally relates to a depth or height control system for equipment that includes implements to be raised and lowered. More particularly, the present application relates to an improved depth or height control system for farm equipment.
BACKGROUND
[0003] Large scale farming involves the use of power-driven assemblies of cultivation equipment to allow for cultivating and planting fields faster, more efficiently, and with less expenditure of resources. In many cases, the equipment, such as tillage equipment, includes a frame or platform that is towed behind a powered vehicle, such as a tractor. These equipment frames can be raised or lowered in relation to supports, typically wheels, in order to bring the tools in contact with the ground or crops at an appropriate height. Maintaining an appropriate height can be an important factor. For example, in planting, seed depth impacts when the plants will germinate and subsequently grow. This can determine when a crop matures and can have an impact on yield or the like.
[0004] The raising and lowering of the equipment frame can be handled by hydraulic or similar systems provided on the equipment (here, the term “hydraulics” is intended to include both air and oil types). A disadvantage of using hydraulic systems is the tendency to leak fluid. In these systems, the seals required to separate the pressurized hydraulic fluid from the atmosphere can wear and leaks may occur. Further, when the pressure within the hydraulic system is fluctuating due to differing pressures from the farm implements and the like, additional stresses are placed on the mechanical components of the hydraulic systems, which increases the likelihood of breakdown. If there is a leak or breakdown, the hydraulic system will not be able to maintain or change the height of the frame.
[0005] Some conventional systems make use of mechanical stops or the like to maintain height if, for example, the hydraulics fail or are overloaded. However, systems making use of a mechanical stop can be difficult to adjust to a preferred height or depth because they need to be adjusted under a load, whether due to the hydraulics or because the farm implements are in a lowered position or the like. In these systems, the hydraulics typically need to be depressurized before the mechanical stop can be set.
[0006] As such, there is need for an improved depth control for height adjustment systems.
SUMMARY
[0007] Generally speaking, the embodiments herein relate to a depth or height control for a depth/height adjustment system on a piece of equipment. In particular, the embodiments relate to a depth control system that provides an improved mechanical stop or locking mechanism in relation to a depth setting of a frame of a piece of equipment. The mechanical stop can be adjusted by a predetermined amount, for example, every ½″, to set the frame at the desired working depth. The depth control system is configured such that it can be adjusted from the front of the equipment, with ease under no load or resistance when the equipment is raised or in the transport mode. There is no need to depressurize the hydraulics or the like.
[0008] In one aspect there is provided a depth control system for a frame mounted to a movement system, wherein the frame is mounted such that the frame can be raised and lowered in relation to the movement system by a depth adjustment system, the depth control system comprises: a depth control support attached to the depth adjustment system and configured to move with the frame during depth adjustment; a depth control arm extending from the depth control support towards a first end of the frame, a frame guide incorporated to the first end of the frame designed to receive the depth control arm; and a locking mechanism adapted to receive and lock the depth control arm in relation to the frame guide such that the depth control support prevents the frame from moving in at least one direction.
[0009] In a particular case, the locking mechanism of the depth control system may have a sleeve designed to abut against the frame guide, the sleeve comprising at least one positioning hole that matches a plurality of positioning holes within the depth control arm.
[0010] In this case, the locking mechanism further may further have a pin designed to fit the at least one positioning hole of the sleeve and the plurality of positioning holes in the depth control arm.
[0011] In one particular case, the plurality of positioning holes within the depth control arm may be offset every ½ inch.
[0012] In another particular case, the depth control system may include a fine adjustment mechanism. The fine adjustment mechanism may have a clevis and a threaded bolt provided to the connection between the depth control support and the depth control arm.
[0013] In some cases, the depth the depth adjustment system may have a suspension system.
[0014] In some particular cases, the suspension system further may have hydraulics.
[0015] In another aspect, there is provided a depth control system for a frame mounted to a wheel frame, wherein the depth control system is mounted between the frame and the wheel frame such that the frame may be lowered in relation to the wheels, the depth control system comprising: a depth control support and a frame support wherein the depth control support and the frame support are configured to move during depth adjustment; a depth control arm extending from the depth control support towards a first end of the frame, the depth control arm comprising a plurality of positioning holes on an end; a support arm extending from the frame support towards the first end of the frame; a frame guide incorporated to the first end of the frame designed to receive the depth control arm and the support arm; a sleeve designed to abut against the frame guide, the sleeve comprising at least one hole that matches the plurality of positioning holes within the depth control arm; and a pin designed to fit the at least one positioning of the sleeve and the plurality of positioning holes in the depth control arm such that the depth control support prevents the frame from moving in at least one direction.
[0016] In a particular case, the plurality of positioning holes within the depth control arm may be offset every ½ inch.
[0017] In another particular case, the depth control system may include a fine adjustment mechanism. The fine adjustment mechanism may have a clevis and a threaded bolt provided to the connection between the depth control support and the depth control arm.
[0018] In a particular case, the depth control system may be operatively connected to a suspension system. The suspension system may have hydraulics.
[0019] In still another aspect, there is provided farm equipment comprising: a movement system; a center frame; a depth control system mounted between the center frame and the movement system such that the center frame can be raised or lowered in relation to the movement system by a depth adjustment system, the depth control system comprising: a depth control support attached to the depth adjustment system and configured to move with the frame during depth adjustment; a depth control arm extending from the depth control support towards a first end of the frame; a frame guide incorporated to the first end of the frame designed to receive the depth control arm; and a locking mechanism adapted to receive and lock the depth control arm in relation to the frame guide such that the depth control support prevents the center frame from moving in at least one direction.
[0020] In one case, the farm equipment of claim may have at least one side attachment attached to the center frame wherein the at least one side attachment comprises: a side attachment movement system; a side attachment frame and a depth control system mounted between the side attachment frame and the side attachment movement system such that the side attachment frame can be raised or lowered in relation to the side attachment movement system by a depth adjustment system at a different depth than the center frame, the depth control system comprising: a depth control support attached to the depth adjustment system and configured to move with the frame during depth adjustment; a depth control arm extending from the depth control support towards a first end of the frame; a frame guide incorporated to the first end of the frame designed to receive the depth control arm; and a locking mechanism adapted to receive and lock the depth control arm in relation to the frame guide such that the depth control support prevents the side attachment frame from moving in at least one direction.
[0021] In some cases the depth control system of the center frame and the depth control system of the at least one side attachment may have a fine adjustment mechanism. The fine adjustment mechanism may have a clevis and a threaded bolt provided to the connection between the depth control support and the depth control arm.
BRIEF DESCRIPTION OF FIGURES
[0022] For a better understanding of the embodiments described herein and to show more clearly how they may be carried into effect, reference will now be made, by way of example only, to the accompanying drawings which show example embodiments and in which:
[0023] FIG. 1 is a photo showing a piece of farm equipment, in particular, farm equipment for tillage, including an embodiment of the depth control system;
[0024] FIG. 2 is a photo showing further detail relating to the depth control system of the farm equipment of FIG. 1 ;
[0025] FIG. 3 is a perspective view of another piece of farm equipment including an embodiment of the depth control system;
[0026] FIG. 4A is a perspective view of the farm equipment of FIG. 3 with a height adjustment system in an up position;
[0027] FIG. 4B is a side view of the farm equipment of FIG. 4A ;
[0028] FIG. 5A is a perspective view of the farm equipment of FIG. 3 with a height adjustment system in a down position;
[0029] FIG. 5B is a side view of the farm equipment of FIG. 5A ;
[0030] FIG. 6A shows a simplified view of the farm equipment of FIG. 3 showing details of the height adjustment system in an up position;
[0031] FIG. 6B shows a detailed view of the height adjustment system of FIG. 6A ;
[0032] FIG. 7A shows a simplified view of the farm equipment of FIG. 3 showing details of the height adjustment system in a down position;
[0033] FIG. 7B shows a detailed view of the height adjustment system of FIG. 7A ;
[0034] FIG. 8 is a detailed illustration of a fine adjustment mechanism for the farm equipment of FIG. 3 ; and
[0035] FIG. 9 is a detailed illustration of the suspension of the farm equipment according to one embodiment.
[0036] It will be appreciated that for simplicity and clarity of illustration, where considered appropriate, reference numerals may be repeated among the figures to indicate corresponding or analogous elements or steps. In addition, numerous specific details are set forth in order to provide a thorough understanding of the exemplary embodiments described herein. However, it will be understood by those of ordinary skill in the art that the embodiments described herein may be practiced without these specific details. In other instances, well-known methods, procedures and components have not been described in detail so as not to obscure the embodiments described herein. Furthermore, this description is not to be considered as limiting the scope of the embodiments described herein in any way, but rather as merely describing the implementation of the various embodiments described herein.
DETAILED DESCRIPTION
[0037] In the following description, the embodiments relate to farm equipment used for tillage. It will be understood by one of skill in the art that similar principles may be applied to other equipment in a similar way, and should not be considered limited to farm equipment. The embodiments may be applied to equipment with a frame that is mounted to a movement system where it is desirable for the frame to be raised and lowered in relation to a movement system. Other farm implements that may benefit from this system include cultivator blades, chisel plows, or the like. The farm equipment is typically towed behind a powered vehicle, most often a tractor.
[0038] FIGS. 1 and 2 are photographs showing a piece of farm equipment including an improved depth control system. In this case, the farm equipment is configured for tillage. FIG. 3 is a perspective view of another piece of farm equipment 100 . The farm equipment typically includes an equipment frame 105 comprising a grid of longitudinal structural members 110 and lateral cross-members 115 that define a roughly rectangular or quadrilateral arrangement. Other equipment may take alternate shapes, for example, a more triangular arrangement, depending on the farm equipment in use. Farm implements, such as cultivator discs and chisel plows, may then be placed on the structural members 110 of the equipment frame 105 . A hitch 120 may be provided to allow the farm equipment 100 to be attached to a tractor or other powered vehicle (not shown). Other attachments may be used, such as a drawbar. The farm equipments includes a depth control system 125 and a height adjustment mechanism 130 , in this case a hydraulic suspension system, mounted between the equipment frame 105 and a wheel frame 135 . Wheels 140 are provided to the wheel frame 135 and provide ground contact points. The wheels 140 are an example of a movement system but the systems herein may also be used with other movement systems, for example continuous track or caterpillar track systems.
[0039] FIGS. 4A , 4 B and 5 A, 5 B show perspective and side views of the farm equipment 100 in up and down positions, respectively. Note that FIG. 5A shows an embodiment in which the equipment includes “wings” as shown in FIG. 1 and described further below. As shown in these figures, the frame 105 can be raised as in FIGS. 4A and 4B and lowered as in FIGS. 5A and 5B with respect to the wheel frame 135 of the equipment 100 . As shown in FIG. 5A , the farm equipment may further include “wings”, which are side attachments 142 , which may increase the useable area of the farm equipment. The use of side attachments 142 , and how they are attached to the farm equipment frame 105 is generally known in the art. The side attachments 142 may also be adapted to include a depth control system 125 and a height adjustment mechanism 130 per each side attachment 142 . As each depth control system 125 and height adjustment mechanism 125 may be adjusted independently the side attachments 142 may be at a different depth than each other and than the center frame of the farm equipment 100 .
[0040] FIGS. 6A and 7A show additional detail of the equipment frame 105 and height adjustment/suspension system 130 in up and down positions, respectively, with FIG. 7A providing a simplified view of the frame 105 . The suspension system 130 drives a frame support 145 that is positioned between the equipment frame 105 and the wheel frame 135 to raise or lower the equipment frame 105 in relation to the wheel frame 135 by acting in conjunction with a support arm 150 . In this embodiment, a depth control support 155 is provided to the wheel frame 135 and a depth control arm 160 is provided to the depth control support 155 . The depth control arm 160 extends from the depth control support to a frame guide 165 , which, in this embodiment, is placed at the front of the frame 105 . The frame guide 165 may be provided in the frame itself or may be provided as a separate element welded, bolted or otherwise provided to the frame.
[0041] The depth control arm 160 extends through the frame guide 165 , through an aperture incorporated within the frame guide 165 . The depth control arm 160 is provided with a locking mechanism to lock the depth control arm 160 in relation to the frame guide 165 to prevent movement in at least one direction. In this example, the locking mechanism includes one or more positioning holes 170 on at least a portion of the depth control arm 160 that extends through the frame aperture. Another component of the locking mechanism is a sleeve 175 that is provided to fit over the depth control arm 160 . The sleeve 175 is larger than the aperture in the frame guide 165 and includes one or more positioning holes that match with the positioning holes 170 on the depth control arm 160 such that the sleeve 175 can be placed at predetermined positions along the depth control arm 160 by use of a pin 180 or the like that passes through the positioning holes 170 of the sleeve 175 and the depth control arm 160 . The at least one positioning hole in the sleeve 175 are configured to match the positioning holes 170 in the depth control arm 160 by having a similar diameter, in order for the pin 180 (a component of the locking mechanism) to fit through the positioning holes in both the sleeve 175 and the depth control arm 160 . The positioning holes 170 of the depth control arm may be spaced at, for example, approximately ½″ intervals although larger or smaller intervals may be preferred depending on the farm implement being used and the variations of depth required. It will be understood that either of the sleeve 175 or the depth control arm 160 may have a plurality of holes to allow the sleeve 175 to be positioned at the appropriate location for a desired depth setting.
[0042] A secondary frame guide (not shown) may be attached to the frame 105 to enclose the sleeve 175 between the frame guide 165 and secondary frame guide. The secondary frame guide would also include an aperture through which the depth control arm 160 may extend. A secondary sleeve (not shown) similar to sleeve 175 could then be used to lock the depth control arm 160 in place in relation to the secondary frame guide to control movement of the depth control arm 160 in a second direction.
[0043] FIGS. 6B and 7B show additional detail of the depth control arm 160 and sleeve 175 in up and down positions, respectively. As shown in FIG. 7B , when the equipment frame 105 is lowered, the sleeve 175 will abut the frame guide 165 because it is larger than the aperture in the frame guide 165 and, because of the connection with the depth control arm 160 , will not allow the frame 105 to move any lower in relation to the wheels, than the predetermined height set by the sleeve 175 . This is intended to be the case even if the hydraulics were to fail. As shown in FIG. 7A , when the frame 105 is raised, the sleeve 175 can be easily moved on the depth control arm 160 to change or set the height/depth without having to depressurize the hydraulic system 130 . As such, it is possible to set the depth control system 125 using a locking mechanism, such as a sleeve, in a situation where the depth control system 125 is not under load and the user can easily and efficiently change the setting.
[0044] In some cases, there may also be a fine adjustment mechanism 190 that will normally be set before the use of the farm equipment 100 . In the embodiment of FIG. 3 , the fine adjustment mechanism is at the depth control support 155 where the depth control arm 160 is connected or at the frame support 145 where the support arm 150 is connected. FIG. 8 shows additional detail of this embodiment of the fine adjustment mechanism 190 . The fine adjustment mechanism includes a clevis 195 and a threaded bolt 200 provided where the depth control arm 160 connects to the depth control support 155 . The depth control arm 160 can be adjusted along the threaded bolt 200 to allow for fine adjustment of the eventual positioning of the sleeve and positioning holes for the depth control system 125 .
[0045] FIG. 9 shows additional detail of the suspension system 130 . The suspension system 130 includes a hydraulic cylinder 205 that connects at one end to the depth control support 155 or wheel frame 135 and at the other end to the frame support 145 . When the frame 105 is to be raised or lowered, the hydraulic cylinder 205 causes the frame support 145 to pivot around a suspension pivot point 210 connected to the frame 105 and cause the frame 105 to raise or lower in relation to the wheels 140 . In this process, the depth control support 145 moves such that, as the frame 105 is raised, the depth control arm 160 slides through the frame guide 165 and the sleeve 175 is adjustable. As the frame 105 is lowered, the depth control arm 160 slides through the frame guide 165 until the sleeve 175 abuts the frame guide 165 and serves to prevent the frame 105 from lowering any further and locks the depth of the frame 105 so that the action of the farm implements cannot pull the frame 105 lower and protects the hydraulic cylinder 205 from excess forces.
[0046] In the embodiment of the farm equipment having “wings”, as each of the centre part of the frame and the side attachments may have their own depth control systems 125 and suspension system 130 , each suspension system 130 may be operated individually and independently to create different depth levels as required.
[0047] It will be understood that other arrangements and embodiments will be apparent to those skilled in the art based on the disclosure of the above embodiments. Further, various modifications can be made to the exemplary embodiments described and illustrated herein, without departing from the general scope of the application.
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A depth control system for a frame mounted to a movement system, wherein the frame is mounted such that the frame can be raised and lowered in relation to the movement system by a depth adjustment system, the depth control system comprising: a depth control support attached to the depth adjustment system and configured to move with the frame during depth adjustment; a depth control arm extending from the depth control support towards a first end of the frame; a frame guide incorporated to the first end of the frame designed to receive the depth control arm; and a locking mechanism adapted to receive and lock the depth control arm in relation to the frame guide such that the depth control support prevents the frame from moving in at least one direction.
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BACKGROUND OF THE INVENTION
[0001] 1. Field of the Invention
[0002] The present invention relates to microwave multiplexers used in satellite communication systems and, more particularly, to a composite multiplexer having improved thermal performance based on an overall system having a low coefficient of thermal expansion and a high thermal conductivity heat dissipation path.
[0003] 2. Brief Description of Related Developments
[0004] It is now prevalent in satellite microwave communications systems for such systems to process multiple channels. This requires the combination or separation of the channels either for transmission or for processing after acquisition. This function is usually accomplished by means of a multiplexer.
[0005] The typical multiplexer consists of a series of input channels connected to a waveguide manifold through ports defined by irises. Each of the channels are tuned and the irises designed for maximum efficiency of the overall system. The connections of the input channels to the manifold must be accurately positioned according to strict spacing requirements governed by the wavelength λ of the transmitted microwave energy. The spacing is measured along the longitudinal axis of the manifold from a shorted end.
[0006] High power, multi-carrier, microwave space antenna multiplexers are important to the communication capability of a satellite that is orbiting the earth. Conventional multiplexers are hollow tubes made preferably from a material having a low coefficient of thermal expansion and are internally metal plated to effect conductivity, a preferable plating material being copper.
[0007] The process of launching satellites into space involves a very weight conscious process. It has been calculated that the cost for launching a pound of payload material into space is on the order of many thousands of dollars. Therefore, it is incumbent upon satellite manufacturers to use materials that are lightweight, yet function with equal effectiveness as their full weight counterparts. Thus, the use of graphite or other light weight materials in the fabrication of multiplexers has evolved as a standard practice.
[0008] Since RF multiplexers are sensitive to changes in volume a significant amount of design effort involved in constructing a composite light weight multiplexer, is therefore directed to volume stability. Volume stability is an important characteristic of a microwave multiplexer in order to provide stable resonant frequencies.
[0009] It is a purpose of this invention to provide a light weight multiplexer having improved volume stability.
[0010] One factor that is significant in this effort is the thermal expansion of the multiplexers as it is subjected to changes in ambient temperature.
[0011] Different approaches attempt to use materials having a low coefficient of thermal expansion. One of such approaches involves the construction of a multiplexer from metal alloys, such as INVAR, which is an iron/nickel alloy. In this instance it is required to heat the multiplexer in order to maintain operation of the device in the geometrically stable range of the material. There is a weight penalty paid for this approach.
[0012] Another approach is to use a non thermally conductive graphite composite material, such as carbon reinforced composite. In this approach the cavities and iris' are bonded together. Because of the lack of thermal conductivity, hot spots may develop at tuning collars and irises. In addition, the coefficient of thermal expansion mismatch between the bonding adhesive and the composite structure, increases interface stresses under thermal load. A source of external heat is also needed for this approach.
[0013] Yet another approach uses an aluminum alloy in conjunction with mechanical means to compensate for volume changes.
[0014] It is an object of this invention to construct a significantly lighter multiplexer using composite materials which provide both a low coefficient of thermal expansion and reduce the need for thermal and mechanical compensation by providing high thermal conductivity.
SUMMARY OF THE INVENTION
[0015] For illustration purposes the multiplexer of this invention comprises a pair of input channels connected to a manifold through irises. Each of the channels consists of a tube constructed of two types of carbon fibers in the form of a tape/cloth/resin matrix. One of the fibers used is selected for its negative coefficient of thermal expansion and its high thermal conductivity. The other fiber is selected for its positive coefficient of thermal conductivity. The two types of fibers are laid up on a resin impregnated tape and cloth material and cured in a tubular shape. The fibers are laid up at an angle to form a helical orientation in the cured tube. In the preferred embodiment the fibers are oriented at an angle to each other of 45° and extend in a helix around the longitudinal axis of the channel tube.
[0016] Connection flanges are bonded in place at either end of a tubular channel section that forms part of a resonant cavity. In the illustrated embodiment, a complete resonant cavity is formed by connecting two channel sections together by bolting the flanges with an iris in between. The iris is fixed to a support bracket for mounting on a frame. The flanges, irises and brackets are constructed of a carbon fiber composite material having high thermal conductivity. A thermal dissipation path away from the multiplexer to the frame is constructed in the overall assembly by the cooperation of the high thermally conductive fibers and the high thermally conductive components.
[0017] The internal surface of the channel tube is coated with copper and silver layers by a plating process to provide electrical conductivity for the resonant cavity. In operation a composite tube of this construction exhibits a near zero coefficient of thermal expansion because of the mutually compensating effects of the two types of fibers and their layup angles.
[0018] In the method of this invention the fibers are used in a tape form and laid up in angular orientation on the resin cloth which provides the matrix. The dual fiber composite is then cured into a rigid tube and plated with a conductive material on its internal surface. Connection flanges are then bonded to the tube at both ends. Multiple tubes may be connected to form a resonant cavity.
[0019] Tuning ports are drilled and tapped to receive threaded tuning plugs which are in turn drilled and tapped to accept tuning screws. To strengthen the channel tube in the area of the tuning screws, a doubler collar may be used surrounding the tube at the tuning port location. The doubler is also constructed of a high thermally conductive material to connect with the thermal dissipation path provided by the high thermally conductive fibers. The tuning plugs are secured by the engagement of threads between the plug and drilled openings and by bonding in place.
[0020] In this manner a multiplexer is constructed, which has a stable volume over its thermal operating range. A composite material is used that utilizes a fabric having fibers of opposing coefficients of thermal expansion. Such fibers are assembled at an angle to each other so that resulting expansion and contractions counter act and cancel.
BRIEF DESCRIPTION OF THE DRAWINGS
[0021] The foregoing aspects and other features of the present invention are explained in the following description, taken in connection with the accompanying drawing in which:
[0022] [0022]FIG. 1 is a perspective view of a multiplexer according to this invention;
[0023] [0023]FIG. 2 is a perspective view of a resonant cavity according to this invention;
[0024] [0024]FIG. 3 is a perspective view of a manifold according to this invention; and
[0025] [0025]FIG. 4 is a schematic illustration of the tube material of this invention.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
[0026] The system of this invention is constructed for use in a satellite communications network in which multiple channels are commonly used. In the process of receiving and transmitting microwave signals, either at a ground station or on board an orbiting satellite, it is necessary to combine or separate the communication channels before further processing. This task is accomplished by means of a multiplexer.
[0027] For illustration purposes an output multiplexer 1 for use on a satellite is described with reference to FIGS. 1 - 4 . Depending on the application to which the components are adapted, the channeled output of the multiplexer 1 may be fed to an antenna (not shown) for transmission to a ground station.
[0028] For the purpose of illustration, the multiplexer 1 is shown in FIG. 1 as an assembly of two channels or resonator cavities 2 and 3 which are coupled to the manifold 4 , as shown in FIG. 1. Each of the input channels 2 and 3 receive microwave signals through input ports 17 and 18 and are coupled to the manifold 4 by a coupling mechanism 5 . The input channels 2 and 3 will generally be coupled through an iris 6 as part of coupling mechanism 5 .
[0029] Each of the channels 2 and 3 are constructed, as shown in FIG. 2 and is an assembly of two tubular sections 7 and 8 and 9 and 10 respectively. Each tubular section is constructed, as shown in FIG. 4, of two types of carbon fibers A and B laid up on a resin impregnated cloth matrix C. One of the fibers used is selected for its negative coefficient of thermal expansion (CTE) and its high thermal conductivity, such as the pitch based fiber tape K13DTU, available from Mitsubishi. The other fiber is selected for its positive coefficient of thermal expansion and for its insulating properties, for example the pan fiber T300, manufactured by Amoco. These fibers are selected for their relatively opposing CTE's. The fibers have a longitudinal axis a-a and b-b respectively and generally are manufactured as a series of parallel extending strands in a tape like configuration. The high and low CTE fibers, A and B are laid up on resin/cloth/tape matrix C and cured in a tubular shape, such as tubular sections 7 - 10 . The fibers A and B are laid up with their respective longitudinal axes at an angle θ to each other, to form a helical orientation in the cured tube, as shown in FIG. 4.
[0030] In the preferred embodiment, the fibers are oriented at an angle of 45° and extend in a helix around the longitudinal axis x-x of the channel tube. The angle θ can be constructed in a range of between 0 and 90 degrees. The angle is selected such that the expansion and contraction of the fibers during thermal cycling counter act each other and tend to cancel out. The laid up cured tubes are then cut to shape for further assembly.
[0031] Connection flanges, such as flanges 11 - 14 , as shown in FIG. 2, are compression molded of a material that has high thermal conductivity, for example, 10 to 150 W/m-K. A connection flange is then bonded to both ends of tube sections 7 - 10 . The coupling mechanism 5 , as shown in FIG. 2, consists of a pair of connection flanges 12 and 13 which are bolted together with an iris 6 in between. The irises 6 are also compression molded of a high thermally conductive material and are connected to a structural frame 16 through mounting brackets 23 , 24 and 25 , as shown in FIG. 1. Mounting brackets 23 - 25 are constructed of similar material, i.e. having high thermal conductivity. The coupling mechanism 5 , including flanges 11 - 14 , irises 6 , and brackets 23 - 25 , form a high thermally conductive path to the frame for heat dissipation.
[0032] In order to provide a tuning capability within resonant cavities 2 and 3 tuning ports (not shown) may be drilled and tapped to accommodate tuning plugs, as shown in FIG. 1 at 19 and 20 . Tuning plugs 19 and 20 consist of a threaded copper plug which is itself drilled and tapped to receive a copper tuning screw 21 . In order to strengthen the structure of tubes section 7 - 10 in the area of the tuning plugs, a doubler collar, as shown at. 22 in FIG. 2, may be used. Doubler collar 22 circumscribes the tube, as shown in FIGS. 1 and 2 and has drilled and tapped holes which align with tuning ports drilled in the tubes 7 - 10 . The doubler collar 22 is constructed of a high thermally conductive material to connect to the heat dissipating path of the overall multiplexer 1 . This will assist in avoiding hot spots, which may occur at the tuning plugs.
[0033] Manifold 4 is constructed similarly to the tubes 710 , using fiber strands A and B laid up on a cloth/tape/resin matrix C, as described above. Connecting flanges 19 - 22 are compression molded as separate components using a material having high thermal conductivity. The flanges 19 - 22 are then bonded to the manifold 4 , as shown in FIG. 3. Connecting flanges 19 - 22 of manifold 4 are bolted to a connecting flange of a resonant cavity, such as flange 11 , in FIG. 2, to form a coupling mechanism 5 , including an iris 6 . The cross section of the manifold 4 is generally rectangular and the internal surface is coated with a conductive film, such as copper/silver.
[0034] To construct the resonant cavities 2 and 3 . Tapes containing fibers A and B are laid up on the resin impregnated cloth C in a sticky state. The tapes are oriented relative to each other to provide an angle θ between the longitudinal axes fibers A and B. The angle θ can be in the range of 0 to 90 degrees, but an angle θ equal to 45° has proven successful. A solid composite tube is then formed by curing the laid up materials. The tube is vacuum bagged and cured under pressure in an autoclave. In this manner the tubes can be manufactured in elongated sections and cut to length as needed.
[0035] In a separate process the components of the coupling mechanism 5 are compression molded of a material having high thermal conductivity. This would include connecting flanges 11 - 14 , as needed, irises 6 , as needed and mounting brackets 23 - 25 , as needed. If doubler collars are used, these are also compression molded in ring form with the inside diameter slightly larger than the outside diameter of the tubes 7 - 10 . Collars 22 are then assembled in place and bonded to the tube. The connecting flanges 11 - 14 are then bonded in place at the ends of each tube section 7 - 10 . A complete resonant cavity 2 or 3 may be assembled by inserting an iris element 6 between two adjacent tube sections, such as 7 and 8 , and bolting the assembly together with their longitudinal axes aligned. The assembled cavity is then plated on its internal surface with a conductive film such as and alloy of copper and silver. A manifold may be constructed following a similar procedure.
[0036] In this manner a resonant cavity and multiplexer is provided which has approximately a zero coefficient of thermal expansion for the structure over a wide temperature range. This is provided by the use of dual fibers A and B having near opposite coefficients of thermal expansion. The thermal stresses generated by the diverse fibers are opposing to compensate for the thermal stress generated by changes in temperature of the multiplexer. This is accomplished while providing an effective thermal dissipation path away from the cavity through the cooperation of a fiber of high thermal conductivity with components having a similar characteristic. This performance improvement is accomplished while reducing the weight of the multiplexer to one/sixth of comparably performing units.
[0037] It should be understood that the foregoing description is only meant to be illustrative of the invention. Various alternatives and modifications can be devised by those skilled in the art without departing from the invention. The present invention is intended to embrace all such alternatives, modifications and variances which fall within the scope of the appended claims.
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A multiplexer is constructed, which has a stable volume over its thermal operating range. A composite material is used that utilizes a fabric having fibers of opposing coefficients of thermal expansion. Such fibers are assembled at an angle to each other so that resulting expansion and contractions counter act and cancel. One of the fibers is selected for its high thermal conductivity and extends over the length of the multiplexer to form a heat dissipating path.
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CROSS-REFERENCE TO RELATED CASES
[0001] This case claims priority from and the benefit thereof and incorporates entirely: U.S. Provisional Application 60/737,808, filed Nov. 18, 2005, and entitled “System and Method to Modulate Phrenic Nerve to Prevent Sleep Apnea;” U.S. Provisional Application 60/743,062, filed Dec. 21, 2005, and entitled “System and Method to Modulate Phrenic Nerve to Prevent Sleep Apnea;” and U.S. Provisional Application 60/743,326, filed Feb. 21, 2006, and entitled “System and Method to Modulate Phrenic Nerve to Prevent Sleep Apnea.”
FIELD OF THE INVENTION
[0002] The present invention relates generally to implantable medical devices and more particularly to a device and method for controlling breathing and for treating Central Sleep Apnea.
BACKGROUND OF THE INVENTION
[0003] History
[0004] Sleep Disordered Breathing (SDB) and particularly Central Sleep Apnea (CSA) is a breathing disorder closely associated with Congestive Heart Failure (CHF). The heart function of patients with heart failure may be treated with various drugs, or implanted cardiac pacemaker devices. The breathing function of patients with heart failure may be treated with Continuous Positive Air Pressure (CPAP) devices or Nocturnal Nasal Oxygen. These respiratory therapies are especially useful during periods of rest or sleep. Recently, implanted devices to directly address respiration disturbances have been proposed. Some proposed therapeutic devices combine cardiac pacing therapies with phrenic nerve stimulation to control breathing.
[0005] Phrenic nerve pacing as a separate and stand alone therapy has been explored for paralyzed patients where it is an alternative to forced mechanical ventilation, and for patients with the most severe cases of central sleep apnea. For example, Ondine's Curse has been treated with phrenic nerve pacemakers since at least the 1970 's. In either instance, typically, such phrenic nerve pacemakers place an electrode in contact with the phrenic nerve and they pace the patient's phrenic nerve at a constant rate. Such therapy does not permit natural breathing and it occurs without regard to neural respiratory drive.
[0006] Motivation for Therapy
[0007] SDB exists in two primary forms. The first is central sleep apnea (CSA) and the second is obstructive sleep apnea (OSA). In OSA the patient's neural breathing drive remains intact, but the pulmonary airways collapse during inspiration, which prevents air flow causing a form of apnea. Typically, such patients awake or are aroused as a result of the apnea event. The forced airflow of CPAP helps keep the airways open providing a useful therapy to the OSA patient.
[0008] CSA patients also exhibit apnea but from a different cause. These CSA patients have episodes of reduced neural breathing drive for several seconds before breathing drive returns. The loss of respiratory drive and apnea is due to a dysfunction in the patient's central respiratory control located in the brain. This dysfunction causes the patient's breathing pattern to oscillate between too rapid breathing called hyperventilation and periods of apnea (not breathing). Repeated bouts of rapid breathing followed by apnea are seen clinically and this form of disordered breathing is called Cheyne-Stokes breathing or CSR. Other patterns have been seen clinically as well including bouts of hyperventilation followed by hypopneas only.
[0009] In patients with CHF, prognosis is significantly worse when sleep apnea is present. A high apnea-hypopnea index (a measure of the number of breathing disturbances per hour) has been found to correlate to a poor prognosis for the patient. The swings between hyperventilation and apnea characterized by central sleep apnea have three main adverse consequences, namely: large swings in arterial blood gases (oxygen and carbon dioxide); arousals and shifts to light sleep; and large negative swings in intrathoracic pressure during hyperventilation. The large swings in blood gases lead to decreased oxygen flow to the heart, activation of the sympathetic nervous system, endothelial cell dysfunction, and pulmonary arteriolar vasoconstriction. Arousals contribute to increased sympathetic nervous activity, which has been shown to predict poor survival of patients with heart failure. Negative intrathoracic pressure, which occurs during the hyperventilation phase of central apnea, increases the after load and oxygen consumption of the left ventricle of the heart. It also causes more fluid to be retained in the patient's lungs. As a result of these effects the patient's condition deteriorates.
[0010] In spite of advances in care and in knowledge there is a large unmet clinical need for patients with sleep disordered breathing especially those exhibiting central sleep apnea and congestive heart failure.
SUMMARY OF THE INVENTION
[0011] The device of the present invention can sense the patients breathing and it can distinguish inhalation or inspiration from exhalation or expiration.
[0012] The device can periodically stimulate the phrenic nerve as required. In some embodiments the stimulation may be invoked automatically in response to sensed physiologic conditions. In some embodiments the device can stop the delivery of therapy in response to sensed conditions. In some embodiments the device can be prescribed and dispensed and the therapy delivered without regard to the sensed conditions. As a result, the device may be used to detect and intervene in order to correct episodes of sleep disordered breathing or the device may intervene to prevent episodes of sleep disordered breathing from occurring. The methods that are taught here may be used alone to treat a patient or they may be incorporated into a cardiac stimulating device where the respiration therapy is merged with a cardiac therapy. The therapy and its integration with cardiac stimulation therapy and the architecture for carrying out the therapy are quite flexible and may be implemented in any of several forms.
[0013] Hardware implementation and partitioning for carrying out the methods of the invention are also flexible. For example the phrenic nerve stimulation may be carried out with a transvenous lead system lodged in one of the cardiophrenic vein a short distance from the heart. One or both phrenic nerves may be accessed with leads. Either one side or both (right and left) phrenic nerves may be stimulated. Alternatively the phrenic nerve may be accessed through a large vein such as the jugular or the superior vena cava. As an alternative a stimulation electrode may be place in the pericardial space on the heart, near the phrenic nerve but electrically isolated from the heart. Implementation of respiration detection may also take any of several forms. Transthoracic impedance measurement may be taken from electrodes implanted at locations in the body to measure or sense the change in lung volume associated with breathing. Alternatively one or more implanted pressure transducers in or near the pleural cavity may be used to track pressure changes associated with breathing. Knowledge of breathing rates and patterns are useful in carrying out the invention but distinguishing reliably the inspiration phase from expiration phase is a breath is particularly important for timing the delivery of the stimulation.
[0014] We consider that breathing has an inspiration phase followed by an expiration phase. Each breath is followed by a pause when the lungs are “still” before the next breath's inspiration. The device delivers phrenic nerve stimulation after the start of inspiration preferably toward the start of exhalation. The duration and magnitude of the stimulation is selected to “extend” the expiration phase or the respiratory pause of a naturally initiated breath. We note relatively little change in lung volume and little air exchange during the stimulation phase of the therapy. We have observed that prolongation of a natural breath, while keeping some air trapped in the lungs, delays the inspiration phase of next natural breath until the air trapped in the lungs is exhaled. For this reason our therapy has a tendency to lower the observed breathing rate. Typically the stimulation maintains activation of the diaphragm long enough to mimic a patient holding their breath by not letting the diaphragm relax. This mechanism of action controls the rate of breathing by increasing the effective duration of each breath.
[0015] Our experimental animal work has demonstrated the ability of the stimulation regime to down-regulate breathing rate (and minute ventilation) to a desired (preset) value while maintaining natural inspiration (i.e. by prolonging exhalation and extending the respiratory pause phases of the breath) without blocking the phrenic nerve. We believe that maintenance of natural inspiration is important since it allows prevention of airway collapse and retains certain capacity of the body to auto regulate rate of inspiration and depth of breathing. We also demonstrated that unilateral and transvenous stimulation is sufficient to carry out the invention and insures adequate levels of patient safety. In the process of prolonging the respiratory pause we “stilled” the lungs (no air movement occurred) while keeping one lung inflated. We believe that the mechanism of action for this observed effect is a physiologic feedback that prevents the respiration control center of the central nervous system from initiating the following breath. In other words we have invented a novel and practical therapy by substantially immobilizing at least one lung of the patient by maintaining the diaphragm in the contracted state by transvenous electrical stimulation of a phrenic nerve for the duration sufficient to substantially reduce breathing rate and alter the blood gas composition of the patient.
BRIEF DESCRIPTION OF THE DRAWINGS
[0016] A preferred embodiment and best mode of the invention is illustrated in the attached drawings where identical reference numerals indicate identical structure throughout the figures and where multiple instances of a reference numeral in a figure show the identical structure at another location to improve the clarity of the figures, and where:
[0017] FIG. 1 is a schematic diagram;
[0018] FIG. 2 is a schematic diagram;
[0019] FIG. 3 is a schematic diagram;
[0020] FIG. 4 is a schematic diagram;
[0021] FIG. 5 is diagram showing experimentally derived physiologic data displayed in two panels A and B;
[0022] FIG. 6 is a schematic diagram showing physiologic data known in the prior art; and
[0023] FIG. 7 is a schematic diagram showing physiologic data and device timing information.
DETAILED DESCRIPTION OF THE INVENTION
[0024] FIG. 1 is schematic diagram showing an implanted medical device (IMD) 101 implanted in a patient's chest for carrying out a therapeutic stimulation of respiration. The patient has lungs shown in bold outline and indicated at 102 overlying the heart 103 . The right phrenic nerve 104 passes from the head alongside the heart to innervate the diaphragm 106 at location 105 .
[0025] In this embodiment a transvenous lead 107 passes from the IMD 101 and passes through venous vasculature to enter the cardiophrenic vein 108 on the right side of the patient. The cardiophrenic vein 108 lies next to the phrenic nerve 104 along the heart. Electrical stimulation pulses supplied to the stimulation electrode 110 on lead 107 interact with the phrenic nerve to stimulate it and thus activate the diaphragm 106 . In the figure a series of concentric circles 112 indicate electrical stimulation of the phrenic nerve. In this embodiment the stimulation electrode 110 lies far enough away from the heart 103 to avoid stimulating the heart 103 . In this embodiment only one branch of the phrenic nerve 104 is stimulated and the other side of nerve is under normal physiologic control.
[0026] A respiration electrode 114 on lead 107 cooperates with an indifferent electrode on the can of the IMD 101 to source and sink low amplitude electrical pulses that are used to track changes in lung volume over time. This well known impedance plethysmography technique is used to derive the inspiration and expiration events of an individual breath and may be used to track breathing rate. This impedance measurement process is indicated in the diagram by the dotted line 116 radiating from the electrode site of respiration electrode 114 to the IMD 101 . Transvenous stimulation of the phrenic nerve from a single lead carrying an impedance measuring respiration electrode is a useful system since it permits minimally invasive implantation of the system. However other architectures are permissible and desirable in some instances.
[0027] FIG. 2 is a schematic diagram showing alternative electrode and lead placements for use in carrying out the stimulation regime of the invention. In some patients it may be easier or more suitable to access the phrenic nerve in the neck in the jugular vein at electrode location 200 . In some instances it may be preferable to place electrodes in veins both near the right phrenic nerve as indicated by the deep location of a stimulation electrode 110 and in the left phrenic nerve at electrode location 202 . Other potential locations for the stimulation electrodes are the large vessel (SVC) above the heart indicated by electrode 203 . Unilateral stimulation is preferred but having multiple sites available may be used to reduce nerve fatigue. Non-venous placement is possible as well. For example, placement of a patch electrode in the pericardial space between the heart and within the pericardial sac is suitable as well, as indicated by electrode location 205 . In this embodiment the insulating patch 206 isolates spaced electrodes 207 and electrode 208 from the heart. The lead 204 connects this bipolar pair of electrodes to the IMD 101 .
[0028] Also seen in this figure is a pressure transducer 209 located in the pleural cavity and connected to the IMD 101 via a lead. The pressure transducer 209 tracks pressure changes associated with breathing and provides this data to the implanted device 101 . The pressure transducer is an alternative to the impedance measurement system for detecting respiration. Such intraplueral pressure signal transducers are known in the respiration monitoring field.
[0029] FIG. 3 shows a schematic diagram of a system for carrying out the invention. The system has an implanted portion 300 and an external programmer portion 301 .
[0030] The IMD 101 can provide stimulation pulses to the stimulation electrode 110 . A companion indifferent electrode 306 may be used to sink or source the stimulation current generated in analog circuits 303 . A portion of the exterior surface 302 of the IMD 101 may be used with respiration electrode 114 to form an impedance plethysmograph. In operation, logic 305 will command the issuance of a train of pulses to the respiration electrode 114 and measure the amplitude of the signal as a function of time in circuits 304 . This well known process can measure the respiration of the patient and find the inspiration phase and the expiration phase of a breath. Respiration data collected over minutes and hours can be logged, transmitted, and/or used to direct the therapy.
[0031] When the therapy is invoked by being turned on by the programmer 301 or in response to high rate breathing above an intervention set point, the logic 305 commands the stimulation the phrenic nerve via the stimulation electrode 110 at a time after the beginning of the inspiration phase. Preferable the stimulation begins after the onset of exhalation. There is some flexibility in onset of stimulation. The shape of the stimulation pulses is under study and it may be beneficial to have the logic 305 command stimulation at higher amplitudes of energy levels as the stimulation progresses. It may also be desirable to have stimulation ramp up and ramp down during the therapy. It may prove desirable to stimulate episodically. The therapy may be best administered to every other breath or in a random pattern. The programmer may permit the patient to regulate the therapy as well. However in each case the stimulation of the diaphragm “stills” the diaphragm resulting in an amount of air trapped in at least one lung and extends the breath duration.
[0032] The duration of the stimulation is under the control of logic 305 . It is expected that the therapy will be dispensed with a fixed duration of pulses corresponding to breathing rate. It should be clear that other strategies for setting the duration of stimulation are within the scope of the invention. For example the breathing rate data can be used to set the stimulation duration to reduce breathing rate to a fraction of the observed rate. The therapy may also be invoked in response to detected high rate breathing or turned on at a fixed time of day. In a device where activity sensors are available the device may deliver therapy at times of relative inactivity (resting or sleeping).
[0033] FIG. 4 shows a schematic diagram of an alternate partitioning of the system. In this implementation, the respiration sensing is carried out outside the patient with sensor 404 , while the implanted portion 400 communicates in real time with an external controller 401 via coils 403 and 402 . This respiration sensor 404 may be a conventional respiration belt or thermistor based system. Real time breathing data is parsed in the controller 401 and control signal sent to the IPG 101 to drive stimulation of the phrenic nerve via lead 107 . This implementation simplifies IMD 101 portion for the system and may be useful for delivery of therapy to a resting or sleeping patient.
[0034] FIG. 5 is set forth as two panels. The data collected from an experimental animal (pig) is presented in the two panels and should be considered together. Panel 5 B plots airflow into and out of the animal against time, while panel 5 A plots volume against time. In the experiment the volume data was computed (integrated) from the airflow measurement. The two panels are two ways of looking at the same data collected at the same time. In each panel the dotted tracing 500 in 5 B and 502 in panel 5 A represent the normal or natural or not-stimulated and therefore underlying breathing pattern of the animal. In panel 5 A the inspiration phase of tracing 502 is seen as segment 514 . After tracing 502 peaks, the expiration phase begins as indicated by segment 516 . The figure shows that along trace 502 , the air that is inhaled is exhaled before 2 seconds has elapsed, as indicated by the dotted trace 502 returning to the zero volume level.
[0035] Trace 504 is associated with the unilateral delivery of stimulation 508 to a phrenic nerve. In the tracing the start of stimulation at time 518 is well after the start of inspiration and corresponds approximately to the reversal of airflow from inspiration to expiration as seen at time 518 . Very shortly after the stimulation begins the animal inhales more air seen by the “bump” 520 in the tracing 504 in panel 5 B. A small increment in the total volume corresponding to this bump is seen at the same time in panel 5 A. Of particular interest is the relatively flat tracing 522 corresponding to no significant change in lung volume during stimulation. Once stimulation terminates the lungs expel air as seen at volume change 524 in panel 5 A corresponding to outflow labeled 512 in panel 5 B. Only after the exhalation outflow 512 was complete did the sedated experimental animal initiate the next breath (not shown). Thus duration of breath was extended in this case from approximately 2 seconds to approximately 6 seconds resulting in the breathing rate reduction from 30 to 10 breaths per minute. The data support the assertion that adequate phrenic stimulation initiated after inspiration and during expiration can “prolong” or “hold” the breath and thus regulate or regularize breathing which it the value of the invention.
[0036] FIG. 6 shows a bout 601 of rapid breathing 603 followed by or preceded by apnea 602 events. This waveform is a presentation of Cheyne-Stokes respiration (CSR) well known in the prior art. The corresponding tracing of blood gas 607 indicates that the rapid breathing drives off blood carbon dioxide (CO 2 ) as indicated the slope of line 606 . CSR begins with the rise of CO 2 as indicated by ramp line 605 which triggers the rapid breathing. The ventilation drives the CO 2 too low resulting in a loss of respiratory drive and an apnea event 602 . During the apnea the level of CO 2 rises as indicated by the slope of line 604 . Once a threshold is reached the cycle repeats.
[0037] FIG. 7 shows a schematic diagram showing the delivery of the inventive therapy in the context of a patient experiencing CSR respiration. The patient experiences several quick breaths 701 and then the device is turned on as indicated by the stimulation pulses 709 . The device looks for a natural inspiration and waits until about the turn from inspiration to expiration, then the burst 709 of stimulation is delivered to a phrenic nerve. As explained in connection with FIG. 5 the stimulation delays breath 706 . This next breath is also a candidate for the therapy and stimulation burst 710 is delivered to the phrenic nerve delaying breath 707 . In a similar fashion the device intervenes in breaths 707 and 708 . It is expected that the lower rate breathing resulting from repeated application of the therapy will keep the CO 2 level in a “normal” range 715 and prevent CSR. The therapy could also be invoked in response to a detected bout of CSR but this is not necessary and it is believed that keeping a patient out of CSR is the better therapy.
[0038] It may be noted that the stimulation waveforms vary in FIG. 7 with stimulation 710 rising in amplitude while stimulation 711 decreases in amplitude. Note as well that stimulation 712 ramps up and then down during the therapy. It is expected that the best waveform may vary from patient to patient or may vary over time. Also seen in the figure is a refractory period typified by period 730 that may be implemented in the logic 302 to prevent the device from issuing the therapy too close in time to the last intervention. In general the refractory period effectively disables the deliver of therapy until the refractory period expires. This places an effective low rate on stimulated rate of breathing. The refractory may be fixed, programmable or adjusted based on sensed breathing rate.
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An implantable medical device for treating breathing disorders such as central sleep apnea wherein stimulation is provided to the phrenic never through a transvenous lead system with the stimulation beginning after inspiration to extend the duration of a breath and to hold the diaphragm in a contracted condition.
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This is a continuation-in-part of U.S. patent application Ser. No. 08/561,404, filed Nov. 21, 1995, now U.S. Pat. No. 5,678,967.
FIELD OF THE INVENTION
This invention relates to ophthalmic lens generating apparatus and more particularly, the present invention relates to ophthalmic lens generating apparatus having vibration dampening properties.
BACKGROUND OF THE INVENTION
The surface finish on an ophthalmic lens is generally affected by two common types of surface defects inherent in a lens machining operation. The first type of defects is caused by the actual removal of material from the lens surface, and the second type is caused by the vibration of one or more of the machine's elements.
The major factors influencing surface defects of the first type are the outline of the cutting tool in contact with the lens, the microstructure and chemical composition of the material of the lens, and thermal effects occurring during the material-removal process. In this respect, improvement in surface finish may be obtained to various degrees by increasing the cutting speed, decreasing the feed of cut and changes in cutting fluid and tool geometry.
Surface defects of the first type generally have surface irregularities of a relatively small extent; usually less than 78 microinches (2 microns) peak-to-valley. This type of surface defects is usually entirely coverable by a clear resinous coating well known in the art of lens making.
Vibration of machine elements, however, is often the cause of deeper irregularities on the surface of generated lenses. Vibration of machine elements is very complex, and often has a combination of interrelated causes as explained below.
Rotating machines in general are known to vibrate according to three basic types of vibration. A first basic type of vibration is caused for example, by an unbalance of the tool, eccentricity in the tool chuck, and defects in a drive belt. This first type of vibration has an amplitude in a radial direction relative to the axis of rotation of the tool.
The second basic type of vibration in rotating machines has an amplitude in an axial direction along the axis of rotation of the tool spindle for example. This axial vibration is often caused by a vacillating plane of rotation of the tool's cutting face, or by intermittent cutting forces. Because the cutting force applied on a tool has a vectorial component in the axial direction, a vibration of the radial type also tends to cause a vibration in the axial direction.
The third basic type of vibration in rotating machines is a torsional vibration. This type of vibration is often associated with torque pulses inherent with some types of electric motors and motor controls. These pulses tend to alternatively increase and reduce the amount of material being removed from the surface of the lens during a full rotation of the tool. This torsional vibration, when cutting forces are present, is also known to cause vibration of the radial and axial types.
It is further known from the science of vibration analysis that any of the above three types of vibration can excite a resonant condition in the structure of the machine, with the consequence of increasing the amplitude of the vibrating element.
The problem of vibration in a lens generating apparatus has been partially addressed in the past. For example, a first apparatus for manufacturing ophthalmic lenses is described in U.S. Pat. No. 4,434,581 issued on Mar. 6, 1984 to Robert G. Spriggs. This apparatus has X-Y fluid-bearing tables mounted on a granite bed weighing about 4,000 pounds. This bed is undoubtedly particularly efficient for reducing the amplitude of a vibration in the radial direction, that is in a direction perpendicular to the table. However, it will be appreciated that a massive table is less appropriate for reducing vibrations of the axial and torsional types where the lens holder or the tool spindle is mounted at some distance for the surface of that table.
In another example, U.S. Pat. No. 4,760,672 issued on Aug. 2, 1988 to Darcangelo et al. describes a lens grinding and polishing apparatus wherein a drive motor is mounted remotely from the tool supporting table, and is driving a micrometer drive via a drive belt. This type of mounting isolates the tool and work spindles from the vibration of the drive motor.
Although the apparatus in both the above examples are most likely efficient in dampening the radial vibrations of the tool and work support spindles, these apparatus as well as other optical lens generating apparatus of the prior art lack vibration dampening properties in the axial and circumferential directions relative to the rotary tool and work holder.
SUMMARY OF THE INVENTION
In the present invention, however, there is provided an ophthalmic lens generating apparatus having a massive base for dampening radial vibrations, a massive upright block for dampening axial vibrations and a high-inertia tool spindle for dampening the torsional vibrations of the rotating elements of the apparatus.
In one aspect of the present invention, there is provided an ophthalmic lens generating apparatus having a tool spindle comprising a motor, a lens surfacing tool and a coupling mounted between the motor and the lens surfacing tool for retaining the lens surfacing tool to the arbor of the motor. The apparatus of the present invention also comprises a first actuated table mounted under the tool spindle for supporting the tool spindle in a movable manner along the longitudinal axis of the apparatus. The massive base is mounted beneath the first actuated table for supporting the table and for dampening vibrations of the tool spindle having a displacement in a direction generally perpendicular to the longitudinal axis of the apparatus.
The apparatus of the present invention further comprises a lens holder having chuck means and structural lens-holder-support means for holding an ophthalmic lens in a plane substantially perpendicular to the longitudinal axis of the apparatus. A massive upright block is mounted on the massive base behind the structural lens-holder-support means for supporting the structural lens-holder-support means and for dampening vibrations of the tool spindle and of the lens holder, having a displacement in a direction generally parallel to the longitudinal axis of the apparatus. Computerized control means are further provided for operating the spindle and the first movable table, and for moving the lens surfacing tool along a prescribed path relative to the lens holder.
The major advantage of the apparatus of the present invention is that the optical surfaces generated thereon are exceptionally smooth. The ophthalmic lenses generated on the apparatus of the present invention have a surface finish which is an optically acceptable final finish, and no further polishing is required.
In another aspect of the present invention, the tool spindle has a nominal moment of inertia about an axis of rotation thereof, and the coupling is a kinematic coupling having first and second circular disks. The first and second circular disks have a respective mass and radius of gyration whereby when the tool spindle rotates about its axis of rotation, both disks increase the nominal moment of inertia of the spindle and enhance the dampening of the torsional vibrations of the spindle.
As will be explained later, a radial vibration of a lens grinding tool is substantially tangential to the surface of the lens being generated. This type of vibration leaves only superficial impressions on the surface of a lens. The axial vibration, however, is substantially perpendicular to the surface of the lens and contributes largely to the roughness of the lens surface. Similarly, torsional vibrations coupled with axial vibrations tend to form circular grooves detrimental to generating high quality surfaces on optical lenses.
While the dampening of axial and torsional vibrations in ophthalmic lens generating apparatus has been generally overlooked in the past, the apparatus of the present invention has dampening structure to reduce the effect of the most common types of vibrations found in rotating machines. The ophthalmic lens generating apparatus of the present invention has a plurality of vibration dampening masses which are cooperatively positioned to absorb the radial, axial and torsional vibrations of the elements of the apparatus. As a result, an optically acceptable final surface finish is obtainable in a single operation.
BRIEF DESCRIPTION OF THE DRAWINGS
The preferred embodiment of the present invention will be further understood from the following description, with reference to the drawings in which:
FIG. 1 is a top and left side perspective view of the ophthalmic lens generating apparatus of the preferred embodiment;
FIG. 2 is a top view of the ophthalmic lens generating apparatus of the preferred embodiment;
FIG. 3 is a left side, partial sectional view of the ophthalmic lens generating apparatus of the preferred embodiment, as taken along line 3--3 in FIG. 2;
FIG. 4 is an exploded side view of the elements of the tool spindle of the ophthalmic lens generating apparatus of the preferred embodiment;
FIG. 5 is a side perspective view of the lens surfacing tool of the ophthalmic lens generating apparatus of the preferred embodiment;
FIG. 6 illustrates a schematic top view of a typical lens surfacing operation;
FIG. 7 is a vector diagram illustrating the forces present during a lens surfacing operation;
FIG. 8 illustrates a first type of dynamic vibration absorber.
FIG. 9 is a cross-section view along line 9 in FIG. 8 illustrating a cylindrical auxiliary mass.
FIG. 10 illustrates a second type of dynamic vibration absorber.
FIG. 11 is a cross-section view along line 11 in FIG. 10 illustrating a ring-shaped auxiliary mass.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
The ophthalmic lens generating apparatus of the preferred embodiment is illustrated in its entirety in FIGS. 1, 2 and 3. The apparatus of the preferred embodiment comprises a tool spindle 20 which is mounted on a support structure having at least two degrees of freedom. The tool spindle 20 is mounted on an actuated turntable 22 which is pivotal about a vertical axis along the generally illustrated Z-axis, in a direction designated by α in FIG. 2. The turntable 22 is mounted on a base plate 24 which is movable on a first actuated linear slide 26 along the longitudinal axis of the apparatus. The longitudinal axis is generally designated as the X-axis of the apparatus.
A lens holder 30 is also supported on a movable mounting plate 32. The mounting plate 32 comprises part of a second actuated linear slide 34' slidably accommodated within a third actuated linear slide 36. The second linear slide 34' including the mounting plate 32 move up and down along the Z-axis, and the third linear slide 36 moves the plate 32 transversely relative to the longitudinal axis of the apparatus along the generally designated Y-axis.
The lens holder 30 may also be rotatable about an axis parallel to the longitudinal axis by means of a rotary actuator (not shown), for the purpose of angularly positioning a lens according to the requirement of a prescription, prior to the lens-surface generating process.
All the linear slides 26, 34' and 36 are preferably mounted on high-precision pressurized fluid bearings. Similarly the turntable 22 and the tool spindle 20 are also preferably mounted on high-precision fluid bearings. Since such bearings are well-known types of bearings generally, they have not been illustrated.
The movements of the actuated linear slides and the actuated turntable are controlled by computer (not shown) according to the requirements of a prescription of the lens to be generated. During operation of the ophthalmic lens generating apparatus of the preferred embodiment, the tool spindle 20 advances toward the lens along the X-axis, and pivots about the Z-axis in a clockwise direction when viewed from above the apparatus. The lens holder 30 moves along the Y-axis simultaneously to the movement of the tool spindle 20, such that an arc along the edge of the tool describes a determined curvature across the surface of the lens. The arc along the edge of the tool and the determined curvature define a toric surface on the lens.
The ophthalmic lens generating apparatus of the preferred embodiment also has a massive granite base 40 which contributes largely to the overall stiffness and stability of the machine. The granite base 40 is especially efficient in absorbing the vibrations of the tool spindle 20 and of the lens holder 30 in a radial direction relative to the spindle and holder and the mass of base 40 must have a magnitude sufficient for such purpose.
The structure of the apparatus of the preferred embodiment also comprises a massive upright granite block 42 supporting the third linear slide 36. The primary purpose of this upright granite block 42 is for absorbing the vibration of the lens holder 30, and the tool spindle 20 in the axial direction relative to the lens holder 30 and the block 42 must have adequate mass for such purpose. The upright granite block 42 is affixed to the granite base 40 by means of through bolts 44 as illustrated in FIG. 3.
Representative preferred characteristics for the massive granite base 40 and the massive upright granite block 42 are as follows:
Granite Base: 32 inches wide by 60 inches long by 8 inches thick; having a total weight of 1,536 lbs.
Upright Granite Block: 31 inches wide by 24 inches high by 14 inches thick; having a total weight of 1,041 lbs.
Referring now to FIGS. 4 and 5, the tool spindle of the lens generating apparatus of the preferred embodiment is illustrated therein. The major elements of the tool spindle 20 are: the cutting tool 50, the circular face plate 52 and the spindle drive motor 54. The cutting tool 50 comprises a cup-shaped body 56 having at least two cutter inserts 58 made of a material containing tungsten-carbide or similar material. The cup-shaped body 56 is mounted on a circular disk plate 60 having means 62 for positioning within mating grooves 64 on the circular face plate 52 and engaging the circular face plate 52. The cutting tool 50 also has a tension rod 66 for extending through the face plate 52 and for engaging with a latching sleeve (not shown) mounted inside the rotating arbor or core of the spindle drive motor 54. This type of tool-mounting arrangement is herein referred to as a kinematic coupling, and is described in co-pending U.S. patent application Ser. No. 08/561,404, filed on Nov. 21, 1995. The tool-mounting arrangement maintains the cutting tool axis of rotation coaxial with the axis of rotation of the motor rotating arbor.
The tool 50 illustrated in FIG. 5 is preferably balanced to a precision characterized by a total displacement peak-to-valley of 1.0 microinch (25 nanometer) when this tool is rotating at an operational speed of about between 7,500 and 10,000 RPM.
The advantage of using a cutting tool 50 with a kinematic coupling is primarily for allowing quick and precise replacement of tools on the tool spindle 20. More importantly, the tool and kinematic coupling have a first large circular disk plate 60 and a second circular face plate 52 having respectively a large moment of inertia for absorbing torsional vibration in the tool spindle 20. Preferably, the disk plate 60 has a moment of inertia expressed in weight units of about 9 lbs-in 2 , and the face plate 52 has a moment of inertia expressed in weight units of about 24 lbs-in 2 .
Furthermore, the spindle drive motor 54 is also selected such that its moment of inertia is as large as practically possible. The tool spindle 20 of the ophthalmic lens generator of the preferred embodiment is characterized by the magnitude of the following representative moments of inertia. The spindle drive motor 54 including face plate 52 has a moment of inertia expressed in weight units of 70.1 lbs-in 2 , and the moment of inertia of a typical cutting tool 50 with disk plate 60, is 11.3 lbs-in 2 .
Referring now to FIGS. 6 and 7, there is illustrated therein a vectorial representation of the forces and vibrations present during a lens generating operation. The radial vibrations of the rotating spindle are represented by the arrow labelled "R". The axial vibrations are represented by arrow labelled "A", and the torsional vibrations represented by the arrow labelled "α".
The radial vibrations "R" are in a direction generally perpendicular to the axis of rotation of the tool. The axial vibrations "A" are in a direction along the axis of rotation of the tool, and the torsional vibrations are in an angular direction relative to the axis of rotation of the tool 50.
Likewise, the vectorial illustration of FIG. 7 represents the forces present during the removing of material from the surface of the lens 72. The cutting force "F" is generally perpendicular to the cutting edge of the tool. The force "F" has a radial component "F R " in the feed direction and an axial component "F A " in an axial direction relative to the axis of rotation of the tool 50.
The magnitude of the cutting force "F" and of its components "F R " and "F A " are proportional to the feed rate and the depth of cut of the tool insert 70. Therefore, when a radial, axial or torsional vibration disrupts the thrust of the tool 50, both the radial "F R " and axial "F A " components are inevitably affected.
In the light of the foregoing, one will understand that any vibration in the radial, axial or circumferential direction relative to the tool spindle has a direct effect on the magnitude of the cutting forces. Because a certain degree of elasticity is found in most machine structures, variations in the cutting forces are often accompanied by microscopic deflections in the elements of the apparatus, and are translated into more or less material being taken off from the surface of the lens.
One will also appreciate that radial vibrations are translated into dominant radial forces "F R " which are oriented in a plane which is substantially tangent to the surface of the lens. Therefore, the defects associated by fluctuations in the radial forces "F R " have a relatively shallow depth. The defects associated by fluctuating axial forces "F A ", however, have a deeper dimension and contribute largely to the optical quality of a generated lens.
As noted above, the apparatus of the preferred embodiment has a massive upright granite block 42 for increasing the stiffness of the structure supporting the lens holder 30, and for absorbing the axial vibrations of the tool spindle 20 and the lens holder 30. The tool spindle 20 of the apparatus of the preferred embodiment has a large moment of inertia whereby any fluctuations in the angular speed of the tool spindle are efficiently reduced to imperceptible levels. Hence, the masses of the base 40, the upright block 42 and the moment of inertia of the tool spindle 20 cooperate with one-another for reducing the overall vibration of the elements of the apparatus. Most importantly the masses of the upright block 42 and the spindle 20 cooperate with one-another for reducing the axial vibration of the tool 50 and the lens holder 30.
The operation of the ophthalmic lens generating apparatus of the preferred embodiment is characterized by a remarkable smoothness wherein a high quality optical surface is generated in a single operation. The ophthalmic lenses generated thereon do not need further polishing. Surface roughness measurements of under 1 micron are generally consistently obtainable on the lenses generated by the apparatus of the preferred embodiment. A surface roughness measure being defined as the arithmetic average deviation from the best fit surface of the lens.
As a further disclosure, the circular face plate 52 and the circular disk plate 60 have each sufficient dimensions for accommodating dynamic vibration absorbers such as those illustrated in FIGS. 8 to 11. Dynamic vibration absorbers are often referred to in the art of vibration analysis as auxiliary mass dampers and are used to reduce the torsional or angular vibration in rotating elements. Although quantitative results are not yet available for the application of these absorbers to the tool spindle 20 of the apparatus of the preferred embodiment, it is believed that the optical surfaces generated by the apparatus of the preferred embodiment can still be improved by the use of such accessories.
A first suggested model of dynamic absorber is illustrated in FIGS. 8 and 9. A circular disk plate 60' has a series of vibration dampers comprising each a cylindrical mass 80 which is loosely confined in a through hole 82 in the disk plate 60'. Each cylindrical mass 80 has a circular groove 84 around its cylindrical surface for mating over a circular rib 86 around the inside surface of the through hole 82 such that the cylindrical mass 80 is held in a coplanar alignment with the circular plate 60'.
A second suggested type of dynamic absorber which is compatible with the shape of the circular face plate 52 or of the circular disk plate 60 is illustrated in FIGS. 10 and 11. In this example, a circular disk plate 60" has a groove around the rim portion thereof. A ring-shaped mass 90 is resiliently bonded into this groove by means of a layer of soft rubber 88 or other similar elastic material, such that the ring-shaped mass 90 can absorb fluctuations in the circumferential speed of the disk plate 60".
Although the dynamic vibration absorbers thus described and their effects in reducing torsional vibration are known in the art of vibration analysis and rotating machinery, the lens generating apparatus of the prior art do not have a structure for accommodating such devices. The tool spindle 20 of the apparatus of the preferred embodiment, however, has a circular face plate 52, and a circular disk plate 60 wherein the dampers may be advantageously readily incorporated.
While the above description provides a full and complete disclosure of the preferred embodiment of this invention, various modifications, alternate constructions and equivalents may be employed without departing from the true spirit and scope of the invention. Such changes might involve alternate materials, components, structural arrangements, sizes, construction features or the like. Therefore, the above description and the illustrations should not be construed as limiting the scope of the invention which is defined by the appended claims.
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An ophthalmic lens generating apparatus having a tool spindle comprising a motor, a lens surfacing tool and a coupling mounted between the motor and the lens surfacing tool for retaining the lens surfacing tool to the arbor of the motor. The apparatus of the present invention also comprises a first actuated table supporting the tool spindle in a movable manner along the longitudinal axis of the apparatus. A massive base is mounted beneath the first actuated table for supporting the table and for dampening radial vibrations of the tool spindle. The apparatus further comprises a lens holder for holding an ophthalmic lens in a plane substantially perpendicular to the longitudinal axis of the apparatus. A massive upright block is mounted on one end of the massive base behind the structural support supporting the lens holder, for dampening axial vibrations of the tool spindle and of the lens holder. The coupling of the tool spindle is a kinematic coupling having first and second disks having each substantial mass and radius of gyration. Thus, when the tool spindle rotates, both disks increase the nominal moment of inertia of the spindle and dampen the torsional vibrations of the spindle.
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BACKGROUND OF THE INVENTION
1. Field of the Invention
The invention relates to sports rackets.
2. Description of prior art:
Rackets are currently provided for different functions or sports and each provided with a hand holdable shaft having a longitudinal axis. The head or frame of each racket are generally circular and arranged with centre of the circle on the longitudinal axis. It is quite common and currently a requirement that a sportsman will have several rackets, one for each different sport or recreation but the handles are usually the same or generally the same for each racket. If the sportsman intends to play more than one sport, he must have two or more rackets. The leads to double or more of expense and similar extra storage and transport space.
SUMMARY OF THE INVENTION
It is an object of the invention to overcome or at least reduce this problem.
According to the invention there is provided a sports racket having a hand holdable shaft with a longitudinal axis, and two different generally circular playing surfaces arranged to be fixed edge to edge with their centres in line with the longitudinal axis.
The racket may have an integral frame which extends from the shaft and around the two playing surfaces.
The racket may have separate frames for each of the playing surfaces which are permanently fixed together.
The racket may have separate frames for each of the playing surfaces which are releasably fixed together. The frames are arranged to be fixed together with the one playing surface covering the other playing surface.
At least one of the playing surfaces is preferably transparent. At least one of the playing surfaces may be formed of tensioned strings. At least one of the playing surfaces may be formed by an apertured panel. The panel preferably has a solid central region.
BRIEF DESCRIPTION OF DRAWINGS
A sports racket according to the invention will now be described by way of example with reference to the accompanying drawings in which:
FIG. 1 is an isometric top view of the racket;
FIG. 2 is a plan view of the racket;
FIG. 3 is a side view of the racket;
FIG. 4 is an isometric view of an alternative embodiment of the racket;
FIG. 5 is an isometric view of the racket showing the top portion of the racket folded onto the bottom portion of the same; and
FIG. 6 is an isometric view of an alternative embodiment thereof.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
Referring to the drawings, the racket has a hand holdable shaft 10 with a longitudinal central axis shown as A--A in FIG. 2. Two circular playing surfaces 11 and 12 are provided and supported by an integral frame so that the playing surfaces are fixed or supported edge to edge each with their centres on the longitudinal axis. The playing surfaces may be provided in any suitable form such as by rigid or flexible solid panels, tensioned strings and so on. The surface 12 in this embodiment is formed by an apertured panel with a solid central region 12A.
It is preferable that the playing surface 11 is transparent, which could include for a practical purposes a stringed surface. If the surface is not transparent then some loss of view of an object to be hit during play when using the surface 12 may spoil the accuracy of striking the subject.
Generally stated, embodiments of the invention will be most often provided for casual games or recreation on the beach for example where fine balance and calibration of the racket may be less important than the convenience of being able to play with different objects. For example, a soft toy ball may be used together with the surface 11 and a more robust ball used together with the surface 12. Also, games may be played and the striker differently rewarded or handicapped, to even out the relative skills of the players, according to which surface he uses or is allowed to use in a contest.
The racket frame may be made in two parts and arranged to be releasably joined together. This allows the racket to be more efficiently stored or transported. It is also possible to arrange for the two parts to fit together so that the surface 12 covers the surface 11. This could provide a playing surface that combined a solid or apertured panel and strings, say, so that the racket could be switched, that is turned over, to strike a ball either with the strings or the solid panel to give a different acceleration or flight to the ball being struck with same or different shots at the choice of the striker.
Further, the racket may be used with the playing surface (and frame part) removed, for say hand-ball. The same racket could be used with the surface 12 attached, in the configuration as shown in the drawings, in which case the surface 12, then stringed, would be used for striking a tennis ball.
In any event, embodiments of the invent ion provide a single racket which can be used for more than one sport or recreation. This leads to a saving in cost and convenience for storage. Further, the two surfaces 11 and 12 may be used in combination either as shown in FIG. 1, say, or in an overlaying configuration. When the frame is formed in two parts, the overall size (i.e. length) of the racket can be significantly reduced by folding the surface 12 over the surface 11 where the two parts are hinged together or by removing the part with the surface 12 when they are releasably detachable from one another. As the same shaft is used for each configuration or each activity, there is not only an inherent saving in costs but the user can adapt or choose where preferred a particular form and size of grip on the shaft for his own preference.
It will be appreciated that the playing surfaces can not only be different in terms of their strength and performance but also different sizes. Also, the surfaces are normally circular or generally circular but it is intended that "generally circular" includes other shapes particularly elliptical shapes, known per se, in normal sports rackets.
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A sports racket has a handle 10 and two different playing surfaces 11 and 12. The same racket can therefore be conveniently used for different sports or recreations, or used for different purposes or different scoring in a single recreation.
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BACKGROUND OF THE INVENTION
1. Field of the Invention
The invention relates generally to the technical field of executing a program that is intended for a virtual machine, on a portable data carrier that has a processor. A portable data carrier of that kind may be especially a chip card in various forms or a chip module. More specifically, the invention relates to the controlled execution of a program in order to detect faults or attacks and in order to prevent the security of the portable data carrier from being compromised by such faults or attacks.
2. Description of the Related Art
Portable data carriers that have a virtual machine for executing programs are known, for example, under the trademark Java Card™. Such data carriers are described in Chapter 5.10.2 of the book “Handbuch der Chipkarten” by W. Rankl and W. Effing, Hanser Verlag, 3 rd edition, 1999, pages 261 to 281. A detailed specification of the Java Card standard, the virtual machine JCVM (Java Card Virtual Machine) used therewith and of the programs (Java Card Applets) that are executed is to be found on the Internet pages of the company Sun Microsystems, Inc., at java.sun.com/products/javacard.
Portable data carriers are frequently used for applications where security is crucial, for example in connection with financial transactions or in electronic signature of documents. Techniques for attacking portable data carriers have already become known in which the execution of a program is disrupted by external interference. Such disruption may be caused, in particular, by voltage pulses, by the effect of heat or cold, by electric or magnetic fields, electromagnetic waves or particle radiation. For example, it is possible to alter register contents in the processor or memory contents by directing flashes of light onto the exposed semiconductor chip. Such interference may possibly compromise the security of the data carrier if, for example, the data carrier outputs a defectively encrypted text which, when analysed, allows inferences to be made about a secret key.
There is therefore the problem of safeguarding a data carrier of the kind mentioned in the introduction from being compromised by attacks that interfere with the execution of a program by a virtual machine.
GB 2 353 113 A discloses a computer network that is capable of compensating for software faults to a certain extent. At least two computers, each executing a virtual machine, are provided in that computer network. If one of the virtual machines is found to be operating incorrectly, execution of the program is continued by the other virtual machine or machines.
The system known from GB 2 353 113 A is foreign to the generic type in question here, since it is intended not for a portable data carrier but for a complex network comprising a plurality of computers. The virtual machines are executed by a plurality of processors which are only loosely coupled to one another. Execution of the program is continued even when one virtual machine is disrupted. That teaching is not suitable for application in a portable data carrier having a single processor.
SUMMARY OF THE INVENTION
An object of the invention is to avoid the problems of the prior art at least to some extent. In particular, the invention should provide a technique for the controlled execution of a program, the program being intended for a virtual machine, on a portable data carrier, by means of which technique security risks in the event of an attack or a malfunction are avoided. In some embodiments, reliable protection is to be achieved with as little loss of performance of the portable data carrier as possible.
According to the invention, the above object is completely or partially achieved by a method for the controlled execution of a program, the program being intended for a virtual machine, on a portable data carrier, wherein the data carrier has a processor which executes at least a first and a second virtual machine, the program is executed both by the first and by the second virtual machine, the operating state of the first virtual machine and the operating state of the second virtual machine are checked during execution of the program for correspondence, and execution of the program is aborted if a difference is found between the operating state of the first virtual machine and the operating state of the second virtual machine.
Further according to the invention, the above object is completely or partially achieved by a portable data carrier having a processor, an operating system, at least a first and a second virtual machine, and a program, wherein the processor executes both the first and second virtual machine, the program is executed both by the first and by the second virtual machine, the operating system controls the processor to check the operating state of the first virtual machine and the operating state of the second virtual machine during execution of the program for correspondence, and the operating system controls the processor to abort execution of the program if a difference is found between the operating state of the first virtual machine and the operating state of the second virtual machine.
Yet further according to the invention, the above object is completely or partially achieved by a computer program product having program instructions for causing a processor of a portable data carrier to perform a method for the controlled execution of a program, the program being intended for a virtual machine, wherein the processor executes at least a first and a second virtual machine, the program is executed both by the first and by the second virtual machine, the operating state of the first virtual machine and the operating state of the second virtual machine are checked during execution of the program for correspondence, and execution of the program is aborted if a difference is found between the operating state of the first virtual machine and the operating state of the second virtual machine.
The invention is founded on the basic idea of having the one processor of the portable data carrier execute a plurality of virtual machines which in turn execute one and the same program. This measure provides a redundancy in the program execution, which can be utilised to detect malfunctions. It is a surprising result of the present invention that such a redundancy can also be obtained in a portable data carrier that has only a single processor.
According to the invention, the execution of the program is aborted if a difference is found between the operating states of the virtual machines. An attempt is not made, therefore, to identify one of the virtual machines as operating correctly and to continue execution of the program with that virtual machine. By aborting the program as provided according to the invention, especially high security against attacks is achieved.
The invention offers the considerable advantage that it can be implemented without any difficulty on conventional hardware. In addition, no adaptation of the program that is to be executed to the attack protection according to the invention is required. All programs intended for the standard virtual machine will run unchanged on the data carriers configured in accordance with the invention, which greatly furthers the acceptance of the invention.
When the operating states of the virtual machines are being checked for correspondence, the comparison that takes place is preferably not a complete comparison. Rather, in preferred embodiments, merely a comparison of contents of a few important registers and/or memory contents is provided. The important registers in question may, for example, be the program counters and/or the stack pointers of the virtual machines. An example of important memory contents that are compared with one another in some embodiments of the invention is the most recent (“uppermost”) element in the stacks of the virtual machines at the time in question.
Since the virtual machines on the portable data carrier are executed by a single processor, an interleaved program sequence generally takes place. That does not, however, exclude individual operations being executed truly in parallel if the processor of the portable data carrier is equipped to do so.
Checking of the operating states of the virtual machines may be carried out at any of the times when the virtual machines should have identical states if operating correctly. Although checking is not in principle tied, therefore, to the instruction boundaries of the program executed, in preferred embodiments it is provided that this checking is performed after each execution of an instruction of the program by the virtual machines. In alternative embodiments, the comparison of the virtual machines either may be carried out as soon as parts of instructions have been executed or may not be carried out until several instructions have been executed in each case.
Preferably, each instruction of the program is executed first by the first virtual machine and then by the second virtual machine. In some embodiments, execution of the instruction by the first virtual machine is first completed before the processor of the portable data carrier begins to execute the instruction using the second virtual machine. In other embodiments, on the other hand, the processor may execute each of a number of portions of the instruction first on the first virtual machine and then on the second virtual machine, provided, however, that the first virtual machine does not lag behind the second virtual machine.
Owing to the use of at least two—and in some embodiments more—virtual machines, the computing capacity available for each virtual machine is correspondingly reduced. With regard to the actual program run time, however, it should be borne in mind that, in a typical portable data carrier, a great deal of time is required for write operations to a non-volatile memory of the data carrier.
In preferred embodiments, therefore, it is provided that the virtual machines access a common heap in the non-volatile memory of the portable data carrier, with write operations being performed by only one of the virtual machines. The other virtual machine(s) may either skip the write operation entirely or, instead of performing the write operation, may check whether the location that is to be written to in the memory already contains the value that is to be written. If the program to be executed contains a large number of write operations to the heap, these will require a considerable proportion of the total run time. Through the use of the embodiment of the invention just described, that portion of the total run time remains unchanged whereas only the purely computing time of the processor—which, as mentioned, matters less—increases.
The portable data carrier according to the invention is preferably in the form of a chip card or a chip module. The computer program product according to the invention has program instructions for implementing the method according to the invention. Such a computer program product may be a physical medium, for example a semiconductor memory or a diskette or a CD-ROM, on which a program for executing a method according to the invention is stored. The computer program product may, however, alternatively be a non-physical medium, for example a signal transmitted via a computer network. The computer program product may especially be intended for use in connection with the production and/or initialisation and/or personalisation of chip cards or other data carriers.
In preferred embodiments, the data carrier and/or the computer program product have features corresponding to the features described above and/or to the features mentioned in the dependent method claims.
BRIEF DESCRIPTION OF THE DRAWINGS
Further features, advantages and objects of the invention will be apparent from the following detailed description of an illustrative embodiment and a number of alternative embodiments. Reference will be made to the schematic drawings, in which:
FIG. 1 is a block diagram showing functional units of a portable data carrier according to an illustrative embodiment of the invention,
FIG. 2 is a conceptual illustration of components that are active when the program is being executed by the portable data carrier,
FIG. 3 is a flow diagram of a main loop which is followed for each program instruction during execution of the program,
FIG. 4 is a flow diagram of the checking of the operating states of the virtual machines for correspondence.
DETAILED DESCRIPTION OF EXEMPLARY EMBODIMENTS
In the illustrative embodiment under consideration, the data carrier 10 shown in FIG. 1 is in the form of a chip card conforming to the Java Card standard. The data carrier has, on a single semiconductor chip, a processor 12 , a plurality of memory areas implemented in various technologies, and an interface circuit 14 for contactless or contact-bound communication. In the illustrative embodiment under consideration, a working memory 16 , a read-only memory 18 and a non-volatile memory 20 are provided as memory areas. The working memory 16 is in the form of RAM, the read-only memory 18 in the form of mask-programmed ROM and the non-volatile memory 20 in the form of electrically erasable and programmable EEPROM. Write accesses to the non-volatile memory 20 are relatively time-consuming and require, for example, thirty times as long as a read access.
In the read-only memory 18 —and partly also in the non-volatile memory 20 —there is an operating system 22 which provides a multitude of functions and services. The operating system 22 comprises inter alia a code module 24 that implements a virtual machine—a JCVM (Java Card Virtual Machine) in the illustrative embodiment under consideration.
FIG. 1 shows by way of example a program 26 to be executed which is located in the non-volatile memory 20 and which, in the illustrative embodiment under consideration, is in the form of a Java Card Applet. The program 26 may also be held partly or completely in the read-only memory 18 , and further programs for execution by the portable data carrier 10 may be provided. One area in the non-volatile memory 20 is reserved as a heap 28 in order for objects and other data structures to be held during execution of the program.
In order to execute the program 26 under the control of the operating system 22 the processor 12 starts two instances of the code module 24 each of which forms a virtual machine VM, VM′. As shown in FIG. 2 , the two virtual machines VM, VM′ execute one and the same program 26 which is present in the non-volatile memory 20 only once. When the two virtual machines VM, VM′ fetch an instruction of the program 26 , therefore, they access identical addresses in the non-volatile memory 20 .
As the program runs, the two virtual machines VM, VM′ perform access operations to the common heap 28 . Once again, the objects and data structures stored in the heap 28 are each present only once. The first virtual machine VM performs both read operations R and write operations W on the heap 28 . The second virtual machine VM′, on the other hand, although performing read operations R′, does not perform any write operations but, rather, performs verification operations V.
The virtual machines VM, VM′ each have their own registers, FIG. 2 showing for each of the latter a program counter PC, PC′ and a stack pointer SP, SP′. Those registers are disposed in the working memory 16 or are implemented by registers of the processor 12 . Each virtual machine VM, VM′ further has its own stack ST, ST′ each disposed in a respective area of the working memory 16 . The most recent (“uppermost”) entries in the stacks ST, ST′ at the time, to which the respective stack pointers SP, SP′ point, are labeled @SP and @SP′ in FIG. 2 .
As a modification of the illustration shown in FIG. 1 , the virtual machines VM, VM′ may be disposed in separate hardware: in separate memories 20 which may also be assigned to separate processors. It may also be provided that the virtual machines VM, VM′ be in the form of hardware components.
When the program 26 is being executed, the operating system 22 follows the loop shown in FIG. 3 . One pass of the loop is made for each instruction of the program 26 . The instruction is first executed in step 30 by the first virtual machine VM. There are no differences here compared with the execution of a program in a prior art system by a single virtual machine. In particular, the first virtual machine maintains its registers PC and SP and the stack ST and, where appropriate, performs a read operation R from and/or a write operation W to the heap 28 .
When execution of the instruction by the first virtual machine VM has been completed, in step 32 the second virtual machine VM′ executes the same instruction of the program 26 again. In this case also, maintenance of the registers PC′ and SP′, maintenance of the stack ST′ and, where appropriate, an operation R′ of reading from the heap 28 are performed in the usual manner.
Execution of the instruction by the second virtual machine VM′ differs, however, from execution of the instruction by the first virtual machine VM in that, instead of any write operation which may be specified by the instruction, a comparison operation V is performed in which the value that is actually to be written to the heap 28 is compared with the current contents of the heap 28 at the address that is to be written to. If the calculation operations of the two virtual machines VM, VM′ correspond, then the first virtual machine VM has already written the value that is now determined in step 32 by the second virtual machine VM′ to the heap 28 in step 30 . The verification operation V in step 32 therefore yields a correspondence, and the calculation sequence is continued. If, on the other hand, a difference is found between the values in step 32 , that indicates a malfunction of one of the virtual machines VM, VM′. Execution of the program is then aborted as being defective. That possibility is indicated in FIG. 3 by a dashed-line arrow.
After the program instruction has been executed by both virtual machines VM, VM′, in step 34 it is examined whether the operating states reached by the two virtual machines correspond. For that purpose, in the illustrative embodiment described herein only some of the register and memory values are examined for correspondence, as shown in FIG. 4 . First, in sub-step 34 . 1 , it is examined whether the two program counters PC, PC′ have the same value after the instruction has been executed. If that is the case, in sub-step 34 . 2 examination of the two stack pointers SP, SP′ for correspondence takes place. If that test also is successful, in sub-step 34 . 3 it is examined whether the most recent entries @SP, @SP′ in the stacks ST, ST′ at the time, that is to say, the entries to which the stack pointers SP, SP′ point, are identical.
If a correspondence has been found in all three queries 34 . 1 , 34 . 2 , 34 . 3 , step 34 ( FIG. 3 ) assumes correct execution of the program by the two virtual machines VM, VM′. A return is then made to the start of the loop, and the next instruction of the program 26 is executed first by the first and then by the second virtual machine VM, VM′.
If, however, a difference is found in one of the three sub-steps 34 . 1 , 34 . 2 , 34 . 3 during checking of the operating states, that indicates a malfunction of one of the two virtual machines VM, VM′. That in turn is regarded as an indication of a fault or of an attack on the hardware of the portable data carrier 10 . Since the processor 12 performs steps 30 to 32 in strict succession, when an attack occurs, for example by a flash of light, only the operation of one of the two virtual machines VM, VM′ is affected. Even in the event of a rapid succession of light flashes it would be improbable that both virtual machines VM, VM′ would be disrupted in the same manner.
If a difference in the operating states is found in step 34 , execution of the program is aborted as being defective. The operating system 22 then puts the data carrier 10 into a secure state. It is to be particularly noted in this connection that, after a program abort, the data carrier 10 is not intended to perform any more output operations. Depending on the security requirements to be met by the data carrier 10 , it may be provided that the data carrier 10 is ready for use again after a normal reset, or a special enable procedure may be required, or the data carrier 10 may be completely deactivated.
The particulars contained in the above description of sample embodiments should not be construed as limitations of the scope of the invention, but rather as exemplifications of preferred embodiments thereof. Accordingly, the scope of the invention should be determined not by the embodiments illustrated, but by the appended claims and their legal equivalents.
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In a method for the controlled execution of a program ( 26 ), the program ( 26 ) being intended for a virtual machine (VM, VM′), on a portable data carrier, wherein the data carrier has a processor that executes at least a first and a second virtual machine (VM, VM′), the program ( 26 ) is executed both by the first and by the second virtual machine (VM, VM′). If, during execution of the program ( 26 ), a difference is found between the operating state of the first virtual machine (VM) and the operating state of the second virtual machine (VM′), execution of the program is aborted. A data carrier and a computer program product exhibit corresponding features. The invention provides a technique for the controlled execution of a program, which technique prevents security risks due to an attack or a malfunction of the data carrier.
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[0001] This application is a continuation application of U.S. patent application Ser. No. 09/602,963, filed Jun. 23, 2000.
BACKGROUND OF THE INVENTION
[0002] 1. Field of the Invention
[0003] The present invention relates generally to signal transmission and reception in a wireless code division multiple access (CDMA) communication system. More specifically, the invention relates to a system and method of transmission using an antenna array to improve signal reception in a wireless CDMA communication system.
[0004] 2. Description of the Prior Art
[0005] A prior art CDMA communication system is shown in FIG. 1. The communication system has a plurality of base stations 20 - 32 . Each base station 20 communicates using spread spectrum CDMA with user equipment (UEs) 34 - 38 within its operating area. Communications from the base station 20 to each UE 34 - 38 are referred to as downlink communications and communications from each UE 34 - 38 to the base station 20 are referred to as uplink communications.
[0006] Shown in FIG. 2 is a simplified CDMA transmitter and receiver. A data signal having a given bandwidth is mixed by a mixer 40 with a pseudo random chip code sequence producing a digital spread spectrum signal for transmission by an antenna 42 . Upon reception at an antenna 44 , the data is reproduced after correlation at a mixer 46 with the same pseudo random chip code sequence used to transmit the data. By using different pseudo random chip code sequences, many data signals use the same channel bandwidth. In particular, a base station 20 will communicate signals to multiple UEs 34 - 38 over the same bandwidth.
[0007] For timing synchronization with a receiver, an unmodulated pilot signal is used. The pilot signal allows respective receivers to synchronize with a given transmitter allowing despreading of a data signal at the receiver. In a typical CDMA system, each base station 20 sends a unique pilot signal received by all UEs 34 - 38 within communicating range to synchronize forward link transmissions. Conversely, in some CDMA systems, for example in the B-CDMA™ air interface, each UE 34 - 38 transmits a unique assigned pilot signal to synchronize reverse link transmissions.
[0008] When a UE 34 - 36 or a base station 20 - 32 is receiving a specific signal, all the other signals within the same bandwidth are noise-like in relation to the specific signal. Increasing the power level of one signal degrades all other signals within the same bandwidth. However, reducing the power level too far results in an undesirable received signal quality. One indicator used to measure the received signal quality is the signal to noise ratio (SNR). At the receiver, the magnitude of the desired received signal is compared to the magnitude of the received noise. The data within a transmitted signal received with a high SNR is readily recovered at the receiver. A low SNR leads to loss of data.
[0009] To maintain a desired signal to noise ratio at the minimum transmission power level, most CDMA systems utilize some form of adaptive power control. By minimizing the transmission power, the noise between signals within the same bandwidth is reduced. Accordingly, the maximum number of signals received at the desired signal to noise ratio within the same bandwidth is increased.
[0010] Although adaptive power control reduces interference between signals in the same bandwidth, interference still exists limiting the capacity of the system. One technique for increasing the number of signals using the same radio frequency (RF) spectrum is to use sectorization. In sectorization, a base station uses directional antennas to divide the base station's operating area into a number of sectors. As a result, interference between signals in differing sectors is reduced. However, signals within the same bandwidth within the same sector interfere with one another. Additionally, sectorized base stations commonly assign different frequencies to adjoining sectors decreasing the spectral efficiency for a given frequency bandwidth. Accordingly, there exists a need for a system which further improves the signal quality of received signals without increasing transmitter power levels.
SUMMARY OF THE INVENTION
[0011] The invention provides for transmission and reception of a data signal using a plurality of transmitting antennas. Each antenna transmits a different reference signal having a pseudo random chip code sequence. A receiver filters each transmitted reference signal using that reference signal's chip code. The filtered reference signals are weighted and combined. Each reference signal's weight is adaptively adjusted in part on a signal quality of the combined signal. A data signal is transmitted such that different spread spectrum versions of the data signal are transmitted from each transmitting antenna. Each version having a different chip code identifier. Upon reception, each version is filtered with its associated chip code. The filtered versions are weighted in accordance with the adjusted weights associated with the reference signal of the respective antenna.
BRIEF DESCRIPTION OF THE DRAWINGS
[0012] [0012]FIG. 1 is a prior art wireless spread spectrum CDMA communication system.
[0013] [0013]FIG. 2 is a prior art spread spectrum CDMA transmitter and receiver.
[0014] [0014]FIG. 3 is the transmitter of the invention.
[0015] [0015]FIG. 4 is the transmitter of the invention transmitting multiple data signals.
[0016] [0016]FIG. 5 is the pilot signal receiving circuit of the invention.
[0017] [0017]FIG. 6 is the data signal receiving circuit of the invention.
[0018] [0018]FIG. 7 is an embodiment of the pilot signal receiving circuit.
[0019] [0019]FIG. 8 is a least mean squarred weighting circuit.
[0020] [0020]FIG. 9 is the data signal receiving circuit used with the pilot signal receiving circuit of FIG. 7.
[0021] [0021]FIG. 10 is an embodiment of the pilot signal receiving circuit where the output of each RAKE is weighted.
[0022] [0022]FIG. 11 is the data signal receiving circuit used with the pilot signal receiving circuit of FIG. 10.
[0023] [0023]FIG. 12 is an embodiment of the pilot signal receiving circuit where the antennas of the transmitting array are closely spaced.
[0024] [0024]FIG. 13 is the data signal receiving circuit used with the pilot signal receiving circuit of FIG. 12.
[0025] [0025]FIG. 14 is an illustration of beam steering in a CDMA communication system.
[0026] [0026]FIG. 15 is a beam steering transmitter.
[0027] [0027]FIG. 16 is a beam steering transmitter transmitting multiple data signals.
[0028] [0028]FIG. 17 is the data receiving circuit used with the transmitter of FIG. 14.
[0029] [0029]FIG. 18 is a pilot signal receiving circuit used when uplink and downlink signals use the same frequency.
[0030] [0030]FIG. 19 is a transmitting circuit used with the pilot signal receiving circuit of FIG. 18.
[0031] [0031]FIG. 20 is a data signal receiving circuit used with the pilot signal receiving circuit of FIG. 18.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0032] The preferred embodiments will be described with reference to the drawing figures where like numerals represent like elements throughout. FIG. 3 is a transmitter of the invention. The transmitter has an array of antennas 48 - 52 , preferably 3 or 4 antennas. For use in distinguishing each antenna 48 - 52 , a different signal is associated with each antenna 56 - 60 . The preferred signal to associate with each antenna is a pilot signal as shown in FIG. 3. Each spread pilot signal is generated by a pilot signal generator 56 - 60 using a different pseudo random chip code sequence and is combined by combiners 62 - 66 with the respective spread data signal. Each spread data signal is generated using data signal generator 54 by mixing at mixers 378 - 382 the generated data signal with a different pseudo random chip code sequence per antenna 48 - 52 , D1 -D N . The combined signals are modulated to a desired carrier frequency and radiated through the antennas 48 - 52 of the array.
[0033] By using an antenna array, the transmitter utilizes spacial diversity. If spaced far enough apart, the signals radiated by each antenna 48 - 52 will experience different multipath distortion while traveling to a given receiver. Since each signal sent by an antenna 48 - 52 will follow multiple paths to a given receiver, each received signal will have many multipath components. These components create a virtual communication channel between each antenna 48 - 52 of the transmitter and the receiver. Effectively, when signals transmitted by one antenna 48 - 52 over a virtual channel to a given receiver are fading, signals from the other antennas 48 - 52 are used to maintain a high received SNR. This effect is achieved by the adaptive combining of the transmitted signals at the receiver.
[0034] [0034]FIG. 4 shows the transmitter as used in a base station 20 to send multiple data signals. Each spread data signal is generated by mixing at mixers 360 - 376 a corresponding data signal from generators 74 - 78 with differing pseudo random chip code sequences D 11 -D NM . Accordingly, each data signal is spread using a different pseudo random chip code sequence per antenna 48 - 52 , totaling N×M code sequences. N is the number of antennas and M is the number of data signals. Subsequently, each spread data signal is combined with the spread pilot signal associated with the antenna 48 - 52 . The combined signals are modulated and radiated by the antennas 48 - 52 of the array.
[0035] The pilot signal receiving circuit is shown in FIG. 5. Each of the transmitted pilot signals is received by the antenna 80 . For each pilot signal, a despreading device, such as a RAKE 82 - 86 as shown in the FIG. 5 or a vector correlator, is used to despread each pilot signal using a replica of the corresponding pilot signal's pseudo random chip code sequence. The despreading device also compensates for multipath in the communication channel. Each of the recovered pilot signals is weighted by a weighting device 88 - 92 . Weight refers to both magnitude and phase of the signal. Although the weighting is shown as being coupled to a RAKE, the weighting device preferably also weights each finger of the RAKE. After weighting, all of the weighted recovered pilot signals are combined in a combiner 94 . Using an error signal generator 98 , an estimate of the pilot signal provided by the weighted combination is used to create an error signal. Based on the error signal, the weights of each weighting device 88 - 92 are adjusted to minimize the error signal using an adaptive algorithm, such as least mean squared (LMS) or recursive least squares (RLS). As a result, the signal quality of the combined signal is maximized.
[0036] [0036]FIG. 6 depicts a data signal receiving circuit using the weights determined by the pilot signal recovery circuit. The transmitted data signal is recovered by the antenna 80 . For each antenna 48 - 52 of the transmitting array, the weights from a corresponding despreading device, shown as a RAKE 82 - 86 , are used to filter the data signal using a replica of the data signal's spreading code used for the corresponding transmitting antenna. Using the determined weights for each antenna's pilot signal, each weighting device 106 - 110 weights the RAKE's despread signal with the weight associated with the corresponding pilot. For instance, the weighting device 88 corresponds to the transmitting antenna 48 for pilot signal 1 . The weight determined by the pilot RAKE 82 for pilot signal 1 is also applied at the weighting device 106 of FIG. 6. Additionally, if the weights of the RAKE's fingers were adjusted for the corresponding pilots signal's RAKE 82 - 86 , the same weights will be applied to the fingers of the data signal's RAKE 100 - 104 . After weighting, the weighted signals are combined by the combiner 112 to recover the original data signal.
[0037] By using the same weights for the data signal as used with each antenna's pilot signal, each RAKE 82 - 86 compensates for the channel distortion experienced by each antenna's signals. As a result, the data signal receiving circuit optimizes the data signals reception over each virtual channel. By optimally combining each virtual channel's optimized signal, the received data signal's signal quality is increased.
[0038] [0038]FIG. 7 shows an embodiment of the pilot signal recovery circuit. Each of the transmitted pilots are recovered by the receiver's antenna 80 . To despread each of the pilots, each RAKE 82 - 86 utilizes a replica of the corresponding pilot's pseudo random chip code sequence, P 1 -P N . Delayed versions of each pilot signal are produced by delay devices 114 - 124 . Each delayed version is mixed by a mixer 126 - 142 with the received signal. The mixed signals pass through sum and dump circuits 424 - 440 and are weighted using mixers 144 - 160 by an amount determined by the weight adjustment device 170 . The weighted multipath components for each pilot are combined by a combiner 162 - 164 . Each pilot's combined output is combined by a combiner 94 . Since a pilot signal has no data, the combined pilot signal should have a value of 1+j0. The combined pilot signal is compared to the ideal value, 1+j0, at a subtractor 168 . Based on the deviation of the combined pilot signal from the ideal, the weight of the weighting devices 144 - 160 are adjusted using an adaptive algorithm by the weight adjustment device 170 .
[0039] A LMS algorithm used for generating a weight is shown in FIG. 8. The output of the subtractor 168 is multiplied using a mixer 172 with the corresponding despread delayed version of the pilot. The multiplied result is amplified by an amplifier 174 and integrated by an integrator 176 . The integrated result is used to weight, W 1M , the RAKE finger.
[0040] The data receiving circuit used with the embodiment of FIG. 7 is show for a base station receiver in FIG. 9. The received signal is sent to a set of RAKEs 100 - 104 respectively associated with each antenna 48 - 52 of the array. Each RAKE 100 - 104 , produces delayed versions of the received signal using delay devices 178 - 188 . The delayed versions are weighted using mixers 190 - 206 based on the weights determined for the corresponding antenna's pilot signal. The weighted data signals for a given RAKE 100 - 104 are combined by a combiner 208 - 212 . One combiner 208 - 212 is associated with each of the N transmitting antennas 48 - 52 . Each combined signal is despread M times by mixing at a mixer 214 - 230 the combined signal with a replica of the spreading codes used for producing the M spread data signals at the transmitter, D 11 -D NM . Each despread data signal passes through a sum and dump circuit 232 - 248 . For each data signal, the results of the corresponding sum and dump circuits are combined by a combiner 250 - 254 to recover each data signal.
[0041] Another pilot signal receiving circuit is shown in FIG. 10. The despreading circuits 82 - 86 of this receiving circuit are the same as FIG. 7. The output of each RAKE 82 - 86 is weighted using a mixer 256 - 260 prior to combining the despread pilot signals. After combining, the combined pilot signal is compared to the ideal value and the result of the comparison is used to adjust the weight of each RAKE's output using an adaptive algorithm. To adjust the weights within each RAKE 82 - 86 , the output of each RAKE 82 - 86 is compared to the ideal value using a subtractor 262 - 266 . Based on the result of the comparison, the weight of each weighting device 144 - 160 is determined by the weight adjustment devices 268 - 272 .
[0042] The data signal receiving circuit used with the embodiment of FIG. 10 is shown in FIG. 11. This circuit is similar to the data signal receiving circuit of FIG. 9 with the addition of mixers 274 - 290 for weighting the output of each sum and dump circuit 232 - 248 . The output of each sum and dump circuit 232 - 248 is weighted by the same amount as the corresponding pilot's RAKE 82 - 86 was weighted. Alternatively, the output of each RAKE's combiner 208 - 212 may be weighted prior to mixing by the mixers 214 - 230 by the amount of the corresponding pilot's RAKE 82 - 86 in lieu of weighting after mixing.
[0043] If the spacing of the antennas 48 - 52 in the transmitting array is small, each antenna's signals will experience a similar multipath environment. In such cases, the pilot receiving circuit of FIG. 12 may be utilized. The weights for a selected one of the pilot signals are determined in the same manner as in FIG. 10. However, since each pilot travels through the same virtual channel, to simplify the circuit, the same weights are used for despreading the other pilot signals. Delay devices 292 - 294 produce delayed versions of the received signal. Each delayed version is weighted by a mixer 296 - 300 by the same weight as the corresponding delayed version of the selected pilot signal was weighted. The outputs of the weighting devices are combined by a combiner 302 . The combined signal is despread using replicas of the pilot signals' pseudo random chip code sequences, P 2 -P n , by the mixers 304 - 306 . The output of each pilot's mixer 304 - 306 is passed through a sum and dump circuit 308 - 310 . In the same manner as FIG. 10, each despread pilot is weighted and combined.
[0044] The data signal recovery circuit used with the embodiment of FIG. 12 is shown in FIG. 13. Delay devices 178 - 180 produce delayed versions of the received signal. Each delayed version is weighted using a mixer 190 - 194 by the same weight as used by the pilot signals in FIG. 12. The outputs of the mixers are combined by a combiner 208 . The output of the combiner 208 is inputted to each data signal despreader of FIG. 13.
[0045] The invention also provides a technique for adaptive beam steering as illustrated in FIG. 14. Each signal sent by the antenna array will constructively and destructively interfere in a pattern based on the weights provided each antenna 48 - 52 of the array. As a result, by selecting the appropriate weights, the beam 312 - 316 of the antenna array is directed in a desired direction.
[0046] [0046]FIG. 15 shows the beam steering transmitting circuit. The circuit is similar to the circuit of FIG. 3 with the addition of weighting devices 318 - 322 . A target receiver will receive the pilot signals transmitted by the array. Using the pilot signal receiving circuit of FIG. 5, the target receiver determines the weights for adjusting the output of each pilot's RAKE. These weights are also sent to the transmitter, such as by using a signaling channel. These weights are applied to the spread data signal as shown in FIG. 15. For each antenna, the spread data signal is given a weight by the weighting devices 318 - 322 corresponding to the weight used for adjusting the antenna's pilot signal at the target receiver providing spatial gain. As a result, the radiated data signal will be focused towards the target receiver. FIG. 16 shows the beam steering transmitter as used in a base station sending multiple data signals to differing target receivers. The weights received by the target receiver are applied to the corresponding data signals by weighting devices 324 - 340 .
[0047] [0047]FIG. 17 depicts the data signal receiving circuit for the beam steering transmitter of FIGS. 15 and 16. Since the transmitted signal has already been weighted, the data signal receiving circuit does not require the weighting devices 106 - 110 of FIG. 6.
[0048] The advantage of the invention's beam steering are two-fold. The transmitted data signal is focused toward the target receiver improving the signal quality of the received signal. Conversely, the signal is focused away from other receivers reducing interference to their signals. Due to both of these factors, the capacity of a system using the invention's beam steering is increased. Additionally, due to the adaptive algorithm used by the pilot signal receiving circuitry, the weights are dynamically adjusted. By adjusting the weights, a data signal's beam will dynamically respond to a moving receiver or transmitter as well as to changes in the multipath environment.
[0049] In a system using the same frequency for downlink and uplink signals, such as time division duplex (TDD), an alternate embodiment is used. Due to reciprocity, downlink signals experience the same multipath environment as uplink signals send over the same frequency. To take advantage of reciprocity, the weights determined by the base station's receiver are applied to the base station's transmitter. In such a system, the base station's receiving circuit of FIG. 18 is co-located, such as within a base station, with the transmitting circuit of FIG. 19.
[0050] In the receiving circuit of FIG. 18, each antenna 48 - 52 receives a respective pilot signal sent by the UE. Each pilot is filtered by a RAKE 406 - 410 and weighted by a weighting device 412 - 416 . The weighted and filtered pilot signals are combined by a combiner 418 . Using the error signal generator 420 and the weight adjustment device 422 , the weights associated with the weighting devices 412 - 416 are adjusted using an adaptive algorithm.
[0051] The transmitting circuit of FIG. 19 has a data signal generator 342 to generate a data signal. The data signal is spread using mixer 384 . The spread data signal is weighted by weighting devices 344 - 348 as were determined by the receiving circuit of FIG. 19 for each virtual channel.
[0052] The circuit of FIG. 20 is used as a data signal receiving circuit at the base station. The transmitted data signal is received by the multiple antennas 48 - 52 . A data RAKE 392 - 396 is coupled to each antenna 48 - 52 to filter the data signal. The filtered data signals are weighted by weighting devices 398 - 402 by the weights determined for the corresponding antenna's received pilot and are combined at combiner 404 to recover the data signal. Since the transmitter circuit of FIG. 19 transmits the data signal with the optimum weights, the recovered data signal at the UE will have a higher signal quality than provided by the prior art.
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The invention provides for transmission and reception of a data signal using a plurality of transmitting antennas. Each antenna transmits a different reference signal having a pseudo random chip code sequence. A receiver filters each transmitted reference signal using that reference signal's chip code. The filtered reference signals are weighted and combined. Each reference signal's weight is adaptively adjusted in part on a signal quality of the combined signal. A data signal is transmitted such that different spread spectrum versions of the data signal are transmitted from each transmitting antenna. Each version having a different chip code identifier. Upon reception, each version is filtered with its associated chip code. The filtered versions are weighted in accordance with the adjusted weights associated with the reference signal of the respective antenna.
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BACKGROUND ART
[0001] The concept of apoptosis was first proposed in 1972 by Kerr et al, and refers to a well organized and autonomous death form different from cell necrosis, which is controlled by multiple genes. It plays an indispensable role in the evolution, homeostatic process and development of multiple systems of organisms (Renehan et al., 2001; Nijhawan et al., 2000; Opferman and Korsmeyer, 2003; Osborne, 1996). The mechanism of apoptosis is highly complicated, and involves the implication of a series of energy-dependent cascade reactions. Till now, two major apoptotic pathways have been found: extrinsic pathway or death receptor pathway and intrinsic pathway or mitochondrial pathway, and there is a link between the two pathways (Igney and Krammer, 2002); there is another pathway known as perforin/granzyme pathway, whereby granzyme A or granzyme B is involved in T cell-mediated cytotoxicity and perforin-granzyme dependent cell killing. Finally, the extrinsic pathway, intrinsic pathway and granzyme B pathway converge to the same execution pathway, i.e. caspase-3 cleavage, DNA breakage, cytoskeletal and nucleoprotein degradation, protein crosslink, formation of apoptotic bodies, expression of ligand of phagocytic cell receptor, and eventually being swallowed. The apoptosis triggered by extrinsic pathway requires the interaction between ligands and transmembrane death receptors, and these death receptors belong to the tumor necrosis factor (TNF) receptor superfamily (Locksley et al., 2001). The members of TNF receptor superfamily share similar cysteine-rich extracellular binding domain and an intracellular death domain with approximately 80 amino acids (Ashkenazi and Dixit, 1998). Death domain plays a key role in the transmission of death signals from the cell surface to inside of the cell, at present, the well-established ligand/death receptor pathways include FasL/FasR, TNF-α/TNFR1, Apo3L/DR3, Apo2L/DR4 and Apo2L/DR5 (Chicheportiche et al., 1997; Ashkenazi et al., 1998; Peter and Kramer, 1998; Suliman et al., 2001; Rubio-Moscardo et al., 2005).
[0002] Apoptosis occurs under many physiological conditions, such as embryonic development, and clonal selection in the immune system (Itoh et al., 1991). Apoptosis under the physiological conditions is controlled by precise regulation, and excessively upregulation or downregulation of apoptosis will result in pathological changes, such as developmental defects, autoimmune disease, neurodegenerative disease, or malignancy and the like. Malignancy is now considered as the result of excessive cell proliferation and/or decrease of cell removal due to the dysfunction of the normal cell cycle control mechanisms (King and Cidlowski, 1998). The inhibition of apoptosis plays a key role in the onset and development of some tumors (Kerr et al., 1994).
[0003] In tumor cells, its apoptosis can be inhibited through a variety of molecular mechanisms, such as the expression of anti-apoptotic protein, downregulation of expression of pro-apoptotic proteins or inactivation of mutation of pro-apoptotic protein. Based on the understanding of the role of apoptosis in the onset and development of tumor and signal transduction pathways of apoptosis, drugs promoting apoptosis of tumor cells have been developed or are developed. The development of the novel drugs targeting extracellular apoptotic pathway of the death receptor is one research focus of recent years, in particular, DR4/DR5. Several drug candidates targeting DR4/DR5 are now in clinical trials.
[0004] TNF related apoptosis inducing ligand (TRAIL) gene was first cloned and named by Wiley, et al. in 1995. In 1996, the same gene was cloned and named as Apo2L by Pitti et al. TRAIL/Apo2L is widely expressed in various tissues of normal human (lung, liver, kidney, spleen, thymus, prostate, ovary, small intestine, peripheral lymphocytes, heart, placenta, skeletal muscle, etc.) (Wiley et al., 1995; Pitti et al., 1996). TRAIL/Apo2L exists in vivo in two forms, i.e., membrane-bound and soluble TRAIL/Apo2L, both of which can form a stable homotrimer and bind with receptor to perform biological effects. A large number of in vivo and in vitro experiments show that, TRAIL/Apo2L can selectively induce apoptosis of several tumor cells and transformed cells; application of recombinant TRAIL/Apo2L protein in tumor-bearing animals can significantly inhibit tumor cell growth and even result in tumor regression without obvious damage to the host. The specificity, efficiency and non-toxicity of TRAIL/Apo2L killing tumor cells are significantly advantageous than that of CD95L and TNFα in the same family, since the latter can lead to the systemic and hard-to-be-controlled inflammation and severe toxicity such as degeneration, necrosis, hemorrhage to liver tissue, and even death (Tartaglia L, 1992). The anti-tumor activity and safety of TRAIL/Apo2L are significantly advantageous than the clinically used radiotherapy and chemotherapy etc. Animal experiments have confirmed that, TRAIL/Apo2L combined with radiotherapy and chemotherapy can produce a synergistic effect, thereby reducing the dosage and side effects of the latter. Therefore, TRAIL/Apo2L is now considered as the most promising anticancer drugs. Immunex Inc. (U.S.) discloses the gene sequence, expression vectors, and host cells of the wild-type TRAIL, and anti-TRAIL antibody (US6284236). Genentech, Inc. (U.S.) discloses a method of using wild-type APO2L for treatment of breast, colon, lung, prostate and glioma cancer (US6030945, US6746668, US6998116). The other two patent applications to Genentech Inc. disclose certain amino acid positions in APO2L polypeptide were replaced (US6740739; WO 03/029420A2). Due to low activity of the recombinantly prepared soluble wild type TRAIL/APO2L, it is not applicable for industrial and clinical applications, therefore, the structure of wild-type TRAIL/APO2L is reconstructed and modified to acquire a permuted TRAIL/APO2L with high activity is a main way to develop these drugs.
[0005] WO2005/042744 discloses a circularly permuted form of TRAIL, which has a significant selective inhibitory effect on tumor.
SUMMARY OF THE INVENTION
[0006] The present invention relates to a fusion protein comprising circularly permuted form of TRAIL, which:
[0007] (1) is the fusion protein comprising circularly permuted form of TRAIL and oligopeptides located at the N-terminus and/or C-terminus of the permuted form, the oligopeptides contain a repeating sequence consisting of 3-10 histidine residues, and the components of the circularly permuted form of TRAIL from N-terminus to C-terminus are: (a) amino acids 135-281 of TRAIL, (b) a linker, and (c) amino acids 121-135 of TRAIL or amino acids 114-135 of TRAIL or amino acids 95-135 of TRAIL or any fragments of amino acids 95-135 of TRAIL containing amino acids 121-135 of TRAIL; or
[0008] (2) is the fusion protein comprising circularly permuted form of TRAIL having at least 80%, preferably 85%, 90%, 95%, 96%, 97%, 98%, or 99% amino acid sequence identity to (1), the fusion protein comprising circularly permuted form of TRAIL has a tumor inhibitory activity which is at least 20%, e.g. 90-110%, 80-120%, 70-130%, 60-140%, 50-150%, 40-160%, 30-170%, 20-180%, or above of that of the fusion protein comprising circularly permuted form of TRAIL as set forth in SEQ ID NO: 5. The identity is calculated using procedures well known in the art, for example, BLAST, using default parameters, see, e.g., Altschul et al., J. Mol. Biol. 1990; 215: 403-410; Altschul et al., Nucleic Acids Res. 1997; 25: 3389-402 (1997). In some embodiments, the difference thereof from (1) exists only in the amino acid sequence of the circularly permuted form of TRAIL. In further embodiments, the difference thereof from (1) exists only in the amino acid sequence of (a), (b) and/or (c) of the circularly permuted form of TRAIL. In some embodiments, the difference thereof from (1) exists only in the amino acid sequence other than the circularly permuted form of TRAIL. In some embodiments, the difference thereof from (1) exists in the amino acid sequence in the circularly permuted form of TRAIL as well as that other than the circularly permuted form of TRAIL.
[0009] (3) is the fusion protein comprising circularly permuted form of TRAIL derived from amino acid sequence of (1) by substitution, deletion or addition of one or more amino acids residues, the fusion protein comprising circularly permuted form of TRAIL has a tumor inhibitory activity which is at least 20%, e.g. 90-110%, 80-120%, 70-130%, 60-140%, 50-150%, 40-160%, 30-170%, 20-180%, or above of that of the fusion protein comprising circularly permuted form of TRAIL as set forth in SEQ ID NO: 5. In some embodiments, the difference thereof from (1) exists only in the amino acid sequence of the circularly permuted form of TRAIL. In further embodiments, the difference thereof from (1) exists only in the amino acid sequence of (a), (b) and/or (c) of the circularly permuted form of TRAIL. In some embodiments, the difference thereof from (1) exists only in the amino acid sequence other than the circularly permuted form of TRAIL. In some embodiments, the difference thereof from (1) exists in the amino acid sequence in the circularly permuted form of TRAIL as well as that other than the circularly permuted form of TRAIL. In some embodiments, the number of amino acid residues subjected to substitution, deletion or addition is 1-20, 1-15, 1-14, 1-13, 1-12, 1-11, 1-10, 1-9, 1-8, 1-7, 1-6, 1-5, 1-4, 1-3, 1-2, or 1.
[0010] Said “tumor inhibitory activity” can be characterized by its inhibitory activity on tumor cell lines, e.g., lung cancer, multiple myeloma and/or colon tumor cell lines etc. In some embodiments, the tumor inhibitory activity can be characterized by IC50 of the killing activity on tumor cell lines. In some embodiments, the “tumor inhibitory activity” can be characterized by its inhibitory activity on lung cancer cell lines. In some embodiments, the tumor inhibitory activity can be characterized by IC50 of the killing activity on lung cancer cell line, e.g. can be characterized by IC50 measured by the method as described herein in Example 6.
[0011] Said “any fragments of amino acids 95-135 of TRAIL containing amino acids 121-135 of TRAIL” refers to an amino acid fragment of TRAIL, whose N-terminus is at any position between the positions 95-121 of TRAIL and C-terminus is at position 135 of TRAIL.
[0012] In some embodiments, the number of histidine residues in the oligopeptide at the N-terminus and/or C-terminus in the fusion protein of the present invention is 3-9, preferably 6-9.
[0013] In some embodiments, the oligopeptide at the N-terminus in the fusion protein of the present invention comprise structure MG a -His b , wherein a is 0 or 1, and b is an integer between 3 to 9, preferably an integer between 6 to 9.
[0014] The linker as described herein is the linker generally used in the fusion protein art, and one skilled in the art can readily design and prepare such a linker. In some embodiments, the linker in the fusion protein of the present invention is 3-15 amino acids in length, preferably 3-10 amino acids, more preferably 5-7 amino acids, preferably, the amino acid sequence of the linker is consisting of several Gs or consisting of several continuous Gs interspersed with one S, and more preferably, the amino acid sequence of the linker is selected from the group consisting of SEQ ID NO:41, 42 and 43.
[0015] The TRAIL as described herein include various TRAILs, including natural TRAIL and unnatural TRAIL, preferably wild-type human TRAIL disclosed in the prior art (Wiley et al., 1995; Pitti et al., 1996). In some embodiments, in the fusion protein of the present invention, the sequence of the amino acids 135-281 of TRAIL is SEQ ID NO:37, the sequence of the amino acids 121-135 of TRAIL is SEQ ID NO:38, the sequence of the amino acids 95-135 of TRAIL is SEQ ID NO:39, and the sequence of the amino acids 114-135 of TRAIL is SEQ ID NO:40.
[0016] The amino acid positions of TRAIL as described herein are the positions in the above wild-type TRAIL, or the corresponding positions when optimally aligned with the above wild-type TRAIL. The alignment is carried out using procedures well known in the art, for example, BLAST, using default parameters, see, e.g., Altschul et al., J. Mol. Biol. 1990; 215: 403-410; Altschul et al., Nucleic Acids Res. 1997; 25: 3389-402 (1997).
[0017] In some embodiments, the sequence of the fusion protein of the present invention is selected from the group consisting of SEQ ID NO: 5-11 and 15-16.
[0018] The present invention also relates to an isolated nucleic acid encoding the fusion protein of the invention. The present invention also relates to a vector, preferably an expression vector, comprising the nucleic acid encoding the fusion protein of the invention. The present invention also relates to a host cell comprising the above vector, and the host cell is from bacteria, fungi, plants, animals, humans, etc., e.g., Escherichia coli.
[0019] The present invention also relates to a pharmaceutical composition for treatment of tumor comprising the fusion protein of the present invention, optionally further comprising one or more additional drug(s) for treatment of tumor.
[0020] The present invention also relates to a kit for treatment of tumor comprising the fusion protein of the present invention, and optionally one or more additional drug(s) for treatment of tumor. In the kit, the fusion protein and additional drug(s) for treatment of tumor are mixed together or placed separately.
[0021] The present invention also relates to a method for treatment of tumor comprising administering to a subject the fusion protein of the invention, optionally further comprising administering to the subject one or more additional drug(s) for treatment of tumor, wherein the fusion protein can be administered simultaneously or sequentially with the additional drug(s).
[0022] The present invention also relates to use of the fusion protein of the invention or the composition comprising the fusion protein in the manufacture of a medicament for treatment of tumor, wherein said medicament optionally further comprises one or more additional drug(s) for treatment of tumor.
[0023] In some embodiments of the present invention, terms “comprise/comprising”, “include/including”, “have/having” as used herein all encompass “consisting of . . . ”.
[0024] The tumors as described herein include, but are not limited to, multiple myeloma, lymphoma, splenic tumor, melanoma, neuroglioma, mediastinal tumor, ureter tumor, gynecological tumor, endocrine system tumor, central nervous system tumor, lung cancer, colon cancer, gastric cancer, esophageal cancer, intestinal cancer, liver cancer, pancreatic cancer, rectal cancer, kidney adenocarcinoma, bladder cancer, prostate cancer, urethral cancer, testicular cancer, ovarian cancer, breast cancer, leukemia and the like. In some embodiments, the tumor(s) is(are) selected from lung cancer, multiple myeloma, and colon cancer.
[0025] The additional drug(s) for treatment of tumor as described herein include(s), but are not limited to, melphalan, dexamethasone, thalidomide, lenalidomide, Velcade, vincristine, vinorelbine, doxorubicin, liposomal doxorubicin, cyclophosphamide, irinotecan, prednisone, paclitaxel, carboplatin, cisplatin, VP16, 5-FU and the like. In some embodiments, the additional drug(s) for treatment of tumor is(are) selected from the group consisting of melphalan, prednisone, paclitaxel, and carboplatin.
BRIEF DESCRIPTION OF THE FIGURES
[0026] FIG. 1 . Observation of the killing effect of NCPT-1.M1 on H460 cells under phase contrast microscope.
[0027] FIG. 2 . The time-effect relationship of NCPT-1.M1 in killing RPMI8226 cells. Incubation of varying concentration of NCPT-1.M1 with human multiple myeloma RPMI8226 cells for 6 h could result in maximum killing, without significant difference from those for 8 h, 24 h, and 48 h.
[0028] FIG. 3 . The morphological change of the apoptosis of human multiple myeloma cell RPMI 8226 induced by NCPT-1.M1. The cells were incubated with NCPT-1.M1 (200 ng/ml) for 3 h and then prepared as smears before MGG staining. A(1000×), C(200×) represent the control group, wherein the cytoplasms are basophilic and stained as blue, the nucleus are eosinophilic, stained as homogeneous red with clear nucleoli; B(1000×), D(200×) represent NCPT-1.M1 group, the membranes are intact but with large bubbles, the chromatin exhibits aggregation at the periphery, karyopyknosis, and karyorrhexis with darker staining.
[0029] FIG. 4 . TUNEL assay of apoptosis of human lung cancer cell line NCI-H460 induced by NCPT-1.M1. The NCI-H460 cells were incubated with NCPT-1.M1 (15 ng/ml) for 4 h and then prepared as smears before TUNEL staining. Almost all of the tumor cells exhibit characteristic of apoptosis as karyopyknosis, karyorrhexis, and brown staining of the fractured chromatins etc under microscope (B). In control group, nucleus remains intact, and no characteristic brown stained chromatins are seen (A).
[0030] FIG. 5 . The agarose gel electrophoresis analysis of internucleosomal DNA fragmentation of NCI-H460 cells after incubated with NCPT-1.M1 for varying time.
[0031] Marker: 200 bp-2000 bp DNA markers with 200 bp interval;
[0032] Control: solvent control;
[0033] 2 h, 4 h, 6 h: represent incubation with 15 ng/ml NCPT-1.M1 for 2 h, 4 h, 6 h, respectively.
[0034] FIG. 6 . Caspase-8 inhibitor (zIETD-fmk) can inhibit the pro-apoptotic activity of NCPT-1.M1 on H460 cells.
[0035] H460 cells were incubated with NCPT-1.M1 (1.2 or 10 ng/ml) in the presence or absence of Caspase-8 inhibitor zIETD-fmk (concentration of 30 μmmol/L, added 1 h earlier than NCPT-1.M1) for 24 h, and then cell survival rate was measured by MTT assay.
[0036] FIG. 7 . NCPT-1.M1 can result in apoptosis of a large number of tumor cells in tumor tissue.
[0037] Athymic nude mice were subcutaneously inoculated with human MM RPMI8226 tumor cells and treated with NCPT-1.M1, then tumor tissue was resected and subjected to conventional HE staining (A, B) and TUNEL staining of apoptotic cells (C, D). A large number of cells exhibit karyopycnosis, karyorrhexis (B), brown staining of nuclei (D) and other characteristics of apoptosis, while there are only a few apoptotic cells in the control group (A, C).
[0038] FIG. 8 . The growth of human PRMI 8226 xenograft tumor in mice is significantly inhibited by NCPT-1.M1. Athymic nude mice (Beijing Huafukang Biotechnology Co., Ltd.) were subcutaneously inoculated with RPMI8226 tumor cells (5×10 6 /mouse). When the tumor grew to about 500 mm 3 , the mice were divided into several groups, which were intraperitoneally injected with normal saline (control group), NCPT-1.M1 (15 mg/kg) and wild-type TRAIL (wtTRAIL, 15 mg/kg or 45 mg/kg) respectively once a day for 8 consecutive days. The tumor volumes were measured with a vernier caliper every two days. Tumor growth rate of NCPT-1.M1 group with a dose of 15 mg/kg is significantly lower than that of wtTRAIL group with a dose of 45 mg/kg, suggesting that NCPT-1.M1 has an inhibitory activity stronger than that of wtTRAIL on RPMI8226 xenograft tumor.
[0039] FIG. 9 . NCPT-1.M1 combined with melphalan can improve the killing effect on human multiple myeloma cell line U266. U266 cells are insensitive to CPT. At the concentration of 1 μg/ml, NCPT-1.M1 alone has a mild killing effect on U266 (<20%), but with the presence of melphalan (12.5˜50 μg/ml), both of them can cause enhanced killing effect. The cell viability was assayed with ATPlite luminescent system (PerkinElmer), the data as shown in this figure are all represented as the mean±standard deviation, n=4, #P<0.05, ##P<0.01 vs. melphalan group; *P<0.05 vs. NCPT-1.M1 group.
[0040] FIG. 10 . NCPT-1.M1 combined with melphalan has a synergistic killing effect on human MM cell line H929. The melphalan (12.5 μg/ml) combined with varying concentrations of NCPT-1.M1 (31˜1000 ng/ml) were incubated with H929 cells. The cell survival rate was assayed with ATPlite luminescent system (PerkinElmer). A combination index (CI, marked above the histogram) represents the nature of the interaction between the two drugs: CI<0.9 represents a synergistic effect, CI>1.1 represents an antagonistic effect, and CI between 0.9 and 1.1 represents an additive effect.
[0041] FIG. 11 . NCPT-1.M1 combined with melphalan has a synergistic killing effect on human MM cell line RPMI8226. The melphalan (25 μg/ml) combined with varying concentrations of NCPT-1.M1 (2˜500 ng/ml) were incubated with RPMI8226 cells. The cell survival rate was assayed with ATPlite luminescent system (PerkinElmer). A combination index (CI, marked above the histogram) represents the nature of the interaction between the two drugs: CI<0.9 represents a synergistic effect, CI>1.1 represents an antagonistic effect, and CI between 0.9 and 1.1 represents an additive effect.
[0042] FIG. 12 . The inhibitory effect of NCPT-1.M1 on the growth of human PRMI 8226 xenograft tumor in mice is significantly enhanced by NCPT-1.M1 combined with Melphalan and Prednisone.
[0043] FIG. 13 . The inhibitory effect of NCPT-1.M1 on the growth of human PRMI 8226 xenograft tumor in mice is significantly enhanced by NCPT-1.M1 combined with chemotherapy (PC regimen: paclitaxel plus carboplatin).
DESCRIPTION OF THE PREFERRED EMBODIMENTS
Example 1
Construction of the Wild-Type Human TRAIL Encoding Gene
[0044] A plasmid containing a gene expressing the sequence of amino acid 114-281 of wild-type human TRAIL was constructed.
[0045] (1) The First Step PCR
[0046] PCR was carried out with human spleen cDNA library (Clontech) as a template and P1, P2 as downstream and upstream primers using added pfu DNA polymerase (Invitrogen) according to the following parameters on a PCR instrument: 30 cycles of 94° C. denaturation for 1 min, 55° C. annealing for 1 min and 68° C. extension for 1 min, and a final cycle of 68° C. extension for 10 min.
[0000]
(SEQ ID NO: 17)
P1: cgttcatatg gtgagagaaagaggtcctcagagag
(SEQ ID NO: 18)
P2: ctta ggatcc ttagccaactaaaaaggccccgaaaaaac
[0047] (2) Construction of TRAIL Plasmid
[0048] The resulting PCR product of the preceding step was purified, digested with restriction endonucleases Nde I and BamH I, ligated with T4 ligase into the digested vector pET42a with the same endonucleases, cultured on plate and propogated before plasmid isolation, digestion test and preliminary screen of positive clones. The expression plasmid of recombinant human TRAIL gene was confirmed by DNA sequencing, and the contructed plasmid is named as pET42a-TRAIL114-281.
Example 2
Construction of a Gene Expressing a Recombinant Human Circularly Permuted TRAIL
[0049] A gene encoding a recombinant human circularly permuted TRAIL (Circularly Permuted TRAIL, referred to as CPT) was constructed. The amino acid sequences encoded by said gene from N-terminus to C-terminus are: (a) amino acids 135-281 of TRAIL, (b) a linker, and (c) amino acids 122-135 of TRAIL.
[0000]
CPT polypeptide sequence
(SEQ ID NO: 1)
(TLSSPNSKNEKALGRKINSWESSRSGHSFLSNLHLRNGELVIHEK
GFYYIYSQTYFRFQEEI
KENTKNDKQMVQYIYKYTSYPDPILLMKSARNSCWSKDAEYGLY
SIYQGGIFELKENDRI FVSVTNEHLI
DMDHEASFFGAFLVGGGGGGVAAHITGTR GRSNT)
[0050] (1) The First Step PCR Amplification
[0051] PCR was carried out with plasmid pET42a-TRAIL114-281 as a template and P3, P4 as downstream and upstream primers using added pfu DNA polymerase (Invitrogen) according to the following parameters on a PCR instrument: 30 cycles of 94° C. denaturation for 1 min, 55° C. annealing for 1 min and 68° C. extension for 1 min, and a final cycle of 68° C. extension for 10 min.
[0000]
(SEQ ID NO: 19)
P3: catgcatatgacattg tcttctccaa actc
(SEQ ID NO: 20)
P4: agttatgtgagctgctacaccaccaccaccaccgccaactaaaaaggccccaaaaaaactg
[0052] (2) The Second Step PCR
[0053] PCR was carried out with the PCR product from the first step as a template and P3, P5 as downstream and upstream primers using added pfu DNA polymerase (Invitrogen) according to the following parameters on a PCR instrument: 30 cycles of 94° C. denaturation for 1 min, 55° C. annealing for 1 min and 68° C. extension for 1 min, and a final cycle of 68° C. extension for 10 min.
[0000]
(SEQ ID NO: 21)
P5: cg ggatcc ttatgtgttgcttcttcctctggtcccagttatgtgagctgctacaccacc
(BamHI restriction site)
[0054] (3) Construction of CPT Plasmid
[0055] The PCR product from the second step was purified, digested with restriction endonucleases Nde I and BamH I, ligated with T4 ligase into the digested vector pET42a with the same endonucleases, cultured on plate and propogated before plasmid isolation, digestion test and preliminary screen of positive clones. The expression plasmid of the recombinant human circularly permuted TRAIL was confirmed by DNA sequencing, and the contructed plasmid is named as pET42a-CPT.
Example 3
Construction of Novel Genes Encoding Various Recombinant Human Circularly Permuted TRAILs
[0056] 1. Construction of a gene encoding recombinant human New Circularly Permuted TRAIL-1 (New Circularly Permuted TRAIL-1, referred to as NCPT-1).
[0057] The amino acid sequences encoded by said gene from N-terminus to C-terminus are: (a) amino acids 135-281 of TRAIL, (b) a linker, and (c) amino acids 121-135 of TRAIL.
[0000]
NCPT-1 polypeptide sequence
(SEQ ID NO: 2)
(TLSSPNSKNEKALGRKINSWESSRSGHSFLSNLHLRNGELVIHEK
GFYYIYSQTYFRFQEEI
KENTKNDKQMVQYIYKYTSYPDPILLMKSARNSCWSKDAEYGLY
SIYQGGIFELKENDRI FVSVTNEHLI
DMDHEASFFGAFLVGGGGGG RVAAHITGTR GRSNT)
[0058] (1) PCR Amplification of a Gene Encoding Amino Acids 135-281 of TRAIL
[0059] PCR was carried out with human spleen cDNA library (Clontech) as a template and P6, P7 as downstream and upstream primers using added pfu DNA polymerase (Invitrogen) according to the following parameters on a PCR instrument: 30 cycles of 94° C. denaturation for 1 min, 55° C. annealing for 1 min and 68° C. extension for 1 min, and a final cycle of 68° C. extension for 10 min.
[0000]
(SEQ ID NO: 22)
P6: ggaattc catatg acattgtcttctccaaactccaag(NdeI
restriction site)
(SEQ ID NO: 23)
P7: cg ggatcc gccaactaaaaaggccccaaaaaaactggcttc
(BamH I restriction site)
[0060] The PCR product and plasmid pET42a (Novagen) were digested with the restriction endonucleases NdeI and BamH I, and ligated by T4 DNA ligase. The ligated product was transformed into the competent BL21 (DE3) (Invitrogen) bacteria. The transformed bacteria was cultured on plate and propogated before plasmid isolation, digestion test and preliminary screen of positive clones. The positive clones were then confirmed by DNA sequencing. The constructed plasmid is named as pET42a-TRAIL135-281.
[0061] (2) The Second Step PCR
[0062] PCR was carried out with plasmid pET42a-TRAIL135-281 as a template and P6, P8 as downstream and upstream primers using added pfu DNA polymerase (Invitrogen) according to the following parameters on a PCR instrument: 30 cycles of 94° C. denaturation for 1 min, 55° C. annealing for 1 min and 68° C. extension for 1 min, and a final cycle of 68° C. extension for 10 min.
[0000]
(SEQ ID NO: 24)
P8: agttatgtgagctgctactctaccaccaccaccaccgccaactaaaaaggccccaaaaaaactg
[0063] (3) The Third Step PCR
[0064] PCR was carried out with the PCR product from the second step as a template and P6, P9 as downstream and upstream primers using added pfu DNA polymerase (Invitrogen) according to the following parameters on a PCR instrument: 30 cycles of 94° C. denaturation for 1 min, 55° C. annealing for 1 min and 68° C. extension for 1 min, and a final cycle of 68° C. extension for 10 min.
[0000]
(SEQ ID NO: 25)
P9: cg ggatcc ttatgtgttgcttcttcctctggtcccagttatgtgagctgctactctaccacc(BamH I
restriction site)
[0065] (4) Construction of NCPT-1 Plasmid
[0066] The PCR product from the third step was purified, digested with restriction endonucleases Nde I and BamH I, ligated with T4 ligase into the digested vector pET42a with the same endonucleases, cultured on plate and propogated before plasmid isolation, digestion test and preliminary screen of positive clones. The expression plasmid of recombinant human NCPT-1 gene was confirmed by DNA sequencing, and the contructed plasmid is named as pET42a-NCPT-1.
[0067] 2. Construction of a gene encoding a recombinant human New Circularly Permuted TRAIL-2 (New Circularly Permuted TRAIL-2, referred to as NCPT-2).
[0068] The amino acid sequences encoded by said gene from N-terminus to C-terminus are: (a) amino acids 135-281 of TRAIL, (b) a linker, and (c) amino acids 95-135 of TRAIL.
[0000]
NCPT-2 polypeptide sequence
(SEQ ID NO: 3)
(TLSSPNSKNEKALGRKINSWESSRSGHSFLSNLHLRNGELVIHEKG
FYYIYSQTYFRFQEEIKENTKNDKQMVQYIYKYTSYPDPILLMKSA
RNSCWSKDAEYGLYSIYQGG IFELKENDRI FVSVTNEHLI
DMDHEASFFGAFLVGGGGGG
TSEETISTVQEKQQNISPLVRERGPQ
RVAAHITGTR GRSNT)
[0069] (1) The First Step PCR
[0070] PCR was carried out with plasmid pET42a-TRAIL135-281 as a template and P6, P10 as downstream and upstream primers using added pfu DNA polymerase (Invitrogen) according to the following parameters on a PCR instrument: 30 cycles of 94° C. denaturation for 1 min, 55° C. annealing for 1 min and 68° C. extension for 1 min, and a final cycle of 68° C. extension for 10 min.
[0000]
(SEQ ID NO: 26)
P10: agaaatggtttcctcagaggtaccaccaccaccaccgccaactaaaaaggccccaaaaaaactg
[0071] (2) The Second Step PCR
[0072] PCR was carried out with the PCR product from the first step as a template and P6, P11 as downstream and upstream primers using added pfu DNA polymerase (Invitrogen) according to the following parameters on a PCR instrument: 30 cycles of 94° C. denaturation for 1 min, 55° C. annealing for 1 min and 68° C. extension for 1 min, and a final cycle of 68° C. extension for 10 min.
[0000]
P11:
(SEQ ID NO: 27)
tctcactaggggagaaatattttgttgcttttcttgaactgtaga
aatggtttcctcagag
[0073] (3) The Third Step PCR
[0074] PCR was carried out with the PCR product from the second step as a template and P6, P12 as downstream and upstream primers using added pfu DNA polymerase (Invitrogen) according to the following parameters on a PCR instrument: 30 cycles of 94° C. denaturation for 1 min, 55° C. annealing for 1 min and 68° C. extension for 1 min, and a final cycle of 68° C. extension for 10 min.
[0000]
P12:
(SEQ ID NO: 28)
cagttatgtgagctgctactctctgaggacctctttctctcacta
ggggagaaatattttg
[0075] (4) The Forth Step PCR
[0076] PCR was carried out with the PCR product from the third step as a template and P6, P13 as downstream and upstream primers using added pfu DNA polymerase (Invitrogen) according to the following parameters on a PCR instrument: 30 cycles of 94° C. denaturation for 1 min, 55° C. annealing for 1 min and 68° C. extension for 1 min, and a final cycle of 68° C. extension for 10 min.
[0000]
P13:
(SEQ ID NO: 29)
cg ggatcc ttatgtgttgcttcttcctctggtcccagttatgt
gagctgctac
[0077] (5) Construction of NCPT-2 Plasmid
[0078] The PCR product from the forth step was purified, digested with restriction endonucleases Nde I and BamH I, ligated with T4 ligase into the digested vector pET42a with the same endonucleases, cultured on plate and propogated before plasmid isolation, digestion test and preliminary screen of positive clones. The expression plasmid of the recombinant human circularly permuted TRAIL (NCPT-2) was confirmed by DNA sequencing, and the contructed plasmid is named as pET42a-NCPT-2.
[0079] 3. Construction of a gene encoding a recombinant human New Circularly Permuted TRAIL-3 (New Circularly Permuted TRAIL-3, referred to as NCPT-3).
[0080] The amino acid sequences encoded by said gene from N-terminus to C-terminus are: (a) amino acids 135-281 of TRAIL, (b) a linker, and (c) amino acids 114-135 of TRAIL.
[0000]
NCPT-3 polypeptide sequence
(SEQ ID NO: 4)
(TLSSPNSKNEKALGRKINSWESSRSGHSFLSNLHLRNGELVIHEKG
FYYIYSQTYFRFQEEIKENTKNDKQMVQYIYKYTSYPDPILLMKSA
RNSCWSKDAEYGLYSIYQGG IFELKENDRI
FVSVTNEHLIDMDHEASFFGAFLVGGGGGGVRERGPQRVAAHITG
TR GRSNT)
[0081] (1) The First Step PCR
[0082] PCR was carried out with plasmid pET42a-TRAIL135-281 as a template and P6, P14 as downstream and upstream primers using added pfu DNA polymerase (Invitrogen) according to the following parameters on a PCR instrument: 30 cycles of 94° C. denaturation for 1 min, 55° C. annealing for 1 min and 68° C. extension for 1 min, and a final cycle of 68° C. extension for 10 min.
[0000]
P14:
(SEQ ID NO: 30)
gagctgctactctctgaggacctctttctctcacaccaccaccaccac
cgccaactaaaaaggccccaaaaaaactg
[0083] (2) The Second Step PCR
[0084] PCR was carried out with the PCR product from the first step as a template and P6, P15 as downstream and upstream primers using added pfu DNA polymerase (Invitrogen) according to the following parameters on a PCR instrument: 30 cycles of 94° C. denaturation for 1 min, 55° C. annealing for 1 min and 68° C. extension for 1 min, and a final cycle of 68° C. extension for 10 min.
[0000]
P15:
(SEQ ID NO: 31)
cg ggatcc tta tgtgttgcttcttcctctggtcccagttatgtgagc
tgctactctctgagg
[0085] (3) Construction of NCPT-3 Plasmid
[0086] The PCR product from the second step was purified, digested with restriction endonucleases Nde I and BamH I, ligated with T4 ligase into the digested vector pET42a with the same endonucleases, cultured on plate and propogated before plasmid isolation, digestion test and preliminary screen of positive clones. The expression plasmid of the recombinant human circularly permuted TRAIL (NCPT-3) was confirmed by DNA sequencing, and the contructed plasmid is named as pET42a-NCPT-3.
Example 4
Construction of Genes Encoding Various Mutants of NCPT-1, NCPT-2, and NCPT-3
[0087] 1. Construction of a Gene Encoding NCPT-1.M1
[0088] Met-Gly-His-His-His-His-His-His gene sequence was fused to the upstream of a gene encoding NCPT-1, i.e. Met-Gly-His-His-His-His-His-His amino acid sequence was fused to the N-terminus of NCPT-1 polypeptide (MG+His6+NCPT-1).
[0000]
NCPT-1.M1 polypeptide sequence
(SEQ ID NO: 5)
MGHHHHHHTLSSPNSKNEKALGRKINSWESSRSGHSFLSNLHLRN
GELVIHEKGFYYIYSQTYFRFQEEIKENTKNDKQMVQYIYKYTSY
PDPILLMKSARNSCWSKDAEYGLYSIYQGGIFELKENDRIFVSVTN
EHLIDMDHEASFFGAFLVGGGGGGRVAAHITGTRGRSNT
[0089] PCR was carried out with pET42a-NCPT-1 as a template and P16, P9 as a pair of downstream and upstream primers using added pfu DNA polymerase (Invitrogen) according to the following parameters on a PCR instrument: 30 cycles of 94° C. denaturation for 1 min, 55° C. annealing for 1 min and 68° C. extension for 1 min, and a final cycle of 68° C. extension for 10 min.
[0000]
P16:
(SEQ ID NO: 32)
catg ccatgg gccaccaccaccaccaccacacattg
tcttctccaa actc
[0090] The resulting PCR product of the preceding step was purified, digested with restriction endonucleases Nde I and BamH I, ligated with T4 ligase into the digested vector pET28b with the same endonucleases, cultured on plate and propogated before plasmid isolation, digestion test and preliminary screen of positive clones. The positive clones were then confirmed by DNA sequencing, and the resulting plasmid is named as pET28b-NCPT-1.M1.
[0091] 2. Construction of a Gene Encoding NCPT-1.M2
[0092] Met-Gly amino acid sequence was fused to the N-terminus of NCPT-1 polypeptide, and His-His-His-His-His-His amino acid sequence was fused to the C-terminus of NCPT-1 polypeptide (MG+NCPT-1+His6).
[0000]
NCPT-1.M2 polypeptide sequence
(SEQ ID NO: 6)
MGTLSSPNSKNEKALGRKINSWESSRSGHSFLSNLHLRNGELVIHE
KGFYYIYSQTYFRFQEEIKENTKNDKQMVQYIYKYTSYPDPILLM
KSARNSCWSKDAEYGLYSIYQGGIFELKENDRIFVSVTNEHLIDM
DHEASFFGAFLVGGGGGGRVAAHITGTRGRSNTHHHHHH
[0093] PCR was carried out with pET42a-NCPT-1 as a template and P18, P17 as a pair of primers using added pfu DNA polymerase (Invitrogen) according to the following parameters on a PCR instrument: 30 cycles of 94° C. denaturation for 1 min, 55° C. annealing for 1 min and 68° C. extension for 1 min, and a final cycle of 68° C. extension for 10 min.
[0000]
P17:
(SEQ ID NO: 33)
cg ggatcc ttagtggtggtggtggtggtgtgtgttgcttcttcctctggt
cccagttatgtg
P18:
(SEQ ID NO: 34)
catgccatgggcacattg tcttctccaa actc
[0094] The resulting PCR product of the preceding step was purified, digested with restriction endonucleases Nde I and BamH I, ligated with T4 ligase into the digested vector pET28b with the same endonucleases, cultured on plate and propogated before plasmid isolation, digestion test and preliminary screen of positive clones. The positive clones were then confirmed by DNA sequencing, and the resulting plasmid is named as pET28b-NCPT-1.M2.
[0095] 3. Construction of a Gene Encoding NCPT-1.M3
[0096] Met-Gly-His-His-His amino acid sequence was fused to the N-terminus of NCPT-1 polypeptide (MG+His3+NCPT-1).
[0000]
NCPT-1.M3 polypeptide sequence
(SEQ ID NO: 7)
MGHHHTLSSPNSKNEKALGRKINSWESSRSGHSFLSNLHLRNGEL
VIHEKGFYYIYSQTYFRFQEEIKENTKNDKQMVQYIYKYTSYPDPI
LLMKSARNSCWSKDAEYGLYSIYQGGIFELKENDRI
FVSVTNEHLIDMDHEASFFGAFLVGGGGGGRVAAHITGTRGRSNT
[0097] PCR was carried out with pET42a-NCPT-1 as a template and P19, P9 as a pair of downstream and upstream primers using added pfu DNA polymerase (Invitrogen) according to the following parameters on a PCR instrument: 30 cycles of 94° C. denaturation for 1 min, 55° C. annealing for 1 min and 68° C. extension for 1 min, and a final cycle of 68° C. extension for 10 min.
[0000]
P19:
(SEQ ID NO: 35)
catg ccatgg gccaccaccacacattg tcttctccaa actc
[0098] The resulting PCR product of the preceding step was purified, digested with restriction endonucleases Nde I and BamH I, ligated with T4 ligase into the digested vector pET28b with the same endonucleases, cultured on plate and propogated before plasmid isolation, digestion test and preliminary screen of positive clones. The positive clones were then confirmed by DNA sequencing, and the resulting plasmid is named as pET28b-NCPT-1.M3.
[0099] 4. Construction of a Gene Encoding NCPT-1.M4
[0100] His-His-His-His-His-His gene sequence was fused to the upstream of a gene encoding NCPT-1, i.e. His-His-His-His-His-His amino acid sequence was fused to the N-terminus of NCPT-1 polypeptide (His6+NCPT-1).
[0000]
NCPT-1.M4 polypeptide sequence
(SEQ ID NO: 8)
HHHHHHTLSSPNSKNEKALGRKINSWESSRSGHSFLSNLHLRNGE
LVIHEKGFYYIYSQTYFRFQEEIKENTKNDKQMVQYIYKYTSYPD
PILLMKSARNSCWSKDAEYGLYSIYQGGIFELKENDRIFVSVTNEH
LIDMDHEASFFGAFLVGGGGGGRVAAHITGTRGRSNT
[0101] PCR was carried out with pET42a-NCPT-1 as a template and P20, P9 as a pair of downstream and upstream primers using added pfu DNA polymerase (Invitrogen) according to the following parameters on a PCR instrument: 30 cycles of 94° C. denaturation for 1 min, 55° C. annealing for 1 min and 68° C. extension for 1 min, and a final cycle of 68° C. extension for 10 min.
[0000]
P20:
(SEQ ID NO: 36)
catg catatg caccaccaccaccaccacacattg tcttctccaa actc
[0102] The resulting PCR product of the preceding step was purified, digested with restriction endonucleases Nde I and BamH I, ligated with T4 ligase into the digested vector pET42a with the same endonucleases, cultured on plate and propogated before plasmid isolation, digestion test and preliminary screen of positive clones. The positive clones were then confirmed by DNA sequencing, and the resulting plasmid is named as pET42a-NCPT-1.M4.
[0103] The construction of other mutants, namely NCPT-1.M5, NCPT-1.M6, NCPT-1.M7, NCPT-1.M8, NCPT-1.M9, NCPT-1.M10, NCPT-2.M11, NCPT-3.M12 can be carried out following the above method and “Molecular cloning: a laboratory manual”.
[0104] Construction of NCPT-1.M5: Met-Gly-His-His-His-His-His-His amino acid sequence was fused to the N-terminus of NCPT-1 polypeptide using a linker with amino acid sequence of Gly-Ser-Gly-Gly-Gly (MG+His6+NCPT-1 linker:GSGGG).
[0105] Construction of NCPT-1.M6: Met-Gly-His-His-His-His-His-His amino acid sequence was fused to the N-terminus of NCPT-1 polypeptide using a linker with amino acid sequence of Gly-Gly-Ser-Gly-Gly-Gly-Gly (MG+His6+NCPT-1_linker:GGSGGGG).
[0106] Construction of NCPT-1.M7: Met-Gly-His-His-His-His-His-His-His-His-His gene sequence was fused to the upstream of a gene encoding NCPT-1, i.e. Met-Gly-His-His-His-His-His-His-His-His-His amino acid sequence was fused to the N-terminus of NCPT-1 polypeptide (MG+His9+NCPT-1).
[0107] Construction of NCPT-1.M8: Met-Gly and amino acids 129-134 of TRAIL were fused to the N-terminus of NCPT-1 polypeptide (MG+129-134+NCPT-1).
[0108] Construction of NCPT-1.M9: Met-Gly-Asn-Asn-Asn-Asn-Asn-Asn gene sequence was fused to the upstream of a gene encoding NCPT-1, i.e. Met-Gly-Asn-Asn-Asn-Asn-Asn-Asn amino acid sequence was fused to the N-terminus of NCPT-1 polypeptide (MG+Asn6+NCPT-1).
[0109] Construction of NCPT-1.M10: Met-Gly amino acid sequence was fused to the N-terminus of NCPT-1 polypeptide, and amino acids 136-141 of TRAIL was fused to the C-terminus of NCPT-1 polypeptide (MG+NCPT-1+aa136-141).
[0110] Construction of NCPT-1.M11: Met-Gly-His-His-His-His-His-His gene sequence was fused to the upstream of a gene encoding NCPT-2, i.e. Met-Gly-His-His-His-His-His-His amino acid sequence was fused to the N-terminus of NCPT-2 polypeptide (MG+His6+NCPT-2).
[0111] Construction of NCPT-1.M12: Met-Gly-His-His-His-His-His-His gene sequence was fused to the upstream of a gene encoding NCPT-3, i.e. Met-Gly-His-His-His-His-His-His amino acid sequence was fused to the N-terminus of NCPT-3 polypeptide (MG+His6+NCPT-3).
[0000]
NCPT-1.M5 polypeptide sequence
(SEQ ID NO: 9)
MGHHHHHHTLSPNSKNEKALGRKINSWESSRSGHSFLSNLHLRN
GELVIHEKGFYYIYS
QTYFRFQEEIKENTKNDKQMVQYIYKYTSYPDPILLMKSARNSCW
SKDAEYGLYSIYQGG IFELKENDRI FVSVTNEHLI
DMDHEASFFGAFLVGGSGGG RVAAHITGTR GRSNT
NCPT-1.M6 polypeptide sequence
(SEQ ID NO: 10)
MGHHHHHHTLSSPNSKNEKALGRKINSWESSRSGHSFLSNLHLRN
GELVIHEKGFYYIYS
QTYFRFQEEIKENTKNDKQMVQYIYKYTSYPDPILLMKSARNSCW
SKDAEYGLYSIYQGG
IFELKENDRIFVSVTNEHLIDMDHEASFFGAFLVGGGSGGGGRVAA
HITGTRGRSNT
NCPT-1.M7 polypeptide sequence
(SEQ ID NO: 11)
MGHHHHHHHHHTLSSPNSKNEKALGRKINSWESSRSGHSFLSNLH
LRNGELVIHEKGFYYIYSQTYFRFQEEIKENTKNDKQMVQYIYKY
TSYPDPILLMKSARNSCWSKDAEYGLYSIYQGGIFELKENDRIFV
SVTNEHLIDMDHEASFFGAFLVGGGGGGRVAAHITGTRGRSNT
NCPT-1.M8 polypeptide sequence
(SEQ ID NO: 12)
MGTRGRSNTLSPNSKNEKALGRKINSWESSRSGHSFLSNLHLRNG
ELVIHEKGFYYIYSQTYFRFQEEIKENTKNDKQMVQYIYKYTSYP
DPILLMKSARNSCWSKDAEYGLYSIYQGGIFELKENDRIFVSVTN
EHLIDMDHEASFFGAFLVGGGGGGRVAAHITGTRGRSNT
NCPT-1.M9 polypeptide sequence
(SEQ ID NO: 13)
MGNNNNNNTLSPNSKNEKALGRKINSWESSRSGHSFLSNLHLRN
GELVIHEKGFYYIYS
QTYFRFQEEIKENTKNDKQMVQYIYKYTSYPDPILLMKSARNSCW
SKDAEYGLYSIYQGG
IFELKENDRIFVSVTNEHLIDMDHEASFFGAFLVGGGGGGRVAAHI
TGTRGRSNT
NCPT-1.M10 polypeptide sequence
(SEQ ID NO: 14)
MGTLSPNSKNEKALGRKINSWESSRSGHSFLSNLHLRNGELVIHE
KGFYYIYSQTYFRFQEEIKENTKNDKQMVQYIYKYTSYPDPILLM
KSARNSCWSKDAEYGLYSIYQGGIFELKENDRIFVSVTNEHLIDM
DHEASFFGAFLVGGGGGGRVAAHITGTRGRSNTLSSPNS
NCPT-2.M11 polypeptide sequence
(SEQ ID NO: 15)
MGHHHHHHTLSPNSKNEKALGRKINSWESSRSGHSFLSNLHLRN
GELVIHEKGFYYIYS
QTYFRFQEEIKENTKNDKQMVQYIYKYTSYPDPILLMKSARNSCW
SKDAEYGLYSIYQGG IFELKENDRI FVSVTNEHLI
DMDHEASFFGAFLVGGGGGG
TSEETISTVQEKQQNISPLVRERGPQRVAAHITGTR GRSNT
NCPT-3.M12 polypeptide sequence
(SEQ ID NO: 16)
MGHHHHHHTLSPNSKNEKALGRKINSWESSRSGHSFLSNLHLRN
GELVIHEKGFYYIYS
QTYFRFQEEIKENTKNDKQMVQYIYKYTSYPDPILLMKSARNSCW
SKDAEYGLYSIYQGG IFELKENDRI FVSVTNEHLI
DMDHEASFFGAFLVGGGGGG VRERGPQRVAAHITGTR GRSNT
Example 5
Expression and Purification of the Recombinant Human Circularly Permuted Form of TRAIL and Mutant Thereof
[0112] The expression plasmid was transformed into E. coli strain BL21 (DE3), and the transformed E. coli was inoculated into 10 ml LB liquid medium containing 20 μg/ml of kanamycin, and cultured on shaking table at 37° C. for 12 hours. 10 ml culture was then inoculated into 1 L LB liquid medium containing 20 μg/ml kanamycin and cultured, when the OD 600 value reached 0.6, 0.2 ml 1M IPTG was added into 1 L culture to induce protein expression. After 3 hours of induction, the cells were collected by centrifugation, the pellet was suspended in 100 ml buffer containing 100 mM Tris (pH7.9), 150 mM NaCl.
[0113] After lysis of the cells by sonication at 4° C., the lysate was centrifuged at 15,000 rpm in a centrifuge with Beckman JA20 rotor. Since the expressed protein can bind to a metal chelate resin, it can be purified by metal chelate chromatography. After centrifugation, the supernatant was pumped into the Ni chromatography column containing the resin, and the contaminating proteins therein were removed by rinse with a buffer containing 50 mM Tris (pH7.9), 0.5M NaCl and 50 mM imidazole. Then the bound protein was eluted with a buffer containing 50 mM Tris (pH7.9), 0.5M NaCl and 200 mM imidazole, and the eluted protein was dialyzed against PBS buffer.
[0114] Finally, the protein was purified by the ion exchange column and Superdex 200 (Pharmacia) gel chromatography mounted in AKTA HPLC system (Pharmacia). The purified protein of interest was stored at −80° C., determined for molecular weight and amino acid sequenced etc for further use.
Example 6
Assay of Killing Activity of Various Mutants of NCPT-1, NCPT-2, and NCPT-3 on Lung Cancer Cell Line
[0115] The NCI-H460 cells (ATCC) were cultured in flasks until logarithmic growth phase, digested with 0.25% trypsin (Amresco), collected by centrifugation (1000 rpm, 5 min), resuspended in RPMI1640 medium (Invitrogen) containing 3% fetal bovine serum (FBS), counted and adjusted to 1.5×10 5 /ml cell suspension, added into 96-well culture plates (Nunc) at 100 μl/well, and incubated at 37° C. in 5% CO 2 incubator overnight. The sample to be tested was diluted to a certain concentration with 1640 medium containing 3% FBS, and further diluted at 4-fold dilutions (8 dilutions). The supernatant in the culture plate was discarded, and serial dilutions of the sample to be tested was added into the plate at 100 μl/well with a negative control and blank control set aside, incubated at 37° C. under 5% CO 2 for 20-24 hours. Following examination under microscope, the supernatant was discarded, each well was added 50 μl 0.05% crystal violet solution (50 mg crystal violet was dissolved in 20 ml anhydrous ethanol, and water was added to the volume of 100 ml, then stored at room temperature) and stained for 3-5 minutes. The crystal violet was carefully washed with flowing water, the remaining water was removed by spin-drying, a destaining solution (50 ml distilled water, 50 ml anhydrous ethanol, and 0.1 ml glacial acetic acid were thoroughly mixed and stored at room temperature) was added at 100 μl/well, then the reading at OD570 was measured on a microplate reader (Bio-Rad 680) (reference wavelength of 630 nm). The inhibitory concentration 50 (IC50) of each sample was calculated by a four-parameter Logistic fitting using Sigmaplot10.0 software. The IC50 for CPT and each mutant of NCPT-1, NCPT-2, and NCPT-3 were calculated, and the activity change of each mutant was represented as a ratio of the IC50 of each mutant to that of CPT (Table 1). The results show that, among various mutants, the activities of NCPT-1.M1, NCPT-1.M2, NCPT-1.M3, NCPT-1.M4, NCPT-1.M5, NCPT-1.M6, NCPT-1.M7, NCPT-2.M11, and NCPT-3.M12 are significantly higher than that of CPT; the activities of NCPT-1.M8 and NCPT-1.M9 are significantly decreased compared to that of CPT; and the activity of NCPT-1.M10 is slightly decreased compared to that of CPT.
[0000]
Ratio of IC50 of mutants to IC50 of CPT
NCPT-1 mutants
(H460 cells)
NCPT-1.M1
0.1
NCPT-1.M2
0.1
NCPT-1.M3
0.4
NCPT-1.M4
0.12
NCPT-1.M5
0.15
NCPT-1.M6
0.15
NCPT-1.M7
0.3
NCPT-1.M8
1.5
NCPT-1.M9
3.0
NCPT-1.M10
1.2
NCPT-2.M11
0.47
NCPT-3.M12
0.38
Example 7
Time-Effect Relationship of NCPT-1. M1 in Killing Tumor Cells In Vitro
[0116] Time-Effect Relationship of NCPT-1. M1 in Killing Lung Cancer Cell Line
[0117] At 37° C., H460 cells (ATCC) were adherently cultured to logarithmic growth phase in RPMI1640 medium containing 10% FBS in cell culture flask in 5% CO 2 incubator. NCPT-1.M1 was added to a final concentration of 50 ng/ml, and cultured for 1 h, 2 h, 4 h and 6 h respectively, and then the cellular morphological changes were observed under inverted phase contrast microscope: in the vehicle control group, at 6 h after the addition of vehicle solution, no morphological changes of cell damage were seen ( FIG. 1A ); at 1 h after NCPT-1.M1 addition, no obvious morphological changes of H460 cells were seen ( FIG. 1B ); at 2 h after NCPT-1.M1 addition, morphological changes occurred on some cells: cell shrinkage, cell membrane blebbling, refraction decreased, but detached cells are still rare ( FIG. 1C ); at 4 h after NCPT-1.M1 addition, the above morphological changes occur on a large number of cells, but the detached cells remain rare ( FIG. 1D ); at 6 h after NCPT-1.M1 addition, almost all cells exhibited the above morphological changes, detached from the flask bottom, floated and aggregated into pellets, with only a few normal cells scattered ( FIG. 1F ). At a higher magnification, the cells with morphological changes exhibited the characteristics typical of apoptosis: cytoplasma shrinkage, cell shrinkage, membrane blebbing, resulting in a plurality of apoptotic bodies ( FIG. 1E ). The results show that, the incubation of NCPT-1.M1 with H460 cells for 1-2 h result in the appearance of morphological apoptosis changes and the incubation for 6 h results in apoptosis of maximum number of cells.
[0118] Time-Effect Relationship of NCPT-1.M1 in Killing Multiple Myeloma Cell Line RPMI8226
[0119] The time-effect relationship of NCPT-1.M1 in killing human multiple myeloma cell line RPMI8226 (ATCC) was measured using Chemiluminescence (ATPlite Luminescence Assay System, PerkinElmer) method. The cells at logarithmic growth phase were collected by centrifugation (1000 rpm, 5 min), resuspended in 3% FBS-1640 medium, counted and adjusted to 2×10 5 /ml cell suspension, and added into 96-well culture plates at 50 μl/well. The NCPT-1.M1 sample was diluted to 500 ng/ml, 63 ng/ml, 7.8 ng/ml with 3% FBS-1640 medium, the above NCPT-1.M1 samples were added into culture wells containing 50 μl cells at 50 μl/well with the final concentration of NCPT-1.M1 of 250 ng/ml, 31.5 ng/ml, 3.9 ng/ml, the negative control well was added with the same volume of medium without NCPT-1.M1, and all the above were further cultured at 37° C. under 5% CO2. At 1, 3, 6, 8, 24, 48 h after treatment with NCPT-1.M1, the cell lysis buffer were added into plates at 30 μl/well, and shaken for 3 minutes. When the cells were completely lysed, cell lysates were removed and added into chemiluminescence plate at 90 ul/well. Then chemiluminescent substrate solution was added in the plate at 30 μl/well and shaken for 3 minutes, then the readings were measured. Inhibition rate of NCPT-1.M1 on the cells is calculated based on the luminescence intensity of NCPT-1.M1 treated cells and control cells. The results show that, at 1 h of incubation of RPMI 8226 cells with 250 ng/ml, 31.5 ng/ml, 3.9 ng/ml NCPT-1.M1, no inhibitory effect is observed; at 3 h, different degrees of inhibition are detected and follow positive dose-effect relationship; at 6 h, maximum inhibition is reached and is not significantly different from the inhibitory intensity at 8, 24, 48 h ( FIG. 2 ).
Example 8
Assay of the Apoptosis-Inducing Activity of NCPT-1.M1 In Vitro
[0120] The apoptosis-inducing activity of NCPT-1.M1 on various human tumor cell lines is detected in the present example.
[0121] 1. Morphological Observation on NCPT-1.M1-Induced Apoptosis of Human Multiple Myeloma Cell RPMI 8226
[0122] The RPMI 8226 cells (ATCC) were cultured in cell culture flasks until logarithmic growth phase, collected by centrifugation, resuspended with complete medium (10% FBS-RPMI1640) at 1×10 6 /well, added into 6-well cell culture plate (Costar). The NCPT-1.M1 was diluted with complete medium, added to a final concentration of 200 ng/ml, incubated at 37° C. in 5% CO2 incubator for 3 h. The cells were collected, prepared as smears, fixed with methanol before May-Grünwald-Giemsa (MGG, May-Grünwald stain, commercial available from Beijing ZhongYe HengYuan Chemicals, Giemsa stain, commercial available from Solarbio) staining. At 3 h of incubation of NCPT-1.M1 with cells, the following obvious features of apoptosis were observed: cytoplasma condensation, cell shrinkage, densely staining of chromatin, chromatin aggregation at the periphery of the nucleus, karyopyknosis, karyorrhexis, formation of apoptotic bodies ( FIG. 3 ).
[0123] 2. TUNEL Staining Showing the Induction of Apoptosis of Human Lung Cancer Cell Line NCI-H460
[0124] During the process of apoptosis, the genomic DNA can be broken into double-strand, low molecular weight DNA fragments and high molecular weight single-stranded DNA fragments with broken ends (gaps), and these DNA strand gaps can be identified using enzyme-labeled nucleotide 3′-terminal labeling method. In the case of catalytic action of terminal deoxynucleotidyl transferase (TdT), FITC-labeled nucleotide can be incoporated to the free 3′ end nucleotide with template-independent manner, and thereby making the gap of the DNA strand labeled (TUNEL method). The labeling FITC can be recognized by horseradish peroxidase (POD) conjuncated sheep-derived Fab fragment. Upon development with DAB (3,3-diaminobenzidine), the cells stained as brown, which were apoptotic cells, were examined under light microscopy. TUNEL technique is a common method to detect apoptosis. The apoptosis upon incubation of NCI-H460 cell with NCPT-1.M1 was examined using TUNEL technique. NCI-H460 cells (10% FBS-RPMI1640) at logarithmic growth phase were incubated with NCPT-1.M1 (15 ng/ml) for 4 h, then all adherent and floating cells were collected, washed twice with PBS, prepared with PBS into cell suspension, applied on a glass slide, air dried naturally, and fixed in 4% paraformaldehyde for 30 minutes at room temperature. Other procedures were carried out following instructions of TUNEL Apoptosis Detection Kit (ZK-8005, Beijing Zhongshan Golden Bridge Biotechnology Co., Ltd.). The results show that, upon incubation with NCPT-1.M1 (15 ng/ml) for 4 h, a large number of NCI-H460 cells experience apoptosis, exhibiting karyopyknosis, fragmentation into many nuclear fragments, dense brown granules with varying sizes ( FIG. 4B ). No apoptotic cells are seen in the negative control group ( FIG. 4A ).
[0125] 3. Analysis of Internucleosomal DNA Fragmentation in the Apoptotic Cells
[0126] NCI-H460 cells at logarithmic growth phase were incubated with NCPT-1.M1 (a final concentration of 15 mg/ml) for 2 h, 4 h, 6 h, and the medium control group was not added with NCPT-1.M1. All adherent and floating cells (approximately 5×10 6 ) were collected, and DNA was extracted (Wen Jinkun, Principles and experimental techniques of medical molecular biology, 236-237 (1999)). DNA sample was removed and mixed with 6× loading buffer, and subjected to 1.8% agarose gel (a final concentration of ethidium bromide of 0.5 μg/ml) electrophoresis. The gel was observed under ultraviolet light source and photographed, and analyzed for DNA fragmentation. H460 cells were incubated with NCPT-1.M1 (15 ng/ml) for 2 hours, and its DNA electrophoresis showed obvious ladder, which is the major biochemical feature of apoptosis [Cohen, Advances in Immunol., 50:55-85 (1991)]. To the contrary, in the DNA electrophoresis of the medium control group, a band corresponding to a macromolecule is very near to the loading well, and there is no DNA fragmentation ladder. With the increasing incubation time with NCPT-1.M1, the DNA ladder becomes weaker and vague, and is illegible ( FIG. 5 ), which might be due to DNA being degraded into smaller fragments.
[0127] 4. Caspase-8 Inhibitor Inhibits the Apoptosis-Inducing Activity of NCPT-1.M1.
[0128] H460 cells were incubated with NCPT-1.M1 of 1.2 ng/ml and 10 ng/ml (the culture method is same as the above) for 24 h, and cell survival rates measured by MTT assay were 60% and 16%, respectively. 30 mmol/L Caspase-8 inhibitor zIETD-fmk (Santa Cruz) was added, and 1 h later, 1.2 ng/ml or 10 ng/ml NCPT-1.M1 was added and co-incubated for 24 h, then, the resulting cell survival rates were 100% and 90%, respectively. The results show that Caspase-8 inhibitor blocks the induction of apoptotic activity of NCPT-1.M1 on H460 cells, suggesting that activation of Caspase-8 is involved in the signal transduction pathways of the apoptosis induced by NCPT-1.M1 on H460 cells ( FIG. 6 ).
Example 9
Assay of the Apoptosis-Inducing Activity of NCPT-1.M1 In Vivo
[0129] Balb/c nu athymic nude mice (Beijing Huafukang Biotechnology Co., Ltd.) were subcutaneously inoculated with human MM RPMI8226 tumor cells. When the tumor grew to the volume of 700-800 mm3, the mice were divided into a control group (n=3) and a CPT treatment group (n=3), and were intraperitoneally injected with control or NCPT-1.M1 at a dose of 15 mg/kg once a day for 3 consecutive days. On day 4, the tumor volumes were measured (method same as the above), all animals were sacrificed, the tumors were resected and fixed in 10% formaldehyde solution. The tumor tissues were embedded in paraffin, cut into sections, and HE stained following the conventional methods. The apoptotic assay of the paraffin-embedded tissue sections were carried out following instructions of TUNEL Apoptosis Detection Kit (ZK-8005, Beijing Zhongshan Golden Bridge Biotechnology Co., Ltd.). Following three consecutive days of treatment with NCPT-1.M1, the average tumor volume was significantly reduced from 798 mm 3 before dosing to 286 mm 3 . HE staining shows a lot of apoptotic cells with condensed and fractured nucleus of blue-black staining, and pale red cytoplasma ( FIG. 7B ). To the contrary, the nucleus of normal cells are light blue or blue ( FIG. 7A ). Upon TUNEL staining, the nuclei of apoptotic cells are stained as brown ( FIG. 7D ). The results show that NCPT-1.M1 treatment can quickly result in apoptosis of a lot of MM tumor cells.
Example 10
The Inhibitory Activity of NCPT-1.M1 on Xenograft Tumors in Nude Mice
[0130] The inhibitory activity on human colon cancer xenograft tumors:
[0131] 4 to 5 weeks old Balb/c nu mice ♂ (Institute of Experimental Animals, Chinese Academy of Medical Sciences) were subcutaneously inoculated with COLO 205 human colon tumor tissue pieces. When the tumor grew to the volume of 120 mm3, the tumor-bearing mice were divided into 4 groups (n=7/group), which were intraperitoneally injected with normal saline (negative control group), NCPT-1.M1 5 mg/kg, NCPT-1.M1 15 mg/kg and wtTRAIL 15 mg/kg once a day for 10 consecutive days. Upon the withdrawal, the mice were observed for further 12 days before the end of the experiment. During the experiment, the tumor length diameter (a) and wide diameter (b) were measured every two days with a vernier caliper, and tumor volume (TV) was calculated according to the following formula: TV=½×a×b 2 ; From the above, the relative tumor volume (RTV) was calculated according to following formula: RTV=V t /V 0 . Wherein V 0 is the tumor volume measured on the day of the administration, but before administration (i.e., d0), and V t is the tumor volume measured every time. The relative tumor proliferation rate T/C (%) is used as an evaluation index. Evaluation criteria: T/C (%)>40% means no effect; T/C (%)≦40% and the statistical significance of P<0.05 means being effective.
[0000] T/C %=RTV T /RTV C *100%.
[0132] (RTV T : RTV of the treatment group; RTV T : RTV of the negative control group).
[0133] As can be seen from Table A, T/C (%) of both two dosage groups of NCPT-1.M1 and wtTRAIL group are all <40%, P<0.05 when compared with the control group, which shows that both two dosage groups of NCPT-1.M1 and wtTRAIL are effective in this tumor model. The efficacy of wtTRAIL with dosage of 15 mg/kg is significantly weaker than that of NCPT-1.M1 with the same dosage (P<0.05), and is comparable to that of NCPT-1.M1 with dosage of 5 mg/kg.
[0000]
TABLE A
The growth of human COLO 205 xenograft tumor in mice
was significantly inhibited by NCPT-1.M1
tumor
Tumor
proliferation
Number of
volume
TV(mm 3 )
relative tumor
rate
Groups
animals
beginning
ending
volume RTV
T/C(%)
Negative control
7
124 ± 49.1
624 ±
246.0
4.65 ±
1.667
NCPT-1.M1
7
117 ± 20.4
197 ±
146.2
1.39 ±
0.571*
29.89
5 mg/kg
NCPT-1.M1
7
118 ± 21.0
15 ±
14.6
0.12 ±
0.117**
2.58
15 mg/kg
wtTRAIL
7
127 ± 38.3
212 ±
80.7
1.58 ±
0.372*#
33.98
15 mg/kg
*P < 0.05;
**P < 0.001 vs. the negative control group
#P < 0.05: vs. CPTm1 15 mg/kg group
[0134] The inhibitory activity on xenograft tumor of human multiple myeloma:
[0135] Athymic nude mice (Beijing Huafukang Biotechnology Co., Ltd.) were subcutaneously inoculated with 5×10 6 RPMI8226 tumor cells/mouse. When the tumor grew to the volume of 500 mm3, the mice were divided into several groups, which were intraperitoneally injected with normal saline (negative control group), NCPT-1.M1 (15 mg/kg) and wtTRAIL (15 mg/kg or 45 mg/kg) once a day for 8 consecutive days. The tumor volumes were measured with a caliper every two days. Tumor growth rate of NCPT-1.M1 group with a dose of 15 mg/kg is significantly lower than that of TRAIL group with a dose of 45 mg/kg, suggesting that NCPT-1.M1 has a tumor inhibitory activity stronger on RPMI8226 than that of wild-type TRAIL ( FIG. 8 ).
Example 11
The Inhibitory Activity of NCPT-1.M1 Combined with Chemotherapeutics on Human Multiple Myeloma Cell Lines
[0136] In this example, the tumor-killing effects of NCPT-1.M1 combined with chemotherapeutic agent Melphalan (Glaxo SmithKline) on human multiple myeloma cell line RPMI 8226, H929, U266 B1 (all from ATCC) were measured using chemiluminescence (ATPlite Luminescence Assay System, PerkinElmer) method, wherein both RPMI8226 and H929 are cell lines sensitive to NCPT-1.M1 and U266B1 is insensitive to NCPT-1.M1. The cells at logarithmic growth phase were collected by centrifugation, prepared with RPMI1640 medium containing 10% fetal bovine serum (FBS) into cell suspension at a density of 2×10 5 ˜3×10 5 /ml, and added into 96-well culture plates (NUNC) at 1×10 4 ˜1.5×10 4 /well. The NCPT-1.M1 and melphalan were 2-(or 3- or 4-) serial diluted with the above medium, and melphalan (or NCPT-1.M1) was diluted with NCPT-1.M1 solution (or melphalan sulution) of a certain concentration, added into the above culture plate, incubated at 37° C. in 5% CO 2 incubator for 48 h before stopping the reaction, then the chemiluminescence was detected. The cell survival rates were calculated based on the luminous intensity value of the experimental wells and control wells, the results of combination treatment were analyzed using the median efficiency analysis software CalcuSyn V2 (BIOSOFT), and CI means a Combination Index. CI between 0.9 and 1.1 is indicative of an additive effect of the two drugs; CI<0.9 is indicative of a synergistic effect of the two drugs; and CI>1.1 is indicative of an antagonistic effect of the two drugs.
[0137] U266B1 is insensitive to NCPT-1.M1, following 48 h incubation with 1 μg/ml NCPT-1.M1, over 80% cells survived. However, the cell survival rate (7.0-62.4%) in the co-presence of melphalan (12.5˜50 μg/ml) was significantly lower than that of NCPT-1.M1 alone (85.0%) or melphalan alone (11.9˜100.9%), suggesting that the combination of them has an enhanced killing activity ( FIG. 9 ). The combinations of melphalan (12.5 μg/ml) with varying concentrations of NCPT-1.M1 (63˜1000 ng/ml) were added to H929 cells sensitive to NCPT-1.M1, and the survival rate was significantly lower than that of the melphalan alone and NCPT-1.M1 alone. There was a synergistic effect of them (CI index of 0.563˜0.835) ( FIG. 10 ). Similarly, the combination of melphalan (25 μg/ml) with varying concentrations of NCPT-1.M1 (2˜500 ng/ml) were added to RPMI 8226 cells sensitive to NCPT-1.M1, and a synergistic effect of them was observed (CI index of 0.039˜0.368) ( FIG. 11 ).
Example 12
The Inhibitory Activity of NCPT-1.M1 Combined with Chemotherapeutics on Xenograft Tumors in Nude Mice
[0138] The inhibitory activity of NCPT-1.M1 combined with melphalan and prednisone on human multiple myeloma xenograft tumor.
[0139] Male Balb/c nu athymic nude mice (Beijing Huafukang Biotechnology Co., Ltd.) were subcutaneously inoculated with 5×10 6 RPMI8226 tumor cells/mouse. When the tumor grew to about 500 mm 3 -600 mm 3 , the mice were divided into normal saline control group (ip.), NCPT-1.M1 group (15 mg/kg, ip, once a day for 10 consecutive days), melphalan (0.75 mg/kg, po., once a day for 5 consecutive days) combined with prednisone group (10 mg/kg, PO. once a day for 10 consecutive days, ig.), NCPT-1.M1 combined with melphalan and prednisone group (dosage, administration method and frequency of each drug were same as the above). The tumor volumes were measured with a caliper every two days. At the end of the experiment, the tumor volumes of NCPT-1.M1 combined with melphalan and prednisone group were significantly lower than that of NCPT-1.M1 monotherapy group and melphalan combined with prednisone group (P<0.05). When these three drugs are combined, the tumors completely disappeared in 57% mice, and in NCPT-1.M1 monotherapy group, the tumors completely disappeared in only 16% mice, and no tumor completely disappeared in melphalan combined with prednisone group. The results suggest that the tumor inhibitory effect of the triple combination of NCPT-1.M1, melphalan and prednisone on RPMI8226 tumor is significantly enhanced ( FIG. 12 ).
[0140] The inhibitory effect of NCPT-1.M1 combined with paclitaxel and carboplatin on human lung cancer xenograft tumor.
[0141] 5-6 weeks old Balb/c nu athymic nude mice ♂ (provided by Institute of Experimental Animals, Chinese Academy of Medical Sciences) were subcutaneously inoculated with NCI-H460 human lung tumor. When the tumor grew to the size of about 150 mm3, the mice were divided into following and administered: normal saline control group (ip.), NCPT-1.M1 monotherapy group (15 mg/kg, i.p., once a day for 9 consecutive days), chemotherapy group (PC regimen: paclitaxel 30 mg/kg i.p. and carboplatin 60 mg/kg i.p., administered once on the first day), NCPT-1.M1 combination chemotherapy group (administration manner and dosage of each drug are same as the above). During the experiment, the tumor length diameter (a) and wide diameter (b) were measured every two days with a vernier caliper, and tumor volume (, TV) is calculated according to the following formula: TV=½×a×b 2 . From the above, the relative tumor volume (RTV) was calculated according to following formula: RTV=V t /V 0 . Wherein V 0 is the tumor volume measured on the day of the administration, but before administration (i.e., d0), and V t is the tumor volume measured every time. The relative tumor proliferation rate T/C (%) is used as an evaluation index.
[0000] T/C %=RTV T /RTV C *100%.
[0142] (RTV T : RTV of the treatment group; RTV T : RTV of the negative control group).
[0143] As can be seen from Table B, T/C (%) of NCPT-1.M1 monotherapy group and chemotherapy group are 43.9% and 39.8% respectively, and the tumor inhibitory effect of them are significantly improved compared with control group (P<0.05). The T/C (%) of NCPT-1.M1 combination chemotherapy group is 0.8%, which is significantly better than that of NCPT-1.M1 monotherapy group and chemotherapy group (P<0.001). With the NCPT-1.M1 combination chemotherapy, the tumor completely disappear in 66.7% of the mice, while no tumor completely disappear in the other groups, suggesting that the combination of NCPT-1.M1 and chemotherapeutics may have stronger therapeutic effect on those patients with clinical lung cancer ( FIG. 13 ).
[0000]
TABLE B
The tumor-inhibiting effect of NCPT-1.M1 alone and its
combination with paclitaxel and carboplatin on H460 tumor in nude mice
Number
of
animals
beginning/
Body weight(g)
Tumor size(mm 3 )
groups
ending
begining
ending
begining
ending
RTV
T/C
Negative
6
6
17.7 ± 2.71
18.9 ± 2.84
142 ± 74.8
1854 ± 458.6
16.67 ± 9.218
control
NCPT-1.M1
6
6
19.9 ± 3.08
20.9 ± 3.32
156 ± 82.6
867 ± 255.7
7.32 ± 3.736*
43.9%
15 mg/kg
###+++
paclitaxel,
carboplatin
6
6
19.4 ± 1.16
21.5 ± 1.36
172 ± 87.9
32 ± 45.2
0.13 ± 0.194**
0.8%
+
NCPT-1.M1
15 mg/kg
paclitaxel
30 mg/kg
6
6
19.7 ± 1.32
21.1 ± 1.07
144 ± 42.4
962 ± 311.6
6.64 ± 0.999*
39.8%
carboplatin
60 mg/kg
Note:
*P < 0.05,
**P < 0.005 vs. the negative control group;
###: P < 0.001, vs. the chemotherapy drugs paclitaxel 30 mg/kg and carboplatin 60 mg/kg group alone
+++: P < 0.001, vs. NCPT-1.M1 15 mg/kg group alone
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Provided is a fusion protein comprising circularly permuted form of TRAIL, and the fusion protein contains circularly permuted form of TRAIL and oligopeptides located at the N-terminus and/or C-terminus of the permuted form. The oligopeptides contain a repeating sequence consisting of 3-10 histidines. The components of the circularly permuted form of TRAIL from N-terminus to C-terminus are: (a) amino acids 135-281 of TRAIL, (b) a linker, and (c) amino acids 121-135 of TRAIL or amino acids 114-135 of TRAIL or amino acids 95-135 of TRAIL or any fragments of amino acids 95-135 of TRAIL containing amino acids 121-135 of TRAIL. Also provided is a method for treating cancer by using the fusion protein.
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RELATED APPLICATIONS
This application is related to and claims the benefit and priority of U.S. Provisional Application 61/540,147, bearing the same title, filed on Sep. 28, 2011, which is, along with the references cited therein, herein incorporated by reference.
TECHNICAL FIELD
The present application relates to dermatological treatments, including the treatment of scars and other skin damage benefiting from surface frictional or vibratory action at a location of said conditions.
BACKGROUND
Various conditions of the skin can be treated by topical action or applications. For example, topically applied compounds, drugs or healing substances can improve an unwanted condition of the skin, reduce its effect, or alleviate the suffering caused by the condition. Examples of conditions of this nature include recovering wounds and cuts, scars, blemishes, acne, and others.
As an example, wounds leave behind scars after the wound heals, scars varying in their degree of visibility depending on several factors. One reason that scars are visible to the eye is that scars may be created in geometrical patterns, such as in straight lines as would happen if a sharp instrument caused the wound that resulted in the scar. Also, when the skin heals following a wound, the formation of the scar may cause contraction or pulling on adjacent areas of skin and this tension in the skin may cause deformation in the adjacent skin or organs, especially if the scar is near a facial organ such as the lips or eye lids. Another reason that scars are visible and considered unsightly is that they may carry a discoloration or a different color from the surrounding skin. Typically, scars may have a pale appearance or may have a reddish or brown colored appearance sometimes known as hyper pigmentation. Hyper pigmentation is sometimes treated with bleaching agents. When a scar causes redness this may sometimes be treated with a laser that softens the appearance of redness. Loss of color or hardening in the scar tissue is sometimes treated using steroid injections to soften the tissue in the vicinity of the scar.
For especially unsightly scars, cosmetic surgery may be applied after the scar is well formed, which is usually six or twelve months following the healing of the wound. An evaluation of the scar is made by a cosmetic surgeon and a variety of surgical techniques may be applied to the scar to mitigate its appears or to reduce the obviousness of the scar to the observers eye. As stated above, since scars are sometimes more visible when they are formed in straight lines that are readily apparent to the observer's eye, surgical techniques may be applied to break up the geometric or straight line configuration of the scar. In one technique a geometric broken line repair is made that causes a previously straight scar to have a more convoluted shape. In other techniques, a procedure known as z-plasty applies small fresh cuts in the vicinity of the scar and rolls them inward to cause an irregular appearance, which is applied in cases of where there is insufficient tissue near the scar to perform a geometric broken line repair. In yet other circumstances, a so-called “running w-plasty” is performed, which is a compromise of the two techniques described above.
For scars that have caused unsightly hard tissue at the surface of the skin, a mechanical dermabrasion or sanding of the scar tissue may be performed to reduce this appearance.
The above cosmetic surgical procedures are generally expensive and only required or appropriate for severe scarring. These procedures generally require the creation of fresh wounds deliberately that cut into the skin so as to create correspondingly newer scars that have a less offensive appearance. Therefore, there are risks and discomfort issues associated with the above techniques that are both expensive painful and inconvenient. Following the above-mentioned surgical procedures, the patient is required to typically wait several months for the surgical cuts and wounds to heal, after which the desired reconfigured scars become apparent and in the best cases outcomes, the new reconfigured scars are less unsightly than the original scar. It can be appreciated that the inconvenience, cost and discomfort, as well as the invasive nature of the above surgical procedures are not ideal or pleasant for the patient that undergoes them.
In other modalities, physical and mechanical stimulation of scar tissue has been found to soften and ameliorate the intensity of the scar in certain patients. As an example, physical therapy including massage and rubbing of the scar tissue and adjacent skin has been found to provide certain benefits to patients with scars. The procedures for reduction of the size or appearance of a scar are generally referred to here in as scar revision. It has also been found that in some situations acoustics may be used, such as by application of ultrasound to scar tissue in order to cause vibratory mechanical treatment of the scar tissue that assists in scar revision. However, the devices and techniques presently employed for scar revision are collectively expensive, inconvenient, uncomfortable, and not as effective as would be desired.
Some existing efforts to apply vibratory action to a skin surface are found in the art. US Pub. No. 2009/0259168 A1, which is directed to a vibrating element in a sticky bandage that is stuck to the skin for application of cosmetic agents or drugs thereto through massaging action of the vibrating element, including battery powered embodiments and embodiments having programmable activation logic. But this reference adheres its bandage (the “sticky bandage” or “SB”) to the skin and is not useful for treating conditions that benefit from abrasive action of the applicator or that require relative movement between a surface and the affected skin region.
U.S. Pat. No. 7,628,764 applies a portable ultrasonic source to purportedly heal wounds. The transducer is placed proximal to the wound and emits ultrasonic energy towards the wound as longitudinal or shear waves. The ultrasonic frequency used in this reference is rather high for most applications that benefit from massaging action and the ultrasonic transducer is not configured in the reference to apply relative movement or abrasive action.
U.S. Pat. No. 4,372,296 is directed to a composition that is topically applied to skin for treatment of acne and purportedly speeds the healing of scars through stimulation of the production of collagen and if the composition is sonicated into the affected area using an ultrasonic vibrating element.
US Pub. No. 2008/0058648 A1 is directed to an ultrasonic device for treatment of wounds whereby the device is powered to cause acoustic cavitation in the wound and thereby purportedly increase the delivery of energy to the debrided tissue regions for enhancing healing. This apparatus cannot be applied conveniently or for prolonged periods of time to a patient, and causes effects from the cavitation and ultrasonic energy that are generally not consistent with the action desired in the present application.
US Pub. No. 2003/0212350 is directed to treatment of scar tissue using a suction device that raises the scar tissue so that manual manipulation or sonic vibration can be applied to disrupt the fibrous tissues of the scar. This apparatus like others above is not suited for convenient application to a user's skin and is awkward to use, heavy, and cannot be applied for lengthy time periods. Also, it lacks the desired curative action of the present disclosure as will be clear below.
Accordingly, the present disclosure describes embodiments for an apparatus and a technique for treatment of skin conditions and for accelerating or allowing scar revision using vibratory energy applied at or near the location of a scar.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 illustrates an exemplary block diagram of an apparatus for scar revision and other beneficial dermatological effects;
FIG. 2 illustrates some exemplary modes of movement of the surface against the skin;
FIG. 3 illustrates an exemplary apparatus with prime mover for scar revision and other beneficial dermatological effects;
FIG. 4 illustrates another exemplary apparatus with prime mover for scar revision and other beneficial dermatological effects; and
FIG. 5 illustrates a band wrappable about a limb or organ for securing a scar revision device to an area of the skin having a wound or scar.
DETAILED DESCRIPTION
FIG. 1 illustrates an exemplary apparatus 10 for treating wounds and causing or enhancing scar revision. The device of FIG. 1 may preferably be light and small in size so that it can be applied to a location on the skin of a person without difficulty or discomfort. In some embodiments, the device is applied using a sticky substance or adhesive strip or patch so that it adheres to the scarred location of the skin. The device then ameliorates the scar and achieves or assists in scar revision by action as described below.
Generally, the device 10 applies a mechanical vibratory action to a local region of skin tissue proximal to the lower face of the device. The vibratory action assists in scar revision through a number of ways, including by massaging the area to enhance healing blood flow, stimulation of tissue and nerves, mechanical rubbing of the scarred skin, enhancement of the uptake of medicinal agents into the skin, gentle thermal action, or other useful means. The device is battery powered, said battery power providing the energy to drive the vibratory action of the device and also to allow for other electronic functions as will be explained further in the context of the present exemplary embodiments.
The following discussion describes one or more preferred embodiments for the sake of illustration. Alternative embodiments will become apparent to those skilled in the art, and various ways of interconnecting and arranging the elements and components of the device are possible. Some items described herein are optional and do not need to be implemented in every instance, while other optional variations may be added to those presently disclosed without substantially departing from the nature of the invention.
As mentioned previously, the housing 100 of scar revision device 10 is preferably compact and lightweight and contains a number of components. A power source 130 (e.g., a battery) is disposed in a location in the housing 100 that permits replacement of the battery 130 . For example, a small battery such as is used in wrist watches, hearing aids, or similar small devices is employed and located below a cover at the upper face of housing 100 . The cover and housing may be water resistant or water proof. A first light emitting diode (LED) 190 may be positioned at the upper face of the device to alert to a low-battery condition so that the user may replace the battery for continued operation.
A microprocessor 110 is powered from battery 130 and controls some or all electronic operations of the device. Microprocessor 110 may be an application specific integrated circuit (ASIC) or an off the shelf semiconductor integrated circuit (IC) chip, or other electronic circuit having logic elements to carry out simple tasks. A digital memory device 120 may be coupled to microprocessor 110 . The memory 120 can hold program instructions to be executed by the microprocessor 110 , and may be programmable in ways known to those skilled in the microprocessor and programming arts. In some embodiments, the device 10 comes preconfigured from the manufacturing source with program instructions residing in memory 120 . In other embodiments, memory 120 has program instructions loaded into it that are customized for a particular user of the device. In a specific example, a clinical practitioner can program instructions (by way of an interface 125 ) to suit the medical needs of the patient. The instructions can be generated automatically by a computer that interfaces with the practitioner using a high-level user interface and then interfaces to device interface 125 through suitable hardware, which can include a wireless data connection.
Memory 120 may include volatile as well as non-volatile sections. Memory 120 may also be used to store operating condition information that can later be uploaded to a computer for review by a practitioner or physician. The operating condition information can be a log of certain parameters sensed by the device or a log of the operating schedule of the device. Microprocessor 110 can retrieve the log of the operating condition information from memory 120 and transmit this to a computer through a wireless or hard wired interface 115 . In some cases, the operation of the unit 10 can be monitored by bringing the unit into proximity with an appropriate sensor/reader. The reader can pick up data and operating information from the device accordingly.
Once programmed to operate, microprocessor 110 drives an amplifier or other electrical energy driver 140 at a determined rate. Driver 140 may be an amplifier that receives a driving signal from microprocessor 110 and amplifies the signal to drive a transducer (e.g., a piezoelectric crystal) 150 accordingly. The transducer 150 then vibrates or generates mechanical or acoustical oscillations. In some embodiments, the transducer 150 is mechanically coupled or fixed to a solid substrate 160 that better transmits the energy from transducer 150 into the underlying proximal scar tissue 180 . The transmission of vibratory energy from the transducer 150 and solid substrate 160 may in some embodiments be enhanced by application of a transmission gel 170 that better couples the device 10 to the tissue 180 . The transmission gel may be medicated with balms or medicinal substances intended for topical application to the affected tissue 180 , and in some embodiments, may also be designed for penetration into or through the dermis of the patient to achieve a deeper effect.
In some embodiments, very fine spikes 165 are fixed to the solid substrate 160 . Spikes 165 can act to mechanically anchor and secure the device 10 to the patient's tissue, but are fine enough not to cause pain or bleeding. Also, the spikes can act to transmit the vibratory energy from the transducer 150 and solid substrate 160 to regions deeper than the surface of tissue 180 . In addition, the spikes can act to allow better introduction of medicated liquids or gels or topical applications of medicinal agents into the tissue 180 .
A second LED 195 may be controlled by microprocessor 110 to indicate certain conditions to the user. In one example, LED 195 is illuminated when transducer 150 is powered. In another example, the LED is illuminated to indicate a fault condition in the circuitry of the device 10 . In yet another example, the LED 195 is made to blink at a rate corresponding to a state of operation of the device 10 . In still another example, LED 195 indicates a communication state, for example, indicative of a connection status of the device 10 .
As mentioned, one aspect of the present system and method is application of surface vibratory, abrasive and/or mechanical relative motion between a surface of the apparatus and the surface of the skin at the area to be treated. The gentle repetitive scraping and massaging and exfoliating actions made possible thereby can be programmably and suitably adapted for many applications and ailments and situations. In some embodiments, a direction of relative motion between the vibrating applicator and the underlying skin is determined for the given context in which it is used. In other aspects, the apparatus may be made to apply a plurality of types of vibratory motion with respect to the skin as will be described below. Circulation in the skin tissue proximal to the abrasive or massaging or rubbing action as well as improved oxygen delivery to the same can accelerate healing and have other beneficial effects.
FIG. 2 illustrates a number of exemplary ways of applying vibrational or relative motion between the vibrating apparatus and the skin. In example 22 , the abrasive surface is made to provide unidirectional undulating movement with respect to the skin. In practice this may be provided by micromechanical elements in the abrasive surface or in a layer attached to the abrasive surface. Alternatively, mechanical rollers or piezo electric synchros may provide the rolling or stretching motion of the abrasive surface so that it rubs the skin or a scar along a preferred direction. The preferred direction may be for example along an axis of the abrasive surface device, which may be configured like a bandage having a central portion of its face proximal to the skin that is not adhesive but instead allows rubbing, massaging, scraping, exfoliating, or vibrating of the collagen and tough fibers of a scar. The motion according to example 22 may be applied cross-wise or perpendicular to a direction of the scar or collagen fibers.
In the same figure, example 24 illustrates an embodiment whereby the undulation or substantially linear wiping movement of the abrasive surface goes back and forth as indicated by the arrows, such that there is an axial effect to the rubbing motion but it is equally applied in a forward and a backward direction.
In example 26 of the same figure, a substantially circular movement about a central axis perpendicular to the plane of the abrasive surface and the skin surface occurs. The bandage-like applicator has optionally some adhesive edges but a central portion that is not adhered to the skin and that can provide relative motion between the abrasive surface and the skin to rub the skin along the circular pattern or patterns. Again, micro electro-mechanical elements or piezo layers may be used to cause the present motion. Also, small motors or mechanical rollers can also be coupled to a layer near the abrasive layer so as to transmit the mechanical movement thereof to the surface of the affected skin.
In example 28 of the same figure the movement of the abrasive surface is radially applied along a plurality of directions with respect to a center of the motion.
Note that an apparatus can be programmed or controlled by software instructions and/or a microprocessor having embedded or stored commands to cause the apparatus to switch between one or more of the above movement types as well as many others that would occur to one skilled in the art. It can cycle through several motion types, dwelling on each a determined period of time.
Still optionally, the apparatus may include a sensor. The sensor can sense some environmental or biological parameter. The sensor provides a signal indicative of the detected parameter. This signal can then be used by a controller or microprocessor logic to decide when to activate, stop, or switch the mode or operation or the intensity of the vibratory movement of the motion driver in the apparatus. So, as mentioned before, the device can switch on, off, or between one or more states based on a dwell time or duty cycle program. Also, the device can sense a temperature, pulse rate, perfusion level, oxygen level, perspiration activity or other parameter to cause the above state changes to the operation of the apparatus.
FIG. 3 illustrates an exemplary cross section of a vibrating apparatus 30 for treating a dermatological condition. The apparatus is generally contained in a housing or strip (here not drawn to scale for clarity) or package 300 . A driver or vibrator 310 , which can be a piezo element, small motor, or other repetitive vibrating component, vibrates or oscillates when driven by an electric power source. The electric power may be derived from a battery or electrical coupling or may be solar-powered by way of a small solar (light) collecting panel at the top surface of housing or package 300 .
Mechanical energy is transmitted from driver 310 through a support post or rigid member 320 to abrasive layer 340 , said support post 320 being mechanically coupled to both the vibratory driver 310 as well as the abrasive layer 340 on a first face (e.g. an upper face) thereof. A second (e.g. a lower face) of abrasive layer 340 is applied to a patient's skin 360 without gluing, fixing, adhering or otherwise sticking abrasive layer 340 to skin 360 , but rather, abrasive layer 340 is allowed to rub and scratch and abrade the skin 360 according to the movement supplied by driver 310 and support post 320 .
A semi-rigid layer 330 may surround abrasive layer 340 . Also, a sticky or adhesive layer 350 can separate a portion of the device 30 and the skin 360 and allow adhesion of the device 30 to the skin 360 while still allowing the abrasive layer 340 to move with respect to the skin 360 . That is, a central portion of the apparatus proximal to the skin can be allowed to dry or wet abrade the skin while the device as a whole is secured to or taped to the skin at portions that are proximal to the skin but generally outside the abrasive treatment zone.
FIG. 4 illustrates yet another exemplary embodiment in cross section. The apparatus 40 includes a housing or package 400 (not drawn to scale for clarity). Inside housing or packaging 400 resides a vibrating powered element 410 similar to those described above. The abrasive layer 440 is not directly coupled to or driven by the driver 410 . But instead, the movement of the driver 410 is transmitted through posts or couplings 420 to a rigid or semi-rigid layer 430 . Since layer 430 is mechanically coupled to the abrasive layer 440 .
In either, both or other similar embodiments, cosmetic or medicinal agents or lotions or drugs may be placed between the most proximal surface of apparatus 30 , 40 and the skin being treated. The substances between apparatus 30 , 40 and the skin may be topical agents to assist in scar remediation or other skin condition treatment as known to those skilled in the art.
Those skilled in the art would also appreciate that programming the device 10 to vibrate at preferred frequency and intensity and cycles can assist in scar revision. For example, the device can operate continuously at a resonance frequency of transducer 150 . Alternatively, the device can vibrate with a given duty cycle (ON-OFF or ON-OFF-OFF etc.) as needed. This can save battery life and prolong the time the treatment can go on before a battery needs replacement. Also, it may be optimal for the scar revision to allow the tissue to be quiescent for some time between applications of the vibratory action. The intensity of the vibration can also be modulated according to a program by application of varying power by driver 140 . In some embodiments, the vibratory action is centered about a given center frequency determined to enhance scar revision.
FIG. 5 illustrates an apparatus 50 for wound treatment or scar revision according to some embodiments. A patient's body or a limb for example is shown in cross section 530 . For example, the apparatus or device 50 is to be applied to a patient's forearm to treat a wound or apply scar revision thereto. A scar 532 is depicted graphically at some location on the surface of the body part 530 . The active frictional or vibrating element 500 may be similar to those described above.
In an aspect, the frictional or vibrating element 500 is part of or secured to a band 510 . The band 510 may be elastic (stretchable) to apply pressure around the body 530 in an embodiment, e.g., made of a medical type of elastic fabric material. The band 510 may also be not stretchable in other embodiments, e.g., made of plastic, leather, fabric or other suitable material. The band 510 is wrapped about the patient (or his or her limb in the above example) 530 . The band 510 may be secured by any of a number of appropriate methods of securing the band 510 about the patient 530 . For example, hook-and-loop fasteners 516 can be provided on proximal faces of band 510 near a first end 512 and a second end 514 thereof. Alternately, or in addition, a snap, rivet, magnetic or mechanical latch, or other similar mating pair of fasteners 542 may be provided to so secure the band 510 about the patient 530 . Belt buckles, zipper ties and other fastening methods are also contemplated hereby, but not limited to those given here by way of example.
The band 510 is applied so that the active frictional or vibrating element 500 is positioned over the skin at the location of the scar 532 to be treated. The band 510 is tightened as shown by 544 to an appropriate firmness about the patient 530 . The device 50 is then operated as described above to treat the wound or scar.
Note that the band 510 does not necessarily need to circumferentially extend all the way around the patient 530 in some embodiments, but may be clamped around a portion of the patient's anatomy (like a bracelet) using flexible members that secure the active vibrating element 500 in place with respect to the scar 532 .
The examples described and shown are exemplary. These and other features and alternatives would now be apparent to those skilled in the art and are comprehended hereby so that the scope of the present disclosure is not limited to the illustrative embodiments described and explicitly shown.
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An apparatus provides controlled vibratory stimulation to skin at an area suffering from a condition, for example scarred tissue locations. The vibratory action and other action of agents used in conjunction with the apparatus permit revision of scars and general treatment of skin conditions and improved or accelerated healing thereof.
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FIELD OF THE INVENTION
This invention relates to ventilation and more particularly to floor type registers and more specifically to a motorized air vent.
BACKGROUND
Air vents and air diffusers are well known in HVAC systems for commercial and residential applications. However an easily operated motorized air vent is required to prevent stooping and bending of the back when opening or closing them. Another requirement is to have a motorized air vent that can be remotely controlled from a wall mounted fixture by radio communications. Still a further requirement is to have a motorized air vent that can be logically tied to thermostats to regulate opening and closing as a function of heat demand in a particular room.
My invention seeks to satisfy these requirements by providing a motorized air vent that is easy to operate, remotely operable and capable of operation in concert with thermostats.
SUMMARY
In satisfaction of the above-cited requirements my invention provides for a motorized air vent for controlling an air flow in an HVAC system. The motorized air vent comprises a first rectangular frame adapted for supported placement abutting a planar surface; air diffusion means mounted within the first rectangular frame; a second rectangular frame depending from the first rectangular frame; vent closure means mounted operatively within the second rectangular frame and positioned adjacent to the air diffusion means; and, means for sliding the vent closure means open and closed. The first rectangular frame is sized for placement around a rectangular hole in a planar surface such as a floor, a wall or a ceiling. The first rectangular frame supports the motorized air vent within the rectangular hole. The air diffusion means comprises a first mesh pattern adapted for omni-directional air diffusion and comprises a plurality of equally spaced and parallel horizontal and vertical members forming a matrix of equally sized rectangular apertures. The vent closure means comprises a thin rectangular damper comprising a second matrix matching the first matrix. When the second matrix and the first matrix coincide the motorized air vent is full open and when the second matrix and the first matrix are fully offset, the motorized air vent is fully closed. An electric motor and cam assembly is used to move the second matrix from side to side between an open and closed position. The electric motor has control means which comprise remote control means operable from a wall consol or by operation of a thermostat.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a bottom and top perspective view of one example of the invention.
FIG. 2 is a disassembled view of one example of the invention.
FIG. 3 comprises a number of views of the moveable damper of one example of the invention.
FIG. 4 is a bottom view of one example of the invention in a disassembled state.
FIG. 5 comprises two views of the drive motor assembly in a disassembled state in one example of the invention.
FIG. 6 comprises a variety of views of the drive motor assembly in an assembled state in one example of the invention.
FIG. 7 comprises a variety of views of the cam body and cam head of one example of the invention.
DETAILED DESCRIPTION
Referring now to FIG. 1A and FIG. 1B , my invention is a motorized air vent ( 10 ) comprises a first rectangular frame ( 14 ) having a top surface ( 16 ), a bottom surface ( 18 ), a length ( 20 ) and a width ( 22 ). The first rectangular frame ( 14 ) is adapted for supported placement abutting a planar surface such as a floor surface, a wall surface or a ceiling surface. Within the first rectangular frame is air diffusion means ( 24 ) adapted for distributing the air flow ( 12 ) in an omni-directional pattern. In other examples of my invention, the air diffusion means can direct air in specific directions. The invention also comprises a second rectangular frame ( 26 ) depending from the first rectangular frame ( 14 ). Vent closure means ( 28 ) is mounted operatively within the second rectangular frame ( 26 ) and positioned below and adjacent to the air diffusion means ( 24 ). The invention further comprises means ( 30 ) for sliding the vent closure means ( 28 ) open and closed. Means ( 30 ) for sliding is in an operative relationship with the air diffusion means ( 24 ) permitting air flow control. In one embodiment of the invention, the motorized air vent is remotely controlled from a wall-mounted unit.
The first rectangular frame ( 14 ) is sized for placement around a rectangular hole in the planar surface. The rectangular hole terminates an air duct. The rectangular hole is sized to receive the second rectangular frame ( 26 ) in relatively air tight agreement so that the air flow through the duct is directed to the air diffusion means ( 24 ). The first rectangular frame ( 14 ) supports the motorized air vent ( 10 ) within the rectangular hole.
Referring now to FIG. 2 , the air diffusion means ( 24 ) comprises a first mesh pattern ( 32 ) adapted for omni-directional air diffusion. The first mesh pattern comprises a plurality of equally spaced and parallel horizontal ( 34 ) and vertical ( 36 ) members forming a matrix of equally sized rectangular apertures ( 38 ). The first mesh pattern is surrounded by rectangular frame ( 14 ) and generally flush with it. The vent closure means ( 28 ) comprises a thin rectangular damper ( 40 ) comprising a second mesh pattern ( 42 ) comprising vertical members ( 46 ) and horizontal members ( 48 ) thereby forming a matrix of apertures ( 44 ) matching the first matrix of apertures ( 38 ). When the apertures ( 44 ) of the second matrix and the apertures ( 38 ) of the first matrix coincide the motorized air vent ( 10 ) is fully open. When the second mesh pattern ( 42 ) and the first mesh pattern ( 32 ) are fully offset, the vertical members ( 46 ) of the damper ( 40 ) block the apertures ( 38 ) and the motorized air vent ( 10 ) is fully closed. The motorized air vent is adjustable by sliding means ( 30 ) between a fully open and a fully closed position, that is, when the first and second matrices are partially offset.
Referring now to FIG. 3 A to F there is shown a variety of views of the damper ( 40 ). “A” is a top view, “B” is a long-side view, “C” is a bottom view, “D” is a short-side view, “E” is a top perspective view and “F” is a bottom perspective view. Illustrated elements are the apertures ( 44 ), the vertical elements ( 46 ) of the mesh and the horizontal elements of the mesh ( 48 ). FIGS. 3C and F illustrate recess ( 114 ) located at the bottom of the damper ( 40 ). Recess ( 14 ) is open at the bottom and closed at the top ( 115 ). Recess ( 114 ) is adapted to engage the sliding means ( 30 ) as more fully explained below.
Referring now to FIG. 4 , the second rectangular frame ( 26 ) comprises a first ( 48 ) and a second ( 50 ) parallel long side rectangular members and a first ( 52 ) and a second ( 54 ) parallel short side rectangular members. These four members are joined together and define a rectangular bulkhead dimensioned to fit snuggly within the rectangular floor or wall hole while allowing easy removal of the motorized air vent from the hole. The rectangular damper ( 40 ) is permitted a sliding action within the rectangular bulkhead between a fully open position and a fully closed position along a series of bearing tabs ( 83 ) disposed on the inside surface of each parallel long side rectangular member. The rectangular damper ( 40 ) is motivated for sliding action by means ( 30 ). Also within each parallel long side rectangular members ( 48 ) and ( 52 ) are apertures ( 82 ) adapted to receive corner tabs ( 78 ) disposed on side ( 80 ) and opposite side ( 81 ) of mounting plate ( 60 ) of sliding means ( 30 ). Once assembled, the damper ( 40 ) will be disposed below the first mesh pattern ( 32 ) and slide along tabs ( 83 ). Recess ( 114 ) will engage the sliding means ( 30 ) as more fully explained blow. Sliding means will be supported from mounting board ( 60 ) which will be suspended from frame ( 26 ) by corner tabs ( 78 ) engaged with apertures ( 82 ).
Referring now to FIGS. 5 A and 5 B there are shown a top and a bottom perspective view of the sliding means ( 30 ) comprising a mounting plate ( 60 ) disposed beneath the rectangular damper ( 40 ) as shown in FIG. 4 and supportively attached width-wise to the second rectangular frame ( 26 ) by means of tabs ( 78 ) engaging apertures ( 82 ) in frame ( 26 ). Illustrated in FIGS. 5A and 5B are electric DC motor ( 62 ), a battery ( 64 ) in communication with the electric motor ( 62 ) and actuation means comprising a cam body ( 66 ) and a cam head ( 67 ). The cam head is in mechanical communication with rectangular damper ( 40 ) recess ( 114 ). As the cam head is turned by the motor clock-wise or counter clock-wise the damper slides from an open position to a closed position. Stop member ( 69 ) is inserted within the cam body ( 66 ) and acts to limit the movement of the cam body and cam head between a damper full open position and a damper full closed position. Mounting plate ( 60 ) comprises a top surface ( 70 ), a bottom surface ( 72 ) and a central aperture ( 74 ). As illustrated in FIG. 1 and FIG. 4 , the mounting plate ( 60 ) is mounted width-wise across the second rectangular frame by mounting means comprising projections ( 78 ) protruding from each short side ( 80 ) of the mounting plate engaging apertures ( 82 ) in the long sides ( 48 ) and ( 50 ) of the rectangular frame ( 26 ).
Referring back to FIG. 5 , battery ( 64 ) is mounted to the bottom surface ( 72 ) of the mounting plate ( 60 ) by battery mounting means. In FIG. 5 , the battery is a 9 volt battery and mounting means are clasps ( 86 ) and ( 88 ) adapted to engage the battery terminals ( 90 ) and ( 92 ). On the top surface ( 70 ) of the mounting plate ( 60 ) there is electrical contact means ( 96 ) in electrical communication with the electric motor ( 62 ). The top surface also mounts electric motor control means ( 98 ) which may take the form of a programmable circuit to actuate the motor on a programmable basis or a radio frequency receiver to actuate the motor on a remote-control basis from either a wall mounted control or a thermostat. The electric motor ( 62 ) includes a drive shaft ( 100 ) that protrudes through aperture ( 74 ) to connect with the cam body ( 66 ). The electric motor is disposed below the mounting plate and mounted thereto by screws ( 104 ) and ( 105 ) that protrude through apertures ( 108 ) and ( 109 ) to engage threaded holes ( 106 ) and ( 107 ) in the top surface ( 63 ) of the motor casing.
Referring now to FIGS. 6A to D there are shown a variety of views of the sliding means ( 30 ) in an assembled state. Illustrated are the cam body ( 66 ) and cam head ( 67 ) mounted to the drive shaft ( 100 ) and disposed above the mounting plate ( 60 ); the battery ( 64 ) and the DC electric motor ( 62 ), the electrical connection ( 96 ) and the control means ( 98 ).
Referring now to FIGS. 7A to F there are shown top, side and bottom views of the cam body ( 66 ) and cam head ( 67 ). The cam head is adapted for engagement with a complementary recess ( 114 ) (See FIG. 4 ) centrally disposed in the lower surface ( 109 ) of rectangular damper ( 40 ). The attachment collar ( 111 ) depends from the cam body ( 66 ) and includes a “D” shaped orifice ( 116 ) that fits over the “D” shaped drive shaft ( 100 ). In operation, the rotation of the cam head ( 67 ) within the complementary recess ( 114 ) moves the rectangular damper ( 40 ) between fully open and fully closed. The rotation control means (Item 69 FIG. 5 ) restricts the rotation of the drive shaft to about 180 degrees.
Although the description above contains much specificity, these should not be construed as limiting the scope of the invention but as merely providing illustrations of some of the presently preferred embodiments of this invention. Thus the scope of the invention should be determined by the appended claims and their legal equivalents.
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A motorized air register, air diffuser or vent for HVAC systems in commercial and residential applications comprises a supporting frame abutting a floor, wall or ceiling and a second depending frame for enclosing a damper. The damper is motor driven from a first fully open position to a second fully closed position. The damper can be controlled remotely from a wall consol or in accordance with thermostat logic.
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CROSS-REFERENCE TO RELATED APPLICATION
[0001] This application claims the benefit of the filing date of U.S. Provisional Application Ser. No. 61/159,287 filed Mar. 11, 2009 and entitled “On-Site—Custom Fitted Hearing Equalizer Optimized For Personal Hearing Needs and Preferences and for Insertion Loss Compensation”. The '287 application is hereby incorporated herein by reference.
FIELD
[0002] The invention pertains to modular rechargeable Audio Processing Apparatuses—Assistive Listening devices which can be coupled wirelessly to personal digital assistants, computers or the like for use, initial adjustment and configuration. More particularly, the invention pertains to such devices implementable as customizable, wireless headsets.
BACKGROUND
[0003] Current Headsets provide wired or wireless connectivity with cellular phones or music players via non custom or semicustom ear canal adaptors that result in poor retention and inconsistent sound level and frequency response. More people wear headsets for longer periods of time and they tend to leave them on even when they are not in use (communicating with external devices, cell-phones, etc). Very few of those devices may have a pass-thru mode, where sounds are passed from the microphone to the speaker/receiver of the headset.
[0004] When the physical fit is tight, the headset acts as an earplug, if the pass-thru mode is not available, reducing contact of the user with the environment in addition to being uncomfortable both because of the pressure applied on the ear canal walls as well as the fullness of the occluded canal.
[0005] When the fit is loose, the device is not acting as an earplug to the surrounding sounds but it is still uncomfortable since it needs to be continuously readjusted and repositioned. More importantly, because sound enters the ear directly, the signal enhancing processing algorithms such as noise reduction, or directionality are heavily compromised. When the device is used in a pass thru mode, where sound from the microphone is passed to the speaker/receiver of the unit, higher levels of amplification/equalization are not possible due to the loose physical fit (large volume of air) and the echo/feedback cancellation processing is compromised.
[0006] The current headsets over-amplify the low frequencies to compensate for the loose fit but cannot adjust the low frequencies to match the variability of the fit. Miniature extended frequency response receivers/speakers suitable for the small volumes of the enclosed ear canal depend on a good tight fit to deliver extended frequency response for a true pass-thru mode especially for non hearing impaired users.
[0007] There are Further yet, the current headset devices do not provide for a way for equalization (other than over all volume) nor for hearing compensation procedures and tools. The receivers/speakers used in current headsets are not suitable for users with hearing impairment because they have extended lower frequencies in addition to over amplifying them and causing masking to upper frequencies where the impairment is usually manifested.
BRIEF DESCRIPTION OF THE DRAWINGS
[0008] FIGS. 1A-1C are a sequence of images illustrating various aspects of two configurations of one embodiment—Normal Mode of operation s of the invention;
[0009] FIG. 2 is a block diagram of one embodiment—Normal Mode of operation of the invention;
[0010] FIG. 3 is a block diagram of a second embodiment—Fine Tuning mode of operation of the invention;
[0011] FIG. 4 is a block diagram of a third embodiment—Testing and Amplification Emulation Mode of the invention;
[0012] FIG. 5 is a block diagram of another embodiment—Repair Mode of the invention; and
[0013] FIGS. 6A-6C illustrate aspects of a method in coupling to the ear with an aspect of the invention;
[0014] FIG. 7A illustrate aspects of a method for electrical charging of the invention; and
[0015] FIG. 7B illustrates a configuration of the invention as shown in its FIG. 4 . Embodiment.
DETAILED DESCRIPTION
[0016] While embodiments of this invention can take many different forms, specific embodiments thereof are shown in the drawings and will be described herein in detail with the understanding that the present disclosure is to be considered as an exemplification of the principles of the invention, as well as the best mode of practicing same, and is not intended to limit the invention to the specific embodiment illustrated.
[0017] Embodiments of the invention can include, a custom fitted hearing device with good comfortable retention in the ear canal and sufficient attenuation which allow for the full utilization of the speech enhancing processing both while the device receives sounds from external devices or when it operates in a pass-thru/transparent mode.
[0018] Another aspect includes an instant, on the spot, process for creating a custom mold that can be easily administered by the user or with the help of a minimally trained helper in certain markets, as in the developing world.
[0019] A consistent, easy quick-to-administer detection of the equalization settings based on user needs. An interactive parameter adjustment procedure for fitting/programming the instrument. An optional wireless remote (PDA, cell phone or computer) that adds more flexibility in optimizing/customizing the device. These procedures can be self administered by the user or with the help of a minimally trained helper in certain markets.
[0020] A modular device, FIG. 1A (separate modules for electronics, battery, receiver, ear mold and such modules distributed over the ear, in front of the ear concha and in the ear canal with adjustable length interconnections) allows for easy on the spot adjustments, repair or servicing, and extends the use and the life of the product. A smart hearing aid detection and repair process implemented on the optional wireless remote (PDA, cell phone or computer). Modularity is very critical for the success of the device in underdeveloped markets.
[0021] A rechargeable battery and a charger that supports solar and user generated energy sources such as a hand cranked generator, as well as conventional power sources.
[0022] Other aspects of the invention can include:
A custom FIGS. 6A-6B or semi-custom FIG. 6C on the spot mold that allows for comfortable retention and provides sufficient attenuation from environmental sound distractions and allows the signal enhancing processing (noise reduction, directionality, equalization) to control the sound that gets into the ear either in communication or pass-thru mode of operation. Consistent and predictable equalization and amplification because of the consistent placement due to the custom ear mold. Reduced cognitive effort for the user by overcoming hearing difficulties (by equalization and signal enhancement) based on environmental or personal physical limitations. Transparent/pass-thru mode (sound comes from microphone on the unit) that takes into consideration the attenuation introduced by having a mold covering the ear canal. It wirelessly communicates and receives/transmits sounds to many devices such as cell phones or wireless adaptors for regular phones, mp3 players, TV audio wireless adaptors, computers etc. Takes into consideration the listening environment and adjusts accordingly as to increase sound clarity and reduce cognitive effort by the user (normal or impaired hearing) in difficult environments. Equalization of device is dependent on self hearing assessment (or with third party assistance) to correctly set the preferred equalization/amplification level. Hearing and preference assessment is accomplished through generating sounds via an algorithm that determines hearing/preference level of the individual wearing the device. The wearer indicates when the sound is heard via responding to a signal from the sound generating device which could be the hearing device or other hand held device (mobile phone, PDA, his own personal computer, etc). The hearing assessment program monitors the environmental sound level to determine if environment is suitable for assessment of the specific individual's hearing limitations. The hearing device is capable of picking up signals from the microphone (environmental sounds) or external signals through an internal antenna (such as signals generated by remote devices such cell phone, MP3 player, computer, PDA). The device can adjust it settings based on environment automatically or manually. The device allows for user adjustment of its equalization parameters with the help of appropriate cue sounds. The device automatically adjusts its default setting based on past adjustment history. The hearing device contains algorithms that are activated based on input signal characteristics. The hearing device can switch automatically between input signals. The hearing devices can be used on both ears with individual assessment of both ears. The hearing devices when worn binaurally can act independently of one another or in coordination with regard to input. A modular device that allows for onsite repair. Parts can be snapped to and from the device. The optional remote (PDA, Cell phone, computer) generates diagnostic tests for each module and calls for the replacement/needed repair.
[0041] In yet another aspect of the invention, an off-the-self, relatively inexpensive personal digital assistant, (PDA), and included fuzzy logic-type, expert system, software can be used by individuals with very limited training to accurately measure hearing, compensate for noisy ambient environments during testing and detect underlying medical conditions for follow-up. The same PDA could be used to carry out fitting, fine tuning, or on-site repair of the respective hearing device.
[0042] In yet another aspect of the invention, user's can adjust the device to suit their particular requirements from casually listening to downloaded music to improving their reception of locally generated audio. Adjustments can be made directly via local controls on the device or via a programmed PDA which the user could carry.
[0043] Rechargeable batteries can be provided. A hand cranked generator can be used for recharging where no utility supplied energy is available.
[0044] In a further aspect of the invention, a very low cost, custom ear mold can be provided using a standard, preformed inflatable balloon. A balloon, which might include inserts such as a sound tube, or removable shapes, for example for coupling to an associated electronics package, can be inserted into the ear of a user. The balloon can be filled with silicone which when cured will correspond to the user's ear canal. The cured silicone shape can then be removed from the user's ear and attached to the electronics package.
[0045] In a further aspect of the invention, very low cost, selection of semicustom ear molds can be provided allowing for accommodation of a wide range of ear sizes both in terms of ear canal circumference and length.
[0046] Another embodiment of the invention can be used to carry out testing of various types to evaluate hearing loss. This alternate embodiment can also be used with a local, programmed PDA. Separate microphones and audio output devices, receivers, can be provided for each ear.
[0047] FIG. 1A illustrates two configurations ( 10 and 11 ) of the Normal Mode of operation embodiment in accordance with the invention. An ear nodule 12 A or 12 D is coupled to a receiver module 12 C which is coupled to module electronics/wireless module 12 C. The electronics module can be either in front of the ear (configuration 10 ) or behind the ear (configuration 11 ). In configuration 10 the electronics module 12 B is connected via an “adjust length and lock” tube with the microphone module 14 A behind the ear. In the same configuration, a magnetic or mechanical “snap-on” battery module 14 B is connected with the microphone module 14 A. In configuration 11 the removable “snap on” battery module is connected directly to the electronics module 12 B. FIGS. 1B-1C illustrates configurations 10 and 11 coupled to the ear of a user.
[0048] FIG. 2 illustrates a block diagram of one implementation of the embodiment, in configurations 10 and 11 configured as a stand alone hearing device 20 which could be used with a wirelessly coupled cellular telephone 22 A, a wirelessly coupled MP3 music player 22 B, or a wirelessly coupled displaced microphone 22 C.
[0049] Device 20 can also include a rechargeable battery module 14 B, a user audio input microphone module 22 b which can be carried in unit 12 B, and a receiver module 12 c which can also be carried by unit 12 B, to provide audible output to the user's ear canal. Unit 12 B can include a short range wireless transceiver 12 a, for example, a BLUETOOTH brand transceiver, along with digital processing circuitry 12 b which can carry out speech processing, noise reduction, feedback cancellation and other functions to improve a user's hearing experience relative to local audio input, via microphone 14 A, or from any of the devices 22 A, B or C.
[0050] The battery module 14 B can be recharged by use of a manually operable battery charger 16 , for example, a hand crankable generator.
[0051] FIG. 3 illustrates a block diagram of another implementation which includes an embodiment, such as the embodiment 10 , wirelessly coupled to one of a personal digital assistant, a cellular-type telephone or a computer 30 . In the implementation of FIG. 3 , the unit 20 can be selectively adjusted, fine-tuned, hearing loss testing can be carried out, or amplification emulation can be implemented, via the unit 30 . The unit 30 can also include a short range wireless transceiver 30 a, compatible with the transceiver 12 a.
[0052] FIG. 4 illustrates a block diagram of a test/evaluation unit 40 usable to develop control parameters for use with the unit 10 , 11 or 20 . Unit 40 includes an electronics module 42 which can include one or more programmed processors as well as digital signal processing software 44 . Left and right audio input/output microphones 46 a, b, and telephone-type phone output audio devices 47 a, b coupled to unit 40 receive audio from, or provide audio to the person being evaluated. A local short range wireless transceiver 42 a, for example a BLUETOOTH brand device can be coupled to the electronics package and software 44 for communication to a wireless control unit 30 .
[0053] The unit 30 can be implemented as a programmed PDA, cellular-type phone or a computer with a compatible transceiver 30 a. Software implemented functions can include one or more of a Hearing-loss testing expert system, a fitting/adjusting programming expert system, an amplification emulation system, on-site repair system, as well as a local patient database, all without limitation.
[0054] FIG. 5 illustrates a block diagram of the unit 10 , 11 , 20 combined with the test/evaluation unit 40 to implement a repair mode. It will be understood that other functions can be provided using the combination of FIG. 5 , without limitation.
[0055] FIGS. 6A-6B illustrate an exemplary method of producing the ear mold 12 A. A balloon is provided as in FIG. 6A . The balloon, with any internal inserts, is inserted in the ear canal of the user, as in FIG. 6B . The balloon is filled with a fast curing silicone as in FIG. 6B . Once the silicone has cured, the mold can be removed from the user's ear and attached to a corresponding electronics package as in FIG. 1A .
[0056] FIG. 7A illustrates an exemplary method of coupling the rechargeable battery 14 B in configuration 10 to the charger unit 16 using “snap on” magnetic coupling.
[0057] FIG. 7B illustrates an exemplary method of adjusting the cable length of the Evaluation-Testing apparatus/Medallion, unit 40 .
[0058] From the foregoing, it will be observed that numerous variations and modifications may be effected without departing from the spirit and scope of the invention. It is to be understood that no limitation with respect to the specific apparatus illustrated herein is intended or should be inferred. It is, of course, intended to cover by the appended claims all such modifications as fall within the scope of the claims.
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A modular, cost effective customizable sound processing unit can provide enhanced audio from a displaced source to a user. The source can be wirelessly coupled to the unit via a short range transceiver. The processing unit can include circuitry and software to process incoming audio and to compensate for the loss of hearing due to the device been coupled to the user ear canal, making it acoustically transparent for sound sources picked by the on the unit microphone(s) and provide an enhanced audio experience for the user.
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Latin name of the genus and species claimed: Prunus salicina.
Variety denomination: ‘Suplumfortythree’.
BACKGROUND AND SUMMARY OF THE INVENTION
This invention relates to the discovery and asexual propagation of a new and distinct variety of plum, Prunus salicina cv. ‘Suplumfortythree’. The new variety was first hybridized in March 1997 by David W. Cain and selected in August 2000 by Terry Bacon as breeder number: ‘97P040-010-244’. The new variety was first evaluated by Terry Bacon near Wasco, Calif. in Kern County. The variety ‘Suplumfortytfour’ was originated by hybridization.
The new variety ‘Suplumfortythree’ is characterized by red flesh with black skin.
The seed parent is ‘93P-007’ (unpatented), and the pollen parent is ‘90P-055’ (unpatented). The parent varieties were first crossed in March of 1997, with the date of sowing being January 1998, and the date of first flowering being March 1999. The new plum variety ‘Suplumfortythree’ was first asexually propagated by Terry Bacon near Wasco, Kern County, Calif. in January 2002, by budding.
The new variety ‘Suplumfortythree’ is distinguished from its seed parent, ‘93P-007’ (unpatented), in that while both of the varieties ripen at a similar time, ‘93P-007’ has amber flesh compared to red flesh for the new variety.
The new variety ‘Suplumfortythree’ is distinguished from its pollen parent, ‘90P-055’ (unpatented), in that both varieties have red flesh but ‘90P-055’ ripe date is July 1 st while the new variety ripe date is August 1 st .
The new variety ‘Suplumfortythree’ has a similar ripening time as ‘Friar’ (unpatented), but has red flesh compared to amber flesh for ‘Friar.’
The new variety ‘Suplumfortythree’ has been shown to maintain its distinguishing characteristics through successive asexual propagations by, for example, budding.
BRIEF DESCRIPTION OF THE PHOTOGRAPH
The accompanying color photographic illustration shows typical specimens of the foliage and fruit of the present new plum variety ‘Suplumfortythree’. The illustration shows the upper and lower surface of the leaves, an exterior and sectional view of a fruit divided across its suture plane to show flesh color, pit cavity and the stone remaining in place. The photographic illustration was taken shortly after being picked and the colors are as nearly true as is reasonably possible in a color representation of this type.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
Throughout this specification, color names beginning with a small letter signify that the name of that color, as used in common speech is aptly descriptive. Color names beginning with a capital letter designate values based upon The R.H.S. Colour Chart published by The Royal Horticultural Society, London, England, 1986.
The descriptive matter which follows pertains to 13 year old ‘Suplumfortythree’ plants on ‘Nemaguard’ (unpatented) rootstock, grown in the vicinity of Wasco, Kern County, Calif., during 2010, and is believed to apply to plants of the variety grown under similar conditions of soil and climate elsewhere.
TREE
General: (Measurements taken on 13 year old tree unless otherwise noted.).
Size .—Medium. Normal for most plum varieties. Reaches a height of approximately 3-5 meters with normal pruning. Spread .—Approximately 3-5 meters. Vigor .—Moderately vigorous, about 1.5 to 2 meters in height the first growing season. Growth .—Semi-upright. Productivity .—Productive. Form .—Vase formed. Bearer .—Regular. Fertility .—Unknown, should be planted with another variety to ensure consistent production. Canopy density .—Medium. Hardiness .—Hardy in all fruit growing areas of California. Winter chilling requirement is approximately 600 hours at or below 7.2° C. Disease resistance/susceptibility .—Under close observation in Kern County, Calif., no particular plant/fruit disease resistance/susceptibility has been observed. Insect resistance/susceptibility .—Under close observation in Kern County, Calif., no particular plant/fruit insect resistance/susceptibility has been observed.
Trunk: (Measurements at approximately 30 cm above soil line on mature tree).
Diameter .—Approximately 18 cm, varies with soil type, fertility, climatic conditions and cultural practices. Texture .—Medium shaggy, increases with age of tree. Trunk color .—About Medium Grey-Brown 199B to Brown 200B; becomes darker with age.
Branches: (Measurements at approximately 90 cm above soil line.).
Size .—Diameter approximately 7 to 9 cm. Texture .—Smooth on first year wood and increasing roughness with tree age. Color .—Varying from about Medium Grey-Brown 199B to Brown 200B. Lenticels .—Present.
Lenticels:
Number .—Numerous. Density .—about 2/cm 2 but varies with tree vigor and climatic conditions. Color .—About Medium Grey-Brown 199B. Size .—Medium. Length.— 3 mm. Width.— 2 mm.
Flowering shoots: (Data taken in July at mid-point of season growth.).
Size .—Average diameter approximately 5 mm. Color .—Topside: About Medium Yellow-Green 152A. Underside: About Medium Yellow-Green 152A. Internode length .—Medium; approximately 2 cm. Midway on flowering shoot. Flowering shoot lenticels .—Medium amount. Color: About Medium Grey-Brown 199B. Diameter: Approximately 1.0 mm. Flowering shoot leaf buds .—Shape: Obovate. Width: Approximately 1.5 mm. Length: Approximately 2.1 mm. Color: About Dark Greyed-Orange 177A. Flowering shoot flower buds .—Shape: Elliptic. Width: Approximately 1 mm. Length: Approximately 1.8 mm. Color: About Dark Greyed-Orange 177A. Number of buds per node: Usually 2. Density of buds .—Medium. Flower bud distribution .—On spurs and one year old shoots. Ratio of wood ( leaf ) buds to flowering buds.— ½ on nodes. Anthocyanin intensity .—None or very slight.
FOLIAGE
Leaves: (Data taken in July on fully expanded leaves at mid-point of the season growth).
Size .—Medium. Average length .—Medium; approximately 100 mm. Average width .—Medium; approximately 55 mm. Thickness .—Medium. Color .—Upper surface: About Dark Green 131A. Lower surface: About Medium Green 137D. Form .—Broad obovate. Tip .—Cuspidate. Base .—Irregularly V-shaped. Margin .—Crenate. Venation .—Pinately net veined. Vein color .—About Medium Yellow-Green 146D. Surface texture .—Smooth. Leaf blade ( ratio of length to width ).—2:1. Shape in the cross section .—Flat. Angle at apex .—Small. Profile .—Flat. Leaf blade tip .—Slightly curved downwardly. Angle of tip .—Acute. Undulation of margin .—Slight.
Petiole:
Average length .—Medium; approximately 13 mm. Average diameter .—Approximately 1.5 mm. Color .—About Medium Yellow-Green 146D but can be darker with more light exposure.
Stipules:
Number/leaf bud .—Approximately 1 per leaf bud when present. Typical length .—Approximately 3 mm. Color .—About Medium Greyed-Orange 164B. Persistence .—Falls off.
Leaf glands:
Form .—Globose. Average number .—Usually 2. Position .—On petiole/leaf base transition area, alternate. Average size .—Small; approximately 0.5 mm. Color .—About Dark Grey-Brown 199B.
FLOWERS
General:
Flower blooming period .—First bloom: Approximately Feb. 24, 2010. Full bloom: Approximately Feb. 28, 2010. Location of first bloom .—Older wood. Location of full bloom .—Uniform throughout the canopy. Time of bloom .—Medium. Duration of bloom .—Medium; approximately 12 days. Diameter of fully opened flower .—Medium, approximately 10 mm. Flower aroma .—Very slight aroma. Shape .—Rosaceous.
Peduncle:
Length .—Medium; approximately 10 mm. Diameter .—Medium; approximately 1 mm. Color .—About Medium Yellow-Green 144B. Pubescence .—Absent.
Petals:
Number.— 5. Arrangement .—Overlapping slightly. Length .—Approximately 12 mm. Diameter .—Approximately 10 mm. Shape .—Obovate. Apex shape .—Rounded. Base shape .—Narrows at point of attachment. Color of inner and outer surface .—White. Surface texture .—Smooth. Margins .—Slightly undulating. Frequency of flowers with double petals .—None. Size .—Medium, about 10 mm wide. Claw length .—Medium. Margin waviness .—Medium. Base angle .—Narrow. Division of upper margin .—Entire. Pubescence of inner surface .—Absent. Pubescence of outer surface .—Absent.
Sepals:
Number.— 5. Length .—Approximately 3 mm. Diameter .—Approximately 2 mm. Shape .—Elliptic. Color .—About Medium Yellow-Green 144A. Surface texture .—Smooth. Margins .—Entire. Positioning .—Adpressed to petals. Pubescence of inner surface .—Absent. Pubescence of outer surface .—Absent. Frequency of flowers with double sepals .—None.
Stamens:
Number .—Ranges from about 20 to about 30, average 25. Average length .—About 7 mm. Filament color .—White. Anther color .—About Medium Greyed-Orange 167A after starting to dry. Flower pollen color .—About Light Greyed-Orange 163C when first opened. Position .—Perigynous.
Pistil:
Number .—Usually one. Average length .—Approximately 9 mm. Ovary diameter .—Approximately 0.5 mm. Pubescence .—None. Stigma extension in comparison to anthers .—Level or slightly above anthers. Style frequency of supplementary pistils .—Absent.
Flower buds:
Hardiness .—Hardy. Size .—Medium. Length .—Medium. Shape .—Pointed. Positioning .—Slightly free. Pubescence .—Absent. Color .—About Dark Greyed-Orange 177A.
Receptacle:
Depth .—Medium Pubescence of inner surface .—Absent. Pubescence of outer surface .—Absent.
FRUIT
General: (Description taken near Wasco, Kern County, Calif. on Aug. 1, 2010).
Date of first pick .—Approximately Jul. 28, 2010. Date of last pick .—Approximately Aug. 7, 2010. Maturity when described .—Firm. Season ripening .—Medium. Position of maximum diameter .—Towards the middle. Symmetry about the suture .—Symmetric.
Size:
Length ( stem end to apex ).—Approximately 55 mm. Diameter in line with suture plane .—Approximately 55 mm. Diameter perpendicular to suture plane .—Approximately 63 mm. Average weight .—Approximately 128 gm.
Form:
Viewed from apex .—Rounded, symmetrical. Viewed from side, facing suture .—Rounded, slightly flattened, symmetrical. Viewed from side, perpendicular to suture .—Rounded, slightly flattened, symmetrical.
Apex shape: Flattened.
Apex base: Rounded.
Fruit stem cavity:
Shape .—Flaring. Depth .—Medium; Approximately 8 mm. Breadth .—Approximately 8 mm. Width .—Narrow.
Fruit stem:
Length .—Medium; approximately 8 mm. Diameter .—Approximately 2 mm. Color .—About Medium Green 143C. Adherence to stone .—Medium.
Fruit skin:
Thickness .—Medium. Adherence to flesh .—Medium. Surface texture .—Medium. Pubescence .—None. Bloom .—Slight. Ground color .—Not visible. Overcolor .—About Black 202A covering 100% f the fruit skin Taste .—Mildly Tart. Reticulation .—Absent. Roughness .—Absent. Tenacity .—Tenacious to flesh. Tendency to crack .—Slight.
Flesh:
Ripens .—Evenly. Texture .—Fine-juicy. Fibers .—Medium. Flavor .—Sweet-tart. Brix .—Approximately 22°. Juice .—Abundant to moderate. Aroma .—Slight. Color .—Ranging from Medium Red 47C to Darker Red 46B. Anthocyanin color under skin .—Strongly expressed. Anthocyanin color of flesh .—Strongly expressed. Anthocyanin color around stone .—Strongly expressed. Amygdalin .—Wanting. Acidity .—Medium-high. Sugar content .—High. Eating quality .—Good. Stone/flesh ratio.— 1/30. Firmness .—Medium.
Pit cavity size:
Length .—Approximately 20 mm. Diameter perpendicular to suture plane .—Approximately 10 mm. Diameter in line with suture .—Approximately 20 mm.
Fruit use: Fresh market.
Fruit shipping and keeping quality: Medium.
Stone:
Stone freeness .—Semi-free. Degree of adherence to flesh .—Weak. Stone size .—Size: Small. Size compared to Fruit: Small. Length: Medium, approximately 20 mm. Diameter in line with suture plan: Approximately 20 mm. Diameter perpendicular to suture plane: Approximately 10 mm. Width of Stalk End: Medium. Angle of Stalk end: Acute angle. Hilum: Oval. Stone form .—Viewed from side: Nearly round to slightly obovate. Viewed from ventral end: Flattened, symmetrical. Viewed from Stem end: Flattened, symmetrical. Stone shape .—Base shape: Nearly straight. Apex shape: Rounded with small sharp point. Stone surface .—Somewhat smooth with sharp ridges running from base to apex. Stone halves .—Nearly symmetrical. Stone ridges .—Continuous. Stone outgrowing keel .—Well-developed. Stone tendency to split .—Almost none. Stone color .—About Light Greyed-Orange 164C when dried. Position of maximum .—Middle. Sides .—Nearly equal. Pits .—Angular. Fibers .—Parts from flesh smoothly. Ventrical edge .—Medium. Dorsal edge .—Narrow. Ground color .—Not visible. Extent of overcolor .—Very large. Pattern of overcolor .—None.
Suture:
Line .—Shallow.
Ventral surfaces:
Lips .—Nearly equal. Depression of apex .—Indistinct. Pistil base .—Not persisting. Pubescence at apex .—Absent.
Pistil point:
Shape .—Flattened.
|
A new and distinct plum tree variety, Prunus salicina , cv. ‘Suplumfortythree’ is characterized by red flesh, black skin, firm fruit, with a medium bloom and ripening in the middle of the season
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CO-PENDING APPLICATIONS
Various methods, systems and apparatus relating to the present invention are disclosed in the following co-pending applications filed by the applicant or assignee of the present invention May 23, 2000:
09/575,197
09/575,195
09/575,159
09/575,132
09/575,123
09/575,148
09/575,130
09/575,165
09/575,153
09/575,118
09/575,131
09/575,116
09/575,144
09/575,139
09/575,186
09/575,185
09/575,191
09/575,145
09/575,192
09/575,181
09/575,193
09/575,156
09/575,183
09/575,160
09/575,150
09/575,169
09/575,184
09/575,128
09/575,180
09/575,149
09/575,179
09/575,133
09/575,143
09/575,187
09/575,155
09/575,196
09/575,198
09/575,178
09/575,164
09/575,146
09/575,174
09/575,163
09/575,168
09/575,154
09/575,129
09/575,124
09/575,188
09/575,189
09/575,162
09/575,172
09/575,170
09/575,171
09/575,161
09/575,141
09/575,125
09/575,142
09/575,140
09/575,190
09/575,138
09/575,126
09/575,127
09/575,158
09/575,117
09/575,147
09/575,152
09/575,176
09/575,151
09/575,177
09/575,175
09/575,115
09/575,114
09/575,113
09/575,112
09/575,111
09/575,108
09/575,109
09/575,110
09/575,182
09/575,173
09/575,194
09/575,136
09/575,119
09/575,135
09/575,157
09/575,166
09/575,134
09/575,121
09/575,137
09/575,167
09/575,120
09/575,122
The disclosures of these co-pending applications are incorporated herein by cross-reference. Each application is identified by its United States Serial Number.
BACKGROUND OF THE INVENTION
The following invention relates to a laminated ink distribution structure for a printer.
More particularly, though not exclusively, the invention relates to a laminated ink distribution structure and assembly for an A4 pagewidth drop on demand printhead capable of printing up to 1600 dpi photographic quality at up to 160 pages per minute.
The overall design of a printer in which the structure/assembly can be utilized revolves around the use of replaceable printhead modules in an array approximately 8 inches (20 cm) long. An advantage of such a system is the ability to easily remove and replace any defective modules in a printhead array. This would eliminate having to scrap an entire printhead if only one chip is defective.
A printhead module in such a printer can be comprised of a “Memjet” chip, being a chip having mounted thereon a vast number of thermo-actuators in micro-mechanics and micro-electromechanical systems (MEMS). Such actuators might be those as disclosed in U.S. Pat. No. 6,044,646 to the present applicant, however, there might be other MEMS print chips.
The printhead, being the environment within which the laminated ink distribution housing of the present invention is to be situated, might typically have six ink chambers and be capable of printing four color process (CMYK) as well as infra-red ink and fixative. An air pump would supply filtered air to the printhead, which could be used to keep foreign particles away from its ink nozzles. The printhead
It is another object of the present invention to provide an ink distribution structure suitable for the pagewidth printhead assembly as broadly described herein.
It is another object of the present invention to provide a laminated ink distribution assembly for a printhead assembly on which there is mounted a plurality of print chips, each comprising a plurality of MEMS printing devices.
It is yet another object of the present invention to provide a method of distributing ink to print chips in a printhead assembly of a printer.
SUMMARY OF THE INVENTION
The present invention provides an ink distribution assembly for a printhead to which there is mounted an array of print chips, the assembly serving to distribute different inks from respective ink sources to each said print chip for printing on a sheet, the assembly comprising:
a longitudinal distribution housing having a duct for each said different ink extending longitudinally therealong,
a cover having an ink inlet port corresponding to each said duct for connection to each said ink source and for delivering said ink from each said ink source to a respective one of said ink ducts, and
a laminated ink distribution structure fixed to said distribution housing and distributing ink from said ducts to said print chips.
Preferably the laminated ink distribution structure includes multiple layers situated one upon another with at least one of said layers having a plurality of ink holes therethrough, each ink hole conveying ink from one of said ducts enroute to one of said print chips.
Preferably one or more of said layers includes ink slots therethrough, the slots conveying ink from one or more of said ink holes in an adjacent layer enroute to one of said print chips.
Preferably, the slots are located with ink holes spaced laterally to either side thereof.
Preferably the layers of the laminated structure sequenced from the distribution housing to the array of print chips include fewer and fewer said ink holes.
Preferably one or more of said layers includes recesses in the underside thereof communicating with said holes and transferring ink therefrom transversely between the layers enroute to one of said slots.
Preferably the channels extend from the holes toward an inner portion of the laminated structure over the array of print chips, which inner portion includes said slots.
Preferably each layer of the laminated is a micro-molded plastics layer.
Preferably, the layers are adhered to one another.
Preferably, the slots are parallel with one another.
Preferably, at least two adjacent ones of said layers have an array of aligned air holes therethrough.
The present invention also provides a laminated ink distribution structure for a printhead, the structure comprising:
a number of layers adhered to one another, each layer including a plurality of ink holes formed therethrough, each ink hole having communicating therewith a recess formed in one side of the layer and allowing passage of ink to a transversely located position upon the layer, which transversely located position aligns with a slot formed through an adjacent layer.
Preferably the slot in any layer of the structure is aligned with another slot in an adjacent layer of the structure and the aligned slots are aligned with a respective print chip slot formed in a final layer of the structure.
Preferably the layers are micro-molded plastics layers.
The present invention also provides a method of distributing ink to an array of print chips in a printhead assembly, the method serving to distribute different inks from respective ink sources to each said print chip for printing on a sheet, the method comprising:
supplying individual sources of ink to a longitudinal distribution molding having a duct for each said different ink extending longitudinally therealong,
causing ink to pass along the individual ducts for distribution thereby into a laminated ink distribution structure fixed to the distribution housing, wherein
the laminated ink distribution structure enables the passage therethrough of the individual ink supplies to the print chips, which print chips selectively eject the ink onto a sheet.
The present invention also provides a method of distributing ink to print chips in a printhead assembly of a printer, the method utilizing a laminated ink distributing structure formed as a number of micro-molded layers adhered to one another with each layer including a plurality of ink holes formed therethrough, each ink hole communicating with a channel formed in one side of a said layer and allowing passage of ink to a transversely located position within the structure, which transversely located position aligns with an aperture formed through an adjacent layer of the laminated structure, an adjacent layer or layers of the laminated structure also including slots through which ink passes to the print chips.
As used herein, the term “ink” is intended to mean any fluid which flows through the printhead to be delivered to a sheet. The fluid may be one of many different coloured inks, infra-red ink, a fixative or the like.
BRIEF DESCRIPTION OF THE DRAWINGS
A preferred fo of the present invention will now be described by way of example with reference to the accompanying drawings wherein:
FIG. 1 is a front perspective view of a print engine assembly
FIG. 2 is a rear perspective view of the print engine assembly of FIG. 1
FIG. 3 is an exploded perspective view of the print engine assembly of FIG. 1 .
FIG. 4 is a schematic front perspective view of a printhead assembly.
FIG. 5 is a rear schematic perspective view of the printhead assembly of FIG. 4 .
FIG. 6 is an exploded perspective illustration of the printhead assembly.
FIG. 7 is a cross sectional end elevational view of the printhead assembly of FIGS. 4 to 6 with the section taken through the centre of the printhead.
FIG. 8 is a schematic cross-sectional end elevational view of the printhead assembly of FIGS. 4 to 6 taken near the left end of FIG. 4 .
FIG. 9A is a schematic end elevational view of mounting of the print chip and nozzle guard in the terminated stack structure of the printhead
FIG. 9B is an enlarged end elevational cross section of FIG. 9A
FIG. 10 is an exploded perspective illustration of a printhead cover assembly.
FIG. 11 is a schematic perspective illustration of an ink distribution molding.
FIG. 12 is an exploded perspective illustration showing the layers forming part of a laminated ink distribution structure according to the present invention.
FIG. 13 is a stepped sectional view from above of the structure depicted in FIGS. 9A and 9B,
FIG. 14 is a stepped sectional view from below of the structure depicted in FIG. 13 .
FIG. 15 is a schematic perspective illustration of a first laminate layer.
FIG. 16 is a schematic perspective illustration of a second laminate layer.
FIG. 17 is a schematic perspective illustration of a third laminate layer.
FIG. 18 is a schematic perspective illustration of a fourth laminate layer.
FIG. 19 is a schematic perspective illustration of a fifth laminate layer.
FIG. 20 is a perspective view of the air valve molding
FIG. 21 is a rear perspective view of the right hand end of the platen
FIG. 22 is a rear perspective view of the left hand end of the platen
FIG. 23 is an exploded view of the platen
FIG. 24 is a transverse cross-sectional view of the platen
FIG. 25 is a front perspective view of the optical paper sensor arrangement
FIG. 26 is a schematic perspective illustration of a printhead assembly and ink lines attached to an ink reservoir cassette.
FIG. 27 is a partly exploded view of FIG. 26 .
DETAILED DESCRIPTION OF THE INVENTION
In FIGS. 1 to 3 of the accompanying drawings there is schematically depicted the core components of a print engine assembly, showing the general environment in which the laminated ink distribution structure of the present invention can be located. The print engine assembly includes a chassis 10 fabricated from pressed steel, aluminium, plastics or other rigid material. Chassis 10 is intended to be mounted within the body of a printer and serves to mount a printhead assembly 11 , a paper feed mechanism and other related components within the external plastics casing of a printer.
In general terms, the chassis 10 supports the printhead assembly 11 such that ink is ejected therefrom and onto a sheet of paper or other print medium being transported below the printhead then through exit slot 19 by the feed mechanism. The paper feed mechanism includes a feed roller 12 , feed idler rollers 13 , a platen generally designated as 14 , exit rollers 15 and a pin wheel assembly 16 , all driven by a stepper motor 17 . These paper feed components are mounted between a pair of bearing moldings 18 , which are in turn mounted to the chassis 10 at each respective end thereof.
A printhead assembly 11 is mounted to the chassis 10 by means of respective printhead spacers 20 mounted to the chassis 10 . The spacer moldings 20 increase the printhead assembly length to 220 mm allowing clearance on either side of 210 mm wide paper.
The printhead construction is shown generally in FIGS. 4 to 8 .
The printhead assembly 11 includes a printed circuit board (PCB) 21 having mounted thereon various electronic components including a 64 MB DRAM 22 , a PEC chip 23 , a QA chip connector 24 , a microcontroller 25 , and a dual motor driver chip 26 . The printhead is typically 203 mm long and has ten print chips 27 (FIG. 13 ), each typically 21 mm long. These print chips 27 are each disposed at a slight angle to the longitudinal axis of the printhead (see FIG. 12 ), with a slight overlap between each print chip which enables continuous transmission of ink over the entire length of the array. Each print chip 27 is electronically connected to an end of one of the tape automated bond (TAB) films 28 , the other end of which is maintained in electrical contact with the undersurface of the printed circuit board 21 by means of a TAB film backing pad 29 .
The preferred print chip construction is as described in U.S. Pat. No. 6,044,646 by the present applicant. Each such print chip 27 is approximately 21 mm long, less than 1 mm wide and about 0.3 mm high, and has on its lower surface thousands of MEMS inkjet nozzles 30 , shown schematically in FIGS. 9A and 9B, arranged generally in six lines—one for each ink type to be applied. Each line of nozzles may follow a staggered pattern to allow closer dot spacing. Six corresponding lines of ink passages 31 extend through from the rear of the print chip to transport ink to the rear of each nozzle. To protect the delicate nozzles on the surface of the print print chip which enables continuous transmission of ink over the entire length of the array. Each print chip 27 is electronically connected to an end of one of the tape automated bond (TAB) films 28 , the other end of which is maintained in electrical contact with the undersurface of the printed circuit board 21 by means of a TAB film backing pad 29 .
The preferred print chip construction is as described in U.S. Pat. No. 6,044,646 by the present applicant. Each such print chip 27 is approximately 21 mm long, less than 1 mm wide and about 0.3 mm high, and has on its lower surface thousands of MEMS inkjet nozzles 30 , shown schematically in FIGS. 9A and 9B, arranged generally in six lines—one for each ink type to be applied. Each line of nozzles may follow a staggered pattern to allow closer dot spacing. Six corresponding lines of ink passages 31 extend through from the rear of the print chip to transport ink to the rear of each nozzle. To protect the delicate nozzles on the surface of the print chip each print chip has a nozzle guard 43 , best seen in FIG. 9A, with microapertures 44 aligned with the nozzles 30 , so that the ink drops ejected at high speed from the nozzles pass through these microapertures to be deposited on the paper passing over the platen 14 .
Ink is delivered to the print chips via a distribution molding 35 and laminated stack 36 arrangement forming part of the printhead 11 . Ink from an ink cassette 93 (FIGS. 26 and 27) is relayed via individual ink hoses 94 to individual ink inlet ports 34 integrally molded with a plastics duct cover 39 which forms a lid over the plastics distribution molding 35 . The distribution molding 35 includes six individual longitudinal ink ducts 40 and an air duct 41 which extend throughout the length of the array. Ink is transferred from the inlet ports 34 to respective ink ducts 40 via individual cross-flow ink channels 42 , as best seen with reference to FIG. 7 . It should be noted in this regard that although there are six ducts depicted, a different number of ducts might be provided. Six ducts are suitable for a printer capable of printing four color process (CMYK) as well as infra-red ink and fixative.
Air is delivered to the air duct 41 via an air inlet port 61 , to supply air to each print chip 27 , as described later with reference to FIGS. 6 to 8 , 20 and 21 .
Situated within a longitudinally extending stack recess 45 formed in the underside of distribution molding 35 are a number of laminated layers forming a laminated ink distribution stack 36 . The layers of the laminate are typically formed of micro-molded plastics material. The TAB film 28 extends from the undersurface of the printhead PCB 21 , around the rear of the distribution molding 35 to be received within a respective TAB film recess 46 (FIG. 19 ), a number of which are situated along a chip housing layer of the laminated stack 36 . The TAB film relays electrical signals from the printed circuit board 21 to individual print chips 27 supported by the laminated structure.
The distribution molding, laminated stack 36 and associated components are best described with reference to FIGS. 7 to 19 .
FIG. 10 depicts the distribution molding cover 39 formed as a plastics molding and including a number of positioning spigots 48 which serve to locate the upper printhead cover 49 thereon.
As shown in FIG. 7, an ink transfer port 50 connects one of the ink ducts 40 (the fourth duct from the left) down to one of six lower ink ducts or transitional ducts 51 in the underside of the distribution molding. All of the ink ducts 40 have corresponding transfer ports 50 communicating with respective ones of the transitional ducts 51 . The transitional ducts 51 are parallel with each other but angled acutely with respect to the ink ducts 40 so as to line up with the rows of ink holes of the first layer 52 of the laminated stack 36 to be described below.
The first layer 52 incorporates twenty four individual ink holes 53 for each of ten print chips 27 . That is, where ten such print chips are provided, the first layer 52 includes two hundred and forty ink holes 53 . The first layer 52 also includes a row of air holes 54 alongside one longitudinal edge thereof.
The individual groups of twenty four ink holes 53 are formed generally in a rectangular array with aligned rows of ink holes. Each row of four ink holes is aligned with a transitional duct 51 and is parallel to a respective print chip.
The undersurface of the first layer 52 includes underside recesses 55 . Each recess 55 communicates with one of the ink holes of the two centre-most rows of four holes 53 (considered in the direction transversely across the layer 52 ). That is, holes 53 a (FIG. 13) deliver ink to the right hand recess 55 a shown in FIG. 14, whereas the holes 53 b deliver ink to the left most underside recesses 55 b shown in FIG. 14 .
The third layer 60 also includes an array of air holes 54 aligned with the corresponding air hole arrays 54 provided in the first and second layers 52 and 56 .
The third layer 60 has only eight remaining ink holes 53 corresponding with each print chip. These outermost holes 53 are aligned with the outermost holes 53 provided in the first and second laminate layers. As shown in FIGS. 9A and 9B, the third layer 60 includes in its underside surface a transversely extending channel 61 corresponding to each hole 53 . These channels 61 deliver ink from the corresponding hole 53 to a position just outside the alignment of slots 59 therethrough.
As best seen in FIGS. 9A and 9B, the top three layers of the laminated stack 36 thus serve to direct the ink (shown by broken hatched lines in FIG. 9B) from the more widely spaced ink ducts 40 of the distribution molding to slots aligned with the ink passages 31 through the upper surface of each print chip 27 .
As shown in FIG. 13, which is a view from above the laminated stack, the slots 57 and 59 can in fact be comprised of discrete co-linear spaced slot segments.
The fourth layer 62 of the laminated stack 36 includes an array of ten chip-slots 65 each receiving the upper portion of a respective print chip 27 .
The fifth and final layer 64 also includes an array of chip-slots 65 which receive the chip and nozzle guard assembly 43 .
The TAB film 28 is sandwiched between the fourth and fifth layers 62 and 64 , one or both of which can be provided with recesses to accommodate the thickness of the TAB film.
The laminated stack is formed as a precision micro-molding, injection molded in an Acetal type material. It accommodates the array of print chips 27 with the TAB film already attached and mates with the cover molding 39 described earlier.
Rib details in the underside of the micro-molding provides support for the TAB film when they are bonded together. The TAB film forms the underside wall of the printhead module, as there is sufficient structural integrity between the pitch of the ribs to support a flexible film. The edges of the TAB film seal on the underside wall of the cover molding 39 . The chip is bonded onto one hundred micron wide ribs that run the length of the micro-molding, providing a final ink feed to the print nozzles.
The design of the micro-molding allow for a physical overlap of the print chips when they are butted in a line. Because the printhead chips now form a continuous strip with a generous tolerance, they can be adjusted digitally to produce a near perfect print pattern rather than relying on very close toleranced moldings and exotic materials to perform the same function. The pitch of the modules is typically 20.33 mm.
The individual layers of the laminated stack as well as the cover molding 39 and distribution molding can be glued or otherwise bonded together to provide a sealed unit. The ink paths can be sealed by a bonded transparent plastic film serving to indicate when inks are in the ink paths, so they can be fully capped off when the upper part of the adhesive film is folded over. Ink charging is then complete.
The four upper layers 52 , 56 , 60 , 62 of the laminated stack 36 have aligned air holes 54 which communicate with air passages 63 formed as channels formed in the bottom surface of the fourth layer 62 , as shown in FIGS. 9 b and 13 . These passages provide pressurised air to the space between the print chip surface and the nozzle guard 43 whilst the printer is in operation. Air from this pressurised zone passes through the micro-apertures 44 in the nozzle guard, thus preventing the build-up of any dust or unwanted contaminants at those apertures. This supply of pressurised air can be turned off to prevent ink drying on the nozzle surfaces during periods of non-use of the printer, control of this air supply being by means of the air valve assembly shown in FIGS. 6 to 8 , 20 and 21 .
With reference to FIGS. 6 to 8 , within the air duct 41 of the printhead there is located an air valve molding 66 formed as a channel with a series of apertures 67 in its base. The spacing of these apertures corresponds to air passages 68 formed in the base of the air duct 41 (see FIG. 6 ), the air valve molding being movable longitudinally within the air duct so that the apertures 67 can be brought into alignment with passages 68 to allow supply the pressurized air through the laminated stack to the cavity between the print chip and the nozzle guard, or moved out of alignment to close off the air supply. Compression springs 69 maintain a sealing inter-engagement of the bottom of the air valve molding 66 with the base of the air duct 41 to prevent leakage when the valve is closed.
The air valve molding 66 has a cam follower 70 extending from one end thereof, which engages an air valve cam surface 71 on an end cap 74 of the platen 14 so as to selectively move the air valve molding longitudinally within the air duct 41 according to the rotational positional of the multi-function platen 14 , which may be rotated between printing, capping and blotting positions depending on the operational status of the printer, as will be described below in more detail with reference to FIGS. 21 to 24 . When the platen 14 is in its rotational position for printing, the cam holds the air valve in its open position to supply air to the print chip surface, whereas when the platen is rotated to the non-printing position in which it caps off the micro-apertures of the nozzle guard, the cam moves the air valve molding to the valve closed position.
With reference to FIGS. 21 to 24 , the platen member 14 extends parallel to the printhead, supported by a rotary shaft 73 mounted in bearing molding 18 and rotatable by means of gear 79 (see FIG. 3 ). The shaft is provided with a right hand end cap 74 and left hand end cap 75 at respective ends, having cams 76 , 77 .
The platen member 14 has a platen surface 78 , a capping portion 80 and an exposed blotting portion 81 extending along its length, each separated by 120°. During printing, the platen member is rotated so that the platen surface 78 is positioned opposite the printhead so that the platen surface acts as a support for that portion of the paper being printed at the time. When the printer is not in use, the platen member is rotated so that the capping portion 80 contacts the bottom of the printhead, sealing in a locus surrounding the microapertures 44 . This, in combination with the closure of the air valve by means of the air valve arrangement when the platen 14 is in its capping position, maintains a closed atmosphere at the print nozzle surface. This serves to reduce evaporation of the ink solvent (usually water) and thus reduce drying of ink on the print nozzles while the printer is not in use.
The third function of the rotary platen member is as an ink blotter to receive ink from priming of the print nozzles at printer start up or maintenance operations of the printer. During this printer mode, the platen member 14 is rotated so that the exposed blotting portion 81 is located in the ink ejection path opposite the nozzle guard 43 . The exposed blotting portion 81 is an exposed part of a body of blotting material 82 inside the platen member 14 , so that the ink received on the exposed portion 81 is drawn into the body of the platen member.
Further details of the platen member construction may be seen from FIGS. 23 and 24. The platen member consists generally of an extruded or molded hollow platen body 83 which forms the platen surface 78 and receives the shaped body of blotting material 82 of which a part projects through a longitudinal slot in the platen body to form the exposed blotting surface 81 . A flat portion 84 of the platen body 83 serves as a base for attachment of the capping member 80 , which consists of a capper housing 85 , a capper seal member 86 and a foam member 87 for contacting the nozzle guard 43 .
With reference again to FIG. 1, each bearing molding 18 rides on a pair of vertical rails 101 . That is, the capping assembly is mounted to four vertical rails 101 enabling the assembly to move vertically. A spring 102 under either end of the capping assembly biases the assembly into a raised position, maintaining cams 76 , 77 in contact with the spacer projections 100 .
The printhead 11 is capped when not is use by the full-width capping member 80 using the elastomeric (or similar) seal 86 . In order to rotate the platen assembly 14 , the main roller drive motor is reversed. This brings a reversing gear into contact with the gear 79 on the end of the platen assembly and rotates it into one of its three functional positions, each separated by 120°.
The cams 76 , 77 on the platen end caps 74 , 75 co-operate with projections 100 on the respective printhead spacers 20 to control the spacing between the platen member and the printhead depending on the rotary position of the platen member. In this manner, the platen is moved away from the printhead during the transition between platen positions to provide sufficient clearance from the printhead and moved back to the appropriate distances for its respective paper support, capping and blotting functions.
In addition, the cam arrangement for the rotary platen provides a mechanism for fine adjustment of the distance between the platen surface and the printer nozzles by slight rotation of the platen 14 . This allows compensation of the nozzle-platen distance in response to the thickness of the paper or other material being printed, as detected by the optical paper thickness sensor arrangement illustrated in FIG. 25 .
The optical paper sensor includes an optical sensor 88 mounted on the lower surface of the PCB 21 and a sensor flag arrangement mounted on the arms 89 protruding from the distribution molding. The flag arrangement comprises a sensor flag member 90 mounted on a shaft 91 which is biased by torsion spring 92 . As paper enters the feed rollers, the lowermost portion of the flag member contacts the paper and rotates against the bias of the spring 92 by an amount dependent on the paper thickness. The optical sensor detects this movement of the flag member and the PCB responds to the detected paper thickness by causing compensatory rotation of the platen 14 to optimize the distance between the paper surface and the nozzles.
FIGS. 26 and 27 show attachment of the illustrated printhead assembly to a replaceable ink cassette 93 . Six different inks are supplied to the printhead through hoses 94 leading from an array of female ink valves 95 located inside the printer body. The replaceable cassette 93 containing a six compartment ink bladder and corresponding male valve array is inserted into the printer and mated to the valves 95 . The cassette also contains an air inlet 96 and air filter (not shown), and mates to the air intake connector 97 situated beside the ink valves, leading to the air pump 98 supplying filtered air to the printhead. A QA chip is included in the cassette. The QA chip meets with a contact 99 located between the ink valves 95 and air intake connector 96 in the printer as the cassette is inserted to provide communication to the QA chip connector 24 on the PCB.
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A laminated ink distribution structure for a printhead has a number of layers adhered to one another with each layer including a number of ink holes formed therethrough. Each ink hole has communicating therewith a channel formed in one side of the layer and allowing passage of ink to a transversely located position upon the layer, the transversely located position aligning with a slot formed through an adjacent layer of the laminate. The laminated ink distribution structure is fixed to a distribution housing via which different inks are conveyed from an ink cassette. The laminated structure distributes the different inks to an array of print chips of a color printer.
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This application is a divisional of application Ser. No. 11/867,228 filed Oct. 4, 2007, the contents of which are herein incorporated by reference in its entirety.
TECHNICAL FIELD
The invention relates to microelectronic semiconductor chips, manufacturing equipment, and manufacturing processes. More particularly, the invention relates to wirebonding methods and apparatus for the manufacture of IC (integrated circuit) packages.
BACKGROUND OF THE INVENTION
Wirebonding is a widely used technique for electrically connecting contacts within a semiconductor package. Commonly, a precious metal wire, normally gold within the range of approximately 0.0010 and 0.0015 inches in diameter, has one end ball-bonded to a bond pad on an IC, and another end stitch (or wedge) bonded to a lead on a leadframe. In order to accomplish this, the wire is fed through a capillary associated with a moveable bond head. For a ball bond, a ball is formed on the exposed end of the wire using an electronic flame off (EFO) mechanism. The ball is pulled against the end of the capillary and is then pressed into position on a pre-heated bond pad where a combination of heat, pressure, and ultrasonic vibration is used to cause the ball to adhere to the surface of the bond pad. With the ball end of the wire secured to the bond pad, the gold wire is payed out through the capillary as the bond head moves into position at the appropriate lead. A stitch bond is formed on the lead, and a tail wire is payed out through the capillary, clamped, and severed. A new ball is then formed readying the wire end for the next ball bond, and the cycle is repeated.
Bond head machinery typically includes a fixed ultrasonic horn, which includes the capillary and is equipped for movement along the z-axis. Various peripheral mechanical and electronic systems support the implementation of the general wirebonding procedure described. Associated wire handling machinery typically includes a spool, tensioner, clamp, ball detector, and gas-powered venturi for feeding wire to the capillary. Movement in the x- and y-axes is implemented primarily by moving the bond head assembly in order to position the horn over the bond target.
In efforts to overcome various problems in the arts, dual bond head systems and techniques are sometimes used. In some applications, for example, two separate bond heads are oriented for making bonds perpendicular to one another. In such a dual bond head configuration, each bond head independently performs wirebonding with a capillary on a horn in a fixed orientation. Supposing, for instance, that a 20-pin IC required fourteen bonds oriented in one direction and six oriented in a direction perpendicular relative to the others. Using a dual head bonder known in the arts, each head may perform the first six of its bond wire installations simultaneously. One bond head would then be idled, while the other completed the remaining, in this case eight, bond wires. Such workload imbalances are relatively common among dual head bonding systems and methods using apparatus known in the arts. Thus, inefficiency is a problem with the dual bond head approach current in the art.
A significant portion of IC package manufacturing costs is due to the expense of precious metals, thus there are ongoing efforts to reduce the precious metal content of IC packages. Many IC package applications may be characterized as having at least two clearly separable groups of bond wires that, in theory, may employ significantly different wire gauges and still maintain reliable function. For example, a buffer function is readily separable into supply and output stages with high current demands, while input stages operate at current demands that are very small in comparison. Despite the opportunity for precious metal reduction by using smaller wire gauges on the input side, predominant applications commonly deploy the same wire size throughout an assembly, using the wire gauge demanded by the worst-case current path. Previous attempts to reduce gold content by use of dual head tandem arrangements have found little acceptance because such arrangements tend to reduce overall throughput due to the workload imbalance between the heads.
Due to these and other technological problems, improved apparatus and methods for wirebonding with more than one wire source would be useful and advantageous contributions to the art. The present invention is directed to overcoming, or at least reducing, problems present in the prior art, and also contributes one or more heretofore unforeseen advantages indicated herein.
SUMMARY OF THE INVENTION
In carrying out the principles of the present invention, in accordance with preferred embodiments thereof, the invention provides apparatus and methods useful for forming bond wires using two or more separate wires with a single bond head. The separate wires may be identical, or may differ in size and/or composition.
According to one aspect of the invention, a preferred method for wirebonding in an IC package includes steps for bringing a first capillary of a dual capillary bond head to bear on bond targets, dispensing a wire from the first capillary, and attaching bond wires to selected bond targets. In further steps, a second capillary of the dual capillary bond head is brought to bear on bond targets and a second wire is dispensed from the second capillary and is attached to selected bond targets to form bond wires.
According to another aspect of the invention, a method for IC wirebonding includes providing a bond head having two capillaries adapted for dispensing wire for bonding to bond targets on an IC assembly. Each of the capillaries is operable in a bonding mode and an idle mode. In further steps, one of the capillaries is operated in a bonding mode and the other capillary is contemporaneously maintained in an idle mode.
According to another aspect of the invention, in an example of a preferred embodiment, dual capillary bond head apparatus includes a horizontally moveable bond head assembly positioned on a bonding table. An ultrasonic horn extends over the bonding table with a pair of capillaries for selectably dispensing separate strands of wire and for forming bond wires on bond targets.
According to yet another aspect of the invention, a dual capillary bond head assembly in a preferred embodiment includes a horizontally moveable bond head assembly positioned on a bonding table with an ultrasonic horn extending over the bonding table as described above. A pair of capillaries offset at an acute angle to one another are provided on an ultrasonic horn adapted for rotating either of the capillaries into position for wirebonding on a bond target.
According to still another aspect of the invention, a method for dual capillary IC wirebonding includes steps for using two dual capillary bond heads for contemporaneously attaching bond wires to selected bond targets on one or more IC package assemblies.
According to another aspect of the invention, an IC assembly manufactured using apparatus and methods of the invention includes both insulated and un-insulated bond wires.
The invention has advantages including but not limited to one or more of the following: improved wirebonding methods and apparatus; improved wire deployment equipment and techniques, particularly in applications where it is desirable to use two or more wires having different characteristics; improved wirebonding process throughput; precious metal conservation; and decreased costs. These and other features, advantages, and benefits of the present invention can be understood by one of ordinary skill in the arts upon careful consideration of the detailed description of representative embodiments of the invention in connection with the accompanying drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
The present invention will be more clearly understood from consideration of the following detailed description and drawings in which:
FIG. 1 is a schematic diagram illustrating examples of preferred embodiments of methods and apparatus implementing dual capillary wirebonding according to the invention;
FIG. 2 is a partial cutaway side view of an example of apparatus in an implementation of a preferred embodiment of the invention;
FIGS. 3A and 3B are cutaway side views of a portion of the apparatus shown in FIG. 2 in an example of a preferred embodiment of the invention;
FIGS. 4A and 4B are cutaway side views of another portion of the apparatus shown in FIG. 2 in an example of a preferred embodiment of the invention;
FIG. 5 is a cutaway side view of another portion of exemplary apparatus implementing the invention as shown in the embodiment of FIG. 2 ;
FIGS. 6A through 6C provide simplified top views depicting an example of the implementation of a preferred embodiment of the invention; and
FIG. 7 is a combined simplified top view and process flow diagram depicting an example of the implementation of a preferred embodiment of the invention.
References in the detailed description correspond to like references in the various drawings unless otherwise noted. Descriptive and directional terms used in the written description such as first, second, top, bottom, upper, side, etc., refer to the drawings themselves as laid out on the paper and not to physical limitations of the invention unless specifically noted. The drawings are not to scale, and some features of embodiments shown and discussed are simplified or amplified for illustrating the principles, features, and advantages of the invention.
DESCRIPTION OF PREFERRED EMBODIMENTS
The invention provides novel and useful methods and apparatus for IC wirebonding whereby two separate wires may be dispensed and installed using a single bond head. Alternative embodiments of the invention may be implemented, either using identical wires, or wires of various compositions. Methods and apparatus of the invention may also be combined in order to provide multiple bond head wirebonding with advantageous gains in productivity and cost savings.
First referring primarily to FIG. 1 , an overview of an example of the operation of preferred embodiments of the invention is shown in a schematic diagram. The operation of the invention is shown with reference to a first capillary 102 and second capillary 104 . As indicated in their two respective loops in FIG. 1 , either of the first or second capillaries 102 , 104 , may be active while the other is idle, as indicated by the alternative states 106 , 108 , respectively, of the capillary selection loop 110 . As shown in each of the active loops 102 , 104 , of the diagram, a wire 120 is held in position (a) with a ball 122 formed at its end by exposure to a ball-forming mechanism, such as an electronic flame-off (EFO) electrode 124 . The ball 122 is bonded (b) to a first bond target surface, e.g., a bond pad 126 on an IC. With the ball bond 128 secure, the capillary 102 , 104 is moved (c) in order to form (d) a bond wire spanning between the ball bond 128 and a second bond target, e.g., a lead 130 on a package leadframe. A stitch bond 132 is formed (e) at the second bond target 130 , the wire 120 is payed out (f) through the capillary, 102 , 104 , clamped and pulled (g). The pulling (g) severs the wire 120 between the stitch bond 132 and the capillary 102 , 104 , and the tail of wire protruding (h) from the capillary 102 , 104 , is then presented to the EFO electrode 124 for the formation of a new ball 122 (i) at the end of the wire 120 so that the cycle 100 may be repeated. The individual steps, (a) through (i), may be generally familiar to those skilled in the arts, however, the details and advantages inherent in the capability of executing the steps using two capillaries performing in concert, as indicated by the two intersecting process loops 102 , 104 joined by capillary selection loop 110 , bears additional description and illustration.
Now referring primarily to FIG. 2 , a partial cutaway simplified side view of an example of a bond head assembly 200 according to the invention is shown. A bond head assembly housing 202 , preferably moveable in the x-y axis, resides on a bonding table 204 . The bonding table 204 also preferably supports a workpiece such as a partially assembled IC package 206 having an IC 208 affixed to a leadframe 210 . The IC 208 and leadframe 210 each have bond targets, such as bond pads and leads. An ultrasonic horn 212 extends from the housing 202 , accompanied by a boom 214 . A mechanism is provided for raising and lowering the horn 212 , preferably a galvo arm 216 and pivot 218 , although suitable alternatives may also be used. The horn 212 has two capillaries 102 , 104 , for positioning above the bond targets of the workpiece 206 . Suitable duplicate bond system components such as wire clamps 220 , venturi 222 , wire spools (not shown), and possibly other associated components are preferably provided in order to accommodate independent feed control of each of the wires (e.g., FIG. 1 , 120 ). FIG. 2 depicts an example of the general placement of these peripheral components provided to support the operations of each of the independent capillaries 102 , 104 . It should be appreciated that capillaries of various materials, dimensions, and configurations may be used in various combinations depending upon the requirements of the application at hand. For example, in some instances it may be desirable to use identical capillaries, while in other instances it may be preferable to use a combination of standard, fine pitch, ultra-fine pitch, bottlenose, ceramic, ruby, and or alumina capillaries having different hole diameters, tip diameters, chamfer diameters, and so forth. Capillary selection may be made based on factors such as bond pad pitch, wire diameter, space available, and durability. The selectability of the capillaries during wirebonding operations, preferably by rotation of the ultrasonic horn as further described, provides advantages heretofore unavailable in the art.
FIGS. 3A-3B , and 4 A- 4 B, show additional details of aspects of the horn 212 in this example of a preferred embodiment of the invention. A rotating mechanism 300 is provided for rotating the ultrasonic horn 212 in order to bring the capillaries 102 , 104 into alignment with the workpiece 206 as desired. Rotating mechanisms such as stepper motors or other mechanical, electromechanical, pneumatic, or other means for rotating the horn 212 to align the capillaries 102 , 104 may be used. In the example depicted in FIGS. 3A and 3B , horn 212 rotation is accomplished using a stator winding 302 with four poles 304 that may be used to apply torque to a permanent magnet 306 , rotating the horn 212 into a desired position. The stator windings 304 and switch 308 arrangements are configured such that only one pair of opposing poles are energized at a time, and the active pair produces a north pole at one side and a south pole at the other. Such a configuration causes the permanent magnet 306 to align itself with the electromagnetic field, and so causes the horn 212 to rotate the capillaries into the desired positions. Positioning of the electromagnet poles 304 is such that each pair may rotate its respective capillary 102 , 104 into a bonding position, preferably providing ultrasonic horn 212 rotation for two possible stationary alignments. The range of rotation is sufficient to position the capillaries 102 , 104 , to avoid interference with one another during bonding, while avoiding excessive rotation to prevent excessive wire deformation. The axes of the capillaries 102 , 104 form an acute angle to one another, preferably about 45 degrees. In operation, rotation of the ultrasonic horn 212 serves to move one capillary into an active bonding position, e.g., FIG. 4A , 102 , while the other 104 simultaneously rotates to an idle position. The rotation preferably is performed with the horn 212 in an ‘up’ state, lifted by suitable mechanisms.
An example of a preferred capillary configuration is shown in FIGS. 4A and 4B . In this example, the first capillary 102 and second capillary 104 are oriented at an acute angle, preferably about 45 degrees apart from one another. Rotation of the ultrasonic horn 212 causes one or the other of the capillaries 102 , 104 to align with a bond target. The rotatable ultrasonic horn 212 of the invention is also capable of being locked into position during use of either of the capillaries 102 , 104 for bond formation. It should be recognized by those reasonably skilled in the arts that various rotating and locking mechanisms may be used within the scope of the invention. For example, as shown in the bearing lock mechanism 500 of FIG. 5 , solenoids 502 , or hydraulically-driven arrestor pins, or an electromagnet mechanism, may be used to firmly hold the horn 212 at a desired position during wirebonding. The ultrasonic horn 212 is preferably fitted into a dual-race 504 , 506 , bearing 508 . This bearing 508 is fitted into the bond head assembly housing 202 , so that the horn 212 is laterally fixed, but is free to rotate about its axis upon the inner race 504 . The axes of the capillaries preferably form an acute angle to one another, as shown in FIGS. 4A and 4B . In operation, rotation of the ultrasonic horn 212 serves to move one capillary into an active bonding position, while moving the other capillary into an idle position. Once the active capillary is selected and the initial horn 212 alignment is made, the bearing lock mechanism 500 is preferably engaged in preparation for wirebonding. The bearing 508 preferably includes a symmetrical array of holes about the central circumference of both the inner and outer races 504 , 506 in order to accept arrestor pins 510 for locking the inner and outer bearing races 504 , 506 together, firmly immobilizing horn 212 rotation when engaged. As shown, each arrestor pin 510 is preferably an extended solenoid 502 plunger, with sufficient travel for full engagement of the inner race 504 . At each pinning location, the arrestor pins 510 preferably pass through the bearing 508 into an inner race seat 512 . Each solenoid plunger 510 is loaded against a light spring 514 , so that in a deactivated state, each spring 514 decompresses and retracts the arrestor pins 510 fully from the inner race 504 , allowing free horn 212 rotation. Preferably, each arrestor pin 510 is tapered so that constraints of initial horn 212 orientation are less critical, and upon activation of the rotation mechanism, e.g., FIGS. 3A-3B , 300 , precise capillary alignment occurs. Once the solenoids 502 energize, overcoming the spring 514 force and engaging the arrestor pins 510 , the current source to stator the windings 304 is deactivated, thus the stator 302 has no influence on ultrasonic horn 212 performance during wirebonding. The bearing lock 500 solenoids 502 remain activated throughout a bonding cycle, and ball-and-stitch operations then continue with the selected capillary in a manner similar to that used with conventional wire bond machinery.
It should be appreciated that the capability of switching capillaries during a wirebonding cycle can be used to provide notable advances in workload efficiency. The disclosed rotatable ultrasonic horn enables installation of dual capillaries oriented as desired in a single horn. Of course, the dual capillary arrangement of the invention has flexibility inherent in its design. It may be used for single-wire bonding, for example, as with a conventional bond head. In this mode of operation, the rotatable horn is locked in a single position and the second wire is held in an idle state. Considering that some wirebonding applications do not require the use of dual capillaries, this capability may be an important feature in some instances. Some noteworthy advantages in efficiency may nevertheless be achieved in such applications using the invention. For example, changing from one capillary to another provides a rapid means of replenishing the wire supply, or of changing wire sizes when switching production between packages requiring different gauge wires. Using the invention, throughput interruption occurs only during the selection of the active capillary, accompanied by a short x-y table move to align the bond target. Changing the active capillary requires only a ‘z-up’ operation, preferably accompanied by this sequence: unlock horn; rotate horn; lock horn; deactivate stator. In a single bond head operation, this selection cycle may occur twice as bonding progresses from one IC assembly to another, but in order to minimize interruption, one of the capillary changes may be made during the transport index cycle.
An aspect of the invention is the potential for conserving precious metals used in the wire bonds of an IC package. An example is shown in FIGS. 6A though 6 C, in which an IC assembly 600 has a sixteen-bit driver IC 602 affixed to a leadframe 604 , with forty eight pins 606 requiring wirebonding to the leads 608 of the leadframe 604 . The IC 602 includes twelve supply pins 610 , sixteen output pins 612 , and twenty input pins 614 . Using the invention, as shown in FIG. 6A , the twenty input pins 614 are preferably wirebonded using one capillary of a bond head, in this case using gold bond wire 616 of approximately 0.6 mils in diameter in order to provide the capability of carrying up to approximately 18 mA of current. As shown in FIG. 6B , the output 612 and supply pins 610 , in this example requiring 180 mA capacity, are preferably wirebonded with 1.3 mil diameter gold bond wires 618 using the other capillary of the bond head. The resulting wirebonded IC assembly 620 , shown in FIG. 6C prepared for encapsulation into an IC package, thus realizes a nearly one-third reduction in gold bond wire content compared to methods for using one wire gauge. This is but one example representative of the advantageous precious metal conservation aspect of the invention. Of course, many other examples abound, but cannot all be shown. The invention may be used with numerous types of IC assemblies with particular advantages in assemblies in which it is desirable to use wires of different sizes or composition. To cite a few more examples, the advantages of the invention may also be exploited further by using wires of different compositions according to application requirements, such as, gold and copper, or various alloys (e.g., different levels of gold purity), or combinations of insulated and un-insulated wires. It should be understood that according preferred embodiments of the invention, an IC package assembly may be partitioned into two bond wire groups, such as a small bond wire group and a large bond wire group, or one alloy group and another, or insulated and un-insulated bond wires. The different wirebonds may be made without significantly slowing throughput compared to common single bond head techniques, and significant advantages may be realized in terms of reducing precious metal content. Further advantages may be realized in packages for which the IC dimensions are influenced by the minimum bond pad size. In some cases, using the invention to reduce bond wire sizes for some of the bond pads may enable the use of smaller bond pads spaced more closely. As a result, smaller ICs and smaller packages may in turn be realized by implementing the invention.
Revisiting the workload efficiency aspect of the invention, a conventional dual bond head approach for producing the IC assembly 620 of FIG. 6C would introduce a workload imbalance; the bond head installing the twenty smaller bond wires would run continuously while the bond head installing the larger bond wires would remain idle during the time that four of the small bond wires were being bonded. With the conventional approach, the greater the disparity in the number of each type of bond wire required, the greater the inefficiency. Using the invention as described in this single bond head example, regardless of the number of bond wires of each type, the nonproductive bond head time is limited to the minimal time required to rotate the horn in order to change the active capillary.
The invention provides further new and unique aspects of improved work flow in wirebonding processes, such as that denominated “interlaced” wirebonding herein. It has been determined during the course of developing the invention, that by using two rotatable ultrasonic horn bond head assemblies in a dual bond head configuration, additional advantages may be obtained. Now referring primarily to FIG. 7 , an example of dual capillary, dual bond head, interlaced wirebonding according to the invention is shown. The workflow 700 in a preferred embodiment of an interlaced bonding method is shown in terms of three time slots 702 , 704 , 706 for showing the progression of the process. The activities of two dual capillary bond heads 708 , 710 may be seen as follows. For the sake of this example, it is assumed that a particular type of IC-leadframe assembly is to be mass-produced using two different gauges of bond wire. Since each dual capillary bond head possesses the capability of installing both wire gauges, as further described herein, each dual capillary bond head is preferably used to perform alternating small wire and large wire bonds while indexing from one IC assembly to another, e.g., from IC assembly 712 , to IC assembly 714 . With the exception of initial start-up in the first time slot 702 , when one bond head, e.g. 710 in this example, is idle, both bond heads, 708 , 710 , perform identical bonding operations at any given time. As shown, beginning with the first time slot 702 , the first bond head 708 is brought to bear on the first IC assembly 712 . The first bond head 708 initially installs bond wires of a first gauge 716 , for example large output wires, on the first IC chip 718 , then a bond wire of a second gauge 720 , e.g., a reference pin bond with a single small wire, on the next IC 722 , and alternately repeating this sequence thereafter. Initially, as shown in the first time slot 702 , the second bond head 710 remains idle. In the second time slot 704 , the first bond head 708 alternately installs bond wires of two gauges 716 , 720 on a second IC assembly 714 , but in this example, in reverse order compared to the sequence it used in the first time slot 702 . Also during the second time slot 704 , the second bond head 710 preferably performs identical operations on the first IC assembly 712 , alternately bonding large wires 716 ′ and small wires 720 ′ at the bond targets bypassed by the first bond head 708 during the previous timeslot 702 . As shown in the third time slot 706 , the first IC assembly 712 has now been completed and may be ejected, as indicted by arrow 722 , for further manufacturing processes such as encapsulation, and the second IC assembly 714 takes its position for further bonding by the second bond head 710 . Meanwhile, a third IC assembly 724 is moved into a position accessible to the first bond head 708 . The first bond head 708 completes large wire 716 and small wire 720 bonds on the third IC assembly 724 . While the second bond head 710 completes the wire bonds 716 ′, 720 ′ on the second IC assembly 714 , but in an order opposite to the previous, i.e., second, time slot 704 sequence. It may be seen that the operations occurring in the second and third time slots 702 , 704 may be repeated cyclically numerous times until a desired number of IC assemblies are wirebonded. Thus, the interlaced wirebonding methods of the invention provide a remarkable and novel process flow with a workload very nearly evenly distributed between dual bond heads. It has been found that using adaptations of the disclosed apparatus and methods within the scope of the invention, interlaced wirebonding may be used to provide balanced throughput wirebonding workloads with any combination of differing wire sizes, wire compositions, and pin counts. It should be noted that the changes between capillaries of the dual capillary bond heads are preferably performed during the transport index, or x-y table move to an adjacent IC, making such changes transparent to throughput.
The methods and systems of the invention provide one or more advantages including but not limited to improved workload efficiency and precious metal conservation. While the invention has been described with reference to certain illustrative embodiments, those described herein are not intended to be construed in a limiting sense. For example, variations or combinations of steps or materials in the embodiments shown and described may be used in particular cases without departure from the invention. Various modifications and combinations of the illustrative embodiments as well as other advantages and embodiments of the invention will be apparent to persons skilled in the arts upon reference to the drawings, description, and claims.
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The invention discloses apparatus and methods for the formation of bond wires in integrated circuit assemblies by attaching two separate wires using a dual capillary bond head. The separate wires are preferably non-identical, for example, being of different gauges and/or material composition. According to a preferred embodiment of the invention, dual capillary bond head apparatus includes a rotatable ultrasonic horn with a pair of capillaries for selectably dispensing separate strands of bond wire and for forming bonds on bond targets. According to another aspect of the invention, a method is provided for dual capillary IC wirebonding including steps for using two dual capillary bond heads for contemporaneously attaching non-identical bond wires to selected bond targets on one or more IC package assemblies.
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This application claims the benefit of U.S. Provisional Application No. 60/265,033, filed on Jan. 30, 2001, which provisional application is incorporated by reference herein.
TECHNICAL FIELD
Our invention relates to the field of recumbent bicycles.
BACKGROUND OF THE INVENTION
An ever-increasing segment of the cycling public, particularly in the United States, rides and enjoys recumbent bicycles due to their comfort and performance. The basic configuration for a recumbent bicycle places the pedals ahead of, rather than below, the cyclist. This configuration allows the use of a more comfortable seat with seat back, which is typically placed lower to the ground than on ordinary bicycles. However, it also leads to problems that are distinctive to the field of recumbent bicycles.
One of the most important of these problems is shock absorption. As the recumbent cyclist is in a seated position with legs forward, he (or she) cannot absorb the extreme jolts and shocks associated with riding over rough surfaces or traversing potholes by utilizing his legs as shock absorbers. The bicycle and its frame must handle all shock absorption. This has led many manufacturers to utilize a bifurcated frame with a pivot placed in a structural member between the front wheel and the rear wheel. This pivot serves (in combination with a shock absorber of some type) to help absorb the shocks of the ride.
Unfortunately, the presence of a bifurcated frame has led to a problem for which no adequate solution has been found. This problem is formally referred to in the art as “pedaling induced suspension activation”, and more informally referred to as “pogoing”. It occurs when the cyclist pushes a pedal forward, putting stress on the upper part of the chain linkage between the pedal sprocket (which is ahead of the rider) or an intermediate mid-drive sprocket and the rear wheel sprocket. In effect, it causes this section of chain to temporarily shorten, which, in turn, causes the pivot to move upward and the bicycle frame to become temporarily shorter. As the pedals move into a more neutral position before the beginning of the next drive stroke by the rider's other foot, the pivot sags downward and the frame lengthens. This situation can rapidly develop into a steady, undesirable, up-and-down oscillation of the rider and frame—“pogoing”.
Another important problem involves provision of adequate means for seat positioning. Positioning of the seat vis-à-vis the pedals becomes a more critical issue on a recumbent bicycle. The recumbent cyclist does not have the option of standing to pedal and thereby minimizing the importance of seat positioning. Further, he cannot adjust his distance to the pedals by sliding slightly forward or backward on the seat, as is possible for the user of a standard bicycle. Finally, the leverage relied upon by the recumbent cyclist is gained by working against the seat back of the recumbent bicycle seat. It is, therefore, absolutely necessary that the recumbent bicycle seat be not only comfortable, but also precisely and minutely adjustable for the comfort and mechanical advantage of the user. At the same time, the seat must be able to maintain its position, once established, against the constant and repeated force exerted by the rider as he pushes back against the seat on each pedal stroke.
No adequate solution to this problem has been achieved to date in the art of recumbent bicycles. Some manufacturers utilize seats with anchoring members that fit into rigid track notches. Such seats do not slide, but they lack the minute adjustability sought by discerning riders. Other manufacturers have utilized seats that are freely adjustable by sliding on a seat track. The distance between such seats and the pedals of the recumbent bicycle can be adjusted with precision. However, such seats are generally maintained in position by a clamp attached to the track. This clamp is, in turn, tightened and held in position by tightening a screw threaded bolt or other member. Screw threaded elements of this type are difficult to tighten to the degree necessary to hold the bicycle seat in position. Most have shown an inevitable tendency to begin moving over a period of time under the stresses created by pedaling the recumbent bicycle. In addition, such clamps are not easily and freely adjustable, but require the use of tools to loosen, adjust, and re-tighten.
SUMMARY OF THE INVENTION
Our invention solves the problems outlined above; significantly improves recumbent bicycle performance, comfort, and ease of use; and involves or creates numerous other subsidiary improvements and inventions of significance in the field of recumbent bicycles. It is hinged on our finding that the problems described above are interrelated and can both be solved simultaneously by (i) the use of a cantilevered bicycle seat in conjunction with (ii) a coaxial bicycle pivot and mid-drive sprocket. The first solution also led to the creation of a bicycle seat that was stable, was easily adjustable without tools, and could be adjusted with the type of precision demanded by the field. The second solution, in turn, led to the creation of a recumbent bicycle that was foldable. This innovation is extremely desirable for the recumbent cyclist as it leads to a bicycle that can be folded to occupy a smaller space. This not only eases storage problems; it creates a recumbent bicycle that can be placed easily in an automobile trunk or other vehicle storage area for transport to settings where the user wishes to ride his bicycle. Thus, it also greatly increases bicycle portability. These and other innovations unique to our design will become apparent upon review of the accompanying drawings and the more detailed description that follows.
DESCRIPTION OF THE DRAWINGS
FIG. 1 provides a side view of a preferred embodiment of our recumbent bicycle.
FIG. 2 provides a view from above of the preferred embodiment illustrated in FIG. 1 with its seat and handlebars removed.
FIG. 3A provides a side view of the preferred embodiment with its seat and forward wheel removed.
FIG. 3B provides a side view of the preferred embodiment in the process of being folded with its handlebars reversed and its shock absorber detached.
FIG. 3C provides a side view of the preferred embodiment of our recumbent bicycle after folding.
FIG. 4 provides a partial cross-sectional view of the upper structural member of the preferred embodiment and further shows the rails provided thereon for the mounting of the base for the recumbent bicycle's seat.
FIG. 5 provides a partial cross-sectional view of the upper structural member of the preferred embodiment with the base mounting member of the recumbent bicycle's seat mounted thereon.
FIG. 6 provides a back view of the preferred embodiment of a seat for our recumbent bicycle, including its base mounting member.
FIG. 7 provides a side view of the preferred embodiment illustrating the means by which its seat is moved and adjusted horizontally.
FIG. 8 provides a side view of the seat in its opened and closed positions.
FIG. 9 provides a side view of an alternative preferred embodiment of a seat for our recumbent bicycle.
FIG. 10 provides a back view of the preferred embodiment of a seat for our recumbent bicycle, further incorporating reflectors and utility pockets.
DESCRIPTION OF THE INVENTION
The general features of the preferred embodiment are illustrated in FIG. 1 and FIG. 2 . Our recumbent bicycle is provided with an upper structural member 1 with pedal sprocket 2 at its forward extremity. Pedal sprocket 2 interfaces with a forward chain 3 linked to mid-drive sprockets (denoted generally by arrow 4 ). Mid-drive sprockets 4 are linked via rear chain 5 to rear wheel sprockets (denoted generally by arrow 6 ). These elements provide the essential drive train for our recumbent bicycle.
The distance between the pedal sprocket 2 and the rear wheel sprockets 6 is extended in recumbent bicycles. This has led some manufacturers to position mid-drive sprocket(s) intermediate pedal sprocket 2 and rear wheel sprockets 6 . However, our decision to make the mid-drive sprockets 4 and the pivot (denoted by arrow 7 ) coaxial is almost without precedent in this field. It has, either alone or in conjunction with the other design innovations described, below, led to other advantageous developments. First, it serves to completely eliminate the problem of pedaling induced suspension activation. Second, in conjunction with the other unique features described below, it allows the forward portion (indicated generally by bracket 8 ) and rear portion (indicated generally by bracket 9 ) of the recumbent bicycle we have developed to fold together for compactness around central pivot 7 .
The first advantage derived from the use of a concentric mid-drive/pivot system arises from the fact that the distance between the mid-drive sprockets 4 and the rear wheel sprockets 6 , as well as between the mid-drive sprockets 4 and the pedal sprocket 2 , is fixed. In the first case, this distance is maintained by the rigid structure of rear portion 9 and interconnected lower members 9 A thereof. In the second case, this distance is maintained by the rigid structure of forward portion 8 and interconnected connective members 8 A. In neither case can stress placed on the upper chain link connecting the sprockets in question serve to pull these sprockets closer together and thereby initiate pogoing.
The second advantage also relies on a concentric mid-drive/pivot system. Without such a system, any significant degree of folding (i.e.—movement around the pivot 7 beyond the small amount that is necessary for shock absorption) would create an unacceptable amount of slack in the lubricated drive chain(s) used. Such slack could become entangled in other parts; could cause the drive chain to slip from the sprockets; and would, in other respects, be a source of problems, inconvenience, and mess. Even with a concentric mid-drive/pivot system, however, further innovation is necessary to produce a folding recumbent bicycle. Our innovations in this area principally relate to the manner in which the lower support members of the front portion 8 and the rear portion 9 are constructed. The front portion 8 features lower connective members 8 A that are spread to the outside and linked to central pivot 7 outside of the link between lower members 9 A. Both of these features are necessary. The spread or splaying of lower connective members 8 A creates a substantial gap into which rear portion 9 can be folded. In addition, lower members 9 A must be linked inside of lower connective members 8 A in order to keep them from binding against these members as the front portion 8 and rear portion 9 are folded together.
These features allow the recumbent bicycle of our invention to be folded following, in general, the sequence illustrated in FIGS. 3A through 3C. In FIG. 3A, the bicycle seat 10 has been removed. (This can be easily and simply accomplished by loosening and removing lower bolt 15 .) The front wheel 16 has also been removed utilizing a standard quick release mechanism. In FIG. 3B, the handlebar 111 has been turned around (allowing it to be folded downward adjacent to upper structural member 1 , as illustrated in sequence in FIGS. 3 A through 3 C). Further, the quick release connecting shock absorber 17 to rear portion 9 has been utilized to disconnect these two elements, allowing rear portion 9 to be swung forward around pivot 7 . In FIG. 3C, the operation is complete, with rear portion 9 folded into forward portion 8 . Seat 10 can be folded via seat pivots 10 A. Thus, the folded recumbent bicycle along with its removed forward wheel 16 and removed and folded seat 10 can be placed together into a very small space for the convenience of the user, maker, or seller for storage, transportation, or shipping.
As shown most clearly in FIGS. 4, 5 , and 6 , the seat 10 of our recumbent bicycle is attached via base mounting member 11 . Base mounting member 11 is provided with a semi-deformable nylon upper lock block 12 . This is secured to base mounting member 11 via upper bolt 13 . It is also provided with a semi-deformable nylon lower lock block 14 , which is secured to base mounting member 11 by lower bolt 15 . As will be noted upon review of FIG. 1 and FIG. 7, lower lock block 14 is connected to base mounting member 11 ahead of upper lock block 12 . With the user positioned against seat back 10 B, his weight will be behind both upper lock block 12 and lower lock block 14 . This cantilevered arrangement turns upper lock block 12 into a weight-bearing fulcrum, pushing it down hard against upper rail 12 A. It likewise forces lower lock block 14 , which is at the end of the lever arm formed by base mounting member 11 , strongly upward against lower rail 14 A. This forms a strong frictional grip between the vertical facing surfaces of each lock block and its respective rail. (Likewise, since a pedal being pushed by the rider results in a force applied to seat back 10 B at a point above the level of the fulcrum formed, the push itself acts to torque seat 10 downward and further increase the frictional forces that prevent seat 10 from sliding.)
The cross-sectional tapered shape of the lock blocks and rails described also allows the formation of strong frictional grips between the horizontal facing surfaces of each lock block and its respective rail. Upper lock block 12 and lower lock block 14 are each formed with a “U”-shaped interior cross section with each arm of the “U” being approximately vertical and the horizontal facing surface of the “U” being approximately horizontal. Upper rail 12 A and lower rail 14 A both have a slightly tapered wedge shape with narrow ends terminating at a vertical facing surface. (These vertical facing surfaces have approximately the same width as the horizontal facing surfaces of the upper lock block 12 and lower lock block 14 .) When nylon upper lock block 12 and nylon lower lock block 14 are forced against upper rail 12 A and lower rail 14 A, these parts wedge together and the semi-rigid materials forming the arms of upper lock block 12 and lower lock block 14 are forced to deform outward slightly. This wedging as well as the inward bias of the arms of these “U”-shaped members help to establish a strong frictional grip between the horizontal facing surfaces of these lock blocks and the horizontal facing surfaces of their respective rails.
Lifting seat 10 disengages base mounting member 11 from upper rail 12 A and lower rail 14 A. This allows it to be freely moved and readjusted as illustrated in FIG. 7 . Moving from right to left in this drawing figure, the seat 10 may be seen as being lifted (and disengaged) from a forward position and then moved back and settled in a rear position. Alternatively, moving from left to right, this drawing figure serves to show the seat 10 being lifted (and disengaged) from a rear position and moved to a forward position prior to being dropped and re-engaged. From either, standpoint, the adjustable and versatile nature of the recumbent bicycle seat of our invention is manifest.
As previously noted, our seat 10 is foldable around seat pivots 10 A. This allows seat back 10 B to fold downward against seat base 10 C as illustrated in FIG. 8 . The ability of our seat 10 to be collapsed in this manner is important for storage purposes. However, it is also of particular importance when the recumbent bicycle is being transported via automobile roof-top mounting. When such mounting is used, the long axis of the bicycle is typically aligned with the long axis of the vehicle. In this position, an open seat back would create an obstruction that would raise air resistance and possibly tend to catch on low hanging branches or other obstacles. Our foldable seat 10 helps to avoid these problems. When upright, seat back 10 B may be supported in numerous ways. In the preferred embodiment, seat back 10 B is supported by cables 10 D attached to seat base 10 C. (Chains, webbing, or some equivalent means attached between seat back 10 B and seat base 10 could also be used for this same purpose.) In the alternative preferred embodiment illustrated in FIG. 9, two new sets of members interact to achieve this result: seat base extensions 10 E and seat back braces 10 F.
Finally, the seat back 10 B of our design is provided with biasing means that serve to bias it towards either a fully opened position or a closed (folded) position. Thus, when opened fully (as illustrated in FIG. 8 ), our seat back 10 B will tend to remain open unless the user exerts moderate force to bring it back across center line 12 . Likewise, it will tend to remain closed unless the user exerts moderate force to raise it up past center line 12 . The former quality is desirable while the recumbent bicycle is in use, while the latter quality becomes important when it is transported, particularly on an automobile roof top mount. In this situation, we have found that the biasing means provided serves to maintain seat 10 in a closed position even when facing into the onrush of air caused by the forward motion of the vehicle on which it is mounted. The tangible elements forming this biasing means are part of the basic structure of chair 10 . The somewhat elastic materials making up the cover (denoted generally by arrow 10 E) of chair 10 are anchored at the rear by straps 10 F to lower tube member 10 G. As the back 10 B is moved forward from its fully opened position, this material is stretched. It reaches its maximum extension when seat back 10 B is close to vertical and straps 10 F are aligned with seat pivots 10 A. The material moves into a less stretched configuration as it approaches a horizontal position. Thus, force must be exerted both to raise the seat up past the vertical center line 12 from a horizontal position and from its fully opened position.
The seat 10 of our recumbent bicycle is also provided with additional convenient features for the use of the rider as shown in FIG. 10 . These include integral pockets for several purposes. Thus, there is a hydration pack pocket 13 and a water bottle pocket 14 of appropriate dimension for these purposes as well as a utility pocket 15 of general usefulness. Finally, reflective strips 16 are provided for the safety of the rider. Numerous other changes and additions can be made without exceeding the scope of the inventive concept as set forth herein.
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A recumbent bicycle with (i) a cantilevered bicycle seat and (ii) a coaxial pivot and mid-drive sprocket around which the bicycle can be folded so as to form a more compact configuration. The folding of the bicycle is facilitated by the splaying of support arms for the coaxial pivot and mid-drive sprocket, which splaying allows the rear portion of the bicycle to be folded into a position lying between the splayed support arms.
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CROSS REFERENCES TO CO-PENDING APPLICATIONS
None.
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention is for a collapsible frame for a cloth or canvas-like top for a boat, and more particularly, pertains to a collapsible frame for a bimini sun top for a pontoon boat.
2. Description of the Prior Art
Prior art pontoon boat frames have been constructed of formed aluminum. Such prior art frames, while being relatively or somewhat secure, are still fairly unstable and, hence, are susceptible to vibrating, wiggling, swaying, and generally rocking with a harmonic motion on the pontoon boat when in the water or while trailering. These movements are objectionable.
The present invention overcomes the disadvantages of the prior art by providing a secure and sturdy framework for a bimini sun top for a pontoon boat.
SUMMARY OF THE INVENTION
The general purpose of the present invention is to provide a collapsible frame for a bimini sun top which secures to the railings of a pontoon boat and which can be opened and collapsed with ease.
According to one embodiment of the present invention, there is provided a collapsible frame for a sun top for a pontoon boat which includes extruded components which engage with square tubular extruded aluminum members. The combination of the extruded components and the supporting framework provides a stable and sturdy frame for support of a cloth, canvas or polymer-like cloth sun top structure.
One significant aspect and feature of the present invention is a collapsible frame structure which can be unfolded from a closed storage position to an open position for supporting a canvas, cloth or polymer top.
Another significant aspect and feature of the present invention is a frame structure which is sturdy and as a stable unit rides with the pontoon boat rather than wobbling with the motion of the pontoon boat.
A further significant aspect and feature of the present invention is a combination of a frame structure and extruded fittings which slidably and closely engage with close tolerance over square tubular extruded aluminum members, thereby providing inherent stability for the collapsible frame.
Having thus described significant aspects and features of the present invention, it is the principal object of the present invention to provide an improved sun top frame for a pontoon boat.
BRIEF DESCRIPTION OF THE DRAWINGS
Other objects of the present invention and many of the attendant advantages of the present invention will be readily appreciated as the same becomes better understood by reference to the following detailed description when considered in connection with the accompanying drawings, in which like reference numerals designate like parts throughout the figures thereof and wherein:
FIG. 1 is a perspective view of a frame in the unfolded raised position on a pontoon boat;
FIG. 2 is a starboard side view of a frame in the unfolded raised position on a pontoon boat;
FIG. 3 is an isometric view of an extruded long H-bracket;
FIG. 4 is an isometric view of an extruded short H-bracket;
FIG. 5 is an isometric view of an extruded transition bracket;
FIG. 6 is an isometric view of an extruded pivot bracket;
FIG. 7 is a view illustrating the manner in which the rear bow frame and the front bow frame members are secured to the railing framework via a long H-bracket;
FIG. 8 is a view illustrating the manner in which the bow member and the support member are secured to the front bow frame member;
FIG. 9 is a view illustrating the manner in which the support member is secured to the railing framework via a short H-bracket; and,
FIG. 10 is a cross sectional view of a pivot bracket along line 10--10 of FIG. 8.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
FIG. 1 is a perspective view of a frame 10 supporting a cover 12 and being secured to opposing railing frameworks 14 and 16 of a pontoon boat 18. The cover 12 may be cloth, canvas or polymer-like cloth material.
FIG. 2 is a starboard side view of the frame 10, where all numerals correspond to those elements previously described. Now, elements on the starboard side of the pontoon boat 18 will be described in detail, recognizing that there are identical opposing elements on the port side of the pontoon boat. A long H-bracket 20 of extruded aluminum with three sets of holes 22a, 22b, 24a, 24b, 26a and 26b, as illustrated in FIG. 3, is secured to the railing framework 14 with stainless steel machine screws or bolts through appropriate holes in the railing framework 14. The chemical reaction (electrolysis) between the aluminum H-bracket 20 and the stainless steel machine screws or bolts forms a chemical bond, thereby securing the machine screws or bolts to the long H-bracket 20. The long H-bracket 20 is described in greater detail with reference to FIG. 3.
A rear bow frame member 28 pivotally mounts to the long H-bracket 20, as illustrated in FIG. 7. The lower end of a transition bracket 30 secures over and about the lower region of the rear bow frame member 28. A front bow frame member 32 pivotally secures to the other end of the transition bracket 30.
With reference to FIGS. 8, 1 and 2, pivot brackets 34, 36, 38 and 40 align and fastly secure over and about the front bow frame member 32 and the rear bow frame member 28, respectively. A support member 42 pivotally secures on one end to pivot bracket 34; the opposing end of support member 42 pivotally secures to a short H-bracket 44 secured by stainless steel hardware to the railing framework 14. One end of bow member 46 pivotally secures to pivot bracket 36 and the other end to the corresponding framework on the port side. One end of an optional pivot bracket 48, similar to brackets 34, 36, 38 and 40, secures over and about the lower mid-region of the bow member 46 to pivotally support one end of an optional bow member 50.
A support member 52 pivotally secures on one end to pivot bracket 38; the opposing end of support member 52 pivotally secures to a short H-bracket 54 secured by stainless steel hardware to the railing framework 14. One end of a bow member 56 pivotally secures to pivot bracket 40 and the other end to the corresponding framework on the port side. One end of an optional pivot bracket 58, similar to brackets 34, 36, 38 and 40, secures over and about the lower mid-region of the bow member 56 to pivotally support one end of an optional bow member 60.
All framework members and the railing frameworks are of 11/4 square aluminum tubing which fit in close tolerance to the long and short H-brackets and the pivot brackets to provide for maximum coupled stability. All H-brackets and pivot brackets are of thick wall construction to eliminate flex and to promote stability.
FIG. 3 is an isometric view of the extruded long H-bracket 20, where all numerals correspond to those elements previously described. A horizontally aligned planar web member 66 intersects vertically aligned wall members 68 and 70 to form an upper channel 72 and a lower channel 74. A body hole 26a and a threaded hole 26b align through the upper portion of wall members 70 and 68, respectively, to accommodate a bolt for pivotal mounting of framework members in the upper channel 72. Body holes 22a and 24a, and threaded holes 22b and 24b, align through the lower portion of wall members 70 and 68, respectively, to accommodate bolts for mounting of the long H-bracket 20 to the railing framework 14. Short H-brackets, such as H-bracket 44, have the same cross sectional profile as the long H-bracket 20, but are shortened, as illustrated in FIG. 4 and include only one set of lower bolt mounting holes.
FIG. 4 is an isometric view of the short extruded H-bracket 44, where all numerals correspond to those elements previously described. The short extruded bracket 44 has a cross section similar to that of the long H-bracket 20, but is a shortened version thereof. A horizontally aligned planar web member 67 intersects vertically aligned wall members 69 and 71 to form an upper channel 73 and a lower channel 75. A body hole 77a and a threaded hole 77b align through the upper portion of wall members 71 and 69, respectively, to accommodate a stainless steel bolt or machine screw for pivotal mounting of framework members in the upper channel 73. Optionally, a removable pin can be inserted through holes 77a and 77b to provide for a quick disconnect of the support member 42 from the short H-bracket 44 when it is desired to collapse the majority of the frame 10 backwardly to an oblique position resting against rear bow frame member 28. The same mode of operation with short H-bracket 54 can be utilized if total collapsing of the frame 10 to the horizontal position is required, whereupon the entirely collapsed frame 10 positions along the rear portions of the railing frameworks 14 and 16. Body hole 79a and threaded hole 79b align through the lower portion of wall members 71 and 69, respectively, to accommodate a stainless steel mounting bolt or machine screw for mounting of the short H-bracket 44 to the railing framework 14.
FIG. 5 is an isometric view of a transition bracket, 30 where all numerals correspond to those elements previously described. The main body 76 includes a bore space 78. A square hole 80 aligns to one side of the main body 76 for accommodation of a framework member. Vertically oriented planar extensions 82 and 84 extend from the main body 76 to form a channel area 92 with one side of the main body 76. A threaded set-screw hole 86 extends through one side of the transition bracket leading to the square hole 80 for securement of a framework member in the square hole 80. A body hole 88 and a threaded hole 87 are included in the planar extensions 84 and 82, respectively, to pivotally secure a framework member to the channel area 92 of the transition bracket 30.
FIG. 6 is an isometric view of a pivot bracket 34, where all numerals correspond to those elements previously described. A square hole 94, similar in size to square hole 80 of the transition bracket 30, extends from the main body 98 and includes a threaded set screw hole 96. Square hole 94 accommodates a framework member which is secured therein by a set screw in the threaded set screw hole 96. Vertically oriented planar extensions 100 and 102 extend from the main body 98 to form a channel area 108 with one side of the main body 98. A body hole 106 and a threaded hole 104 are included in the planar extensions 102 and 100, respectively, to pivotally secure a framework member to the channel area 108 of the pivot bracket 34.
FIGS. 7, 8 and 9 illustrate the method of attachment of various style brackets and associated components to various framework members as typically incorporated in the invention.
FIG. 7 illustrates the mounting of the rear bow frame member 28 and the front bow frame member 32 to the railing framework 14, where all numerals correspond to those elements previously described. The lower channel 74 aligns over and about the railing framework 14. Bolts 110 and 112 engage holes 24a and 24b, and holes 22a and 22b, of the long H-bracket 20, as well as appropriate holes in the railing framework 14 to secure the long H-bracket 20 to the railing framework. Electrolysis forms a chemical bond between the threads of the bolts and the corresponding threaded screw holes 22b and 24b in the long H-bracket 20 to assist in thread-to-thread securement. In addition, body holes 22a and 24a can be closely fitted to the bolt diameters to effect a similar chemical bond. Bolt 114 engages holes 26a and 26b in a similar fashion and extends also through holes in the rear bow frame member 28 to pivotally secure the rear bow frame member 28 to the long H-bracket 20. The square hole 80 closely engages the lower portion of the rear bow frame member 28 and is secured therein by a set screw 116 in set screw hole 86. One end of the front bow frame member 32 is pivotally secured in the channel area 92 of the transition bracket 30 by stainless steel bolt 118 accommodated by holes 88 and 87 (of FIG. 5) and through appropriate holes at the end of the front bow frame member 32. Again, chemical bonding at the threaded junction occurs to assist in securement of the bolt 118 with the transition bracket 30.
FIG. 8 illustrates the securement of the bow member 46 and the support member 42 to the front bow frame member 32, where all numerals correspond to those elements previously described. Square hole 94 of pivot bracket 34 closely engages the front bow frame member 32 and is secured thereto by a stainless steel set screw 120 in set screw hole 96. A stainless steel bolt 122 is accommodated by holes 106 and 104 in the pivot bracket 34 and appropriate holes in the end of the support member 42 to pivotally secure the support member 42 in the channel area 108. Pivot bracket 36 aligns and secures in a similar fashion over and about the front bow frame member 32. Bow member 46 is pivotally secured to the pivot bracket 36 in the same manner as that just described.
FIG. 9 illustrates the mounting of support member 42 to railing framework 14 via a short H-bracket 44, where all numerals correspond to those elements previously described. A bolt 126 is accommodated by holes 79a and 79b in the walls of the lower channel 75 which fits over and about the railing framework 14, and appropriate holes in the railing framework 14 to secure the short H-bracket 44 to the railing framework 14. A bolt 128 is accommodated by holes 77a and 77b and holes in the end of the support member 42 to pivotally secure the support member 42 within the upper channel 73.
FIG. 10 is a cross sectional view of the short H-bracket 44 along line 10--10 of FIG. 8, where all numerals correspond to those elements previously described. Stainless steel set screw 120, having a cup point 121, is tightened in set screw hole 96 to secure the front bow frame member 32 within the square hole 94. Electrolysis forms a chemical bond between the threaded set screw hole 96 of the extruded aluminum pivot bracket 34 and threads of the stainless steel set screw 120. Stainless steel bolt 122 is illustrated in alignment in holes 106 and 104, as well as through holes 130 and 132 in the support member 42. Electrolysis forms a chemical bond between the threaded hole 104 of the extruded aluminum pivot bracket 34 and the threads 134 of the stainless steel bolt 122.
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A collapsible bimini sun top frame for a pontoon boat including square aluminum tubes and extruded aluminum fittings securing the frame to the railings of the pontoon boat. The frame supports a soft top of water resistant canvas or other material for protection from sun and rain in an open position, and is collapsible to a storage position. The soft top can be secured, such as with hook and loop fasteners, to the collapsible frame and, with appropriate fasteners, to the railings of the pontoon boat. The extruded fittings also can be utilized with other frames for other types of boats, such as speed boats, water skiing boats, or any other type of structure requiring a frame.
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CROSS-REFERENCE TO RELATED APPLICATIONS
This is a continuation-in-part application of application Ser. No. 11/438,764, entitled Single Phase Fluid Sampling Apparatus and Method for Use of Same, filed on May 23, 2006, which is a continuation-in-part application of application Ser. No. 11/268,311, entitled Single Phase Fluid Sampler Systems and Associated Methods, filed on Nov. 7, 2005 now U.S. Pat. No. 7,197,923.
TECHNICAL FIELD OF THE INVENTION
This invention relates, in general, to testing and evaluation of subterranean formation fluids and, in particular to, a single phase fluid sampling apparatus for obtaining multiple fluid samples and maintaining the samples near reservoir pressure via a common pressure source during retrieval from the wellbore and storage on the surface.
BACKGROUND OF THE INVENTION
Without limiting the scope of the present invention, its background is described with reference to testing hydrocarbon formations, as an example.
It is well known in the subterranean well drilling and completion art to perform tests on formations intersected by a wellbore. Such tests are typically performed in order to determine geological or other physical properties of the formation and fluids contained therein. For example, parameters such as permeability, porosity, fluid resistivity, temperature, pressure and bubble point may be determined. These and other characteristics of the formation and fluid contained therein may be determined by performing tests on the formation before the well is completed.
One type of testing procedure that is commonly performed is to obtain a fluid sample from the formation to, among other things, determine the composition of the formation fluids. In this procedure, it is important to obtain a sample of the formation fluid that is representative of the fluids as they exist in the formation. In a typical sampling procedure, a sample of the formation fluids may be obtained by lowering a sampling tool having a sampling chamber into the wellbore on a conveyance such as a wireline, slick line, coiled tubing, jointed tubing or the like. When the sampling tool reaches the desired depth, one or more ports are opened to allow collection of the formation fluids. The ports may be actuated in variety of ways such as by electrical, hydraulic or mechanical methods. Once the ports are opened, formation fluids travel through the ports and a sample of the formation fluids is collected within the sampling chamber of the sampling tool. After the sample has been collected, the sampling tool may be withdrawn from the wellbore so that the formation fluid sample may be analyzed.
It has been found, however, that as the fluid sample is retrieved to the surface, the temperature of the fluid sample decreases causing shrinkage of the fluid sample and a reduction in the pressure of the fluid sample. These changes can cause the fluid sample to approach or reach saturation pressure creating the possibility of asphaltene deposition and flashing of entrained gasses present in the fluid sample. Once such a process occurs, the resulting fluid sample is no longer representative of the fluids present in the formation. Therefore, a need has arisen for an apparatus and method for obtaining a fluid sample from a formation without degradation of the sample during retrieval of the sampling tool from the wellbore. A need has also arisen for such an apparatus and method that are capable of maintaining the integrity of the fluid sample during storage on the surface.
SUMMARY OF THE INVENTION
The present invention disclosed herein provides a single phase fluid sampling apparatus and a method for obtaining fluid samples from a formation without the occurrence of phase change degradation of the fluid samples during the collection of the fluid samples or retrieval of the sampling apparatus from the wellbore. In addition, the sampling apparatus and method of the present invention are capable of maintaining the integrity of the fluid samples during storage on the surface.
In one aspect, the present invention is directed to an apparatus for obtaining a plurality of fluid samples in a subterranean well that includes a carrier, a plurality of sampling chambers and a pressure source. In one embodiment, the pressure source is selectively in fluid communication with at least two sampling chambers thereby serving as a common pressure source to pressurize fluid samples obtained in the at least two sampling chambers. In another embodiment, the carrier has a longitudinally extending internal fluid passageway forming a smooth bore and a plurality of externally disposed chamber receiving slots. Each of the sampling chambers is positioned in one of the chamber receiving slots of the carrier. The pressure source is selectively in fluid communication with each of the sampling chambers such that the pressure source is operable to pressurize each of the sampling chambers after the fluid samples are obtained.
In another aspect, the present invention is directed to a method for obtaining a plurality of fluid samples in a subterranean well. The method includes the steps of positioning a fluid sampler in the well, obtaining a fluid sample in each of a plurality of sampling chambers of the fluid sampler and pressurizing each of the fluid samples using a pressure source of the fluid sampler that is in fluid communication with each of the sampling chambers.
In a further aspect, the present invention is directed to an apparatus for obtaining a fluid sample in a subterranean well. The apparatus includes a housing having a sample chamber defined therein. The sample chamber is selectively in fluid communication with the exterior of the housing and is operable to receive the fluid sample therefrom. A debris trap piston is slidably disposed within the housing. The debris trap piston includes a debris chamber and, responsive to the fluid sample entering the sample chamber, the debris trap piston receives a first portion of the fluid sample in the debris chamber then displaces relative to the housing to expand the sample chamber.
In one embodiment, the debris trap piston includes a passageway having a cross sectional area that is smaller than the cross sectional area of the debris chamber. In this embodiment, the first portion of the fluid sample passes from the sample chamber through the passageway to enter the debris chamber. Also in this embodiment, the first portion of the fluid sample is retained in the debris chamber due to pressure from the sample chamber applied to the debris chamber through the passageway. Alternatively or additionally, a check valve may be disposed in an inlet portion of the debris trap piston to retain the first portion of the fluid sample in the debris chamber.
In another embodiment, the debris trap piston may include a first piston section and a second piston section that is slidable relative to the first piston section such that the debris chamber is expandable responsive to the fluid sample entering the debris chamber. In this embodiment, as engagement device may be disposed between the first piston section and the second piston section to prevent additional movement of the first piston section relative to the second piston section after expanding the debris chamber to a preselected volume.
In an additional aspect, the present invention is directed to a method for obtaining a fluid sample in a subterranean well. The method includes the steps of disposing a sampling chamber within the subterranean well, actuating the sampling chamber such that a sample chamber within the sampling chamber is in fluid communication with the exterior of the sampling chamber, receiving a first portion of the fluid sample in a debris chamber of a debris trap piston slidably disposed within the sampling chamber, displacing the debris trap piston within the sampling chamber to expand the sample chamber and receiving the remainder of the fluid sample in the sample chamber.
The method may also include passing the first portion of the fluid sample through the sample chamber and through a passageway of the debris trap piston before entering the debris chamber and retaining the first portion of the fluid sample in the debris chamber by applying pressure from the sample chamber to the debris chamber through the passageway. Additionally or alternatively, a check valve disposed in an inlet portion of the debris trap piston may be used to retain the first portion of the fluid sample in the debris chamber.
In certain embodiments, the method may include expanding the debris chamber responsive to the fluid sample entering the debris chamber by sliding a first piston section relative to a second piston section and preventing additional movement of the first piston section relative to the second piston section after expanding the debris chamber to a preselected volume.
In yet another aspect, the present invention is directed to a downhole tool including a housing having a longitudinal passageway. A piston, including a piercing assembly, is disposed within the longitudinal passageway. A valving assembly is also disposed within the longitudinal passageway. The valving assembly includes a rupture disk that is initially operable to maintain a differential pressure thereacross. The valving assembly is actuated by longitudinally displacing the piston relative to the valving assembly such that at least a portion of the piercing assembly travels through the rupture disk, thereby allowing fluid flow therethrough.
In one embodiment, the piercing assembly includes a piercing assembly body and a needle that is held within the piercing assembly body by compression. In this embodiment, the needle has a sharp point that travels through the rupture disk. In addition, the needle may have a smooth outer surface, a fluted outer surface, a channeled outer surface or a knurled outer surface. In certain embodiments, the valving assembly may include a check valve that allows fluid flow in a first direction and prevents fluid flow in a second direction through the valving assembly once the valving assembly is actuated by the piercing assembly.
BRIEF DESCRIPTION OF THE DRAWINGS
For a more complete understanding of the present invention, including its features and advantages, reference is now made to the detailed description of the invention, taken in conjunction with the accompanying drawings in which like numerals identify like parts and in which:
FIG. 1 is a schematic illustration of a fluid sampler system embodying principles of the present invention;
FIGS. 2A-H are cross-sectional views of successive axial portions of one embodiment of a sampling section of a sampler embodying principles of the present invention;
FIGS. 3A-E are cross-sectional views of successive axial portions of actuator, carrier and pressure source sections of a sampler embodying principles of the present invention;
FIG. 4 is a cross-sectional view of the pressure source section of FIG. 3C taken along line 4 - 4 ;
FIG. 5 is a cross-sectional view of the actuator section of FIG. 3A taken along line 5 - 5 ;
FIG. 6 is a schematic view of an alternate actuating method for a sampler embodying principles of the present invention;
FIG. 7 is a schematic illustration of an alternate embodiment of a fluid sampler embodying principles of the present invention;
FIG. 8 is a cross-sectional view of the fluid sampler of FIG. 7 taken along line 8 - 8 ; and
FIGS. 9A-G are cross-sectional views of successive axial portions of another embodiment of a sampling section of a sampler embodying principles of the present invention.
DETAILED DESCRIPTION OF THE INVENTION
While the making and using of various embodiments of the present invention are discussed in detail below, it should be appreciated that the present invention provides many applicable inventive concepts which can be embodied in a wide variety of specific contexts. The specific embodiments discussed herein are merely illustrative of specific ways to make and use the invention, and do not delimit the scope of the invention.
Referring initially to FIG. 1 , therein is representatively illustrated a fluid sampler system 10 and associated methods which embody principles of the present invention. A tubular string 12 , such as a drill stem test string, is positioned in a wellbore 14 . An internal flow passage 16 extends longitudinally through tubular string 12 .
A fluid sampler 18 is interconnected in tubular string 12 . Also, preferably included in tubular string 12 are a circulating valve 20 , a tester valve 22 and a choke 24 . Circulating valve 20 , tester valve 22 and choke 24 may be of conventional design. It should be noted, however, by those skilled in the art that it is not necessary for tubular string 12 to include the specific combination or arrangement of equipment described herein. It is also not necessary for sampler 18 to be included in tubular string 12 since, for example, sampler 18 could instead be conveyed through flow passage 16 using a wireline, slickline, coiled tubing, downhole robot or the like. Although wellbore 14 is depicted as being cased and cemented, it could alternatively be uncased or open hole.
In a formation testing operation, tester valve 22 is used to selectively permit and prevent flow through passage 16 . Circulating valve 20 is used to selectively permit and prevent flow between passage 16 and an annulus 26 formed radially between tubular string 12 and wellbore 14 . Choke 24 is used to selectively restrict flow through tubular string 12 . Each of valves 20 , 22 and choke 24 may be operated by manipulating pressure in annulus 26 from the surface, or any of them could be operated by other methods if desired.
Choke 24 may be actuated to restrict flow through passage 16 to minimize wellbore storage effects due to the large volume in tubular string 12 above sampler 18 . When choke 24 restricts flow through passage 16 , a pressure differential is created in passage 16 , thereby maintaining pressure in passage 16 at sampler 18 and reducing the drawdown effect of opening tester valve 22 . In this manner, by restricting flow through choke 24 at the time a fluid sample is taken in sampler 18 , the fluid sample may be prevented from going below its bubble point, i.e., the pressure below which a gas phase begins to form in a fluid phase. Circulating valve 20 permits hydrocarbons in tubular string 12 to be circulated out prior to retrieving tubular string 12 . As described more fully below, circulating valve 20 also allows increased weight fluid to be circulated into wellbore 14 .
Even though FIG. 1 depicts a vertical well, it should be noted by one skilled in the art that the fluid sampler of the present invention is equally well-suited for use in deviated wells, inclined wells or horizontal wells. As such, the use of directional terms such as above, below, upper, lower, upward, downward and the like are used in relation to the illustrative embodiments as they are depicted in the figures, the upward direction being toward the top of the corresponding figure and the downward direction being toward the bottom of the corresponding figure.
Referring now to FIGS. 2A-2H and 3 A- 3 E, a fluid sampler including an exemplary fluid sampling chamber and an exemplary carrier having a pressure source coupled thereto for use in obtaining a plurality of fluid samples that embodies principles of the present invention is representatively illustrated and generally designated 100 . Fluid sampler 100 includes a plurality of the sampling chambers such sampling chamber 102 as depicted in FIG. 2 . Each of the sampling chambers 102 is coupled to a carrier 104 that also includes an actuator 106 and a pressure source 108 as depicted in FIG. 3 .
As described more fully below, a passage 110 in an upper portion of sampling chamber 102 (see FIG. 2A ) is placed in communication with a longitudinally extending internal fluid passageway 112 formed completely through fluid sampler 100 (see FIG. 3 ) when the fluid sampling operation is initiated using actuator 106 . Passage 112 becomes a portion of passage 16 in tubular string 12 (see FIG. 1 ) when fluid sampler 100 is interconnected in tubular string 12 . As such, internal fluid passageway 112 provides a smooth bore through fluid sampler 100 . Passage 110 in the upper portion of sampling chamber 102 is in communication with a sample chamber 114 via a check valve 116 . Check valve 116 permits fluid to flow from passage 110 into sample chamber 114 , but prevents fluid from escaping from sample chamber 114 to passage 110 .
A debris trap piston 118 separates sample chamber 114 from a meter fluid chamber 120 . When a fluid sample is received in sample chamber 114 , piston 118 is displaced downwardly. Prior to such downward displacement of piston 118 , however, piston section 122 is displaced downwardly relative to piston section 124 . In the illustrated embodiment, as fluid flows into sample chamber 114 , an optional check valve 128 permits the fluid to flow into debris chamber 126 . The resulting pressure differential across piston section 122 causes piston section 122 to displace downward, thereby expanding debris chamber 126 .
Eventually, piston section 122 will displace downward sufficiently far for a snap ring, C-ring, spring-loaded lugs, dogs or other type of engagement device 130 to engage a recess 132 formed on piston section 124 . Once engagement device 130 has engaged recess 132 , piston sections 122 , 124 displace downwardly together to expand sample chamber 114 . The fluid received in debris chamber 126 is prevented from escaping back into sample chamber 114 by check valve 128 in embodiments that include check valve 128 . In this manner, the fluid initially received into sample chamber 114 is trapped in debris chamber 126 . This initially received fluid is typically laden with debris, or is a type of fluid (such as mud) which it is not desired to sample. Debris chamber 126 thus permits this initially received fluid to be isolated from the fluid sample later received in sample chamber 114 .
Meter fluid chamber 120 initially contains a metering fluid, such as a hydraulic fluid, silicone oil or the like. A flow restrictor 134 and a check valve 136 control flow between chamber 120 and an atmospheric chamber 138 that initially contains a gas at a relatively low pressure such as air at atmospheric pressure. A collapsible piston assembly 140 in chamber 138 includes a prong 142 which initially maintains another check valve 144 off seat, so that flow in both directions is permitted through check valve 144 between chambers 120 , 138 . When elevated pressure is applied to chamber 138 , however, as described more fully below, piston assembly 140 collapses axially, and prong 142 will no longer maintain check valve 144 off seat, thereby preventing flow from chamber 120 to chamber 138 .
A floating piston 146 separates chamber 138 from another atmospheric chamber 148 that initially contains a gas at a relatively low pressure such as air at atmospheric pressure. A spacer 150 is attached to piston 146 and limits downward displacement of piston 146 . Spacer 150 is also used to contact a stem 152 of a valve 154 to open valve 154 . Valve 154 initially prevents communication between chamber 148 and a passage 156 in a lower portion of sampling chamber 102 . In addition, a check valve 158 permits fluid flow from passage 156 to chamber 148 , but prevents fluid flow from chamber 148 to passage 156 .
As mentioned above, one or more of the sampling chambers 102 and preferably nine of sampling chambers 102 are installed within exteriorly disposed chamber receiving slots 159 that circumscribe internal fluid passageway 112 of carrier 104 . A seal bore 160 (see FIG. 3B ) is provided in carrier 104 for receiving the upper portion of sampling chamber 102 and another seal bore 162 (see FIG. 3C ) is provided for receiving the lower portion of sampling chamber 102 . In this manner, passage 110 in the upper portion of sampling chamber 102 is placed in sealed communication with a passage 164 in carrier 104 , and passage 156 in the lower portion of sampling chamber 102 is placed in sealed communication with a passage 166 in carrier 104 .
In addition to the nine sampling chambers 102 installed within carrier 104 , a pressure and temperature gauge/recorder (not shown) of the type known to those skilled in the art can also be received in carrier 104 in a similar manner. For example, seal bores 168 , 170 in carrier 104 may be for providing communication between the gauge/recorder and internal fluid passageway 112 . Note that, although seal bore 170 depicted in FIG. 3C is in communication with passage 172 , preferably if seal bore 170 is used to accommodate a gauge/recorder, then a plug is used to isolate the gauge/recorder from passage 172 . Passage 172 is, however, in communication with passage 166 and the lower portion of each sampling chamber 102 installed in a seal bore 162 and thus servers as a manifold for fluid sampler 100 . If a sampling chamber 102 or gauge/recorder is not installed in one or more of the seal bores 160 , 162 , 168 , 170 then a plug will be installed to prevent flow therethrough.
Passage 172 is in communication with chamber 174 of pressure source 108 . Chamber 174 is in communication with chamber 176 of pressure source 108 via a passage 178 . Chambers 174 , 176 initially contain a pressurized fluid, such as a compressed gas or liquid. Preferably, compressed nitrogen at between about 7,000 psi and 12,000 psi is used to precharge chambers 174 , 176 , but other fluids or combinations of fluids and/or other pressures both higher and lower could be used, if desired. Even though FIG. 3 depicts pressure source 108 as having two compressed fluid chambers 174 , 176 , it should be understood by those skilled in the art that pressure source 108 could have any number of chambers both higher and lower than two that are in communication with one another to provide the required pressure source. As best seen in FIG. 4 , a cross-sectional view of pressure source 108 is illustrated, showing a fill valve 180 and a passage 182 extending from fill valve 180 to chamber 174 for supplying the pressurized fluid to chambers 174 , 176 at the surface prior to running fluid sampler 100 downhole.
As best seen in FIGS. 3A and 5 , actuator 106 includes multiple valves 184 , 186 , 188 and respective multiple rupture disks 190 , 192 , 194 to provide for separate actuation of multiple groups of sampling chambers 102 . In the illustrated embodiment, nine sampling chambers 102 may be used, and these are divided up into three groups of three sampling chambers each. Each group of sampling chambers can be referred to as a sampling chamber assembly. Thus, a valve 184 , 186 , 188 and a respective rupture disk 190 , 192 , 194 are used to actuate a group of three sampling chambers 102 . For clarity, operation of actuator 106 with respect to only one of the valves 184 , 186 , 188 and its respective one of the rupture disks 190 , 192 , 194 is described below. Operation of actuator 106 with respect to the other valves and rupture disks is similar to that described below.
Valve 184 initially isolates passage 164 , which is in communication with passages 110 in three of the sampling chambers 102 via passage 196 , from internal fluid passage 112 of fluid sampler 100 . This isolates sample chamber 114 in each of the three sampling chambers 102 from passage 112 . When it is desired to receive a fluid sample into each of the sample chambers 114 of the three sampling chambers 102 , pressure in annulus 26 is increased a sufficient amount to rupture the disk 190 . This permits pressure in annulus 26 to shift valve 184 upward, thereby opening valve 184 and permitting communication between passage 112 and passages 196 , 164 .
Fluid from passage 112 then enters passage 110 in the upper portion of each of the three sampling chambers 102 . For clarity, the operation of only one of the sampling chambers 102 after receipt of a fluid sample therein is described below. The fluid flows from passage 110 through check valve 116 to sample chamber 114 . An initial volume of the fluid is trapped in debris chamber 126 of piston 118 as described above. Downward displacement of the piston section 122 , and then the combined piston sections 122 , 124 , is slowed by the metering fluid in chamber 120 flowing through restrictor 134 . This prevents pressure in the fluid sample received in sample chamber 114 from dropping below its bubble point.
As piston 118 displaces downward, the metering fluid in chamber 120 flows through restrictor 134 into chamber 138 . At this point, prong 142 maintains check valve 144 off seat. The metering fluid received in chamber 138 causes piston 146 to displace downward. Eventually, spacer 150 contacts stem 152 of valve 154 which opens valve 154 . Opening of valve 154 permits pressure in pressure source 108 to be applied to chamber 148 . Pressurization of chamber 148 also results in pressure being applied to chambers 138 , 120 and thus to sample chamber 114 . This is due to the fact that passage 156 is in communication with passages 166 , 172 (see FIG. 3C ) and, thus, is in communication with the pressurized fluid from pressure source 108 .
When the pressure from pressure source 108 is applied to chamber 138 , piston assembly 140 collapses and prong 142 no longer maintains check valve 144 off seat. Check valve 144 then prevents pressure from escaping from chamber 120 and sample chamber 114 . Check valve 116 also prevents escape of pressure from sample chamber 114 . In this manner, the fluid sample received in sample chamber 114 is pressurized.
In the illustrated embodiment of fluid sampler 100 , multiple sampling chambers 102 are actuated by rupturing disk 190 , since valve 184 is used to provide selective communication between passage 112 and passages 110 in the upper portions of multiple sampling chambers 102 . Thus, multiple sampling chambers 102 simultaneously receive fluid samples therein from passage 112 .
In a similar manner, when rupture disk 192 is ruptured, an additional group of multiple sampling chambers 102 will receive fluid samples therein, and when the rupture disk 194 is ruptured a further group of multiple sampling chambers 102 will receive fluid samples therein. Rupture disks 184 , 186 , 188 may be selected so that they are ruptured sequentially at different pressures in annulus 26 or they may be selected so that they are ruptured simultaneously, at the same pressure in annulus 26 .
Another important feature of fluid sampler 100 is that the multiple sampling chambers 102 , nine in the illustrated example, share the same pressure source 108 . That is, pressure source 108 is in communication with each of the multiple sampling chambers 102 . This feature provides enhanced convenience, speed, economy and safety in the fluid sampling operation. In addition to sharing a common pressure source downhole, the multiple sampling chambers 102 of fluid sampler 100 can also share a common pressure source on the surface. Specifically, once all the samples are obtained and pressurized downhole, fluid sampler 100 is retrieved to the surface. Even though certain cooling of the samples will take place, the common pressure source maintains the samples at a suitable pressure to prevent any phase change degradation. Once on the surface, the sample may remain in the multiple sampling chambers 102 for a considerable time during which temperature conditions may fluctuate. Accordingly, a surface pressure source, such a compressor or a pump, may be used to supercharge the sampling chambers 102 . This supercharging process allows multiple sampling chambers 102 to be further pressurized at the same time with sampling chambers 102 remaining in carrier 104 or after sampling chambers 102 have been removed from carrier 104 .
Note that, although actuator 106 is described above as being configured to permit separate actuation of three groups of sampling chambers 102 , with each group including three of the sampling chambers 102 , it will be appreciated that any number of sampling chambers 102 may be used, sampling chambers 102 may be included in any number of groups (including one), each group could include any number of sampling chambers 102 (including one), different groups can include different numbers of sampling chambers 102 and it is not necessary for sampling chambers 102 to be separately grouped at all.
Referring now to FIG. 6 , an alternate actuating method for fluid sampler 100 is representatively and schematically illustrated. Instead of using increased pressure in annulus 26 to actuate valves 184 , 186 , 188 , a control module 198 included in fluid sampler 100 may be used to actuate valves 184 , 186 , 188 . For example, a telemetry receiver 199 may be connected to control module 198 . Receiver 199 may be any type of telemetry receiver, such as a receiver capable of receiving acoustic signals, pressure pulse signals, electromagnetic signals, mechanical signals or the like. As such, any type of telemetry may be used to transmit signals to receiver 199 .
When control module 198 determines that an appropriate signal has been received by receiver 199 , control module 198 causes a selected one or more of valves 184 , 186 , 188 to open, thereby causing a plurality of fluid samples to be taken in fluid sampler 100 . Valves 184 , 186 , 188 may be configured to open in response to application or release of electrical current, fluid pressure, biasing force, temperature or the like.
Referring now to FIGS. 7 and 8 , an alternate embodiment of a fluid sampler for use in obtaining a plurality of fluid samples that embodies principles of the present invention is representatively illustrated and generally designated 200 . Fluid sampler 200 includes an upper connector 202 for coupling fluid sampler 200 to other well tools in the sampler string. Fluid sampler 200 also includes an actuator 204 that operates in a manner similar to actuator 106 described above. Below actuator 204 is a carrier 206 that is of similar construction as carrier 104 described above. Fluid sampler 200 further includes a manifold 208 for distributing fluid pressure. Below manifold 208 is a lower connector 210 for coupling fluid sampler 200 to other well tools in the sampler string.
Fluid sampler 200 has a longitudinally extending internal fluid passageway 212 formed completely through fluid sampler 200 . Passageway 212 becomes a portion of passage 16 in tubular string 12 (see FIG. 1 ) when fluid sampler 200 is interconnected in tubular string 12 . In the illustrated embodiment, carrier 206 has ten exteriorly disposed chamber receiving slots that circumscribe internal fluid passageway 212 . As mentioned above, a pressure and temperature gauge/recorder (not shown) of the type known to those skilled in the art can be received in carrier 206 within one of the chamber receiving slots such as slot 214 . The remainder of the slots are used to receive sampling chambers and pressure source chambers.
In the illustrated embodiment, sampling chambers 216 , 218 , 220 , 222 , 224 , 226 are respectively received within slots 228 , 230 , 232 , 234 , 236 , 238 . Sampling chambers 216 , 218 , 220 , 222 , 224 , 226 are of a construction and operate in the manner described above with reference to sampling chamber 102 . Pressure source chambers 240 , 242 , 244 are respectively received within slots 246 , 248 , 250 in a manner similar to that described above with reference to sampling chamber 102 . Pressure source chambers 240 , 242 , 244 initially contain a pressurized fluid, such as a compressed gas or liquid. Preferably, compressed nitrogen at between about 10,000 psi and 20,000 psi is used to precharge chambers 240 , 242 , 244 , but other fluids or combinations of fluids and/or other pressures both higher and lower could be used, if desired.
Actuator 204 includes three valves that operate in a manner similar to valves 184 , 186 , 188 of actuator 106 . Actuator 204 has three rupture disks, one associated with each valve in a manner similar to rupture disks 190 , 192 , 194 of actuator 106 and one of which is pictured and denoted as rupture disk 252 . As described above, each of the rupture disks provides for separate actuation of a group of sampling chambers. In the illustrated embodiment, six sampling chambers are used, and these are divided up into three groups of two sampling chambers each. Associated with each group of two sampling chambers is one pressure source chamber. Specifically, rupture disk 252 is associated with sampling chambers 216 , 218 which are also associated with pressure source chamber 240 via manifold 208 . In a like manner, the second rupture disk is associated with sampling chambers 220 , 222 which are also associated with pressure source chamber 242 via manifold 208 . In addition, the third rupture disk is associated with sampling chambers 224 , 226 which are also associated with pressure source chamber 244 via manifold 208 . In the illustrated embodiment, each rupture disk, valve, pair of sampling chambers, pressure source chamber and manifold section can be referred to as a sampling chamber assembly. Each of the three sampling chamber assemblies operates independently of the other two sampling chamber assemblies. For clarity, the operation of one sampling chamber assembly is described below. Operation of the other two sampling chamber assemblies is similar to that described below.
The valve associated with rupture disk 252 initially isolates the sample chambers of sampling chambers 216 , 218 from internal fluid passageway 212 of fluid sampler 200 . When it is desired to receive a fluid sample into each of the sample chambers of sampling chambers 216 , 218 , pressure in annulus 26 is increased a sufficient amount to rupture the disk 252 . This permits pressure in annulus 26 to shift the associated valve upward in a manner described above, thereby opening the valve and permitting communication between passageway 212 and the sample chambers of sampling chambers 216 , 218 .
As described above, fluid from passageway 212 enters a passage in the upper portion of each of the sampling chambers 216 , 218 and passes through an optional check valve to the sample chambers. An initial volume of the fluid is trapped in a debris chamber as described above. Downward displacement of the debris piston is slowed by the metering fluid in another chamber flowing through a restrictor. This prevents pressure in the fluid sample received in the sample chambers from dropping below its bubble point.
As the debris piston displaces downward, the metering fluid flows through the restrictor into a lower chamber causing a piston to displace downward. Eventually, a spacer contacts a stem of a lower valve which opens the valve and permits pressure from pressure source chamber 240 to be applied to the lower chamber via manifold 208 . Pressurization of the lower chamber also results in pressure being applied to the sample chambers of sampling chambers 216 , 218 .
As described above, when the pressure from pressure source chamber 240 is applied to the lower chamber, a piston assembly collapses and a prong no longer maintains a check valve off seat, which prevents pressure from escaping from the sample chambers. The upper check valve also prevents escape of pressure from the sample chamber. In this manner, the fluid samples received in the sample chambers are pressurized.
In the illustrated embodiment of fluid sampler 200 , two sampling chambers 216 , 218 are actuated by rupturing disk 252 , since the valve associated therewith is used to provide selective communication between passageway 212 the sample chambers of sampling chambers 216 , 218 . Thus, both sampling chambers 216 , 218 simultaneously receive fluid samples therein from passageway 212 .
In a similar manner, when the other rupture disks are ruptured, additional groups of two sampling chambers (sampling chambers 220 , 222 and sampling chambers 224 , 226 ) will receive fluid samples therein and the fluid samples obtained therein will be pressurize by pressure sources 242 , 244 , respectively. The rupture disks may be selected so that they are ruptured sequentially at different pressures in annulus 26 or they may be selected so that they are ruptured simultaneously, at the same pressure in annulus 26 .
One of the important features of fluid sampler 200 is that the multiple sampling chambers, two in the illustrated example, share a common pressure source. That is, each pressure source is in communication with multiple sampling chambers. This feature provides enhanced convenience, speed, economy and safety in the fluid sampling operation. In addition to sharing a common pressure source downhole, multiple sampling chambers of fluid sampler 200 can also share a common pressure source on the surface. Specifically, once all the samples are obtained and pressurized downhole, fluid sampler 200 is retrieved to the surface. Even though certain cooling of the samples will take place, the common pressure source maintains the samples at a suitable pressure to prevent any phase change degradation. Once on the surface, the samples may remain in the multiple sampling chambers for a considerable time during which temperature conditions may fluctuate. Accordingly, a surface pressure source, such a compressor or a pump, may be used to supercharge the sampling chambers. This supercharging process allows multiple sampling chambers to be further pressurized at the same time with the sampling chambers remaining in carrier 206 or after sampling chambers have been removed from carrier 206 .
It should be understood by those skilled in the art that even though fluid sampler 200 has been described as having one pressure source chamber in communication with two sampling chambers via manifold 208 , other numbers of pressure source chambers may be in communication with other numbers of sampling chambers with departing from the principles of the present invention. For example, in certain embodiments, one pressure source chamber could communicate pressure to three, four or more sampling chambers. Likewise, two or more pressure source chambers could act as a common pressure source to a single sampling chamber or to a plurality of sampling chambers. Each of these embodiments may be enabled by making the appropriate adjustments to manifold 208 such that the desired pressure source chambers and the desired sampling chambers are properly communicated to one another.
Referring now to FIGS. 9A-9G and with reference to FIGS. 3A-3E , an alternate fluid sampling chamber for use in a fluid sampler including an exemplary carrier having a pressure source coupled thereto for use in obtaining a plurality of fluid samples that embodies principles of the present invention is representatively illustrated and generally designated 300 . Each of the sampling chambers 300 is coupled to a carrier 104 that also includes an actuator 106 and a pressure source 108 as depicted in FIG. 3 .
As described more fully below, a passage 310 in an upper portion of sampling chamber 300 (see FIG. 9A ) is placed in communication with a longitudinally extending internal fluid passageway 112 formed completely through the fluid sampler (see FIG. 3 ) when the fluid sampling operation is initiated using actuator 106 . Passage 112 becomes a portion of passage 16 in tubular string 12 (see FIG. 1 ) when the fluid sampler is interconnected in tubular string 12 . As such, internal fluid passageway 112 provides a smooth bore through the fluid sampler. Passage 310 in the upper portion of sampling chamber 300 is in communication with a sample chamber 314 via a check valve 316 . Check valve 316 permits fluid to flow from passage 310 into sample chamber 314 , but prevents fluid from escaping from sample chamber 314 to passage 310 .
A debris trap piston 318 is disposed within housing 302 and separates sample chamber 314 from a meter fluid chamber 320 . When a fluid sample is received in sample chamber 314 , debris trap piston 318 is displaced downwardly relative to housing 302 to expand sample chamber 314 . Prior to such downward displacement of debris trap piston 318 , however, fluid flows through sample chamber 314 and passageway 322 of piston 318 into debris chamber 326 of debris trap piston 318 . The fluid received in debris chamber 326 is prevented from escaping back into sample chamber 314 due to the relative cross sectional areas of passageway 322 and debris chamber 326 as well as the pressure maintained on debris chamber 326 from sample chamber 314 via passageway 322 . An optional check valve (not pictured) may be disposed within passageway 322 if desired. Such a check valve would operate in the manner described above with reference to check valve 128 in FIG. 2B . In this manner, the fluid initially received into sample chamber 314 is trapped in debris chamber 326 . Debris chamber 326 thus permits this initially received fluid to be isolated from the fluid sample later received in sample chamber 314 . Debris trap piston 318 includes a magnetic locator 324 used as a reference to determine the level of displacement of debris trap piston 318 and thus the volume within sample chamber 314 after a sample has been obtained.
Meter fluid chamber 320 initially contains a metering fluid, such as a hydraulic fluid, silicone oil or the like. A flow restrictor 334 and a check valve 336 control flow between chamber 320 and an atmospheric chamber 338 that initially contains a gas at a relatively low pressure such as air at atmospheric pressure. A collapsible piston assembly 340 includes a prong 342 which initially maintains check valve 344 off seat, so that flow in both directions is permitted through check valve 344 between chambers 320 , 338 . When elevated pressure is applied to chamber 338 , however, as described more fully below, piston assembly 340 collapses axially, and prong 342 will no longer maintain check valve 344 off seat, thereby preventing flow from chamber 320 to chamber 338 .
A piston 346 disposed within housing 302 separates chamber 338 from a longitudinally extending atmospheric chamber 348 that initially contains a gas at a relatively low pressure such as air at atmospheric pressure. Piston 346 includes a magnetic locator 347 used as a reference to determine the level of displacement of piston 346 and thus the volume within chamber 338 after a sample has been obtained. Piston 346 included a piercing assembly 350 at its lower end. In the illustrated embodiment, piercing assembly 350 is threadably coupled to piston 346 which creates a compression connection between a piercing assembly body 352 and a needle 354 . Alternatively, needle 354 may be coupled to piercing assembly body 352 via threading, welding, friction or other suitable technique. Needle 354 has a sharp point at its lower end and may have a smooth outer surface or may have an outer surface that is fluted, channeled, knurled or otherwise irregular. As discussed more fully below, needle 354 is used to actuate the pressure delivery subsystem of the fluid sampler when piston 346 is sufficiently displaced relative to housing 302 .
Below atmospheric chamber 348 and disposed within the longitudinal passageway of housing 302 is a valving assembly 356 . Valving assembly 356 includes a pressure disk holder 358 that receives a pressure disk therein that is depicted as rupture disk 360 , however, other types of pressure disks that provide a seal, such as a metal-to-metal seal, with pressure disk holder 358 could also be used including a pressure membrane or other piercable member. Rupture disk 360 is held within pressure disk holder 358 by hold down ring 362 and gland 364 that is threadably coupled to pressure disk holder 358 . Valving assembly 356 also includes a check valve 366 . Valving assembly 356 initially prevents communication between chamber 348 and a passage 380 in a lower portion of sampling chamber 300 . After actuation the pressure delivery subsystem by needle 354 , check valve 366 permits fluid flow from passage 380 to chamber 348 , but prevents fluid flow from chamber 348 to passage 380 .
As mentioned above, one or more of the sampling chambers 300 and preferably nine of sampling chambers 300 are installed within exteriorly disposed chamber receiving slots 159 that circumscribe internal fluid passageway 112 of carrier 104 . A seal bore 160 (see FIG. 3B ) is provided in carrier 104 for receiving the upper portion of sampling chamber 300 and another seal bore 162 (see FIG. 3C ) is provided for receiving the lower portion of sampling chamber 300 . In this manner, passage 310 in the upper portion of sampling chamber 300 is placed in sealed communication with a passage 164 in carrier 104 , and passage 380 in the lower portion of sampling chamber 300 is placed in sealed communication with a passage 166 in carrier 104 .
As described above, once the fluid sampler is in its operable configuration and is located at the desired position within the wellbore, a fluid sample can be obtained into one or more of the sample chambers 314 by operating actuator 106 . Fluid from passage 112 then enters passage 310 in the upper portion of each of the desired sampling chambers 300 . For clarity, the operation of only one of the sampling chambers 300 after receipt of a fluid sample therein is described below. The fluid flows from passage 310 through check valve 316 to sample chamber 314 . It is noted that check valve 316 may include a restrictor pin 368 to prevent excessive travel of ball member 370 and over compression or recoil of spiral wound compression spring 372 . An initial volume of the fluid is trapped in debris chamber 326 of piston 318 as described above. Downward displacement of piston 318 is slowed by the metering fluid in chamber 320 flowing through restrictor 334 . This prevents pressure in the fluid sample received in sample chamber 314 from dropping below its bubble point.
As piston 318 displaces downward, the metering fluid in chamber 320 flows through restrictor 334 into chamber 338 . At this point, prong 342 maintains check valve 344 off seat. The metering fluid received in chamber 338 causes piston 346 to displace downwardly. Eventually, needle 354 pierces rupture disk 360 which actuates valving assembly 356 . Actuation of valving assembly 356 permits pressure from pressure source 108 to be applied to chamber 348 . Specifically, once rupture disk 360 is pierced, the pressure from pressure source 108 passes through valving assembly 356 including moving check valve 366 off seat. In the illustrated embodiment, a restrictor pin 374 prevents excessive travel of check valve 366 and over compression or recoil of spiral wound compression spring 376 . Pressurization of chamber 348 also results in pressure being applied to chambers 338 , 320 and thus to sample chamber 314 .
When the pressure from pressure source 108 is applied to chamber 338 , pins 378 are sheared allowing piston assembly 340 to collapse such that prong 342 no longer maintains check valve 344 off seat. Check valve 344 then prevents pressure from escaping from chamber 320 and sample chamber 314 . Check valve 316 also prevents escape of pressure from sample chamber 314 . In this manner, the fluid sample received in sample chamber 314 is pressurized.
While this invention has been described with a reference to illustrative embodiments, this description is not intended to be construed in a limiting sense. Various modifications and combinations of the illustrative embodiments as well as other embodiments of the invention, will be apparent to persons skilled in the art upon reference to the description. It is, therefore, intended that the appended claims encompass any such modifications or embodiments.
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An apparatus ( 300 ) for obtaining a fluid sample in a subterranean well includes a housing ( 302 ) having a sample chamber ( 314 ) defined therein. The sample chamber ( 314 ) is selectively in fluid communication with the exterior of the housing ( 302 ) and is operable to receive the fluid sample therefrom. A debris trap piston ( 318 ) is slidably disposed within the housing ( 302 ). The debris trap piston ( 318 ) includes a debris chamber ( 326 ). Responsive to the fluid sample entering the sample chamber ( 314 ), the debris trap piston ( 318 ) receives a first portion of the fluid sample in the debris chamber ( 326 ) then displaces relative to the housing ( 302 ) to expand the sample chamber ( 314 ).
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BACKGROUND OF THE INVENTION
This invention relates to transmission units in which the operative ratio is selected by a selection system which includes fluid-pressure-operated actuators under the control of solenoid-operated valves. Such transmission units are used, for example, in agricultural/industrial tractors.
Whilst such transmission units operate effectively they can be prone to break down due to minor electrical problems, etc. which leave the valves and thus the fluid-pressure-operated actuators inoperative thus completely disabling the transmission unit.
It is an object of the present invention to provide an improved form of such a transmission unit in which the problem of transmission disablement is mitigated.
SUMMARY OF THE INVENTION
Thus according to the present invention there is provided a vehicle transmission unit housed in a casing and including a plurality of drive ratio paths selectively engageable by a ratio selection system which includes fluid-pressure-operated actuators under the control of solenoid-operated valves to select the operative drive ratio of the transmission, the transmission also including one or more mechanical actuator members accessible from outside the casing which can be manipulated to select one or more drive ratios of the unit in the event of the failure of the fluid-pressure-operated actuators or valves.
A transmission unit in accordance with the present invention thus provides a "get you home" facility which still enables one or more drive ratios of the unit to be selected manually should the fluid-pressure-operated actuators or valves fail.
Conveniently, the fluid-pressure-operated actuators are connected to ratio engaging means (such as selector forks) via mechanical linkage means and said one or more mechanical actuator members are also connected to said mechanical linkage means.
The mechanical actuator member or members may comprise one or more shafts projecting from the transmission casing which can be manipulated by a spanner, wrench or similar instrument to effect selection of one or more drive ratios in the unit.
The transmission unit may be controlled manually by the operator initiating each drive ratio selection or automatically by, for example, an electronic control system which initiates each drive ratio selection in accordance with predetermined vehicle performance parameters.
BRIEF DESCRIPTION OF THE DRAWING
One embodiment of the present invention as applied to an agricultural tractor transmission will now be described, by way of example only, with reference to the accompanying drawings in which:
FIG. 1 is a diagrammatic representation of the basic tractor transmission layout;
FIG. 2 is a diagrammatic representation of the ratio selection system of a transmission unit embodying the present invention.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
Referring to FIG. 1, this shows the diagrammatic layout of a tractor transmission in which engine E drives front and rear wheels W1 and W2 via differentials D1 and D2, a main clutch C, a planetary gear unit P, a main gearbox G and a transfer box T. As shown in FIG. 1, the gearbox G includes an input shaft, which is connected to the planetary gear unit P and extends within the casing of the transmission, and an output shaft, which extends from within the casing of the transmission and is connected to the transfer case T. The main gearbox G will typically have four ratios and a forward/reverse direction selection train in addition to a high/low range facility indicated in dotted detail H/L in FIG. 1.
U.S. Pat. No. 5,249,481 discloses a suitable form of planetary gear unit P for use in the transmission which has four ratios which provide ranges A, B, C and D of the transmission. Four clutches are provided to engage the ratios of planetary gear unit P. These clutches are divided into two pairs, one clutch of each pair being hydraulically engaged and the other mechanically by spring force. The configuration of the planetary gear train is such that one clutch of each pair must be engaged in order to provide a drive path through the planetary gear unit. Thus in the event of the failure of hydraulic pressure the spring engaged clutch of each pair operates to provide a drive path through the planetary gear unit.
Further details of a suitable form of planetary gear unit and a suitable ratio selection system for the planetary gear unit are contained in the previously referred to U.S. Pat. No. 5,249,481 and will not be repeated here since they form no part of the present invention.
Main gearbox G forms a transmission unit in accordance with the present invention in which its four drive ratios, its forward/reverse direction selection and its high/low range facility are all operated hydraulically using solenoid operated fluid flow control valves.
FIG. 2 shows diagrammatically a ratio selection system for the main gearbox G in which the four ratios of the gearbox are selected by two selector forks one end of each of which is shown at 10 and 11. Selector fork 10 is movable, as indicated by arrows 1 and 2, from the neutral drive condition shown in FIG. 2 to select ratios 1 and 2 of the gearbox. Similarly selector fork 11 is movable in the directions indicated by arrows 3 and 4 to select ratios 3 and 4 of the gearbox. The selector forks are movable by a selector member 12 mounted on a selector shaft 13, this shaft being both rotatable and axially displaceable. Shaft 13 is biased by spring 14 to the axial position shown in FIG. 2 in which selector member 12 engages selector fork 11. As shown in FIG. 2, the spring to is a coiled spring which is disposed about the shaft 13 and reacts between the casing 47 of the transmission and an enlarged portion formed on the outer end of the shaft 13. Selector member 12 is rotatable about the longitudinal axis of shaft 13 by a double acting piston 15 which is slidable in a bore 16 in transmission casing 47 to define end chambers 17 and 18 respectively. Piston 15 is connected to shaft 13 by an arm 19 which is nonrotatably secured on shaft 13 and has a spade-like end portion 20 which engages in a slot 21 in piston 15.
Thus, as will be appreciated, shaft 13 can be rotated in a clock-wise sense as indicated by arrow X by pressurising end chamber 16 using solenoid operated valve 23 thus moving selector fork 11 to engage ratio 3 in gearbox G. Similarly, shaft 13 can be rotated in an anti-clock sense as indicated by arrow Y by pressurizing end chamber 17 using solenoid operated valve 22. This moves selector fork 11 to engage ratio 4 of the gearbox. The axial position of piston 15 and hence the operative position of selector fork 11 (and also selector fork 10 when it is engaged by arm 12) is indicated by a rotary potentiometer 24 which is connected to end portion 20 of arm 19 via a peg 25 which engages a cut-out in an arm 27 mounted on the spindle 24a of the potentiometer 24.
The shaft 13 is displaced axially in direction P by pressurising a chamber 28 which contains a piston portion 29 formed on shaft 13. Pressurization of chamber 28, which is controlled by solenoid operated valve 36, displaces shaft 13 to move selector member 12 out of selector fork 11 into selector fork 10. An interlock member 30 formed on the top of selector member 12 co-operates an interlock formation 31 formed on the housing to ensure that the selector member 12 can only be disengaged from selector fork 11 and engaged with selector 10 when the shaft 13 is in its neutral selection position, as shown in FIG. 2.
The axial position of shaft 13 is indicated by a proximity sensor 32 which co-operates with a disc member 33 mounted on a sliding rod 34. This member 33 which is mounted in bores 47a and 47b in the transmission casing 47 is also received in a cut-out 35 in the mounting boss of arm 19. When the selector member 12 is engaged in the selector fork 11, as shown in FIG. 2, the left-hand edge 35a of the cut-out 35 positions the disc member 33 opposite the sensor 32 to provide a high reading from the sensor. When the shaft 13 is moved in direction P to engage selector fork 10, the right-hand edge 35b of slot 35 contacts disc member 33 during the latter part of the movement of shaft 13 in order to move the disc member 33 away from the proximity sensor 32 in direction P. This thus provides a low reading from the sensor indicating that the shaft has been axially displaced to engage the seector fork 10.
In accordance with the present invention, the shaft 13 is provided with a square or hexagonally-shaped end portion 13a which projects externally from the transmission casing 47 and can be gripped for both rotation and axial displacement by a suitable spanner, wrench or other tool in order to move selector member 12 manually to select any one of the ratios 1 to 4 of the transmission unit should pistons 15 and 29 be incapacitated due to hydraulic or electrical failure.
The forward/reverse drive direction is selected by a fork one end of which is shown at 37. Fork 37 is moved by a double-acting piston 38 movable in a bore 39 to define end chambers 40 and 41 respectively. Piston 38 can be displaced by pressurising either end chamber 40 using solenoid operated valve 42, or chamber 41 using solenoid operated valve 43. A rod 44 connects piston 38 with a selector member 45 which rotates with a mounting shaft 46 supported in the transmission casing 47.
Thus pressurization of end chamber 40 axially displaces rod 44 to the left as viewed in FIG. 2 thus pivoting selector member 45 with rod 46 in an anti-clockwise sense in the transmission casing 47 to displace the selector fork 37 to the left from the neutral position shown. This engages the reverse drive condition in the transmission unit. Similarly, pressurization of end chamber 41 moves the rod 44 to the right thus pivoting the selector member 45 in a clock-wise sense and hence moving the selector fork 37 to the right to engage the forward drive condition of the transmission unit.
The position of the piston 38 and hence the drive condition engaged in the transmission unit is indicated by the reading from a rotary potentiometer 48 which is connected to the selector member 45 via an arm 49, a pin 50 and a slotted arm 51 mounted on the rotary potentiometer spindle 48a.
In accordance with the present invention the mounting shaft 46 is also provided with a square or hexagonally-shaped end portion 46a which projects externally from the transmission casing 47 and can be gripped and rotated by a suitable wrench or other tool in order to displace the selector member 45 thus engaging manually either the forward or reverse drive direction should the piston 38 be incapacitated due to hydraulic or electrical failure.
The high/low range facility of the transmission unit is operated by a piston 55 which operates in a bore 56 thus defining end chambers 61 and 62. Piston 55 is provided with a rod 57 which moves a selector fork of the high/low range facility one end of which is shown at 58. A proximity sensor 59 operates in conjunction with an enlarged diameter port on 60 of rod 57 to indicate the axial position of piston 55 and thus whether the high/low range facility is engaged. To engage the high range facility solenoid-operated valve 63 is operated to connect end chamber 62 to the hydraulic system pressure of line 65. End chamber 61 is permanently connected to line 65 so that both sides of piston 55 are subject to the operating pressure and, as a result of the differential area effect caused by the provision of rod 57 on one side of piston 55 only, the piston is moved to its extreme right-hand travel position shown in FIG. 2.
In order to engage the low range facility chamber 62 is depressurised using valve 63 so that the pressure in chamber 61 moves the piston 55 to the left, thus engaging the low range. No neutral condition is provided on the high/low range facility, thus in the event of an hydraulic or electrical failure the facility will provide either the high or low range drive depending on the condition selected at the time of the failure.
The ratio selection system described above for gearbox G utilizes solenoid-operated valves 22, 23, 36, 42, 43 and 63 and their associated hydraulic actuators in the form of pistons 15, 29, 38 and 55 to select the various ratios, the drive direction and the operative high/low range facility of the gearbox. In order to remove the necessity to maintain the system hydraulic pressure on the pistons 15, 29, 38 and 55 at all times each of these pistons is associated with a detent system (not shown in FIG. 2) which mechanically holds the piston in the position last selected by the hydraulic pressure.
The valves 22, 23, 36, 42, 43 and 63 may be controlled in a wide variety of ways. For example, the valves may be controlled manually by the tractor operator using, for example, the control levers 70, 80 and 90 shown in FIG. 1. Control lever 70 moves in a straight control gate 71 which has selection positions A, B, C and D corresponding to the four ratios of the planetary gear unit P. Control lever 80 moves in a straight gate 81 to select the forward, neutral and reverse drive conditions of the gearbox. Control lever 90 moves in a conventional H-shaped gate 91 with ratio positions 1 to 4 for the selection of the four ratios of gearbox G and a neutral plane N. A two-position button or switch 92 on the top of control lever 90 is used to select either the high or low range facility.
Alternatively, the valves 22 to 63 may be controlled by an automatic transmission control system (with or without a manual override capability for the operator) in response to predetermined tractor operating parameters.
It will be appreciated from the above that the complete transmission is still operable should an hydraulic or electrical failure occur since the planetary gear unit P and high/low range facility still retain their drive capability as explained above and main gearbox G still retains a full mechanical selection capability by using a wrench or other tool on the end portions 13a and 46a of the selection shafts 13 and 46.
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A vehicle transmission unit is housed in a casing and includes a plurality of drive ratio paths selectively engageable by a ratio selection system. The ratio selection system includes fluid-pressure-operated actuators under the control of solenoid-operated valves to select the operative drive ratio of the transmission. The transmission also includes one or more mechanical actuator members accessible from outside the casing which can be manipulated to select one or more drive ratios of the unit in the event of the failure of the fluid-pressure-operated actuators or valves.
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BACKGROUND OF THE INVENTION
1. Field of the Invention
This invention relates to techniques for calibration of gun sights and, more particularly, to a laser precision bore sight assembly.
2. Prior Art
Previously, several different systems have been used for calibration of gun sights. To obtain an accurate alignment of a weapon bore sight or of a training device attached to a weapon, the first step in using a bore sight device is to rotate the bore sight device a minimum of 360 degrees to confirm that the alignment of the bore sight is concentric to the bore of the weapon. If the laser point that is projected from the bore sight device onto a target 10 meters away traces a circle on the target, then the axis of the bore sight device is not concentric with the bore of the weapon.
One type of alignment device, as disclosed in U.S. Pat. No. 4,825,258, uses a light source, such as a laser, which is coaxially mounted outside of the gun barrel on the outer end of a hollow cylindrical metal rod, the inner end of which extends into the bore of a gun barrel. The outer end of the hollow cylindrical rod is a larger cylinder which engages the inside wall of the gun barrel. The inner end of the hollow rod is smaller in diameter than the bore of the gun barrel and has an expandable, split end formed into a number of longitudinal metal fingers. The free ends of the longitudinal fingers are expanded outwardly using a cone-shaped mandrel which is drawn into the metal fingers with a screw which extends out through the hollow rod mechanism to force the cone-shaped mandrel into the fingers. In this manner, the ends of the metal fingers are pushed outwardly to engage the inner wall of the bore of the gun barrel. This arrangement is supposed to fix the inner end of the rod in position in the bore of the gun barrel and to maintain the axis of the rod in alignment with the axis of the bore of the gun barrel.
Note that, this type of a system can be rotated prior to the metal fingers engaging the walls of the gun barrel, but the fit of the fingers is too loose to maintain concentric alignment. If the metal fingers fully contact the barrel, the fingers catch upon the rifling grooves making it difficult to rotate the device while maintaining concentric alignment of a laser beam. When this arrangement is axially rotated in the gun barrel, some of the metal fingers engage the rifling grooves formed in the inside walls of the gun barrel while other metal fingers directly engage the walls of the gun barrel, which causes the inner end of a rotated rod to change its alignments in the gun barrel. The type of metal material used for the fingers also has an effect of the performance of such an arrangement. Use of a material, which is softer than the hard steel of a gun barrel, such as brass, results in wear of the metal fingers and uneven alignment of the metal fingers within the gun barrel so that the inner end of the rod does not remain coaxially aligned with the gun barrel. On the other hand, use of a harder material for the metal fingers results in wear and damage to the rifling within the gun barrel.
U.S. Pat. No. 5,365,669 discloses another system which uses a laser light source mounted in a cartridge-shaped housing that is contained in a cartridge chamber of a gun. This system is not adjustable and is subject to the axial offsets and misalignments between the axis of the cartridge chamber and the axis of the bore of the gun barrel.
What is needed is a system which maintains direct coaxial alignment of a laser light source along the axis of the bore of a gun barrel, particularly when that laser light source is axially rotated.
SUMMARY OF THE INVENTION
The present invention provides a bore sight assembly which is used for aligning optical scopes, mechanical firearm sights, laser sighting devices, firearm training systems, or other devices that are aligned with a target point, such that a projectile or a simulated projectile fired from a weapon or a training device strikes the target point. The present invention provides a precision bore sight alignment assembly which remains in coaxial alignment with the axis of the bore of a gun barrel, particularly when the rod is rotated within the gun barrel, to thoroughly maintain concentric alignment of an alignment laser beam.
The present invention provides a laser precision bore sight system for bore sight alignment of a laser beam along the longitudinal axis of a gun barrel. As mentioned above, this system is suitable for alignment of various types of weapon sights. This system is also suitable for simulating firing of a weapon in a training system using a laser beam to simulate the path of an actual projectile or bullet.
A system according to the invention includes an elongated bore shaft with a longitudinal axis. The bore shaft is adapted to having its proximate end inserted into the bore of the gun barrel. At the proximate end of the elongated shaft is rotatably mounted a compressible barrel insert which has a continuous outer surface. The barrel insert is adapted to be inserted in the gun barrel so that the outer surface thereof resiliently engages the inside wall of the gun barrel. In this way the longitudinal axis of the proximate end of the bore shaft is coaxially aligned with the longitudinal axis of the gun barrel.
The distal end of the bore shaft is also coaxially aligned with the axis of the gun barrel. One embodiment of the invention includes an alignment cone which is fixed to the distal end of the bore shaft. The surface of the alignment cone increases in diameter as it extends distally away from the bore shaft. Depending on the caliber of the gun, a certain area of the conical surface of the alignment cone engages the distal inner edge of the gun barrel. In this way the distal end of the shaft is aligned with the longitudinal axis of the gun barrel.
Coaxially mounted adjacent to the alignment cone is a battery/switch housing which contains a switch assembly. A laser housing assembly is coaxially mounted adjacent to the battery/switch housing and contains a laser subassembly having a laser source which provides a laser beam in a direction coaxial with the longitudinal axis of the shaft. The battery/switch housing and the laser housing assembly have longitudinal end bores formed therein to provide an enclosure for a battery. The battery/switch housing and the laser housing assembly also have corresponding matching threads formed thereon to provide for relative longitudinal axial movement therebetween when they are rotated with respect to each other such that a terminal of the battery engages the switch assembly to activate the laser source.
In one preferred embodiment of the invention, the compressible barrel insert is a cylinder formed of a machined acetal material. In one preferred embodiment, the compressible cylindrical barrel insert is rotatably mounted on the cylindrical bearing surface of a barrel insert retainer shaft which is coaxially screwed to the end of the elongated shaft.
To accommodate a number of gun barrel sizes, the compressible barrel insert is selected from a group of cylindrical barrel inserts, corresponding to a particular gun-barrel caliber.
The laser housing assembly also includes a three point laser alignment mechanism for adjusting the alignment of the laser subassembly so that the laser beam is directed along the longitudinal axes of the shaft and the bore of the gun barrel when the shaft is rotated. One preferred embodiment of the three-point alignment mechanism includes fixed adjustments made at a factory or a service station. Another preferred embodiment of the three-point alignment mechanism is manually adjustable by a user in the field and includes two manually adjustable screw mechanisms, the ends of which contacts the laser subassembly and a spring-loaded bushing, which is fixed to a set screw and which biases the laser subassembly against the first and the second manually adjustable adjustment screws. The two manual adjustment screw mechanisms each includes a fine adjustment screw which moves radially with respect to the axis of the shaft and a detent mechanism provides for stepped manual adjustment of the adjustable screws.
The battery/switch housing switch assembly is contained in a cavity formed in a battery/switch housing and includes a compression spring having flat ends and contained within the cavity. A cup-shaped fiber washer has a center bore formed therethrough to receive a contact pin which is a flat-head brass screw or a smooth sided pin, both with a conical head and an end contact surface. The contact pin is held in the center bore of the fiber washer with the head of the pin on one wide of the fiber washer and a nickel-plated washer on the other side of the fiber washer. A solder blob covers the top surface of the conical head to serve as a contact area for the positive terminal of a battery. The contact pin is soldered to the nickel plated washer. Relative twisting of the battery/switch housing with respect to the laser housing assembly pushes the positive battery terminal into the head of the contact pin such that the contact end of the contact pin contacts the housing to activate the laser source.
The barrel-shaped insert includes a cylindrical base, which is rotatably mounted to the shaft and an attached radially resilient section which resiliently positions the axis of the end of the shaft along the longitudinal axis of the gun barrel. In one preferred embodiment of the invention, the radially resilient section has a peaked cylindrical area which has a maximum diameter which is greater than the diameter of the gun barrel such that when the barrel-shaped insert is inserted into the gun barrel, the external surface of peaked cylindrical area contacts the interior wall of the gun barrel and is pushed radially inwardly to conform to the smaller diameter of the gun barrel. The peaked cylindrical area of the barrel insert snugly engages the wall of the gun barrel to precisely position the one end of the shaft within the gun barrel along the longitudinal axis of the gun barrel and the peaked cylindrical area of the barrel insert provides continuously contact with the inner wall of the gun barrel in spite of the rifling grooves formed in the gun barrel and the tough material of the barrel insert does not damage the interior surface or the rifling of the gun barrel.
One embodiment of the radially resilient barrel-shaped insert has a section which has an interior diameter larger than the interior diameter of the cylindrical base section and a peaked cylindrical area with a maximum diameter which is greater than the diameter of the gun barrel.
Another embodiment of the radially resilient section includes an integral radially outwardly extending support flange from which longitudinally extends an integral cantilevered resilient ring with a peaked cylindrical area which has a maximum diameter greater than the diameter of the gun barrel to prove a snug fit within the barrel of a gun. The integral cantilevered resilient ring is spaced apart from the main cylindrical section and has a ring-shaped space formed beneath it.
The three-point alignment mechanism mounted to the universal housing for adjusting the alignment of the laser subassembly includes two orthogonally aligned adjustable screw mechanisms and a spring-loaded bushing aligned for movement in a direction to bias the laser subassembly against the ends of the first and the second adjustment screws.
A fine adjustment retainer ring has a number of pairs of opposing internal recesses formed therein which are engaged by at least one spring-loaded ball to provide stepped adjustments.
The invention also provides a method for aligning a laser beam along the longitudinal axis of the bore of a gun barrel and includes the following steps: rotatably mounting a cylindrical barrel insert, which has a flexible outer cylindrical surface, to one end of a shaft having a longitudinal axis; inserting the cylindrical barrel insert into the bore of the gun barrel having a longitudinal axis and engaging the inside wall of the gun barrel bore with the outer cylindrical surface of the cylindrical barrel insert; engaging an alignment cone located at the outer end of the shaft with the outer inside edge of the gun barrel such that the longitudinal axis of the shaft is coaxially aligned with the longitudinal axis of the gun barrel when the shaft is inserted and rotated in the gun barrel; mounting a laser housing, which contains a laser source assembly, to the outer end of the shaft; directing a laser beam from the laser source assembly in a direction coaxial with the longitudinal axis of the shaft; and adjusting a three point laser alignment mechanism mounted to the universal housing for adjusting and truing the alignment of the laser beam along the longitudinal axes of the shaft and the bore of the gun barrel, even when the shaft is rotated.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a perspective view of a laser precision bore sight assembly for insertion into the end of a gun barrel and for alignment of a laser beam along the axis of the gun barrel.
FIG. 2 is a partially sectional view of a section of a gun barrel with a laser precision bore sight assembly barrel according to the invention inserted therein.
FIGS. 3 is an exploded view showing a bore sight assembly shaft, into the end of which is inserted a retainer screw on which is axially mounted for rotation a selected one of a number of illustrated barrel inserts, each corresponding to a particular gun-barrel caliber.
FIG. 4A is an enlarged perspective view of one type of typical barrel insert for use with a smaller caliber gun, such as a 0.270 caliber or 7 mm.
FIG. 4B is an enlarged sectional view of the barrel insert of FIG. 4 A.
FIG. 4C is a cross sectional view of the barrel insert of FIG. 4 A.
FIG. 5A is an enlarged perspective view of another type of typical barrel insert for use with a larger caliber gun barrel, such as a 0.50 caliber.
FIG. 5B is an enlarged sectional view of the barrel insert of FIG. 5 A.
FIG. 5C is a cross sectional view of the barrel insert of FIG. 5 A.
FIG. 6A is an end view of an alternative metal spring barrel insert for a small caliber gun.
FIG. 6B is a partially sectional view of the alternative metal spring barrel insert FIG. 6 A.
FIG. 7 is an exploded, perspective view of a laser precision bore sight assembly according to the invention.
FIG. 8 is a sectional view showing a battery/switch housing with a battery switch assembled therein which is actuated by rotating the battery switch housing with respect to the laser housing so as push a battery terminal against one end of a contact pin so that the other end of the contact pin contacts the housing to complete the battery circuit to the laser source.
FIG. 9 is an exploded view showing the battery/switch housing and the battery switch components.
FIG. 10 is a perspective view of a laser housing.
FIG. 11 is an exploded end view showing a laser housing along with a fixed set screw and two adjustable windage/elevation assemblies.
FIG. 12 is an exploded, partially sectional view of an adjustable windage/elevation assembly.
FIG. 13 is a perspective view of an adjustment screw for the windage/elevation assembly of FIG. 12 .
FIG. 14 is a perspective view of a cap for the windage/elevation assembly of FIG. 12 .
FIG. 15A is a perspective view of a bonnet for the windage/elevation assembly of FIG. 12 .
FIG. 15B is a sectional, perspective view of the bonnet, taken along section line 15 B— 15 B of FIG. 15A, for the windage/elevation adjustment assembly of FIG. 15 A.
FIG. 16 is a perspective view of a retainer ring which provides fine adjustment steps for the windage/elevation adjustment assembly of FIG. 12 .
FIG. 17 is a plan view of a base for the windage/elevation assembly of FIG. 12 .
FIG. 18 is a cross sectional view of the laser housing showing a fixed adjustment assembly, which includes a bushing, a spring, and a set screw for biasing a laser module against a pair of adjustable windage/elevation assemblies.
FIG. 19 is an exploded, perspective view of a laser module subassembly.
FIG. 20 is an assembled sectional view of the laser module subassembly of FIG. 19 .
FIG. 21 is a sectional view of laser housing with a showing two windage/elevation adjustment assemblies and a spring loaded bushing for alignment of a laser beam from a laser housing assembly.
FIG. 22 is a sectional view, taken along section line 22 — 22 of FIG. 21, of a laser housing containing a laser assembly, having a windage/elevation adjustment assembly and a spring loaded bushing.
FIG. 23 is an exploded, partially sectional view of a front cap and lens.
FIG. 24 is a sectional view of an assembled front cap and lens.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
Reference will now be made in detail to the preferred embodiments of the invention, examples of which are illustrated in the accompanying drawings. While the invention will be described in conjunction with the preferred embodiments, it should be understood that they are not intended to limit the invention to these embodiments. On the contrary, the invention is intended to cover alternatives, modifications and equivalents, which are included within the spirit and scope of the invention as defined by the appended claims.
FIGS. 1 and 2 illustrate a laser precision bore sight assembly 10 for insertion into the bore 12 of a gun barrel 14 , of, for example, a rifle pistol, or shotgun for alignment of the gun sights. The laser precision bore sight assembly 10 includes a rotatable barrel insert 15 which is mounted on the proximate end of a bore shaft 16 and inserted into the gun barrel. At the distal end of the shaft 16 are coaxially attached a series of elements aligned along a longitudinal axis. These elements include an alignment cone 18 , a coaxial battery/switch housing 20 , and a coaxial laser housing 22 . The function of the laser precision bore sight assembly 10 is to provide a laser beam 23 which is aligned with the longitudinal axis of the gun barrel.
The length of the bore shaft 16 is optionally long or short depending upon whether it is used with a rifle or a pistol. A proximate end 24 of the bore shaft 16 has the rotatable barrel insert 15 mounted thereto. The proximate end of the shaft 16 is inserted into the bore 12 of the gun barrel 14 to align the proximate end of the laser precision bore sight assembly 10 along the axis of the gun barrel. The distal end 26 of the bore shaft 16 is attached to the alignment cone by being press fit into a bore formed through a smaller end face of the alignment cone 18 . The coaxial alignment cone 18 is a truncated cone which increases in diameter as it extends away from the smaller proximate end face to terminate in a larger distal end.
FIG. 2 illustrates that the conical surface of the coaxial alignment cone 18 is adapted to engage the inside edge of the bore 12 of the gun barrel in order to longitudinally position the distal end of the bore shaft 16 along the axis of the gun barrel. For each barrel diameter, somewhere along the alignment cone 18 is a circumference which matches the circumference of the inside edge of the gun barrel to concentrically align the distal end of the shaft with the longitudinal axis of the gun barrel.
FIG. 3 illustrates that the proximate end 24 of the bore shaft 16 has an axial bore 30 which extends 0.060 inches into the end of the bore shaft. A smooth interior surface 31 is followed by a threaded countersink interior, which accommodates external threads 32 formed at one end of a coaxial barrel insert retainer shaft 34 . The barrel insert retainer shaft 34 has a smooth external surface 33 , which is approximately 0.04 inches in length and which is located adjacent to and inboard of the threads 32 . When the external threads of the retainer shaft 34 are screwed into the internal threads in the end of the bore shaft 15 , the surface 33 slip fits inside the surface 31 , with the surfaces overlapping about approximately 0.040 inches to maintain axial alignment of the two shafts. The tolerances on the diameters of the overlapping surfaces 31 , 33 are tightly held to create a very close slip fit therebetween. This helps to lock the retainer shaft 34 to the bore shaft 16 so that the retainer shaft 34 will not back out if the bore sight assembly 10 is counter rotated in the gun barrel.
The barrel insert retainer shaft 34 has an external cylindrical bearing surface 36 . The diameter of the bearing surface 36 is smaller than the diameter of the bore shaft 16 to provide a step or shoulder therebetween. These shoulders hold the rotatable barrel insert 15 in position on the shaft 34 .
FIG. 3 also illustrates a number of cylindrical barrel inserts 41 - 47 each of which is rotatably mountable on the smaller cylindrical bearing surface of the barrel insert retainer shaft 34 between the steps or shoulders formed by the larger shaft 16 and the larger end portion 38 of the barrel insert retainer shaft 34 . The space between the shoulders allows the barrel insert to freely rotate with the rifling in a gun barrel to facilitate insertion of the barrel insert 15 into the gun barrel and to prevent the sharp edges of the barrel rifling from shaving off bits of the barrel insert. Each one of the cylindrical barrel inserts 41 - 47 corresponds to a particular gun-barrel caliber. Barrel insert 41 is used for a 0.22 caliber, 0.223 caliber, or 5.36 mm. gun barrel. Barrel insert 42 is used for a, which extends 0.270 caliber or 7 mm. gun barrel. Barrel insert 43 is used for a 0.30, 3006, 308, or 7.62 mm. gun barrel. Barrel insert 44 is used for a 0.38 caliber, 0.357 caliber, or 9 mm. gun barrel. Barrel insert 45 is used for a 0.40 caliber or 10 mm. gun barrel. Barrel insert 46 is used for a 0.44 caliber or 0.45 caliber gun barrel. Barrel insert 47 is used for a 0.50 caliber gun barrel.
The barrel inserts 41 - 47 are precision machined from a black acetal material. Acetal material, trademarked a Delrin®, is a crystalline thermoplastic polymer with a high melting point which provides a high modulus of elasticity combined with great strength, stiffness and resistance to abrasion. It provides dimensional stability for fabrication of close tolerance items. It has a low coefficient of friction, excellent machinability, good impact and abrasion resistance, and natural lubricity. The barrel inserts are machined from this flexible, resilient, tough, durable material. Acetal provides good slip characteristics over the steel material of a gun barrel without being deformed or marring the gun barrel or rifling. The barrel inserts are slightly oversized to accommodate worn, oversized gun barrels.
Instead of using the cylindrical barrel insert 41 for a 0.22, 0.223, or 5.56 mm. gun barrel, external threads 50 of an alternative metal spring barrel insert 52 are threaded into the internally threaded bore 30 of the shaft 16 .
FIG. 4A, FIG. 4 B and FIG. 4C illustrate in greater detail an exemplary embodiment of one type of typical barrel insert 42 for a smaller caliber gun barrel, such as a 0.270 caliber or 7 mm. gun barrel. The barrel insert 42 has two integral coaxial cylindrical symmetric sections, including a cylindrical base 60 and an attached radially resilient end section 62 . The cylindrical base 60 rotatably mounts the barrel insert 42 to the end of the shaft 16 while the attached radially resilient end section 62 resiliently positions the axis of the end of the shaft 16 coaxially along the longitudinal axis of the gun barrel.
For this exemplary embodiment of a barrel insert, the cylindrical base 60 has a central bore 66 formed therein with an internal diameter D 1 of 0.148+001−0.000 inches. To provide precision rotation of the barrel insert 42 around the retainer shaft 34 , the interior wall defined by the central bore 66 in the section 60 engages the bearing surface 36 of the barrel insert retainer shaft 34 , where the bearing surface 6 of the retainer shaft has a diameter of 0.148+/−0.0005 inches. The smaller external diameter D 2 of the base section 60 is 0.246 inches to accommodate the 0.270 inch diameter of the gun barrel bore.
The external diameter of the radially resilient end section 62 increases from the 0.246 inches of the external diameter D 2 of the base 60 to a peaked cylindrical ridge area 64 which has a maximum diameter D 3 of 0.274 inches. The external diameter of the radially resilient end section 62 then tapers back down to a diameter D 5 , which is the same as the smaller diameter D 2 of the base 60 . The outer end of the resilient end section 62 has an internal bore 70 formed approximately half way through with a diameter D 4 of 0.160 inches. The inner portion of the end section 64 has an internal bore formed therein which decreases in diameter from diameter D 4 to diameter D 1 .
When the barrel insert 42 is positioned in the gun barrel for rotation about the longitudinal axis of the barrel insert retainer shaft 16 , the interior walls of the main cylindrical section 60 of the barrel insert 42 snugly engage the cylindrical bearing surface 36 of the barrel insert retainer shaft 34 to provide precise rotation of the barrel insert 42 . Note that the interior surface of the bores in the end section 64 do not engage the bearing surface 36 of the barrel insert retainer shaft 16 .
When the barrel insert 42 is inserted into the 0.270 diameter gun barrel, the external surface of peaked cylindrical ridge area 64 with the maximum diameter D 3 of 0.274 inches contacts the wall of the gun barrel and is pushed radially inwardly to conform to the smaller 0.270 diameter of the gun barrel. In this manner, the external contact area of the peaked cylindrical ridge area 64 of the barrel insert 42 snugly engages the wall of the gun barrel to precisely coaxially position the one end 24 of the shaft 16 within the gun barrel 14 along the longitudinal axis of the gun barrel.
The smooth cylindrical surface of the peaked cylindrical ridge area 64 of the barrel insert 42 provides continuous contact with the inner wall of the gun barrel in spite of the rifling grooves formed in the gun barrel. The tough black acetal material of the barrel insert 42 does not damage the interior surface or the rifling of the gun barrel.
FIG. 5A, FIG. 5 B and FIG. 5C illustrate in greater detail another embodiment of a barrel insert for a larger caliber gun, i.e., the barrel insert 47 for a 0.50 caliber gun barrel. The barrel insert 47 includes two cylindrically symmetric, coaxial, and partially concentric sections including a main cylindrical section 80 with smaller internal and external diameters and a radially resilient cantilevered section 82 with larger internal and external diameters. The main cylindrical section 80 has a central bore 86 formed there through with an internal diameter D 10 of 0.148+001−0.000 inches to provide precision rotation of the barrel insert 47 around the retainer shaft 34 . The interior wall defined by the central bore 86 in the section 80 engages the bearing surface 36 of the barrel insert retainer shaft 34 , where the bearing surface 34 of the retainer shaft has a diameter of 0.148+/−0.005 inches. The external diameter D 11 of the main cylindrical section 80 is 0.246 inches to clear the wall of a 0.500 caliber gun barrel.
The radially resilient cantilevered section 82 is formed integral with the main cylindrical section 80 and includes an integral radially outwardly extending support flange section 84 from which longitudinally extends an integral cantilevered resilient ring 86 . The support flange 84 has an outside diameter which steadily increases from the external diameter D 11 to a diameter D 12 which is 0.470 inches. The integral cantilevered resilient ring 86 increases in diameter to a peaked cylindrical ridge area 88 which has a maximum diameter D 13 of 0.502 inches. The external diameter of the integral cantilevered resilient ring 86 then tapers back down to a diameter D 14 , which is the same as D 12 . The integral cantilevered resilient ring 86 is spaced apart from the main cylindrical section 80 by having a ring-shaped open space 87 formed beneath it to allow the cantilevered resilient ring 82 to flex inwardly.
When the barrel insert 47 is guided into a 0.500 diameter gun barrel, the external surface of peaked cylindrical ridge area 88 with the maximum diameter D 13 of 0.502 inches contacts the wall of the gun barrel and is pushed radially inwardly to conform to the smaller 0.500 diameter of the gun barrel. In this manner the external contact area of the peaked cylindrical ridge area 88 of the barrel insert 47 snugly engages the wall of the gun barrel to precisely position the proximate end 24 of the shaft 16 within the gun barrel 14 along the longitudinal axis of the gun barrel. The smooth cylindrical shape of the barrel insert peaked cylindrical ridge area 88 provides smooth contact with the inner wall of the gun barrel in spite of the rifling grooves formed in the gun barrel. The tough material of the barrel insert 47 does not damage the interior surface or the rifling of the gun barrel.
FIG. 6 A and FIG. 6B illustrate an alternative metal spring barrel insert 52 for a gun having a small caliber such as a 0.22, 0.223, or 5.56 mm caliber. The spring barrel insert 52 is formed of a rod-shaped body having a diameter of 0.210 inches. External threads 100 are formed at one end of the spring barrel insert 52 for engagement with the internal threads of the bore 30 formed in the one end 24 of the shaft 16 . A longitudinal bore 102 is formed through the other end of the spring barrel insert 52 and three evenly spaced longitudinal slots 104 , 105 , 106 are formed along part of the length of the spring barrel insert to provide flexible longitudinally extending prongs 108 , 109 , 110 . A 0.093 chrome-plated ball 112 is pressed between the prongs to expand the prongs to fit within the barrel of a 0.22, 0.223, or 5.56 mm caliber gun.
FIG. 7 illustrates the various components assembled on the distal end 26 of the shaft 16 of the laser precision bore sight assembly 10 . A bore in the narrow end of the coaxial alignment cone 18 is press fit onto the end of the shaft 16 , where the coaxial alignment cone 18 provides for coaxial alignment of the distal end of the shaft 16 with the distal end of various different caliber gun barrels.
The other larger, distal end of the coaxial cone 18 has an externally threaded stud 118 formed thereon which engages corresponding internal screw threads formed in the proximate end of the battery/switch housing 20 . A battery 120 is contained in a central cavity formed between the distal end of the battery/switch housing 20 and the proximate end of the coaxial laser housing 22 . Internal screw threads 124 in the battery/switch housing 20 engage corresponding external threads 126 formed in the proximate end of the laser housing 22 . Rotation of the laser housing 22 with respect to the battery/switch housing 20 causes a positive terminal of the battery 120 to activate a switch in the battery/switch housing 20 .
The laser housing 22 contains a laser subassembly 122 having a laser source and collimating lens to provide a collimating laser beam which is coaxially aligned along the axis of the gun barrel. Adjustments to the alignment of the laser beam are made with a 3-point adjustment system which includes a pair of windage/elevation adjustment assemblies 127 a, 127 b and one fixed adjustment screw mechanism 128 . A front cap and lens assembly 130 fixed to the end of the laser housing covers the laser subassembly 122 .
FIGS. 8 and 9 illustrate in more detail the battery/switch housing 20 and its contents. The battery/switch housing 20 includes an internally threaded axial bore 132 formed at one end for engagement with the externally threaded stud 118 on the distal end of the coaxial cone 18 shown in FIG. 7. A preferred embodiment has the battery/switch housing 20 and the laser housing 22 made of aluminum. The exterior surfaces of the aluminum battery/switch housing 20 and the laser housing 22 are anodized. All of the threaded surfaces and the interior surfaces are not anodized to facilitate electrical conduction. The distal end of the battery/switch housing 20 includes an innermost cylindrical cavity 134 for containing the components of a switch assembly 136 . The switch assembly 136 includes a compression spring 138 which is contained in the cavity 134 and which has flattened ends. A cup-shaped fiber washer 140 with a counter bore is contained in the cavity 134 and has a center bore 142 formed therethrough for receiving the threads of a contact pin, 144 such as a flat-head brass screw or a smooth pin. The flat-head brass screw 144 has a conical head 146 at one end and an end contact surface 148 at the other end. Solder covers the top surface of the conical head 146 the contact pin is fixed to the fiber washer 14 by being soldered to a nickle-plated washer 149 on the side of the fiber washer 140 opposite the head of the pin 144 .
The compression spring 138 is contained within the cavity 134 and pushes against the inside peripheral surface of the fiber washer 140 . The fiber washer 140 is held inside the cavity 134 with a C-ring retainer which is locked into a circumferential groove 148 formed in the wall of the cylindrical cavity 134 . When the compression spring 138 is extended so that the outside edge of the fiber washer 140 contacts the inside surface of the C-ring retainer, the far end 148 of the flat-head screw 144 does not contact the interior end wall 154 of the cavity 134 .
The external threads 126 of the laser housing 22 engage the internal threads 124 of the battery/switch housing 20 . Rotation of the screw threads of the laser housing 22 into the screw threads of the battery/switch housing 20 causes the positive terminal 160 of the battery 120 to push against the top 146 of the screw 144 to compress the compression spring 138 such that the end surface 148 of the screw 144 contacts the aluminum surface of the interior end wall 154 . This connects the positive terminal 160 of the battery 120 to the aluminum housing 20 . Rotation of the battery and switch housing 20 in the opposite direction with respect to the laser housing 22 causes the compression spring to extend such that the far end 148 of the flat-head screw 144 or contact pin does not contact the interior end wall 154 of the cavity 134 . This breaks the connection of the positive terminal 160 of the battery 120 to the aluminum housing 20 .
FIGS. 10 and 11 illustrate the body of the laser housing 22 . The distal end of the laser housing 22 has a longitudinal central bore 170 formed therein for receiving the cylindrical body of the laser subassembly 122 shown in FIG. 7 . As described herein below, alignment of the laser beam in the laser subassembly 122 is provided using a three-point alignment mechanism which is mounted to the laser housing 22 . The external surface of the distal end of the laser housing 22 has two orthogonal external flat-surfaced dovetailed keyways 172 , 174 formed thereupon for receiving corresponding dovetailed bases of two windage/elevation adjustment assemblies 176 , 178 . The windage/elevation adjustment assemblies 176 , 178 are fixed to the laser housing with bonnet screw threads 180 , 182 . Each bonnet screw thread 180 , 182 screw passes through a respective threaded aperture 184 , 186 in the laser housing 22 such that the ends of respective adjustment screws (not shown) for each windage/elevation adjustment assembly contact the laser subassembly 122 for alignment of the laser beam. One adjustment screw is aligned for movement in a first direction perpendicular to the longitudinal axis of the shaft. A second adjustment screw is aligned for movement in a second direction perpendicular to the longitudinal axis of the shaft and also orthogonal to the first direction of movement of the one adjustment screw.
FIG. 11 also illustrates a third element of the three-point alignment mechanism for the optical assembly which is a spring-loaded fixed screw assembly 190 . The spring-loaded fixed screw assembly 190 is screwed into position in a threaded aperture in the laser housing 22 opposite the adjustment screws and at equal obtuse angles with the directions of the adjustment screws to bias the laser subassembly 122 against the ends of the first and the second adjustment screws.
FIG. 12 illustrates a typical windage/elevation adjustment assembly, which includes an adjustment screw 192 , a cap 194 , a bonnet 196 , and a fine adjustment retainer ring 198 . Waterproofing of the windage 1 elevation adjustment assembly is accomplished with a first O-ring 200 which engages a circumferential slot 201 formed in the bonnet 196 and a second O-ring 202 which engages another circumferential slot 203 formed in the bonnet 196 . Each one of a pair of springs 204 , 205 outwardly biases a respective ball of a pair of 1.5 mm. stainless steel balls 206 , 207 .
FIG. 13 shows that the adjustment screw 192 has external threads 210 formed on its midsection with a slot 212 through its upper end. The adjustment screw 192 includes an end contact surface 215 at its bottom end for contact with the laser subassembly 122 . The external threads 210 of the adjustment screw 192 do not extend to the bottom end of the adjustment screw, which provides an unthreaded, smooth side surface 215 at the lower end of the adjustment screw 192 . FIG. 14 shows that the cap 194 has a cupped body 216 with a centrally located depending rectangular tang 218 which engages the slot 212 in the upper end of the adjustment screw.
FIGS. 12, 15 A, and 15 B show the bonnet 196 with the external threads 800 which are formed on its lower end and which are then threaded into one of the threaded apertures 184 , 186 of the laser housing 22 to anchor the windage/elevation adjustment assemblies 176 , 178 in place. The O-ring 202 in slot 203 provides a water seal between the bonnet and the laser housing. The external threads 210 of the adjustment screw 192 engage internal threads 222 in the bonnet 196 for relative movement of the contact surface 215 at the end of the adjustment screw 192 against the laser subassembly 122 . A horizontal screwdriver slot 221 across the top of the bonnet 196 is used to screw the bonnet 196 to the laser housing 22 . The bonnet has a pair of opposing horizontal radial slots 224 , 226 formed near its top end for containing one of the springs 204 , 205 , which outwardly bias the steel balls 205 , 206 .
FIGS. 12 and 16 show the fine adjustment retainer ring 198 with a number of pairs of opposing recesses, typically shown as 230 , formed near the top of its inside surface. The fine adjustment retainer ring 198 fits around the bonnet 196 . After assembly of the windage/elevation adjustment assembly, an external cylindrical surface of the retainer ring 198 is press fit inside an inner cylindrical surface of the cupped body 216 of the cap 194 . Each of the springs 204 , 205 is retained in one of the slots 224 , 226 and biases one of the pair of steel balls 206 , 207 into engagement with one of the recesses 230 to provide detented or indexed fine adjustment steps for the adjustment screw 192 as the cap 194 is rotated. A water seal protecting the threads of the screw 192 against moisture is provided with the O-ring 200 which is in the slot 201 of the bonnet and which engages an inside circumferential surface 232 in the retainer ring 198 .
FIG. 17 illustrates a base 240 for a windage/elevation adjustment assembly The side edges and the rounded front edge of the base are dovetailed and are received in one of the dovetailed keyways 172 , 174 formed on the laser housing 22 . A through hole 242 accommodates a windage/elevation adjustment assembly and a recessed ring 244 accommodates the cap 194 .
FIG. 18 illustrates the spring-loaded fixed screw assembly 190 which includes a set screw 250 which is screwed into a threaded aperture 260 in the laser housing 22 . A spring 262 is located between the inner end of the screw 250 and a cup-shaped cap, or bushing, 264 which contacts the surface of the laser to bias the laser subassembly 122 against the first and the second adjustment screws 180 , 182 .
FIGS. 19 and 20 illustrate the components of the laser subassembly 122 , which include a hollow pear-shaped laser heatsink 270 which contains a laser diode assembly 272 and an associated circuit board 274 that is soldered to three pins on the laser diode assembly. A disk module 276 is a laminated circuit board with a gold-plated copper layer and apertures which are typically formed therethrough to allow passage of wires 280 , 281 . The space 284 connects to the negative terminal of the battery. The components of the laser subassembly 272 are fixed in position by encapsulation with a block 282 of an epoxy material. The distal end of the laser heatsink 270 contain a lens 290 attached to an end plug 292 , which is adjusted to collimate a laser beam from the laser diode assembly 272 .
A rounded proximate end 294 of the pear-shaped laser heatsink 270 has the largest diameter and is dimensioned to provide a friction fit with a corresponding inner surface of the laser housing 22 . An O-ring 296 is located adjacent to a step 298 at the midsection of the pear-shaped laser heatsink 270 .
FIGS. 21 and 22 illustrate a structural arrangement which provides for three-point adjustment of the laser beam from the laser source in the pear-shaped laser heatsink 270 . The inner surface 299 of the laser housing 22 is shaped to provide a close friction fit with the rounded end 294 of the pear-shaped laser housing 294 . This structural arrangement allows precise pivotal movement of the distal end of the laser module 122 as illustrated in FIG. 11 with the three-point alignment produced by the two windage/elevation adjustment assemblies 176 , 178 and the spring-loaded fixed screw assembly 190 . This allows precise alignment of and orients the laser beam along the axis of the precision bore sight assembly 10 and along the bore of a gun barrel. FIG. 22 shows that the unthreaded, smooth side surfaces 215 at the lower end of the adjustment screws 192 contacts the forward side of the O-ring 296 and compresses the O-ring 10 to 20 per cent to provide friction loading on the ends of the adjustment screws.
FIGS. 23 and 24 illustrate an optional lens assembly 300 which includes an end cap 302 and a lens 304 is an exploded, partially sectional view of a front cap and lens. FIG. 22 is a sectional view of an assembled front cap and lens assembly.
Another embodiment of a different coaxial laser housing is provided where the windage and elevation settings for a bore sight assembly are initially made with set screws which are then sealed with a locking adhesive. This allows a bore sight assembly to be prealigned at, for example, a factory or a service location. A modified coaxial laser housing is provided which is similar to the housing 22 , but which is smaller in diameter and does not have dovetailed sections for mounting manual adjustment assemblies. Bores for the windage and elevation set screws are provided which correspond to the orthongonally aligned bores 184 , 186 but which are smaller in size to directly receive the fixed adjustment screws without a bonnet. A plunger biasing assembly, similar to the plunger assembly 190 is also used. The fixed adjustment screws and the plunger assembly are locked in position with a suitable locking material.
Note that the bore sight assembly according to the invention is useful for sight alignment of optical scopes, mechanical firearm sights, and laser sighting devices. The bore sight assembly according to the invention is also useful for simulating alignment and firing of a weapon use in a firearms training system.
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 teachings. 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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A laser precision bore sight assembly and method aligns a laser beam along the longitudinal axis of a gun barrel. At the proximate end of an elongated bore shaft is rotatably mounted a compressible barrel insert with a continuous outer surface which resiliently engages the inside wall of the gun barrel to coaxially align the longitudinal axis of the proximate end of the shaft with the longitudinal axis of the gun barrel. The exterior surface of an alignment cone is provided on the distal end of the bore shaft. A battery/switch housing, containing a switch assembly, cooperates with a laser housing assembly to provide an enclosure for a battery. A laser source in the laser housing assembly provides a laser beam in a direction coaxial with the longitudinal axis of the shaft. Matching threads provide for relative longitudinal movement such that a terminal of the battery engages the switch assembly to activate the laser source. The compressible barrel-shaped insert is a cylinder formed of a machined acetal material. Different sizes of compressible barrel inserts are provided for different gun-barrel calibers. A three point laser alignment mechanism directs the laser beam along the longitudinal axes of the shaft and the bore of the gun barrel, even when the shaft is rotated. The invention also provides a method for aligning a laser beam along the longitudinal axis of the bore of a gun barrel.
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RELATED APPLICATIONS
This application is a Division of application Ser. No. 13/573,061 filed Aug. 17, 2012.
BACKGROUND OF THE INVENTION
Field of the Invention
Normal hydrocarbon well perforating operations require shutting down radio frequency (RF) transmitters and eliminating stray voltage sources before arming explosive equipment such as perforating guns at the surface of an oil or gas well. The exception is for certain qualified high voltage initiators as recommended by the American Petroleum Institute (API Recommended Practice 67 (RP67), 2 nd Edition, 2007) where explosive preparations are allowed in the presence of uncontrolled external voltages. High voltage initiators (HVI) include devices that utilize exploding foil initiation (EFI) and exploding bridge wire (EBW) as the as the initiating elements. An HVI that uses an semi-conductor bridge (SCB) is safer than a hot-wire detonator but more restrictive than HVIs using EFIs and EBWs.
These technologies were adapted for downhole during the last two decades. The first commercial EFI device for downhole use is described in U.S. Pat. No. 5,088,413 by Huber et al. The efficiency of such devices is determined in part by the overall inductance of a current loop that connects a capacitor, a switch and an EFI or EBW. One simple version was designed in the 1980s by Meyers, Application of Slapper Detonation Technology to the Design of Special Detonation Systems, Los Alamos Report LA-UR-87-391 that used a two conductor flexible cable that incorporated a small hole in the flex cable that served as a barrel between the EFI and the explosive pellet. The capacitor, switch, EFI and flex cable with a hole, used as an EFI infinite flyer barrel, were all part of the same current loop that reduced total resistance and inductance. This concept was followed in the presentation of Lerche and Brooks, “Efficiencies of EFI Firing Systems,” 43 rd NDIA Fuze Conference, April, 1999.
The present high voltage devices for downhole explosive detonations are physically larger than conventional low voltage detonators (commonly called hot-wire detonators that utilize primary explosive), which normally have a slim profile. Low voltage detonators typically are about 0.3-inch diameter and less than 3 inches long. One advantage in using a low voltage detonator is afforded by its small size which allows its insertion into a perforating gun or firing head housing sub-assembly through a relatively small port plug, typically 13/16-inch or 1⅜-inch diameter, permitting easy attachment outside the gun housing of the detonator to the wireline and then to the detonating cord, for example, before inserting the armed detonator back through the port plug hole into the gun housing. High voltage devices, on the other hand, typically do not fit through port plug openings, requiring insertion through one end of a separate arming sub or a special sub, for example, making the arming operation more difficult and adds cost and preparation time at the job site.
A high-voltage device that fits through a port plug opening is needed to reduce cost, improve reliability and improve well-site safety and efficiency. Added safety is afforded by a feature that only allows electrical power to initiate the device by sending a prescribed activation signal.
SUMMARY OF THE INVENTION
The present invention disclosure describes an assembly for initiating explosives downhole using an exploding foil initiator, consisting of an input power supply, a flexible electrical link, a capacitor discharge unit and a secondary explosive transfer to a detonating cord. In one version, the explosive is initiated in a direction approximately parallel to the capacitor discharge unit and in another version the explosive is initiated in a direction approximately perpendicular to the capacitor discharge unit. The unique configurations and construction of the assembly allow installation through a small port plug hole in the gun housing structure for more efficient gun arming.
BRIEF DESCRIPTION OF THE DRAWINGS
The advantages and further features of the invention will be readily appreciated by those of ordinary skill in the art as the same becomes better understood by reference to the following detailed description when considered in conjunction with the accompanying drawings in which like reference characters designate like or similar elements throughout.
FIG. 1 schematically shows a well perforating gun operating assembly with a wireline cable and detonator.
FIG. 2 is a sectional view of a prior art high voltage initiator.
FIG. 3 a is a block diagram of a first invention embodiment.
FIG. 3 b is a block diagram of a second invention embodiment
FIG. 4 is a flow chart of the present invention arming procedure
FIG. 5 is a preferred voltage multiplier schematic with low impedance shunt
FIG. 6 is a flyback concept for stepping up the input voltage with the addition of low impedance shunt.
FIG. 7 a is a first preferred invention embodiment showing a capacitance discharge unit configuration corresponding to FIG. 3 a.
FIG. 7 b is a second preferred invention embodiment showing a capacitance discharge unit configuration corresponding to FIG. 3 b.
FIG. 8 a is another preferred invention embodiment showing a capacitance discharge unit configuration corresponding to FIG. 3 a.
FIG. 8 b is another preferred invention embodiment showing a capacitance discharge unit configuration corresponding to FIG. 3 b.
FIG. 9 is an explosive transfer holder schematic.
FIG. 10 is a block diagram that shows modified circuit to permit powering with an activation signal from the surface.
FIG. 11 is a schematic that show a circuit that detects downhole voltage and uplinks real time downhole measured voltages.
FIG. 12 is a signal format for uplink signal pulses corresponding to FIG. 11
FIG. 13 is an alternative embodiment of FIG. 11
FIG. 14 is a signal format for uplink signal pulses corresponding to FIG. 13
FIG. 15 is a circuit schematic for integrating a voltage detector with a detonator having a voltage multiplier as part of its power supply.
FIG. 16 is a schematic for one embodiment of the overall assembly detonator.
FIG. 17 is a circuit schematic of the CDU with separate flexible cable containing an EFI
FIG. 18 a shows a CDU where the spark gap and bleed resistor are mounted on the capacitor with a separate flexible cable with EFI aligns vertically
FIG. 18 b shows a CDU where the spark gap and bleed resistor are mounted on the capacitor with a separate flexible cable with EFI aligns horizontally
DESCRIPTION OF THE PREFERRED EMBODIMENTS
In a typical wireline perforating operation, the perforating gun 10 is lowered into a well by way of an electrical cable 12 to position the gun at the desired portion in the reservoir ( FIG. 1 ). Conveyance from a truck-mounted reel 14 may be by means of gravity, by fluid pressure, by pushing the gun with small-diameter tubing, or by pushing the gun down with a downhole tractor. Once the gun is positioned at the specified depth, electrical detonation power 16 connected to the cable by means of a wireline cable connector 20 to “fire” the gun by powering a detonator 11 . “Firing” of the gun is represented by the detonation of specialized high explosives such as shaped charges that are radially aligned in the gun housing to produce holes in the well casing and/or reservoir to allow a flow of in situ hydrocarbons from the surrounding formation into the well.
In prior art low voltage perforating operations using hot wire detonators with primary explosive, typically with 50 Ohm input resistance, the shooting power supply 16 produces sufficient voltage, in the range of 10V to 50V at the input of the detonator, to directly initiate these types of explosive devices. However, electro-explosive initiators such as EBW (exploding bridge wire) and EFI (exploding foil initiator) detonators require a discharge voltage in the range of 1000V to 3000V for reliable initiation of a secondary explosive. Because most power supplies are limited to below 500V output, it becomes necessary to provide an integral step-up voltage power supply downhole for the EBW and EFI type detonators.
A basic configuration of such a prior art EFI detonator as described by U.S. Pat. No. 6,752,083 by Nolan C. Lerche et al, is represented by FIG. 2 , and may be composed of three sections: circuitry 22 to boost downhole voltage (first section), a capacitor discharge unit (CDU) 24 (second section) and an explosive housing 26 (third section) which includes a small explosive pellet 112 . A support structure 100 consolidates and houses the cooperative components of the first and second sections. An electric cable connector 104 connects a power source 16 to the active elements of the voltage multiplier circuit 22 within the support structure. A bore 162 within the explosive housing is sized to receive a booster explosive 164 proximate of the explosive pellet 112 . In intimate contact with the booster 164 , the end of a detonating cord 166 is clamped within the bore 162 by a threaded collet mechanism 168 .
The prior art example shown by FIG. 2 is of a typical EFI detonator device typically assembles the three sections 22 , 24 , and 26 in rigid alignment along a common axis making a total length of about 5 inches or greater which is too long to fit through the gun housing service ports of most gun systems. Sections 22 and 24 contain close-coupled, high voltage electronic components that are arranged on the same circuit support structure which determines in large part the overall length of the assembly, making it impossible to fit the detonator through a small port plug hole of most guns.
The present invention, represented schematically by FIGS. 3 a and 3 b are the embodiments of designs that overcome the length disadvantage of prior art such as that of FIG. 2 . In its simplest form, the present invention also has three sections including the voltage multiplier section 30 , a capacitive discharge unit coupled to an EFI 32 and an explosive housing 34 which contains one or more small explosive pellets 164 ( FIG. 9 ), where sections 32 and 34 are rigidly attached. Distinctively, the voltage multiplying section 30 and the capacitive discharge section 32 are joined by a short section of flexible electrical link 36 about 1 inch in length, for example, capable of carrying high voltage. The prior art contained its electronics on a flex cable for single unit assembly. A flex cable is unnecessary for the section 30 because, unlike section 32 , there is no need for low inductance for the voltage step-up section. Moreover, a sturdy circuit board is more robust for handling.
In one version of the invention, FIG. 3 a , the explosive housing section 34 is physically angled relative to the capacitive discharge section 32 a . The flexible link 36 allows the first section 30 to pivot relative to the second section 32 a while maintaining electrical connection through two wires. The width (less than 0.70 inch) of the two sections 30 and 32 a is less than the 13/16-inch diameter opening of a standard perforating gun service port, and fits easily through the opening. The individual lengths of the two sections 30 and 32 a are less than the allowed clearance inside a small diameter 2⅞ inch gun, for example, and are easily placed inside the gun section through a standard service port. By the third section being angled approximately perpendicular to the second section, it too, fits easily inside the gun section, after it is affixed outside the gun to a booster that is connected to flexible detonating cord.
FIGS. 3 b and 16 show another embodiment of the invention that is suited for larger service ports, such as the common 1⅜-inch diameter port plug used with a small diameter 2⅞ inch gun. The capacitive discharge section 32 b is in-line with the explosive housing 34 . The larger diameter service port allows easy insertion of an in-line 34 and 32 b with flexible link 36 and voltage multiplier 30 following.
Partitioning the rigid voltage multiplier section 30 from the rigid unit of sections 32 and 34 is the simplest configuration of the invention and the presently preferred embodiment. However, three or more rigid sections with pivoting electrical connections is also possible, and would allow for more electronic features to fit through a service port.
A flow chart of the loading procedure is given in FIG. 4 . A typical loading procedure at the well site would have the assembly of FIG. 3 a or 3 b connected to wireline wires that have been routed from inside of the gun through the service port hole. The electrical connection is normally done with the assembly inside a safety tube to prevent bodily injury in case of accidental firing. After the electrical connection is made, the end of the detonating cord, also routed through the service port from inside the gun, is capped with a booster-shelled explosive, inserted into the explosive housing section 34 and secure by a collet clamp. Once the assembly is attached to the booster/detonating cord, the linking cord and explosive housing section of the assembly is inserted through the port plug and rotated until sections 34 and 32 are inside the gun section. Finally, section 30 and its connection wires are inserted, enabled by the flexible link that allows section 30 to pivot relative to section 32 . The port plug is then secured to the gun section.
A more detailed description of alternative embodiments of a voltage multiplier and accompanying electronics 30 is shown by FIGS. 5 and 6 . The electronic components are mounted on a hard circuit board. Two input wires 104 A and 104 B are attached to the board and used to make electrical connection to the wireline 12 . A commutating diode allows only positive voltage to power the circuit. A flexible link 36 unsupported by the board attaches to the output side and connects to section 32 . In one embodiment, the link is composed of two short wires; in another embodiment, the link connects to the second section 32 by an unsupported flexible cable.
A unique feature of the FIGS. 5 and 6 embodiments is the inclusion of a low-impedance shunt 31 that is electrically in parallel with the input wires, and having a value in the range of 10 to 500 Ohms, for example, 50 Ohms. For low voltage applications, the first section 30 presents low input impedance onto the wireline. At higher voltages the low impedance shunt 31 opens or maintains a constant current load, presenting higher input impedance for section 30 at higher input voltages. Existing high-voltage detonators have high input impedance, typically between 2,000 and 50,000 Ohms, depending on the device. The resulting charging current is therefore much smaller than that presented to a 50 Ohm hot-wire detonator, for example. The lower current typical for high-voltage detonators makes it difficult to detect the presence of these types of detonators by monitoring current change at the surface when they are switched onto the wireline. The low impedance shunt 31 allows current to be more easily detected at the surface at low voltages during normal firing sequences, as is now common for conventional hot-wire detonators with 50 Ohm resistance. This shunt feature is particularly advantageous when using electronic downhole switches with the present invention to detect a failed or shorted downhole electronic switch when used with high voltage detonators. Some typical electronic downhole switches are described in U.S. Pat. No. 6,283,227 by Lerche et al and U.S. Patent Publication No. 2011/0066378 filed Nov. 3, 2010 by Lerche et al.
One embodiment of a low-impedance shunt is a fusing resistor. Another embodiment would be a depletion mode field effect transistor (DFET) in series with a 50 Ohm resistor, as an example. The DFET and series 50 ohm resistor is again placed in parallel with the input wires of the detonator. A current sense resistor also in series with the DFET and limits the current through the DFET to a predetermined level.
There are other embodiments where a high voltage, high impedance detonator presents a low impedance with low wireline voltages typical during downhole communication of electronic perforating switches. The low impedance shunt can be part of the electronic switch or anywhere between the switch and the detonator.
Two embodiments of the present invention second section 32 are represented schematically by FIGS. 7 a and 8 a and correspond to FIG. 3 a (perpendicular alignment with section 34 ). A CDU circuit including a ceramic capacitor 42 and switching component 44 (spark gap) mounted on a thin, low inductance flex cable, which may or may not include a more rigid composite section. The circuit is supported along a rigid mechanical support 40 underneath. In one embodiment, a controlled gap 48 of between 0.005-0.015 inches separates the top of an EFI 46 and the bottom of an explosive pellet 50 , The FIG. 7 a embodiment engages a small insulated spacer 52 between the EFI 46 and the explosive pellet to control the gap 48 spacing. In the FIG. 8 a embodiment, the control gap 48 is a perforation in the flexible cable and support structure between the EFI 46 and the explosive pellet 50 abutting the flexible cable/support structure 40 .
It is clear to one skilled in the art that other electro-explosive initiators besides an EFI can be used, such as an EBW or an SCB.
Two other embodiments of the present invention section 32 are represented schematically by FIGS. 7 b and 8 b and correspond to FIG. 3 b (parallel alignment with section 34 ). Here the rigid support 40 only supports the low inductance cable up to the EFI 46 , allowing that portion of the cable to be bent as shown.
Two more embodiments of the present invention section 32 are shown in FIG. 18 which uses a portion of the structural surface of the firing capacitor 42 as an substrate for supporting the bleed resistor 41 and the switching component 44 , all in an integrated CDU (see FIG. 17 for circuit schematic). Advanced Monolythic Ceramics, for example, offers such construction. This eliminates the need for the cable support 40 . A separate section of flexible cable, such as a ribbon cable, 43 with an EFI 46 is soldered to the firing capacitor surface to attach the CDU to the initiator element. The flexible cable with the EFI is coupled, in turn, to the explosive section 34 as in FIG. 3 a and FIG. 18 a . or when after bending as in FIG. 3 b and FIG. 18 b.
The most common cause of perforating fatalities is the accidental application of power to the detonator at the surface. Sending and correctly detecting an activation signal at the detonator before firing provide an extra degree of safety. An embodiment of the voltage multiplier section 30 is shown in FIG. 10 that adds this extra margin of safety. FIG. 10 differs from FIGS. 5 and 6 by the inclusion of a receiver and microprocessor for one-way communication from the surface tool control computer 18 ( FIG. 1 ) to the voltage multiplier section 30 of the detonator. A low voltage is applied at the surface to energize the power supply 35 . Next, a downlink activation signal is received and processed by the microprocessor using FSK communication. The microprocessor verifies that it has received the correct activation signal and only then allows the internal high voltage power supply to activate. Finally, shooting voltage is applied at the surface to complete the firing sequence, making for safer operations.
FIG. 11 is a schematic of an additional feature for the detonator that detects downhole voltage and then uplinks real time voltage levels to the surface computer 18 . The voltage detect feature is on a separate circuit board in front of the voltage multiplier 30 ( FIG. 5 and FIG. 6 ), but could also be incorporated as part of section 30 on a common board as depicted in FIG. 3 and schematically shown in FIG. 15
Referring to FIG. 11 , the downhole voltage level is detected and the resulting analog signal is sent to an ND input of a microprocessor. The microprocessor then sends a digital signal to the surface computer 18 in the form of a current induced signal that rides on top of the shooting power supply voltage 16 , known as current loop power line carrier. At the surface, a current viewing resistor (CVR) is placed in series with the wireline in order to detect the current deflection. This signal is then processed and the results are displayed in a plot format or as a digital value. The detector unit would automatically send a series of pulses at a selected predetermined interval.
One type of uplink signal is a binary weighted Manchester represented by FIG. 12 . When surface power supply (SPS) voltage is detected downhole, a 3 bit preamble, 3 null bits and 8 bit data word is sent uplink as a power line carrier on top of the SPS voltage using the Manchester format. The bit rate can be chosen to give reliable uplink detection for a given wireline resistance and capacitance values. Typically a 100 bits/sec would work for all wirelines. The downhole signal would be an induced current in the range of (10-100) ma. Using an 8 bit word, the advantage is a high resolution signal.
In another embodiment variation of FIG. 11 , the FIG. 13 embodiment provides a series of diodes, each with a different breakdown voltage. As the downhole voltage from the power supply 16 increases, sequential signals are sent to a microprocessor which tracts the number of such signals. Each time a signal is detected a designated pulse sequence corresponding to the particular voltage is transmitted up the wireline and recorded at the surface by a computer 18 . The presence of the detonator is confirmed by monitoring these received signals and the last signal corresponding to the last voltage change gives an approximation to the firing voltage of the detonator. Unless there are special provisions, whenever an electronic perforating switch is integrated into a high voltage detonator there is no surface feedback indicating that the detonator is functioning. Instrumentation of the following two methods would provide surface status for operation of a high voltage detonator.
A simple method for the uplink corresponding to FIG. 13 is shown in FIG. 14 . A series of pulses is uplinked, each pulse having a predetermined weighted value. As an example each pulse could represent 50 volts, and 3 pulses would indicate 150 volts. The disadvantage is that the resolution is not as precise while the advantage would be to only count pulses at the surface.
The third section 34 of the invention assembly as schematically illustrated by FIG. 9 attaches the output side of the explosive pellet 50 to an explosive booster 54 that is attached later and is all contained within a housing 56 . The length of section 34 is short enough to fit inside a safety loading tube not shown.
The explosive pellet 50 is normally fine particle HNS (IV) or NONA, both commercially available and has been shown to work with EFIs. A stack of two explosive pellets, one of fine particle HNS at the EFI interface, topped with HMX or coarser particle HNS, for example, is also a variation. Furthermore, the explosive pellet can be included as part of section 32 or as part of section 34 .
The assembly may also be configured without the explosive pellet. The explosive pellet could be incorporated into the booster and attached separately in the field.
Although the invention disclosed herein has been described in terms of specified and presently preferred embodiments which are set forth in detail, it should be understood that this is by illustration only and that the invention is not necessarily limited thereto. Alternative embodiments and operating techniques will become apparent to those of ordinary skill in the art in view of the present disclosure. Accordingly, modifications of the invention are contemplated which may be made without departing from the spirit of the claimed invention.
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A downhole explosive detonation comprises a high voltage electro-explosive initiator comprising an input high voltage power supply with a low impedance shunting fuse, a flexible electrical link and a capacitor discharge unit. Explosive is initiated in a direction approximately parallel, or in another version perpendicular to the capacitor discharge unit. A unique configuration and construction of the assembly allows installation through a small service port in the gun housing structure for more efficient gun arming. A real time downhole voltage monitoring is described that transmits voltage readings to the surface during a firing sequence.
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BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to a liquid crystal display device. More particularly, the invention relates to a high-resolution, high-brightness liquid crystal color display device based on a field sequential system and a driving method for the same.
2. Description of the Related Art
Liquid-crystal display devices (hereinafter abbreviated LCDs) have found widespread commercial applications in a variety of fields ranging from calculators to portable television sets (hereinafter abbreviated TVs) because of their excellent display performance rivaling that of the cathode ray tube (CRT herein after), their space-saving features exemplified by thin and light-weight construction, and other useful features such as low power consumption. While there are problems yet to be resolved, especially in response time and viewability, various improvements have been made in LCD technology because the LCD is a promising display device that is expected to replace the CRT in the near future. Among such improvements, improvements in color LCD technology involve various aspects of display performance and assume an important position in the development of the technology.
The principle of a color display is based on the method called "additive color mixing process". When two or more colored light beams enter the human eye, the light beams are combined on the retina and perceived as different colors. Based on this principle, any color can be obtained by additively mixing light beams of the three primary colors, R (red), G (green), and B (blue) in appropriate proportions. A color display in practical display devices is implemented using one of two systems based on the principle of the additive color mixing process.
One is the National Television System Committee (NTSC) system that uses a principle called "juxtapositional additive color mixing process". In this system, tiny color filters are placed close together in a matrix array in the display area of a single-plate display panel. These color filters are smaller in area than the spatial resolution limit of the human eye so that a combination of tiny color spots is perceived as a color by the eye. The NTSC system is compatible with monochrome television and currently, is the standard system for use in color TVs. However, in this "juxtapositional additive color mixing process", the R, G, and B primary colors become visible as separate colors unless the pixel size is smaller than the spatial resolution limit of the human eye. The juxtapositional additive color mixing process therefore poses a problem in that it reduces image quality when it is employed in a projection LCD or the like which projects an enlarged image for display.
The other system is one that employs a "simultaneous additive color mixing process". To apply this system for a color LCD, three color filters of R, G, and B are used in combination with three LCD panels, and three color images are simultaneously projected onto a screen where the color images are superimposed and merged into one color image. This system eliminates the fabrication difficulty of tiny color filters which is required in the Juxtapositional additive color mixing process. However, if there is a defective pixel in any of the three LCD panels, one of the R, G, and B colors, or a mixed color thereof, appears as a bright spot at the affected pixel position, thus making the defect noticeable. Furthermore, the provision of three LCD panels leads to increased size and cost of the display system.
Color LCDs have the above-mentioned shortcomings. In addition for the demand to overcoming these shortcomings, there is an increasing demand to enhance the resolution and brightness of color LCDs, which is imperative among others in the implementation of high-definition TV as the next-generation visual medium.
Higher resolution and higher brightness are conflicting requirements. On one hand, increasing the pixel density for increased resolution increases the ratio of the switching element area to the pixel area, which results in a reduction in the aperture ratio and consequently, a reduction in brightness. Conversely, if the aperture ratio is to be increased, the pixel area must be increased, which reduces the resolution. While the NTSC system is the standard system for color television today, the field sequential color system has now received renewed attention as a color system to overcome the above problems, for the reasons hereinafter described. The field sequential color system provides the following advantages in terms of high resolution and high brightness characteristics.
(1) The field sequential system uses a principle called "successive additive color mixing process". This process utilizes the resolution limit of the human eye in the time domain. More specifically, this process utilizes the phenomenon that when successive color changes are too fast for the human eye to perceive, the persistence of the previous color causes the color to be mixed with the succeeding color and these colors are combined and perceived as one color to the human eye. As in the simultaneous additive color mixing process, any desired color can be obtained at each pixel, so that the system achieves high image definition and also provides excellent color reproduction. The first color TV standard system utilized the field sequential system.
(2) If there is a defective pixel in the LCD panel, the affected pixel appears as black or white, which is not as noticeable as a colored bright spot. Therefore, pixel defects, up to a certain degree, will not lead to image quality reduction.
(3) Full-color or multi-color images can be displayed using a single LCD panel, which serves to reduce the size and weight of the display system. No cost increase is involved since no more than one LCD panel is required, unlike the simultaneous additive color mixing process which requires the provision of more than one LCD panel.
Color technology based on the field sequential system will be described below. FIG. 19 shows a color filter plate capable of high-speed sequential switching of colors. In the figure, a cyan filter 29C, a magenta filter 29M, and a yellow filter 29Y are formed one on top of another in this order.
The cyan filter 29C includes a pair of transparent substrates 20 and 21 with transparent electrodes (not shown) formed over the entire areas of the opposing surfaces thereof, and a liquid crystal layer 22 including a liquid crystal and cyan dichroic dye, sandwiched between the two substrates 20 and 21.
The magenta filter 29M includes a pair of transparent substrates 23 and 24 with transparent electrodes (not shown) formed over the entire areas of the opposing surfaces thereof, and a liquid crystal layer 25 including a liquid crystal and magenta dichroic dye, sandwiched between the two substrates 23 and 24.
The yellow filter 29Y includes a pair of transparent substrates 26 and 27 with transparent electrodes (not shown) formed over the entire areas of the opposing surfaces thereof, and a liquid crystal layer 28 including a liquid crystal and yellow dichroic dye, sandwiched between the two substrates 26 and 27.
The cyan filter 29C, magenta filter 29M, and yellow filter 29Y are each supplied with an AC voltage from an AC power supply 31, via their associated switching circuits 30C, 30M, and 30Y, respectively. Based on a select signal supplied from a display control circuit 16, the switching circuits 30C, 30M, and 30Y selectively apply the AC voltage to the cyan filter 29C, magenta filter 29M, and yellow filter 29Y, to drive the respective filters.
By controlling the activation and deactivation of each filter in this manner, light beams of the three primary colors, i.e., a red colored light beam, a green colored light beam, and a blue colored light beam are produced. Table 1 below shows the combinations in which the filters are turned on or off, in relationship to the resulting colors of incident light beam.
TABLE 1______________________________________Combination Resulting29C 29M 29Y colors______________________________________ON OFF OFF RedOFF ON OFF GreenOFF OFF ON Blue______________________________________
The operation of the field sequential color system using the above color filters will be described in detail below. FIG. 20 shows a timing chart for explaining the basic operation of a light beam selecting element 15. As shown, a voltage is applied to the cyan filter 29C during the period from time t1 to time t3. The orientation of the liquid crystal does not change immediately upon voltage application, but it takes a prescribed transition period τ. The transition period τ corresponds to the response time of the liquid crystal molecules to the applied electric field. Accordingly, even if voltage application is started at time t1, the liquid crystal in the cyan filter 29C does not immediately change the orientation in response to the applied voltage and the changed orientation does not settle down until time t2, i.e., until after the transition period τ has elapsed. As a result, the light beam selecting element 15 transmits a red colored light beam during a period TR starting at time t2 and lasting until time t3.
In like manner, voltage is applied to the magenta filter 29M, yellow filter 29Y, and cyan filter 29C in sequence, the light beam selecting element 15 transmitting a green colored light beam, blue colored light beam, and red colored light beam, respectively.
The light beam selecting element is not limited to the illustrated construction. It will be recognized that there are other possible constructions that can produce a desired color. For example, a construction including three kinds of liquid crystals containing red, blue, and green dichroic dyes, a construction including a liquid crystal panel combined with color polarizers, or a construction including a liquid crystal panel combined with neutral polarizers may be used.
Color technology based on the field sequential system has been described above. As described earlier, according to the field sequential system, a high-resolution, high-brightness color LCD having excellent image display quality can be achieved with a compact and light-weight construction.
However, LCD implementation of color display based on the field sequential system demands the following.
(1) Increased LCD response speed and stability of signal retention.
(2) Increased operating speed of switching elements.
Description is first given of (1) the increased LCD response speed and the stability of signal retention. FIG. 21 shows the equivalent circuit of a conventional liquid crystal driving circuit for each unit pixel in an active-matrix liquid crystal display device constructed with thin-film transistors (hereinafter abbreviated TFTs). The driving circuit shown includes a TFT 103, a pixel electrode 107, a liquid crystal capacitor LC, a counter electrode 108, and an additional capacitor Cs. The TFT 103 has a gate electrode 104 connected to a scanning line 101, a source electrode 105 connected to a data line 102, and a drain electrode 106 connected to the pixel electrode 107 and the additional capacitor Cs. A data signal corresponding to an image to be displayed is applied to the data line 102, and the signal is written to the pixel when the pixel is selected by applying a scanning signal to its associated scanning line 101. More specifically, when a scanning signal is applied to the scanning line 101, the TFT 103 connected to the scanning line 101 is turned on to selectively drive the pixel electrode 107. A voltage is applied between the selected pixel electrode 107 and the counter electrode 108, and the data signal is written as an electric charge on the liquid crystal capacitor LC between the two electrodes 107 and 108 as well as on the additional capacitor Cs.
In a display device having the liquid crystal driving circuitry as described above, if the minimum frame switching frequency at which the flicker is not perceivable by the human eye is 30 Hz or more, it follows that images in the R, G, and B primary colors must be displayed successively within 1/30 second, which is one frame period, in order to achieve full color display in accordance with the field sequential color system. These three images are merged using the retentivity of the human eye and as a result perceived as a full-color image. More specifically, if the display frequency is 30 Hz, then the images in the R, G, and B primary colors must each be displayed at a frequency of 90 Hz, which means that the LCD must display each color image in about 11 milliseconds. The LCD must be capable of displaying a good quality image within this period. This also means that the stored data signal must be retained in a stable state during the 11-millisecond period. Furthermore, to display 1125 scanning lines used in the High-Vision system, an extremely fast response is required. That is, a scanning signal must be applied to every one scanning line in about 10 microseconds.
Next, description is given of (2) the increased operating speed of the switching elements that is required of the liquid crystal driving circuitry employing the field sequential color system.
To produce images for ordinary High-Vision broadcasts, 1125 scanning lines and 1875 data lines are needed. In this case, the operating speed of about 102 KHz is required to the switching elements in the driving circuit for driving the scanning lines, and the operating speed about 190 MHz or more is required to the switching elements in the driving circuit for driving the data lines.
Thus, very fast switching elements are needed to implement the color display according to the field sequential system.
Materials for switching elements required to achieve such high-speed switching operations will be described below.
Liquid-crystal display devices usually use glass substrates. In active-matrix LCDs, switching elements such as TFTs are formed on such glass substrates. The characteristics of TFTs are determined by the kinds of thin films used to form the TFTs. The materials commonly used for the thin films are generally classified into one of the following three categories.
(1) Amorphous silicon
(2) Low-temperature polysilicon
(3) High-temperature polysilicon
Explanation will be given below of the thin films formed of the respective materials.
(1) Since amorphous silicon thin films can be formed at a relatively low temperature of about 350° C., these thin films can be formed on a low-cost glass substrate, for example, a substrate made of Corning 7059 manufactured by Corning Ltd. However, ordinary low-cost glass cannot be subjected to temperatures of not lower than 600° C. Therefore, a thermal oxide film having high insulating strength and high resistance to pinhole formation cannot be grown on a substrate made of such glass. In addition, there are many trapping states in an amorphous silicon thin film. For instance, the field-effect mobility μe of an amorphous silicon thin film is about 0.1 to 0.5 cm 2 V -1 S -1 . Accordingly, amorphous TFTs formed on a low-cost glass substrate have a large ON resistance, which means that circuits, such as driver circuits, requiring complex and high-performance transistors cannot be fabricated on the same substrate as the display part.
(2) Low-temperature polysilicon is crystallized by long-period annealing or laser annealing. The maximum processing temperature is 550° to 600° C. Since polysilicon TFTs are formed at higher temperatures than amorphous silicon TFTs, polysilicon TFTs generally have good transistor characteristics. That is, the field-effect mobility μe (electron mobility) is about 50 cm 2 V -1 S -1 , and μh (hole mobility) is about 15 cm 2 V -1 S -1 .
(3) Since high-temperature polysilicon can be processed at temperatures as high as 1200° C. when formed on a quartz substrate having excellent heat resistance, TFTs formed of high-temperature polysilicon have the best characteristics among the three categories of TFTs. A field-effect mobility μe of about 100 cm 2 V -1 S -1 can be obtained. Since TFTs having better characteristics than amorphous TFTs can be obtained, polysilicon thin films have the advantage that an IC fabrication process can be used for thin film fabrication and that some of driving circuits can be formed on the same glass substrate as the display part.
However, transistors formed of polysilicon, not to mention transistors formed of amorphous silicon, are slow with respect to operating speed. When the maximum operating frequencies are measured, for example, on CMOS shift registers formed from TFTs, the results are typically 5 MHz for low-temperature polysilicon TFTs, and 15 MHz even for high-temperature polysilicon TFTs. These operating speeds are slower than those needed to realize a color LCD based on the field sequential system. Therefore, TFTs capable of higher operating speeds are in high demand. Furthermore, since polysilicon TFTs have relatively large leakage currents, the TFT size has to be increased to provide a larger on/off ratio, or TFTs have to be connected in series. This makes the reduction of the LCD size difficult.
SUMMARY OF THE INVENTION
The liquid crystal display device of the present invention includes: a first substrate having a single-crystalline silicon layer on one surface thereof; a transparent second substrate disposed opposite the first substrate, the surface of the first substrate having the single-crystalline silicon layer thereon facing the second substrate with a ferroelectric liquid crystal layer sandwiched therebetween; and a plurality of circuit elements formed in the single-crystalline silicon layer in a corresponding relationship to each of a plurality of pixel areas formed on the surface of the first substrate which faces the ferroelectric liquid crystal layer.
In one embodiment of the present invention, the ferroelectric liquid crystal layer includes a ferroelectric liquid crystal of chiral smectic phase, a helical structure of the chiral smectic phase having a pitch smaller than a gap between the first and the second substrates, with resulting suppression of the helical structure.
In another embodiment of the present invention, an alignment film made of an organic polymer is formed over at least one of the surfaces of the first and the second substrates which face the ferroelectric liquid crystal layer, the alignment film being treated with rubbing.
In still another embodiment of the present invention, alignment films are formed on the first and second substrates, and the rubbing treatment is carried out only on the alignment film formed on the second substrate.
In still another embodiment of the present invention, the ferroelectric liquid crystal has only one stable orientation state in the absence of an applied electric field.
In still another embodiment of the present invention, alignment films are formed on the first and second substrates, the alignment film formed on the first substrate is made of a different material from the alignment film formed on the second substrate.
In still another embodiment of the present invention, the alignment film formed on the first substrate and the alignment film formed on the second substrate are treated using different alignment treatment conditions.
In another aspect of the present invention, a driving method for a liquid crystal display device is provided. The liquid crystal display device includes: a first substrate having a single-crystalline silicon layer on one surface thereof, a transparent second substrate disposed opposite the first substrate, the surface of the first substrate having the single-crystalline silicon layer thereon facing the second substrate with a ferroelectric liquid crystal layer sandwiched therebetween, a plurality of circuit elements formed in the single-crystalline silicon layer in a corresponding relationship to each of a plurality of pixel areas formed on the surface of the first substrate which faces the ferroelectric liquid crystal, and a power supply connected to the circuit elements. In the driving method, the ferroelectric liquid crystal layer is placed in one memory state by applying an electric field from the power supply via the circuit elements and a gray scale generation signal is applied to the ferroelectric liquid crystal layer while varying the level of the signal, thereby accomplishing the generation of gray scales.
In one embodiment of the present invention, the ferroelectric liquid crystal has only one stable orientation state in the absence of an applied electric field.
In another embodiment of the present invention, one complete image is scanned for display within 11 milliseconds.
In another aspect of the present invention, a driving method for a liquid crystal is provided. The liquid crystal display device includes:
a first substrate having a single-crystalline silicon layer on one surface thereof,
a transparent second substrate disposed opposite the first substrate, the surface of the first substrate having the single-crystalline silicon layer thereon facing the second substrate with a ferroelectric liquid crystal layer sandwiched therebetween,
scanning lines and signal lines formed in the single-crystalline silicon layer in such a manner as to form a matrix,
a first switching element, a second switching element, and a storage capacitor formed in the single-crystalline silicon layer in each of a plurality of pixel areas formed in the matrix,
a pixel electrode deposited on a protective film formed over the entire surface of the single-crystalline silicon layer of the first substrate and covering the scanning lines, the signal lines, the first switching element, the second switching element, and the storage capacitor, the pixel electrode being provided in each of the plurality of pixel areas, with the first switching element being connected to the associated scanning line and signal line as well as to one electrode of the storage capacitor and the second switching element, and the second switching element being connected to the one electrode of the storage capacitor and the pixel electrode, and
a transparent counter electrode deposited on the surface of the second substrate facing the first substrate.
In the driving method for the liquid crystal display device, when a scanning signal is applied to the first switching element through the scanning line to turn on the first switching element, a data signal is applied to the second switching element through the first switching element to turn on the second switching element, thereby applying a voltage across a region of the ferroelectric liquid crystal layer between the pixel electrode connected to the second switching element and the transparent counter electrode corresponding to the pixel electrode, and thus holding that region at a prescribed potential while, at the same time, retaining the data signal in the storage capacitor, and
during the OFF period of the first switching element, the second switching element is held ON using the data signal retained in the storage capacitor during the ON period of the first switching element, thereby allowing a voltage from the power supply to be applied across the ferroelectric liquid crystal between the pixel electrode and the transparent counter electrode so that the ferroelectric liquid crystal layer is held at the substantially same potential as when the first switching element is ON.
Thus, the invention described herein makes possible the advantages of (1) providing a liquid crystal color display device based on the field sequential system, and (2) providing a driving method for the same.
These and other advantages of the present invention will become apparent to those skilled in the art upon reading and understanding the following detailed description with reference to the accompanying figures and tables.
BRIEF DESCRIPTION OF THE DRAWINGS
FIGS. 1A to 1E are schematic diagrams illustrating the bistability of ferroelectric liquid crystal molecules.
FIGS. 2A, 2B and 2C are diagrams for explaining the principle of gray scale generation in a ferroelectric liquid crystal display device.
FIG. 3 is a diagram showing the output voltage (the transmittance) as a function of the applied voltage for a ferroelectric liquid crystal.
FIG. 4 is a diagram showing the transmittance as a function of the applied voltage for a ferroelectric liquid crystal.
FIG. 5 is a diagram showing the transmittance as a function of the applied voltage for a ferroelectric liquid crystal.
FIG. 6 is a diagram showing the transmittance as a function of the applied voltage for a ferroelectric liquid crystal.
FIG. 7 is a diagram showing the transmittance as a function of the applied voltage for a ferroelectric liquid crystal.
FIG. 8 is a diagram showing the transmittance as a function of the applied voltage for a ferroelectric liquid crystal.
FIG. 9 is a diagram showing the transmittance as a function of the applied voltage for a ferroelectric liquid crystal.
FIG. 10 is a diagram showing the transmittance as a function of the applied voltage for a ferroelectric liquid crystal.
FIG. 11 is a diagram showing the transmittance as a function of the applied voltage for a ferroelectric liquid crystal.
FIG. 12 is a diagram showing the transmittance as a function of the applied voltage for a ferroelectric liquid crystal.
FIGS. 13A and 13B show diagrams showing the intensity of transmitted light as a function of the applied voltage for monostable and bistable ferroelectric liquid crystals, respectively.
FIG. 14 is a diagram showing the response speed as a function of the applied voltage for a ferroelectric liquid crystal.
FIG. 15 is a diagram showing the response speed as a function of the applied voltage for a ferroelectric liquid crystal.
FIG. 16 is a diagram showing the response speed as a function of the applied voltage for a ferroelectric liquid crystal.
FIGS. 17A and 17B are a cross-sectional view and a plan view of a unit pixel area in a liquid crystal display device according to an example of the present invention.
FIG. 18 is an equivalent circuit diagram of a liquid crystal driving circuit for a unit pixel area in the liquid crystal display device according to the present invention.
FIG. 19 is a diagram showing a color filter for high-speed sequential switching of colors.
FIG. 20 is a timing chart for explaining the basic operation of a color shutter.
FIG. 21 is an equivalent circuit of a driving circuit for an active-matrix liquid crystal display device according to the prior art.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
Hereinafter, the present invention will be described by way of illustrative examples with reference to the drawings and tables.
In the liquid crystal display device according to the present invention, since a ferroelectric liquid crystal is used as the liquid crystal material, a fast response can be obtained. Further, the ferroelectric liquid crystal display device of the invention uses the display mode in which the transmittance varies continuously with applied voltage in a stable state. This makes it possible to display gray scales.
Since a single-crystalline silicon substrate is used as the base substrate and switching transistors are formed in a single-crystalline silicon layer, the switching transistors have large current-driving capabilities, small size and are capable of high speed switching operations.
Since the single-crystalline layer allows increased packing density of circuit elements, two transistors and a storage capacitor are provided for each unit pixel area in the invention. The first transistor is connected to a scanning line and a signal line. The drain of the first transistor is connected to one electrode of the storage capacitor as well as to the second transistor. The other electrode of the storage capacitor is grounded. The second transistor is also connected to a power supply and a pixel electrode.
The first transistor applies a data signal to the second transistor. The storage capacitor has the function of storing the data signal from the first transistor. The second transistor is a switching transistor for applying the data signal voltage from the power supply to the liquid crystal when the first transistor is ON. This second transistor continues to apply a voltage corresponding to the data signal stored on the storage capacitor, to the liquid crystal after the first transistor is turned off, until the first transistor is turned on again.
The ferroelectric liquid crystal exhibits a spontaneous polarization; when a voltage is applied, a transient current flows due to a change in the molecular orientation of the liquid crystal. As for the time required to write data to the scanning lines, if a total of 1125 scanning lines are to be scanned in 1/30 second, the write time allowed for one scanning line is about 10 microseconds to implement the field sequential color system. The change of the molecular orientation in the ferroelectric liquid crystal takes several tens of microseconds, which means that the transient current flows for a period longer than the write time. According to the above-described construction of the invention, since the voltage corresponding to the data signal stored on the storage capacitor continues to be applied to the liquid crystal during one field period, the transient current does not affect the liquid crystal potential.
Examples
An example of the present invention will be described below. In LCD applications where a particularly clear display is required, active-matrix LCDs having switching transistors or the like at each pixel location are used. A typical display mode used in active-matrix LCDs is the twisted nematic mode (herein-after abbreviated TN mode). In the TN mode, the liquid crystal molecules in the liquid crystal cell are initially twisted nearly 90°; the liquid crystal cell is placed between a pair of polarizers, and display is produced by utilizing the optical properties of the cell, i.e, the optical rotatory power in the absence of an electric field and cancellation of the optical rotatory power under the influence of an applied field.
While the field-effect nematic liquid crystal display devices utilize the dielectric anisotropy of liquid crystal molecules, ferroelectric liquid crystal display devices produce display by utilizing the property that the ferroelectric liquid crystal molecules possess a spontaneous polarization and switch in such a manner that the polarity of their spontaneous polarization matches the polarity of an applied electric field. Display devices using ferroelectric liquid crystals are described, for example, in N. A. Clark and S. T. Lagerwall, Appl. Phys. Lett., 36, 899 (1980), Japanese Laid-Open Patent Publication No. 56-107216, and U.S. Pat. No. 4,367,924. FIGS. 1A to 1E show schematic diagrams illustrating the spontaneous polarization in the ferroelectric liquid crystal and associated elec- tro-optic effects. The liquid crystal molecules in the ferroelectric liquid crystal layer are oriented in a helical structure as shown in FIG. 1A. When the ferroelectric liquid crystal is filled into a cell whose thickness is smaller than the helical pitch, the helical structure is suppressed and two stable states result. To produce a ferroelectric liquid crystal cell having bistable states by suppressing the helical structure, Japanese Laid-Open Patent Publication No. 56-107216 and U.S. Pat. No. 4,367,924 propose methods wherein the helical structure is suppressed by making the helical pitch larger than the cell thickness. These methods utilize the strong property of the liquid crystal molecules to align parallel with the substrate interface. Such a ferroelectric liquid crystal cell is called a surface stabilized ferroelectric liquid crystal cell (SSFLC cell). In FIG. 1B, the reference numeral 900 designates the normal to the smectic layer, and 901 indicates the direction of the long axis of the ferroelectric liquid crystal molecule (orientation direction). The angle between 900 and 901 is the tilt angle θ of the liquid crystal molecule. By applying an electric field across the ferroelectric liquid crystal, as shown in FIG. 1C, the spontaneous polarization of the ferroelectric liquid crystal molecules can be oriented in the direction of the electric field. By changing the polarity of the applied field, as shown in FIG. 1D, the orientation state of the liquid crystal molecules can be switched from one state to the other. Even after the applied voltage is removed, the orienting directions of the molecular axes in the respective states can be retained, as shown in FIG. 1E. This is the memory effect, one of the electro-optic effects exhibited by the ferroelectric liquid crystal.
The switching between the two states changes the birefringence of the ferroelectric liquid crystal layer in the cell. Therefore, with the ferroelectric liquid crystal cell sandwiched between two polarizers, transmission of light passing through it can be controlled. Since the spontaneous polarization of the liquid crystal and the electric field interact directly to achieve the switching, very fast response times of the order of microseconds can be obtained. In the present example, a ferroelectric liquid crystal of chiral smectic C phase is used in order to achieve a fast-response color LCD based on the field sequential system.
Since the conventional display device using ferroelectric liquid crystal material can only be switched between two states, as described above, gray scales cannot be displayed with such a device. Heretofore, it has generally been believed that an intermediate state between these two stable states cannot be produced.
However, it has recently been found that an intermediate state can be created depending on the condition of the electric field applied to the ferroelectric liquid crystal. More specifically, a voltage of an AC waveform is used and its peak values are varied to generate intermediate states, thereby achieving generation of gray scales. The principle of this gray scale generation will be described in further detail with reference to FIG. 2.
FIG. 2A shows the relationship of the memory angle relative to the tilt angle in the presence of an applied field in a ferroelectric liquid crystal. In the figure, the reference numeral 900 designates the direction of the normal to the smectic layer, and 901 and 901' indicate the orienting directions of the long axes of the ferroelectric liquid crystal molecules in bistable states when no field is applied. Memory angles θ m and θ m are defined as the angles that the long-axis directions 901 and 901' of the ferroelectric liquid crystal molecules make with the normal 900 to the smectic layer. The reference numerals 902 and 902' in the figure show the apparent long-axis directions of the ferroelectric liquid crystal molecules when a sufficient voltage is applied in positive and negative directions, respectively; the angle between 902 or 902' and 900 is the tilt angle θ or θ'. As shown, the memory angles θ m and θ m' are normally smaller than the tilt angles θ and θ' obtained when a sufficient electric field is applied to the ferroelectric liquid crystal layer. When a voltage is applied across the ferroelectric liquid crystal, the liquid crystal molecules deflect to the right or to the left in the figure, depending on the polarity of the applied voltage. When a sufficiently large voltage is applied, the liquid crystal molecules deflect fully to the position of 902 (or 902'); with a smaller applied voltage, the deflection angle of the liquid crystal molecules stays somewhere between 902 (or 902') and 900.
Here, when the ferroelectric liquid crystal layer is sandwiched between two polarizers, with the polarization axis 951 of one polarizer aligned parallel to the long axis direction 901 of one stable state and the polarization axis 952 of the other polarizer aligned at right angles to it, as shown in FIG. 2B, an intermediate state can be created. Using this, gray scales can be achieved.
Next, examples relating to the generation of gray scales by the ferroelectric liquid crystal display device will be described below.
Example 1
First, a pair of glass substrates were used as the substrates for the liquid crystal cell, and a conductive ITO film was deposited and patterned on the surface of each substrate.
Next, an insulating film was formed over the entire surface of each substrate in such a manner as to cover the conductive film.
Then, polyimide PSI-A-2001 (manufactured by Chisso Corporation) was applied over the entire surface of the insulating film by spin coating, which was then treated with rubbing. The pair of glass substrates thus prepared were held opposite each other with their polyimide film sides facing inside and their rubbing directions parallel to each other, and were attached together to provide a cell thickness of 2 μm.
Finally, a ferroelectric liquid crystal mixture 1 was vacuum injected into the empty cell to form the ferroelectric liquid crystal cell. The physical properties of the ferroelectric liquid crystal mixture 1 are shown in Table 2.
TABLE 2__________________________________________________________________________L.C. compound Amount__________________________________________________________________________ ##STR1## 28(%) ##STR2## 14 ##STR3## 14 ##STR4## 12.5 ##STR5## 9.5 ##STR6## 8.5 ##STR7## 8.5 ##STR8## 5Transition temperature SC.sup.58 SA.sup.71 N.sup.87 IP = -14.5 nC/cm.sup.2 (25 C.)τ = 64 μsec (±5 V/μm, 25 C. 0-50%)__________________________________________________________________________ (*indicates asymmetric carbon)
After placing the ferroelectric liquid crystal in a memory state by applying an electric field, two polarizers were arranged in a crossed Nicols state with one of their polarization axes aligned parallel to one of the extinction directions of the ferroelectric liquid crystal layer. In this situation, the intensity of transmitted light was measured at 25° C. while applying a square wave of 60 Hz. The results of the measurements are shown in FIG. 3. As can be seen from the figure, the transmittance increases continuously with increasing voltage. Continuous gray scales can be achieved using this characteristic. Since the voltage applied to the liquid crystal is balanced between the positive and negative polarities, there is no problem with reliability.
Example 2
First, a pair of glass substrates were used as the substrates for the liquid crystal cell, and a conductive ITO film was deposited and patterned on the surface of each substrate.
Next, an insulating film was formed over the entire surface of each substrate in such a manner so as to cover the conductive film. Then, nylon 66 was applied on the entire surface of the insulating film by spin coating, and only one of the substrates was treated with rubbing. The pair of glass substrates thus prepared were held opposite each other with their nylon 66 sides facing inside, and attached together to provide a cell thickness of 1.2 μm.
Finally, a ferroelectric liquid crystal mixture FLC-6430 (Hoffman-LaRoche) was vacuum injected into the empty cell to form the ferroelectric liquid crystal cell. Physical properties of the ferroelectric liquid crystal mixture are shown in Table 3.
TABLE 3______________________________________Physical properties of FLC-6430______________________________________Spontaneous polarization 90nC/cm.sup.2Helical pitch 0.43 μmTilt angle θ 27°Memory angle 2θ 46°______________________________________
The ferroelectric liquid crystal cell was placed under a polarizing microscope, and the intensity of transmitted light was measured at 20.5° C. while applying a square wave of 60 Hz. The results of the measurements are shown in FIG. 4. As can be seen from the figure, the transmittance increases continuously with increasing voltage.
Example 3
In Example 3, various ferroelectric liquid crystal cells were fabricated in addition to the same ones fabricated in Examples 1 and 2, and the relationships between applied voltage and transmittance, and between applied voltage and response speed were examined for each ferroelectric liquid crystal cell. For each cell, glass substrates were used on both sides, and ITO films were formed and patterned on the opposing surfaces of the substrates. Further, an insulating film and an alignment film were formed in this order to cover the ITO film formed on each of the opposing surfaces of the substrates. The films were not formed for some of the cells. Other test conditions, and test results such as transmittance and response characteristics, are shown in Table 4. In the table "◯" indicates the insulation film was formed and "X" indicates the insulation film was not formed.
TABLE 4__________________________________________________________________________Upper substrate Lower substrateInsulation Alignment Insulation AlignmentCell No.film film film film Rubbing Liquid crystal Memory V-T Response__________________________________________________________________________1 ∘ PSI-S-2001 ∘ PSI-S-2001 Parallel Mixture No. 1 Bistable FIG. -- (Chisso) (Chisso) (Table 2)2 ∘ Nylon 66 ∘ Nylon 66 Upper only FLC-6430 Monostable FIG. FIG. 14 (Roche)3 ∘ PSI-A-2101 ∘ PSI-A-2101 Upper only FLC-6430 Monostable FIG. FIG. 15 (Chisso) (Chisso) (Roche)4 ∘ PSI-A-2101 ∘ PSI-A-2101 Antiparallel FLC-6430 Monostable FIG. FIG. 16 (Chisso) (Chisso) (Roche)5 ∘ PSI-A-2101 ∘ PSI-A-2101 Parallel Mixture No. 2 Bistable FIG. -- (Chisso) (Chisso) (Table 5˜7)6 ∘ PSI-A-2101 ∘ PSI-A-2101 Parallel Mixture No. 3 Bistable FIG. -- (Chisso) (Chisso) (Table 5˜7)7 ∘ PSI-A-2101 ∘ PSI-A-2101 Parallel Mixture No. 4 Bistable FIG. -- (Chisso) (Chisso) (Table 5˜7)8 ∘ PSI-A-2001 x PSI-A-2001 Parallel Mixture No. 2 Monostable FIG. -- (Chisso) (Chisso) (Table 5˜7)9 x LX-1400 x LX-1400 Upper only ZU-5014/000 Bistable FIG. -- (Hitachi chemical) (Hitachi (Merck) chemical)10 ∘ PSI-A-2101 x PSI-A-2101 Upper only Mixture No. 2 Monostable FIG. -- (Chisso) (Chisso) (Table 5˜7)11 ∘ PSI-A-2001 x PSI-A-2001 Parallel Mixture No. 5 Monostable -- (Chisso) (Chisso) (Table 8)__________________________________________________________________________
Table 5 shows the structures and phase transition temperatures for six kinds of compounds (compounds 1 to 6) that form the liquid crystal mixtures 2 to 4 used.
TABLE 5__________________________________________________________________________ Compounds Chemical structure Transition temperature (°C.)Compound No. (*indicates asymmetric carbon) K SC SA N I__________________________________________________________________________Compound 1 ##STR9## . 50 (. 42) -- . 63 .Compound 2 ##STR10## . 40 . 52 61 . 65 .Compound 3 ##STR11## . 63 . 93 . 126 . 127 .Compound 4 ##STR12## . 60 . 109 . 128 -- .Compound 5 ##STR13## . 86 -- -- -- .Compound 6 ##STR14## . 47 -- -- (. 42) .__________________________________________________________________________
Table 6 shows the composition of mixtures 2 to 4 represented by the weight percentages of the compounds 1 to 6 shown in Table 5 and the phase transition temperatures for each of the mixtures 2 to 4.
TABLE 6__________________________________________________________________________ Compound (wt %) Transition temperature (°C.)Mixture No. 1 2 3 4 5 6 K SC SA N I__________________________________________________________________________Mixture 2 24.5 24.5 24.5 24.5 2.0 . <RT . 66 . 81 . 86 .Mixture 3 24.5 24.5 24.5 24.5 2.0 . <RT . 69 . 81 . 87 .Mixture 4 22.5 22.5 22.5 22.5 10.0 . <RT . 67 . 79 . 85 .__________________________________________________________________________
Table 7 shows the amount of spontaneous polarization, tilt angle, memory angle, and response time for each of the mixtures 2 to 4.
TABLE 7______________________________________ Spontaneous Tilt Memory Tesponse polarization angle angle timeMixture No. (nC/cm.sup.2) θ(°) 2θ(°) (μsec)______________________________________Mixture 2 -1.5 24 23 170Mixture 3 <0.5 23 19 147Mixture 4 1.1 24 20 172______________________________________
Table 8 shows the kinds of compounds forming mixture 5, along with the weight percentages of the compounds, the phase transition temperatures, and the amount of spontaneous polarization.
TABLE 8__________________________________________________________________________ Compounds (wt %) Transition Spontaneous SCE-13R SCE-13 temperature (°C.) polarizationMixture No. (Merck) (Merck) K SC SA N I (nC/cm.sup.2)__________________________________________________________________________Mixture 5 90.0 10.0 . <RT . 60 . 87 . 105 . 0.7__________________________________________________________________________
The transmittance was measured for each of these cells while applying a square wave of 60 Hz. The results are shown in FIGS. 5 to 12. As can be seen from any of these figures, the transmittance varies continuously with the applied voltage. In this manner, according to the present invention, continuous gray scales can be achieved with the liquid crystal cells constructed of liquid crystal materials exhibiting ferroelectricity.
It is known that there are two stable modes in ferroelectric liquid crystals, one being the bistable mode first described and the other the monostable mode hereinafter described. Continuous gray scale generation, such as described above, can be achieved with both the bistable and monostable modes. However, when bistable devices and monostable devices are compared, it will be shown that the monostable type devices shows stable properties compared to the bistable type devices, for the following reason.
When using a polarizer with a ferroelectric liquid crystal display device, the polarization axis of the polarizer is aligned with the orienting direction of the liquid crystal molecules in a stable state when no electric field is applied. This is the same for both monostable and bistable devices. For bistable devices, the polarization axis is aligned with the molecular orientation in either of the two stable states. In the case of bistable devices, however, the following problems occur.
(1) When the device is left for a long period without the application of an electric field, a region occurs in the liquid crystal layer that tends to shift to the other stable state. This causes the darkest area in the display to gradually become lighter, leading to instability of the display.
(2) Since there are two stable states, light transmission differs, depending on which stable state the molecules return to when the applied electric field is removed.
The above point (1) does not present much of a problem for the liquid crystal display device of the invention that is designed to refresh the display continually. On the other hand, the above point (2) poses a serious problem. This problem will be described in further detail below.
In the liquid crystal display device of the invention constructed with a ferroelectric liquid crystal, when switching the display from the brightest state, an image display state, to the darkest state (or from the darkest state to the brightest state), the voltage being applied to the liquid crystal is set to 0 V.
In the case of a bistable device, when the voltage being applied to the liquid crystal becomes 0 V, the liquid crystal molecules are put in either of the two stable states, 901 or 901', as shown in FIGS. 2A and 2B. At this time, if the liquid crystal is put in the stable state 901', the darkest state is attained as desired. On the other hand, if it is put in the state 901, the display is switched to the brightest state when the darkest state is desired. When the voltage becomes 0 V, whether the molecular orientation in the liquid crystal layer assumes state 901 or 901' is determined by the polarity and magnitude of the voltage being applied to the liquid crystal immediately before it becomes 0 V.
On the other hand, in the case of a monostable device, the molecular orientation has only one stable state 903, as shown in FIG. 2C. That is, when the voltage applied to the liquid crystal becomes 0 V, the liquid crystal molecules can take only one stable state 903. Accordingly, the polarization direction of the polarizer should only be aligned parallel to the direction of 903.
FIGS. 13A and 13B show the variation of transmitted light intensity with applied voltage for monostable and bistable devices, respectively. In the monostable device, when the applied voltage becomes 0 V, the darkest state is attained, as shown in FIG. 13A, regardless of the polarity, positive or negative, of the immediately preceding voltage.
In the bistable device, on the other hand, when the applied voltage is set to 0 V after application of a negative voltage, the darkest state is obtained, but when the applied voltage is set to 0 V after application of a positive voltage, the darkest state is not attained, as shown in FIG. 13B. This is because when the immediately preceding voltage is negative, the liquid crystal molecules are oriented in the direction of 901' in FIG. 2B (in alignment with the polarization direction 951 of the polarizer), whereas when the immediately preceding voltage is positive, the liquid crystal molecules are oriented in the direction of 901 in FIG. 2B, so that the orienting direction of the liquid crystal molecules goes out of alignment with the polarizing direction 951 of the polarizer. For this reason, the monostable type has practical advantages over the bistable type.
Referring now to the column of memory effect of ferroelectric liquid crystal molecules in Table 4 that summarizes the experimental conditions and results of the foregoing examples, it can be seen that in any monostable device, the two substrates are made asymmetric to each other in terms of rubbing treatment or in terms of the presence or absence of an insulating film on the respective substrates. For example, for cells Nos. 2 and 3, only one substrate is treated with rubbing, while for cell No. 4, both substrates are treated with rubbing, but the rubbing directions are antiparallel to each other. For cells Nos. 8 and 11, only one substrate is provided with an insulating film. For cell No. 10, rubbing treatment is performed on one substrate only, and also, the insulating film is formed on one substrate only. Thus, the inventors of the present application verified by experiment that the asymmetry between the two substrates in terms of alignment treatment or in terms of the provision of an insulating film is effective in realizing monostable ferroelectric liquid crystals.
It will be noted that in addition to the rubbing treatment, oblique evaporation is also an effective alignment treatment technique in the fabrication of ferroelectric liquid crystal display devices according to the present invention.
When only one substrate is to be treated with rubbing to realize the monostable mode of ferroelectric liquid crystal layer, it is preferable that of the two substrates, the substrate on which no active elements are formed be treated with rubbing. This is because the static electricity generated by rubbing may cause the transistor or other element characteristics to change or may lead to insulation breakdown between interconnections.
In SID 90 Digest, 106 (1990), a ferroelectric liquid crystal cell is disclosed which, unlike the above-described SSFLC cell (surface stabilized ferroelectric liquid crystal cell), has a helical pitch substantially shorter than the cell thickness and yet has the effect of suppressing the helical structure, thus exhibiting bistability. This cell is called a short-pitch bistable ferroelectric liquid crystal (SBFLC) cell, in contrast with the SSFLC cell. This short-pitch ferroelectric liquid crystal mode has the following advantages.
(1) In the conventional ferroelectric liquid crystal mode, the spontaneous polarization needs to be made large if the response speed is to be increased. Making the spontaneous polarization larger, however, has the tendency to make the helical pitch shorter. Therefore, the gap between the substrates needs to be reduced so that the helix can be suppressed. Reducing the substrate gap, however, makes the fabrication of liquid crystal cells difficult, leading to reduced fabrication yield.
On the other hand, in the short-pitch ferroelectric liquid crystal mode, a helix-suppressed state can be achieved without reducing the substrate gap. Therefore, the above-stated difficulty will not occur even if the spontaneous polarization is made large to increase the response speed.
(2) In the conventional ferroelectric liquid crystal mode, the characteristics such as response time and memory angle are strongly dependent on temperature, requiring temperature control of the liquid crystal panel. On the other hand, in the short-pitch ferroelectric liquid crystal mode, the temperature dependence of these characteristics is small.
Furthermore, though this does not directly affect the display performance, the conventional ferroelectric liquid crystal mode has a problem in impact resistance. Therefore, a shock absorber or the like has to be provided to protect the liquid crystal panel from impact. This has posed a big barrier to the reduction of size of the display device. In comparison, the short-pitch liquid crystal mode provides excellent impact resistance, which eliminates the need for a shock absorber and other items which have no relevance to the display performance.
The reason has not yet been determined why, in the short-pitch ferroelectric liquid crystal, the helical structure can be suppressed despite the helical pitch being smaller than the cell thickness. The ferroelectric liquid crystal material FLC-6430 from Hoffman-LaRoche, described in the aforementioned paper and used in some of the examples of the invention, is the only example of SBFLC cell currently known. Cell Nos. 2 to 4 shown in Table 4 are constructed using this liquid crystal material.
Example 4
In Example 4, the relationship between applied voltage and response time for various ferroelectric liquid crystals was examined. The voltage waveform shown in FIG. 13 was applied to each of the ferroelectric liquid crystal cells of cell Nos. 2 to 4 in Table 4. The response time was measured based on the change in the transmittance observed at this time. Here, the response time means how fast the transmitted light intensity changes (from 10% to 90% or from 90% to 10%) in response to a positive pulse voltage. The results are shown in FIGS. 14 to 16. In the figures, each solid black dot indicates the time required to change from the dark to the light state (the rise time) and each black square indicates the time required to change from the light to the dark state (the fall time).
The invention aims to achieve a frame display time of 11 milliseconds or less. To achieve this, the time allowed for writing must be sufficiently shorter than 11 milliseconds. In fact, it is desirable that the response time be kept under 1 millisecond.
FIG. 14 shows that response times of about 1 millisecond can be achieved when the applied voltage is 1 V. Similarly, it is shown that response times of 1 millisecond or less can be obtained with an applied voltage of 10 V or larger in the case of FIG. 15, and 7 V or larger in the case of FIG. 16. Thus, by using ferroelectric liquid crystals as the liquid crystal material, response times within 1 millisecond can be achieved.
The above experiment was conducted with the liquid crystals in a chiral smectic C phase, but it was also confirmed that similar results could be obtained with ferroelectric liquid crystals in other phases such as a chiral smectic F phase, a chiral smectic I phase, etc.
In the present invention, in order to obtain switching elements having high operating speeds enough to implement the field sequential color system, switching transistors for driving pixel electrodes are formed in single-crystalline silicon. Since single-crystalline silicon has a high mobility (approx. 1500 cm 2 V -1 s -1 ), TFTs can be obtained that have performance far superior to the amorphous silicon TFTs or polysilicon TFTs given in the description of the prior art. Table 9 shows a comparison of performance among the various categories of transistors.
TABLE 9______________________________________ Single- Poly- crystalline crystalline Amorphous Si Si Si______________________________________Mobility(cm.sup.2 · v.sup.-1 · s.sup.-1)Electron 1500 100 0.1˜0.5Hole 600 50 --Ion/Ioff >10.sup.3 10.sup.7 10.sup.6Operation frequency Several GHz 20 MHz 5 MHz(CMOS shift (1 μm rule) (L = 10 μm) (L = 10 μm)register) (W = 30 μm) (W = 30 μm)______________________________________
From Table 9, it can be seen that transistors formed in single-crystalline silicon provide switching elements having greater current-driving capabilities and larger current on/off ratios.
As described above, a ferroelectric liquid crystal is used as the liquid crystal material to achieve fast response as well as gray scale generation, and switching transistors formed in single-crystalline silicon layers provide switching elements capable of high speed operations. These solve some of the problems associated with the implementation of a color display based on the field sequential system. A remaining problem concerns the stability of LCD signal retention. The following describes how this problem can, be solved.
FIGS. 17A and 17B show the circuit configuration of one unit pixel area in a liquid crystal color display device according to the present example. FIG. 17B is a plan view, and FIG. 17A is a cross-sectional view taken along line A-A' in FIG. 17B. As shown in FIG. 17A, this liquid crystal display device uses p-type single-crystalline silicon to form a base substrate 1, on top of which an NMOS switching circuit is formed. The display device uses two transistors, a first transistor Q1 and a second transistor Q2, for every one unit pixel area. Sources Q1s and Q2s and drains Q1d and Q2d of the respective transistors Q1 and Q2 are formed as n-type diffusion layers 2 diffused into the p-type single-crystalline silicon layer. Gate electrodes Q1g and Q2g of the respective transistors Q1 and Q2 are formed above the silicon layer of the base substrate 1 between the respective sources Q1s and Q2s and drains Q1d and Q2d, and each of the gate electrodes Q1g and Q2g is entirely surrounded by an insulating film 3. In this example, the gate electrodes Q1g and Q2g are formed of polysilicon, and gate insulating films 3 g are silicon oxide films. The gate electrodes Q1g and Q2g of the transistors Q1 and Q2 are separated by a silicon oxide film 6 and a polysilicon electrode 7a on the base substrate 1. In the unit pixel area, a storage capacitor Cs is formed along with the two transistors Q1 and Q2. This storage capacitor Cs is formed from an aluminum line 7b formed in the silicon oxide film 6 adjacent to the second transistor Q2, an n-type diffusion layer 2 formed in the silicon layer in the corresponding position, and a gate insulating film 3g formed between them.
A protective film 8 is formed over the entire surface of the base substrate 1 and covering the gate insulating film 3g, insulating film 3 (containing each gate electrode), silicon oxide film 6, polysilicon electrode 7a, and aluminum line 7b. The protective film 8 is provided to protect the circuit formed on the base substrate 1.
A throughhole 9 is opened in the protective film 8 in a position where the polysilicon electrode 7a formed between the transistor Q2 and the silicon oxide film 6 adjacent to the transistor Q2 spreads over the silicon oxide film 6. A pixel electrode 10 is formed over a designated region of the protective film 8 in each unit pixel area. The pixel electrode 10 is connected via the throughhole 9 to the underlying polysilicon electrode 7a which in turn is electrically connected to the drain Q2d of the transistor Q2.
Further, as shown in FIG. 17B, the gate electrode Q1g of the first transistor Q1 is connected to a scanning line 4, while the source electrode Q1s of the first transistor Q1 is connected to a signal line 5 which intersects the scanning line 4. The drain electrode Q1d of the first transistor Q1, the gate electrode Q2g of the second transistor Q2, and the polysilicon electrode 7a associated with the storage capacitor Cs are connected to the common aluminum line 7b formed on the silicon oxide film 6.
A transparent counter electrode 12 is formed over the entire area of the surface of a glass substrate 11 that faces the base substrate 1. An alignment film (not shown) is formed over the counter electrode 12.
The glass substrate 11 and the base substrate 1 are held opposite each other, and a ferroelectric liquid crystal layer 13 is sealed between the two substrates 1 and 11. The glass substrate 11 is placed on the light incident side. (See Table 4 for materials of the liquid crystal layer 13, alignment films, and other details.)
We will now describe a driving circuit for the liquid crystal display device and a method for driving the same according to the present example. FIG. 18 shows an equivalent circuit of the liquid crystal driving switching circuit of the present example shown in FIG. 17. The circuit shown in FIG. 18 illustrates the configuration of one unit pixel area.
The first transistor Q1 is connected to the scanning line 4 and signal line 5 near the intersection of these two lines. More specifically, the gate Q1g of the first transistor Q1 is connected to the scanning line 4, and the source Q1s of the first transistor Q1 is connected to the signal line 5. The drain Q1d of the first transistor Q1 is connected to one electrode of the storage capacitor Cs and also to the gate Q2g of the second transistor Q2. The other electrode of the storage capacitor Cs is grounded. On the other hand, the source Q2s of the second transistor Q2 is connected to a power supply, and the drain Q2d of the second transistor Q2 is connected to the pixel electrode 10.
The second transistor Q2 has the characteristic that the potential of the drain Q2d varies substantially linearly with the potential of the gate Q2g. Since the first transistor Q1 functions to supply a data signal to the second transistor Q2, the off leakage current must be kept as small as possible. The storage capacitor Cs has the function of holding the data signal from the first transistor Q1. The second transistor Q2 is used to apply a voltage to the liquid crystal LC. Since the voltage is applied directly to the liquid crystal LC, the second transistor Q2 is required to sustain the voltage needed for switching the liquid crystal LC.
This circuit is driven in the following manner. First, when a data signal is input onto the signal line 5, and a scanning signal is applied to the scanning line 4 on scan line 1, the first transistor Q1 in each pixel electrode connected to the scanning line 4 is turned on, and the data signal is applied sequentially to the first transistors Q1 connected to the scanning line 4, the data signal being stored on each associated storage capacitor Cs. Since the second transistor Q2 has the characteristic of being able to control the supply voltage in linear relationship with the scanning signal voltage, a data signal voltage corresponding to the scanning line voltage is applied to the liquid crystal LC. Here, the voltage applied to the liquid crystal LC is controlled by the voltage retained on the storage capacitor Cs; since this voltage is retained until the next field, a constant voltage continues to be applied to the liquid crystal LC. After the first transistor Q1 is turned off, the second transistor Q2 remains in the on state until the first transistor Q1 is turned on again. Accordingly, the second transistor Q2 continues to apply the voltage, corresponding to the data signal voltage from the storage capacitor Cs, to the liquid crystal LC.
In the present invention, ferroelectric liquid crystal is used for the liquid crystal LC. As previously described, ferroelectric liquid crystal materials exhibit spontaneous polarization. When a voltage is applied to a liquid crystal LC having a large spontaneous polarization, a transient current flows due to a change in the orientation of the liquid crystal LC, In the case of ferroelectric liquid crystal, the change of the orientation takes several tens of microseconds, during which time the transient current flows. As for the time required to write data to the scanning lines 4, if a total of 1125 scanning lines 4 are to be scanned in 1/30 second, the scanning time per line is about 30 microseconds. To implement the field sequential color system, the write time needs to be shortened to one-third of that time, which means the write time allowed for one scanning line 4 is about 10 microseconds. Since the transient current flows for a period longer than the write time, proper display cannot be produced by a conventional line sequential method since the voltage being applied to the liquid crystal LC varies due to the transient current that flows after the write period.
However, according to the configuration of the driving circuit and the driving method for the present invention, a constant voltage continues to be applied to the liquid crystal LC (ferroelectric liquid crystal) beyond the write period, as explained above. This prevents voltage variations due to the transient current, so that proper display can be produced.
After the scanning signal has been written to the scanning line 4 on scan line 1, the scanning signal is turned off, and the scanning signal is now applied to the scanning line 4 on scan line 2, to write a data signal to each pixel connected to the scanning line 4 on line 2. When data write is complete on the scanning line 4 on scan line 2, the write operation next proceeds to the scanning line 4 on scan line 3. In this manner, data is written across the entire display area, to complete the display of one field.
In the above illustrated example, the circuit is constructed using two transistors and one storage capacitor, but a circuit of any appropriate configuration may be used as long as the circuit has similar functions to those provided by the above-described circuit.
According to the invention, color display based on the field sequential color system can be realized. As a result, the invention is effective in achieving a super high-resolution, single-plate, full color liquid crystal display device.
Various other modifications will be apparent to and can be readily made by those skilled in the art without departing from the scope and spirit of this invention. Accordingly, it is not intended that the scope of the claims appended hereto be limited to the description as set forth herein, but rather that the claims be broadly construed.
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A liquid crystal display device includes: a first substrate having a single-crystalline silicon layer on one surface thereof; a transparent second substrate disposed opposite the first substrate, the surface of the first substrate having the single-crystalline silicon layer thereon facing the second substrate with a ferroelectric liquid crystal layer sandwiched therebetween; and a plurality of circuit elements formed in the single-crystalline silicon layer in a corresponding relationship to each of a plurality of pixel areas formed on the surface of the first substrate which faces the ferroelectric liquid crystal layer.
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FIELD OF THE INVENTION
[0001] The invention relates to agricultural combines. More particularly, it relates to crop processing elements of those combines. Even more particularly, it relates to a harvested crop residue chopper and distribution arrangement for a combine with a straw chopper.
BACKGROUND OF THE INVENTION
[0002] Agricultural combines are large machines that harvest, thresh, separate, and clean agriculturally planted harvested crop that carry corn. The cleaned corn, so obtained, is stored in a corn tank on the combine. As a rule, the threshed-out straw is either chopped and distributed on the field across the width of the cutter head or conducted around the straw chopper and deposited in a swath on the field without being chopped, in order to pick it up subsequently with a baler. The harvested crop residue remaining at the rear outlet of the cleaning arrangement, such as chaff and small straw particles, is distributed across the field by a chaff spreader or is conducted through the straw chopper and distributed across the field.
[0003] DE 199 08 111 C and DE 101 33 965 A describe combines with a straw chopper and two impeller blowers, arranged side by side alongside each other, that follow the straw chopper for the widely distributed straw ejection across the field. The outlet of the straw chopper and the inlet of the impeller blowers are arranged in a housing, that include impeller blades rotating about an approximately vertical axis and are arranged in a plane for the sake of unidirectional harvested crop transfer. The impeller blades are fastened to a central circular cylindrical shaft underneath a cover plate and are brought into rotation by a drive element arranged above the cover plate.
[0004] EP 1 074 175 A and US 2007/0015556A that is seen as establishing a class, describe impeller blowers in which the straw is thrown against the impeller blowers by means of an ejection drum without being chopped at an angle to the combine from above (EP 1 074 175 A) or through a straw chopper in the chopped form at an angle to the combine from below (US 2007/0015556A), the impeller blowers are built up by impeller blades on a circular disk and extend radially and vertically to the surface of the disk. The blades are configured in a wedge shape, where the outer ends of the blade have a greater vertical length than the inner ends of the blades. No blades are provided in the area of the axis of rotation. In EP 1 074 175 A, cylindrical bodies are located therethrough which the shaft driving the impeller blowers extends, while according to US 200710015556 A, a pot shaped attachment for the shaft is located there.
[0005] DE 100 63 554 A describes a combine with a straw chopper that rotates about a vertical axis and includes a conical body about whose circumference the chopper knives are attached in a spiral arrangement.
[0006] U.S. Pat. No. 1,625,353 A describes a combine whose straw shakers eject the straw without chopping it onto an impeller blower with a vertical axis of rotation. The impeller blower includes a conical disk, with blades arranged at its outer edge that extend vertically and radially to the outside.
[0007] As already noted, in the arrangement according to DE 199 08 111 C the outlet of the straw chopper and the inlet of the impeller blower are arranged in a single plane. However, such an arrangement has a disadvantage since the material delivered at the circumference of the straw chopper is inadequately grasped by the impeller blower, since only an (upper) part of it interacts with the lowest part of the impeller blade, while the remaining material falls to the ground. To avoid this problem, circular disks are attached underneath the impeller blades that rotate with the impeller blades, according to DE 101 33 965 A.
[0008] If the disk underneath the impeller blades were omitted in order to avoid the aforementioned problem and a non orthogonal angle between the axis of rotation of the impeller blower and the plane of the outlet of the straw chopper were provided, as is known from US 2007/0015556 A, a considerable part of the harvested crop would be thrown against the inner regions of the blades and towards the axis of rotation by the straw chopper, which would result in a problematical delivery of the harvested crop on the basis of the lower centrifugal force existing there and the missing impeller blades in the area of the axis of rotation. This problem also exists in the case of the arrangements according to EP 1 074 175 A and US 2007/0015556 A.
[0009] DE 100 63 554 A refers to only one straw chopper and cannot contribute to the solution of this problem, since it does not concern itself with the transition of the harvested crop residue from a straw chopper to an impeller blower, this is the same as U.S. Pat. No. 1,625,353 A that describes only one impeller blower.
SUMMARY OF THE INVENTION
[0010] The problem underlying the invention is seen in the need to make available harvested crop residue chopper and distribution arrangement of the kind cited initially for a combine, that permits an improved flow of harvested crop residue. This problem is solved according to the invention by the teaching of patent claim 1 , where the further patent claims cite characteristics that further develop the solution to great advantage.
[0011] In accordance with one aspect of the Invention, a chopper and distribution arrangement for harvested crop residue is provided that includes a straw chopper with an outlet arranged in the plane of the outlet that chops the straw and/or the chaff conducted to it and ejects it in the plane of the outlet. An impeller blower (or two or more impeller blowers arranged side by side alongside each other) is arranged downstream of the outlet of the straw chopper that includes impeller blades that can be brought into rotation by an appropriate drive about an axis of rotation in the plane of a impeller blower. The plane of the outlet of the straw chopper and the plane of the impeller blower are inclined relative to each other—that is, they are not parallel to each other, but are arranged inclined to each other by an angle differing from 0°. Preferably the plane of the impeller blower is inclined downward relative to the forward operating direction of the combine and further to the rear than the plane of the outlet, so that the harvested crop residue ejected to the rear from the straw chopper is deflected downward by the impeller blower at the aforementioned angle. This angle avoids the aforementioned transition problems or the need for a lower disk located underneath the impeller blade. In order to prevent harvested crop residue from reaching the radially inner region of the impeller blower and being inadequately carried away from that area, the invention proposes that the impeller blades be connected to a central cylindrical body and to provide it with a conical shape facing the outlet of the straw chopper. The conical shape deflects harvested crop residue ejected by the straw chopper to the outside in a radial direction, so that it is grasped by the impeller blades and ejected. The actual body of the impeller blower of the inner region rotates at a low circumferential speed or none and covers it so that no harvested crop residue exists there.
BRIEF DESCRIPTION OF THE DRAWINGS
[0012] An embodiment of the invention is explained on the basis of the illustrations.
[0013] FIG. 1 shows a partial section of a side view of a combine with a straw chopper and impeller blowers.
[0014] FIG. 2 shows an enlarged side view of the straw chopper and an impeller blower in a first operating position.
[0015] FIG. 3 shows a perspective view of the impeller blowers and their retention as seen from below.
[0016] FIG. 4 shows an enlarged side view of the straw chopper and of an impeller blower in a second operating position.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
[0017] In the following description and claims, directions such as “front”, “forward”, “forwardly” refer to the forward operating direction of the combine 10 (i.e. pointing to the left in FIG. 1 ). Directions such as “rear”, “rearward”, “rearwardly”, refer to a direction that is opposite to the forward operating direction of the combine 10 .
[0018] FIG. 1 shows an agricultural combine 10 with a chassis 12 with wheels 14 in contact with the ground. Wheels 14 are fastened to the chassis 12 and are used for the forward propulsion of the combine 10 in the forward operating direction. The forward operating direction is to the left in FIG. 1 . The operation of the combine 10 is controlled from the operator's cab 16 . A cutter head 18 is used in order to harvest crop containing corn and to conduct it to a slope conveyor 20 . The harvested crop is conducted by a guide drum 22 to a slope conveyor 20 . The guide drum 22 guides the harvested crop through an inlet transition section 24 to an axial harvested crop processing arrangement 26 .
[0019] The harvested crop processing arrangement 26 includes a rotor housing 34 and a rotor 36 , arranged within it. The rotor 36 includes a hollow drum 38 to which crop processing elements are fastened for a charging section 40 , a threshing section 42 , and a separating section 44 . The charging section 40 is arranged at the front end of the axial harvested crop processing arrangement 26 . The threshing section 42 and the separating section 44 are located downstream in the longitudinal direction and to the rear of the charging section 40 . The drum 38 is in the form of a truncated cone located in the charging section 40 . The threshing section 42 includes a forward section in the form of a truncated cone and a cylindrical rear section. The cylindrical separating section 44 of the drum 38 is located at the end of the axial harvested crop processing unit 26 . In place of an axial harvested crop processing unit 26 a tangential threshing drum with a following axial threshing section or a straw chopper could also be used.
[0020] Corn and chaff that fall through a thresher basket associated with the threshing section 42 and through a separating grate associated with the separating section 44 are conducted to a cleaning system 28 with a blower 46 and sieves 48 , 50 with louvers. The sieves can be oscillated in a fore-and-aft direction. The cleaning system 28 removes the chaff and guides the clean corn over a screw conveyor 52 to an elevator for clean corn (not shown). The elevator for clean corn deposits the clean corn in a corn tank 30 . The clean corn in the corn tank 30 can be unloaded by means of an unloading screw conveyor 32 to a corn wagon, trailer, or truck. Harvested crop remaining at the lower end of the lower sieve 50 is again conducted to the harvested crop processing arrangement 26 by a screw conveyor 54 and an overhead conveyor (not shown). The harvested crop residue delivered at the upper end of the upper sieve 48 that consist essentially of chaff and small straw particles are conveyed by means of an oscillating sheet conveyor 56 to the rear and to a lower inlet 58 of a straw chopper 60 .
[0021] Threshed-out straw leaving the separating section 44 is ejected through an outlet 62 from the harvested crop processing arrangement 26 and conducted to an ejection drum 64 . The ejection drum 64 that interacts with a sheet 66 arranged underneath it to eject the straw to the rear. A wall 68 is located to the rear of the ejection drum 64 . The wall 68 guides the straw into an upper inlet 70 of the straw chopper 60 .
[0022] The straw chopper 60 is composed of a housing 72 with a rotor 74 arranged within it that can rotate about an axis extending horizontally and transverse to the direction of operation, and is also composed of chopper knives 76 , pendulously suspended in pairs and distributed around the circumference of the rotor 74 , that interact with opposing knives 78 , fixed to the housing. Two impeller blowers 82 arranged side by side alongside each other, are provided downstream of an outlet 80 of the straw chopper 60 . Only a single blower 82 can be seen in FIG. 1 . The impeller blowers 82 include a number of impeller blades 84 , each of which is connected rigidly to an upper circular disk 86 , that can rotate about central axes 88 . The disks 86 with the impeller blades 84 that extend radially can be brought into rotation by a hydraulic motor 90 that is attached above a bottom sheet 102 which is connected with the housing 72 of the straw chopper 60 . At their radially inner ends the impeller blades 84 are connected to a cylindrical central body 92 that transitions into a cone 94 with a point on its end facing away from the disk 86 . The impeller blades 84 are rectangular and the height of the body 92 (without cone 94 ) is equal to the height of the impeller blades 84 . The cross section of the body 92 and the cone 94 is circular, although it could also have a multifaceted shape.
[0023] As can be seen in FIG. 2 , the straw chopper 60 defines an outlet plane 86 extending at an angle to the rear and upward in which the harvested crop residue is ejected. The impeller blades 84 of the impeller blowers 82 on the other hand rotate in a plane of the impeller blowers 98 that extends to the rear and downward. The harvested crop residue are conveyed by the impeller blower 82 in the plane of the impeller blower 98 and ejected to the rear and to the side and distributed on the field across the width of the cutter head 18 . The lowest regions of the cone 94 including its point are arranged underneath the plane of the outlet 96 in the operating position of the impeller blowers 82 according to FIG. 2 . On the other hand the regions of the cone 94 located above these are arranged within the flow of the harvested crop residue ejected by the straw chopper.
[0024] As indicated by the arrow 100 the cone 94 deflects the harvested crop residue (straw and/or chaff) impacted on it from the straw chopper 60 upward and to the side, so that it can be grasped by the impeller blades 84 . Due to the relatively large diameter of the body 92 , the circumferential speed of all the areas of the impeller blowers 94 that interact with the flow of the harvested crop residue are sufficiently large so as to readily accommodate the flow of the harvested crop residue.
[0025] FIG. 3 shows a perspective view of the impeller blowers 82 that operated in opposite directions during the operation. The directions of rotation are indicated by arrows on each impeller in FIG. 3 . A harvested crop flow separating element 106 , arranged to the rear of the axes of rotation 88 of the impeller blowers 82 , includes a forward point that intrudes into the intermediate region between the impeller blowers, and two side walls, each of which adjoins an impeller blower 82 . Retainers 109 are used to attach the bottom sheet 102 with the impeller blowers 82 at the housing 72 of the straw chopper 60 .
[0026] The impeller blowers 82 can be adjusted by means of appropriate adjusting mechanisms to pivot about an axis 108 that extends through the center of the body 92 and also extends horizontally and transverse to the direction of operation. This relative pivoting can be seen in FIGS. 2 and 4 ; in which one pivoted position is shown in FIG. 2 in the second pivoted position is shown in FIG. 4 . The pivoting can be performed manually by an operator or by means of external forces in order to vary the ejection distance of the impeller blowers.
[0027] It should be noted that an adjustable flap could still be arranged between the ejection drum 64 and the upper inlet 70 of the straw chopper 60 with which the straw can selectively slide past the rear of the straw chopper 60 and can be deposited in a swath on the field in the long straw deposit operation.
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A harvested crop residue chopper—and distribution arrangement for a combine ( 10 ) has a straw chopper ( 60 ) with an outlet ( 80 ) arranged in the plane of the outlet ( 96 ), with at least one impeller blower ( 82 ) arranged downstream of the outlet ( 80 ) of the straw chopper (60) with impeller blades ( 84 ) that can be rotated in the plane of the impeller blower ( 98 ) about an axis of rotation ( 88 ), where the plane of the impeller blower ( 98 ) may be inclined relative to the plane of the outlet ( 96 ). The impeller blades ( 84 ) make be connected with a central body ( 92 ) that is connected to a cone ( 94 ) facing the outlet ( 80 ) of the straw chopper ( 60 ).
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BACKGROUND OF THE INVENTION
1. Field of the Invention
This invention relates to the injection of fluids having nuclei detectable by NMR measuring devices into wells for purposes of well stimulation, secondary-type oil recovery, reservoir modification, permeability control, and fluid encroachment prevention; and the selection of materials for such uses. More particularly, it relates to the injection of fluids, containing nuclei detectable by NMR detection devices, which interact with the reservoir and/or with fluids in the reservoir in conformance with predetermined criteria.
2. Description of the Prior Art
Pulsed NMR has been used in the field of well logging to determine the presence of hydrocarbons. See U.S. Pat. Nos. 3,456,183, 3,289,072, and 3,528,000; publications by Loren et al, Soc. Petrol. Engrs. Preprint 2529 (1969), Timur et al, Soc. Petrol. Well Logging Analysts Symposium, (May 2-5, 1971); Senturia et al, Soc. Petrol. Engrs. Journal (Sept. 1970), p. 237. In the course of some of these logging processes, fluids having paramagnetic properties have been injected to cancel out the "noise" background of water in the reservoir. Nuclear magnetic resonance has also been utilized in the analysis of a wide variety of liquid-solid systems, e.g. in biology, in geology (in the determination of the water saturation of clays).
Many fluids are used in petroleum production operations which contain nuclei detectable by NMR devices, such as the pulsed NMR detection devices. The fluids used in these processes include semi-polar compounds such as alcohols used as cosurfactants, surfactants of various sorts such as the petroleum sulfonate surfactants and certain polymers. These fluids are used in a variety of processes where fluids are injected into wells drilled into formations. These include injection for corrosion inhibition, U.S. Pat. No. 3,072,192; oil recovery, U.S. Pat. Nos. 3,254,714, 3,261,399, 3,506,070, 3,599,715, and 3,759,325; separation of gas and oil and oil and water interfaces, U.S. Pat. Nos. 3,495,661 and 3,710,861; well stimulation, U.S. Pat. No. 3,568,772; water coning inhibition, U.S. Pat. No. 3,554,288; prevention of salt water encroachment, U.S. Pat. No. 3,587,737; formation fracturing, U.S. Pat. No. 3,603,400; plugging, U.S. Pat. No. 3,604,508, acidizing, U.S. Pat. No. 3,831,679 and in drilling fluids, U.S. Pat. No. 3,734,856. The fact that the processes of the instant invention can be used with such a wide variety of oil field operations makes the invention particularly important.
SUMMARY OF THE INVENTION
Many references teach well treatment and oil recovery techniques. Many of these processes use fluids which can be designed through use of NMR techniques to design fluids having minimal interaction.
The procedures pertinent to secondary-type oil recovery are also useful in selecting fluids for well stimulation, prevention of fluid encroachment and foam flooding. In other instances, the fluids injected must react with either fluids in the reservoir or with the reservoir itself. These include some forms of prevention of fluid encroachment, plugging, mobility control and acidizing. In such instances, the fluids selected for injection will be those which are most interactive with the fluids in the reservoir and/or the reservoir rock itself. From the above, it is readily apparent that one desiring to use NMR in injected fluid selection will have to predetermine the criteria necessary for the fluid to be injected. That is, whether the fluid will or will not interact with the fluid and/or rock in the reservoir.
The term "interact" for purposes of this invention, means:
(a) the chemical reaction of injected fluid or components thereof with organic or inorganic components of reservoir fluids to form precipitate, to form a surface tension changing agent, to provide a compound for changing the rate of chemical or physical reaction or change, or to change permeability of all or a portion of a reservoir;
(b) the changing of surface tension;
(c) the sorption of injected material onto or the elution of material from the rock surface;
(d) the dissolution of injected particles; or
(e) solution or solubilization of fluids by fluids containing surfactant and/or semi-polar organic compounds.
DESCRIPTION OF THE INVENTION
This invention comprises contacting a porous matrix substantially representative of a fluid-bearing subterranean strata with fluids containing nuclei detectable by nuclear magnetic resonance measuring devices and selected by: determining the NMR response to each nuclei-bearing fluid in association with said matrix, determining the NMR response of one or more samples of each fluid or component thereof to be brought into contact with the matrix, determining the NMR response of each such sample fluid or component thereof while in contact with the fluids in association with said matrix in said matrix, and contacting the subterranean strata with the fluid which substantially meets predetermined criteria for interaction with the matrix and/or fluid associated with the matrix.
The process is preferably used in processes for the production of crude oil and most preferably in the selection of fluids for secondary type oil recovery.
While the process is useful in any of the processes described in the above-listed patents, it will be most particularly described with reference to secondary-type oil recovery operations, i.e., recovery operations after completion of primary oil recovery.
More specifically, the selection of various ingredients for use in oil recovery can be made on the basis of core floods monitored by nuclear magnetic resonance detection devices; preferably, by pulsed nuclear magnetic resonance. Generally, a measurement, e.g. spin-lattice relaxation time (T), is separately made for each of the components of the fluid to be injected into the reservoir and of the whole fluid(s) to be injected, and for each of the in situ reservoir fluids as reconstituted within the core. A portion of the oil and in situ water is then displaced by injection of a quantity of the injected displacement fluids. The NMR measurements are then taken for the core together with each of the injected and in situ components. Fluids which contribute minimally to the displacement of the in situ fluids and/or which are destroyed by interaction with the in situ fluids and/or the rock sample are replaced by fluids or fluid components which interact with the in situ fluids in the rock to better displace one or more of the in situ fluids and/or enhance the integrity of the injected fluids. For example, nonyl phenol can be substituted for a more water-soluble alcohol such as isopropanol if a micellar dispersion which is relatively hydrophilic in character containing isopropanol is destroyed by the in situ fluids and a more hydrophobic dispersion is required or a lower mean equivalent weight petroleum sulfonate can be substituted if the NMR measurements indicate a need for a more hydrophilic micellar system.
The invention will find its primary use in the selection of micellar systems of water and surfactant; water, surfactant, and cosurfactant; or water, surfactant, cosurfactant, and hydrocarbon (whether oil-external, water-external, or of intermediate externality), water and cosurfactant (alcohol) systems for use in various processes leading to oil recovery.
BRIEF DESCRIPTION OF DRAWINGS
FIGS. 1a, 1b and 1c are graphic representations of the results of Example 2 which the "ideal" or expected NMR response for a miscible piston-like displacement (shown by open circles) is compared to the measured or observed NMR response of the displacement liquid. Curve A shows the amount (in pore volumes) of slug injected vs. the water displaced by the PV slug; Curve B shows the amount of slug injected vs. the oil displaced by the slug; Curve C shows the amount of slug injected vs. the intact slug in the core. The difference between the ideal NMR response and the observed NMR response in any of the curves is indicative of an ineffective displacement fluid. (FIGS. 3-9 relate the same type of information but in relation to different examples.)
FIGS. 2a, 2b and 2c are graphic representations of NMR outputs of Example III.
FIGS. 3a, 3b and 3c are graphic representations of NMR outputs of Example IV.
FIGS. 4a, 4b and 4c are graphic representations of the NMR outputs of Example V.
FIGS. 5a, 5b and 5c are graphic representations of the NMR outputs of Example VI.
FIGS. 6a, 6b and 6c are graphic representations of the NMR outputs of Example VII.
FIGS. 7a, 7b and 7c are graphic representations of the NMR outputs of Example VIII.
FIGS. 8a, 8b and 8c are graphic representations of the NMR outputs of Example IX.
FIGS. 9a, 9b and 9c are graphic representations of the NMR outputs of Example X.
Each of the curves shows the amounts of PV slug injected vs. the oil displaced by the slug. As the proportion of CaCl 2 in the displacement liquid increased from Curve A to Curve C, the difference between the ideal NMR output and the observed NMR output for the displacement liquid decreased and the percentage of oil recovery increased.
FIGS. 10a, 10b and 10c are graphic representations of the NMR outputs of Example XI. The curves represent the amount of slug injected vs. the amount of oil displaced by the slug, and show the changes in the difference between the ideal NMR output and the observed NMR output of the displacement liquid as the proportion of primary amyl alcohol of the displacement liquid is altered. The curve which shows the least difference between the ideal and observed NMR output is of the sample showing the greatest oil recovery.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
NMR Outputs: The NMR outputs utilized with the invention can be the free induction decay amplitude which is proportional to the concentration of responding materials or can be the spin-lattice relaxation rate or the spin-spin relaxation rate of the individual component. For additional precision of selection of components, the change in both the relaxation time and the amplitude of a particular component can be observed.
NMR Apparatus: Conventional wideband pulsed NMR apparatus including those commercially available can be utilized without modification. The data presented herein were obtained by the use of a wideband pulsed NMR, Model No. B-KR-322S, produced by Bruker-Physik AG of Karlsruhe, Germany. The instruction manual contains a list of 51 nuclei useful in forming desired fluids. As used herein, "NMR" also includes nuclear magnetic log and analogous techniques.
Analytical Techniques: A convenient technique for use with the present invention is to utilize small cores, e.g. the 0.89 cm diameter by 2.0 cm long cores from the reservoir to be flooded or another representative rock. The more common 1-inch (2.54 cm) by 3-inch (7.62 cm) cores may also be employed provided the apparatus utilized for measuring NMR can accommodate them. Discs and larger cores can be substituted if they can be accommodated by the NMR apparatus.
Displacement Fluid Components: The ingredients of the displacement fluid can be selected from those conventionally employed, e.g. micellar systems commonly containing hydrocarbons, sulfonates such as petroleum sulfonates, cosurfactants, e.g., isopropanol and water; alcohols, e.g., ethanol, isopropanol; surfactant floods comprising water and a surface active agent; thickened water floods in which the mobility of the displacement fluid is adjusted by the addition of polymers such as polyacrylamide, polyethylene oxide, carboxymethyl cellulose, biopolymers and the like. Polymers of the polar types listed are, however, difficult--and sometimes impossible--to measure utilizing pulsed nuclear magnetic resonance in its present state of development.
The methods needed to take the desired nuclear magnetic resonance measurements are well known to those skilled in the art as are the selection of fluids to be injected which contain sufficient amounts of protons to be measurable using nuclear magnetic resonance detecting devices. The particular method used, the temperature at which the measurements are made, etc. are not critical and any desired method may be selected. Preferably, however, the rock sample or matrix being utilized, the reservoir fluids, and fluid compositions being utilized, should closely simulate the actual reservoir conditions, rock and fluid compositions. Most preferably, the rock and fluids will be taken from the reservoir and measurements will be taken at reservoir temperatures.
Temperature: The temperature is not narrowly critical, but preferably, should be the same during each NMR measurement. Additional accuracy can be obtained by running both sets of NMR measurements at the approximate temperature to be encountered in the subterranean reservoir.
The following examples more fully describe the invention but are not to be taken as limiting:
EXAMPLE I
To illustrate the practice of the invention, a series of displacement processes in which decane (substituted for petroleum because its NMR characteristics are sharply different from those of the displacement fluids and provide better illustration of the practice of the invention) and water are displaced from sandstone and ceramic cores (as described in each of the tables below) with a water-external micellar dispersion (See British Pat. No. 1,378,724). The slugs are composed of different materials and interaction between slug components and the rock sample is observed as slug injection proceeds.
In each slug, the core (approximately 0.89 cm diameter by 20 cm length) is initially saturated with water, then flooded with decane to S wi followed by water to S or , prior to injection of the slug. This process simulates tertiary recovery (after normal water flooding) of a petroleum reservoir. During injection of a micellar system, each flood is periodically stopped and a free induction decay of spin-lattice relaxation decay (T 1 ) measured by use of the specific NMR equipment described above. These NMR outputs are obtained for each of the nuclei-containing materials in the core. From these outputs, the slug saturation (f s ), water saturation (f w ) and oil saturation (fc 10 ) are determined from a knowledge of the T 1 of the components. In certain of the examples, in order to observe micellar slug solubilization by water in place and decane, the drive fluid is prepared with deuterium oxide in place of water and with a chlorocarbon in place of the hydrocarbon.
Data analysis is accomplished by comparing experimentally determined saturations to those expected for completely miscible piston-like displacement, i.e. "ideal" displacement. Other assumptions are that no oil is produced until after the first 0.25 PV of slug injection and that all in situ water and oil are produced at 1 PV slug injection.
EXAMPLE II
A water-external slug is prepared with H 2 O so that response from the slug is due to H 2 O and surfactant alone. Table 1 and FIG. 1 show the results obtained for the displacement from a sandstone core. FIG. 1 shows that this displacement is almost piston-like with respect to both oil and water. Only in the very early part of the flood is there some dilution of the slug by in situ water. By 0.5 PV slug injection, the water, oil and slug saturations follow exactly that expected for a miscible piston-like displacement. Oil recovery for the slug was 97% at 1 PV slug injection.
EXAMPLE III
Results for the same flood of Example II in a ceramic core are shown in Table 2 and FIG. 2. Unlike the flooding data shown in FIG. 1, there is a mild dilution of the slug of the in situ water at 0.5 PV slug injection. This leads to inefficient oil displacement, i.e. the oil saturation exceeds that expected, and an ultimate recovery of 71%.
EXAMPLES IV & V
These examples utilize similar floods to those of Examples II and III with the exception that the slug is prepared with D 2 O instead of water so that the only component of the slug that was seen by NMR was the surfactant. The results are as shown in Tables 3 and 4 and FIGS. 3 and 4. Oil recovery, 17% and 56% for both slugs respectively, is poor. This is due to immediate dilution of the slug by in situ water and an ultimate bypass of in-place oil.
EXAMPLES VI-IX
These examples are conducted in the same manner as were Examples II-V with the exception that the micellar slugs are oil-external. The results are shown in Tables 6-9 and FIGS. 6-9. The oil recovery of all of these examples are poor. The figures show the dilution of the slug by reservoir water is severe and occurs early in the flood. The extent of the dilution with water is more pronounced in the sandstone than in the ceramic core material. Following dilution with water the slug displaces only reservoir water and left the oil essentially in place. In the ceramic core material oil is solubilized into the slug; this is the only oil produced.
EXAMPLE X
Using the same technique employed in Examples II-IX and employing a micellar slug having the composition: 14.0 weight percent petroleum sulfonate (420 equivalent weight), 73.5 percent water, and 12.5 percent hydrocarbon, a sandstone core is first flooded with the slug alone and the NMR spin lattice relaxation rate measured. Similar individual measurements are made for the core saturated with petroleum-in-place and, separately with the reservoir water. The NMR outputs are shown as the closed curves in FIG. 11, graphs A, B and C. Curve A represents the first result using the above micellar system containing no primary amyl alcohol.
Next the core is flooded with the oil in place and thereafter flooded with water to simulate tertiary recovery as described above. The core is then successively flooded with 0.25, 0.50, and 1.0 pore volumes of micellar solution and the NMR spin lattice relaxation rate is measured at each point. These NMR values measured on the combination of fluids are shown as the black circles in Curve A.
Comparison of the calculated NMR curve (open circles) and the composite NMR curve (black circles) indicates substantial differences between the respective values, indicating that the micellar system will be relatively inefficient during an actual displacement flood.
Accordingly, 0.75 mls of primary amyl alcohol per 100 gms slug is added to a reformation of the above micellar displacement slug and the individual NMR measurements, the calculations and the composite NMR measurements are repeated as above. Inspection of graph 9B indicates that the differences in NMR values are substantially lessened, indicating the improvement in predicted efficiency caused by the addition of the primary amyl alcohol.
To determine whether further efficiency can be obtained by adding more primary amyl alcohol, graph 9C is obtained using corresponding measurements on a slug containing 1.58 mls of an amyl alcohol per 100 gms of slug. As can be seen from inspection of graph 9C, the predicted efficiency is not improved so the expense of adding these additional quantities of a relatively expensive alcohol component can be avoided.
EXAMPLE XI
Using the same techniques employed in Example X and the same basic micellar slug composition, the effect of the amount of calcium chloride dissolved in the in situ water is studied.
Inspection of graphs 10A, 10B, and 10C readily shows that the micellar system of graph 10C described in Example X above, is most efficient in reservoirs containing in situ water having high (4,000 ppm) calcium chloride compositions.
TABLE 1__________________________________________________________________________WATER-EXTERNAL SLUG - H.sub.2 O AND SURFACTANT RESPONSESANDSTONE CORECore* Condition PV Flood f.sub.s f.sub.w f.sub.c10 T.sub.s (msec) T.sub.w (msec) T.sub.c10 (msec)__________________________________________________________________________100% H.sub. 2 O 0.28 0.72 -- 52 340 --100% Slug** 0.24 0.76 -- 20 180 --C.sub.10 displaced by H.sub.2 O 10 0.63 -- 0.37 130 -- 1600H.sub.2 O/C.sub.10 displaced bySlug 0.25 0.26 0.22 0.52 91 180 1600 0.5 0.41 0.30 0.29 110 190 1600 1.0 0.26 0.74 < 0.01 43 270 1600 5.0 0.23 0.77 < 0.01 35 250 1600__________________________________________________________________________ *Sandstone core - [C. Neville No. 2, Byron Tensleep], porosity, Φ = 20%, permeability, k = 120 mD **Slug composition 8.5 wt % 410 EW gas oil sulfonate 59.6 wt % H.sub.2 O 28.6 wt % Chlorocarbon (C.sub.4 3.3 wt % IPA Slug relaxation characteristics: f.sub.s = 0.07, T.sub.s = 40 msec, T.sub.L = 1800 msec Brookfield viscosity = 35 cp at 6 rpm f = fraction T = spin-lattice relaxation decay s = slug w = water C.sub.10 = oil (decane)
TABLE 2__________________________________________________________________________WATER-EXTERNAL SLUG- H.sub.2 O AND SURFACTANT RESPONSECERAMIC CORECore* Condition PV Flood f.sub.s F.sub.w f.sub.c10 T.sub.s (msec) T.sub.w (msec) T.sub.c10 (msec)__________________________________________________________________________100% H.sub.2 O -- 1.0 -- -- 640 -- --100% Slug** -- 0.44 0.56 -- 220 610 --C.sub.10 displaced by H.sub.2 O 10 0.66 -- 0.34 370 -- 1600H.sub.2 O/C.sub.10 displaced bySlug 0.25 0.23 0.38 0.39 230 450 1600 0.5 0.49 0.19 0.32 230 810 1600 1.0 0.51 0.39 0.10 210 560 1600 4.0 0.38 0.62 0.01 170 450 1600__________________________________________________________________________ *Ceramic Core (DP 12C), Φ = 40%, k = 210 ml) **Slug composition 8.5 wt % 410 EW gas oil sulfonate 59.6 wt % H.sub.2 O 28.6 wt % Chlorocarbon (C.sub.4 3.3 wt % IPA Slug relaxation characteristics: f.sub.s = 0.07, T.sub.s 32 40 msec, T.sub. L = 1800 msec Brookfield viscosity = 35 cp at 6 rpm
TABLE 3__________________________________________________________________________WATER-EXTERNAL SLUG - SURFACTANT RESPONSESANDSTONE CORECore* Condition PV Flood f.sub.s f.sub.w f.sub.c10 T.sub.s (msec) T.sub.w (msec) T.sub.c10 (mesc)__________________________________________________________________________100% H.sub.2 O -- 0.28 0.72 -- 52 340 --100% Slug** -- 0.33 0.67 -- 42 260 --C.sub.10 displaced by H.sub.2 O 10 0.70 -- 0.30 120 -- 1600H.sub.2 O/C.sub.10 displaced by Slug 0.25 0.21 0.28 0.51 44 260 1600 0.50 0.21 0.33 0.46 38 250 1600 1.0 0.06 0.69 0.25 40 150 1600 5.0 0.19 0.67 0.14 38 170 1600__________________________________________________________________________ *Sandstone core - C. Neville No. 2, Φ = 20%, k = 120 **Slug composition: 8.0 wt % 410 EW gas oil sulfonate 61.8 wt % D.sub.2 O 27.0 wt % Chlorocarbon (C.sub.4 3.2 wt % IPA Slug relaxation characteristics: f.sub.s = 0.50, T.sub.s = 34 msec, T.sub.L = 560 msec Brookfield viscosity = 46 cp at 6 rpm
TABLE 4__________________________________________________________________________WATER-EXTERNAL SLUG - SURFACTANT RESPONSECERAMIC CORECore* Condition PV Flood f.sub.s f.sub.w f.sub.c10 T.sub.s (msec) T.sub.w (msec) T.sub.c10 (msec)__________________________________________________________________________100% H.sub.2 O 1.0 -- -- 640 -- --100 % Slug** 0.49 0.51 -- 130 830 --C.sub.10 displaced by H.sub.2 O 10 0.66 -- 0.34 330 -- 1600C.sub.10 /H.sub.2 O displaced by Slug 0.25 0.17 0.29 0.54 99 410 1600 0.5 0.25 0.08 0.67 92 340 1600 1.0 0.44 0.41 0.15 120 950 1600 5.0 0.41 0.42 0.17 100 420 1600__________________________________________________________________________ *Ceramic Core (DP 12C), Φ = 40%, k = 210 **Slug composition: 8.0 wt % 410 EW gas oil sulfonate 61.8 wt % D.sub.2 O 27.0 wt % Chlorocarbon (C.sub.4 3.2 wt % IPA Slug relaxation characteristics: f.sub.s = 0.5, T.sub.s = 34 msec, T.sub. - 560 msec Brookfield viscosity = 46 cp at 6 rpm
TABLE 5__________________________________________________________________________OIL-EXTERNAL SLUG - H.sub.2 O AND SURFACTANT RESPONSESANDSTONE CORECore* Condition PV Flood f.sub.s f.sub.w f.sub.c10 T.sub.s (msec) T.sub.w (msec) T.sub.c10 (msec)__________________________________________________________________________100% H.sub.2 O -- 0.28 0.72 -- 52 340 --100% Slug** -- 0.38 0.62 -- 11 89 --H.sub.2 O displaced by C.sub.10 15 0.29 -- 0.71 44 -- 1600C.sub.10 displaced by H.sub.2 O 15 0.18 0.42 0.40 20 200 1600H.sub.2 O/C.sub.10 displaced by Slug 0.25 0.26 0.27 0.47 30 220 1600 0.50 0.32 0.18 0.50 32 240 1600 1.0 0.38 0.38 0.24 32 290 1600 6.0 0.39 0.57 0.04 19 150 1600__________________________________________________________________________ *Sandstone core - c. Neville No. 2, Φ = 20%, k = 120 **Slug composition: 7.1 wt % Shell Sulfonate 19.1 wt % H.sub.2 O 2.8 wt % IPA 71.0 wt % Chlorocarbon (C.sub.4 Slug relaxation characteristics: f.sub.2 = 0.20, T.sub.s = 75 msec, T.sub.L = 1600 msec Brookfield viscosity = 26 cp at 6 rpm
TABLE 6__________________________________________________________________________OIL-EXTERNAL SLUG - H.sub.2 O AND SURFACTANT RESPONSECERAMIC CORECore* Condition PV Flood f.sub.s f.sub.w f.sub.c10 T.sub.s (msec) T.sub.w (msec) T.sub.c10 (msec)__________________________________________________________________________100% H.sub.2 O 1.0 640100% Slug** 0.38 0.62 62 340C.sub.10 displaced by H.sub.2 O 10 0.67 -- 0.33 300 -- 1600H.sub.2 O/C.sub.10 displaced by Slug 0.2 0.10 0.56 0.34 62 342 1600 0.4 0.16 0.47 0.37 61 350 1600 0.9 0.21 0.48 0.31 59 270 1600 5.0 0.39 0.54 0.07 73 340 1600__________________________________________________________________________ *Ceramic core (DP 12C), Φ = 40%, k = 210 **Slug composition: 7.1 wt % Shell Sulfonate 19.1 wt % H.sub.2 O 2.8 wt % IPA 71.0 wt % Chlorocarbon (C.sub.4 Slug relaxation characteristics: f.sub.s = 0.20, T.sub.s =75 msec, T.sub. = 1600 msec Brookfield viscosity = 26 cp at 6 rpm
TABLE 7__________________________________________________________________________OIL-EXTERNAL SLUG - SURFACTANT RESPONSESANDSTONE CORECore* Condition PV Flood f.sub.s f.sub.w f.sub.c10 T.sub.s (msec) T.sub.w (msec) T.sub.c10 (msec)__________________________________________________________________________100% H.sub.2 O 0.28 0.72 -- 52 340 --100% Slug** 0.27 0.73 -- 54 120 --H.sub.2 O displaced by C.sub.10 15 0.29 -- 0.71 44 -- 1600C.sub.10 displaced by H.sub.2 O 15 0.21 0.43 0.36 20 160 1700H.sub.2 O/C.sub.10 displaced by Slug 0.25 0.27 0.27 0.46 30 170 1500 0.50 0.32 0.21 0.47 30 200 1700 1.0 0.39 0.32 0.29 30 220 1400 5.0 0.28 0.72 -- 22 170 --__________________________________________________________________________ *Sandstone core - C. Neville No.2, Φ = 20%, k = 120 **Slug composition 6.9 wt % Shell sulfonate 20.6 wt % D.sub.2 O 2.8 wt % IPA 69.7 wt % Chlorocarbon (C.sub.4 Slug relaxation characteristics: f.sub.s = 0.61, T.sub.s = 90 msec, T.sub.L = 770 msec
TABLE 8__________________________________________________________________________OIL-EXTERNAL SLUG - SURFACTANT RESPONSECERAMIC CORECore* Condition PV Flood f.sub.s f.sub.w f.sub.c10 T.sub.s (msec) T.sub.w (msec) T.sub.c10 (msec)__________________________________________________________________________100% H.sub.2 O -- 1.0 640100% Slug** -- 0.46 0.54 66 300C.sub.10 displaced by H.sub.2 O 10 0.62 -- 0.38 290 1600H.sub.2 O/C.sub.10 displaced by Slug 0.25 0.16 0.44 0.40 59 350 1600 0.50 0.23 0.39 0.38 60 330 1600 1.0 0.26 0.42 0.32 62 290 1600 5.0 0.31 0.56 0.13 62 200 1600__________________________________________________________________________ *Ceramic Core (DP 12C), Φ = 40%, k = 210 **Slug composition 6.9 wt % Shell sulfonate 20.6 wt % D.sub.2 O 2.8 wt % IPA 69.7 wt % Chlorocarbon (C.sub.4 Slug relaxation characteristics: f.sub.s = 0.61, T.sub.s = 90 msec, T.sub.L = 770 msec
During the course of a field-scale flooding operation, cores are sometimes taken to determine the effect of the injected fluids on oil displacement, the state of the injected fluids and the conformance of the injected with ideal conditions. The originally injected fluids may be modified if such cores, when subjected to analysis by nuclear magnetic resonance detecting devices and other means, shown that there is a difference in the interaction between the injected fluids and fluids found in the newly taken core or that the interaction between the formation fluids and the injected fluids as modulated by time and distance within the reservoir are not as desirable as originally thought.
Another approach to the nuclear magnetic resonance analysis is as follows: The determination of the NMR output for each of the components can be done by calculating the output for each component based on an ideal miscible piston-like displacement (that is, using the assumption that the NMR relaxation rate, T, for each included component remains constant throughout the displacement process.) The NMR value for each component can then be calculated by means of a simple material balance which accounts for injection and production of fluids as displacement proceeds. These calculated NMR values for components can then be compared with measured NMR values for the composite system. This comparison can be repeated at a number of points during the displacement process and deviation from the ideal values minimized by substitution of components where necessary. A more detailed discussion of the calculation is set forth below.
CALCULATION OF IDEAL DISPLACEMENT______________________________________ Equation______________________________________A.sub.s (t) = f.sub.s e.sup.-.sup.t/Ts 1A.sub.w (t) = f.sub.w e.sup.-.sup.t/Tw 2A.sub.o (t) = f.sub.o e.sup.-.sup.t/TW 3A (t) = f.sub.s e.sup.-.sup.t/Ts + f.sub.w e.sup.-.sup.t/Tw + f.sub.oe.sup.-.sup.t/To 4A (t) = A.sub.s (t) + A.sub.w (t) A.sub.o (t) 5______________________________________
where
A(t) is the amplitude
f is fraction of the component
t is time
T is the spin-lattice relaxation time of the component and the s, w and o denote components slug, water and oil respectively.
A s (t) is measured on rock and slug as discussed above and equation 1 used to calculate T s , setting f s = 1.
Similar measurements and calculations are made for T w and T o .
The values of T w , etc. are inserted into equation 4 for various pore volumes of displacement to arrive at the curve of theoretical piston-like displacement.
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Fluids are injected into porous strata for many purposes. These include, for example, well stimulation, secondary-type oil recovery, mobility control, regulation of formation "wetness" and regulation of the encroachment of fluids. Fluids used for the above purposes are readily selected using nuclear magnetic resonance (NMR) measurements in the laboratory to measure the interaction between the fluids being injected into the reservoir rock and the in situ fluids or between injected fluids and the porous material. NMR measurements are taken for each component of sample fluids proposed to be injected in the reservoir for a desired purpose, or the sample fluid per se and each of the in situ fluids. NMR measurements are then taken of the interaction between the nuclei of sample fluids injected, the reservoir rock, and the nuclei of fluids in situ.
If the injected fluid is to be used for some purposes, for example, well stimulation or secondary-type oil recovery, the fluids are selected which interact least with the rock and with in situ fluids. If the wetness of the reservoir is to be changed, then the fluid is selected which interacts well with the reservoir rock. If a material is to be precipitated or formed in situ, the fluid is selected which interacts well with either the reservoir rock or the formation fluids. Additionally, the best combination of components for a particular fluid to be injected can also be determined using NMR, preferably pulsed, detection devices.
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TECHNICAL FIELD
The present invention relates to a knitted lingerie article corresponding to what is currently marketed under the name “boxer short” and which generally designates a short knitted underpants, for men as well as for women of all ages. It is understood here that the term boxer short is not limited to the short underpants but also extends to long underpants, for example of the type known under the name “long boxer short”, “legging”, etc.
BACKGROUND
The boxer short is a relatively complex article as it is intended to cover the low part of the trunk as well as the top part of the thighs over a sufficient length. It comprises a panty portion ended at its upper portion by a belt positioned at the waist, and at its lower portion by two lapels separately positioned on the thighs. It is commonly made from a knitted tube corresponding to a diameter allowing to seamlessly dress the low part of the trunk, and is equipped during a confection operation of a sewn crotch bottom allowing to link the two tubes dressing the thighs. We know how to knit on the circular machines such as the machines SANTONI of SM8-8 type, for example for diameters comprised between 10 and 16 inches (between 25 and 40 cm), tubes intended for of the confection of boxer shorts with a double belt in the top portion and a double lapel in the low portion, this tube may be knitted in both directions (belt-lapel or lapel-belt). We also know the confection of the tube bottom to make the low part of the boxer short, with an attached bottom which can be made on the same type of knitting machine. According to the known prior art of documents US2000073 and FR2805285, the crotch bottom or gusset is a substantially rectangular piece which is put between the edges of two slots or incisions performed at the front and at the back of the knitted tube. The enclosed FIGS. 1 to 3 show in more detail this confection operation. The boxer short 101 is made in the shape of a knitted tube, with an upper belt 102 and a lower border 103 , where lapels or reinforcements corresponding to future thigh passages are formed or may be formed. The knitted tube 101 comprises a front face 105 and rear face 106 (in one piece since it is about a circular knitting). The portion 104 intended to form the front pocket of the boxer short intended to maintain the genitals is represented by hatching on the front face 105 . We proceed ( FIGS. 1 and 2 ) to a cutting operation creating an incision 107 at the front part 105 and an identical or different incision 108 at the back 106 of the knitted tube, in the middle, at its lower portion. The incision 107 has edges 110 , 111 and the incision 108 has edges 112 , 113 . Each incision 107 , 108 is then laterally spaced apart and stretched, as suggested by the arrows of FIGS. 1 and 2 , so as to put substantially, in the extension of one another, the edges 110 , 111 on the one hand and 112 , 113 on the other hand, and form thus substantially rectilinear bottom lines which are sewn together by means of a substantially rectangular crotch bottom 115 (called here “bottom lines” the lower edges of the front and the back of the tubular knitted fabric, intended to be sewn to one another, between the thigh passages, directly or by means of additional pieces of crotch bottom such as the gusset). The document FR2805285 had represented an improvement compared to the classical confection by providing bottom lines with a different length at the front and at the back and by making the crotch bottom 115 with different elastic zones at the front and at the back. This suggestion has allowed to partially solve an often encountered problem with this type of garment, namely the absence of wearing comfort, related in particular to the presence of troublesome seams at the crotch and/or to a bad conformation of this bottom to the anatomy of the wearer, and more particularly to the presence of troublesome seams on the front at the genitals, in particular for man. However, the wearing comfort remains to improve further and this is the purpose of the present invention. More precisely, it is about finding a new method for the confection of the crotch, remaining simple, but leading to an improved comfort.
We know, from the documents WO 2012087210 and WO 2011008138, two methods for the confection of boxer shorts from two knitted rectilinear strips which are applied one on the other. These documents teach that it is possible to tie the two strips together according to some patterns of parallel or T lines which are then incised, so as to give rise to particular crotch shapes. These two methods do not relate to the confection of the boxer shorts from tubular knitted fabric and do not give transposable teaching to this manufacturing method.
BRIEF SUMMARY
The purpose of the invention is achieved thanks to a method for manufacturing a boxer short comprising the circular knitting of a main tube, the preparation of a crotch bottom, the cutting in the low portion at the front and at the back of the incisions tube, the opening by lateral extension of the incisions to form first and second globally transverse bottom lines and the sewing of the crotch bottom to the globally transverse bottom lines for forming the crotch and the thighs passage and for confectioning the boxer short, characterized in that we cut, respectively at the front or at the back, two incisions forming, by opening of the incisions, a first globally transverse bottom line composed, on the one hand, of a low transverse edge and, on the other hand, of a top transverse edge of bottom line rising higher than the low transverse edge, in that at least one incision is cut, respectively, at the back or at the front, forming, by opening of the incision, a second bottom line having at least one low transverse edge, in that the crotch bottom is prepared in the shape of at least one crotch piece, and in that said low transverse edge of the first bottom line is sewn to a portion facing the low transverse edge of the second bottom line and in that the at least one crotch piece is sewn between the top edge of the first bottom line and a portion facing the second bottom line.
Preferably, particularly for a male garment, it is at least at the front that the two incisions are cut, the back may have just a single incision. It is indeed at the front that it is mainly appropriate to improve the comfort of the garment. However, it is possible to provide a boxer short where the two incisions are provided at the back and only one at the front. It is also possible, and sometimes even advantageous, to provide a boxer short where the front as well as the back include two incisions.
The incisions may be formed at the front and/or at the back of the knitted tube by simple symmetrical incisions with respect to the median vertical axis of a front or rear face, which are vertical or slightly oblique with respect to the vertical. The incisions are preferably rectilinear, but may also be curved, formed of segments, etc.
The two incisions formed on the front (or rear) side, are in a preferred embodiment, two substantially vertical and symmetrical incisions with respect to the median axis of the boxer short. When the knitted fabric is laterally stretched to open these incisions and form the first globally transverse bottom line, a kind of central tab is formed between the incisions, the edge of which will constitute the low transverse edge of the bottom line, surrounded on either side by two lateral ends of bottom line rising higher than the tab edge. In this case the crotch bottom is prepared in the shape of two separate crotch pieces; the low edge of the front tab is sewn, situated in the middle of the first bottom line, in the middle of the second facing bottom line and the two separate crotch pieces are sewn between the ends of the first bottom line and the ends facing the second bottom line.
If the second bottom line is formed by a single incision, normally on the rear face, this second bottom line after lateral extension of the incision is substantially a rectilinear transverse or slightly arched line. Advantageously, the length of the cuts at the front and at the back is not the same: the length of the cut at the back is normally superior to that of the cuts at the front so as to form two transverse bottom lines which have a substantially equivalent transverse extension.
Thus, according to this embodiment, there is a method for manufacturing a boxer short comprising the circular knitting of a main tube, the preparation of a crotch bottom, the cutting in the low portion at the front and at the back of the incisions tube, the opening of the incisions for forming first and second bottom lines and the sewing of the crotch bottom to the bottom lines to form the crotch and the thighs passage and for confectioning the boxer short, characterized in that we cut at the front two incisions forming, by opening of the incisions, a first bottom line composed, on the one hand, of a low edge of front tab between the two incisions and, on the other hand, of two lateral ends of bottom line rising higher than the tab edge, in that an incision is cut at the back forming, by opening of the incision, a second bottom line, in that the crotch bottom is prepared in the shape of two separate crotch pieces, and in that said front tab edge is sewn, situated in the middle of the first bottom line, in the middle of the second bottom line and in that the two separate crotch pieces are sewn between the ends of the first bottom line and the ends of the second bottom line.
The second bottom line is situated, after confection, at the rear side of the boxer short, so that the tab portion fastened thereto and which comes from the front portion, seamlessly surrounds, and therefore without discomfort, the genitals of the wearer. The two crotch pieces are rejected on the edges of the tab and participate in the formation of the thigh passages.
In a variant of this same embodiment, it may be provided that the second bottom line is equally formed by two substantially vertical and symmetrical incisions, in which case there is formed by extension of the incisions, a central tab provided with a low edge: the low edge of the first tab is sewn on the low edge of the second tab and the separate crotch pieces are sewn between the ends facing the first and the second bottom line. In this variant, the length of the two cuts at the front and at the back is advantageously the same, so as to form two transverse bottom lines which have a substantially equivalent transverse extension.
According to a second embodiment, the two incisions formed at the front and/or at the back of the knitted tube are in the shape of a double T incision, that is to say an incision including the T base starting from the edge of the knitted fabric and the T-bar transversely disposed at the base. When the knitted fabric is laterally stretched to open this double T incision and form the first globally transverse bottom line, a low edge is laterally formed on either side of a central portion of the bottom line which rises higher than the edge situated at the two ends of the bottom line. In this case a crotch bottom in the shape of only one separate central piece is prepared; the low double lateral edge situated at the ends of the first bottom line is sewn to the portions facing the ends of the second bottom line and the central piece is sewn separate from crotch between the central portion rising higher than the first bottom line and the central portion facing the second bottom line.
The shape of the two incisions forming a T may admit variations: for example the branches of the T bar may be curves and/or may not be completely at right angle with respect to the T base.
If the second bottom line is formed by a single incision, normally on the rear face, this second bottom line after lateral extension of the incision is substantially a rectilinear transverse or slightly arched line. Advantageously, the length of the cut at the back is superior to that of the T at the front so as to form, at the back and at the front, two transverse bottom lines which have a substantially equivalent transverse extension.
In a variant of this same second embodiment, it can be provided that the second bottom line is also formed by two incisions forming a T, in which case a bottom line substantially resembling the first bottom line is formed by extension, with a low edge on either side of a higher central portion. The low edges facing the two bottom lines are sewn to one other, and the central piece separate from the crotch is sewn between the less low central portions of the facing bottom lines. In this variant as in the others, the length of the two cuts at the front and at the back is provided so as to form two transverse bottom lines which have a substantially equivalent transverse extension.
Thus according to the invention, it is understood that the at least one of the two bottom lines obtained by incisions and lateral stretching is not exclusively rectilinear transverse but on the contrary, though always globally transverse, it comprises, on the one hand, a low transverse edge (in one portion, for example central portion, or in many portions, for example lateral portions) and, on the other hand, a top edge of bottom line rising higher than the low transverse edge (this top edge being possibly in two portions, for example lateral portions, or in one portion, for example central portion), whereby, when this non rectilinear bottom line is placed facing the other bottom line, the low edge can be directly sewn to the other line and the crotch piece(s) can be placed between the top edge and the other line.
We used here the verb “sew”, but it is clear that this term does not only cover the seam with a thread, but any method allowing to assemble edge to edge two textile pieces.
As said above, the second bottom line is advantageously substantially rectilinear or arched in shape. It is understood that in this case, said low edge of the second bottom line extends over the entire length of the bottom line.
The first bottom line is advantageously in the shape of broken line.
The low edge of first bottom line (for example that of the tab in the first embodiment) may be formed by the low border of the circular knitted fabric itself, after possible unrolling of the lapel which was formed during knitting when appropriate, or long after a transverse complementary cut at the front, between the incisions, to remove the lapels.
The crotch portion(s) is/are advantageously obtained also by knitting, the two pieces (when there are two) can be easily formed from a common draft, which may be obtained from a transversely cut strip. The crotch portion(s) can also come from another knitted fabric than the knitted fabric of the boxer short itself, another jersey type material. These two portions may, according to their material, possibly bring an additional benefit to the product: ventilation (“mesh” type material), anti-friction type material, anti-irritation treated material, etc.
The invention also relates to a boxer short obtained by the method above.
It is about a boxer short formed in a knitted main tube, including a front and a back linked in low portion by a crotch bottom separating two thigh passages, the low portions of the front and of the back ending with a first and a second bottom line globally transverse between which the crotch bottom is sewn, characterized by a first globally transverse bottom line composed, on the one hand, of a low transverse edge and, on the other hand, of a top edge of bottom line rising higher than the low transverse edge, a second bottom line having at least one low transverse edge, in that said low transverse edge of the first bottom line is sewn to a portion facing the low transverse edge of the second bottom line, and in that the crotch bottom is in the shape of at least one separate crotch piece sewn between the top edge of the first bottom line and a portion facing the second bottom line.
In a particular case of embodiment, it is about a boxer short formed in a knitted main tube, including a front and a back linked in low portion by a crotch bottom separating two thigh passages, the low portions of the front and the back ending with a first and a second bottom line between which the crotch bottom is sewn, characterized by a first bottom line composed, on the one hand, of an edge of front tab and, on the other hand, of two lateral ends of bottom line rising higher than the edge of tab, in that the crotch bottom is in the shape of two separate crotch pieces, and in that that said edge of front tab, situated in the middle of the first bottom line, is sewn in the middle of the second bottom line and in that the two separate crotch pieces are sewn between the ends of the first bottom line and the ends of the second bottom line.
BRIEF DESCRIPTION OF THE DRAWINGS
Other features and advantages of the invention will appear from the following description. Reference will be made to the accompanying drawings on which:
FIG. 1 schematically represents in a front view a knitted tube at the first step of its confection, according to the prior art.
FIG. 2 schematically represents in a back view a knitted tube at the first step of its confection, according to the prior art.
FIG. 3 schematically represents in a bottom view the knitted tube of FIGS. 1 and 2 , after sewing of the crotch bottom, according to the prior art.
FIG. 4 schematically represents in a front view a knitted tube at the first step of its confection, according to the invention.
FIG. 5 schematically represents in a back view a knitted tube at the first step of its confection, according to the invention.
FIG. 6 is a view of a crotch draft according to the invention.
FIG. 7 is a view of a lateral crotch piece according to the invention.
FIG. 8 schematically represents in a bottom view the knitted tube of FIGS. 4 and 5 , after sewing of the two lateral pieces of the crotch bottom, according to the invention.
FIG. 9 represents in perspective in a low angle view a particular example of embodiment of a boxer short in accordance with the invention.
FIGS. 10A to 13 ′C represent various embodiments of the incisions at the front and at the back of the tubular knitted fabric, and FIGS. 10 ′A and 12 ′A, similar to FIGS. 3 and 8 , illustrate the shape of the crotch obtained according to the method of the invention. More precisely,
FIG. 10A describes the first preferred embodiment of the invention, with two front vertical symmetrical incisions, one back vertical incision, with in FIG. 10 ′A the illustration of the corresponding crotch.
FIGS. 10B and 10C are two variants of this first embodiment, where the frontal symmetrical incisions are oblique.
FIG. 11A describes an alternative variant of the first preferred embodiment of the invention, two front symmetrical vertical incisions, two back vertical symmetrical incisions, with in FIG. 11 ′A, the illustration of the corresponding crotch.
FIGS. 11B and 11C are two variants of this first embodiment, where the frontal symmetrical incisions are oblique.
FIG. 12A describes the second preferred embodiment of the invention, with two front T-shaped incisions, a back vertical incision, with, in FIG. 12 ′A, the illustration of the corresponding crotch.
FIGS. 12B and 12C are two variants of this second embodiment, where the incision forming the T-bar has a curved or oblique shape on the horizontal, with, in FIG. 12 ′C, the illustration of the crotch corresponding to FIG. 12C .
FIG. 13A describes an alternative variant of the second preferred embodiment of the invention, with two front and back T-shaped incisions, with, in FIG. 13 ′A, the illustration of the corresponding crotch.
FIGS. 13B and 13C are two variants of this second embodiment, where the incision forming the front T-bar has a curved or oblique shape on the horizontal, with, in FIG. 13 ′C, the illustration of the crotch corresponding to FIG. 13C .
DETAILED DESCRIPTION
The enclosed FIGS. 4 to 8 show in detail the confection operation of a boxer short according to the invention according to a first preferred embodiment. As according to the prior art, the boxer short 1 is made in the shape of a knitted tube, with an upper belt 2 and a lower border 3 corresponding to future leg cuffs. The knitted tube comprises a front face 5 and a rear face 6 . It is further represented in hatching on the front face 5 of the portion 4 intended to form the front pocket of the boxer short intended to maintain the genitals. There is defined on the knitted tube a vertical direction going from the belt 2 at the top to the lower border 3 and a transverse direction, orthogonal to the vertical direction, and going from one side of a front or rear face to the other.
According to the invention, we proceed ( FIGS. 4 and 5 ) to a cut operation creating two parallel vertical incisions 7 and 7 ′ at the front 5 of the boxer short 1 : these incisions have edges 10 , 11 and 10 ′, 11 ′ and form a tab 14 having a lower edge or low edge 16 . The lower edge 16 may be directly the edge of the knitted tube if the lapel is not formed yet, or be the edge of the tab 14 after dismantling the lapel, or even—and preferably—be obtained by the shortening of the tab 14 through an additional transverse cut (not represented) between the two incisions 7 , 7 ′. In practice, the contour portion 4 may advantageously go lower than it has been represented on FIGS. 4 and 8 (to avoid confusing the reading) and come in the tab 14 between the two edges 11 , 11 ′ and almost until to its low edge to ensure more comfort to the genitals.
We proceed at the back part 6 of the knitted tube to a central vertical incision 8 , creating two edges 12 , 13 .
We also prepared, preferably in a knitted fabric, two lateral crotch pieces 15 , 15 ′ in one piece 17 represented in FIG. 6 , which can itself be obtained by cutting a long knitted strip. The piece 17 includes, on its two edges, borders 23 , 23 ′ with lapels corresponding to portions 3 of the tubular knitted fabric 1 intended to form the thigh passage. An oblique cut 18 allows to form, from the piece 17 , two pieces 15 and 15 ′ symmetrical in rectangular trapezia. The piece 15 , represented on FIG. 7 , includes, in addition to its reinforced edge 23 , parallel edges 1510 and 1513 and an oblique edge 1511 .
We then go to the sewing of the crotch pieces 15 , 15 ′ on the knitted tube. For that, each incision 7 , 7 ′ is laterally spaced apart, in the transverse direction, so as to put the edges 10 , 11 and 10 ′, 11 ′ substantially in the shape represented in FIG. 8 , where they are at an obtuse angle together, always with the tab 14 therebetween and the edge 16 thereof at low portion. These elements form a broken front bottom line 10 , 11 , 16 , 11 ′, 10 ′, in which the edge 16 is a low edge and the portions 10 , 11 , 11 ′, 10 ′ a top edge (with respect to the low edge). In the same time, the incision 8 is spaced apart so as to put the edges 12 , 13 substantially in the extension of one another, as represented, so as to form a practically rectilinear rear bottom line 12 , 13 .
the low edge 16 is then sewn in the middle of the rear bottom line 12 , 13 , in the portion facing the low edge 16 , and the lateral crotch trapezia 15 , 15 ′ are attached and sewn between the lateral portions of front bottom line 10 , 11 and 10 ′, 11 ′ constituting the top edge and the ends of the rear bottom line 12 , 13 . The lateral crotch trapezia 15 , 15 ′ therefore participate in the constitution of each thigh girth 19 by the reinforced edge 23 , 23 ′.
The shape of the lateral crotch pieces 15 , 15 ′ is not limited to the trapezium. These pieces can also be triangular, or of other shape, and their edges are not necessarily rectilinear, but may be curves. Likewise, the rear bottom line 12 , 13 represented rectilinear on FIG. 8 can be arched, curvilinear or broken.
An example of a boxer short obtained in accordance with the invention is represented on FIG. 9 . It shows the lateral crotch pieces 15 , 15 ′, placed inwardly and forwardly of each thigh. The front edge 16 forms with the rear bottom line 12 , 13 a seam 20 which extends more or less in an arc between the thighs; two sewing branches go from this seam 20 , sewing the lateral pieces 15 , 15 ′ at the edges 10 , 11 , 10 ′, 11 ′. The fact that the front edge 16 joins the rear bottom line 12 , 13 situated at the back allows to carry to the back the seam and the resulting discomfort in a less sensitive zone, which significantly contributes to the improved comfort of the boxer short of the invention.
The invention is particularly well combined with an embodiment of the front contoured portion in the more or less oval zone 4 shape surrounded by a peripheral marginal zone 21 made within a mesh different from that of the zone 4 , advantageously a more elastic mesh (higher elasticity module).
On FIGS. 4 to 8 the preferred embodiment of the invention was described in detail, but it will be seen on FIGS. 10 to 13 that we can, without departing from the spirit of the invention, bring several modifications to what has been described, according to the exact way with which the two incisions are made on the face that receives them, and on the number of incisions on the other face. Figures are too schematic to allow to easily understand the principle of the modifications. The tube 1 is represented with its front face 5 and rear face 6 , either in perspective, or in a bottom view after assembling the crotch.
On FIGS. 10A and 10 ′A is resumed the basic construction of FIGS. 4-5 and 8 , with two symmetrical vertical incisions 7 , 7 ′ at the front and one 8 in the middle at the back, which allow to obtain a globally transverse bottom line at the front formed of a low central edge 16 and of a top double lateral edge 10 , 10 ′ (the vertical portion, which passes from one to the other, is neglected). This front bottom line cooperates with a substantially rectilinear rear bottom line to which it is directly sewn at the low edge 16 , and linked by means of the crotch pieces 15 , 15 ′ on the ends.
The variations of FIGS. 10B and 10C are distinguished by the symmetrical slightly oblique position of the front incisions 7 , 7 ′.
According to FIGS. 11A and 11 ′A, we provided two vertical symmetrical incisions 7 , 7 ′ at the front and 8 , 8 ′ at the back, thus this results in two quite similar front and rear bottom lines which are directly sewn to one another by their low edge 16 and on the sides by means of the separate crotch pieces 15 , 15 ′.
The variations of FIGS. 11B and 11C are distinguished by the slightly oblique symmetrical position of the front incisions 7 , 7 ′.
According to FIGS. 12A and 12 ′A, a vertical central incision 8 was provided at the back, and two central T-shaped incisions, 7 , 7 ′ were provided at the front, thus this results in that the rear bottom line is still rectilinear and that the front bottom line is characterized by a low edge 16 rejected on the sides while its top edge 10 directly formed by the incision 7 ′ is central. The low edge 10 at the ends is directly sewn to the portion facing the rear bottom line, while the top central edge 10 is sewn to the portion facing the rear bottom line by means of the separate central crotch piece 15 .
The variations of FIGS. 12B and 12C are distinguished by the curved or oblique shape of the T branches, that is to say, of the second incision 7 ′, which leads as it is seen on FIG. 12 ′C to a slightly modified shape of the top edge 10 and therefore of the separate crotch piece 15 .
According to FIGS. 13A and 13 ′A, a double incision in T 7 , 7 ′ and 8 , 8 ′ is provided at the front and at the back, which leads to two bottom lines of identical shape which will be sewn edge to edge at their end portions end forming the low edge 16 and by means of a central crotch piece 15 at their top edge 10 .
The variations of FIGS. 13B and 13C are again distinguished by the curved or oblique shape of the T branches, that is to say, of the second incision 7 ′, 8 ′ of the incisions of the front face and rear face, which leads as it is seen on FIG. 13 ′C to a slightly modified shape of the top edge 10 and therefore of the separate crotch piece 15 .
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These comfortable boxer shorts are formed from a knitted main tube ( 1 ) comprising a front part ( 5 ) and a back part, the lower portions of which end in a first and second bottom line ( 10, 11, 16, 11′, 10; 13, 12 ) consisting of two front incisions and one rear incision. The first bottom line ( 10 ) ( 10, 11, 16, 11′, 10′ ) is composed of an edge ( 16 ) of a front flap ( 14 ) and of two bottom line side ends ( 10, 11; 11′, 10′ ) that rise higher than the edge ( 16 ) of the flap ( 14 ). Said edge ( 16 ) of the front flap ( 14 ) is sown to the middle of the second bottom line ( 13, 12 ), at the rear of the boxer shorts, and two separate crotch parts ( 15, 15 ′) ( 15 ) are sown between the ends ( 10, 11; 11′, 10′ ) of the first bottom line and the ends of the second bottom line ( 13, 12 ).
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This application claims benefit of USC Provisional Appl. 60/052,137, filed Jul. 10, 1997.
BACKGROUND OF THE INVENTION
This invention relates generally to the comminution, separation, recovery and recycling of fractional components of carpet by a process utilizing a cyclonic comminuter.
Carpet recycling has presented a major challenge to the carpet industry that has not been adequately satisfied. The lack of effective recycling processes has resulted in a large volume of carpet material being sent to the landfill. Carpet material is largely non-biodegradable, which is an undesirable situation for the landfills. Furthermore, it is difficult to separate the fractional components of carpet without resulting in the destruction of the components, which limits re-cycling opportunities. A process that would permit the effective recycling of carpet components would require that the fractional components not be destroyed so that the recovered components can be re-manufactured into quality carpet.
Carpet is manufactured in two general configurations, defined by the backing material, although each of the backing materials is formulated in various forms. These two general classifications of carpet backing are jute and vinyl (which is also referred to as rubber-backed carpet). Jute-backed carpet is manufactured with a top layer of nylon 6 or nylon 6-6, or a mixture of these two nylon fibers. These nylon fibers are woven into strings that are affixed to the backing to present the layer on which the carpet is walked upon. The backing includes polypropylene fibers which are substantially coarser in shape and larger in size than the nylon fibers.
The polypropylene fibers are used to hold the woven nylon strings in place and to fasten the entire matrix of fibers to the backing. Jute, being the primary fiber in burlap, is a glossy plant fiber grown primarily in India. A bonding agent, such as latex, is used to stabilize the jute backing to the polypropylene and, therefore, to the nylon fibers. A weaving process hold the respective fractional components of the carpet together, but the latex bonding agent is the stabilizer. Generally, the latex bonding agent/stabilizer is water soluble.
Vinyl backed carpet, also referred to as rubber-backed carpet, is manufactured similarly to the jute-backed carpet, except for the backing thereof. The vinyl may or may not have a stabilizing agent associated therewith, but generally, fiberglass fibers are utilized as a stabilizer. The bonding of the vinyl backing to the other fractional components of the carpet is typically accomplished through a heat process or through the use of a bonding agent, or both.
Accordingly, a process, method and apparatus for separating, recovering and recycling the fractional components of carpet would provide a substantial improvement over the known prior art processes for disposing of used carpet. Not only would landfill charges be saved, but the recovered fractional components of the carpet have substantial value for the re-manufacture of quality carpet.
SUMMARY OF THE INVENTION
It is an object of this invention to provide a process to reduce used carpet into component fractions to facilitate the recycling of used carpet.
It is a feature of this invention that used carpet can be recycled in an economical manner.
It is an advantage of this invention that the recycling of used carpet will reduce the amount of used carpet being disposed in landfills.
It is another object of this invention to utilize a cyclonic comminuter to reduce used carpet pieces into component fractions.
It is still another object of this invention to provide a process for recycling used carpet.
It is another feature of this invention that the used carpet is first pre-cut into appropriately sized pieces before being fed into a cyclonic comminuter.
It is another advantage of this invention that pre-soaking the used carpet pieces will enhance the reduction of the carpet into fractional components within the cyclonic comminuter.
It is still another feature of this invention that the process will be operable for both jute-backed and vinyl-backed carpets.
It is yet another feature of this invention that the final separation of the fractional components of the used carpet pieces can be accomplished by proven operations, such as carding, static charges or pressure gradients.
It is yet another object of this invention to provide a process for recycling used vinyl-backed carpets that utilizes sequential comminuting operations to remove only the vinyl backing from the carpet pieces without any significant disruption of the remaining fractional components of the carpet pieces.
It is a further feature of this invention that the first comminuting operation for recycling vinyl-backed carpet is set at a relatively low level so that the extent of comminution removes only the vinyl backing.
It is a further advantage of this invention that the incomplete comminution of the first comminuting operation of the used carpet pieces leaves most of the fiberglass stabilizer intact with the vinyl material to facilitate the removal of the fiberglass stabilizer as a fractional component.
It is a further object of this invention to provide a process for recycling used carpet for separating and recovering fractional components of the used carpet, including the steps of:
(a) conditioning the used carpet by reducing the carpet to pieces of a pre-determined range of sizes;
(b) feeding the reduced carpet pieces into an air flow of a cyclonic dehumidifying comminuter to separate the fractional components of the carpet pieces to create a mass of separated, entwined fractional component fibers discharged from a discharge opening of said comminuter;
(c) filtering the air flow after being exhausted from the comminuter through a filtering mechanism to recover fractional component fibers carried out of the comminuter with the air flow;
(d) passing the mass of entwined fractional component fibers through a separating mechanism to separate the entwined fractional component fibers from the mass discharged from the comminuter; and
(e) collecting the fractional component fibers from the filtering mechanism and the separating mechanism.
It is a further object of this invention to provide a process for the separating and recovery of fractional components of used carpet to facilitate the recycling thereof which is inexpensive in operation, and simple and effective in use.
These and other objects, features, and advantages are accomplished according to the instant invention by providing a process for the separation and recovery of fractional components of used carpet. Although the disclosed process is operable with either jute-backed or vinyl-backed carpet, an alternative process is preferred for vinyl-backed carpet to permit the sequential removal of the vinyl backing with most of the fiberglass stabilizer intact. The process includes the pre-cutting and preferable pre-soaking of the used carpet into appropriate sized pieces, followed by the introduction of the pre-conditioned used carpet pieces into a cyclonic comminuter which reduces the carpet pieces into fractional components. Processes for the recovery of the separated fractional components include collecting the components from the respective discharges from the cyclonic comminuter, washing, and separating by carding, static charges, pressure gradients and the like. This effective process will allow for greater utilization of carpet recycling operations to prevent used carpet from being disposed in land fills.
BRIEF DESCRIPTION OF THE DRAWINGS
The advantages of this invention will be apparent upon consideration of the following detailed disclosure of the invention, especially when taken in conjunction with the accompanying drawings wherein:
FIG. 1 is a schematic view of apparatus for accomplishing the comminution, separation and recovery of carpet utilizing only a single pass through a comminuting/dehydrating machine, particularly for the recycling of jute-backed carpet;
FIG. 2A is a schematic view of apparatus corresponding to the first comminuter/dehydrator for accomplishing the comminution, separation and recovery of carpet utilizing sequential comminuting/dehydrating steps, particularly for the recycling of vinyl-backed carpet;
FIG. 2B is a schematic view of apparatus corresponding to the second comminuter/dehydrator for accomplishing the comminution, separation and recovery of carpet utilizing sequential comminuting/dehydrating steps, particularly for the recycling of vinyl-backed carpet;
FIG. 3 is a process flow chart for the method of comminuting, separating and recovering fractional components of carpet for recycling thereof utilizing a single comminuting/dehydrating machine, as schematically depicted in FIG. 1; and
FIG. 4 is a process flow chart for the method of comminuting, separating and recovering fractional components of carpet for recycling thereof utilizing sequential comminuting/dehydrating machines, as schematically depicted in FIGS. 2A and 2B.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
Comminuting dense material through a cyclonic comminuting/dehydrating machine, such as shown in U.S. Pat. No. 3,794,251, issued on Feb. 26, 1974, for a "Material Reducing System and Apparatus", is well known in the art. A cyclonic comminuting/dehydrating machine similar to that disclosed in U.S. Pat. No. 5,236,132, is schematically depicted in FIGS. 1-3. The descriptive portions of the aforementioned U.S. Pat. No. 3,794,251 and U.S. Pat. No. 5,236,132 are incorporated herein by reference, particularly with respect to the manner and mechanism through which a cyclonic comminuting/dehydrating machine operates.
Such a cyclonic comminuting/dehydrating machine 10 operates to create a high velocity stream of air from a blower 11 that is directed through a conduit 12 into an inverted conical housing 15. The stream of air is directed into a tornado-like swirling motion within the housing 15 before being discharged out the exit opening 16 at the top center portion of the housing 15. A damper 19 controls the flow of air through the air exit opening 16 and the depth of the swirling motion of the air within the housing 15.
A cylindrical sleeve 18, co-operable with the damper 19, is axially movable within the housing 15 to also control the depth of cyclonic comminution of material within the housing 15. The positioning of the sleeve 18 deep into the housing 15 provides for greater comminution of the material fed through the conduit 12, while a shallow penetration of the sleeve 18 into the housing allows for a more rapid exit of the swirling air from the housing 15 through the air exit opening 16 and, therefore, provides only minimal comminution of the material.
A discharged air recovery mechanism 20 captures the discharged stream of air from the air exit opening 16 to prevent the discharge of any fractional components within the discharged air into the atmosphere to control pollution and allow the recovery of any fractional component therein, as will be discussed in greater detail below. A material infeed hopper 13 meters the flow of material into the air stream in the conduit 12 so that the material to be comminuted enters the housing 15 with the stream of air from the conduit 12. Preferably, the infeed hopper 13 includes an air lock 13a having a rotational member that limits the escape of air from the conduit 12 while feeding material into the conduit 12 for flow into the housing 15.
The housing 15 includes a cylindrical portion 17 that receives the air stream, and material flowing therein, from the conduit 12 and directs the air stream into a swirling motion within the housing 15. Depending immediately below the cylindrical portion 17 is a conical portion 17a that directs the swirling air flow into decreasing-radius turns until the air can escape up through the sleeve 18, past the damper 19 and into the discharged air recovery mechanism 20. The conical portion 17a terminates in a material discharge opening 14 at its lowermost extremity for the discharge of comminuted material from the housing 15.
The cylindrical portion 17 is lined with hardened steel rasp bars (not shown) that, coupled with the differential forces associated with the tornado-like swirling motion of the air stream within the housing 15, serve to comminute material fed therein through implosion, impaction and centrifugal force, on the basis of quantity and density of the material fed therein. At least the upper areas of the conical portion 17a preferably also have spirally arranged members (not shown) that assist in the comminution of material within the housing 15 and deflect material upwardly toward the cylindrical portion 17 to further the comminuting process.
For example, if a bucket of limestone rocks were fed into the housing 15 through the infeed hopper 13, the rocks would be pulverized into small pieces that would drop by gravity through the material discharge opening 14 formed by truncating the end of the inverted conical housing 15. Similarly, a bucketful of steel bolts fed into the housing 15 would also be pulverized into small pieces. If, however, a handful of steel bolts were fed into the air stream with a bucket of limestone rocks, the rocks would still be pulverized, but the steel bolts would be discharged through the material discharge opening 14 substantially unharmed.
The operation of the rasp bars lining the cylindrical portion 17 of the housing 15 serve both to shred and to ricochet solid material particles within the housing 15, which impacts other solid material particles and, coupled with differential velocities of the swirling air within the housing 15, serves to comminute the lesser dense material within the housing 15. Accordingly, with respect to the examples of the limestone rocks and steel bolts given above, the less dense and higher quantity limestone rocks become comminuted into small pieces, while the steel bolts become discharged relatively unharmed.
In Applicants' U.S. Pat. No. 5,727,740, granted on Mar. 17, 1998, the descriptive portions thereof being incorporated herein by reference, method and apparatus for recovering precious stones from soil is disclosed, along with processes for reclaiming precious metals from low grade ore and waste material, recovering lead and lead shot from contaminated soils, and for removing free sulphur from coal. All of these processes involve dense materials or pellets of material having greater density within a lower density medium that needs to be disintegrated and recovered.
Surprisingly, a cyclonic, dehumidifying comminuting machine 10 similar to that described and shown in the aforementioned U.S. Pat. No. 5,236,132, has been found to be operable to disintegrate pieces of considerably less dense material such as carpet. By controlling the level of comminution within the housing 15 through manipulating the depth of the sleeve 18 into the housing 15 and the operation of the damper 19, the amount of comminution of the carpet pieces can be selectively controlled. This control permits the development of processes that can recover the fractional components of both jute-backed and vinyl-backed carpets.
Referring first to FIG. 1, the apparatus for recovering fractional components of carpet, particularly jute-backed carpet can best be seen. The process flow chart is depicted in FIG. 4. While this disclosed process is considered to be particularly applicable to jute-backed carpet, the separation and recovery of vinyl-backed carpet can also be accomplished with this process. Utilizing the cyclonic, dehumidifying comminuter 10 as the central machine in the process, both pre-comminuting and post comminuting devices are necessary for the efficient separation and recovery of the fractional components of carpet.
Used carpet must be pre-cut into pieces having a size and shape suitable for the feeding of the carpet pieces through the material infeed hopper 13. While the size of the comminuter 10 and the size of the air lock 13a will dictate the size and shape of the carpet pieces to be pre-cut, it has been found that pre-cutting the used carpet into squares having sides measuring between one and four inches will provide satisfactory results. It will be understood by one skilled in the art that this process is not confined to the use of carpet pieces in either this size or particular shape. Pre-cutting machinery 25 can include a conventional hammer mill 26 that can break up or chop the used carpet into pieces having the size and shape needed to permit feeding through the air lock 13a. Alternatively, a shredding and cutting apparatus 27 can be used to first cut the used carpet into strips and then into squares of an appropriate size.
After pre-cutting the used carpet into appropriately sized pieces, it is advantageous to pre-soak the pieces in water, preferably with agitation. Pre-soaking enhances the separation of the component fibers of the carpet in the comminuter, particularly with jute-backed carpets. The pre-soaking of the carpet pieces starts to break down the latex backing of the carpet before being introduced into the comminuter 10. Agitation helps to reduce the soak time needed for the carpet pieces and, therefore, the incorporation of an agitator 29 may reduce the size of the pre-soak tanks 28.
It will be recognized by one skilled in the art that not all of these pre-comminution steps, and the machinery associated therewith will be necessary for each of types of carpet to be processed. For example, both a hammer mill 26 and a shredding/cutting machine 27 are not typically necessary; however, a hammer mill 26 and a simple cutting machine might provide the best results, depending on the settings of the hammer mill 26. Furthermore, pre-soaking is not mandatory to the process, but does enhance the operation. With the use of a cyclonic, dehumidifying comminuter 10, the water is removed during the comminution step anyway.
Following the pre-cutting and pre-soaking of the carpet pieces, the carpet pieces are loaded into the material infeed hopper 13 through the air lock 13a to be fed into the air stream forced through the conduit 12. In FIG. 1, an auger conveyor 22 schematically represents a mechanism for transporting the pre-cut and pre-soaked carpet pieces to the infeed hopper 13. The carpet pieces then flow into the cylindrical portion 17 of the housing 15 to start the comminuting and dehydrating step in the process during which the fractional components of the carpet is separated. The carpet pieces are converted into a mass of fibers and powder. The nylon fibers are detached from the polypropylene fibers, etc., but are entwined together in the discharge of materials through the discharge opening 14.
In the case of jute-backed carpet, the latex will fall out the discharge opening 14 as dry powder, while the jute will typically be discharged as both a dry powder and in a fibrous form. Because the cyclonic dehumidifying comminuter 10 both comminutes and dehydrates, the water absorbed by the carpet pieces during the pre-soak stage of the process is completely removed and is discharged with the air flow through the sleeve 18 into the discharged air recovery mechanism 20. Some of the lighter nylon fibers may also be trapped in the air flow and exit the comminuter 10. Accordingly, the discharged air recovery mechanism 20 will direct the flow of discharged air into a filtering mechanism 30 where the nylon fibers can be extracted from the air stream and recovered.
Final separation of the entwined fractional carpet components occurs after being discharged from the conical portion 17a of the housing 15 through the discharge opening 14. The entwined materials are conveyed to a wash bath 32 to remove the powdery latex, which is water-soluble. Some of the nylon fibers will float to the top of the wash bath 32 and will be removed by a recovery device 33, such as a static precipitator or screening mechanism, with the bath water to be recovered. The latex can be precipitated from the bath water either chemically or by filtering through a precipitator 34 and also recovered before the water is discharged or recirculated back through the wash bath. Materials exiting the wash bath 32 can receive a final rinse before being conveyed to a carding apparatus 35. This water can be recirculated back into the wash bath tank 32.
The nylon and polypropylene fibers that are still entwined after being discharged from the wash bath tank 32 are conveyed to a carding apparatus 35 to effect separation of the component materials. The entwined nylon and polypropylene fibers can be separated in the carding apparatus 35 by a combing process, commonly referred to as "carding", or by the use of static charges, or by a combination of both. Separation of these fibers can also be accomplished by using air or a washing process either alone or in combination with carding or static charges. Carding also aligns all the fibers so that they are oriented in the same direction, thus allowing the heavier materials, such as the polypropylene fibers, to drop out of the mass or to be removed by static charges or pressure gradients or both. The separated materials can then be recovered and re-utilized in the manufacturing of new carpet.
Vinyl-backed carpet can also be separated into its fractional components and the components recovered for recycling by the above-described process. The problem encountered by using this process to recover vinyl-backed carpet components is that the full comminution of the carpet pieces also comminutes and separates the vinyl backing and the fiberglass fibers that are used as a stabilizer. Freeing fiberglass fibers, whether carried up through the sleeve 18 to be recovered in the filtering mechanism 30 or allowed to fall through the discharge opening 14 at the bottom of the comminuter 10, is not desirable. The preferred process for recycling vinyl-backed carpet is described below with respect to FIGS. 2, 3 and 5.
Referring now to FIG. 2A, the first phase of the process is substantially the same as described above with respect to FIG. 1. The used carpet is selectively pre-conditioned before being fed into the first comminuter 10, such as by shredding or cutting the carpet into appropriate sized pieces and by pre-soaking. Even though vinyl-backed carpet does not use latex as a stabilizer, the absorption of water into the carpet pieces is still believed to enhance the subsequent comminution process; however, pre-soaking of vinyl-backed carpet is not a necessary step in the process.
The carpet pieces are then fed into the first cyclonic dehumidifying comminuter through the air lock 13a and into the air stream flowing through the conduit 12. The primary difference between this first phase of separating vinyl-backed carpet and the process above for recycling primarily jute-backed carpet is the comminution setting on the first comminuter 10. Preferably, the sleeve 18 is withdraw to a shallow setting within the housing 15 and the damper 19 is set so that the extent of comminution is set at a relatively low level so that only the vinyl backing is removed from the carpet pieces without any significant disruption of the remaining fractional components of the carpet pieces.
Because the vinyl material is substantially heavier than the other carpet materials, the vinyl will settle out by gravity through the discharge opening 14 at the bottom of the conical portion 17a of the first comminuter. Generally, the vinyl material will come out of the first comminuter 10 in comparatively large pellets, which permit relatively easy separation of the vinyl materials from the remaining carpet. A separating device 39, such as a sieve, screening apparatus, air stream or other appropriate devices, can be utilized to separate the vinyl from the remaining carpet materials. Because of the incomplete comminution of the carpet pieces, most of the fiberglass stabilizer remains intact with the vinyl.
Referring now to FIG. 2B, the remaining carpet material is then preferably washed in a secondary wash tank 32 to remove any powdery residue and to add additional moisture to the materials to enhance the further comminution thereof in the second cyclonic dehumidifying comminuter 40. Again a auger conveyor 22 symbolically depicts the conveyance of the remaining carpet materials from the wash tank 32 to the material infeed hopper and air lock 43 of the second comminuter 40 which is set for full comminution by lowering the sleeve 48 well into the housing 45.
The comminuting effect of the second cyclonic dehumidifying comminuter 40 is similar to the operation defined above with respect to FIG. 1. The nylon fibers are disengaged from the polypropylene fibers and are generally recovered in the filtering mechanism 30, which can be a shared filter with the first comminuter 10 or a separate device. The polypropylene fibers, along with some entwined nylon fibers, are discharged through the discharge opening 44 of the second comminuter 40 into a collection device 49, where the fibers are transported to a separating mechanism 50, which may including a carding apparatus or static or pressure gradient devices, as described above, to recover the polypropylene and nylon fibers.
Any remaining backing materials are reduced to powder and generally exit the discharge opening 44, but may be entrapped in the air flow for removal by the filtering mechanism 30. Accordingly, the separating mechanism 50 may require a tertiary bath to cleanse the polypropylene and nylon fibers. One skilled in the art will realize that the above described process utilizing first and second cyclonic dehumidifying comminuters 10, 40, can also be used for the recycling of jute-backed carpet pieces with most of the jute backing and latex stabilizer being removed in the first comminuter 10 and the remaining fibers recovered from the second comminuter 40.
In the alternative, it is believed that the fractional carpet components may be recovered in the comminuter before being discharged through the discharge opening. Because density of materials effects the path of each individual fractional component material inside of the comminuter 10, 40, such as the nylon 6-6 or nylon 6 or polypropylene fibers, separation of these materials can be accomplished inside of the comminuter by utilizing the density differences and centrifugal forces, or by the use of static electricity in the form of an electrostatic precipitator.
The lighter materials, such as the nylon fibers, can be brought out the top of the comminuter with the air flow and collected by the filtering mechanism 30. The heavier and larger materials, such as the polypropylene fibers will gravitate toward the discharge opening and can be collected before being discharged. The other heavier materials, such as the latex and vinyl components will be pulverized into a powder and allowed to exit the discharge opening.
Because of the potential volume of used carpet to be processed and the fractional components thereof to be recovered and recycled, it is expected that a typical processing plant will require several units, or multiples of units as described above, in order to process a substantial amount of carpet efficiently. In such an operation, many of the machinery components described above can be combined and constructed in a larger magnitude. For example, the filtering mechanism 30 can be constructed to process the air flow from several comminuters 10. Similarly, the pre-soak tanks 28 and the pre-cutting machinery 25 can be sized to accommodate the volume of carpet pieces that will satisfy the capability of multiple comminuters. The same order of magnitude would also apply to the post-comminuting machinery, such as the carding apparatus 35 and the wash bath tank 32.
It will be understood that changes in the details, materials, steps and arrangements of parts which have been described and illustrated to explain the nature of the invention will occur to and may be made by those skilled in the art upon a reading of this disclosure within the principles and scope of the invention. The foregoing description illustrates the preferred embodiment of the invention; however, concepts, as based upon the description, may be employed in other embodiments without departing from the scope of the invention.
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A process is disclosed for the separation and recovery of fractional components of used carpet. Although the disclosed process is operable with either jute-backed or vinyl-backed carpet, an alternative process is preferred for vinyl-backed carpet to permit the sequential removal of the vinyl backing with most of the fiberglass stabilizer intact. The process includes the pre-cutting and preferable pre-soaking of the used carpet into appropriate sized pieces, followed by the introduction of the pre-conditioned used carpet pieces into a cyclonic comminuter which reduces the carpet pieces into fractional components. Processes for the recovery of the separated fractional components include collecting the components from the respective discharges from the cyclonic comminuter, washing, and separating by carding, static charges, pressure gradients and the like. This effective process will allow for greater utilization of carpet recycling operations to prevent used carpet from being disposed in land fills.
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FIELD OF THE INVENTION
The present invention relates to PDP (plasma display panels) and more particularly to a method for implementing error diffusion on PDP so as to solve low level contouring occurred thereon.
BACKGROUND OF THE INVENTION
The brightness of a typical color television (TV) may be expressed in following equation (1) in terms of input voltage by utilizing the physical characteristic of cathode ray tube (CRT) of color TV:
brightness= k ×( V INPUT /V MAX ) γ (1)
where γ=2.2, k is a variable representing gray scale of color TV (e.g., k=256 if gray scale of color TV is 256), V INPUT is input voltage varied as gray scale of color TV, and V MAX is a maximum voltage required for showing a maximum gray scale of color TV. Hence, the relationship of input gray scale versus output brightness of color TV may be plotted as a curve (FIG. 1 a ). Conventionally, prior to sending a video signal (e.g., NTSC or HDTV), a Gamma (γ) compensation process (called compensation process hereinafter) is performed on the original video signal by utilizing above physical characteristic thereof. That is, a compensation process is performed with respect to γ in equation (1). As such, the relationship of input brightness versus output gray scale of color TV may be plotted as a curve (FIG. 1 b ). In one example of γ=0.45 (i.e., obtained from 1/2.2), the video signal received by color TV is converted into image for showing on screen of CRT of color TV. Hence, the relationship of input brightness versus output brightness of color TV may be plotted as a straight line (FIG. 1 c ). As a result, a high quality image is shown on the typical color TV without distortion.
As to recently available PDP (plasma display panels) brightness of respective discharge unit on panel thereof is controlled by discharge number. Hence, brightness may be expressed in following equation (2) in terms of discharge number as below (i.e., a straight line):
brightness= k 2 ×discharge number (2)
where k 2 is a variable representing gray scale of PDP (e.g., k 2 =256 if gray scale of PDP is equal to 256). In view of this, the higher discharge number the brighter of PDP. This is similar to the effect that the larger input voltage the brighter of a typical color TV.
Referring to FIGS. 2 a , 2 b and 2 c , a compensation process is performed on received video signal by PDP by substituting γ=0.45 into equation (1) by similarly utilizing the physical characteristic of typical color TV. As such, the relationship of input brightness versus output gray scale of PDP may be plotted as a curve (FIG. 2 a ). Further, the relationship of input gray scale versus output brightness of PDP may be plotted as a straight line (FIG. 2 b ). Furthermore, video signal received by PDP is converted into image for showing on screen of PDP. Hence, the relationship of input brightness versus output brightness of PDP may be plotted as a curve (FIG. 2 c ) by similarly substituting γ=0.45 into equation (1). As a result, a distorted image with poor contrast is shown on PDP.
Typically, an anti compensation process is performed for solving above drawbacks. In detail, in one example, an anti compensation process is performed on received video signal by PDP by substituting γ=2.2 into equation (1). As such, in PDP the relationship of input gray scale versus output gray scale may be plotted as a curve (FIG. 3 b ). In another example, an anti compensation process is performed on received video signal by PDP by substituting y=0.45 into equation (1). Hence, in PDP the relationship of input brightness versus output gray scale may be plotted as a curve (FIG. 3 a ). As to image shown on PDP, the relationship of input gray scale versus output brightness of PDP may be plotted as a straight line (FIG. 3 c ). By combining FIGS. 3 a , 3 b and 3 c , in PDP the relationship of input brightness versus output brightness may be plotted as a straight line (FIG. 3 d ). In other words, a linear relationship exists between image shown on PDP and received video signal. As a result, a high quality image is shown on PDP without distortion.
As to current PDP, signal input/output and processing are done by a digital technique. Moreover, in most cases gray scale of PDP is expressed as a power of 2. For example, in PDP eight bits are needed for representing 256 gray scales. Typically, in performing a compensation process an analog-to-digital conversion is performed on video signal prior to substituting γ=0.45 into equation (1). Then an anti compensation process is performed by substituting γ=2.2 into equation (1) for effecting an inverse transform on video signal. Finally, an image is shown on PDP. As brightness of PDP is proportional to discharge number thereof. If brightness of one discharge of PDP is equal to N cd/m 2 (N is an integer) N is a minimum brightness of PDP. As such, brightness of PDP may be expressed as a multiple of one discharge of PDP. That is, brightness of PDP is a multiple of N. Hence, brightness of a plurality of k discharges is k 3 ×N (where k 3 is a positive integer). In other words, a brightness of f×N is not obtainable if f is not an integer (e.g., a brightness of 0.5×N).
In view of above, it is known that a brightness of PDP can not be expressed by a discharge number having a non-integer value (e.g., decimal). Hence, the decimal has to be converted into an integer. In the case of the original video signal having 256 gray scales, the number of gray scale is reduced to 184 after first being processed in an analog-to-digital conversion and subsequently by substituting γ=2.2 into equation (1) for performing an anti compensation process thereafter. In another case that the original video signal having a gray scale of 22, the number of gray scale is reduced to 1.62738 after an inverse transform is performed by substituting γ=2.2 into equation (1). Since decimal fraction of gray scale can not be shown on PDP only gray scale having value one rather than 1.62738 is shown on PDP (see Table I below.)
TABLE I
gray scale of
gray scale after
gray scale of image
original video signal
γ = 2.2 conversion
shown on PDP
1
0.001295
0
2
0.005949
0
3
0.014515
0
. . .
. . .
. . .
21
1.049625
1
22
1.162738
1
. . .
. . .
. . .
29
2.135145
2
30
2.30048
2
. . .
. . .
. . .
43
5.079049
5
44
5.342539
5
45
5.613314
5
. . .
. . .
. . .
255
255
255
Total gray scale = 256
Total gray scale = 256
Total gray scale = 184
Hence, a problem of insufficient gray scale of video signal is occurred in the range of low gray scale after such anti compensation process. And in turn a low level contouring is occurred in the range of low gray scale. Consequently, a poor contrast of gray scale is occurred in the range of low gray scale. This can degrade the image quality.
SUMMARY OF THE INVENTION
It is thus an object of the present invention to provide a method for implementing error diffusion on a plasma display panel (PDP) comprising the steps of: performing an anti compensation process on a received video signal of the PDP; diffusing an error generated by a first one of a plurality of pixels to a plurality of adjacent pixels; absorbing errors generated by the plurality of adjacent pixels by the first pixel; and multiplying each of a plurality of numeric weightings and the error of each of the adjacent pixels to obtain an error function of the first pixel. This utilizes a cost effective while simple addition circuit in implementing error diffusion for solving the problem of low level contouring in PDP due to insufficient gray scale of video signal in the range of low gray scale.
The above and other objects, features and advantages of the present invention will become apparent from the following detailed description taken with the accompanying drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 a is a graph showing a relationship of input brightness versus output gray scale of a conventional color TV;
FIG. 1 b is a graph showing a relationship of input gray scale versus output brightness of the conventional color TV;
FIG. 1 c is a graph showing a relationship of input brightness versus output brightness of the conventional color TV;
FIG. 2 a is a graph showing a relationship of input brightness versus output gray scale of a conventional plasma display panel (PDP);
FIG. 2 b is a graph showing a relationship of input gray scale versus output brightness of the conventional PDP;
FIG. 2 c is a graph showing a relationship of input brightness versus output brightness of the conventional PDP;
FIG. 3 a is a graph showing a relationship of input brightness versus output gray scale of the conventional PDP after an anti compensation process is performed thereon;
FIG. 3 b is a graph showing a relationship of input gray scale versus output gray scale of the conventional PDP after the anti compensation process is performed thereon;
FIG. 3 c is a graph showing a relationship of input gray scale versus output brightness of the conventional PDP after the anti compensation process is performed thereon;
FIG. 3 d is a graph showing a relationship of input brightness versus output brightness of the conventional PDP after the anti compensation process is performed thereon;
FIG. 4 a is a graph illustrating an error generated by a pixel being diffused to adjacent eight pixels implemented in a conventional technique;
FIG. 4 b is a graph similar to FIG. 4 a where errors generated by adjacent pixels are diffused to (i.e., absorbed by) a central pixel;
FIG. 5 a is a graph illustrating nine adjacent pixels is simplified to five adjacent pixels;
FIG. 5 b is a graph similar to FIG. 5 a where errors generated by four adjacent pixels are diffused to (i.e., absorbed by) a central pixel;
FIG. 6 is a graph similar to FIG. 5 b where errors generated by four adjacent pixels are weighted;
FIG. 7 is a graph showing a relationship of input gray scale versus output gray scale obtained in the conventional technique; and
FIG. 8 is an enlarged graph of a portion of FIG. 7 showing a relationship of input gray scale versus output gray scale where curves before error diffusion implementation (i.e., in prior art) and after error diffusion implementation (i.e., in a method according to the invention) are plotted for comparison.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
Typically, for solving the problem of low level contouring in PDP due to insufficient gray scale of video signal in the range of low gray scale an error diffusion implementation is carried out for compensating the video signal of PDP. It is required to define error (see Table II) prior to carrying out such error diffusion implementation.
TABLE II
gray scale of
gray scale after
original video signal
γ = 2.2 conversion
0-14
0
15-24
1
25-31
2
32-36
3
37-40
4
41-44
5
45-48
6
49-51
7
52-54
8
55-57
9
58-59
10
. . .
. . .
255
255
Total gray scale = 256
Total gray scale = 184
For example, a video signal has a gray scale of I after first being processed in an analog-to-digital conversion. Subsequently γ=2.2 is substituted into equation (1) for performing an anti compensation process. As a result, gray scale of the video signal is reduced to 0.001295. As stated above, since decimal fraction of gray scale can not be shown on PDP only gray scale having value zero rather than 0.001295 is shown on PDP. That is, there is an error of 0.001295 in gray scale. Likewise, in another example a video signal has a gray scale of 30 after first being processed in an analog-to-digital conversion. Subsequently γ=2.2 is substituted into equation (1) for performing an anti compensation process. As a result, gray scale of the video signal is reduced to 2.30048. As stated above, since decimal fraction of gray scale can not be shown on PDP only gray scale having value two rather than 2.30048 is shown on PDP. That is, there is an error of 0.30048 in gray scale. In view of above, the generation of such error is totally caused by decimal fraction of gray scale which can not be shown on PDP (i.e., only integer gray scale is shown).
Referring to FIG. 4 a , an error generated by a central pixel on PDP is diffused to adjacent eight pixels in a conventional technique. Likewise, errors generated by eight adjacent pixels are diffused to (i.e., absorbed by) the central pixel (FIG. 4 b ). Since each pixel can absorb errors generated by eight adjacent pixels the to be rounded decimal fraction of gray scale may carry forward to become an integer due to the addition of errors of eight adjacent pixels in the process of anti compensation. In other words, such decimal fraction of gray scale is not rounded as expected. Hence, the obtained gray scale is not correct. Further, a practical circuit for implementing error diffusion on PDP is also considered. In a typical technique, nine adjacent pixels is simplified to five adjacent pixels (e.g., A, B, C, D, and E in FIGS. 5 a and 5 b ). In addition, errors generated by pixels A, B, C and D are diffused to (i.e., absorbed by) the central pixel E. For obtaining an optimum visual effect by such error diffusion, a suitable numeric weighting is multiplied by each pixel having a different location. For example, {fraction (1/16)}, {fraction (5/16)}, {fraction (3/16)} and {fraction (7/16)} are multiplied by pixels A, B, C and D respectively (FIG. 6 ). Hence, gray scale P′ of pixel E after error diffusion implementation may be expressed as an addition of original gray scale P and error function Err(f) in a following equation 3:
P′=P+Err ( f ) (3)
where error function Err(f) is expressed as an addition of four adjacent pixels each of which is a multiplication of an associated weighting and error function thereof in a following equation 4:
Err ( f )={fraction (1/16)} Err ( A )+{fraction (5/16)} Err ( B )+{fraction (3/16)} Err ( C ){fraction (7/16)} Err ( D )
The variation of gray scale of video signal before and after error diffusion implementation on PDP may be best illustrated by referring to FIG. 7 . In FIG. 7, a graph shows a relationship of input gray scale versus output gray scale after performing a Gamma anti compensation on video signal. Unfortunately, it is not possible to observe a significant variation of gray scale of video signal in the whole range of gray scale before and after error diffusion are implemented. A curve portion in the range of gray scale of 0 to 80 is enlarged in FIG. 8 for further illustrating a relationship of input gray scale versus output gray scale. As shown, a zigzag line is obtained by substituting γ=2.2 into equation (1) for performing an anti compensation process. It is observed that there is a discontinuity in the low gray scale portion which in turn causes a low level contouring of image. In comparison, a bold line is obtained by substituting γ=2.2 into equation (1) for performing an anti compensation process and an error diffusion is further implemented on the line. It is observed that this bold line is substantially continuous and smooth. As a result, the low level contouring of image is much improved.
In a practical technique, an additional multiplication circuit is required to incorporate into a control circuit of PDP for carrying out the error diffusion implementation as expressed in equations 3 and 4. However, it requires a complex multiplication circuit design, resulting in an increase of manufacturing difficulty.
For solving above problem, a method for implementing error diffusion on PDP is carried out wherein weighting as represented conventionally by decimal is converted into one other than above by the invention. This utilizes an addition circuit in a cost effective and simple manner as detailed below.
Referring to FIGS. 5 a and 5 b again, for obtaining an optimum visual effect by error diffusion implementation, pixel E may absorb errors generated by adjacent pixels A, B, C and D. Further, a suitable weighting is multiplied by each of pixels A, B, C and D respectively. Hence, error function Err(f) may be expressed in a following equation 5:
Err ( f )=wl Err ( A )+w2 Err ( B )+w3 Err ( C )+w4 Err ( D ) (5)
where each of w1, w2, w3, and w4 is a weighting of the associated pixel. In a preferred embodiment of the invention, each of w1, w2, w3, and w4 may be represented by a negative power of integer (e.g., 2) or an addition of a plurality of ones each having a negative power of integer (e.g., 2). For example, w1={fraction (1/16)}=2 −4 , w2={fraction (5/16)}={fraction (1/16)}+{fraction (2/16)}+{fraction (2/16)}={fraction (1/16)}+¼=2 −4 +2 −2 , w3={fraction (3/16)}={fraction (1/16)}+{fraction (2/16)}={fraction (1/16)}+⅛=2 −4 +2 −3 , and w4={fraction (7/16)}={fraction (1/16)}+{fraction (2/16)}+{fraction (4/16)}={fraction (1/16)}+⅛+¼=2 −4 +2 −3 +2 −2 . By substituting above w1, w2, w3 and w4 into equation 5, error function Err(f) may be expressed in a following equation 6:
Err ( f )=2 −4 Err ( A )+(2 −4 +2 −2 ) Err ( B )+(2 −4 +2 −3 ) Err ( C )+(2 −4 +2 −3 +2 −2 ) Err ( D ) (6)
By comparing equations 6 and 4, it is found that each of weightings as represented conventionally by decimal is converted into a negative power of integer 2 or an addition of a plurality of ones each having a negative power of integer 2 by the invention. This utilizes a cost effective while simple addition circuit in implementing error diffusion, resulting in an elimination of error caused by decimal of gray scale as experienced in prior art.
Since picture shown at one time is different from that shown at the other time (i.e., dynamic picture), one error generated by a pixel in one picture may be different from that generated by the same pixel in the other picture. Hence, in another preferred embodiment of a method for implementing error diffusion on PDP according to the invention, a time varying weighting function (e.g., d1(t), d2(t), d3(t), or d4(t)) is multiplied by the associated numeric weighting. Hence, error function Err(f) may be expressed in a following equation 7:
Err ( f )=w1 d 1( t ) Err ( A )+w2 d 2( t ) Err ( B )+w3 d 3( t ) Err ( C )+w4d4( t ) Err ( D ) (7)
As a result, an optimum image is shown on PDP.
While the invention has been described by means of specific embodiments, numerous modifications and variations could be made thereto by those skilled in the art without departing from the scope and spirit of the invention set forth in the claims.
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A method for implementing error diffusion on a plasma display panel (PDP) comprises the steps of performing an anti compensation process on a received video signal of the PDP; diffusing an error generated by a first one of a plurality of pixels to a plurality of adjacent pixels; absorbing errors generated by the plurality of adjacent pixels by the first pixel; and multiplying each of a plurality of numeric weightings and the error of each of the adjacent pixels to obtain an error function of the first pixel. This is effected in a cost effective while simple addition circuit for solving the problem of low level contouring in PDP due to insufficient gray scale of video signal in low gray scale.
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1. FIELD OF THE INVENTION
[0001] The present invention relates to a coated board of wood-based material, in particular for producing a floor, ceiling or wall covering as well as a method for coating a board of wood-based material.
2. BACKGROUND
[0002] A plurality of covering boards on wood-based material are known from the prior art. In the simplest case such a board consists of a solid real wood. Such boards of solid wood are however very expensive and as panels it only can be laid by well skilled specialists. However, such so-called real wood planks provide a highly attractive surface. In order to avoid high costs of real wood floorings and to provide the attractive surface of such floorings at the same time, veneer covering boards have been developed. Veneer are thin sheets, as a rule 0.3 to 0.8 mm, from a high quality wood which are applied with glue to a base material. As a rule, the base materials consist of cheaper wood-based materials and are strikingly thicker than the veneer layer. A drawback of such coverings is the relative sensitive surface which, for example, can be easily damaged by means of wetness or by means of mechanical action.
[0003] Furthermore, laminate panels for floor or ceiling coverings are known from the prior art. In comparison with the covering boards mentioned at the beginning, laminate panels are relative inexpensive. As a rule, laminate panel consists of a 4 to 12 mm thick base board of MDF or HDF raw material thus of a relative low priced wood-based material wherein onto its upper side a paper printed with a décor is bonded. As a rule, at the bottom side of the base board there is situated a so-called counteracting paper which is to counteract a distortion of the base board by means of the applied décor layer. In order to improve the durability of the décor layer, a so-called overlay paper is typically applied onto the décor layer wherein the overlay paper is impregnated with a resin, for example an amino resin, and onto the resin are applied very fine abrasion-resistant particles as for example aluminium oxide particles. By pressing under application of heat and pressure the different layers of the laminate panel are joint together and the used resins are cured. Therefore, the result is a durable abrasion-resistant decorative surface.
[0004] In order to improve the durability and thus also the optical properties of the boards of wood-based material, as they are used for example for wall, ceiling or floor panel, there have been recommended several methods for coating and materials the prior art. In principle such coatings can be applied onto any kind of board of wood-based material, including the above mentioned real wood panels and laminate panels, in order to increase the durability of the surfaces.
[0005] For example, a method for coating of a board of wood-based material is known from the WO 2007/042258 A1, wherein in a single coating step a relative thick protective layer of plastic material is applied onto the surface of a board. The used plastic material thereby is a polymerisation able acrylate system which can cure by means of a polymerisation. The polymerisation is started by means of radiation so that a complete conversion occurs through the thickness of the applied layer.
[0006] Based from these prior art there is the object to provide a coated board of wood-based material and also a method for coating aboard comprising specific advantageous mechanical properties.
[0007] These and other objects will be apparent in the following description or will be recognizable from the person skilled in the art and will be solved with a coated board of wood-based material according to claim 1 and with a method for coating according to claim 9 .
[0008] By means of the present invention abrasion values of the highest abrasion grade AC 5 according to prEN 15468 are achieved by optical good transparency of the coating and furthermore by good brilliance of a printed design applied underneath or therein. The surface is characterized by high micro scratch resistant (Mar-Resistance) and impact resistance according to grade 33 (prEN 15468). The characteristic values for chemical resistance and water vapor resistance, castor chair test and case leg test are certain in accordance with the prEN 15468. Furthermore, the method allows a surface in which additionally to the pressure a deep embossed decorative structure for example a brushed wood structure or a stone structure can be brought in. The invention is therefore particularly suitable for providing of floor panels.
3. DETAILED DESCRIPTION OF THE INVENTION
[0009] The coated board of wood-based material is in particular a floor, ceiling or wall panel and respectively a board of wood-based material which is provided for further processing to a floor, ceiling or wall panel, and comprises a front side and a rear side wherein at least the surface of the front side is provided with a polymer coating. The term board of wood-based material is to understand wide and comprises for example both boards made of real wood and boards made MDF, HDF, chip boards, composite boards, OSB boards and the like. The board of wood-based material can further be provided with additional coatings, papers, veneers or the like onto their surfaces of front side and/or rear side. Thus, when a coating of the surface of the board of wood-based material is mentioned, this necessarily means not a direct coating of the board of wood-based material, but the same for example can be provided with a décor paper, wherein the coating is then applied onto the décor paper. According to the invention the polymer coating comprises a hardness gradient after curing so that the hardness of the polymer layer decreases with increasing depth viewed from the surface. That is, the polymer layer has preferably the maximum hardness at its outer surface and has the minimum hardness nearby the boundary surface between coating and surface of the board of wood-based material, with a decreasing course between the both extremes.
[0010] Up to now it has always been desired to achieve preferably a maximum hardness over the over-all layer thickness. The coating according to the invention deviates from this teaching and however surprisingly results in excellent mechanical durability values. An explanation therefore could be that by means of a preferably steady decrease of hardness there not occur high peaks in the properties of the coating and therefore the coating is particularly durable.
[0011] The present invention also relates to a method for coating a board of wood-based material, in particular a floor, ceiling or wall panel, and respectively to a board of wood-based material which is processed to a floor panel, wherein in a first step a first liquid coating means is applied onto a board of wood-based material and onto the still wet first coating means a second liquid coating means is applied, wherein the liquid layers penetrate each other according to the physics of liquids. The outcome of this is a gradient of the concentration of both liquids. While in the outer areas of the total layer (upper side respectively lower side of the over-all layer) the respective liquid of the original single layers is pre-dominant, there exists a concentration gradient of the first liquid and respectively of the second liquid to the center and along to the respective other side of the layer. In the ideal case the respective gradient course corresponds to a straight line. Since in case of higher viscous liquids at short mixing times interruptions may occur to the ideal case, one has to assume that the effective concentration curves only approximately correspond to straight lines and deviations are possible. When the liquids for example are polymerisation able acrylate systems, which are different in the double pond rate, so it follows from the above mentioned that analog to the concentration gradient of the both liquids together, a gradient arises in the number of the double bonds from one side to the other side of the layer. When now a polymerisation is actuated in such a layer, for example by means of UV radiation, and one assume that under inert conditions an almost complete conversion of the double bonds occurs so there arise a polymer layer with a gradient of the cross-linking points. While the side with high double bond concentration is accordingly strong cross-linked, the other side with the low double bond rate has accordingly a lower cross-linking. According to the polymer physics the hardness of such a system gives an information of the cross-linking density. When, for example, the micro hardness (Martens hardness DIN EN ISO 14577) is measured within a layer which is accordingly produced from two polymerisation able liquids, there occurs a hardness gradient analog to the cross-linking density. The layer can be removed in stages for example with a Taber-Abrasion-Test (Taber-Abraser-Test) according to EN 13329. The curve progression of the hardness gradient similarly corresponds to the above described concentration gradient of both liquids. In the ideal case of the mixing of the liquids straight lines occur. In practice, however, there will occur deviations to the straight lines. Mathematical it may therefore be expected that the function y=f(x) has a progression deviating from a straight line (wherein y is the Martens hardness and x is the abrasion depth in the layer).
[0012] The described context shall be illustrated to the person skilled in the art with the following example:
[0013] Onto a HDF base board a first layer of 45 g/m 2 is rolled on via a roll applicator wherein the coating means of the first layer for example consists of 35% from a 1,6 hexanediol diacrylate and of 65% from a polyester acrylate. A second layer with a mass of 40 g/m 2 is immediately applied thereafter onto this layer wherein the coating means of the second layer for example consists of a mixture of 70% polyurethane acrylic ester and of 30% dipropylene diacrylate. Both layers presently include a photoinitiater. The so produced liquid over-all layer is subjected to a UV radiation under nitrogen atmosphere and the over-all layer is polymerized. The double bond conversion thereby is approximately 98%.
[0014] In order to analyze the resultant coating, the coating has subsequently gradually been removed with the Taber-Abraser-Test by means of respectively 200 rotations (described in the EN 13329). The Martens hardness was respectively measured of each an abrasion step. When one chart in a coordinate system the Martens hardness in N/mm 2 to the y-axis and the corresponding abrasion depth in μm to the x-axis, the outcome of this is approximately a straight line with the y=134.8−1.03 x. The coefficient of determination has been determined with 87.8% which shows a very high accuracy of this mathematical correlation for wood-based materials.
[0015] When coatings according to the invention for example are used for a hard-wearing floor covering the layers may additionally be provided with abrasion-resistant particles, such as fine corundum particles. These particles may for example be present in one or both coating means in a dispersion before the coating process or the particles can be spread onto the still wet bat already applied coating means in a separate process step.
[0016] The person skilled in the art recognizes on the basis of the present description of the invention that according to the application coating means can be used with other concentrations as preferably denoted in the example. Preferably the concentration of 1,6 hexanediol diacrylate can be between 10 and 60%, more preferably between 20 and 40%; the concentration of polyester acrylate can be between 40 and 90%, more preferably between 50 and 80%; the concentration of polyurethane acrylic ester can be between 45 and 95 more preferably between 55 and 75% and the concentration of dipropylen glycol diacrylate can be between 5 and 55%, more preferably between 15 and 35%. The mentioned substances shall clarify the principle of a layer with hardness gradients according to a preferred embodiment. It is self-evident that a plurality of further or other polymerisation able substances can be used instead of the above mentioned. Polymerisation able acrylates are particularly preferred substances for the herein described coatings.
[0017] The coating means of the first layer as well as of the second layer and maybe of farther layers can consist of a single polymerise able substance or of mixtures of substances. Particularly preferred suitable substances are polymerising able acrylates as in general and here in particular the substances: 1,6 hexanediol diacrylate, polyester acrylate, polyurethane acrylic ester and dipropylen glycol diacrylate. Particularly suitable for the first layer is a mixture of 1,6 hexanediol diacrylate and polyester acrylate. For the second layer is a mixture of polyurethane acrylic ester and dipropylen glycol diacrylate particularly suitable.
[0018] In the coatings means further additives can be present such as flow additives, wetting additives, dyestuffs, abrasion-resistant particles and so on. Important therefore is that these further components allow the above described cross-linking and penetration, respectively, and that a polymerisation is still possible.
[0019] By selecting of the coating means for the single layer the mentioned substances are preferred, however, the person skilled in the art recognizes that it does not depend on the use of the denoted substances but substantially on the provision of polymerise able coating means.
DETAILED DESCRIPTION OF EXEMPLARY EMBODIMENTS
[0020] To the following, a detailed description of exemplary embodiments will be given by means of the enclosed diagrams and figures.
[0021] FIG. 1 is a schematic illustration of a coating process;
[0022] FIG. 2A to 2C are schematic illustrations in which the procedure of mixing of two liquid layers is shown;
[0023] FIG. 3 is a diagram, which shows the course of the hardness against the depth of the coating;
[0024] FIG. 4 is a diagram, which illustrates the upper and lower boundaries of the hardness gradient according to a preferred embodiment of the invention;
[0025] FIG. 5 is a diagram, which illustrates the upper and lower boundaries of a more preferred embodiment of the invention; and
[0026] FIG. 6 is a diagram, which illustrates the upper and lower boundaries of the hardness gradient of a further preferred embodiment.
[0027] In FIG. 1 a coating plant for coating of boards of wood-based material 10 is schematically shown. The boards of wood-based material 10 , such as boards of solid wood, HDF, MDF or chip boards, are guided by means of a roller conveyer plant 12 through the different stations of the coating plant. In a first coating station 14 a first liquid coating means 20 is applied in a passage coating onto the boards of wood-based material 10 by means of a rotating applicator roller 15 .
[0028] The applicator roller 15 is provided with coating means by means of a supply device 16 . In the second coating station 17 a second liquid coating means 21 is applied onto the still wet first coating means 20 by means of a further rotating applicator roller 18 . The applicator roller 18 is provided with the second liquid coating means by means of a supply device 19 . It is self-evident that the applying can also be done with any other suitable applying process, such as by means of a spraying device or a coating blade or the like. Therefore, it is only important that the applying of the second layer takes place as long as the first layer is still wet enough, so that a partial mixing of the two layers can take place. Furthermore, it is self-evident that further coating stations can be provided after the second coating station 17 in order to apply for example a third liquid coating means onto the still wet second coating means 21 or also additional stations in order to apply abrasion-resistant particles onto and respectively into the wet layers.
[0029] After leaving of the coating station 17 the coated boards 10 are conveyed to a hardening station 30 , where the layers are hardened by means of UV radiators 31 . On their way from the coating station 17 to the hardening station 30 a partial mixing of the liquid coating means 20 and 21 occurs, which particularly takes place at the boundary surfaces of the two coating means. Thereby, naturally the mixing is stronger, the closer one is located at the boundary surface of the two layers. By curing of the layers in the curing station 30 the mixing process is stopped and the once adjusted mixing proportion and therefore the mechanical properties of the produced coating is set. The extent of the mixing at the boundary surfaces which takes place itself and preferably without external mechanical action depends on the time duration which passes between the applying of the second coating means 21 onto the still wet first coating means 20 and the curing in the curing station 30 . Furthermore, the mixing of the two coating means is also influenced by the respective viscosity of the coating means wherein the general rule is that the higher the viscosity, the lower the mixing per time unit.
[0030] The principle of the mixing of the two applied coating means can be seen best from the schematically illustration of FIG. 2A to 2C . Therefore, FIG. 2A shows the condition of the two coating means 20 and 21 applied onto a board of wood-based material 10 immediately after applying of the second coating means 21 . At that time practically no mixing has taken place. In the present case, the coating means 20 and 21 are polymers, which have respectively different numbers of C—C carbon double bonds. Therefore, as schematically depicted in FIG. 2A , the first coating means 20 has a lower number of C—C double bonds than the second coating means 21 . Due to the higher number of C—C double bonds in the coating means 21 , the same will have a higher hardness after the curing than the coating means 20 which is provided with lower amount of C—C double bonds.
[0031] As the two coating means 20 and 21 are applied wet on wet, a mixing of the two layers occurs starting from the boundary surface 22 of the two layers, as it is indicated in FIG. 2B . This means that due to the mixing process in the area close to the boundary surface 22 there are more double bonds in the underlying layer and accordingly in the area close to the boundary surface 22 of the overlying layer there are fewer double bonds, as before the mixing. FIG. 2C shows the two layers after the mixing has advanced some more and has reached a suitable mixing grade. If at this point of time the curing of the coating means occurs, for example by means of UV radiation, this mixing rate is set, since in the hardened layers naturally no mixing can occur any more.
[0032] In the diagram of FIG. 3 the hardness course of a coating according to the invention (example with hardness gradient) and a coating according to the prior art are plotted. The example according to the invention consisted of an abraded board of wood-based material provided with a primer on which the two different coating means were applied wet on wet. The first applied coating means consisted of approximately 35% 1,6 hexanediol diacrylate and approximately 65% polyester acrylate and was applied with 45 g/m 2 . The second coating means which was applied onto the still wet first layer consisted of approximately 70% polyurethane acrylic ester and approximately 30% dipropylene glycol diacrylate and was applied with 40 g/m 2 . After applying of the second layer there was a waiting time of 10 seconds in order to make it possible for the viscous liquid materials to mix. Afterwards, the two layers were completely hardened together.
[0033] The example according to the state of the prior art consisted of a conventional coating, wherein multiple thin layers of materials were applied separately and wherein between the respective applying procedures the pre-applied layer was hardened. The lower three layers consisted of a mixture of 70% polyester acrylate and 30% 1,6 hexanediol diaerylate with an applying intensity of 12 g/m 2 . The two upper layers consisted of 70% polyurethane glycol diacrylate and 30% dipropylene acrylic ester and the two upper layers contained 15% corundum with an average particle size of D 50 of 25 μm.
[0034] The test was carried out according to the European standard for laminate panels DIN EN 13329 with a Taber-Abraser-Tester 5151 of Taber Industries. After 200 rotations respectively with S-41 abrasive paper the hardness and the trace depth of the samples were determined. The determination of the Martens hardness (registering hardness test under test application of a force) was carried out according to DIN EN ISO 14577. A “Fischerscope H100” of Helmut Fischer GmbH was used as a test apparatus. The following test parameters were used: maximal strength: 50/30 mN as well as measuring period: 20 seconds. The determination of the trace depth was carried out with a mechanic brush analyzer. A Perthometer S3P of Perthen was used as a test apparatus.
[0035] During the measurement of the samples it became apparent that probably due to the used relative soft materials more or less deviations occur in the hardness of a given layer depth. Therefore, it is necessary to measure at several points in order to get representative data by means of an average determination. During the carried out measurements the hardness as well as the trace depth was respectively measured after 200 rotations of the abrasive paper at four points. It became apparent that in most of the majority of cases four measurement points provide a sufficient accuracy. It is self-evident that one can get more accurate measurement results by using more than four measuring points, like eight for example.
[0036] In the below depicted table the individual measured data for the sample of the example according to the invention are depicted. The measurement was carried out on the completely cured coating that means the condition in which respective products would be really used as floor panel.
[0000]
TABLE 1
Example with hardness gradient
depth measurement
depth trace
of hardness
Martens hardness
[μm]
[μm]
[N/mm 2 ]
rotation
1
2
3
4
1
2
3
4
1
2
3
4
3.6
3.8
3.3
3.4
134.8
118.7
159.0
150.6
AV
3.5
140.8
200
20.0
20.0
20.0
20.0
3.5
3.7
4.3
3.9
139.7
125.2
93.5
112.2
AV
20.0
3.9
117.7
400
20.0
20.0
20.0
25.0
4.5
5.0
4.0
3.9
65.9
69.9
106.9
113.2
AV
21.3
4.4
84.5
600
25.0
25.0
25.0
30.0
4.7
4.7
4.3
4.0
60.5
79.6
95.0
106.1
AV
26.3
4.4
90.3
800
30.0
30.0
30.0
35.0
4.1
4.1
4.0
4.2
103.8
103.1
109.7
100.3
AV
31.3
4.1
104.2
1000
40.0
40.0
40.0
45.0
4.7
4.2
3.9
4.5
78.5
99.3
112.0
87.5
AV
41.3
4.3
94.3
1200
50.0
50.0
50.0
50.0
4.3
5.4
4.2
4.8
93.7
59.8
98.6
82.6
AV
50.0
4.6
83.7
1400
55.0
55.0
60.0
60.0
5.4
4.5
4.0
5.0
60.1
85.0
106.7
70.6
AV
57.5
4.7
80.7
1600
60.0
65.0
70.0
70.0
4.7
4.4
4.3
4.6
47.8
53.6
55.5
48.9
AV
66.3
4.5
51.5
1800
65.0
70.0
75.0
75.0
4.0
4.6
4.9
5.3
64.5
50.1
43.7
37.1
AV
71.3
4.7
48.9
2000
75.0
80.0
80.0
75.0
5.8
4.9
6.2
6.0
31.3
43.6
27.3
41.6
AV
77.5
5.5
38.0
2200
95.0
105.0
105.0
100.0
4.5
5.1
6.1
4.9
51.4
40.8
28.1
43.7
AV
101.3
5.2
41.0
[0037] In the above depicted table the column “rotation” indicates the number of rotations which were carried out with the Taber-Abraser-Tester. The column “depth trace” indicates how many micrometer material of the coating starting from the original surface was removed at the four measuring points 1-4. The column “depth measurement of hardness” indicates how many micrometers the test pin entered into the coating at the four measuring points 1-4 respectively, in the column “Martens hardness” the hardness is indicated in Newton per mm 2 for the four measuring points 1-4 respectively. Below the individual values the respective average value for the four measuring points is indicated. From the above depicted table it is easy to recognize that the Martens hardness decreases the deeper one penetrate into the completely cured layer. It is also apparent that at 800 and 1000 (over-all) rotations a moderate rise of the Martens hardness can be noted. This is due to the irregular mixing of the two used coating means which in the praxis can only fully be avoided.
[0038] Nevertheless it is apparent in the diagram of FIG. 3 that in the example with hardness gradient there is a nearly continuous decrease of hardness without great peaks. However, the comparison example according to the state of the prior art does not show such a continuous progress of the hardness, but moreover at a depth of 60 to 80 μm it has a pronounced point of discontinuity up to the original initial hardness.
[0039] The average values of the test sample are depicted in the below-mentioned table 2.
[0000]
TABLE 2
Average values of the example with hardness gradient
depth
Martens hardness
Standard deviation of the
rotation
[μm]
[N/mm 2 ]
Martens hardness [N/mm 2 ]
3.5
140.8
15.4
200
23.9
117.7
17.0
400
25.6
94.5
17.6
600
30.7
90.3
11.0
800
42.1
104.2
3.4
1000
45.8
87.5
12.6
1200
54.8
82.8
14.9
1400
62.2
80.7
17.4
1600
70.8
51.4
3.2
1800
76.0
48.9
10.1
2000
83.0
36.9
6.8
2200
106.4
41.0
8.4
[0040] The values of the comparison test sample according to the prior art are shown in the below-mentioned tables 3 and 4.
[0000]
TABLE 3
Sample according to prior art
depth measurement
depth trace
of hardness
Martens hardness
[μm]
[μm]
[N/mm 2 ]
rotation
1
2
3
4
1
2
3
4
1
2
3
4
3.1
3.5
3.1
3.0
180.6
141.8
173.1
192.4
AV
3.2
172.0
200
30.0
25.0
25.0
25.0
4.2
4.2
3.7
4.7
99.9
99.6
124.5
79.3
AV
26.3
4.2
100.8
400
35.0
35.0
35.0
35.0
3.7
3.8
4.0
4.1
126.9
117.2
110.1
105.3
AV
35.0
3.9
114.9
600
45.0
45.0
45.0
45.0
3.7
3.8
4.6
4.8
128.4
122.2
83.2
74.7
AV
45.0
4.2
102.1
800
50.0
50.0
50.0
50.0
4.0
4.7
4.8
4.0
108.2
80.9
75.4
110.9
AV
50.0
4.4
93.8
1000
60.0
60.0
60.0
60.0
3.5
3.1
4.0
3.6
143.7
177.4
108.0
129.9
AV
60.0
3.6
139.8
1200
66.0
70.0
70.0
70.0
3.3
3.4
3.6
3.0
160.7
145.1
135.0
186.1
AV
68.8
3.3
156.5
1400
70.0
75.0
75.0
75.0
3.3
3.0
3.1
3.8
157.7
191.6
178.0
119.3
AV
73.8
3.3
161.7
1600
76.0
80.0
80.0
80.0
2.3
2.9
2.6
2.4
183.6
124.8
147.9
174.4
AV
78.8
2.6
157.7
1800
80.0
85.0
85.0
85.0
3.8
3.0
3.4
3.1
71.4
112.3
88.6
107.0
AV
83.8
3.3
94.5
2000
85.0
90.0
85.0
85.0
5.1
3.5
2.6
3.0
40.9
82.3
146.4
112.6
AV
86.3
3.6
95.6
2200
85.0
95.0
90.0
90.0
3.6
3.0
3.0
2.7
81.2
116.0
114.5
137.5
AV
90.0
3.1
112.3
2400
90.0
100.0
100.0
95.0
3.7
5.2
3.1
3.0
77.6
39.7
108.2
111.8
AV
96.3
3.8
84.3
2600
100.0
100.0
105.0
100.0
5.3
3.3
5.0
3.9
37.8
92.6
42.4
67.7
AV
101.3
4.4
60.1
[0000]
TABLE 4
Average values of the sample according to the prior art
depth
Martens hardness
Standard deviation of the Martens
rotation
[μm]
[N/mm 2 ]
hardness [N/mm 2 ]
3.2
172.0
18.7
200
30.4
100.8
16.0
400
38.9
114.9
8.1
600
49.2
102.1
23.5
800
54.4
93.8
15.9
1000
63.6
139.8
25.2
1200
72.1
156.5
18.9
1400
77.1
169.7
27.3
1600
81.3
167.7
23.1
1800
87.1
94.8
16.1
2000
89.8
95.6
38.9
2200
93.1
112.3
20.1
2400
100.0
84.3
29.0
2600
105.7
60.1
21.9
[0041] It has turned out experimentally that especially good mechanical properties of the complete over-all layer can be achieved, if the hardness gradient of the finished over-all layer—like it is shown in an exemplary manner in FIG. 3 —essentially corresponds to the following formula:
[0000] (−3.0* x ) +C≦Y ( x )≦(−0.2* x )+ C
wherein: x is the absolute value of the depth in μm of the coating viewed from the surface of the coating; Y(x) is the absolute value of the hardness in N/mm 2 at a certain depth x; and C is the absolute value of the initial hardness in N/mm 2 of the coating at a depth of approximately x≈0-5 μm.
[0046] Under the “absolute” values it is to be understood that in the above formula only the plain numerical value is entered that means without the associated measuring unit “μm” and “N/mm 2 ” respectively. It for example, the initial value of the above example with hardness gradient is 140.8 N/mm 2 (see table 2), in the above table are inserted only the absolute values, that means C=140.8. In the same way for x is inserted only the absolute values, for example x=3.5. The result of this is, for example, upper and lower boundaries for Y(x=3.5) of 140.1 and 130.3 respectively. At a depth of x=40 μm the result is then, for example, 132.8 for the upper boundary and 20.8 for the lower boundary respectively. These upper and lower boundaries for Y(x) have the measurement unit N/mm 2 . Important is that the absolute values, starting from the mentioned measurement units “μm” and “N/mm 2 ”, are used in the formula and not starting, for example, from “mm” or “N/m 2 ”. It should be clear for the person skilled in the art that the above formula is no mathematical formula to the description of the hardness gradient itself, but it rather defines a range, in which it should run.
[0047] The initial value of hardness of the coating is the value in the first few μm of the coating. Due to the typically used measurement method by means of a test pin which penetrates a few μm into the coating, it is difficulty to determine the hardness for the depth of penetration “0 μm”. The formulation “substantially” is therefore elected because it is difficulty to achieve a perfect uniform mixing of the materials so that in reality it can always come to single tiny outliers, such as the hardness value of 104.2 Newton/mm 2 at a depth of 42.1 μm (see table 2) of the above discussed example with hardness gradient. Furthermore, the values very close to the surface of the board of wood-based material are generally inaccurate, since the residual layer thickness to be measured must have a certain minimum thickness in order to allow useful measurements. The residual layer thickness for useful measurements should therefore be at least 5 μm, preferably 10 μm and further preferably at least 20 μm. With other words, the last 20 μm of the layer, close to the board of wood-based material, must not necessarily follow the above mentioned preferred hardness gradient although this is naturally preferred.
[0048] In a further preferred embodiment the hardness gradient substantially follows the following formula:
[0000] (−2.5* x )+ C≦Y ( x )≦(−0.4* x )+ C
[0049] And in another further preferred embodiment it substantially follows:
[0000] (−2.0* x )+ C≦Y ( x )≦(−0.6* x )+ C
[0050] In the FIG. 4 to 6 the meaning of the above mentioned formulas of hardness gradients are illustrated according to examples with hardness gradient. It should be clear that the indicated absolute values for hardness and depth are only exemplary. It is self-evident that it is possible to apply over-all layers with significant larger thicknesses or lower thicknesses. Furthermore, the absolute value of hardness certainly depends on the used materials and can also be larger or lesser than the values of the example with hardness gradient. However, the order of magnitude of the cited values for the example with hardness gradient is most preferred and suitable for the use in a floor panel.
[0051] The person skilled in the art recognizes by means of the detailed description of the method according to the invention how he can achieve a coating of a board of wood-based material according to the invention. This means naturally that all materials mentioned and named in connection with the description of the methods, such as the substances for the coating means, can also be used by the coating of the board of wood-based material according to the invention.
[0052] The presented method is in particular suitable for coating of floor panels, and respectively for coating of boards of wood-based materials which are subsequently further to floor panels processed since the advantageously mechanical properties of the hardness gradient have here a strong effect. In the same way the presented coated board of wood-based material is for the same reason preferably a floor panel and respectively a coated board of wood-based material, which is intended to be further processed to a floor panel.
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A coated board of wood-based material and a method for coating a board of wood-based material, wherein the board of wood-based material is in particular a wall panel or floor panel or is intended for producing such a panel, comprising a front side and a rear side, wherein at least the surface of the front side is provided with a polymer coating and wherein the polymer coating has a hardness gradient, so that the hardness of the polymer layer decreases with increasing depth from the surface.
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CROSS-REFERENCE TO RELATED APPLICATIONS
[0001] Not Applicable.
STATEMENT REGARDING FEDERALLY SPONSORED RESEARCH OR DEVELOPMENT
[0002] Not Applicable.
BACKGROUND OF THE INVENTION
[0003] This invention relates to methods and compositions for containing particulate matter within open top receptacles including but not limited to open top hopper cars, trucks, piles, and similar storage and/or shipping containers. Treating a load of particulate material (and in particular coal) with a binding agent (sometimes referred to as a crusting agent) to encrust a surface and thereby retain valuable material as well as prevent the spreading of dust from the particulate is known. Prior binding agents are described among other places in U.S. Pat. No. 5,441,566. These binding agents include latexes, petroleum products, and pine tar resins. Other binding agents include phenolaldehyde resin mixed with a polyisocyanate in the presence of a catalyst (described in U.S. Pat. No. 5,244,473), alkaline phenolic resin (described in U.S. Pat. No. 5,089,540), and styrene in a hygroscopic solvent (methyl ethyl ketone), polyvinyl acetate and water (described U.S. Pat. No. 5,487,764). Additional dust suppressants are described in U.S. Pat. Nos. 5,181,957 and 5,747,104, 5,648,116, US Published Patent Application 2009/0189113 A1, and Published PCT Applications 02/12574 A1, 2010/110805 A1 and 2009/023652 A1.
[0004] Unfortunately many of these binders cause the particulate material to retain large amounts of water which can lead to diminished value and effectiveness. In the context of coal, increased water content results in decreased. BTU content and increased likelihood of spontaneous combustion from water induced oxidation of the coal. Furthermore the binders tend to form brittle coatings which tend to shatter and dissipate as the particulate material settles and shifts due to the effects of transit and storage. Problems due to the brittleness of the binder coatings become exacerbated when the material is stored in environments where the temperature fluctuates above and below freezing. This is because freezing and melting moisture further shifts the materials further shattering the binder coating.
[0005] Prior art binding materials also have a number of winter handling problems that can render application difficult and potentially ineffective. This is because such products often have a freezing point near that of water and once frozen, they no longer work. Even worse these prior art binder coatings after being frozen are not recoverable even after they have thawed or melted if they have been frozen. This greatly limits the conditions in which they can be used and applied.
[0006] Thus it is clear that there is clear utility in novel methods and compositions for binding the top of particulate materials stored or shipped in open top containers. The art described in this section is not intended to constitute an admission that any patent, publication or other information referred to herein is “Prior Art” with respect to this invention, unless specifically designated as such. In addition, this section should not be construed to mean that a search has been made or that no other pertinent information as defined in 37 CFR §1.56(a) exists.
BRIEF SUMMARY OF THE INVENTION
[0007] At least one embodiment of the invention is directed towards a method of inhibiting the release of dust from a pile of particulate material. The method comprises the step of applying to the exposed surface of the pile a binder composition. The binder composition comprises VAE and crude glycerin in a ratio of between 90:10 and 10:90.
[0008] The composition may further comprise water but the composition does not pass significant amounts of water to the pile. The cure rate of the composition may be slowed to allow settling of the pile. The pile may be within an open topped container. The pile may be within an open topped railroad car which is moving at least a part of the time. The particulate material may be coal.
DETAILED DESCRIPTION OF THE INVENTION
[0009] The following definitions are provided to determine how terms used in this application, and in particular how the claims, are to be construed. The organization of the definitions is for convenience only and is not intended to limit any of the definitions to any particular category.
[0010] “Crude glycerin” means a by-product derivative from a transesterification reaction involving triglycerides including transesterification reactions involving biodiesel manufacturing processes, in which the by-product comprises glycerin and at least one component selected from the list consisting of: fatty acids, esters, salt, methanol, tocopherol, sterol, mono-glycerides, di-glycerides, and tri-glycerides.
[0011] “Particulate material” means” a material that has a tendency to form dust particles when handled, processed, or contacted, which includes but is not limited to coal, dirt, wood chips, agricultural products, fruits, fertilizers, ores, mineral ores, fine materials, sand, gravel, soil, fertilizers, or other dust generating material, and any combination thereof.
[0012] “PVA” means polyvinyl acetate polymer.
[0013] “Mong” means non glycerol organic material and typically consists of soaps, free fatty acids, and other impurities.
[0014] “VAE” means vinyl acetate ethylene co-polymer. In at least one embodiment the repeating units of VAE are selected from one of formula I, II, III, IV, and any combination thereof wherein:
[0000]
[0015] wherein n is the number of cross linking units, m is the number of first chain units, and o is the number of second chain units, either, some, or all of n, m, and o can be 1 or more, although m and o will frequently be 2 or 3 or 4 or more, either or both of the first and second chain units can be left side end (terminal) units of a polymer chain and/or right side end (terminal) units of a polymer chain. VAE can also comprise co-polymers containing additional cross linking units and can comprise additional polymer chains.
[0016] In the event that the above definitions or a description stated elsewhere in this application is inconsistent with a meaning (explicit or implicit) which is commonly used, in a dictionary, or stated in a source incorporated by reference into this application, the application and the claim terms in particular are understood to be construed according to the definition or description in this application, and not according to the common definition, dictionary definition, or the definition that was incorporated by reference. In light of the above, in the event that a term can only be understood if it is construed by a dictionary, if the term is defined by the Kirk - Othmer Encyclopedia of Chemical Technology, 5th Edition, (2005), (Published by Wiley, John & Sons, Inc.) this definition shall control how the term is to be defined in the claims.
[0017] In at least one embodiment the surface of a pile of particulate matter is treated with a binder to prevent the loss of material and the release of dust from the pile. The binder is a composition comprising a VAE copolymer and crude glycerin The crude glycerin is derived from a transesterification reaction involving triglycerides.
[0018] Biodiesel is typically made through a chemical process called transesterification in which vegetable oil or animal fats are converted to fatty acid alkyl esters and crude glycerin by-product. Fatty acids and fatty acid alkyl esters can be produced from oils and fats by base-catalyzed transesterification of the oil, direct acid-catalyzed esterification of the oil and conversion of the oil to fatty acids and subsequent esterification to biodiesel.
[0019] The majority of fatty acid alkyl esters are produced by the base-catalyzed method. In general, any base may be used as the catalyst used for transesterification of the oil to produce biodiesel, however sodium hydroxide or potassium hydroxide are used in most commercial processes.
[0020] Suitable examples of crude glycerin and its manufacture can be found in among other places in U.S. patent application Ser. No. 12/246,975. In the biodiesel manufacturing process, the oils and fats can be filtered and preprocessed to remove water and contaminants. If free fatty acids are present, they can be removed or transformed into biodiesel using special pretreatment technologies, such as acid catalyzed esterification. The pretreated oils and fats can then be mixed with an alcohol and a catalyst (e.g. base). The base used for the reaction is typically sodium hydroxide or potassium hydroxide, being dissolved in the alcohol used (typically ethanol or methanol) to form the corresponding alkoxide, with standard agitation or mixing. It should be appreciated that any suitable base can be used. The alkoxide may then be charged into a closed reaction vessel and the oils and fats are added. The system can then be closed, and held at about 71 degrees C. (160 degrees F.) for a period of about 1 to 8 hours, although some systems recommend that the reactions take place at room temperature.
[0021] Once the reactions are complete the oil molecules (e.g. triglycerides) are hydrolyzed and two major products are produced: 1) a crude fatty acid alkyl esters phase (i.e. biodiesel phase) and 2) a crude glycerin phase. Typically, the crude fatty acid alkyl ester phase forms a layer on top of the denser crude glycerin phase. Because the crude glycerin phase is denser than the biodiesel phase, the two can be gravity separated. For example, the crude glycerin phase can be simply drawn off the bottom of a settling vessel. In some cases, a centrifuge may be employed to speed the separation of the two phases.
[0022] The crude glycerin phase typically consists of a mixture of glycerin, methyl esters, methanol, mong and inorganic salts and water. Methyl esters are typically present in an amount of about 0.01 to about 5 percent by weight.
[0023] In at least one embodiment, methanol can be present in the crude glycerin in an amount greater than about 5 weight percent to about 30 weight percent. In at least one embodiment, the crude glycerin comprises about 30 to about 95 weight percent of glycerin.
[0024] VAE is a copolymer in which multiple vinyl acetate polymers contain ethylene side branches which form cross linkages and connect the polymers to each other forming copolymer networks.
[0025] In at least one embodiment the binder composition comprises between 90:10 and 10:90 of VAE copolymer to crude glycerin by mass. In at least one embodiment the composition further comprises water. In at least one embodiment the composition comprises water and the crude glycerin both prevents the freezing of the water and prevents its evaporation thereby increasing the lifespan and flexibility of the resulting coating. In at least one embodiment the binder coating contains water but does not transfer water to the coal bound by it.
[0026] In at least one embodiment the composition is applied according to any one of the methods or apparatuses of U.S. Pat. No. 5,441,566. In at least one embodiment the binder is applied to a pile within an open top container and forms a binder coating which prevents the substantial release of dust from the pile and the erosion of the pile by the release of such dust. In at least one embodiment the pile is within an open top railroad car and the binder coating prevents dust release and erosion while the car is travelling at railroad shipping speeds (for example >0 mph-250 mph).
[0027] The components of the coating composition may be mixed immediately before addition to the particulate material or may be pre-mixed or some components may be pre-mixed and other components may be mixed immediately before addition to the particulate material. The material may be applied in liquid form by a spray boom having one or more spray heads. In at least one embodiment the binder composition is applied to the material to be coated by at least one of the methods disclosed in U.S. Pat. No. 5,622,561.
[0028] In at least one embodiment the particulate material is drying slurry. Often in industrial applications a particulate material is or becomes heavily intermixed with water or another liquid and forms slurry. This slurry needs to have some or all of the liquid removed before a subsequent process can be performed on the material. While drying (whether by a de-watering technique or if left out to evaporate away the liquid by heat, sunlight, or the like) some or all of the slurry dries out and can generate dust emissions. The composition can be applied to a surface of the slurry to control dust emissions. The composition can be applied to the material when it is slurry, partially dry, completely dry, and any combination thereof. In at least one embodiment the slurry is Red Mud from a Bauxite mining and/or refining operation. In at least one embodiment the dust that is controlled comprises Sodium Carbonate particles. In at least one embodiment the composition is applied to slurry that is left to dry in a retaining pond or other sort of pond, basin, pool, or straining, drying, or filtering receptacle.
[0029] In at least one embodiment the composition is applied as the pile is being formed. When a particulate material is poured or dumped to form a pile, some of the material billows away from the pile in form of airborne dust. This can occur for example when material is loaded into a rail car, dump truck, storage facility, silo, or ship's hold. The composition can be applied to the material before and/or as it is poured or dumped into a pile. In at least one embodiment the material passes along a conveyer belt before it is poured or dumped and the composition is applied to the material as it travels along the belt. In at least one embodiment the composition functions as a tackifier which holds together the material in the form of larger clumps that are less likely to launch as airborne dust.
[0030] The inventive composition is quite effective and displays a number of unexpected and beneficial results. Prior art coating formulations such as PVA form a rigid glue shell or crust. This rigid glue shell contains particulate matter when intact, but suffers from a number of constraints. Prior art shells tend to be brittle and shatter when subjected to significant movement or displacement. With particulate material, particularly coal, and especially coal contained in a rapidly moving, jostling, and bumping railcar, the particulate material shifts as it settles into a more compact arrangement and this movement tends to shatter the brittle prior art shells. Railcars also tend to be impacted rather hard when being shunted in transfer stations which further increases the likelihood of shattering prior art binding coatings.
[0031] The unique chemistry of the composition however allows the binding coating of the invention to avoid shattering during settling and while moving at high speeds in a railroad car or when undergoing bumps or impacts. Without limitation to theory and in particular the scope of the claims, it is believed that the ethylene cross linkages between the polymer strands function as flexible hinges between the polymers. This allows the polymer strands to move, bend, and flex relative to each other more than prior art coatings allow, while at the same time providing an as good or better “glue” effect to the pile. The crude glycerin provides a synergistic effect which enhances the flexibility of the copolymer without impairing its structural strength.
[0032] In at least one embodiment, the cure rate (the amount of time needed before the glue like coating hardens) of the composition is an amount of time greater than it takes for the pile of particulate material to settle into a consistent arrangement. Thus when treated, the pile is always held in place, first by a more flexible coating and later by a harder cured coating. The composition has a longer cure rate than either VAE or other prior art binder coatings have by themselves.
[0033] In at least one embodiment the unique eutectic point of the crude glycerin enhances the performance of the composition. Crude glycerin is known to have a relatively high freezing point (similar to water) when it is nearly pure (more than 90%) or very dilute (less than 10%). However when it is cut with VAE, the freezing point of the blended material is reduced as is the freezing point of any water in solution with the blended material. As a result, when crude glycerin is combined with VAE in the above mentioned ratios (both with and without water), the overall composition is more resistant to freezing and therefore becomes far less brittle (and cures more slowly) than a composition containing a higher or lower ratio of crude glycerin or other prior art binding coatings would otherwise have. Moreover as previously stated, many coating formulations become ruined once they become frozen and will not form adequate coatings even after thawed out again. Because the composition is less prone to freezing, it can be applied under conditions in which prior art coatings would become frozen and are therefore unusable.
EXAMPLES
[0034] The foregoing may be better understood by reference to the following examples, which are presented for purposes of illustration and are not intended to limit the scope of the invention.
[0035] Tailings slurry from a minerals processing operation was used in a study to assess the inhibition of dust generation under various treatment regimes.
[0000] The treatments used included:
Water—as used by many minerals processing operations to control dust formation in holding dams and/or tailings ponds. Comparative example #1: A commercially available dust control product comprised of a styrene-acrylate copolymer. Comparative example #2: A commercially available dust control product comprised of a concentrated glycerin solution in water. Product A—a binder comprising a 50:50 mixture of VAE copolymer and crude glycerin.
[0040] A sample of tailings slurry was collected from a minerals processing facility and sub-samples were placed into plastic tubs (dimensions ˜33×33×28 cm) which were lined with filter cloth and had a series of holes in the base to allow free drainage of any runoff liquid. Samples were stored in a greenhouse and allowed to dry for one week. Treatments as outlined in table 1 were then applied as 1% solutions to the surface of the dried tailings over a 10 week period. Each application used 500 ml of 1% solution applied evenly to the surface of the dried tailings using a pump sprayer. Tests were completed using duplicate samples for each treatment regime.
[0041] After the 10 weeks of drying and treatment the consolidated surface crust of each tailings sample was carefully removed and the underside brushed gently back into the tub to recover any dust present. A vacuum attachment which covered the bulk of the sample area was then gently pressed on the dried surface and the sample was vacuumed for 2 minutes. The collected dust (separate coarse and fine fractions from 2 filtration systems inbuilt in the vacuum cleaner) was weighed.
[0000]
TABLE 1
Total Dust Collected
Application
(kg/m 2 ) (Average of
Product
regime
duplicate samples)
Water
Weekly
1.11
Water
Twice weekly
0.88
Comparative example #1
Weekly
0.19
Comparative example #1
Twice weekly
0.11
Comparative example #2
Weekly
0.92
Comparative example #2
Twice weekly
1.10
Product A
Weekly
0.03
Product A
Twice weekly
0.02
[0042] After the 10 weeks of drying and treatment the consolidated surface crust of each tailings sample was carefully removed and the underside brushed gently back into the tub to recover any dust present. A vacuum attachment which covered the bulk of the sample area was then gently pressed on the dried surface and the sample was vacuumed for 2 minutes. The collected dust (separate coarse and fine fractions from 2 filtration systems inbuilt in the vacuum cleaner) was weighed.
[0043] The vacuum attachment also had 4 side inlets that were closed in the first dust collection. For a second collection air was fed air at 50 psi into the four inlets (generating a ‘mini cyclone’ environment) while the attachment was again pressed on the mud surface and the surfaces re-vacuumed for a further 2 min (Collection 2).
[0044] Total dust collected was recorded in kg/m 2 based on the weight of dust collected and the surface area of the vacuum attachment used to cover the surface where dust was collected.
[0045] The results in table 1 indicate the superior and surprising dust control properties of Product A when compared both to the two separate conventional, commercially available dust control treatments, as well as water as a dust control measure.
[0046] While this invention may be embodied in many different forms, there described in detail herein specific preferred embodiments of the invention. The present disclosure is an exemplification of the principles of the invention and is not intended to limit the invention to the particular embodiments illustrated. All patents, patent applications, scientific papers, and any other referenced materials mentioned herein are incorporated by reference in their entirety. Furthermore, the invention encompasses any possible combination of some or all of the various embodiments described herein and incorporated herein.
[0047] The above disclosure is intended to be illustrative and not exhaustive. This description will suggest many variations and alternatives to one of ordinary skill in this art. All these alternatives and variations are intended to be included within the scope of the claims where the term “comprising” means “including, but not limited to”. Those familiar with the art may recognize other equivalents to the specific embodiments described herein which equivalents are also intended to be encompassed by the claims.
[0048] All ranges and parameters disclosed herein are understood to encompass any and all subranges subsumed therein, and every number between the endpoints. For example, a stated range of “1 to 10” should be considered to include any and all subranges between (and inclusive to of) the minimum value of 1 and the maximum value of 10; that is, all subranges beginning with a minimum value of 1 or more, (e.g. 1 to 6.1), and ending with a maximum value of 10 or less, (e.g. 2.3 to 9.4, 3 to 8, 4 to 7), and finally to each number 1, 2, 3, 4, 5, 6, 7, 8, 9, and 10 contained within the range.
[0049] This completes the description of the preferred and alternate embodiments of the invention. Those skilled in the art may recognize other equivalents to the specific embodiment described herein which equivalents are intended to be encompassed by the claims attached hereto.
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The invention is directed towards methods and compositions for treating piles of particulate materials to inhibit and prevent the loss of valuable fuel or mineral dust from being released from storage piles or open containers. The method involves applying to the pile a binder coating containing VAE and crude glycerin. The binder coating cures and hardens slowly so it is able to remain flexible while the pile or payload is still settling, jostling, being bumped, and otherwise moving around. This coating is especially effective for coal piles and also for piles within and for being moved by open topped railroad cars. The coating's flexibility prevents the coating from becoming brittle and shattering. The coating has better performance than its ingredients do alone. The coating is effective both when it is flexible and after it cures. As a result the invention can both prevent unwanted dust pollution as well as save its users money by avoiding loss of blown away material.
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FIELD OF THE INVENTION
This disclosure relates to hydraulic unloading valves and, more particularly, to hydraulic unloading valves suitable for relieving the load form a hydraulic pump, and, thereby, an engine under certain conditions such as, for example, cold starts.
BACKGROUND OF THE INVENTION
Off road equipment such as diesel powered work vehicles can from time to time experience difficulties making cold starts at cold temperatures such as, for example, temperatures less than 0° C. This can, inter alia, result from a combination of: (1) greater difficulties starting an unloaded engine at cold temperatures; and (2) the contiguous application of parasitic loading (e.g., hydraulic loading) on the engine at startup. As engines become more and more fine tuned to the work requirements of the vehicle, i.e., built and tuned to maximize work efficiency as well as energy efficiency, demanding starting conditions may become a more critical challenge for all.
SUMMARY OF THE INVENTION
Described herein is an invention that improves the conditions under which cold starts are made by significantly lowering the parasitic loading on the engine. The parasitic loading is lowered by reducing hydraulic loads on the engine via unloading valves.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is an illustrative example of a work vehicle on which the invention may be used for cold starts;
FIG. 2 is a perspective view of an exemplary hydraulic pump and integrated unloader valve;
FIG. 3 is an exemplary view of a hydraulic circuit utilizing the invention; and
FIG. 4 illustrates an exemplary flow chart for the invention.
DESCRIPTION OF THE PREFERRED EMBODIMENT
FIG. 1 illustrates a work vehicle 10 , having a cab 18 and ground engaging means 20 , that may incorporate the invention for the purpose of improving cold starts. In such vehicles there may be many parasitic hydraulic loads, e.g., pumps for hydraulic fans, hydrostatic charge pumps, etc. Parasitic hydraulic loads may be significantly reduced via the use of unloader valves to relieve hydraulic loads in areas where functionality requiring such hydraulic loads may be, at the time, non-essential. FIG. 2 illustrates an exemplary integrated hydraulic fan pump 100 having a pump portion 110 and an unloader valve portion 120 . While unloading may be accomplished in a non-integrated fashion, such integration may save valuable space via its compactness, increase reliability via reducing the number of exposed and connected parts, and increase efficiency via a reduction in the travel distance of hydraulic oil.
FIG. 3 , is an illustration of a system showing an exemplary embodiment of the integrated hydraulic pump 100 operably connected to an engine 160 , which may be, in this embodiment, via a conventional mechanical connection to a transmission 125 ; and a vehicle controller unit (VCU) 140 which may be in electrical communication with a temperature sensor 140 a located in hydraulic fluid reservoir 150 for detecting the temperature of hydraulic fluid 151 and an engine speed sensor 140 b which, in this embodiment, may be located within the engine 160 . As illustrated, the integrated hydraulic fan pump 100 may include a pump portion 110 having an inlet 110 a and an outlet 110 b and an unloader valve portion 120 . The unloader valve portion 120 may have a closed position 120 a , an open position 120 b , an actuator which is, in this case, a solenoid 120 c , and a biasing device which is, in this embodiment, a spring 120 d . As illustrated, the unloader valve portion 120 may be biased to the closed position 120 a via the spring 120 d or other device; it may move to the open position 120 b upon being energized by an electrical signal from the VCU 140 to its solenoid 120 c or via some other method. As illustrated, a hydraulic fan 130 having a hydraulic fan motor 131 and fan blades 132 may be powered by pressurized hydraulic fluid 151 from the outlet 110 b . The VCU 140 may continually monitor input from the temperature sensor 140 a and the engine speed sensor 140 b . Also included in this embodiment is a conventional ignition (not shown) having on and off positions and a conventional starter for the engine. In this embodiment, the engine 160 is started via conventional means.
As illustrated, when the unloader valve portion 120 is, by default, in the closed position 120 a , the hydraulic fluid 151 pressurized by the pump portion 110 may flow directly to the hydraulic fan motor 131 , thereby biasing the system, i.e., the integrated hydraulic pump 100 toward conventional vehicle operating conditions, i.e., greater hydraulic loads when the unloader valve portion 120 is not energized.
When the ignition is on, the engine 160 is off, i.e., when the engine speed detected by the speed sensor 140 b is less than a predetermined speed value (300 rpm in this embodiment), and the temperature of the hydraulic fluid, as detected by the temperature sensor 140 a , is less than a predetermined temperature value of, for example, 0° C. as in this embodiment, the VCU 140 signals the unloader valve portion 120 to move to the open position 120 b , thereby allowing hydraulic fluid 151 to flow through the unloader valve portion 120 . This arrangement may keep the inlet 110 a and outlet 110 b to the pump portion open but allow a significant amount of hydraulic oil moved by the pump portion 110 to recirculate between the pump portion 110 and the unloader valve portion 120 and, thereby, significantly reduce hydraulic loading from the fan motor 131 as fluids tend to take the path of least resistance which may be, in this case, the path between the pump portion 110 and the unloader valve portion 120 .
When the engine 160 has achieved a speed greater than 850 rpm as detected by the engine speed sensor 140 b , or the hydraulic fluid 151 has a temperature greater than or equal to 0° C. as detected by the temperature sensor 140 a , the VCU 140 stops the energizing signal to the unloader valve portion 120 allowing the unloader valve portion 120 to move to the closed position 120 . Once the unloader valve portion 120 is in the closed position 120 b , the hydraulic fluid may cease to recirculate between the pump portion 110 and the unloader valve portion 120 and follow the new path of least resistance, i.e., moving from the pump portion 110 to the hydraulic fan motor 131 . The unloader valve portion 120 may remain in the closed position until the following three conditions are met: (1) the ignition is on; (2) the engine speed is less than 300 rpm; and (3) the detected temperature of the hydraulic fluid 151 is less than 0° C.
The actions above are captured in the logic of the program/routine 200 followed by the VCU 140 as illustrated in the flow chart of FIG. 4 . As illustrated in FIG. 4 , if the ignition is on at 210 and the engine is off, i.e., the engine speed is less than 300 rpm, at 220 , and the temperature of the hydraulic fluid 151 is less than 0° C. at 230 , unloader valve portion 120 is energized to open at 240 . As illustrated, the unloader valve 120 is energized to remain open until the engine 160 achieves an engine speed greater than the predetermined speed of 850 rpm. Once the engine speed is greater than 850 rpm, the unloader valve portion 120 is de-energized and allowed to close at 260 , i.e., the VCU 140 ceases to energize the unloader valve portion 120 . If, at 220 , the engine speed is greater than or equal to 300 rpm, or at 230 , the temperature of the hydraulic fluid 151 is greater than or equal to 0° C., the unloader valve 120 is set to close.
Having described the preferred embodiment, it will become apparent that various modifications can be made without departing from the scope of the invention as defined in the accompanying claims. The invention has been described as an integral hydraulic pump and valve arrangement but would work if the pump portion 110 and the unloader valve portion 120 were, not integrated, i.e., physically separated, yet in fluid communication with each other.
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Parasitic hydraulic loading on an engine is significantly reduced during cold starts by using an unloader valve to divert the flow of hydraulic fluid from a hydraulic pump to a hydraulic actuator, i.e., load source, recirculating the hydraulic fluid between the hydraulic pump and the unloader valve.
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This is a division of application Ser. No. 07/760,745, filed Oct. 15, 1992, which is a division of application Ser. No. 07/478,136, filed Feb. 9, 1990 now U.S. Pat. No. 5,136,685.
TECHNICAL FIELD
The present invention relates to a fuzzy logic operation circuit in which charge coupled devices (CCD) are used and more particularly to a fuzzy logic operation circuit and a fuzzy computer using the logic operation circuit which is capable of performing high-speed logic operations by utilizing the properties of CCDs.
BACKGROUND OF THE INVENTION
Since professor L. A. Zadeh of the University of California presented the fuzzy theory and its applications in "Journal of Information and Control" in 1965, research and development for practical applications of fuzzy control fuzzy computers and fuzzy artificial intelligence in which the fuzzy theory is employed have been ongoing.
Fuzzy control expresses control algorithms by using an "if . . . then" format (fuzzy control routine). A fuzzy computer executes the algorithms by using fuzzy inference in order to measure the senses of a human or the ambiguity of a word such as, for example: "knack": that which is obtained from a long period of experience of those skilled workers (expert) in a specific field.
That is ambiguous word information corresponding, for example, to "slow", "medium" and "quick", as used to describe a speed, is expressed by respective membership functions. One fact is verified by the respective fuzzy rules of an "if . . . then" format to check its approximate agreement. A membership function of the consequent section "then" is cut by the agreement of the antecedent section "if" of the above-mentioned rule, and after respective inference results are obtained, an essence is extracted from all the inference results consisting of the ambiguous information (this is called defuzzification).
Numerous defuzzification methods have been proposed. However, in practice, a center-of-gravity method is most widely used.
Next, let's consider a computer which performs fuzzy inference (here, this is tentatively called a "fuzzy computer"). Information handled by a conventional digital computer is all definite information expressed by binary information (binary words of a combination of 0 and 1). A fuzzy computer, however, must handle information specified by a membership function for each ambiguous word information. Hence, a fuzzy computer must process a great amount of information expressed by decimals, for example, 0., 0.1, 0.2, 0.3, . . . in grades from 0 to 1 with respect to respective membership functions, concerning a word to be processed (this is tentatively called a "fuzzy word").
Although a fuzzy computer handles ambiguous word information such as "slow", "quicker" and so forth, a "fact" (input information) of the inference executed by a fuzzy logic operation circuit in a fuzzy computer and output information are definite values (e.g., 15°, 5 V, etc.). Accordingly, if this input and output information cannot be processed at high speed, even if fuzzy inference in execution in the fuzzy computer is performed at high speed, its processing is limited greatly.
Even after professor Mamdani of London University presented in 1974 the first expert system by means of fuzzy control in which fuzzy theory is applied (fuzzy control for a steam engine), the history of fuzzy control technology is still short. It has not been until recently that some full-fledged expert systems with highly rated advantages have been realized.
In the execution of fuzzy inference for fuzzy control, it has been found in the art that the inference operation may be completed faster by utilizing dedicated hardware (i.e. a digital computer). Accordingly, the speed from the time a "fact" is input to the time the result of its inference is displayed on a display section is limited by the processing performance of the above-mentioned digital computer. As a result, fuzzy logic operation circuits exclusively used for a fuzzy computer have been expected which are capable of effectively performing not only input and output of fuzzy information but also the very fuzzy logic operations themselves.
A method of directly mapping the current state quantity of devices to control quantity via digital memory has been proposed. The method has the possibility of reducing logic operation time remarkably. Fine adjustments of the parameters are, however, difficult. In addition, analog fuzzy information processing chips composed of a combination of a number of operational amplifications and so forth have now been developed, but they are not sufficient in logic operation, speed or processing performance.
Charge transfer type devices represented by CCDs are comparatively new Si devices announced by Boyle in 1970 and utilize minority carriers and dynamic electric-field effects. The devices have been developed considerably by novel technical concepts such that functional devices are constituted by charge transfer and the use of LSI technology. By using the properties of CCDs, image pickup devices, large capacity memories, analog signal processing, and numerous kinds of filters, including matched filters, delay lines and so forth, have been put to practical use. However, at present, they are not used to any degree in a high-level information processing apparatus such as a fuzzy computer.
An object of the present invention is to provide a basic fuzzy logic operation circuit in which the properties of the CCDs, resulting from a charge transfer function, are employed to provide the following multi-functionality: analog memory; direct handling of an analog quantity; low power consumption; low noise; and an economical fuzzy computer using the circuit.
The minimum functions necessary for a fuzzy operation can be realized by the following two kinds of basic functions and their combination because of the properties of a well-known "fuzzy inference engine" (e.g., architecture in which A and B as a knowledge and A' as a fact are input and B' is output as a conclusion), (for details, see "Concept of a Fuzzy Computer", by Retsu Yamakawa, published in Aug. 19, 1988, Kodansha Publishing Co.). The minimum functions are summarized as follows:
i) a function to select a maximum or minimum quantity of information from among a plurality of fuzzy information and output it, and
ii) a function capable of determining its representative value for a plurality of ranked fuzzy information.
The present invention comprises basic fuzzy logic operation circuit devices and a defuzzifier using CCDs and a fuzzy computer composed of a number of the above-mentioned fuzzy logic operation circuit devices and connected with the above-mentioned defuzzifier.
Since a basic fuzzy logic operation circuit device and defuzzifier having AND and OR functions are constructed by using CCDs, a high-speed fuzzy computer exclusively used for fuzzy control can be realized. This is done by connecting as many of the above-mentioned circuit devices in parallel as there are numbers of fuzzy variables and connecting the above-mentioned defuzzifier to its output side.
BRIEF DESCRIPTION OF THE DRAWINGS
These and other objects, features and advantages of the present invention will become clear by the following description of the preferred embodiments of the present invention with reference to the accompanying drawings, wherein:
FIGS. 1(a) and (b) are views showing an embodiment of an output selection circuit for two inputs using CCDs, which is one of the embodiments of a basic circuit of the present invention, and its symbols;
FIGS. 2(a) and (b) are views of another embodiment of an output selection circuit for two inputs of charge input type;
FIGS. 3(a) and (b) are views showing a large and small selection circuit for two inputs which is formed of a combination of the two from the circuits of FIG. 1 or 2 and their symbols;
FIGS. 4(a) and (b) are views showing an embodiment of a large input signal selection circuit for a number of input signals in which a number of selection circuits of FIG. 3 are used and resistors and operational amplifiers are connected in a matrix form and their symbols;
FIGS. 5(a) and (b) are views showing an embodiment of a fuzzy AND-OR circuit and its symbols;
FIG. 6 is a view showing logic operation outputs of two fuzzy membership functions;
FIG. 7(a) and (b) are views showing an embodiment of a defuzzifier using CCDs and its symbols;
FIG. 8 is a view showing an embodiment of a fuzzy computer formed by a number of respective basic circuits of the present invention;
FIG. 9(a) and (b) are simulation model views for explaining a process from the time a fuzzy input is given and a truncation and composition signal is output through an agreement calculation; and
FIG. 10(a) and (b) are a schematic configurational view of a fuzzy computer in the case where a fuzzy control rule has two AND front subject sections.
DETAILED DESCRIPTION OF THE INVENTION
In the figures, ID indicates an input diode; G 1 and G 2 , the first and second gate electrodes respectively; T 1 , T 2 and T 3 , the first to third transfer electrodes respectively; OG 1 and OG 2 , the first and second output gate electrodes respectively; OD1 and OD2, the first and second output diodes respectively; FG, a floating gate; H, a channel stop; 1 and 2, OR gates; 3, an inverter; 4, a FG amplifier; 50 and 60, shift registers; M 11 to M KN , the first group of memory devices; 100, an agreement calculation section; 200, a truncation and composition section; M 11 , to M KN ', the second group of memory devices; 300, a defuzzifier; C, a large and small selection circuit for inputs; E, a maximum input selection circuit for a number of inputs; and A 1 to A K , amplifiers.
FIG. 1(a) shows one embodiment of a fuzzy logic operation circuit using CCDs of the present invention. In this embodiment, a three-phase PE (potential equilibration) method is adopted to inject signal charges to the potential well of the transfer electrodes of CCDs.
In the figure, ID indicates an input diode; G 1 , the first gate electrode; G 2 , the second gate electrode; T 1 , the first transfer electrode; T 2 , the second transfer electrode; T 3 , the third transfer electrode; FG, a floating gate; OG 1 , the first output gate electrode; OG 2 , the second output gate electrode; OD 1 , the first output diode; OD 2 , the second output diode; 1 and 2, OR gates; 3, an inverter; 4, a FG amplifier; H, a channel stop; S, an input terminal; φ 1 , φ 2 and φ 3 , input terminals for driving pulses; F, a control signal pick-out terminal; C, an input terminal for a selection signal; and OUT 1 and OUT 2 , output terminals.
In operation, a short-pulse voltage is applied to an ID and charges from the ID are injected into the potential well of G 2 by crossing the barrier of G 1 . Next, the ID is reverse biased and extra charges exceeding the barrier of G1 are injected into the ID, after which driving pulses φ 2 , φ 3 and φ 1 are respectively provided in turn to T 2 , T 3 and T 1 to transfer charges.
When the charges transferred from the input side reach the floating gate (FG), the charges are detected by the floating gate. A voltage signal corresponding to the charge quantity is induced and amplified via a floating gate amplifier 4, after which a corresponding signal is picked out from the pick-out terminal.
On the other hand, since a selection signal is provided to the terminal C, the output gate OG 1 or OG 2 is actuated via gate 1 or 2, and a charge signal is output from the corresponding output diode OD 1 or OD 2 . When the selection signal is low, the output signal OUT 2 (which is greater) may be selected. When its level is high, the output signal OUT 1 (which is smaller) may be selected.
FIG. 1(b) is a view showing the logic operation circuit of FIG. 1(a) which is formed to operate as described above by using one symbol.
As described later, in the present invention, another selection circuit is formed by combining a number of basic circuit devices represented by symbols.
In a case where input and output signals are input and output to the basic circuit in the form of charges, an input diode ID at the input side, the first and second gate electrodes G 1 and G 2 , and the first and second output diodes OD 1 and OD 2 can be omitted. FIG. 2(a) shows such a structure, and FIG. 2(b) illustrates their symbols.
FIG. 3(a) shows an embodiment of a minimum value selection circuit for two input signals formed of a combination of two basic circuits shown in FIG. 1(b) or FIG. 2(b). The above-mentioned basic circuits 10 and 11 are connected in parallel. Each of the terminals F is connected to each of the inputs of a comparator 12, and the output side of the above-mentioned comparator 12 is connected to the terminal C of a basic circuit 10 via an inverter 13 and connected to the terminal C of a basic circuit 11. As a result, by comparing a control signal detected by each of the floating gate terminals F of the two basic circuits 10 and 11, an output corresponding to the greater transfer charges can be obtained from the output terminal OUT 2 and an output corresponding to the smaller transfer charges can be obtained from the output terminal OUT 1 .
FIG. 3(b) shows symbols of the basic circuit of FIG. 3(a) which is integrally formed to operate in this way.
FIG. 4(a) shows an embodiment of a selection circuit which selects a maximum input signal from among a number of input signals and outputs it.
In this embodiment, a matrix-like structure (equivalent to an analog electronic circuit model of a neural network; see "Neural Computers" by Aihara Kazuyuki, published by Tokyo Denki University, 1988) of the outputs from F 1 , F 2 , F 3 . . . F N terminals and inputs provided to C 1 , C 2 , C 3 . . . C N is provided using operational amplifiers A 1 , A 2 , A 3 . . . A N and resistors R 11 to R 1N , R 21 to R 2N , R 31 to R 3N , . . . R N1 to R NN as shown in FIG. 4(a). Using basic circuits 1, 3, 3, . . . N as shown in FIG. 1(b) or FIG. 2(b) enables a selection of the output from the basic circuit in which is given a maximum input signal among all input signals to be made.
When input and output characteristics of respective operational amplifiers are as shown in FIG. 4, an equal number of input voltages are added via resistors R i1 to R iN (i=1, 2, 3 . . . N) at each stage. Therefore, by making the threshold value of the input and output characteristics of respective amplifiers proper, a maximum signal among input signals can be picked out from the output terminal.
FIG. 4(b) shows the basic circuit of FIG. 4(a) which selects a maximum signal among a number of input signals in this way by a symbol as a single unit. In FIG. 4, output from the terminal D rain is not necessary for the time being. However, it is apparent to one skilled in the art that a minimum signal among a number of input signals can also be selected by properly selecting input and output characteristics of an amplifier.
FIG. 5(a) shows an embodiment of fuzzy OR and fuzzy AND circuits by which OR logic and AND logic functions can be achieved. In this embodiment, if a plurality of two-input selection circuits shown in FIG. 3(b) are connected in parallel and denoted by 21, 22, 23, . . . ij, and elements F 1 and F 2 constituting two membership functions are input respectively to the two-input selection circuit, a fuzzy AND output can be picked out from one of the output terminals and a fuzzy OR can be picked out from the other output terminal. That is, as shown in FIG. 6, of the two membership functions F 1 and F 2 , a double-humped envelope becomes a fuzzy OR and the envelope of the common portion becomes a fuzzy AND.
FIG. 5(b) shows the symbols of the fuzzy AND-OR operation device of FIG. 5(a) which is formed to operate as mentioned above.
FIG. 7a and 7b shows an embodiment in which a defuzzifier necessary for a fuzzy computer is composed of CCDs. In the figure, T 1 indicates the first transfer electrode; T 2 , the second transfer electrode; T 3 , the third transfer electrode; G 1 , a gate electrode; T 4 , the fourth transfer electrode; B 1 , the first bus; B 2 the second bus; S 1 and S 2 , FET transistors; R 1 and R 2 , resistors; OR, an operational amplifier; H, a channel stop.
The gate electrode G 1 is divided into two different lengths b 1 and b 2 in each of the channels CH 1 to CH N . The length division ratio b1:b2 is varied for each channel at a predetermined ratio. This ratio is called an effective area, which is effected by areas of the two portions of electrodes G 1 . For example, it is structured as b 1 /(b 1 +b 2 )=0.1, 0.2, 0.3 . . . 0.9 from the left. Each channel corresponds to the number of elements forming a membership function, namely, the number of elements of a fuzzy word.
With such a structure, a function to determine a representative value for a plurality of ranked signals (the function ii mentioned at the beginning) can be achieved. In other words, an operation to find the center of gravity of the whole fuzzy inference results can be performed.
In operation, charges q 1 , q 2 , q 3 . . . q N provided to the input of the defuzzifier are transferred via transfer electrodes T 1 , T 2 , and T 3 , to which driving pulses φ 3 , φ 1 and φ 2 , are applied to the gate electrode G 1 . Until they reach the transfer electrode T 4 , after passing through channels of different division ratios b 1 /(b 1 +b 2 ) in the gate electrode G 1 , charges determined by the above-mentioned division ratio b 1 and b 2 are collected on buses B 1 and B 2 . Because bus B 2 is connected to the source of a FET transistor S 2 and bus B 1 is connected to the source of a FET transistor S 1 , when φ 1 is provided to the gate electrode S 1 and S 2 , a potential difference corresponding to the integrated difference in charges between buses B 1 and B 2 is picked out and output via the operational amplifier OP.
Potentials VB 1 on the bus B 1 and VB 2 on the bus B 2 and potential difference V between VB 1 and VB 2 are expressed by the following formulae respectively:
VB.sub.1 =K{(b.sub.1·1 ×q.sub.1)+(b.sub.1·2 ×q.sub.2)+(b.sub.1·3 ×q.sub.3)+. . . +(b.sub.1·n ×q.sub.n)}
VB.sub.2 =K{(b.sub.2·1 ×q.sub.1)+(b.sub.2·2 ×q.sub.2)+(b.sub.2·3 33 q.sub.3)+ . . . +(b.sub.2·n ×q.sub.n)}
V=VB.sub.1 -VB.sub.2
=K[{(b.sub.1·1 ×q.sub.1)+(b.sub.1·2 ×q.sub.2)+ . . . +(b.sub.1·n ×q.sub.n)}-{(b.sub.2·1 ×q.sub.1)+(b.sub.2·2 ×q.sub.2)+ . . . +(b.sub.2·n ×q.sub.n)}]
For example, because the G 1 of each channel is divided at ratios of 1:9, 2:8, 3:7 . . . 9:1 from the left in the embodiment shown in FIG. 7(a) (assuming that it has 10 channels), the potential V output from the operational amplifier OP is expressed by:
V=K{(0.9×q.sub.1 +0.8×q.sub.2 +0.7×q.sub.3, . . . 0.1×q.sub.9)-(0.1×q.sub.1 +0.2×q.sub.2 +0.3×q.sub.3, . . . 0.9×q.sub.9)}
(where K is a sensitivity coefficient determined by a circuit).
The center-of-gravity position of the charge distribution can be picked out from the fourth transfer electrode T 4 by providing a means (not shown) capable of detecting the total amount of charge transferred via all the channels. That is, the above-mentioned V is the same as that of the equation for finding the moment of the charge quantity of all channels. Therefore, in a case where the above-mentioned V directly expresses the center position of the charge distribution and the total quantity of charge fluctuates, if the total quantity of input charges q 1 +q 2 +q 3 + . . . q 9 is constant, the center-of-gravity position can be determined similarly by dividing the output by the total quantity of charges detected by T 4 . In this way, a defuzzifier, in which the center-of-gravity of a final membership function obtained from each fuzzy inference result is calculated, can be operated by fuzzy control.
FIG. 7(b) shows symbols of the basic circuit of the defuzzifier of FIG. 7(a) which is formed to operate as described above.
FIG. 8 shows an embodiment of a fuzzy computer configured using the above-mentioned basic circuit devices of the present invention.
The fuzzy computer of the present invention is broadly comprised of the following three sections: an agreement calculation section 100; a truncation and composition section 200; and a defuzzifier 300.
The agreement calculation section 100 comprises memory devices M 11 to M 1N in which the elements of the first membership function f 1 are stored, memory devices M 21 to M 2N in which the elements of the second membership function f 2 are stored, . . . memory devices M K1 to M KN in which the elements of the K-th membership function f K are stored. These correspond to respective antecedent sections "if" of fuzzy control rules 1, 2, 3, . . . K. The calculation section 100 also comprises selection circuit C composed of the elements shown in FIG. 3(b) which select the smaller of two inputs, and selection circuit E shown in FIG. 4(b) which selects a maximum value among the signals output from the selection circuit.
The truncation and composition section 200 comprises memory devices M 11 ' to M 1N ' in which the elements of the first membership function f 1 ' are stored, memory devices M 21 ' to M 2N ' in which the elements of the second membership function f 2 are stored, . . . memory devices M K1 ' to M KN ' in which the elements of the K-th membership function f K ' are stored. These correspond to respective consequent sections "then" of fuzzy control rules 1, 2, 3, . . . K. The truncation and composition section 200 also comprises respective selection circuits C which truncate (cut out) respective membership functions of the above-mentioned consequent section "then" by respective outputs from respective maximum value selection circuits E of the agreement calculation section 100, and respective selection circuits E which select a maximum output from among the outputs from the above-mentioned respective selection circuits C.
The defuzzifier 300 comprises a basic circuit shown in FIG. 7(b).
In FIG. 8, 50 designates a first shift register which sends respective element information of the above-mentioned respective membership functions f 1 , f 2 . . . f k , input from the input terminal A, to the above-mentioned respective storage devices. A second shift register 60 sends respective element information of the above-mentioned respective membership functions f 1 ', f 2 ', . . . f K ' input from the input terminal B, to the above-mentioned respective memory devices M 11 ' to M 1N ', M 21 ' to M 2N ' . . . , M K1 ' to M KN ', and A 1 to A K , amplifiers.
The operation of the fuzzy computer of the present invention constructed as described above will be described below.
When respective elements N 11 to N 1N forming a fuzzy word (a membership function of a fact) corresponding to one "fact" are input to the agreement calculation section 100, they are compared with the contents of respective membership functions f 1 , f 2 , . . . f K stored in respective memory devices M 11 to M 12 , M 21 to M 2N . . . , M K1 to M KN and a smaller signal is selected from respective selection circuits C. Maximum outputs among the outputs from respective selection circuits C, corresponding to respective fuzzy control rules 1, 2, 3 . . . K, are output from respective selection circuits E and then are sent to the truncation and composition section 200 via respective amplifiers A 1 A N .
In this way, respective outputs from respective circuits E (respective maximum values) and respective membership functions f 1 ', f 2 ', . . . f N ' of the consequent section "then" of fuzzy control rules, which are stored in respective memory devices M 11 ' to M 1N ', M 21 ' to M 2N ' . . . , M K1 ' to M KN ', are truncated.
In this way, respective maximum values corresponding to envelopes of respective membership functions f 1 ', F 2 ', . . . f N 40 , which are cut by predetermined values (i.e., signals u 1 to u N ) corresponding to one total inference result membership function in which respective fuzzy information results are combined, are output from respective maximum value selection circuits C of the truncation and composition section 200, and these signals are provided to the defuzzifier 300.
The defuzzifier 300 determines the moment of respective input signals u 1 to u N to find the center-of-gravity position of the above-mentioned total inference result membership function on the basis of the principles explained in FIG. 7(a), and outputs it as a determined value.
FIG. 9(a) shows a state in which the agreement of the fuzzy input, which is input to the agreement calculation means 100 of the fuzzy computer of FIG. 8 as one fact, is checked with respective membership functions of the fuzzy control rule antecedent section stored in respective vertical storage devices. These agreement distribution outputs are shown as generated in a simulation model.
FIG. 9(b) shows a state in which respective membership functions of the consequent sections of the above-mentioned fuzzy rules are cut and combined by respective agreement outputs applied to the truncation and composition section 200 of the fuzzy computer shown in FIG. 8, in another simulation model.
In the fuzzy computer shown in FIG. 8, since input Fi (shown in FIG. 10) is one membership function, the antecedent sections of the fuzzy control rules are one each. That is, for simplification, FIG. 8 can be shown as in FIG. 10(a).
However, in a case where the antecedent section "if" of the above-mentioned rule is set, for example, with the following two conditions (AND) as in "if A 1 and A 2 and d, then let B be e", two membership functions of Fi 1 and Fi 2 are handled for the input of a fact. Therefore, it can be structured as shown in FIG. 10(b) in this case. That is, two agreement calculation sections 100 are used to pick out a fuzzy AND output of the fuzzy AND-OR circuit shown in FIG. 5. It is provided to the truncation and composition section 200. If the center of gravity is picked out via defuzzifiers 300-1 and 300-2, then more complex operations can be performed.
Since the same is true of a case involving three or more antecedent sections of a fuzzy control rule, more complex logic operation control can be performed by the fuzzy computer of the present invention.
Heretofore, embodiments of numerous kinds of basic logic operation circuits required to perform fuzzy logic operations and a fuzzy computer using these circuit devices have been explained. In the present invention, basic logic operation circuits are constructed, including defuzzifiers, by using CCD devices having well suited properties and characteristics, and a full-fledged fuzzy computer is constructed using a number of such fuzzy logic operation circuit devices.
Unlike a fuzzy control apparatus in which a conventional digital computer is used in the input and output sections, the fuzzy computer of the present invention is constructed in "massive parallelism". Therefore, fast and efficient information processing can be performed.
The use of a CCD light-receiving device group as a fuzzy input signal source, as in the basic circuits shown in FIGS. 1 and 2, enables an illuminance distribution state on a light-receiving device group to which light is radiated to be processed directly. Therefore, the present invention is effective in the fields of photometry and image processing.
As many apparently widely different embodiments of this invention may be made without departing from the spirit and scope thereof, it is understood that the invention is not limited to the specific embodiments thereof except as defined in the appended claims.
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A fuzzy computer includes a defuzzifier composed of charge coupled devices which intake and transfer a set of fuzzy data elements in parallel. Pairs of positive and negative gate electrodes are located transversely to the charge coupled devices. The gate electrodes in each pair differ in their effective area to the corresponding charge coupled devices and all the positive and negative electrodes are connected together in respective groups. Each of the positive and negative groups senses independently as an electronic signal, such as voltage, the sum of weighted charge value at each charge coupled device behind the electrodes, multiplying by the weighing factors which are determined by the effective area of each electrode. A total output is obtained as the difference of the output signals at the positive and negative electrode groups.
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ORIGIN OF THE INVENTION
The invention described herein was made by an employee of the United States Government and may be manufactured and used by or for the Government for governmental purposes without payment of any royalties thereon or therefor.
BACKGROUND OF THE INVENTION
1. Technical Field of the Invention
The present invention relates in general to wing systems for use on a vehicle in aerodynamic or hydrodynamic applications, and it more particularly relates to a low-speed, conformally stowable secondary wing system for use in high speed civil transport aircraft to optimize vehicle performance and efficiency.
2. Description of the Prior Art
Canards, including small forward-mounted secondary wings, increase the total wing surface area of an aircraft for improving the low speed lift-to-drag ratio and trim characteristics of the aircraft. While canard concepts have been used in supersonic aircraft to increase low-speed performance, these designs do not allow for optimal high-speed performance and aerodynamic efficiency.
Existing canard concepts for application to high-speed aircraft fall into two general categories: fixed non-retractable configurations, and symmetrically retractable configurations which stow into cavities within the forward fuselage. An exemplary fixed canard is used in the supersonic XB-70 Valkyrie aircraft and remains deployed throughout all phases of flight. Such fixed canards allow for increased lift capabilities and greater stability at lower speeds, thus decreasing the amount of engine thrust and noise during takeoff and landing. Because fixed canards remain exposed to the airstream at supersonic cruise speeds, their induced, profile, and skin friction drags represent significant portions of the overall drag on the aircraft. Because the economic success of a high speed civil transport aircraft is highly dependent upon reducing the cruise drag to the lowest possible level, fixed canards are not desirable in this or similar vehicles.
A hybrid concept of the fixed canard design was employed by the Beechcraft Starship 1 aircraft, which utilized relatively long and narrow, dual-position symmetric canards. At low speeds the canard is fully deployed, while at high speeds the canard is partially swept back. The canard is used in the forward position during take-off and landing to offset the negative pitching moments induced by extension of the trailing edge flaps on the main wing, while it is partially swept back to decrease drag and optimize trim characteristics at cruise speeds. While this variable geometry canard design offers a compromise between low speed performance and high speed efficiency, it is not an optimal design for high speed civil transport aircraft as the canard remains exposed to the airstream during all phases of flight.
In an attempt to optimize low speed performance and high speed efficiency, the Tupolev Tu-144 supersonic transport vehicle employed two symmetrically retractable canards which stow independently into cavities within the forward fuselage. While the retractable canard concept improves upon the problems of fixed-wing and variable geometry canards, several shortcomings remain. First, the two separate hinge and actuation systems or mechanisms required to fold and support the right and left canards add to the overall weight of the aircraft. Second, the structural complexity of the hinge and deployment/retraction actuation systems increases the probability of failure during flight. Third, although the canards are stowed quasi-conformally within cavities in the upper fuselage behind the cockpit, the overall surface smoothness of the fuselage is compromised by the presence of the canards. Fourth, the rectangular platform (e.g., wing shape) used for the Tu-144 canards is not ideal for optimum aerodynamic efficiency. While leading and trailing edge high-lift devices (e.g., slats and flaps) may be used to optimize lift characteristics, such devices further add to the structural complexity and overall weight of the canard and may increase the probability of mechanical failure.
Another aircraft designed to provide low-speed high-lift capability while maintaining high-speed efficiency is the NASA AD-1 oblique wing aircraft. This small aircraft utilizes a single, quasi-elliptical, pivotable wing which rotates about a central axis. At low flight speeds, the wing is positioned perpendicularly to the fuselage, thus providing good lift characteristics without complex high-lift systems. During high-speed flight, the wing is pivoted to form an oblique angle of up to 60 degrees with the main axis of the fuselage, thus reducing drag and increasing speed. However, because the oblique wing is the primary lifting surface of the aircraft, it is not conformally stowed during the high speed flight phase.
A movable wing is used in the pivotable mono wing cruise missile described in U.S. Pat. No. 4,842,218 to Groutage et al. The missile has a single, pivotable wing which is positionable to either a captive carry position or an extended free-flight position. While the pivotable wing described in the Groutage et al. patent may be suitable as a primary wing for a cruise missile, it is not suitable for use as a low-speed secondary wing system on a supersonic aircraft. The spring-loaded, one-way deployment mechanism described in the Groutage et al. patent is not capable of retracting the wing during flight, nor is the wing conformally stowable.
Various canard concepts that relate to the general field of the present invention are illustrated in the following patents:
U.S. Pat. No. 4,161,300 to Schwaerzler, et al.;
U.S. Pat. No. 4,542,866 to Caldwell, et al.;
U.S. Pat. No. 4,641,800 to Rutan;
U.S. Pat. No. 4,484,700 to Lockheed;
U.S. Pat. No. 4,899,954 to Pruszenski, Jr.;
U.S. Pat. No. 5,071,088 to Betts;
U.S. Pat. No. 5,192,037 to Moorefield;
U.S. Pat. No. 5,398,888 to Gerhardt;
U.S. Pat. No. 5,495,999 to Cymara;
U.S. Pat. No. 5,564,652 to Trimbath;
SUMMARY OF THE INVENTION
The present invention provides a secondary wing system having a single pivoting canard that can be deployed to augment the lift, stability, and control of an aircraft during various flight regimes, and that can be conformally retracted into the fuselage in order to minimize drag at high speeds.
The secondary wing system of the present invention includes a single-canard with an aerodynamically efficient planform shape for reducing engine power required for low-speed operation, thus resulting in lower noise levels during take-off, climb-out, approach, and landing.
The secondary wing system of the present invention provides a retractable canard with leading and trailing-edge control surfaces to enhance the aerodynamic performance of the airplane.
The system of the present invention further provides a high-strength ring and track mounting and rotation mechanism that connects the canard to the aircraft fuselage, and that permits the canard to rotate and to change incidence, while minimizing intrusion of the mechanical rotation hardware into the volume of the fuselage.
The secondary wing system of the present invention also provides a novel assembly of retractable fairings which streamline the leading and trailing edges of the canard when it is stowed, thus optimizing aerodynamic efficiency for high-speed flight.
Briefly, the foregoing and further features and objects of the present invention are realized by a secondary wing system that augments the lift, stability, and control of the aircraft at subsonic speeds. The secondary wing system includes a mechanism that allows the canard to be retracted within the contour of the aircraft fuselage from an operational position to a stowed position.
The top surface of the canard is exposed to air flow in the stowed position, and is contoured to integrate aerodynamically and smoothly within the contour of the fuselage when the canard is retracted for high speed flight. The bottom portion of the canard is substantially flat for rotation into a storage recess within the fuselage. The single canard rotates about a vertical axis at its spanwise midpoint. The canard can be positioned between a range of sweep angles during flight and a stowed position in which its span is substantially parallel to the aircraft fuselage.
The canard can be deployed and retracted during flight. The deployment mechanism includes a circular mounting ring and drive mechanism that connects the canard with the fuselage and permits it to rotate and to change incidence. The deployment mechanism further includes retractable fairings which serve to streamline the wing when it is retracted into the top of the fuselage.
The canard of the present invention may additionally include a mechanism for securing the tips of the secondary wing to the fuselage when stowed, to prevent flutter and damage to the wing due to aerodynamic loads at high-speed, supersonic flight conditions.
An alternative embodiment of the secondary wing system of the present invention includes a constant-chord retractable canard configuration with arc-shaped wing tips that can be used on fuselage shapes with a constant area distribution from front to back. Additional alternative embodiments of the present invention include application of the secondary wing system concept as a retractable horizontal tail for use at the rear of an aircraft, and application of the secondary wing system to other classes of vehicles (e.g. hydrodynamic vehicles) to enhance maneuverability and performance.
BRIEF DESCRIPTION OF THE DRAWING
The above and other features of the present invention and the manner of attaining them will become apparent, and the invention itself will be best understood, by reference to the following description and the accompanying drawing, wherein:
FIG. 1 is a top plan view of an aircraft equipped with a secondary wing system according to the present invention, and showing a single-piece canard in stowed, intermediate, and deployed positions;
FIG. 2 is an enlarged top plan view of the secondary wing system of FIG. 1;
FIG. 3 is a side view of the aircraft of FIG. 1, showing the canard in the deployed position;
FIG. 4 is an enlarged side view of the canard of FIG. 3, shown in the deployed position;
FIG. 5 is an enlarged side view of the canard of FIG. 3 shown in the stowed position;
FIG. 6 is a front view of the aircraft of FIG. 1 showing the canard in the deployed position;
FIG. 7 is a cross sectional view of an upper fuselage of the aircraft of FIG. 5, taken along line 7--7, showing the canard in the stowed position;
FIG. 8 is a cross-sectional view of the upper fuselage of the aircraft of FIG. 5, taken along line 8--8, showing a retractable fairing which engages a side-facing step created between one half of the leading-edge of the canard and the top of the fuselage when the canard is stowed;
FIG. 9 is an enlarged cross-sectional view of the upper fuselage of FIG. 8, showing the retractable fairing in its extended position (solid lines) and its retracted position (dashed lines);
FIG. 10 is a cross sectional view of the aircraft of FIG. 6, taken across line 10--10, showing a variable incidence mechanism in use with the canard in its deployed position;
FIG. 11 is a top view of an alternative canard in use on an aircraft with a fuselage having a constant cross-sectional area;
FIG. 12 is a side view of the aircraft of FIG. 11, showing the canard in the deployed position;
FIG. 13 is a bottom view of part of an aircraft fuselage equipped with a secondary wing system according to the present invention, showing a retractable tail in stowed, intermediate, and deployed positions; and
FIG. 14 is a side view of the aircraft fuselage of FIG. 11, showing the retractable horizontal tail in a deployed position (solid line) and in a stowed position (dashed line).
Similar numerals refer to similar elements in the drawing. It should be understood that the sizes of the different components in the drawing are not in exact proportion, and are shown for visual clarity and for the purpose of explanation.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
FIG. 1 illustrates an aircraft 10 having a fuselage 11 equipped with a secondary wing system 12 according to the present invention. The secondary wing system 12 is incorporated in the upper portion 14 of a forward fuselage 15 that forms part of the fuselage 11. The secondary wing system 12 is positioned at an intermediate location between a nose 16 and a main or primary wing 18 of the aircraft 10.
The secondary wing system 12 includes a one-piece secondary wing or canard 20 which is secured via a structural attachment and rotation ring assembly 22 to the forward fuselage 15. The canard 20 is deployed and retracted within a selected range of angles by rotating about a vertical axis of rotation R--R at the midpoint of its span, as illustrated in FIGS. 4 through 8. When deployed, the canard 20 provides supplementary lift, stability and flight control. When the canard 20 is not in use, it is stowed fully and conformally within the aerodynamic contour of the upper portion 14 of the forward fuselage 15, so that it does not increase the drag on the aircraft 10.
The operation of the secondary wing system 12 will be described with further reference to FIG. 2. Prior to takeoff, the aircraft pilot activates the secondary wing system 12 by deploying the canard 20 from an initial stowed position (shown in dashed lines and referenced by the numeral 24) within the contour of the forward fuselage 15 to a fully deployed position (shown in solid lines and referenced by the numeral 26), such that the longitudinal axis X--X of the canard 20 is substantially normal to the longitudinal axis Y--Y of the forward fuselage 14. When the canard 20 is deployed it supplements the main wing 18 by providing additional wing surface area for generation of lift at low speeds.
During take-off, the canard 20 remains substantially perpendicular to the forward fuselage 15. As the aircraft 10 accelerates, the canard 20 may be progressively rotated to intermediate positions (shown in dashed lines and referenced by the numeral 25) between the fully deployed position 26 and the stowed position 24, and thereafter to its fully deployed position 26 in order to optimize the control and lift characteristics of the aircraft 10. In these intermediate positions 25 the effective span of the canard 20 is reduced. Alternatively, the canard 20 is rotated to its fully deployed position 26.
In certain phases of the flight, it may be desirable to leave the canard 20 partly or fully deployed to optimize the performance of the aircraft 10. At a predetermined aircraft speed the canard 20 may no longer be necessary to supplement lift and control of the aircraft 10, and is rotated to the conformally stowed position 24 within the contour of the forward fuselage 15 to minimize drag. As soon as the canard 20 is fully stowed, two automatic latch mechanisms 35, 36 (FIG. 5) are activated to secure the ends or tips of the canard 20 against airloads which may arise during high-speed flight, and further to secure the tips of the canard 20 during stowage to prevent against flutter during high-speed cruise. The two latch mechanisms 35, 36 are located in the upper portion 14, and are comprised of automatic fail safe latching pins which engage receptacles on the lower surface of the canard.
On deceleration from cruise flight conditions and landing, the canard 20 is deployed from its stowed position 24 to enhance aircraft performance, stability and control at lower speeds. Low speeds include subsonic speeds such as 250 knots. The angles of deployment of the canard 20 may be automatically adjusted by a flight control system (not shown) for optimized stability and control. Upon approach to landing, the canard 20 may be rotated to its fully deployed position 26 to provide maximum lift.
The canard 20 is an airfoil defined by a leading edge 30 and a trailing edge 32. The leading edge 30 optionally includes one or more control surfaces 52, 54, and the trailing edge 32 optionally includes one or more control surfaces 58, 60. The canard 20 has a quasi-elliptical shape for high aerodynamic efficiency. It should be clear to a person of ordinary skill in the field that the canard 20 may have other aerodynamic shapes. With further reference to FIG. 7, the canard 20 has a substantially flat underside 37 and an upper surface or contour 39 which is determined by, and which complements the external contour 44 of the upper portion 14 of the forward fuselage 15.
The quasi-elliptical planform shape of the canard 20 is derived from a waterline cut through the upper portion 14 of the front of the area-ruled fuselage shape which is characteristic of supersonic aircraft. The canard 20 and its control surfaces 52, 54, 58, 60 may be made of metallic or composite or any other suitable materials. As shown in FIG. 2, the canard 20 may include a high-strength, full-span structural spar (shown in dashed lines and referenced by the numeral 61) located near the axis of rotation R--R, for optimizing the strength of the secondary wing system 12 while minimizing its weight. The spar 61 is tapered to fit within the contour of the canard airfoil 20. The spar 61 may be made of a metallic, composite, or any other suitable material. The spar 61 is similar to a conventional spar, and carries the aerodynamic loads generated by the canard 20 into the structural attachment and rotation ring assembly 22.
With reference to FIG. 2, the leading edge control surfaces or slats 52, 54 are generally identical, and are located symmetrically relative to the longitudinal axis Y--Y of the forward fuselage 15. The slats 52, 54 are movably secured to the leading edge 30 of the canard 20 by means of active or passive deployment mechanisms. The slats 52, 54 alter the flow of air over the canard 20, and thus alter the amount of lift generated by the canard 20.
The trailing control surfaces or flaps 58, 60 are generally identical, and are located symmetrically relative to the longitudinal axis Y--Y of the forward fuselage 15. The flaps 58, 60 are movably secured to the trailing edge 32 of the canard 20, by means of active or passive deployment mechanisms. The flaps 58, 60 alter the flow of air over the canard 20, for changing the amount of lift generated by the canard 20. While the slats 52, 54 and the flaps 58, 60 are described as being symmetrically positioned, it should be clear that in other embodiments these control surfaces may be asymmetrically positioned. The deflection of the slats 52, 54 and/or the flaps 58, 60 may be controlled manually by the pilot or automatically by the flight control system. As shown in FIG. 2, the inboard edges 62, 63 of the flaps 58, 60, respectively, may be scarfed to provide clearance with the forward fuselage 15 when they are deflected.
FIG. 7 illustrates the structural attachment and rotation ring assembly 22 that secures the canard 20 to the upper surface 14 of the forward fuselage 15. The assembly 22 may be a conventional mechanism. For instance, the assembly 22 generally includes a mounting and rotation ring 65, a worm gear drive 67, and a rotation actuator 69. The ring 65 is located mid-span of the canard 20 and has its central axis coincide with the axis of rotation R--R of the canard 20. The ring 65 is circular in shape and has equally spaced-apart ridges or teeth 70 along its outer perimeter. The teeth 70 interface in a substantially normal fashion with the corkscrew-like teeth of the worm gear drive 67. Rotation of the canard 20 occurs when the actuator 69 rotates the worm gear drive 67, causing the ring 65 that is directly fastened to the canard 20 to rotate. The structural attachment and rotation ring assembly 22 provides a high-strength mounting and rotation mechanism which allows the use of a single, stowable canard 20 while minimizing intrusion of the mechanical rotation hardware into the volume of the fuselage 15. It should be clear to a person of ordinary skill in the field that alternative rotation mechanisms may be employed.
Referring to FIGS. 3, 4, 5 and 7, a substantially flat stowage surface 81 is formed in the upper portion 14 of the forward fuselage 15. The stowage surface 81 cooperates with the flat underside 37 of the canard 20 for enabling the canard 20 to rotate with minimal friction between the stowed position 24 and the deployed position 26. The stowage surface 81 is shown in FIG. 2 as being defined by the two dashed lines 83, 84. In one embodiment the length of the stowage surface 81, i.e., the distance between the two lines 83 and 84 is approximately equal to the full length or span of the canard 20.
FIGS. 3 and 4 illustrate that when the canard 20 is deployed, its airfoil shape protrudes above the stowage surface 81. When the canard 20 is stowed, as shown in FIG. 5, the upper surface 39 of the canard 20 forms a generally uniform aerodynamic shape with the contour of the upper portion 14 of the forward fuselage 15. As a result, the canard 20 is stowed, it forms part of the upper surface of the forward fuselage 15 of the aircraft 10, and helps to optimize the aerodynamic efficiency of the aircraft 10 during operation at supersonic or high subsonic speeds.
Referring to FIG. 6, the canard 20 is located on the upper portion 14 of the forward fuselage 15, and has a shorter span than the main wing 18. For instance, the span of the canard 20 may vary between 25 percent and 50 percent of the span of the main wing. The aspect ratio of the canard 20 may vary between ten and twenty. The aspect ratio is defined as the span divided by the mean chord of the canard 20. Alternative embodiments of the present invention may include a canard of different dimensions or location.
With reference to FIG. 7, a longitudinal cavity 86 is formed within the fuselage external contour 44 adjacent to the stowage surface 81. When the canard 20 is in its stowed position, the cavity 86 conforms to, and houses the leading edge 30 of the canard 20, and further enables the external contour be streamlined with the upper contour 39 of the canard 20.
As shown in FIGS. 2 and 8, one half of the cavity 86, either the forward half or the aft half relative to the central axis of rotation R--R, includes a retractable fairing assembly 150 which allows rotation and deployment of the canard 20. FIG. 2 shows the placement of the retractable fairing assembly 150 adjacent to the leading edge 30 of the aft half of the stowed canard 20.
Referring now to FIG. 9, the retractable fairing assembly 150 generally includes three elements: a fairing 152, a drive actuator 154, and a linkage 156. In its extended position (shown in solid lines and referenced by the numeral 152), the fairing contains a concave recess 168 that conforms to the leading edge 30 of the stowed canard 20 for smoothing the outer shape of the forward fuselage 15 with the upper contour 39 of the canard 20 and optimizing aerodynamic efficiency. In its retracted position (shown in dashed lines and referenced by the numeral 153) the fairing fits substantially within a stowage cavity 178 within a fuselage pressure shell 180, thus allowing deployment and rotation of the canard 20.
The fairing drive actuator 154 and linkage 156 connect the fairing 152 to the forward fuselage 15 and control the position of the fairing 152. For deployment of the canard 20, the actuator 154 pulls the inner edge of the fairing 152 (the edge adjacent to the canard 20) downward while the linkage 156 allows controlled rotation of the outer edge of the fairing 152, causing the fairing 152 to retract into the stowage cavity 178. While FIGS. 8 and 9 show a single retractable fairing system 150 to streamline the aft half of the leading edge 30 of the stowed canard 20, alternative embodiments of the present invention may include more than one retractable fairing assembly on the leading and/or trailing edge of the secondary wing and may include actuator/linkage mechanisms of various types.
With reference to FIG. 10, the secondary wing system 12 of the present invention may also include a variable incidence mechanism 230 for changing the angle of incidence of the canard 20. The variable incidence mechanism 230 includes a variable incidence drive actuator 234, a support frame 236, and a hinge 238. The forward end of the frame 236 is connected to the drive actuator 234, while the rearward end of the frame 236 is attached to the hinge 238. The structural attachment and rotation ring assembly 22 is attached to the frame 236. The drive actuator 234 and the hinge 238 are attached to the forward fuselage 15.
The angle of incidence of the canard 20 may be changed from zero incidence (shown in dashed lines and referenced by the numeral 243) to a positive incidence (shown in solid lines and referenced by the numeral 244) by upward displacement of the drive actuator 234. The variable incidence mechanism 230 permits the incidence angle of the retractable canard 20 with respect to the main wing to be varied in order to optimize the aerodynamic performance of the canard 20 in various flight conditions. It should be clear to a person of ordinary skill in the field that alternative features or devices of the variable incidence mechanism 230 may be employed.
FIG. 11 illustrates an alternative secondary wing system 272 according to the present invention, for use on an aircraft 270 having a cylindrical or constant-area forward fuselage 274. The secondary wing system 272 is similar in structure and function to the secondary wing system 12 of FIG. 1. The secondary wing system 272 includes a one-piece canard 276 and structural attachment and rotation ring 278 which are similar in structure and function to the canard 20 and the structural attachment and rotation ring 22, respectively. Because of the cylindrical shape of the forward fuselage 275, the canard 276 has a substantially rectangular planform shape with arc-shaped wing tips 277 that conform to the contour of the forward fuselage 275, when the canard 276 is in its retracted position (shown in dashed lines and referenced by the numeral 282). The canard 276 may optionally include leading edge control surfaces 284 and trailing edge control surfaces 286 that are respectively similar in structure and function to the control surfaces 30, 32 of FIG. 2.
With further reference to FIG. 12, the upper portion of the forward fuselage 275 contains a recess 290 within which the canard 276 fits conformally when stowed (shown in dashed lines and referenced by the numeral 282). When the canard 276 is deployed, the bottom surface 293 of the canard 276 is lower than the upper surface 292 of the cylindrical fuselage 275.
With reference to FIGS. 13 and 14, another alternative embodiment of the present invention includes a secondary tail system 302 for use as a retractable horizontal tail. The secondary tail system 302 generally includes a retractable secondary wing or tail 310 which is similar in structure and function to the canard 276 of FIG. 12, and a structural attachment and rotation ring 312 which is similar in structure and function to the ring 22 of FIG. 1.
The retractable horizontal tail 310 may include leading edge control surfaces 320 and trailing edge control surfaces 322 which are respectively similar in structure and function to the leading and trailing control surfaces 30, 32 of FIG. 2. The retractable horizontal tail 310 rotates about a central axis to the fully deployed position (shown in solid lines and referenced by the numeral 310) which is substantially normal to the aft fuselage 324, to the conformally stowed position (shown in dashed lines and referenced by the numeral 316) within the aft fuselage 324, or to an intermediate position (shown in dashed lines and referenced by the numeral 334).
When stowed, the retractable tail fits conformally within a recess 346 in the lower portion of the aft fuselage 324 as shown in FIG. 14. The secondary tail system 302 may be used in place of, or in addition to, a conventional horizontal tail 350 to optimize control, performance and efficiency of the aircraft 10 during all phases of flight.
While the systems of the present invention are described in use in aircraft, it should be noted that the systems described herein may be applied generally to other types of aerodynamic or hydrodynamic vehicles. Furthermore, while specific embodiments of the present conformally stowable low-speed canard are illustrated and described in accordance with the present invention, modifications and changes of the systems, dimensions, composition, use and operation will become apparent to those skilled in the art, without departing from the scope of the invention.
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A secondary wing system for use on an aircraft augments the lift, stability, and control of the aircraft at subsonic speeds. The secondary wing system includes a mechanism that allows the canard to be retracted within the contour of the aircraft fuselage from an operational position to a stowed position. The top surface of the canard is exposed to air flow in the stowed position, and is contoured to integrate aerodynamically and smoothly within the contour of the fuselage when the canard is retracted for high speed flight. The bottom portion of the canard is substantially flat for rotation into a storage recess within the fuselage. The single canard rotates about a vertical axis at its spanwise midpoint. The canard can be positioned between a range of sweep angles during flight and a stowed position in which its span is substantially parallel to the aircraft fuselage. The canard can be deployed and retracted during flight. The deployment mechanism includes a circular mounting ring and drive mechanism that connects the canard with the fuselage and permits it to rotate and to change incidence. The deployment mechanism further includes retractable fairings which serve to streamline the wing when it is retracted into the top of the fuselage.
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CROSS-REFERENCE TO RELATED APPLICATION
This application is based on provisional application Ser. No. 60/053,118, filed Jul. 18, 1997.
BACKGROUND OF THE INVENTION
Particularly in automotive applications, box sections such as main frame rails are subjected to considerable stress forces where cross members are bolted to the rails. For example, when engine cradles are bolted to main frame rails they produce joints that are susceptible to durability cracking over time. In addition, the bolts which hold such components in place may loosen due to vibration at the joint. Moreover, conventional structures create a “noise path” which extends from the vehicle wheels and engine through the frame and into the passenger compartment.
As will be appreciated by those skilled in the art, in order to bolt a heavy component to the side of a rail section it is necessary to create a reinforced region or support structure at the site of attachment of the bolt. One approach which is used in the art is to provide a stamped bulkhead which supports a metal bushing. The bulkhead generally has three flange portions which are spot welded to the rail C-section. More specifically, the stamped bulkhead has a wall portion that extends from one wall of the rail section to the opposite wall or cap. Thus, the bulkhead forms a partition in the channel or cavity defined by the rail. In order to secure this wall portion in place, the bulkhead has three surfaces or flanges that are perpendicular to the bulkhead wall portion; that is, the bulkhead is in essence a shallow rectangular box that is open on one side. These three surfaces mate with the inner surfaces of the rail and are spot welded in place.
In order to utilize the bulkhead as a support for the cross structure which is attached thereto, it is designed to position a metal bushing that is spot welded to the bulkhead stamping. A bolt then passes through the bushing and secures the cross structure to the rail at the bulkhead-reinforced region. This conventional approach will be more fully illustrated hereinafter.
While the conventional bulkhead design does serve to reinforce the rail section at the attachment site of the cross member, it generally requires large gauge bushings and stampings and can actually increase unwanted vibration and noise. Moreover, the through-bolt, bushing, metal stamping and rail section essentially perform as discrete elements more than a unitary, integral reinforcement structure. This results not only in the above-mentioned increase in vibration and noise, but also fails to provide full reinforcement of the rail, resulting in metal fatigue at the joint and, in particular, at weld locations.
The present inventor has developed a number of approaches to the reinforcement of hollow metal parts such as: a reinforcing beam for a vehicle door which comprises an open channel-shaped metal member having a longitudinal cavity which is filled with a thermoset or thermoplastic resin-based material; a hollow torsion bar cut to length and charged with a resin-based material; a precast reinforcement insert for structural members which is formed of a plurality of pellets containing a thermoset resin with a blowing agent, the precast member being expanded and cured in place in the structural member; a composite door beam which has a resin-based core that occupies not more than one-third of the bore of a metal tube; a hollow laminate beam characterized by high stiffness-to-mass ratio and having an outer portion which is separated from an inner tube by a thin layer of structural foam; an I-beam reinforcement member which comprises a preformed structural insert having an external foam which is then inserted into a hollow structural member; and a metal w-shaped bracket which serves as a carrier for an expandable resin which is foamed in place in a hollow section.
None of these prior approaches, however, deal specifically with solving the problems associated with conventional reinforcing bulkheads in rail sections at cross member attachment sites. The present invention solves many of the problems inherent in the prior art.
It is an object of the present invention to provide a reinforced hollow metal structure which incorporates a bushing and a stamping in a bulkhead structure in a manner in which the components of the bulkhead work together as an integral unit with the reinforced structure.
It is a further object of the invention to provide a reinforced metal box section which provides greater strength to the section without significantly increasing vibration and noise transmission levels.
It is a further object of the present invention to provide a reinforced frame rail section at the attachment of a cross member such as an engine cradle in a manner in which stress forces are distributed over a region of the reinforced rail rather than at the discrete welds and in which noise and vibration are dampened.
These and other objects and advantages of the invention will be more fully appreciated in accordance with the detailed description of the preferred embodiments of the invention and the drawings.
SUMMARY OF THE INVENTION
In one aspect the present invention provides a reinforced structure. The reinforced structure includes a hollow structural member and a reinforcing member disposed therein. The reinforcing member has a pair of opposed walls. A layer of thermally expanded polymer is disposed between and is bonded to the opposed walls. This layer of polymer is also bonded directly to the structural member. A sleeve extends through the polymer parallel with and between the opposed walls. The polymer is bonded to the sleeve and the sleeve defines a passage through the polymer. The reinforced structure has holes that are in alignment with the ends of the sleeve. A bolt is then used to secure a component to the structural member. Thus, the hollow structural member is reinforced locally in the present invention at that position by virtue of the reinforcing member. The polymer is expanded in place by heating the entire structure after assembly, where it expands to fill gaps between the reinforcing structure and the structural member and bonds the reinforcing structure to the structural member.
In another aspect the reinforced structure of the present invention is a motor vehicle rail such as a front rail where local reinforcement for the attachment of components such as an engine cradle is required. In this aspect, the invention reduces vibration and noise transmission as well as increases the strength of the part at the site of the reinforcement.
In still another aspect the sleeve is a thin wall metal bushing, the opposed walls are metal stampings with flanges which are welded to the structural member and the polymer is a thermally expanded epoxy resin which contains hollow microspheres for density reduction.
In still another aspect the present invention provides method of reinforcing a structural member having a longitudinal channel. In this aspect a laminated structure having two opposed walls separated by a layer of thermally expandable polymer is placed in the channel of a rail section or the like. The laminated structure has a sleeve disposed in the layer of thermally expandable polymer. The sleeve defines a passage perpendicular to the opposed walls. The laminated structure also has a pair of end flanges. The laminated structure is placed in the longitudinal channel such that said sleeve passage is perpendicular to the longitudinal channel. The laminated structure is then welded to the structural member at the flanges. The entire structure is then heated to a temperature effective to activate the blowing agent of the polymer and thereby thermally expand the polymer such that it bonds the laminated structure to the structural member.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a diagrammatic exploded perspective view of a conventional prior art bulkhead reinforcement structure;
FIG. 2 is a diagrammatic front elevational view of the structure of FIG. 1 with the cap plate removed;
FIG. 3 is a diagrammatic exploded perspective view of the reinforced rail section of the present invention illustrating the construction of the reinforcing laminate bulkhead;
FIG. 4 is a diagrammatic front elevational view of the structure shown in FIG. 3 with the cap plate removed; and
FIG. 5 is a diagrammatic back view of the bulkhead portion of FIGS. 3 and 4 .
DETAILED DESCRIPTION
Referring now to FIGS. 1 and 2 of the drawings, prior art front rail section 20 is shown having C-section 22 that defines channel 23 and which receives cap plate 24 . Bulkhead stamping 26 is seen having vertical wall 28 and flanges 30 . Bushing 32 is welded to wall 28 at an arcuate bend 33 in wall 28 . Flanges 30 are welded to section 22 to hold bulkhead 26 in place. Bolt 36 extends through cap 24 , bushing 32 and vertical wall 37 of section 22 and then through a component 38 which is to attached to rail 20 . Nut 40 is then attached to bolt 36 to secure component 38 in place. This is representative of the prior art and suffers from the drawbacks described above, i.e. inadequate reinforcement, inadequate sound dampening and vibration problems.
Turning now to FIG. 3 of the drawings, reinforced structure 50 is shown in one embodiment as a reinforced front rail of an automotive frame and includes frame rail C-section 52 which is closed by cap plate 54 such that channel or cavity 56 is defined in reinforced structure 50 . In other words the frame rail is hollow. C-section 52 includes vertical wall portion 58 and opposed wall portions 60 and 62 . Each opposed wall portion 60 , 62 has a flange portion 64 of the attachment of cap plate 54 by welding or the like at the flange areas. Reinforcing member or bulkhead 68 is seen disposed in channel 56 of C-section 52 and has a first wall or side 70 and a second wall or side 72 . Walls 70 and 72 are parallel to one another and are separated by polymer layer 74 ; that is, polymer layer 74 is disposed between walls 70 and 72 .
As best seen in FIGS. 4 and 5 of the drawings, each wall 70 , 72 has an associated arcuate portion ( 76 for wall 72 and 78 for wall 70 ) which is designed to accommodate sleeve 81 in a manner to be more fully described hereinafter. Each arcuate portion 76 , 78 is approximately midway along the length of each wall 70 , 72 and can be viewed as a curved inner surface. Sleeve 81 is a metal bushing or the like and, as best seen in FIG. 4 of the drawings is spot welded to walls 70 and 72 at weld points 83 and 85 . Polymer layer 74 essentially envelopes sleeve 81 as shown in FIG. 4 .
Bulkhead 68 is secured in place in channel 56 by virtue of attachment flanges 80 and 82 which extend from walls 70 and 72 at 90 degree angles. That is, each wall 70 , 72 has at each end a bent portion that mates with a similar portion on the opposed wall to form an attachment flange 80 , 82 that is welded on side wall 60 , 62 , respectively.
The width of walls 70 and 72 (distance between vertical wall 58 and cap plate 54 ) is such that bulkhead 68 is in contact with vertical wall 58 and cap plate 54 . Accordingly, bolt 84 extends through cap plate 54 at hole 66 , through sleeve 81 and through a corresponding hole in vertical wall 58 (not shown). Bolt 84 then extends through a hole in a cross member such as engine cradle 86 which is shown in phantom as fragment 86 . Nut 88 is then secured on bolt 84 to secure engine cradle 86 onto reinforced structure 50 .
Bulkhead 68 is a relatively light weight structure for the amount of strength added to the frame rail. Walls 70 and 72 can be formed of thin steel stampings, for example from 0.02 to about 0.08 inch in thickness. Mild to medium strength steel is particularly preferred. Also, sleeve 81 which is preferably a metal bushing may b a thin wall tube having a wall thickness of from about 0.08 to about 0.2 inch and is preferably mild steel. Of course, these dimensions are merely illustrative and are not intended to limit the full scope of the invention as defined in the claims. Each attachment flange 80 , 82 is generally from about 15 percent to about 30 percent of the length of walls 70 , 72 . The outer diameter of sleeve 81 will typically be from about ½ to about 1 inch. The width of polymer layer 74 will be a function of the distance between walls or plates 70 and 72 and will generally be between about 0.1 and about 0.4 inch. It is to be understood that the entire depth of bulkhead 68 is filled with polymer layer 74 ; that is, as shown in FIG. 5 of the drawings polymer layer 74 extends from the front of bulkhead 68 to the back.
The polymer used to form polymer layer 74 is a resin based material which is thermally expandable. A number of resin-based compositions can be utilized to form thermally expanded layer 74 in the present invention. The preferred compositions impart excellent strength and stiffness characteristics while adding only marginally to the weight. With specific reference now to the composition of layer 74 , the density of the material should preferably be from about 20 pounds per cubic feet to about 50 pounds per cubic feet to minimize weight. The melting point, heat distortion temperature and the temperature at which chemical breakdown occurs must also be sufficiently high such that layer 74 maintains its structure at high temperatures typically encountered in paint ovens and the like. Therefore, layer 74 should be able to withstand temperatures in excess of 320 degrees F. and preferably 350 degrees F. for short times. Also, layer 74 should be able to withstand heats of about 90 degrees F. to 200 degrees F. for extended periods without exhibiting substantial heat-induced distortion or degradation.
The foam 74 may be initially applied to one or both walls 70 , 72 and then expand into intimate contact with both walls and with sleeve 81 . Advantageously heat from the paint oven may be used to expand foam 74 when it is heat expandable.
In more detail, in one particularly preferred embodiment thermally expanded structural foam for layer 74 includes a synthetic resin, a cell-forming agent, and a filler. A synthetic resin comprises from about 40 percent to about 80 percent by weight, preferably from about 45 percent to about 75 percent by weight, and most preferably from about 50 percent to about 70 percent by weight of layer 74 . Most preferably, a portion of the resin includes a flexible epoxy. As used herein, the term “cell-forming agent” refers generally to agents which produce bubbles, pores, or cavities in layer 74 . That is, layer 74 has a cellular structure, having numerous cells disposed throughout its mass. This cellular structure provides a low-density, high-strength material, which provides a strong, yet lightweight structure. Cell-forming agents which are compatible with the present invention include reinforcing “hollow” microspheres or microbubbles which may be formed of either glass or plastic. Also, the cell-forming agent may comprise a blowing agent which may be either a chemical blowing agent or a physical blowing agent. Glass microspheres are particularly preferred. Where the cell-forming agent comprises microspheres or macrospheres, it constitutes from about 10 percent to about 50 percent by weight, preferably from about 15 percent to about 45 percent by weight, and most preferably from 20 percent to about 40 percent by weight of the material which forms layer 74 . Where the cell-forming agent comprises a blowing agent, it constitutes from about 0.5 percent to about 5.0 percent by weight, preferably from about 1 percent to about 4.0 percent by weight, and most preferably from about 1 percent to about 2 percent by weight of thermally expanded structural foam layer 74 . Suitable fillers include glass or plastic microspheres, fumed silica, calcium carbonate, milled glass fiber, and chopped glass strand. A thixotropic filler is particularly preferred. Other materials may be suitable. A filler comprises from about 1 percent to about 15 percent by weight, preferably from about 2 percent to about 10 percent by weight and most preferably from about 3 percent to about 8 percent by weight of layer 74 .
Preferred synthetic resins for use in the present invention include thermosets such as epoxy resins, vinyl ester resins, thermoset polyester resins, and urethane resins. It is not intended that the scope of the present invention be limited by molecular weight of the resin and suitable weights will be understood by those skilled in the art based on the present disclosure. Where the resin component of the liquid filler material is a thermoset resin, various accelerators, such as imidazoles and curing agent, preferably dicyandiamide may also be included to enhance the cure rate. A functional amount of accelerator is typically from about 0.5 percent to about 2.0 percent of the resin weight with corresponding reduction in one of the three components, resin, cell-forming agent or filler. Similarly, the amount of curing agent used is typically from about 1 percent to about 8 percent of the resin weight with a corresponding reduction in one of the three components, resin, cell-forming agent or filler. Effective amounts of processing aids, stabilizers, colorants, UV absorbers and the like may also be included in layer. Thermoplastics may also be suitable.
In the following table, a preferred formulation for layer 74 is set forth. It has been found that this formulation provides a material which full expands and cures at about 320 degrees F. and provides excellent structural properties. All percentages in the present disclosure are percent by weight unless otherwise specifically designated.
PERCENTAGE
INGREDIENT
BY WEIGHT
EPON 828 (epoxy resin)
37.0
DER 331 (flexible epoxy resin)
18.0
DI—CY (dicyandiamide curing agent)
4.0
Imidazole (accelerator)
0.8
FUMED SILICA (thixotropic filler)
1.1
Celogen AZ199 (asodicarbonamide blowing agent)
1.2
83 MICROS (glass microspheres)
37.0
WINNOFIL CALCIUM CARBONATE (CaCO 3 filler)
0.9
While the invention has been described primarily in connection with vehicle parts, it is to be understood that the invention may be practiced as part of other products, such as aircrafts, ships, bicycles or virtually anything that requires energy for movement. Similarly, the invention may be used with stationary or static structures, such as buildings, to provide a rigid support when subjected to vibration such as from an earthquake or simply to provide a lightweight support for structures subjected to loads. Additionally, while the invention has been described primarily with respect to heat expandable foams and with respect to metal parts such as the inner tubes 16 , 58 and 76 , other materials can be used. For example, the foam could be any suitable known expandable foam which is chemically activated into expansion and forms a rigid structural foam. The bulkhead walls 70 , 70 and sleeve 81 could be made of materials other than metal such as various plastics or polymeric materials or various wood type fibrous materials having sufficient rigidity to function as a back drop or support for the foam. Where a heat expandable foam is used the bulkhead walls and sleeve should be able to withstand the heat encountered during the heat curing. Where other types of foam materials are used, however, it is not necessary that the bulkhead walls and sleeve be able to withstand high temperatures. Instead, the basic requirement for the bulkhead walls and sleeve is that it have sufficient rigidity to function in its intended manner. It is also possible, for example, to use as the bulkhead walls and sleeve materials which in themselves become rigid upon curing or further treatment. The invention may also be practiced where the bulkhead walls and sleeve are made of materials other than metal. It is preferred, however, that materials be selected so that the thin unexpanded foam upon expansion forms a strong bond with the bulkhead walls and sleeve so that a structural composition will result.
While particular embodiments of this invention are shown and described herein, it will be understood, of course, that the invention is not to be limited thereto since many modifications may be made, particularly by those skilled in this art, in light of this disclosure. It is contemplated, therefore, by the appended claims, to cover any such modifications as fall within the true spirit and scope of this invention.
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A hollow reinforced structural member has a bulkhead having a layer of thermally expanded resin disposed between opposed side walls. A sleeve is retained within the resin layer and is oriented perpendicular to the longitudinal axis of the reinforce structural member. The sleeve is an alignment with bolt holes in opposite sides of the reinforced structure such that a bolt can be inserted there through. A component can then be bolted to the reinforced structural member at the site of the reinforcement. The invention not only increases the strength of the part, but also reduces vibration and noise transmission.
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FIELD
[0001] Embodiments of the invention relate to the field of microprocessor architecture. More particularly, embodiments of the invention relate to a technique to scale frequency and operating voltage of various functional units within a microprocessor.
BACKGROUND
[0002] In order to help reduce power in microprocessors while minimizing the impact to performance, prior art techniques for reducing processor clock frequency have been developed. Among these prior art techniques are architectures that divide the processor into various clock domains. For example, one prior art technique has a separate clock domain for the integer pipeline, a separate clock domain for the floating point pipeline, and a separate clock domain for memory access logic.
[0003] Using separate clock domains for each pipeline and/or memory access cluster can pose challenges to maintaining the performance of the processor due to the amount of overhead circuitry needed to control each clock domain.
BRIEF DESCRIPTION OF THE DRAWINGS
[0004] Embodiments and the invention are illustrated by way of example and not limitation in the figures of the accompanying drawings, in which like references indicate similar elements and in which:
[0005] FIG. 1 illustrates a clock and voltage scaling architecture according to one embodiment of the invention.
[0006] FIG. 2 illustrates a front-side bus computer system in which one embodiment of the invention may be used.
[0007] FIG. 3 illustrates a point-to-point computer system in which one embodiment of the invention may be used.
DETAILED DESCRIPTION
[0008] Embodiments of the invention relate to a frequency and voltage control architecture for a microprocessor. More particularly, embodiments of the invention relate to techniques to distribute and control a clock and operating voltage among a number of clocking domains within the microprocessor, such that the frequency and operating voltage of each domain can be controlled independently.
[0009] FIG. 1 illustrates a clock and voltage domain architecture according to one embodiment of the invention. In particular, FIG. 1 illustrates a processor architecture 100 that has been divided into three fundamental clocking domains: A front end domain 101 , having a trace cache 102 , branch predictor 103 , renaming unit 104 , decoding unit 105 , sequencer 106 , free list 107 , renaming table 108 , and a re-order buffer (ROB) 109 ; several back end domains 110 , having a memory ordering buffer (MOB) 111 , a first-level cache 112 , physical register files 113 , issue queues 114 , bus interface 116 and execution units 115 ; and a memory domain including a second level cache memory 119 . In one embodiment, the bus interface is a front-side bus interface, while in other embodiments it is a point-to-point bus interface.
[0010] The front-end domain, back-end domains, and the memory domain each have at least one first-in-first-out (FIFO) queue 117 used to help synchronize the exchange of information between the various clock domains. In one embodiment of the invention, at least some of the synchronization queues are queues that provide other functionality within the processor, whereas in other embodiments, the synchronization queues are dedicated to the clock domain control architecture. In addition to clock domains, one embodiment of the invention divides the processor into voltage domains, which can be regulated independently of each other. In at least one embodiment, the clock domains and the voltage domains are the same and include the same functional units, however, in other embodiments the clock domains and voltage domains are not the same and may include different functional units.
[0011] In one embodiment of the invention, each clock within the various clock domains may be synchronized to a reference clock. However, in other embodiments, each domain clock may not be synchronous in relation to other domain clocks. Furthermore, in at least one embodiment, the back-end domains may communicate between each other via signals known as “crossbars”.
[0012] In order to control each of the clock and voltage domains, one embodiment of the invention attempts to minimize a product of the energy and the square of the (“delay 2 ”) of each domain by determining the energy and performance of each domain at certain time intervals. Energy and performance may be determined at two time intervals, in at least one embodiment, by calculating the energy and delay of a domain during a first time interval and estimating the energy and delay of the domain in a subsequent time interval. A frequency and voltage pair for the subsequent time interval may then be chosen by minimizing the ratio between the energy-delay 2 product of the first time interval and that of the subsequent time interval.
[0013] For example, in one embodiment of the invention, the processor energy, “E”, for interval n+1 is estimated according to the following equation:
E n + 1 E n = 1 + E FE , n E n × ( V n + 1 2 V n 2 - 1 )
[0014] In the above equation, “E FE,n ” is the energy of the front-end domain at time interval “n”, where as “E n+1 ” is the energy of the front-end at time interval n+1 and “V n+1 ” is the operating voltage of the front-end domain at time interval n+1, and “V n ” is the operating voltage of the front-end domain at time interval n.
[0015] Performance of the processor as a function of the frequency of the front-end domain can be estimated by using the clock frequency of the front-end domain for a given time interval, the rate at which instructions are fetched by the front-end, and the rate at which micro-operations (decoded instructions) are delivered to subsequent pipeline stages. In one embodiment, the performance estimation, “T n+1 ”, of an interval, n+1, is estimated according to the equation:
T n + 1 T n = 1 + ( f n f n + 1 - 1 ) × 1 - p n 1 + b
[0016] In the above equation, “p n ” is the average number of entries in the front-end queue for the n-th interval, and “b” is the branch misprediction rate. The value, “1+b”, is an indicator of the rate at which the fetch queue may be loaded and “1−pn” is an indicator of average number of entries in the queue. “T n ” is the performance of front-end at interval “n”, “fn” is the frequency of the front-end domain at interval n, and “f n+1 ” is the frequency of the front-end domain at the following time interval.
[0017] Once the energy and performance of the processor has been calculated according to the above equations, in one embodiment, the front-end domain frequency and voltage can be adjusted for the next time interval, n+1, at the end of each time interval, n. In one embodiment, the selection of frequency and voltage is made according to the ratio:
R ( 〈 f , V 〉 ) = E n + 1 E n × T n + 1 T n × T n + 1 T n
[0018] The frequency and voltage selected for the interval n+1 are those that minimize the above ratio. If two or more pairs are-found that result in the same value, R, then the pair with the minimum frequency is chosen, in one embodiment. The frequency and operating voltage of the front-end domain may then be set to the appropriate values for the interval n+1 and the process repeated for the next interval.
[0019] Each back-end frequency and operating voltage may be estimated in a similar manner to the front-end, by estimating the energy and performance of the processor as a function of the operating voltage and frequency of each back-end domain and choosing a frequency and operating voltage that minimizes the ratio between the energy performance product between interval n+1 and interval n. In one embodiment, the processor energy, “E n ”, as a function of the back-end domain energy, “E BE,n ” is estimated according to the equation:
E n + 1 E n = 1 + E BE , n E n × ( V n + 1 2 V n 2 - 1 )
[0020] Performance of the processor as a function of the frequency of each back-end domain can be calculated at each interval, n+1, according to the equation:
T n + 1 T n = 1 + S × ( 1 - 2 m n ) 2 × p ,
where p = - L q , n + L q , n 2 + 4 L q , n 2
and S = ( f n f n + 1 - 1 ) × f n + 1 - f n f max - f min
[0021] In the above equation, m n is the number of second level cache misses divided by the number of committed micro-operations for the interval, n, and L q,n is the average utilization of all micro-operation issue queues for all back-end domains containing execution units. Once the energy and performance of the processor has been calculated according to the above equations, in one embodiment, the back-end domain frequency and voltage can be adjusted for the next time interval, n+1, at the and of each time interval, n. In one embodiment, the selection of frequency and voltage is made according to the ratio:
R ( f n + 1 , V n + 1 ) = E n + 1 E n × T n + 1 T n × T n + 1 T n
[0022] The frequency and voltage selected for the interval n+1 are those that minimize the above ratio. If two or more pairs are found that result in the same value, R, then the pair with the minimum frequency is chosen, in one embodiment. The frequency and operating voltage of the back-end domain may then be set to the appropriate values for the interval n+1 and the process repeated for the next interval.
[0023] FIG. 2 illustrates a front-side-bus (FSB) computer system in which one embodiment of the invention may be used. A processor 205 accesses data from a level one (L 1 ) cache memory 210 and main memory 215 . In other embodiments of the invention, the cache memory may be a level two (L 2 ) cache or other memory within a computer system memory hierarchy. Furthermore, in some embodiments, the computer system of FIG. 2 may contain both a L 1 cache and an L 2 cache, which comprise an inclusive cache hierarchy in which coherency data is shared between the L 1 and L 2 caches.
[0024] Illustrated within the processor of FIG. 2 is one embodiment of the invention 206 . Other embodiments of the invention, however, may be implemented within other devices within the system, such as a separate bus agent, or distributed throughout the system in hardware, software, or some combination thereof.
[0025] The main memory may be implemented in various memory sources, such as dynamic random-access memory (DRAM), a hard disk drive (HDD) 220 , or a memory source located remotely from the computer system via network interface 230 containing various storage devices and technologies. The cache memory may be located either within the processor or in close proximity to the processor, such as on the processor's local bus 207 . Furthermore, the cache memory may contain relatively fast memory cells, such as a six-transistor (6T) cell, or other memory cell of approximately equal or faster access speed.
[0026] The computer system of FIG. 2 may be a point-to-point (PtP) network of bus agents, such as microprocessors, that communicate via bus signals dedicated to each agent on the PtP network. Within, or at least associated with, each bus agent is at least one embodiment of invention 206 , such that store operations can be facilitated in an expeditious manner between the bus agents.
[0027] FIG. 3 illustrates a computer system that is arranged in a point-to-point (PtP) configuration. In particular, FIG. 3 shows a system where processors, memory, and input/output devices are interconnected by a number of point-to-point interfaces.
[0028] The system of FIG. 3 may also include several processors, of which only two, processors 370 , 380 are shown for clarity. Processors 370 , 380 may each include a local memory controller hub (MCH) 372 , 382 to connect with memory 22 , 24 . Processors 370 , 380 may exchange data via a point-to-point (PtP) interface 350 using PtP interface circuits 378 , 388 . Processors 370 , 380 may each exchange data with a chipset 390 via individual PtP interfaces 352 , 354 using point to point interface circuits 376 , 394 , 386 , 398 . Chipset 390 may also exchange data with a high-performance graphics circuit 338 via a high-performance graphics interface 339 .
[0029] At least one embodiment of the invention may be located within the PtP interface circuits within each of the PtP bus agents of FIG. 3 . Other embodiments of the invention, however, may exist in other circuits, logic units, or devices within the system of FIG. 3 . Furthermore, other embodiments of the invention may be distributed throughout several circuits, logic units, or devices illustrated in FIG. 3 .
[0030] While the invention has been described with reference to illustrative embodiments, this description is not intended to be construed in a limiting sense. Various modifications of the illustrative embodiments, as well as other embodiments, which are apparent to persons skilled in the art to which the invention pertains are deemed to lie within the spirit and scope of the invention.
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A method and apparatus for scaling frequency and operating voltage of at least one clock domain of a microprocessor. More particularly, embodiments of the invention relate to techniques to divide a microprocessor into clock domains and control the frequency and operating voltage of each clock domain independently of the others.
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FIELD OF THE INVENTION
This invention relates generally to railroad track switching, and particularly concerns a railroad switch stand and component parts for a railroad switch stand which function to obtain a significantly reduced hand-crank range of operating motion.
BACKGROUND OF THE INVENTION
Many manually-operated railroad switch stands offered and utilized in the United States by the rail transportation industry are provided with a hand-crank assembly that is operated throughout a rotational range of approximately 180 degrees. The assembly has an input shaft that requires only about 120 degrees of rotation to achieve a change in switch operating positions, and a so-called "lost motion" torque-transmitting connection between the hub of the crank arm element and the switch stand input shaft element. Such switch stand units also are normally provided with foot latches or similar devices for locating and retaining the switch stand crank assembly element securely in its alternative and approximately 180 degree-separated extreme operating positions.
It is well-known that railroad operating personnel responsible for manual switch stand operation may frequently experience costly serious back injury, generally in the nature of spinal injury and/or excessive muscular stress, in the course of actuating switch stands having the known crank assembly with a lost motion connection configuration. Some improvement in switch stand operator ergonomics has been achieved by a reconfiguration of the handle element normally attached to the crank lever for use by the switch operator. However, it has been discovered that a still further reduction in operator injury may be realized by additionally applying ergonomic principles to a redesign of the manually-operated stand in a manner that essentially eliminates the need for moving the hand-crank arm element through the range of motion that is excess to the switch input shaft rotation requirement.
SUMMARY OF THE INVENTION
The present railroad switch stand invention utilizes an improved manual-force input crank assembly which is joined to the input shaft of a railroad switch stand that normally actuates conventional railroad track switch points through a cooperating connecting-rod interconnection. The improved switch stand crank assembly has a manually-operated crank arm, a novel latch yoke that is securely attached to the crank operating arm, and an adapter hub element or equivalent that couples the crank operating arm and attached latch yoke to the switch stand input shaft in a manner whereby all motion and torquing forces applied to the crank operating arm are transmitted to and cause motion of the switch stand input shaft. The latch yoke is provided with transversely-oriented arms and integral latch bar elements that are positioned to cooperate with diametrically-opposed conventional foot latches provided in the switch stand assembly and that function to limit manually-caused motion of the crank operating arm to a rotational range that corresponds to the range of rotational motion required by the switch stand input shaft, usually about 120 degrees of rotation. The crank operating arm is additionally fitted with an operator handle element, and preferably with a handle having substantial lateral offsets relative to the longitudinal axis of the crank operating arm.
Additional particulars regarding the invention are provided in the drawings and detailed description. Also, additional advantages associated with utilization of the present invention will become apparent during a careful consideration of the further specification materials.
DESCRIPTION OF THE DRAWINGS
FIG. 1 is a partially-sectioned elevational view of a railroad switch stand installation having a prior art input shaft and operating crank construction;
FIG. 2 is a plan view of a railroad switch stand installation incorporating the present invention;
FIG. 3 is an elevational view of the railroad switch stand installation of FIG. 2;
FIG. 4 is a sectional view of the invention adapter hub taken along the line 4--4 of FIG. 2; and
FIG. 5 is a partial sectioned elevational view of a conventional foot latch assembly provided in the installations of FIGS. 1 through 3 and taken along the line 5--5 of FIG. 2.
DETAILED DESCRIPTION
FIG. 1 illustrates a known type of railroad switch stand (10) mounted on railroad track ties (12 an 14). The switch stand (10) is provided with an input shaft (16), with a manually-operated crank arm/handle (18) , and with diametrically-opposed foot latch assemblies (20 and 22) mounted on ties (12 and 14) respectively. Manual rotation of the arm/handle (18) in a range (R, FIG. 1) of approximately 180 degrees, and from engagement with one latch assembly (20 and 22) to engagement with the other latch assembly (22 and 20), causes, through the functioning of a lost-motion hub (24) attached to the arm/handle (18), rotation of the input shaft (16) of approximately 120 degrees and consequent rotation of a switching crank and switch point connecting rod elements (26) to a new switching position. Thus, as shown in FIG. 1, there is normally provided about 30 degrees of arm/handle free-play at each end of the rotational operating range of the input shaft (16).
An improved railroad switch stand installation (30) that makes use of the present invention and that substantially reduces the angular movement of crank arm/handle (18) required to drive the switch stand (10) from one operating position to the other operating position is shown in plan in FIG. 2. The installation tie elements (32 and 34) and the installation of diametrically-opposed conventional foot latch devices (52 and 54) remain the same as in the FIG. 1 switch stand installation. However, an improved manually-operated crank assembly (36) is incorporated into the installation (30).
The improved manual crank assembly (36) is comprised of a crank arm (38), a handle (40) attached to the crank arm, a novel latch yoke assembly (42) attached to the crank arm (38), and an adapter hub (44) that functions in part to couple the arm/handle and latch yoke combination to a switch stand input shaft (46). Adapter hub (44) rigidly couples arm/handle and latch yoke combination to input shaft (46) such that all motion imparted to the improved crank assembly in any direction and at any time is likewise imparted to the switch stand input shaft (46) thus eliminating any free play or "lost motion" in installation manual operation. A conventional threaded fastener is utilized to secure the assembly (36) to a reduced-diameter threaded end of the switch stand switching input shaft (46).
The yoke assembly (42) is provided with integral latch bar elements (48 and 50) that are positioned distantly and laterally to either side of the longitudinal axis of the operating arm (38), and that function to engage the conventional foot latches (52 and 54) when the manually-operated crank is positioned in either of its extreme operating positions. Each of the latch bar elements (48 and 50) is positioned so as to form an angle of approximately 30 degrees between the longitudinal axis of the crank arm (38) and a line extending from the adapter hub (44) to one of said latch bar elements (48 and 50). The yoke assembly (42) is secured to the crank arm (38) by a conventional threaded fastener (56) and the operating arm (38) has an end opening (not shown) through which the switch stand input shaft (46) passes.
From an operator injury-reduction standpoint it is important to note in FIG. 3, which depicts crank assembly (36) in one of its operating position extremes, that: (1) the crank arm element (38) is significantly elevated in comparison to the position of the FIG. 1 crank arm (18), and (2) the crank handle (40) has an upper, hand-grasped offset that is displaced laterally upwardly relative to the longitudinal axis of the crank arm (38). Each feature contributes to operator injury reduction because of the significantly reduced degree of operator back bending required to accomplish crank assembly rotation. In one actual embodiment of the railroad switch stand (30), the upper extreme of the handle (40) is positioned at a height (H, FIG. 3) approximately 30 inches above the top surface of the track ties (32 and 34) when the switch stand (30) is in either of its extreme operating position. Also, it should be noted that the manual operating range (R, FIG. 3) of the crank assembly (36) is substantially less than the crank assembly manual operating range illustrated in the FIG. 1 prior art railroad switch stand.
FIG. 4 is a sectional view of the adapter element (44) which functions to rigidly couple the crank assembly (36) to the switch stand input shaft (46). At the section 4--4 line of FIG. 2, the switch stand input shaft (46) preferably has a noncircular cross-section such as the rectangular cross-section that is illustrated in FIG. 4. Although the drawings illustrate a crank assembly construction in which the adapter element (44) is a separate component part, it is recognized that the functional features of that element may be equivalently made integral with the crank arm (38) thus eliminating the need for a separate adapter component part.
FIG. 5 schematically illustrates a conventional foot latch assembly (54) in elevation, and shows the engagement of yoke assembly extension (50) with that device when the improved crank assembly (36) is secured in its FIG. 3 extreme operating position.
Normally the principal components of the improved switch stand and its crank assembly elements are made of various forged steels. However, other materials, component shapes, and component preferred sizes may be utilized in the practice of this invention.
Since certain changes may be made in the above-described system and apparatus not departing from the scope of the invention herein and above, it is intended that all matter contained in the description or shown in the accompanying drawings shall be interpreted as illustrative and not in a limiting sense.
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A railroad switch stand for switching railroad track switch points is provided with a manually-operated crank assembly that is coupled to the switch stand switching input shaft without included lost motion and that has an included yoke with latch bars that function to stop and secure the crank assembly in operating positions that reduce operator risk to excessive back stress and lower spine injury.
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CROSS REFERENCE TO RELATED APPLICATIONS
The present application is a 35 U.S.C. §371 National Phase conversion of PCT/EP2013/056923, filed Apr. 2, 2013, which claims benefit of French Application No. 12 52941, filed Mar. 30, 2012, the disclosure of which is incorporated herein by reference. The PCT International Application was published in the French language.
TECHNICAL FIELD OF THE INVENTION
The present invention relates to a material comprising of a continuous aqueous phase and a dispersed phase, dispersed in the form of droplets bonded to each other in a covalent manner, and the uses thereof as a membrane, diaphragm, valve, coating, chemical detector or sensor or for the delivery of agents of interest.
BACKGROUND OF THE INVENTION
The literature describes materials that are water based and whose physical form and properties may be modulated, thereby making possible various applications in fields that are widely varied. For example, mention may be made of hydrogels, which are three dimensional networks based on polymers having a number of applications in the food, agricultural and medical fields (contact lenses, delivery of therapeutic agent, breast implant, dressing, coating for prostheses) (Hamidi et al; Advanced Drug Delivery Reviews, 60, 2008, 1638).
The present invention provides a water based material that is an alternative to hydrogels and having the same advantageous properties, since it is possible to modulate and maintain a physical form and to adapt the physical and chemical properties of the material based on the desired application.
Furthermore, the patent application WO 2011/101602 describes an oil in water nano emulsion in form of a gel for the delivery of hydrophilic and lipophilic agents of interest. The three dimensional network of this gel is formed by the droplets bonded to each other by non covalent interactions. However, this gel is relatively fluid, and after being formed, it fails to sufficiently maintain its form. In addition, this gel when placed in the presence of an aqueous phase (and in particular physiological liquid during in vivo administration thereof) disaggregates rapidly and the three dimensional network of the gel is destroyed. Furthermore, these nano emulsions require high proportions of dispersed phase. These three disadvantages constitute an obstacle for many applications of a gel.
SUMMARY OF THE INVENTION
The present invention provides a material in the form of an oil in water emulsion which does not have these above noted disadvantages. The material is able to take form, remain therein and resist dilution in water. It can thus be used in very diverse applications, and in particular in applications that require the presence of an aqueous phase.
[Material]
According to a first object, the invention relates to a material comprising of a continuous aqueous phase and a dispersed phase, dispersed in the form of droplets containing an amphiphilic lipid and a surfactant having the following formula (I):
(L 1 -H 1 —X 1 —H 1 —Y 1 ) v -G-(Y 2 —H 2 —X 2 -L 2 ) w (I),
wherein:
L 1 and L 2 independently represent lipophilic groups,
X 1 , X 2 , Y 1 , Y 2 and G independently represent a linking group,
H 1 and H 2 independently represent hydrophilic groups including a polyalkoxylated chain,
v and w are independently an integer from 1 to 8,
the droplets of the dispersed phase being bonded to each other in a covalent manner by the surfactant having the formula (I).
The material is present in the form of an oil in water emulsion in which the droplets of the dispersed phase are bound to each other by covalent bonding. The emulsion may be single or multiple, in particular by including in the dispersed phase a second aqueous phase.
DEFINITIONS
Within the scope and context of the present patent application, the term “dispersed phase” is used to refer to oil droplets comprising the optional oil/the optional solubilising lipid/the amphiphilic lipid/the optional co-surfactant/the optional lipophilic agent of interest/surfactant having the formula (I). The dispersed phase is generally free of aqueous phase. The material is typically free of liposomes.
The term “droplet” encompasses both the actual liquid oil droplets as well as the solid particles derived from emulsions of the oil-in-water type in which the oily phase is solid.
The droplets of the material are advantageously monodisperse. The standard deviation between the minimum and maximum diameters of the droplets relative to the mean diameter is generally less than or equal to 30%, preferably 20%. The material is generally presented in the form of an oil in water nano emulsion: the mean diameter of the droplets of the dispersed phase is preferably from 20 nm to 200 nm, notably from 40 nm to 150 nm and in particular from 50 nm to 120 nm. These diameters are measured by means of light scattering. It is also possible to obtain the size of droplets by means of transmission electron microscopy (TEM), cryogenic transmission electron microscopy (cryo TEM) or even by atomic force microscopy (AFM). Diameters measuring less than 20 nm and more than 200 nm are difficult to obtain in practice.
The term “lipid” is used within the context of the discussion in this description to refer to all fatty substances or substances containing fatty acids present in the fats of animal origin and in plant oils. They are hydrophobic or amphiphilic molecules mainly formed of carbon, hydrogen and oxygen and having a density lower than that of water. The lipids may be in the solid state at ambient temperature (25° C.), as in waxes, or in the liquid state, as in oils.
The term “amphiphilic” is used to refer to a molecule possessing a hydrophobic part and a hydrophilic part, for example a hydrophobic apolar part and a hydrophilic polar part.
The term “phospholipid” is used to refer to lipids possessing a phosphate group, in particular phosphoglycerides. Most often, phospholipids include a hydrophilic end formed by the phosphate group possibly substituted and two hydrophobic ends formed by the fatty acid chains. Among the phospholipids, mention should be made in particular of phosphatidyl choline, phosphatidyl ethanolamine, phosphatidyl inositol, phosphatidyl serine and sphingomyelin.
The term “lecithin” is used to refer to phosphatidyl choline, that is to say a lipid formed from a choline, a phosphate, a glycerol and two fatty acids. It covers in a broader sense the phospholipids derived from living systems of plant or animal origin, as long as they primarily consist of phosphatidyl choline. These lecithins generally consist of mixtures of lecithins carrying different fatty acids.
The term “surfactant” is used to refer to compounds having an amphiphilic structure which gives them a special affinity for oil/water type and water/oil type interfaces which gives them the ability to reduce the free energy of these interfaces and thus to stabilise the dispersed systems.
The term “co-surfactant” is used to refer to a surfactant acting in addition to another surfactant in order to further reduce the energy of the interface.
The term “lipophilic” agent of interest, is used to refer to an agent of interest that is predominantly, preferably completely, in the dispersed phase, or inside of or on the surface of the droplets. A lipophilic agent of interest has affinities for oily compounds (fats, oils, waxes, etc) and apolar solvents (toluene, hexane, etc). The forces that enable the solubilisation of the lipophilic agent of interest are predominantly London forces (Van der Waals interactions). A lipophilic agent of interest has a high oil/water partition coefficient.
The term “hydrophilic” agent of interest, is used to refer to an agent of interest that is predominantly, preferably completely, in the continuous aqueous phase. Its solubility in water is generally greater than 1% by weight. The solubilisation in water of the hydrophilic agents of interest generally comes from the hydrogen and/or ionic bonds between the hydrophilic agents of interest and water.
The term “fatty acid” is used to refer to aliphatic carboxylic acids having a carbon chain of at least 4 carbon atoms. Natural fatty acids have a carbon chain of 4 to 28 carbon atoms (generally an even number). Long chain fatty acids refer to those with chains that are 14 to 22 carbon atoms long and very long chain fatty acids refer to those having more than 22 carbon atoms.
The term “hydrocarbon chain” is used to refer to a chain composed of atoms of carbon and hydrogen, whether saturated or unsaturated (double or triple bond). Preferred hydrocarbon chains are alkyl or alkenyl.
The term “alkylene” is used to refer to a divalent aliphatic saturated hydrocarbon group, that is linear or branched, preferably linear.
The term “activated ester” is used to refer to a group having the formula —CO-LG, and the term “activated carbonate” is used to refer to a group having the formula —O—CO-LG, where LG represents a good leaving group in particular selected from among a bromine, a chlorine, an imidazolyl, a pentafluorophenolate, a pentachlorophenolate, a 2,4,5-trichlorophenolate, 2,4,6-trichlorophenolate, an —O-succinimidyl group, an —O-benzotriazolyl, —O-(7-aza-benzotriazolyl) and an —O-(4-nitrophenyl) group.
Surfactant Having the Formula (I)
The material according to the invention includes a surfactant having the formula (I) which is located partially in the continuous aqueous phase and partially in the dispersed phase. Indeed, the surfactant having the formula (I) of the material according to the invention comprises two lipophilic groups (L 1 and L 2 ) and two hydrophilic groups (H 1 and H 2 ). The hydrophilic groups are located predominantly at the surface of the droplets, in the continuous aqueous phase while the lipophilic groups are located in the droplets of the material.
More precisely, the lipophilic group L 1 is located in certain droplets, and the group L 2 is in the adjacent droplets. The droplets of the material according to the invention are bound to each other in a covalent manner by the —(X 1 —H 1 —Y 1 ) v -G-(Y 2 —H 2 —X 2 ) w — group of the surfactant having the formula (I). FIGS. 1 and 2 illustrate the positioning of the surfactant having the formula (I), respectively when v and w represent 1 and when v and w represent 2.
The X 1 and X 2 groups are linking groups linking the lipophilic and hydrophobic groups. The G group is a linking group between at least two [lipophilic-hydrophilic] parts of the surfactant having the formula (I). The Y 1 and Y 2 groups are linking groups linking the G group to the [lipophilic-hydrophilic] parts.
The material according to the invention can advantageously be set in form (for example, by placing it in a mould or a container having a given shape or form), and can remain in the form desired according to the desired application.
Furthermore the material is resistant to dilution in an aqueous phase. More specifically, when an aqueous phase is added to the material according to the invention, it remains in form and is not diluted. In the medium, one observes on the one hand the material comprising the droplets, and on the other hand, an aqueous phase substantially free of droplets.
Without intending to be bound to any particular theory, it appears that the properties of the material according to the invention can be explained by the presence of covalent bonds between the droplets, which serves to confer a very strong cohesion therebetween.
In one embodiment, in the Formula (I) mentioned above:
L 1 and L 2 are independently selected from among:
a R or R—(C═O)— group, where R represents a linear hydrocarbon chain containing from 11 to 23 carbon atoms, an ester or an amide of fatty acids containing from 12 to 24 carbon atoms and of phosphatidyl ethanolamine, such as distearyl phosphatidyl ethanolamine (DSPE), and a poly(propylene oxide), and/or
X 1 , X 2 , Y 1 and Y 2 are independently selected from among:
a single bond, a Z group selected from among —O—, —NH—, —O(OC)—, —(CO)O—, —(CO)NH—, —NH(CO)—, —O—(CO)—O—, —NH—(CO)—O—, —O—(CO)—NH— et —NH—(CO)—NH, a Alk group being an alkylene containing from 1 to 6 carbon atoms, and a Z-Alk, Alk-Z, Alk-Z-Alk or Z-Alk-Z group, where Alk and Z are as defined here above and where the two Z groups of the Z-Alk-Z group are identical or different, and/or
H 1 and H 2 are independently selected from a poly(ethylene oxide) typically comprising from 3 to 500 ethylene oxide units, preferably from 20 to 200 ethylene oxide units, and/or G includes at least one G′ group having one of the following formulas (the Y 1 and Y 2 groups being linked to the left and right of the formulas described here below):
where A 102 represents CH or N, R 102 represents H or a linear hydrocarbon chain containing from 1 to 6 carbon atoms, A 101 represents —O—, —NH—(CO)— ou —O(CO)—, R 100 represents H or a methyl, A 100 represents —O— or —NH— and R 101 represents H, Me or —OMe.
The formula
understood to indicate that the Y 2 group may be linked to any one of the six atoms of cyclooctyl and the formula
is understood to indicate that the A 101 and R 101 group may be linked to any one of the four atoms of phenyl.
In particular, v and w independently represent 1 or 2. v and w preferably represent 1.
The G group may include one or more of the G′ groups defined here above.
Thus, in a first embodiment, the G group is constituted of a G′ group. In this embodiment, in formula (I), v and w represent 1.
In a second embodiment, the G group has the formula -G′-Y 3 -G′- wherein:
Y 3 represents a linking group, in particular selected from among:
a single bond, a Z group selected from among —O—, —NH—, —O(OC)—, —(CO)O—, —(CO)NH—, —NH(CO)—, —O—(CO)—O—, —NH—(CO)—O—, —O—(CO)—NH— et —NH—(CO)—NH, a Alk group being an alkylene containing from 1 to 6 carbon atoms, and a Z-Alk, Alk-Z, Alk-Z-Alk or Z-Alk-Z group, where Alk and Z are as defined here above and where the two Z groups of the Z-Alk-Z group are identical or different,
each of the G′ groups independently represents a group having the formula (XI) to (XXVI) described here above, and preferably, the two G′ groups of the formula -G′-Y 3 -G′- are identical.
In this embodiment, in the formula (I), v and w represent 1.
This embodiment is particularly advantageous when the two G′ groups are identical and include a cleavable function. Indeed, it is then sufficient to cleave only one of the two functions in order to break the covalent bonds between the droplets of the material.
In a third embodiment, the G group is a dendrimer comprising (v+w) G′ groups. The G group may in particular be a dendrimer comprising several G′ groups, such as a dendrimer including a polyamidoamine (PAMAM) group. For example, the G group may have one of the following formulas (XXX) to (XXXIII), which include:
4 G′ groups having the formula (XXVI). v and w represent 2. 4 G′ groups having the formula (XXIV), where R 101 represents —O-Me, A 101 represents —NH—, R 100 represents a methyl and A 100 represents —NH—. v and w represent 2. 4 G′ groups having the formula (XIV). v and w represent 2. 16 G′ groups having the formula (XXVI). v and w represent 8.
When L 1 and/or L 2 represent a R—(C═O)— group, wherein R represents a linear hydrocarbon chain containing from 11 to 23 carbon atoms, L 1 and/or L 2 represent groups derived from a fatty acid containing from 12 to 24 carbon atoms.
The statement “L 1 and L 2 represent an ester or an amide of fatty acids containing from 12 to 24 carbon atoms and of phosphatidyl ethanolamine” is understood to mean that they represent a group having the formula:
wherein
R 3 and R 4 independently represent a linear hydrocarbon chain containing from 11 to 23 carbon atoms, A 3 and A 4 represent O or NH, and M represents H or a cation.
Preferably, L 1 and L 2 are identical and/or X 1 and X 2 are identical and/or H 1 and H 2 are identical. Surfactants having the formula (I) that are particularly preferred are those in which L 1 and L 2 are identical, X 1 and X 2 are identical, and H 1 and H 2 are identical. These surfactants are indeed symmetrical compounds and are thus generally easier to synthesise, and are therefore less expensive.
In one embodiment, in Formula (I) described here above, the L 1 -X 1 —H 1 — and/or L 2 -X 2 —H 2 — radicals consist of one of the groups having the following formulas (the Y 1 or Y 2 group being linked to the right of the formulas described here below):
in which:
R 1 , R 2 , R 3 and R 4 independently represent a linear hydrocarbon chain containing from 11 to 23 carbon atoms, A 1 , A 2 , A 3 and A 4 represent O or NH, m, n, o and p independently represent integers from 3 to 500, preferably from 20 to 200, and represents an integer from 20 to 120, M represents H or a cation.
The L 1 -X 1 —H 1 — and/or L 2 -X 2 —H 2 — radicals having the formula (CII) are preferred. Indeed, they are easy to prepare (in particular by means of formation of an ester or an amide between a fatty acid and a derivative of poly(ethylene glycol). In addition, a material including a surfactant containing a L 1 -X 1 —H 1 — and/or L 2 -X 2 —H 2 — radical having the formula (CII) may generally be prepared with a greater amount of this surfactant than a material including a surfactant containing a L 1 -X 1 —H 1 — and/or L 2 -X 2 —H 2 — radical having the formula (CIII). However, the higher the proportion of surfactant having the formula (I) contained in the material, the greater will the cohesion be between the droplets, and the greater will be the ability of the material to maintain its form and be resistant to dilution. Thus, these two properties can be further exacerbated for a material including a surfactant containing a L 1 -X 1 —H 1 — and/or L 2 -X 2 —H 2 — radical having the formula (CII).
The L 1 -X 1 —H 1 — and/or L 2 -X 2 —H 2 — radicals having the formula (CII) with A 2 representing NH are particularly preferred, because the surfactants containing such radicals allow preventing the escape of lipophilic agents of interest that may possibly be present outside the droplets of the material more effectively than the surfactants containing the L 1 -X 1 —H 1 — and/or L 2 -X 2 —H 2 — radicals having the formula (CII) with A 2 representing O.
In one embodiment, in Formula (I), v and w represent 1, L 1 and L 2 are independently R—(C═O)—, wherein R represents a linear hydrocarbon chain containing from 11 to 23 carbon atoms, H 1 and H 2 are independently poly(ethylene oxide) comprising from 3 to 500 ethylene oxide units, X 1 and X 2 represent —O— or —NH—, G consists of a G′ group representing —S—S— (a group having the formula (XV) above) and Y 1 and Y 2 represent —CH 2 —CH 2 —NH—CO—CH 2 —CH 2 — (Alk-Z-Alk group as above with Alk representing —CH 2 —CH 2 — and Z represents —NH—(CO)—) and the surfactant of the material then has the following formula (I′):
in which:
R 2 and R 5 independently represent a linear hydrocarbon chain containing from 11 to 23 carbon atoms, preferably 17, A 2 and A 5 represent O or NH, preferably NH, and n and q independently represent integers from 3 to 500, preferably from 20 to 200.
In one embodiment, the H 1 and H 2 groups are independently selected from a poly (ethylene oxide) comprising more than 3 units of poly(ethylene oxide), or even more than 20 units, in particular more than 50 units (in the above described formulas, m, n, o, p and/or q are preferably greater than 3, or even 20, in particular more than 50).
In one embodiment, the G group of the surfactant having the formula (I) of the material includes a function that is cleavable, in particular chemically (when the surfactant having the formula (I) is placed in contact with a chemical compound capable of cleaving the function of the G group), electrochemically, at certain pHs (acid or alkaline pH), by enzymes, by light (visible light, infrared or ultraviolet light) and/or beyond certain temperatures. Generally, the G group then comprises a G′ group including a cleavable function.
For example:
the β-ketoaminoester function of the G′ group having the formula (XX) is cleavable at acidic pH (typically of around 5), the disulfide function of the G′ group having the formula (XV) is cleavable by ultraviolet radiation, electrochemically, chemically (for example, by being placed in contact with a reducing agent such as tris(2-carboxyethyl)phosphine (TCEP) or dithiothreitol (DTT)), or by enzymes such as thioreductases, the amide function of the G′ group having the formula (XI) is cleavable by enzymes such as proteases, the phosphate function of the G′ group having the formula (XXII) is cleavable by enzymes such as phosphatases, the imine function of the G′ group having the formula (XXI) and (XIII) are cleavable at acid pH or above certain temperatures, the cyclohexene ring of the G′ group having the formula (XVII) is cleavable beyond certain temperatures (by retro Diels-Alder cleavage), the carbonate function of the G′ group having the formula (XIX) and the carbamate function of the G group having the formula (XII) are cleavable at acidic pH or chemically (for example by reaction with a nucleophilic agent), the ortho nitrobenzyl function of the G′ group having the formula (XXIV) is cleavable by the action of light at 365 nm.
The person skilled in the art, in the light of his general knowledge, knows the functions that are cleavable and the conditions under which that is so. He is in particular in a position to select the function of the G′ group of the surfactant having the formula (I) in order for it to be cleavable under the conditions encountered in the desired application of the material according to the invention.
In one embodiment, cleavage of the cleavable function of the G group of the surfactant having the formula (I) of the material is reversible, that is to say that the function may possibly be re-formed so as to recreate covalent bonds between the droplets. The person skilled in the art knows the reversible chemical reactions and the conditions for cleavage and re-formation of bonds. Purely by way of illustration, for example, the disulfide function of the G′ group having the formula (XV) may be cleaved by being brought in contact with a reducing agent and may be reformed by being brought in contact with an oxidising agent.
Amphiphilic Lipid
The material comprises an amphiphilic lipid as a surfactant which enables the formation of the droplets of the dispersed phase. The amphiphilic nature of the surfactant ensures the stabilisation of the droplets of oil within the continuous aqueous phase.
The amphiphilic lipids comprise a hydrophilic part and a lipophilic part. They are generally selected from among the compounds wherein the lipophilic part includes a linear or branched, saturated or unsaturated chain, having from 8 to 30 carbon atoms. They may be selected from among phospholipids, cholesterols, lysolipids, sphingomyelins, tocopherols (unesterified), glucolipids, stearylamines, cardiolipins of natural or synthetic origin; molecules composed of a fatty acid coupled to a hydrophilic group by an ether or ester function such as sorbitan esters like for example sorbitan monooleate and sorbitan monolaurate sold under the trade names Spana by the company Sigma; polymerised lipids; conjugated lipids with short polyethylene oxide (PEG) chains such as non-ionic surfactants sold under the trade names Tween® by the company ICI Americas, Inc. and Triton® by the company Union Carbide Corp; sugar esters such as mono- and di-laurate, mono- and di-palmitate, sucrose mono stearate and sucrose distearate; the said surfactants may be used alone or in mixtures.
Phospholipids are the particularly preferred amphiphilic lipids, in particular the phospholipids selected from among phosphatidyl choline, phosphatidyl ethanolamine, phosphatidyl serine, phosphatidyl glycerol, phosphatidyl inositol, either non-hydrogenated or hydrogenated phosphatidyl phosphatidic acid, notably sold by the company Lipoid.
Lecithin is the preferred amphiphilic lipid.
Typically the oily phase will comprise from 0.01% to 99% by weight, preferably from 5% to 75% by weight, in particular from 10% to 60%, and most particularly from 15% to 45% by weight of amphiphilic lipid.
The amount of amphiphilic lipid advantageously contributes to controlling the size of droplets of the dispersed phase of the material.
Solubilising Lipid
The material according to the invention may include a solubilising lipid, which in particular provides the ability to:
increase the physical and chemical stability of the material, and where the material comprises a lipophilic agent of interest encapsulated within the droplets:
solubilise the lipophilic agent of interest, and improve control of the release of the lipophilic agent of interest.
Preferably the solubilising lipid is solid at ambient temperature (20° C.).
The solubilising lipid may especially be composed of derivatives of glycerol, and in particular of glycerides obtained by esterification of glycerol with fatty acids, notably in the case where the amphiphilic lipid is a phospholipid.
The preferred solubilising lipids, in particular for phospholipids, are glycerides of fatty acids, especially saturated fatty acids, in particular saturated fatty acids containing from 8 to 18 carbon atoms, more preferably from 12 to 18 carbon atoms. Advantageously, the solubilising lipid consists of a complex mixture of various different glycerides. The term “complex mixture” is used to refer to a mixture of mono, di and triglycerides containing fatty chains of different lengths, the said lengths extending preferentially from C8 to C18, for example, in combination, the C8-, C10-, C12-, C14-, C16-, and C18 chains, or from C10 to C18, including, for example in combination, C10-, C12-, C14-, C16-, and C18 chains.
In one embodiment, the said fatty chains may contain one or more unsaturations.
Preferably, the solubilising lipid consists of a mixture of glycerides of saturated fatty acids comprising at least 10% by weight of C12 fatty acids, at least 5% by weight of C14 fatty acids, at least 5% by weight of C16 fatty acids and at least 5% by weight of C18 fatty acids.
Preferably the solubilising lipid consists of a mixture of glycerides of saturated fatty acids containing 0% to 20% by weight of C8 fatty acids, 0% to 20% by weight of C10 fatty acids, 10% to 70% by weight of C12 fatty acids, 5% to 30% by weight of C14 fatty acids, 5% to 30% % by weight of C16 fatty acids, and 5% to 30% by weight of C18 fatty acids.
The mixtures of solid semi-synthetic glycerides that are solid at ambient temperature, sold under the trade name Suppocire®NB by the company Gattefossé and approved for use in humans are particularly preferred solubilising lipids. The N type Suppocire® are obtained by direct esterification of fatty acids and glycerol. These are semi synthetic glycerides of C8 to C18 saturated fatty acids, of which the qualitative and quantitative composition is indicated in the table here below
TABLE
Fatty acid composition of Suppocire ® NB from Gattefossé
Length of chains
[% by weight]
C8
0.1 to 0.9
C10
0.1 to 0.9
C12
25 to 50
C14
10 to 24.9
C16
10 to 24.9
C18
10 to 24.9
The above noted solubilising lipids make it possible to obtain an advantageously stable material. Without intending to be bound to any particular theory, it is assumed that the aforementioned solubilising lipids make it possible to obtain within the material droplets having an amorphous core. The core thus obtained has a high internal viscosity without however exhibiting any crystallinity. However, crystallisation is detrimental to the stability of the material as it generally leads to an aggregation of the droplets and/or to expulsion of the lipophilic agent of interest, if present, to the exterior of the droplets. These physical properties greatly contribute to the physical stability of the material.
The amount of solubilising lipid may vary widely depending on the nature and the quantity of amphiphilic lipid present in the dispersed phase. Generally, the dispersed phase will comprise from 1% to 99% by weight, preferably from 5% to 80% by weight and most particularly from 30% to 75% by weight of solubilising lipid.
Oil
The dispersed phase of the material according to the invention may also include one or more oils.
The used oils preferably have a hydrophilic-lipophilic balance (HLB) of less than 10 and even more preferably comprised between 3 and 9. Advantageously, the oils are used without prior chemical or physical modification to the formation of the material.
Depending on the envisaged applications, the oils may be selected from the biocompatible oils, and in particular from oils of natural origin (plant or animal) or synthetic origin. Among these oils, mention may in particular be made of oils of natural plant origin among which are notably included oils from soybean, linseed, palm, peanut, olive, sesame, grape seed and sunflower; the synthetic oils among which are included in particular triglycerides, diglycerides and monoglycerides. These oils may be from first pressings, refined or inter-esterified.
The preferred oil is soybean oil.
Generally, if present, the oil will be contained in the dispersed phase in a proportion ranging from 1% to 80% by weight, preferably between 5% and 50% by weight and most particularly from 10% to 30% by weight relative to the total weight of the oily phase.
Aqueous Phase
The continuous aqueous phase of the material according to the invention is preferably constituted of water and/or a buffer such as a phosphate buffer, like for example PBS (“Phosphate Buffer Saline”) or a salt solution, in particular of sodium chloride. Generally, the pH of the aqueous phase is in the range of the physiological pH.
According to one embodiment, the continuous phase further includes a thickening agent such as glycerol, a saccharide, oligosaccharide or polysaccharide, a gum or even a protein, preferably glycerol. Indeed, the use of a continuous phase of higher viscosity facilitates the emulsification and thereby provides the ability to reduce the time of sonication.
The aqueous phase advantageously includes from 0% to 50% by weight, preferably from 1% to 30% by weight and most preferably from 5% to 20% by weight of a thickening agent.
Quite obviously, the aqueous phase may further contain other additives such as dyes, stabilisers and preservatives in appropriate amounts.
Co-Surfactant
The material according to the invention may also comprise a co-surfactant. This co-surfactant is located partially in the continuous aqueous phase and partially in the droplets of the dispersed phase.
Preferably, the co-surfactant contains at least one chain composed of units of ethylene oxide or of ethylene oxide and propylene oxide. It may be selected in particular from among the conjugate compounds polyethylene glycol/phosphatidyl ethanolamine (PEG-PE), ethers of fatty acid and polyethylene glycol, esters of fatty acid and polyethylene glycol, and block copolymers of ethylene oxide and propylene oxide.
The polyalkoxylated chain of the co-surfactant comprises generally from 10 to 200, typically from 10 to 150, especially from 20 to 100, preferably from 30 to 80, units of ethylene oxide/propylene oxide. With less than 10 units, the material is not homogeneous because the dispersed phase includes polydisperse droplets, and does not allow for controlling the time of release of the lipophilic agent of interest if it is present. Beyond 200 units, on the one hand the emulsion is not homogeneous because the dispersed phase includes polydisperse droplets, and does not allow for the possibility of controlling the time of release of the lipophilic agent of interest.
By way of examples of co-surfactants, mention may be made in particular of the conjugate compounds based on polyethylene glycol/phosphatidyl ethanolamine (PEG-PE), ethers of fatty acid and polyethylene glycol such as the products sold under the trade name Brij® (for example Brij® 35, 58, 78 or 98) by the company ICI Americas Inc., esters of fatty acid and polyethylene glycol, such as the products sold under the trade names Myrj® by the company ICI Americas Inc. (for example Myrj s20, s40 or s100, previously referenced as 49, 52 or 59) and block copolymers of ethylene oxide and propylene oxide such as the products sold under the trade names Pluronic® by the company BASF AG (for example Pluronic® F68, F127, L64, L61, 10R4, 17R2, 17R4, 25R2 or 25R4) or the products sold under the trade name Synperonic® by the company Unichema Chemie BV (for example Synperonic® PE/F68, PE/L61 or PE/L64).
Preferably, the ratio of the mass of surfactant having the formula (I) over the mass of the ensemble (surfactant having the formula (I)/co-surfactant) is greater than or equal to 15%. It has indeed been observed that such materials are easier to prepare.
The aqueous phase generally includes from 0.01% to 50% by weight, preferably from 1% to 30% by weight and most particularly from 5% to 20% by weight of co-surfactant.
Generally, the mass fraction of the ensemble [optional co-surfactant/amphiphile lipid/surfactant having the formula (I)] relative to the total weight of the core of the droplets [optional oil/optional solubilising lipid/optional co surfactant/amphiphilic lipid/optional lipophilic agent of interest] is less than or equal to 2, preferably less than or equal to 1. This makes it possible to obtain a physically stable system that is not subject to the effects of destabilisation due to Ostwald ripening or coalescence (separation of the aqueous and oily phases).
Generally, the mass fraction of amphiphilic lipid relative to the weight of the co-surfactant is from 0.005% to 100%, notably from 0.01% to 50%, preferably from 0.1% to 30%. Indeed, below 0.005% and above 100%, the droplets of the dispersed phase are often not sufficiently stable and they coalesce within a few hours and it is often difficult to obtain droplets with a diameter of less than 200 nm.
Generally, the material does not include any additional surfactants: the only surfactants of the material are the amphiphilic lipid, the co-surfactant and the surfactant having the formula (I).
In one embodiment, the polyalkoxylated co-surfactant includes a grafted compound of interest. Typically, the compound of interest has been grafted through a chemical bond, generally a covalent bond, to the co-surfactant as defined here above. The grafting may be carried out prior to or after the formation of the emulsions used to prepare the material (emulsions 1 and 2 here below). The latter case may be recommended when the chemical reactions used are compatible with the stability of the emulsions, in particular in terms of pH. Preferably, the pH during the grafting reaction is comprised between 5 and 11.
Generally, this grafting has been carried out at one end of the polyalkoxylated chain or chains of the co-surfactant, and the compound of interest is thus located at the surface of the droplets of the dispersed phase of the material.
The compounds of interest may for example be:
biological targeting ligands such as antibodies, peptides, saccharides, aptamers, oligonucleotides or compounds such as folic acid; during the release from the droplets of the material, this biological ligand will be recognised in a specific manner by certain cells (for example tumoral cells as for example described in the article of S. Achilefu, Technology in Cancer Research & Treatment, 2004, 3, 393-408) or by certain organs which it is desired to target, which provides the ability to control the localisation of the release of the optional lipophilic agent of interest; a stealth agent: an added entity in order to impart stealth to the material with regard to the immune system, to increase the circulation time thereof in the organism, and to slow down the elimination thereof.
Agent of Interest
In one embodiment, the material may include one or more agent(s) of interest.
The agent of interest may be of highly varied nature depending on the desired application of the material. Thus, the agent of interest may be:
a chemical sensing agent (“scavenger” in English), that is to say a compound that is capable of reacting with a chemical compound that it is desired to eliminate from a medium. The chemical sensor incorporated into the material according to the invention is chosen based on the compound that it is desired to eliminate. For example, a chemical sensor can react with impurities and perhaps can thus be used in order to purify or decontaminate a medium. In another example, during a chemical reaction, a chemical sensor may be used to eliminate the products of a secondary reaction or excess reagent. a chemical detection agent, that is to say a chemical compound that is capable of emitting a signal when it is placed in contact with an analyte that it is desired to be detected and/or quantified. The chemical detector may be a fluorogenic detector (bringing into contact the fluorogenic detector with the analyte produces a detectable fluorescent emission) or a chromogenic detector (bringing into contact the chromogenic detector with the analyte produces a detectable change in colour). The analyte may be of any kind, for example a bacterium (such as in the patent application FR 2 954 911), a metal, a pollutant, etc. The chemical detector incorporated within the material according to the invention is selected based on the analyte that it is desired to detect. For purely illustrative purposes, in order to detect heavy metals, a quinoline derivative may be incorporated in the droplets of the material according to the invention as a fluorogenic detector (Da-Yu Wu et al., Dalton Trans., 2006, 3528-3533). a catalyst, such as a metallic or an organometallic catalyst. an optical agent such as a dye, a chromophore, a fluorophore, for example 1,1′-Dioctadecyl-3,3,3,3-tetramethylindodicarbocyanine perchlorate (DiD), 1,I-Dioctadecyl-3,3,3′,3-tetramethylindotricarbocyanine iodide (DiR), indocyanine green (ICG), or even components having optoelectronic properties, such as saturants or optical absorbents). a phytosanitary or plant protection agent, such as a mineral substance (for example: copper sulphate) or organic substance (for example: carbamate such as carbofuran, furadan, etc), natural substance (for example: Bacillus thuringiensis Bt) or derived from chemical synthesis (for example: Glyphosate). a taste/odour masking agent, such as a flavour substance and/or fragrance or aroma substance, such as menthol or cinnamaldehyde, for pharmaceutical (galenic) use or agrifood application. a cosmetic agent. a therapeutic agent, such as an pharmaceutical active ingredient or a physical agent, such as a radioactive isotope or a photosensitiser.
Therapeutic agents that may be included in the material according to the invention include in particular active ingredients acting via the chemical, physical or biological route. Thus, it may involve pharmaceutical active ingredients or biological agents such as DNA, proteins, peptides or antibodies or even agents that are useful for physical therapies such as compounds useful for thermotherapy, compounds useful for phototherapy that release singlet oxygen when they are excited by a light, and radioactive agents. Among the pharmaceutical active ingredients that are of interest as therapeutic agents, mention may be made in particular of the agents used in the treatment of AIDS, agents used in the treatment of heart disease, analgesics, anesthetics, anorectics, anthelmintics, anti-allergic agents, antianginals, antiarrhythmics, anticholinergics, anticoagulants, antidepressants, antidiabetics, anti-diuretics, antiemetics, anticonvulsants, antifungals, antihistamines, antihypertensives, anti-inflammatories, anti-migraine agents, antimuscarinics, antimycobacterials, anticancer agents including antiparkinson agents, anti-thyroid agents, antivirals, astringents, blocking agents, blood products, blood substitutes, cardiac inotropic agents, cardiovascular agents, central nervous system agents, chelating agents chemotherapy agents, hematopoietic growth factors, corticosteroids, cough suppressants, dermatological agents, diuretics, dopaminergic agents, inhibitors of elastase, endocrine agents, ergot alkaloids, expectorants, gastrointestinal agents, genitourinary agents, the growth hormone releasing factor, growth hormones, hematological agents, hematopoietic agents, hemostatics, hormones, immunological agents, immunosuppressants, interleukins, interleukin analogues, lipid regulating agents, gonadotropin releasing hormone, muscle relaxants, narcotic antagonists, nutrients, nutritional agents, oncology therapies, organic nitrates, parasympathomimetic agents, prostaglandins, antibiotics, renal agents, respiratory agents, sedatives, sex hormones, stimulants, sympathomimetic agents, systemic anti-infectives, tacrolimus, thrombolytic agents, thyroid agents, treatments for attention disorders, vaccines, vasodilators, xanthines, cholesterol lowering agents, healing agents. Among the active ingredients acting via the biological route, mention may be made of oligonucleotides, DNA, RNA, siRNA, microRNA's, peptides and proteins. Quite obviously, the therapeutic agents can be formulated directly in their active form or in the form of a prodrug. Among the physical agents, mention may be made in particular of radioisotopes, and photosensitisers. Among the photosensitisers, mention may be made in particular of those belonging to the class of tetrapyrroles such as porphyrins, bacteriochlorins, phthalocyanines, chlorins, purpurins, porphycenes, pheophorbides, or even those belonging to the class of texaphyrins or hypericins. Mention may also be made of derivatives of 5-aminolevulinic acid and the ester derivatives thereof, these components being known as metabolic precursors of Protoporphyrin IX. Among the first generation photosensitisers, mention may be made of hemato porphyrin and a mixture of hemato porphyrin derivatives (HpD) (sold under the trade name Photofrin® by Axcan Pharma). Among the second generation photo-sensitisers, mention may be made of meta-tetra-hydroxyphenyl chlorin (mTHPC; trade name Foscan Biolitec AG) and the Benzoporphyrin derivative monoacid ring A (BPD-MA sold under the trade mark Visudyne® by QLT and Novartis Opthalmics). Formulations of second generation photosensitisers which combine with these photosensitisers a molecule (lipid, peptide, sugar, etc) qualified as a transporter that makes possible the selective routing and delivery thereof in the tumour tissue are called third generation photosensitisers.
Furthermore, the oily phase can, in addition to the therapeutic agent, also include an imaging agent, in particular for MRI (Magnetic Resonance Imaging), PET (Positron Emission Tomography), SPECT (Single Photon Emission Computed Tomography), ultrasound echography, radiography, x ray tomography and optical imaging (fluorescence, bioluminescence, diffusion, etc). These agents can be used to track and trace the position of the droplets (and thus of the therapeutic agent) after administration of the material to the patient.
The quantities of the agent of interest are dependent upon the intended application as well as upon the nature of the agents.
However, when the agents of interests are therapeutic agents, it would generally be sought to formulate the material with a maximum concentration of the therapeutic agent, in order to limit the volume and/or duration of application, in particular the volume and/or duration of administration to the patient.
However, it has been found that the presence of the solubilising lipid in the oily phase provides the ability to incorporate a fairly significant amount of the lipophilic agent of interest therein. The solubilising lipid indeed facilitates the incorporation of the lipophilic agents of interest into the core of the droplets. Amphiphilic agents of interest are mainly incorporated into the membrane of the droplets.
The material according to the invention will most often contain a quantity from 0.001% to 30% by weight, preferably from 0.01% to 20% by weight, and even more preferably from 0.1% to 10% by weight of the agent of interest.
The agent of interest may be hydrophilic (it would then be located in the aqueous continuous phase of the material) or lipophilic (it would then be encapsulated within the droplets that form the dispersed phase of the material or be located at the interface of the aqueous and oily phases on the surface of the droplets, depending on its amphiphilic or lipophilic affinity).
In one embodiment, the material includes at least one hydrophilic agent of interest and at least one lipophilic agent of interest. For example, the material comprises at least one hydrophilic therapeutic agent and at least one lipophilic therapeutic agent.
Other Properties of the Material
On account of its formulation, the material according to the invention is stable and offers an excellent degree of storage stability (greater than 5 months or than 8 months).
In addition, the material may be formulated in a manner such as to ensure that the surface of the dispersed phase has a low zeta potential, ideally comprised between −25 mV and +25 mV, or even between −20 mV and +20 mV, and in particular between −10 mV and +10 mV, or even zero. Indeed, the polyalkoxylated chains of the co-surfactant and the surfactant having the formula (I), that are hydrated and uncharged, covering the surface of the droplets, serve to screen the charges carried by the amphiphilic lipids at the solid surface of the droplets. The condition found to be brought about is therefore a case of steric stabilisation of the droplets, and not an electrostatic stabilisation thereof. The zeta potential is a key parameter that has significant effect on the interactions with biological media. The droplets that possess a highly positive surface charge, that is to say greater than 25 mV are generally more cytotoxic than droplets with negative or neutral zeta potential.
Furthermore, a low zeta potential has the advantage of limiting the nonspecific recognition of the droplets by macrophages when the material is dispersed, in particular in viva
In contrast to emulsions whose stability is based on electrostatic effects, and which have a high zeta potential and can be spontaneously stable, the emulsions described in the context of this invention require a supply of energy in order to be formed, for example by means of sonication. The emulsion thus obtained is then metastable and comprises droplets whose charge is low or zero.
Preferably, the pH of the material is comprised between 5.5 and 8.5 and preferably between 6 and 7.5. A pH within these ranges is compatible with the use of an appropriate aqueous buffer adapted to the pH of a physiological medium.
[Method of Preparation]
According to a second object, the invention relates to a method for preparing the material defined here above, comprising bringing into contact:
an emulsion 1 comprising a continuous aqueous phase and a dispersed phase, dispersed in the form of droplets containing an amphiphilic lipid and a surfactant having the following formula (LI):
L 1 -X 1 —H 1 —Y 1 -G 1 (LI),
with an emulsion 2 comprising a continuous aqueous phase and a dispersed phase, dispersed in the form of droplets containing an amphiphilic lipid and a surfactant having the following formula (LII):
G 2 -Y 2 —H 2 —X 2 -L 2 (LII)
wherein L 1 , X 1 , H 1 , Y 1 , L 2 , X 2 , H 2 and Y 2 are as defined here above, and G 1 and G 2 are groups that are capable of reacting in order to form the G group as defined here above, under conditions that allow for the reaction of the surfactants having the formulas (LI) and (LII) in order to form the surfactant having the formula (I) as defined here above, whereby covalent bonds between the droplets of the dispersed phase are formed.
According to a preferred embodiment of the invention, the reaction of G1 and G2 in order to form the G group is carried out by irradiation of the mixture formed by the emulsion 1 and the emulsion 2 by means of a light radiation.
When the G group comprises a single G′ group, the G 1 and G 2 groups are typically groups that are capable of reacting with each other so as to form the G group.
When the G group comprises several G′ groups, generally the emulsions 1 and 2 are placed into contact with a compound that is capable of reacting with the surfactants having the formulas (LI) and (LII) in order to form the G group. This compound typically comprises at least v functions G 1 that are capable of reacting with the G 1 group and w functions G′ 2 that are capable of reacting with the G 2 group.
Thus, in the embodiment in which the G group has the formula -G′-Y 3 -G′- as defined here above, the method for preparing the material typically comprises bringing into contact:
an emulsion 1 as defined here above, and an emulsion 2 as defined here above, with a compound having the formula G′ 1 -Y 3 -G′ 2 in which Y 3 is as defined here above, G′ 1 is a group that is capable of reacting with G 1 in order to form the first G′ group as defined here above and G′ 2 is a group that is capable of reacting with G 2 in order to form the second G′ group as defined here above (being of the same or different nature as the first G′ group),
under conditions that allow for the reaction of the surfactants having the formulas (LI) and (LII) and the compound having the formula G′ 1 -Y 3 -G′ 2 in order to form the surfactant having the formula (I) in which the G group has the formula -G′-Y 3 -G′- as defined here above, whereby covalent bonds between the droplets of the dispersed phase are formed.
In similar fashion, in the embodiment defined here above wherein the G group is a dendrimer comprising (v+w) G′ groups, the method for preparing the material typically comprises bringing into contact:
an emulsion 1 as defined here above, and an emulsion 2 as defined here above, with a dendrimer having the formula (G′ 1 ) v -Y 4 -(G′ 2 ) w in which v and w are as defined here above, G′ 1 is independently a group that is capable of reacting with G 1 in order to form a G′ group as defined here above and G′ 2 is independently a group that is capable of reacting with G 2 in order to form a G′ group as defined here above (each G′ group being of the same or different nature as the other G′ groups) and Y 4 is the skeleton of a dendrimer,
under conditions that allow for the reaction of the surfactants having the formulas (LI) and (LII) and the dendrimer having the formula (G′ 1 ) v -Y 4 -(G′ 2 ) w in order to form the surfactant having the formula (I) in which the G group is a dendrimer comprising (v+w) G′ groups, whereby covalent bonds between the droplets of the dispersed phase are formed.
For example, in order to form a G group having the formula (XXX), (XXXI), (XXXII) and (XXXIII), the compound having the formula (G′ 1 ) v -Y 4 -(G′ 2 ) w may respectively have one of the following formulas (XXX′), (XXXI′), (XXXII′) and (XXXIII′):
(wherein G′ 1 and G′ 2 -represent NH 2 and v and w represent 2),
(wherein G′ 1 and G′ 2 -represent NH 2 and v and w represent 2),
(wherein G′ 1 and G′ 2 -represent
and v and w represent 2),
(wherein G′ 1 et G′ 2 -represent NH 2 and v and w represent 8).
Formation of the Surfactant Having the Formula (I) by Reaction Between the Surfactants Having the Formulas (LI) and (LII)
In the light of their general knowledge in chemistry, the person skilled in the art is in a position to select the nature of the G′ 1 , G′ 2 , Y 3 , Y 4 , G 1 and G 2 groups to be used in order to form the G group, as well as the conditions that would allow for the reaction to occur. The usual reactions in organic chemistry may be followed, in particular those described in “Comprehensive Organic Transformations: A Guide to Functional Group Preparations” by Richard C. Larock published by John Wiley & Sons Inc, and the references that are cited therein. Thus, the examples of G 1 and G 2 groups cited here below are intended by way of illustration and are not limiting.
Typically, when the G group consists of a G′ group, the G 1 and G 2 groups of the surfactants having the formulas (LI) and (LII) may for example be chosen as follows:
G 1 represents a thiol (—SH) and G 2 represents:
either a maleimide, a surfactant having the formula (I) in which G comprises a G′ group representing a group having the formula (XIV) wherein A 102 represents N then being formed, or a vinyl sulfone, a surfactant having the formula (I) in which G comprises a G′ group representing a group having the formula (XVI) being then formed, or a group —SS-pyridinyl or —SH, a surfactant having the formula (I) in which G comprises a G′ group representing a group having the formula (XV) being then formed,
G 1 represents a hydroxyl and G 2 represents —COOH or an activated ester, a surfactant having the formula (I) in which G comprises a G′ group representing a group having the formula (XXIII) being then formed, G 1 represents an amine —NH 2 and G 2 represents —COOH or an activated ester, a surfactant having the formula (I) in which G comprises a G′ group representing a group having the formula (XI) then being formed, G 1 represents a hydroxyl and G 2 represents an activated carbonate, a surfactant having the formula (I) in which G comprises a G′ group representing a group having the formula (XIX) then being formed, G 1 represents an amine —NH 2 and G 2 represents an activated carbonate, a surfactant having the formula (I) in which G comprises a G′ group representing a group having the formula (XII) being then formed, G 1 represents an amine NH 2 and G 2 represents an aldehyde CHO, a surfactant having the formula (I) in which G comprises a G′ group representing a group having the formula (XXI) being then formed, G 1 represents a hydrazide having the formula —(C═O)—NH—NH 2 and G 2 represents a group —(C═O)—R10 2 , a surfactant having the formula (I) in which G comprises a G′ group representing a group having the formula (XIII) being then formed, G 1 represents an alkyne and G 2 represents an azide, a surfactant having the formula (I) in which G comprises a G′ group representing a group having the formula (XVIII) being then formed, G 1 represents a cyclooctyne and G 2 represents an azide, a surfactant having the formula (I) in which G comprises a G′ group representing a group having the formula (XVIII′) then being formed, G 1 represents a furan and G 2 represents a maleimide, a surfactant having the formula (I) in which G comprises a G′ group representing a group having the formula (XVII) being then formed, G 1 represents an aldehyde and G 2 represents an amine, a surfactant having the formula (I) in which G comprises a G′ group representing a group having the formula (XXI) being then formed, G 1 represents a phosphate having the formula —O—P(═O)(OH) 2 and G 2 represents a hydroxyl, a surfactant having the formula (I) in which G comprises a G′ group representing a group having the formula (XXII) then being formed, G 1 represents a good leaving group LG and G 2 represents a group having the following formula
a surfactant having the formula (I) in which G comprises a G′ group representing a group having the formula (XXIV) wherein A 101 represents 0 then being formed,
G 1 represents a hydroxyl or an amine —NH 2 and G 2 represents a group having the following formula
a surfactant having the formula (I) in which G comprises a G′ group representing a group having the formula (XXIV) wherein A 101 represents respectively —O—(CO)— or —NH—(CO) being then formed,
G 1 represents a good leaving group LG and G 2 represents a hydroxyl, a surfactant having the formula (I) in which G comprises a G′ group representing a group having the formula (XXV) being then formed,
G 1 represents a good leaving group LG and G 2 represents an amine —NH 2 , a surfactant having the formula (I) in which G comprises a G′ group representing a group having the formula (XXVI) being then formed,
G 1 represents an oxyamine —O—NH 2 and G 2 represents an aldehyde, a surfactant having the formula (I) in which G comprises a G′ group representing a group having the formula (XXVII) being then formed.
When the G group comprises a plurality of G′ groups, the selection of groups reacting together: G′ 1 and G 1 on the one hand and G′ 2 and G 2 on the other hand, may be carried out in the same manner, by replacing the G 1 or G 2 groups in the examples mentioned above with G′ 1 or G′ 2 .
Emulsions 1 and/or 2 Comprising a Surfactant Having the Formula (LI) and (LII) where L 1 -X 1 —H 1 — and/or L 2 -X 2 —H 2 — has (have) the Formula (CII) Mentioned Above
According to another object, the invention relates to a surfactant having the following formula (L):
in which:
R 2 represents a linear hydrocarbon chain containing from 11 to 23 carbon atoms, preferably 17, A 2 represents O or NH, preferably NH, n represents an integer from 3 to 500, preferably from 20 to 200, Y 2 represents a linking group (preferably one of the groups Y 2 mentioned here above), and φ represents a functional group that is capable of binding to an agent of interest.
The invention also relates to an emulsion (referred to as emulsion 3) comprising a continuous aqueous phase and a dispersed phase, dispersed in the form of droplets containing an amphiphilic lipid, a surfactant having the following formula (L), optionally a solubilising lipid and optionally a co-surfactant (in particular the amphiphilic lipid/solubilising lipid/co-surfactant as defined here above).
The droplets of these emulsions 3 advantageously present φ groups that may be functionalised on the surface. It is therefore possible to graft the agents of interest (biological or therapeutic agents, fluorophoric or chromophoric agents, for example) on the surface of these droplets.
In one embodiment, the φ group is a G 1 or G 2 group as defined here above and the emulsion 3 corresponds to the emulsion 1 or 2 defined here above. When the material according to the invention is formed based on an emulsion 1 and an emulsion 2 comprising surfactants having the formula (LI) and (LII) corresponding to the formula (L), the radicals L 1 -X 1 —H 1 — and L 2 -X 2 —H 2 — of the surfactant having the formula (I) of the material correspond to the formula (IIC) as defined here above.
The surfactants having the formula (L) are advantageously easy to prepare (in particular by the formation of an ester or an amide between a fatty acid and a derivative of poly(ethylene glycol)).
In addition, an emulsion can generally be prepared with a greater amount of the surfactant having the formula (L) than of a surfactant type that is an ester or amide of fatty acids containing from 12 to 24 carbon atoms and of phosphatidyl ethanolamine (for example DSPE-PEG). As a consequence, the emulsion comprising a surfactant having the formula (L) advantageously comprises at the surface more of the groups φ that may be functionalised, and it is therefore possible to graft more of the agents of interest at the surface of the droplets.
Furthermore, it has evidently been demonstrated that the surfactant having the formula (L) used in an emulsion leaks out of the droplets to a lesser degree than a surfactant type that is an ester or amide of fatty acids containing from 12 to 24 carbon atoms and of phosphatidyl ethanolamine. This anti leakage effect is more significant for the surfactants having the formula (L) in which A 2 represents NH in comparison with those in which A 2 represents O. In addition, the emulsions comprising the surfactants in which A 2 represents NH are generally more stable than those comprising the surfactants in which A 2 represents O.
Formation of the Emulsions 1 and 2
The emulsions 1 and 2 as described may quite easily be prepared by means of dispersion of suitable quantities of oily phase and aqueous phase under the effect of a shearing action, typically by a process comprising the steps consisting of:
(i) preparing the oily phase comprising of an amphiphilic lipid, (ii) preparing an aqueous phase comprising of a surfactant having the formula (LI) or (LII), (iii) dispersing the oily phase in the aqueous phase under the action of a shearing process that is sufficient to form an emulsion; and (iv) recovering the emulsion thus formed.
In this method, first of all the different oily constituents are mixed in order to prepare an oily premix for the dispersed phase of the emulsion. The mixing of the various different oily constituent substances may be optionally facilitated by bringing about the dissolution of one of the constituents or of the complete mixture in an appropriate organic solvent and subsequent evaporation of the solvent, in order to obtain a homogeneous oily premix for the dispersed phase. The choice of organic solvent depends on the solubility of the constituent substances. The solvents employed may be, for example methanol, ethanol, chloroform, dichloromethane, hexane, cyclohexane, dimethyl sulfoxide (DMSO), dimethylformamide (DMF) or even toluene. In the event a material for the administration of therapeutic agents is involved, use is made preferably of organic solvents that are volatile and/or non-toxic to humans. Furthermore, it is preferable to carry out preparation of the pre-mix at a temperature at which all of the ingredients are liquid.
Advantageously, the oily phase is dispersed in the aqueous phase in the liquid state. If one of the phases solidifies at ambient temperature, it is preferable to perform preparation of the mixture with one or preferably the two phases heated to a temperature greater than or equal to the melting temperature, with the two phases being heated to a temperature preferably lower than 80° C., and more preferably lower than 70° C., and even more preferably lower than 60° C.
The emulsification under the effect of shearing is preferably carried out by making use of a sonicator or a microfluidiser. Preferably, the aqueous phase and then the oily phase are introduced in the desired proportions into a suitable cylindrical vessel and the sonicator is then dipped into the medium and turned on and operated for a sufficient period of time in order to obtain an emulsion, which is usually a few minutes.
The emulsions 1 and 2 are generally nano emulsions. By means of the above process, a homogeneous nano emulsion is obtained in which the average diameter of the droplets is greater than 20 nm and less than 200 nm, in particular from 50 nm to 120 nm.
Preferably, the zeta potential of the emulsion is less than 25 mV in absolute value, that is to say, between −25 mV and 25 mV.
Prior to the preparation of the material according to the invention, the emulsions 1 and/or 2 may be diluted and/or sterilised, for example by filtration or dialysis. This step provides the ability to eliminate any optional aggregates that may have formed during the process of preparation of the emulsions.
The emulsions 1 and 2 thus obtained are ready to be used, after dilution as may be necessary. Quite obviously, it is possible to prepare the material according to the invention by accordingly implementing the process for an emulsion 1 and 2 that may be similar or identical.
The material according to the invention can be prepared regardless of the proportion of the continuous aqueous phase of the emulsions 1 and 2, which is advantageous in terms of cost of preparation because it is possible to prepare the material based on emulsions 1 and 2 wherein the proportion of phase that is dispersed is low. The ratio between the dispersed phase and the aqueous phase may thus vary to a large extent in the emulsions 1 and 2. The dispersed phase of the emulsions 1 and 2 (optional oil/optional solubilising lipid/amphiphilic lipid/optional co-surfactant/optional lipophilic agent of interest/surfactant having the formula (LI) or (LII)) represent generally between 0.1% and 90% by weight relative to the total weight of the emulsion, that is to say, relative to the weight of the continuous aqueous phase and the dispersed oily phase.
According to the reactions involved in the formation of the surfactant having the formula (I), the formation of the material according to the invention may take place in the presence of a cross-linker, by changing of the pH, the action of light or some other means.
In practice, beyond a certain total proportion of aqueous phase upon bringing into contact the emulsions 1 and 2 (which varies from one material to another, in particular according to the nature and the proportions of the various components of the material), it may be noted that there is formation on the one hand, of a material comprising a dispersed phase dispersed in the form of droplets in a continuous aqueous phase, and on the other hand, an aqueous phase that is essentially, generally completely, free of droplets.
[Uses]
The material according to the invention has various applications that are highly varied.
According to a third object, the invention relates to the use of the material as defined here above as a membrane or as a coating.
Advantageously, the material according to the invention may be prepared from biocompatible constituent components and hence be biocompatible. Thus, it may for example be used as a coating for an object or a non biocompatible material intended to be implanted in the body of a human or an animal, such as a prosthesis, an implant or an implantable electrode. The invention therefore also relates to a prosthesis, an implant or an implantable electrode coated by the material according to the invention.
Use of the Material Including a Surfactant Having the Formula (I) Wherein the G Group Includes a Cleavable Function
According to a fourth object, the invention relates to the use of the material including a surfactant having the formula (I) wherein the G group includes a cleavable function such as defined here above, as a valve.
Thus, when a material as defined here above is introduced into a closed environment (pipe, tube, capillary), it may stop or modify (generally slow down) the flow of a fluid, preferably a liquid.
If the material is placed under appropriate conditions that allow for the cleaving of the cleavable function of the G group of the surfactant having the formula (I) (for example by bringing into contact a chemical compound or an enzyme capable of cleaving the function of the G group, or in electrochemical conditions, with conditions related to pH, light or temperature that enable this cleavage, as explained here above), the covalent bonds between the droplets of the material according to the invention are cleaved. Thus, the droplets are no longer bound to each other and the material disaggregates, which has the consequential effect of increasing the flow of fluid. Preferably, the fluid whose flow is modified or stopped by the material according to the invention used as a valve, comprises or is constituted of an aqueous phase.
When the reaction of cleavage of the cleavable function of the G group of the surfactant having the formula (I) is reversible, after the said function has been cleaved, by placing the material under conditions that make possible the re-formation of the cleavable function of the G group of the surfactant having the formula (I) (and thus the re-formation of the covalent bonds between the droplets), it is possible to close the valve. It is then possible to open and close the valve again.
According to a fifth object, the invention also relates to the use of the material including a surfactant having the formula (I) wherein the G group includes a cleavable function as defined here above, as a mask for preparing biochips. Indeed, the material according to the invention is then a coating that is destructible (by means of cleavage of the said function) and optionally eventually reformable (by means of reformation of the said function) and suitable for such use. Use may be made for example of the methods described in Nie, Z H, Kumacheva, E, Patterning Surfaces with Functional Polymers, Nature Materials 2008, 7 (4), 277-290; or Hoffmann, J et al, Photopatterning of Thermally Sensitive Hydrogels Useful for Microactuators. Sensors and Actuators, A: Physical, 1999, 77 (2), 139-144 by using the material according to the invention in place of the materials described therein.
Use of the Material Comprising an Agent of Interest
According to a sixth object, the invention relates to the use of the material comprising an agent of interest as defined here above, as a chemical detector. Indeed, when the agent of interest is a chemical detection agent, the material according to the invention can be used to detect and/or quantify the presence of a chemical compound (analyte, pollutant, metal, etc).
According to a seventh object, the invention relates to the use of the material comprising an agent of interest as defined here above, as a chemical sensor. When the agent of interest is a chemical sensing agent, the material according to the invention can be used as a chemical sensor, in particular for purifying a medium or as a scavenger (chemical sensing agent contained in the material that reacts with the chemical compound that it is desired to eliminate (for example a pollutant, or during a chemical reaction, a product of a secondary reaction or an excess of reagent)).
According to an eighth object, the invention relates to the use of the material comprising an agent of interest as defined here above, for the delivery of the agent of interest, in particular the delivery ex vivo, in vivo or in vitro of agents of interest. Mention may be made in particular of the delivery of an optical agent, a phytosanitary or plant protection agent, a taste/odour masking agent, or a cosmetic agent. The case of the delivery of a therapeutic agent is described here below.
When the material according to the invention comprises a plurality of agents of interest, the invention relates to the use thereof for the delivery of these agents interest where delivery may be combined, simultaneous, or carried out separately at different times.
In the embodiment wherein the material comprises a hydrophilic agent of interest and a lipophilic agent of interest, the invention relates to the use thereof for the delivery of the hydrophilic agent of interest and the lipophilic agent of interest, where delivery thereof may be combined, simultaneous, or carried out separately at different times.
According to a ninth object, the invention relates to the use of the material comprising a catalyst type agent of interest as defined here above, as a catalyst.
Use of the Material Comprising a Therapeutic Agent
According to a tenth object, the invention relates to a material comprising a therapeutic agent for the use thereof for treating or preventing a disease. Indeed, the material may be used for the administration of at least one therapeutic agent to a human or an animal. The invention also relates to the material comprising a therapeutic agent used as a medicament, and to a method of therapeutic treatment consisting of the administration to a human or an animal in need thereof of an effective amount of the material comprising a therapeutic agent for treating or preventing a disease.
Since the material according to the invention may be prepared exclusively from constituent components approved for use in humans or animals, it is particularly advantageous for a parenteral route of administration. However, it is also possible to consider the administration thereof by other routes, including oral or topical routes.
The techniques described in the published paper by Hoffman, The Origins and evolution of “controlled” drug delivery systems, Journal Controlled release 132 (2008) 153-163, may in particular be used, by replacing the materials described therein with the material according to the invention.
For example, the material may be administered by making use of a syringe or a transdermal patch (known as a “patch”), this formulation is thus particularly suitable because the material has an adhesive nature.
Use of the Material Comprising a Hydrophilic Therapeutic Agent and a Lipophilic Therapeutic Agent
According to an eleventh object, the invention relates to the material comprising at least one hydrophilic therapeutic agent and at least one lipophilic therapeutic agent for use thereof for the administration of at least one hydrophilic therapeutic agent and at least one lipophilic therapeutic agent to a human or an animal in order to treat or prevent a disease.
Indeed, the droplets, and in particular the nano droplets, charged with therapeutic agents constitute a solution that is ideal for overcoming the low degree of selectivity of medicinal products, in particular anticancer medicinal products, by making possible by means of the passive targeting and/or active targeting of the cancerous tissues, and thus providing the ability to reduce the severe side effects.
Certain treatments require the administration of multiple therapeutic agents, at times having different rates of solubility, which then involves multiple administration, which is a source of discomfort and a significant loss of time for patients. In addition, it is often desirable for the various different therapeutic agents to not all be released at the same time, or even not in the same location.
The development of formulations that make possible the delivery of multiple therapeutic agents is thus desirable.
The material according to the invention provides the ability to deliver in one single administration/application two or more therapeutic agents, with different release times. At lipophilic therapeutic agent is released at a time t lipophilic , that may be identical to or different from t hydrophilic .
Indeed, the hydrophilic therapeutic agent is located essentially in the continuous aqueous phase of the material. It is trapped between the droplets of the dispersed phase. When the material is administered, it comes in contact with the physiological fluids (blood, plasma, etc) that are exchanged with the continuous aqueous phase of the material, that thereby releases the hydrophilic therapeutic agent. The time of release of the hydrophilic therapeutic agent t hydrophilic is related to the time of exchange between the continuous aqueous phase of the material and the physiological fluids, to the time of diffusion of the hydrophilic therapeutic agent through the material and sometimes to the time of release of the droplets t droplet when the surfactant having the formula (I) includes functions that are capable of being cleaved in the physiological medium (with the cleavage of these functions then leading to the cleaving of the covalent bonds between the droplets and to the disaggregation of the three dimensional network of the material).
In addition, the lipophilic therapeutic agent is essentially located in the dispersed phase of the material, either in the interior of the droplets, or on the surface of the droplets. The time of release of the lipophilic therapeutic agent t lipophilic is related to the time of diffusion of the lipophilic therapeutic agent to the exterior of the droplet, to the time of degradation of the droplets and sometimes to the time of release of the droplets t droplet .
The locations of release of the hydrophilic therapeutic agents L hydrophilic and the lipophilic therapeutic agents L lipophilic may also be different. In particular, if the surfactant having the formula (I) includes functions that are capable of being cleaved in the physiological medium when the material disaggregates at the site where it has been administered, the hydrophilic therapeutic agent is then released at the location of administration and the droplets that are released from the material are carried away by the physiological fluid (blood, plasma), to another site of the subject, wherein the lipophilic therapeutic agent will then be released.
Thus, by adapting the composition of the material according to the invention (nature of the constituent components, mass fraction of the constituent components, size of droplets, etc), based on the physical and chemical properties of the agents, as explained here below, it is advantageously possible to modify these times of release t hydrophilic and t lipophilic as well as the locations L hydrophilic and L lipophilic .
Most certainly, if the material includes more than one hydrophilic therapeutic agent and/or more than one lipophilic therapeutic agent, it is possible to appropriately adapt the composition of the material so as to adjust the times of release of each agent, and to ensure that these latter differ from each other. It would be possible in particular to act on the parameters of the composition of the material that influence the release of the hydrophilic agents of interest or the lipophilic agents of interest in order to ensure that t hydrophilic 1 differs from t hydrophilic 2 and/or that t lipophilic 1 differs from t lipophilic 2 as explained here below. The different locations of release of the agents may also be influenced and made to differ from each other.
The time of release of the hydrophilic therapeutic agent t hydrophilic depends on the composition of the material, in particular:
on the mass fraction of the dispersed phase relative to the total weight of the material; on the number of alkoxylated units of the alkoxylated co-surfactant (and thus on the length of the alkoxylated chain of the alkoxylated co-surfactant); on the diameter of the droplets; on the nature of the surfactant having the formula (I).
The time of release of the lipophilic therapeutic agent t lipophilic is related to the time of diffusion of the lipophilic therapeutic agent to the exterior of the droplet and to the time of release of the droplets t droplet . The time of release of the lipophilic therapeutic agent t lipophilic depends:
on the mean diameter of the droplets, as described in particular in Williams, Y. et al. Small (2009); 5(22): 2581-8, Choi, H S et al. Nanoletters (2009) 9(6): 2354-9 and Massignani, M et al. Small. (2009) 5(21): 2424-32. The droplets of the material according to the invention are advantageously monodisperse in order to provide for a homogenous release over time of the lipophilic therapeutic agent. on the nature of the components of the oily phase, in particular on the solubilising lipid; on the physical and chemical characteristics of the lipophilic therapeutic agent (Nel, A E et al. Nature Materials 8 (2009) pp 543-557), in particular on its log P, which affects the location of the lipophilic therapeutic agent within the interior or on the surface of the droplet.
A highly lipophilic therapeutic agent remains within the droplet and is released only when it is degraded through chemical degradation (by hydrolysis of the components of the droplets following a resultant significant increase or decrease of the medium, for example if the droplets get internalised within the interior of the cells by passing through the lysosomes) or through enzymatic degradation by lipases (Olbrich, C et al. International Journal of Pharmaceutics 237 (2002) pp 119-128 and Olbrich, C International Journal of Pharmaceutics 180 (1999) pp 31-39).
Generally, the release time of the hydrophilic therapeutic agent t hydrophilic is less than the release time of the lipophilic therapeutic agent t lipophilic .
The location of the release of the hydrophilic therapeutic agent L hydrophilic is generally the location of administration of the material.
The location of the release of the lipophilic therapeutic agent L lipophilic is either the location of administration (in this case, L hydrophilic and L lipophilic are generally identical) or another site in the body of the human/animal subject, in particular when the droplets released from the material are carried away by the physiological fluid (interstitial fluid, lymph fluid, blood) to another site. Quite obviously, the location of the release of the lipophilic therapeutic agent also depends on the physical and chemical properties:
on the zone of administration of the material, in particular on the density of tissues and on the presence or absence of physiological barriers, and on the nature and the physical and chemical properties of the lipophilic therapeutic agent itself. Thus, when more than one lipophilic therapeutic agent is used in the material, each lipophilic therapeutic agent has a location of release that is specific to itself.
It is possible in particular, to modulate L Lipophilic by using in the material a polyalkoxylated co-surfactant comprising a grafted biological targeting ligand, which will enable the possibility of the droplets, and therefore the lipophilic therapeutic agent, to be directed to the desired target.
A number of embodiments of the use as a medicinal product of the material according to the invention comprising a hydrophilic therapeutic agent and a lipophilic therapeutic agent may be envisaged.
For example, one of the therapeutic agents may be a pharmaceutical active ingredient for the treatment of the disease being targetted, and the other may be a therapeutic agent that provides the ability to reduce the side effects, particularly those associated with the said pharmaceutical active ingredient.
A material according to the invention in which the hydrophilic therapeutic agent is a wound healing, antibacterial or anti inflammatory agent and the lipophilic therapeutic agent is an anti cancer agent, may in particular be used for the treatment post-resection of a tumour. This material is applied after a tumour resection operation on the site of resection of the tumour.
The healing, antibacterial or anti-inflammatory hydrophilic therapeutic agent is rapidly released in order to decrease the side effects of the resection and to promote the healing process.
The anti cancer lipophilic therapeutic agent is released later, generally during the first hours following the application of the material, and treats the clusters of remaining tumoral cells which have not been excised. It is actually often difficult to completely clear out the whole of the tumour during resection. The material thus provides for a comprehensive treatment of the tumoral area.
The droplets comprising the anti cancer lipophilic agents of the dispersed phase may also reach and join in with the lymphatic and blood circulation and act to treat the possible cancer cells that may be circulating in the circulatory system and serve as the source of metastases.
In particular, the co-surfactant of the material may include a biological targeting ligand for targeting the cancer cells in order to be able to more efficiently target the cancer cells.
Furthermore, a material according to the invention in which the hydrophilic therapeutic agent is an agent stimulating the immune system and the lipophilic therapeutic agent is an anti cancer agent, may notably be used for treatment of a tumour after cryogenic treatments.
Cryogenic treatment for tumour consists of the injection of a cryogenic liquid into a tumour by means of a syringe. The tumoral cells are killed with this treatment and remain inside the body of the treated subject.
The aforementioned material may increase the efficacy of the treatment. The hydrophilic agent that stimulates the immune system is rapidly released in order to activate the immune system and the lipophilic anti cancer agent is released later on, and acts to enable the elimination of the tumour cells that are still alive. There again, the droplets comprising the anti cancer lipophilic agent of the dispersed phase may reach and join in with the lymphatic and blood circulation and act to treat the possible cancer cells that may be circulating in the circulatory system and serve as the source of metastases. In addition, the co-surfactant of the material may include a biological targeting ligand for targeting the cancer cells in order to be able to more efficiently target the cancer cells.
The invention shall be described in more detail by means of examples and accompanying figures, which show the following:
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 shows a diagram illustrating the positioning of the surfactant having the formula (I) in which v and w represent 1 and the droplets of the material according to the invention.
FIG. 2 shows a diagram illustrating the positioning of the surfactant having the formula (I) in which and v and w represent 2 and the droplets of the material according to the invention.
FIG. 3 shows photographs of the materials described in the Example 1 obtained with the emulsions 1 and 2 and comprising the dispersed oily phase of 1%, 5%, 15% or 23%.
FIG. 4 shows photographs of a mixture (material in the Example 1 and aqueous solution of Phosphate Buffer Saline—PBS) immediately after the addition of PBS, and after 5 months of storage.
FIG. 5 shows the results of analysis by DLS (Dynamic Light Scattering), that is, the normalised intensity in % as a function of the size in nm, of the emulsion 1 (solid line) of the material according to the invention (solid line/dotted broken line) and of the emulsion obtained after cleavage of the disulfide function of the material (dotted line).
FIG. 6 shows the percentage loss of surfactant C 17 H 35 —CO—NH—[(CH 2 ) 2 —O] 100 —(CH 2 ) 2 —NH-FITC outside of the droplets of the emulsion 3 A 2 =NH (diamonds, solid line) or of surfactant C 17 H 35 —CO—O—[(CH 2 ) 2 —O] 100 —(CH 2 ) 2 —NH-FITC outside of the droplets of the emulsion 3 A 2 =O (squares, dotted line) as a function of time in hours.
FIG. 7 shows photographs of the materials described in the Example 7: A) the emulsion of droplets of LNP-SPDP [lipid based nanoparticles—N-succinimidyl-3(2-pyridyldithio)propionate]; B) the gel formed after addition of PEG dithiol [poly(ethylene glycol) dithiol]; C) suspension of droplets of LNP-SH obtained after addition of DTT (Dithiothreitol).
FIG. 8 shows photographs of the materials described in the Example 9 before and after irradiation.
DESCRIPTION OF PREFERRED EMBODIMENTS
Examples
Example 1
Preparation of a Material Including a Surfactant Having the Formula (I) Including a G Group Comprising a Reversible Cleavable Function
Preparation of a Surfactant Having the Formula (LII)
A surfactant having the formula (LII) wherein:
L 2 is fatty acid containing 18 carbon atoms (stearic acid); H 2 is a poly(ethylene oxide) comprising 100 units of ethylene oxide; G 2 represents a group —S—S-pyridinyl; X 2 represents —NH—; Y 2 represents —CH 2 —CH 2 —NH—CO—CH 2 —CH 2 —
was prepared by following the reaction scheme as follows:
Synthesis of the Compound (B)
The stearic acid (2 g; 0.6 mmol) and Benzotriazole-1-yl-oxy-tris-(dimethylamino)-phosphonium hexafluorophosphate (BOP) (265.2 mg, 0.6 mmol) were dissolved in CH 2 Cl 2 (15 mL). After 10 minutes of stirring, BocNH-PEG100-NH 2 (MW: 4928, 2 g, 0.4 mmol) (compound (A)) and diisopropylethylamine (DIEA) (104.5 mL, 0.6 mmol) were added to the reaction medium. The disappearance of the starting amine was verified by means of thin layer chromatography (TLC) (CH 2 Cl 2 /MeOH). After stirring for 2 hours, the product was precipitated in cold ether, dissolved in a little water and then dialysed against Milli Q water (cut off 1000). The solution was then recovered and the water was removed either by means of evaporation (ethanol as azeotrope) or by means of lyophilisation, in order to provide 1.5 g of compound (B) (white powder), that is a yield of 70%.
TLC (CH 2 Cl 2 /MeOH 9/1): Rf=0.5
1 H NMR (300 MHz; CDCl3): d: 0.87 (t; J=6.5 Hz; 3H; C H 3 —CH 2 ); 1.24 (m; 28H; 14C H 2 ); 1.44 (s; 9H; C(C H 3 ) 3 ); 1.67 (quin; 2H; C H 2 —CH 2 —CONH); 2.42 (t; J=7.5 Hz; 2H; C H 2 —CONH); 3.3 (t; J=5.0 Hz; 2H; BocNH—C H 2 ); 3.45-3.8 (m; 362H; ×C H 2 (PEG). CH 2 CONH—C H 2 )
Synthesis of the Compound (C)
The compound (B) (1.5 g, 0.29 mmol) was dissolved in 10 mL of dichloromethane and 4 mL of trifluoroacetic acid (TFA). The conversion of compound (C) was monitored by TLC (ninhydrin developer). After stirring for 1 hour, the solvent was evaporated by means of coevaporation with toluene (which eliminates the TFA). The product was dried under vacuum in order to provide 1.3 g of compound (C) (white powder), that is a yield of 86.7%.
TLC (CH 2 Cl 2 /MeOH 9/1): Rf=0.27
1 H NMR (300 MHz; CDCl3): d: 0.87 (t; J=6.5 Hz; 3H; C H 3 —CH 2 ); 1.24 (m; 28H; 14C H 2 ); 1.60 (quin; 2H; CH 2 —CH 2 —CONH); 2.15 (t; J=7.5 Hz; 2H; C H 2 —CONH); 3.17 (bt; 2H; C H 2 —NH 3 + ); 3.4 (m; 2H; CH 2 CONH—C H 2 ); 3.5-3.8 (m; 360H; ×C H 2 (PEG)); 6.14 (bs; 1H; N H CO); 7.9 (bs; 2H; N H 2 /N H 3 + )
Synthesis of the Surfactant (LII)
Under argon, the compound (C) (0.5 g, 0.1 mmol) and diisopropylethylamine, DIEA (52 mL; 0.3 mmol) were dissolved in dichloromethane (10 mL). After 5 minutes of stirring Succinimidyl 3-(2-pyridyldithio)propionate (SPDP) (93 mg, 0.3 mmol) was added into the reaction medium. The disappearance of the amine was monitored by TLC (CH 2 Cl 2 /MeOH 9/1). After 1 hour of reaction, the product was precipitated twice in ether in order to provide after filtration 400 mg of surfactant (LII) (yellowish powder) that is a yield of 76%
TLC (CH 2 Cl 2 /MeOH 9/1): Rf=0.42
1H NMR (300 MHz; CDCl3): d: 0.88 (t; J=6.5 Hz; 3H; C H 3 —CH 2 ); 1.25 (m; 28H; 14C H 2 ); 1.63 (quin; 2H; C H 2 —CH 2 —CONH); 2.17 (t; J=7.5 Hz; 2H; C H 2 —CONH); 2.62 (t; J=7 Hz; 2H; C H 2 —SS); 3.09 (t; J=7 Hz; 2H; NHCO—C H 2 —CH 2 —SS); 3.42 (m; 2H; C H 2 —NHCO); 3.48-3.8 (m; 360H; ×C H 2 (PEG); C H 2 —NHCO); 6.11 (bt; 1H; NH); 6.79 (bt; 1H; NH); 7.11 (m; 1H; CHpyr); 7.67 (m; 2H; 2CHpyr); 8.49 (m; 1H; CHpyr)
Preparation of Emulsions 2 Comprising a Surfactant Having the Formula (LII)
The emulsions 2 were prepared by following the procedures described in the document WO 2010/018223 with the compositions shown in the Table 1, the complete dissolution of Myrj S40 and the surfactant having the formula (LII) with the need to heat the solution to 55° C. and by mixing and then emulsifying the aqueous and oily phases by means of sonication in accordance with the parameters described in the Table 2.
TABLE 1
Compositions of the Emulsions 2
Emul-
Emul-
Emul-
Emul-
sion
sion
sion
sion
Supplier
2 (20%)
2 (15%)
2 (10%)
2 (5%)
Soybean Oil (mg)
CRODA
68
Suppocire ® NB (mg)
Gattefossé
272
Lecithin (mg)
Lipoïd
65
PBS Water 1X (mL)
—
2.5
Myrj S40 (mg)
CRODA
276
293
310
328
surfactant (LII) (mg)
—
69
52
35
17
m (surfactant (LII))/
—
20
15
10
5
[m (surfactant
(LII) + m (Myrj
S40)) * (%)
% dispersed phase
23
Dil (mg)
4
* Ratio of the mass of surfactant having the formula (LII) over the mass of the ensemble (surfactant having the formula (LII)/Myrj S40) (in %). The mass of the ensemble (surfactant having the formula (LII)/Myrj S40) is 345 mg for all the emulsions.
TABLE 2
Sonication Parameters used
Volume of
Probe
Power
Sonication
Pulse
the batch
(φ)
Pmax
Time
on/off
3.25 mL
3 mm
28%
5 min
10 s/30 s
In order to enable better visual observation of the stability and the formation of the material subsequently formed, the droplets were stained by incorporation of a fluorophore, namely 3,3-dioctadecylindocarbocyanine (Dil) (4 mg/emulsion)).
Preparation of Emulsions 1 Comprising a Surfactant Having the Formula (LI)
The emulsions 1 comprising a surfactant having the formula (LI) of the following formula:
was obtained from the emulasion 2 prepared here above.
The thiol group of the surfactant (LI) was obtained by deprotection of the —S—S-pyridinyl functions with a reducing agent dithiothreitol (DTT).
For example, for the emulsion 1 (20%) obtained from the emulsion 2 (20%) mentioned above, 1.5 mL were taken of the emulsion 2 (20%) to which was added 23 mg of DTT (which is 20 molar equivalents/SSpyr). The reaction was then left to be stirred (moving stir plate) for 2 hours
Preparation of the Material According to the Invention from the Emulsions 1 and 2
The emulsions 1 and 2 prepared above were purified by means of dialysis against PBS 1× (MW Cut off 12000-14000 Da, 500 mL; 24 hours).
The size of droplets of the emulsions was determined through measurement by dynamic light scattering, DLS (Zeta Sizer Nano ZS, Malvern). The emulsions have a similar size distribution with sizes of droplet of 65 nm with a polydispersity index of 0.112.
The emulsions have optionally been diluted by the addition of aqueous phase, in order to obtain dispersed oily phase in percentages of 1%, 5%, 15% or 23%.
In order to form the material according to the invention, the emulsions 1 and 2 having:
the same proportion of dispersed phase, and ratios of the mass of surfactant having the formula (LII) over the mass of the ensemble (surfactant having the formula (LII)/Myrj S40), and of the mass of surfactant having the formula (LI) over the mass of the ensemble (surfactant having the formula (LI)/Myrj S40), which are identical,
have been used.
An equivalent volume of emulsions 1 and 2 was mixed, the solution was then stirred and a homogeneous material formed rapidly after 2 to 4 minutes of stirring. A disulfide bond was formed between the surfactants having the formula (LI) of the emulsion 1 and (LII) of the emulsion 2 in order to form the surfactant having the following formula (I):
This surfactant having the formula (I) (wherein G represents —SS—) ensures the covalent bonding between the droplets of the material formed.
Several tests were carried out with various different percentages of the dispersed oily phase (1%, 5%, 15% or 23%).
The appended FIG. 3 shows four pictures of the materials obtained with the emulsions 1 and 2 and comprising dispersed oily phases of 1%, 5%, 15% or 23%. No matter what the proportions of dispersed phases of the emulsions 1 and 2 are, the material is formed rapidly.
Where the dispersed phase is greater than 15%, upon bringing about contacting of the two emulsions, the procedure carried out was as follows in order to obtain a homogenous and uniform material:
Vortexing Heating in order to re-fluidify Vortexing Heating in order to re-fluidify Vortexing Letting stand Influence of the Ratio m (Surfactant (LII))/[m (Surfactant (LII)+m (Myrj S40))
Tests for preparation of the material according to the invention were carried out based on emulsions having ratios m (surfactant (LII))/[m (surfactant (LII)+m (Myrj S40)) that were different (the ratios of the mass of surfactant having the formula (LII) over the mass of the ensemble (surfactant having the formula (LII)/Myrj S40) of the emulsion 2, and of the mass of surfactant having the formula (LI) over the mass of the ensemble (surfactant having the formula (LI)/Myrj S40) of the emulsion 1 being always identical) in order to obtain materials having a ratio m (surfactant (I))/[m (surfactant (I)+m (Myrj S40)) that are different, namely 5%, 10%, 15% and 20% as mentioned in the Table 1. The material is formed more easily when the said ratio is greater than or equal to 15%.
Preparation of the Material According to the Invention from Emulsions 1 and 2 Comprising Droplets of Larger Size (125 nm)
The preparation of an emulsion 2 as described here above was reproduced with the same components, but by ensuring varying of the proportions thereof as indicated in the following Table 3 and with identical sonication parameters.
TABLE 3
Compositions of the Emulsion 2 (20%) bis
Emulsion 2 (20%) bis
Soybean Oil (mg)
150
Suppocire ® NB (mg)
450
Lecithin (mg)
45
PBS Water 1 X (mL)
2.39
Myrj S40 (mg)
172
surfactant (LII) (mg)
43
m (surfactant (LII))/
20
[m (surfactant (LII) +
m (Myrj S40)) * (%)
Dil (mg)
4
The size of droplets of the emulsion 2 (20%) bis obtained was measured by means of DLS (Zeta Sizer Nano ZS, Malvern). They have a size distribution with a mean of 125 nm and a polydispersity index of 0.13.
There again, the emulsion 1 (20%) bis comprising a surfactant having the formula (LI) of the following formula:
was obtained from the emulsion 2 (20%) bis prepared here above as follows:
1.625 mL was taken of the emulsion 2 (20%) bis to which was added 16 mg of DTT (that is 22 molar eq/SSpyr) in order to form the emulsion 1 (20%) bis comprising the surfactant having the formula (LI). The reaction was left to be stirred (moving stir plate) for a period of 15 hours.
Thereafter, the emulsion 1 (20%) bis and the emulsion 2 (20%) bis were set to be dialysed against PBS 1×2 times (MW Cut off 12000-14 000 Da; 500 mL; 24 hours). The material was then prepared from the emulsion 1 (20%) bis and the emulsion 2 (20%) bis by following the same protocol as described here above.
This experiment shows that it is possible to prepare a material comprising droplets of different sizes.
Example 2
Test of Resistance to Dilution of the Material Based on Example 1
The material described in the Example 1 prepared from emulsions 1 and 2 both of which having 23% of dispersed phase and in which m (compound (I))/[m (compound (I)+m (Myrj S40))=20% was recovered with a spatula, then transferred to a pill container, thereafter 1 mL of an aqueous solution of PBS (1×) was added thereto.
The resistance to dilution of the material is total, the material retains its structure even after dilution. The density of the material is less than that of water (the float material). If a strong agitation (that is to say at 3000 rpm/min on a vortex device Vortex Top-Mix 3, Fischer Scientific) is applied, the material gets fragmented into small pieces and then ends up getting re-constituted through the process of creaming after a period of about 6 hours.
Example 3
Tests of Stability the Material Based on Example 1
The material described in Example 1 prepared from emulsions 1 and 2 both of which having 23% of dispersed phase and in which m (compound (I))/[m (compound (I)+m (Myrj S40))=20% was recovered with a spatula, then transferred to a pill bottle, thereafter 1 mL of an aqueous solution of PBS (1×) was added thereto. Subsequently, the mixture obtained was stored for a period of 5 months at ambient temperature (25° C.). the photographs included in the FIG. 4 show that the colouration of the PBS solution remained faint even after 5 months of storage, which demonstrates that the droplets of the material remain bonded to each other and that the material according to the invention is stable.
The test had been repeated by replacing the aqueous solution of PBS with physiological serum (foetal calf serum) (Sigma Aldrich). The material remains intact in this medium for a period of 16 hours at 37° C. or 50° C., which demonstrates the stability thereof in physiological media.
Example 4
Cleavage of the G Group of the Surfactant Having the Formula (I) of the Material Described in Example 1
The material described in the Example 1 prepared from emulsions 1 and 2 both of which having 23% of dispersed phase and in which m (compound (I))/[m (compound (I)+m (Myrj S40))=20% was used.
The disulfide group of the surfactant having the formula (I) of the material was cleaved with a disulfide bond reducing agent, dithiothreitol or Cleland's reagent.
Then 10 mg of DTT (dithiothreitol or Cleland's reagent) was added in order to reduce the intra-particle disulphide bonds over the entire material. The occurrence then observed was the immediate dissolution of the material, that is to say a disaggregation of the droplets which were distributed throughout the entirety of the aqueous phase of the medium. The size of the droplets present in the solution once the cleavage of the disulfide bonds had taken place, is identical to that of the droplets of the emulsions 1 and 2 (prior to creation of the covalent disulfide bonds.)
The colloidal nature of the emulsion thus obtained was verified by means of DLS (dynamic light scattering) (Zeta Sizer Nano ZS, Malvern). The size of the suspended droplets is substantially the same for the emulsion 1 and for the emulsion obtained after cleavage of the disulfide function of the material, whereas the size of the suspended aggregates (clusters of the droplets forming the material) is much greater ( FIG. 5 ).
Example 5
Emulsions Comprising a Surfactant Having the Formula (L)
Demonstration of Evidence of the Ability to Introduce More of the Surfactants Having the Formula (L) in an Emulsion than Surfactants of the DSPE-PEG Type
Preparation of a Surfactant Having the Formula (L) Wherein R 2 Represents C 17 H 35 , A 2 Represents O, n Represents 100 and φ Represents a Succinimidyl Group
A surfactant having the formula (L) wherein R 2 represents C 17 H 35 , A 2 represents O, n represents 100 and φ represents a succinimidyl group
was prepared by following the reaction scheme as follows:
In an anhydrous flask and under argon, Myrj S59 (2.345 g, 0.5 mmol) was dissolved in dry dioxane (15 mL) with heating so as to obtain a clear solution. Then, the reaction medium was brought back to ambient temperature (25° C.), before the addition of disuccinimidyl carbonate (0.77 g; 3 mmol) dissolved in dry acetone (3 mL). The 4-dimethylaminopyridine (0.37 g; 3 mmol), that was previously dissolved in dry acetone (3 mL) was then added slowly and under the effect of stirring to the reaction medium. The reaction was monitored by using TLC (CH 3 Cl/MeOH) 5/1. After a period of 5 hours under the effect of stirring at ambient temperature, the product was precipitated in cold diethyl ether (100 mL), and the solid thus obtained was centrifuged in order to be isolated, then redissolved in acetone, precipitated again, and this was repeated several times. The expected surfactant having the formula (L) was dried under vacuum, so as to be obtained in the form of a white powder (72% yield).
1 H NMR (300 MHz; MeOD): d: 0.87 (t; J=6.5 Hz; 3H; C H 3 —CH 2 ); 1.25 (m; 28H; 14C H 2 ); 1.61 (quin; J=7.5 Hz; 2H; C H 2 —CH 2 —COO); 2.32 (t; J=7.5 Hz; 2H; C H 2 —COO); 2.85 (s, 4H, CH 2 NHS); 3.57-3.95 (m; 362H; ×C H 2 (PEG); 4.22 (t; J=5 Hz; 2H; C H 2 —OOC—CH 2 )
Preparation of an Emulsion 3 Comprising the Surfactant Having the Formula (L) and an Emulsion Comprising a Surfactant Derived from DSPE-PEG (by Way of a Comparison)
The emulsions in which the droplets comprise on the surface the group that may be functionalised N-hydroxysuccinimide (NHS) ester were prepared These emulsions comprise either the surfactant having the formula (L) as prepared here above (molecular weight of about 5000 g mol −1 ), or a surfactant derived from DSPE-PEG-NHS (molecular weight: 3400 g mol −1 ) and they were prepared by following the procedures described in the document WO 2010/018223 with the compositions respectively indicated in the Tables 4 and 5.
DSPE-PEG-NHS (with n=75) from NOF (molecular weight: 3400 g mol −1 )
TABLE 4
Composition of the emulsion 3 comprising
a surfactant having the formula (L)
% of surfactant having the formula (L) by mass/
total mass of the emulsion
4.5%
8.0%
12.0%
15.0%
30.0%
Purified Soybean
85
85
85
85
85
Oil (mg)
Suppocire NC (mg)
255
255
255
255
255
Lecithin Lipoid
65
65
65
65
65
s75 (mg)
Myrj 52 (mg)
314.8
291.4
264.5
244.4
184.1
surfactant having
71.3
126.8
190.1
237.7
380.3
the formula (L) (mg)
PBS (μL)
1208.9
1176.9
1140.3
1112.9
1030.6
TABLE 5
Composition of the Comparative Emulsion
Comprising DSPE-PEG-NHS
% of DSPE-PEG-NHS by mass/
total mass of the emulsion
3.0%
4.5%
Purified Soybean Oil (mg)
85
85
Suppocire NC (mg)
255
255
Lecithin Lipoid s75 (mg)
65
65
Myrj 52 (mg)
322.4
314.8
DSPE-PEG-NHS (mg)
44.1
58.8
PBS (μL)
771.5
778.6
The preparation of emulsions comprising the surfactant having the formula (L) was possible for all the mass percentages of surfactant having the formula (L) tested (up to 30% by mass of surfactant/total mass tested). In contrast, the preparation of emulsions comprising DSPE-PEG-NHS was not possible beyond 4.5% by mass of DSPE-PEG-NHS because the medium became too viscous to be formulated.
It is therefore possible to prepare an emulsion with more of the surfactant having the formula (L) than the surfactant DSPE-PEG-NHS. Thus, the droplets of an emulsion prepared with the surfactant having the formula (L) have more NHS functions on the surface.
Grafting of an Agent of Interest on the Surface of the Emulsions Prepared Above
The droplets of the emulsions as prepared here above have on the surface NHS groups that may be functionalised by agents of interest having an amino group (NH 2 ). In the example here below, a —NH 2 Fluorophore (5-FAM cadaverine) was coupled to the surface of the droplets.
For each of the emulsions, volumes of emulsions were used such that the number of NHS function per liter of emulsion was 4 μmol, that is to say, a volume of emulsion as follows:
TABLE 6
Volume of Emulsion used for the Functionalisation
by 5-FAM Cadaverine
% of surfactant having the
formula (L) by mass/total
Volume of emulsion
mass of the emulsion
used (μL)
4.5
864.8
8
488.5
12
324.9
15
260
The volume of emulsion indicated in the Table 6 here above was mixed with 3.85 mg of 1-Ethyl-3-(3-dimethylaminopropyl)carbodiimide, EDC (5 eq. that is 20 μmol) and 10.86 mg of sulfo-NHS (50 μmol) for 15 minutes at ambient temperature, protected from light (pH=6). 15 .μL of 5-FAM cadaverine at 0.40 μM, that is 6 μMoles (1.5 eq at pH=7.4) were added for 2 hours at ambient temperature, protected from light (sample).
Blank control samples were prepared by replicating these experiments by mixing the volume of emulsion indicated in the Table 6 here above with 3.85 mg of EDC (5 eq. that is 20 μmol) and 10.86 mg of sulfo-NHS (50 μmol) for 15 minutes at ambient temperature, protected from light (pH=6). (No further addition of 5-FAM cadaverine)
The experiment was also replicated with the emulsion prepared from the surfactant DSPE-PEG-NHS.
The emulsions obtained were dialysed against PBS 1× sterile (membrane Da=12 400) for a period of 16 hours (with change of the dialysis water 2×).
The amount of 5-FAM cadaverine grafted to the surface of the droplets was then assayed by absorbance spectrophotometry (Cary 300, Varian) and confirmed by means of spectrofluorimetry (LS50B, Perkin-Elmer). The possible signal of diffusion of nanoparticles was corrected by subtracting it from the negative blank control samples incubated under the same conditions but without 5-FAM-cadaverine. The grafting yields (ratio between the number of fluorophores grafted to the surface and the number of NHS functions introduced) are summarised in the Table 7.
TABLE 7
yields of grafting of the 5-FAM cadaverine on the functionalised
emulsions comprising either a surfactant DSPE-PEG-NHS,
or a surfactant having the formula (L)
Size of
Droplets
% of surfactant by mass/
Grafting
(nm)
Surfactant
total mass of the emulsion
Yield (%)
50
DSPE-PEG-NHS
4.5
10
50
surfactant having
4.5
10
50
the formula (L)
8
57
50
12
51
50
15
58
By using the emulsions comprising a surfactant having the formula (L) including more of surface NHS functions (% of surfactant by mass/higher total mass of the emulsion), a better grafting yield was obtained. The number of 5-FAM-cadaverine (fluorophore-agent of interest) grafted in a covalent manner to the surface of the droplets is thus greater when the surfactant having the formula (L) is used.
Comparison of Leakage of Surfactants Having the Formula L where A 2 Represents NH or O
The emulsions comprising surfactants having the formula (L) where A 2 represents NH or O and grafted with fluorescein isothiocyanate (FITC) (Agent of interest) were prepared.
Preparation of a Surfactant Having the Formula (L) Wherein R 2 Represents C 17 H 35 , A 2 Represents O, n Represents 100 and φ Represents an Amino Group on which Fluorescein Isothiocyanate, FITC has been Grafted
The following reaction scheme was followed:
Synthesis of
Under argon Myrj S100 anhydrous (10 g; 1.98 mmol) and triethylamine (0.8 mL; 5.94 mmol) was dissolved in dichloromethane stabilised on amylene and anhydrous (50 mL). After 5 minutes under stirring, the temperature was lowered to 0° C. and then mesyl chloride (0.46 mL; 5.94 mmol) was added to the reaction medium. After a period of 24 hours at ambient temperature, the excess amount of mesyl chloride was cold quenched with ethanol. After 5 minutes of stirring, the solvent was evaporated under vacuum. The product was then chromatographed on a silica column with a gradient of dichloromethane/methanol (9.5/0.5 to 9/1) as eluent, in order to obtain a white solid with a yield of 23%.
1H NMR (300 MHz; CDCl3): d: 0.84 (t; J=6.5 Hz; 3H; C H 3 —CH 2 ); 1.21 (m; 28H; 14C H 2 ); 1.57 (quin; J=7.5 Hz; 2H; C H 2 —CH 2 —COO); 2.28 (t; J=7.5 Hz; 2H; C H 2 —COO); 3.04 (s; 3H; C H 3 —S); 3.6-3.8 (m; 360H; × CH 2 (PEG)); 4.18 (t; J=5 Hz; 2H; C H 2 —OOC—CH 2 ); 4.33 (m; 2H; C H 2 —OMs)
Synthesis of
The compound from the previous step (2.33 g, 0.45 mmol) and sodium azide (0.29 g, 4.54 mmol) were caused to be suspended in acetonitrile (23.3 mL). The mixture was brought to 85° C. and maintained for a period of 2 days. The solvent was evaporated, the reaction mixture was dissolved in dichloromethane and the NaN 3 in suspension was filtered. The dichloromethane was evaporated under vacuum in order to obtain the desired compound in the form of a white powder (93% yield).
1H NMR (300 MHz; CDCl3): d: 0.88 (t; J=6.5 Hz; 3H; C H 3 —CH 2 ); 1.25 (m; 28H; 14C H 2 ); 1.6 (quin; J=7.5 Hz; 2H; C H 2 —CH 2 —COO); 2.32 (t; J=7.5 Hz; 2H; C H 2 —COO); 3.4 (m; 2H; C H 2 —N 3 ); 3.6-3.8 (m; 360H; ×C H 2 (PEG)); 4.22 (t; J=5 Hz; 2H; C H 2 —OOC—CH 2 )
Synthesis of
The compound from the previous step (2.15 g, 0.42 mmol) and triphenylphosphine (560 mg, 2.12 mmol) were dissolved in tetrahydrofuran, THF (20 mL). After 10 minutes of stirring, 0.4 mL of water was added to the reaction medium. During the course of the reaction, the appearance of the amine was monitored by TLC (CH 2 Cl 2 /MeOH 9/1) with ninhydrin as a developer. After a period of 2 days under stirring, the solvent was evaporated and the product was taken up in hexane and extracted with methanol. The methanol phases were combined and evaporated to dryness. The product was taken up in water, dialysed (pH 6-7) and then lyophilised in order to obtain the expected compound in the form of a white powder (90% yield).
TLC (CH 2 Cl 2 /MeOH 9/1): Rf=0.27
1H NMR (300 MHz; CDCl3): d: 0.88 (t; J=6.5 Hz; 3H; C H 3 —CH 2 ); 1.25 (m; 28H; 14C H 2 ); 1.6 (quin; J=7.5 Hz; 2H; C H 2 —CH 2 —COO); 2.32 (t; J=7.5 Hz; 2H; CH 2 —OOC); 2.88 (t. J=5 Hz; 2H; C H 2 —NH 2 ); 3.53 (t; J=5 Hz; 2H; OC H 2 —CH 2 —NH 2 ); 3.6-3.8 (m; 360H; ×C H 2 (PEG)); 4.22 (t; J=5 Hz; 2H; C H 2 —OOC—CH 2 )
Synthesis of
In an anhydrous flask and under argon, the compound from the previous step (100 mg, 0.02 mmol) was dissolved in dichloromethane (2 mL) and dimethylformamide, DMF (0.1 mL). After 3 minutes under stirring, the fluorescein isothiocyanate, FITC (isomer 1 at 90%) (15.4 mg; 0.04 mmol) and diisopropylethylamine, DIEA (7 mL; 0.04 mmol) were added therein. The reaction was monitored by TLC (CH 2 Cl 2 /MeOH/AcOH) 9/1/0.1. After a period of 10 minutes under stirring, the solvent was evaporated under vacuum, the product was precipitated in ether and the solid thus obtained was washed with ethyl acetate. The expected compound was obtained in the form of a yellow powder (76% yield).
TLC (CH 2 Cl 2 /MeOH 9/1): Rf=0.37
1 H NMR (300 MHz; MeOD): d: 0.91 (t; J=6.5 Hz; 3H; C H 3 —CH 2 ); 1.30 (m; 28H; 14C H 2 ); 1.62 (quin; J=7.5 Hz; 2H; C H 2 —CH 2 —COO); 2.35 (t; J=7.5 Hz; 2H; C H 2 —COO); 3.55-3.9 (m; 362H; ×C H 2 (PEG); C H 2 —NHFITC); 4.22 (t; J=5 Hz; 2H; C H 2 —OOC—CH 2 ); 6.6 (dd; J=2 Hz; J=8.5 Hz; 2H; 2CH aromatic ); 6.7 (d; J=2 Hz; 2H; 2CH aromatic ); 6.82 (d; J=8.5 Hz; 2H; 2CH aromatic ); 7.2 (d; J=8 Hz. 1H; aromatic CH); 7.86 (d; J=8 Hz. 1H; aromatic C H ); 8.21 (s; 1H; aromatic C H )
Preparation of a Surfactant Having the Formula (L) Wherein R 2 Represents C 17 H 35 , A 2 Represents NH, n Represents 100 and φ Represents an Amino Group on which Fluorescein Isothiocyanate, FITC has been Grafted
The synthesis was carried out using the compound (C) from the Example 1 having the formula according to the following reaction scheme:
In an anhydrous flask and under argon, the compound (C) (250 mg; 0.05 mmol) was dissolved in dichloromethane (5 mL) and dimethylformamide, DMF (0.2 mL). After 3 minutes under stirring, the fluorescein isothiocyanate, FITC (isomer 1 to 90%) (30 mg; 0.075 mmol) and diisopropylethylamine, DIEA (25 mL, 0.15 mmol) were added therein. The reaction was monitored by TLC (CH 2 Cl 2 /MeOH/AcOH) 9/1/0.1. After a period of 10 minutes under stirring, the solvent was evaporated under vacuum, the product was precipitated in ether and the solid thus obtained was washed with ethyl acetate. The solid was taken up in water at pH 7.
After dialysis (pore 1000 Da), the solution of the expected compound was lyophilised and the expected compound (200 mg) was obtained in the form of an orange powder (yield 76%).
TLC (CH 2 Cl 2 /MeOH 9/1): Rf=0.37
1 H NMR (300 MHz; MeOD): d: 0.91 (t; J=6.5 Hz; 3H; C H 3 —CH 2 ); 1.31 (m; 28H; 14C H 2 ); 1.62 (quin; J=7.5 Hz; 2H; C H 2 —CH 2 —CONH); 2.2 (t; J=7.5 Hz; 2H; C H 2 —CONH); 3.41 (m; 2H; C H 2 —NHCO); 3.55-3.9 (m; 364H; ×C H 2 (PEG); C H 2 —NH-FITC); 6.56 (m; J=9 Hz; J=2.5 Hz; 4H; 4C H aromatic ); 7.15 (d; J=9 Hz; 2H; 2C H aromatic ); 7.2 (d; J=8.5 Hz; 1H; aromatic C H ); 7.76 (dd; J=8.5 Hz; J=2.5 Hz; 1H; aroma C H ); 7.87 (d; J=2.5 Hz; 1H; aromatic C H )
Preparation of Emulsions or 3 Comprising Either the Surfactant Having the Formula (L) Wherein A 2 Represents NH or the Surfactant Having the Formula (L) Wherein A 2 Represents O
The emulsions 3 functionalised by the group FITC comprising the components indicated in the Table 8 here below were prepared by following the procedures described in the document WO 2010/018223.
TABLE 8
Composition of Emulsion 3 A 2 = NH and Emulsion 3 A 2 = O
Emulsion 3
Emulsion 3
A 2 = NH
A 2 = O
Purified Soybean Oil (mg)
85
85
Suppocire NC (mg)
255
255
Lecithin Lipoid s75 (mg)
65
65
Myrj S40 (mg)
328
328
PBS (uL)
771.5
778.6
C 17 H 35 —CO—NH—[(CH 2 ) 2 —O] 100 —(CH 2 ) 2 —NH-FITC (mg)
17
—
C 17 H 35 —CO—O—[(CH 2 ) 2 —O] 100 —(CH 2 ) 2 —NH-FITC(mg)
—
17
Emulsions comprising droplets of diameter 50 nm were obtained in each case.
Leakage of the Surfactants Out of the Droplets of the Emulsions 3 Formed
Analysis was carried out of the desorption of the surfactants during a dialysis period of 48 hours. The surfactants were quantified in the dialysate by measuring the absorbance at 490 nm (the surfactants in the dialysate correspond to those that have leaked out of droplets). The conditions of dialysis were as follows: 400 mL of emulsion 3 at 20% (w/w) in a “Quick dialyser”, then set to be dialysed in 400 mL of PBS. The dialysis lasted for a period of 120 hours. The leakage of surfactant (C 17 H 35 —CO—NH—[(CH 2 ) 2 —O] 100 —(CH 2 ) 2 —NH-FITC or C 17 H 35 —CO—O—[(CH 2 ) 2 —O] 100 —(CH 2 ) 2 —NH-FITC) was monitored by regularly taking a 300 ml sample of the dialysate. The results have been illustrated in the FIG. 6 .
Thus, after a 48 hour period of dialysis, it was found that 50% of the surfactant C 17 H 35 —CO—NH—[(CH 2 ) 2 —O] 100 —(CH 2 ) 2 —NH-FITC had leaked out of the droplets of the emulsion 3 A 2 =NH, whereas 70% of the surfactant C 17 H 35 CO—O—[(CH 2 ) 2 O] 100 —(CH 2 ) 2 NH-FITC had leaked out of the droplets of the emulsion 3 A 2 =O. The surfactant with A 2 =NH thus desorbs less of the droplets than the surfactant with A 2 =O.
Example 6
An Emulsion Comprising a Material Including a Surfactant Having the Formula (I) Comprising a G Group Including an Irreversible Cleavable Function
In this example use is made in the implementation of a homo-bifunctional compound to form the surfactant having the formula (I) that enables the generation of the covalent bonds between the droplets.
The droplets bearing at their surface a reactive primary amine function are brought to be reacted with a dialdehyde compound, glutaraldehyde, so as to form a Schiff base (imine), which is then reduced (reductive amination). The secondary amine formed then forms an irreversible covalent bond between the droplets.
More specifically, the reaction that is brought into play is of the type illustrated in the diagram here below:
An emulsion comprising droplets bearing at their surface a terminal primary amine group was prepared by following the operational procedure as in Example 1, with the components for the oily phase and aqueous phase, as detailed in the Table 9 here below. After purification, the emulsion LNP-NH2 obtained comprised 11% w/w of the dispersed phase.
To 1 mL of the emulsion thus obtained was added 0.28 .μL of 50% glutaraldehyde in water and these were allowed to react at ambient temperature for a period of 1 hour. Thereafter, 1 ml of emulsion was once again added therein and was then allowed to react for a period of 12 hours before adding 282 μL of sodium cyanoborohydride in 10 mM solution (NaCNBH 3 )
The formation in the reaction mixture of aggregates visible to the naked eye was observed. These aggregates may be isolated by gently pipetting from the tube the reaction mixture containing the droplets that were unreacted. A gel is obtained on the walls of the tube.
When the gel formed was brought to be contacted again with fresh phosphate buffer (Phosphate Buffered Saline PBS 1×), there was no dissolution due to the dilution observed, which serves as evidence demonstrating the existence of a chemical gel. If this gel is subjected to intense agitation, for example by means of vortexing, it is observed that the gel disintegrates into fine aggregates only to be reformed, after a period of rest of 1 hour and:30 min, on the surface of the buffer solution.
TABLE 9
Composition of the emulsion LNP-NH2
Mass (mg)
Lipid Phase
Aqueous Phase
Purified
Wax
Lecithin
SA-PEG(100)-NH 2
Soybean
Suppocire
Lipoid
Myrj ®
(Compound C as in
Oil
NC
s75
S40
Example 1)
PBS 1X
68
272
65
312
33
771.5
Example 7
Formation of a Gel from an Emulsion LNP-NH 2 LNP-SH and a Sulfo-SMCC Cross-Linker
In this example, use is made in the implementation of a cross-linker (Succinimidyl 4-(N-maleimidomethyl)cyclohexane-1-carboxylate, sulfo-SMCC) in order to generate a covalent bond between the droplets bearing the groups —NH 2 (LNP-NH2) on their surface and others bearing the groups —SH on their surface (LNP-SH) and to form a gel.
The reactions that are brought into play are illustrated in the diagram here below.
A. Preparation of an Emulsion of LNP-SH
The oily phase was prepared as in Example 1, by using the ingredients and proportions indicated in the Table 10 here below. A small amount of dichloromethane was added to improve the solubility in the oily phase, it was evaporated thereafter. A fluorophore (DiD) was added to the premix (80 ul, 10 mM in ethanol) in order to enable improved subsequent visual observation of the droplets.
TABLE 10A
Composition of the Emulsion LNP-SH
Mass (mg)
Lipid Phase
Purified
Wax
Lecithin
Aqueous Phase
Soybean
Suppocire
Lipoid
Myrj ®
SA CONH PEG100-
Oil
NC
s75
S40
SSpyr
PBS 1X
68
272
65
276
69
2500
The aqueous phase was prepared as in Example 1, by using the ingredients and proportions set forth in the Table 10A here below. The surfactant SA CONH PEG100-S-S-Pyr (surfactant LII in the Example 1) was added in an amount of up to 20% by mass relative to the total mass of surfactant LII. For the dissolution of surfactants, the mixture was heated to 55° C.
The emulsion was prepared by adding the aqueous phase obtained in the flask containing the oily phase (still hot at 45° C.), and then sonicating the mixture to 50° C. under the conditions indicated in the Table 2 above, but with a power Pmax of 30%.
Thereafter, 46 mg of DTT (dithiothreitol, that is 20 molar eq) was added to the suspension of LNP- SS-PYR and then the particle dispersion was stirred for a period of two hours on a moving stir plate so as to reduce the S—S-PYR functions in thiol form (—SH).
Finally, the LNP-SH were dialysed 2 times against PBS 1× (MW Cut off 12000-14000 Da; 500 mL; 24 hours). After dialysis, the LNP-SH droplets were filtered on filters of 0.2 μm.
B. Preparation of an Emulsion LNP-NH 2
The oily phase was prepared as previously described here above for the emulsion LNP-SH, using the same ingredients and proportions.
The aqueous phase was prepared as in Example 1, by using the ingredients and proportions set forth in the Table 10B here below. The surfactant SA CONH PEG100-NH 3 + TFA − (surfactant C in the Example 1) was added in an amount of up to 20% by mass relative to the total mass of surfactant C. For the dissolution of surfactants, the mixture was heated to 55° C.
TABLE 10B
Composition of the Emulsion LNP-NH2
Mass (mg)
Lipid Phase
Purified
Wax
Lecithin
Aqueous Phase
Soybean
Suppocire
Lipoid
Myrj ®
SA CONH PEG100-
Oil
NC
s75
S40
NH3 + TFA
PBS 1X
85
272
65
276
69
2500
The emulsion was prepared by adding the aqueous phase obtained in the flask containing the oily phase (still hot at 45° C.), and then sonicating the mixture to 50° C. under the conditions indicated in the previous example.
The emulsion LNP-NH 2 thus obtained was dialysed 2 times against PBS 1× (MW Cut off 12000-14000 Da; 500 mL; 24 hours). After dialysis, the LNP-NH2 droplets were filtered on filters of 0.2 microns.
A solution of Sulfo-SMCC (Succinimidyl 4-(N-maleimidomethyl)cyclohexane-1-carboxylate, Pierce, 0.87 mL, 4.58 mM, 4 μmol) was added to the dispersion of LNP-NH 3 + TFA − (0.1 mL, 0.4 μmol of amine functions). The mixture was stirred for a period of 3 hours on a moving stir plate. Then, purification by size exclusion column (Disposable PD-10, GE Healthcare) was carried out in order to eliminate the excess sulfo-SMCC. After purification by column, the fractions containing the droplets were collected.
C. Preparation of a Gel from LNP-SH et LNP-NH 2
In order to prepare the gel, the emulsion LNP-NH 2 obtained above was added to the emulsion LNP-SH (0.1 mL, 0.4 μmol of thiol functions). After reaction over a period of 2 hours with stirring, it was noted that there was formation of aggregates of gel that are insoluble water. groups
Example 8
Formation of Gel from LNP-SS-Pyr and Crosslinker SH-PEG-SH
An emulsion was prepared containing the surfactant SA CONH PEG 100 -SPDP (surfactant LII in the Example 1) with the composition indicated in the Table 11 here below, according to the protocol indicated in the previous example.
The emulsion obtained was purified by dialysis (molecular weight cut offs MWCO 12-14 kDa) against PBS and diluted in a manner so as to obtain a mass fraction of droplets of 20%.
TABLE 11
Composition of the Emulsion LNP-SPDP
Mass (mg)
Lipid Phase
Aqueous Phase
Purified
Wax
Lecithin
SA CONH PEG 100 -SPDP
Soybean
Suppocire
Lipoid
Myrj ®
(Compound LII as in
PBS
Oil
NC
s75
S40
Example 1)
1X
150
450
45
172
43
1140
A quantity of 500 .μL of this emulsion (100 mg of dispersed droplets) was brought to be reacted with 0.9 mg of poly(ethylene glycol) dithiol (average molecular weight 1000 Da) at ambient temperature with a thiol/SPDP ratio of 1:1 under moderate stirring. A gel began to form within a few minutes after the mixing of the reactants. The gel formed was destroyed by addition of an excess amount of DTT (dithiothreitol) in order to provide the droplets dispersed in the aqueous buffer. The photographs in FIG. 7 illustrate the changes in appearance of the initial LNP-SPDP formulation ( FIG. 7A ) after addition of PEG dithio ( FIG. 7B ) and after addition of DTT ( FIG. 7C ).
The study of the size of particles in the gel and then after destruction provides evidence demonstrating that the process did not alter the morphology of the droplets (see Table 12 here below).
TABLE 12
Physical and Chemical Properties
Hydrodynamic Diameter (nm)
Pdl
LNP-SPDP
128 ± 2
0.114 ± 0.001
(before gelling)
LNP-SH
135 ± 2
0.097 ± 0.013
(after gelling)
The principle of the formation and destruction of the gel is shown schematically in the schematic diagrams A and B here below.
Example 9
Formation of Gels by Irradiation
A. Preparation of an Emulsion of LNP-SH
The oily phase was prepared as in Example 1, by using the ingredients and proportions indicated in the Table 12 here below. A small amount of dichloromethane was added to improve the solubility in the oily phase, it was evaporated thereafter. A fluorophore (DiD) was added to the premix (80 ul, 10 mM in ethanol) in order to enable improved subsequent visual observation of the particles.
The aqueous phase was prepared as in Example 1, by using the ingredients and proportions set forth in the Table 12 here below. The surfactant SA CONH PEG100-S—S-Pyr (surfactant LII in the Example 1) was added in an amount of up to 20% by mass relative to the total mass of surfactant LII. For the dissolution of surfactants, the mixture was heated to 55° C.
The emulsion was prepared by adding the aqueous phase obtained in the flask containing the oily phase (still hot at 45° C.), and then sonicating the mixture to 50° C. under the conditions indicated in the Table 2 above, but with a power Pmax of 30%.
Finally, the LNP-SH were dialysed 2 times against PBS 1× (MW Cut off 12000-14000 Da; 500 mL; 24 hours). After dialysis, the LNP-SH droplets were filtered on filters of 0.2 μm.
TABLE 13
Composition of the Emulsion LNP-SH
Mass (mg)
Lipid Phase
Aqueous Phase
Purified
Wax
Lecithin
SA CONH PEG 100 -
Soybean
Suppocire
Lipoid
Myrj ®
SSPyr (Compound
Oil
NC
s75
S40
LII as in Example 1)
PBS 1X
68
272
65
276
69
2500
B. Preparation of a Gel Under the Action of Light
From the emulsion of LNP-SH obtained here above (weight percentage 23%) 1 mL thereof was introduced into a bottle. Then, the sample was irradiated at 365 nm with a power of 15 mW (OSRAM, HBO 750MA lamp).
After irradiation period of 1 hour 30 min, it was noted that there was formation of an insoluble chemical gel in the buffer PBS 1× ( FIG. 8 ).
The mechanism of gelation is attributed to the irradiation of the thiol functions at the surface of the droplets, leading to the formation of the radicals —S° on the surface of the LNP, which are capable of leading to the formation of disulphide bonds binding the droplets to one another.
In order to ascertain whether this gelation is due to the presence of the thiol functions on the surface of the lipid droplets, the example was repeated but by replacing the LNP-SH droplets with standard droplets (LNP with terminal —OH functions and not—SSPyr functions). After irradiation period of 1 hour 30 min, it was noted that there was neither any formation of gel nor any change in viscosity.
Furthermore, it was noted that the gel is destroyed when the disulfide bonds are reduced. Indeed, when the photo-formed LNP-S-S-LNP gels were brought to be reacted with the DTT (dithiothreitol, 10 equivalents relative to the number of SH functions), it was noted that the gel returns to a liquid state after two minutes of agitation.
C. Rheological Measurements
In order to study the evolution of the formation of the chemical gel during the irradiation time period, use was made of an oscillating rheometer (AR2000 EX, TA Instruments) enabling the measuring of the modulus of viscosity and modulus of elasticity of the sample, at an oscillation frequency of 1 Hz, during irradiation thereof (360 nm, power of 60 mW/cm 2 ), by depositing 300 μL of LNP-SH emulsion on the Quartz surface above the UV lamp.
During the irradiation time period, an increase was observed both in the modulus of viscosity (G “) and the modulus of elasticity (G′), this being indicative of the gelation. After 80 minutes of irradiation, it was noted that G′ has become greater than G”, and delta, defined as the tangent (delta)=G′/G″, has become less than 45° C., which indicates the transforming of a viscoelastic liquid into a viscoelastic solid.
The same experiment performed with the emulsion of LNP droplets bearing terminal hydroxyl functions (LNP-myrj s100) makes it possible to verify that no changes in rheological properties have occurred during the irradiation process.
Example 10
Formation of Gels from SA-PEG-ONHPOC
A. Synthesis of the Surfactant SA CONH PEG100NHCO—ONH—POC
This is a polyethylene glycol type surfactant (100 units) bound at one end to a fatty chain (C18) via an amide function and at the other end to another amide function bound to the oxyamine function protected by a protecting group NPPOC (2-(2-nitrophenyl)propyloxycarbonyl).
Its structure (product 3) and its synthesis process diagram are detailed here below.
Synthesis of the Product 1
Carboxymethoxylamine hydrochloride (1 g, 4.57 mmol) was dissolved in an aqueous solution of sodium carbonate 10% (25 mL). The solution was cooled to 0° C., and a solution of 2-(2-Nitrophenyl)propyl chloroformate (NPPOC—Cl) (2.20 g, 9.1 mmol) was added, drop by drop, into the dioxane (20 mL). The stirring was maintained for a period of 3 hours at ambient temperature. The reaction medium was then evaporated to dryness. To the residue obtained, water (250 mL) was added and the aqueous phase was then washed with diethyl ether (200 mL). The aqueous phase was acidified with an aqueous 1N hydrochloric acid solution to pH 3 and extracted with dichloromethane (3×250 mL). Finally, the organic phases were combined and dried over anhydrous sodium sulfate, and evaporated.
The crude product was purified by means of chromatography on silica gel (dichloromethane then dichloromethane/methanol 97/3, v/v). The product 1 was obtained in the form of a white powder (1.17 g, 3.9 mmol, 87.75%).
1 H-NMR (200 MHz, CDCl 3 ): δ ppm 1.34 (3H, d, C H 3 ); 3.5 (1H, m, C H ); 3.76 (2H, d, C H 2 O); 4.37 (s, 2H, COC H 2 O); 7.3-7.6 (4 H A , m); 8.8 (1H, s, COO H ).
Synthesis of the Product 2
The product 1 (1.17 g, 3.9 mmol) was dissolved in dichloromethane (5 mL) and then pentafluorophenol (906.5 mg, 4.63 mmol) was added, followed by the adding drop by drop of a solution of dicyclohexylcarbodiimide DCC (877.26 mg, 4.63 mmol) into the dichloromethane. The mixture was stirred for a period of 4 hours and then filtered. After evaporation, the product 2 was obtained in the form of a yellow oil (1.8 g, 4.63 mmol, 100%).
1 H-NMR (200 MHz, CDCl 3 ): δ ppm 1.34 (3H, d, C H 3 ); 3.5 (1H, m, C H ); 3.76 (2H, d, C H 2 O); 4.37 (s, 2H, COC H 2 O); 7.3-7.6 (4 aromaticH , m).
Synthesis of the Product 3
Under argon, the SA CONH PEG100-NH 3 + TFA − (surfactant C in the Example 1, 519.14 mg; 0.1 mmol) and the diisopropylethylamine, DIEA (25 .μL, 0.2 mmol) were dissolved in dichloromethane (10 mL). After 5 minutes of stirring, the product 2 (50.54 mg, 0.13 mmol) was added to the reaction medium. After a reaction period of 2 hours, the solvent was evaporated. The crude product was purified by dialysis in distilled water (MW Cut off 1000 Da; 2 L; 48 hours). Finally, the product 3 was lyophilised in order to bring about the production of a white powder (428.53 mg, 0.08 mmol, 80%).
1 H-NMR (200 MHz, CDCl 3 ): δ ppm 0.88 (3H, t, CH 3 ); 1.25 (28H, m, 14 CH2); 1.34 (3H, d, C H 3 ); 1.89 (2H, m, CH 2 —CH 2 —CONH); 2.17 (2H, t, CH2-CONH); 3.34 (2H, m, CH2-NH 3 + ); 3.4 (1H, m, C H ); 3.5-3.70 (400H, m, CH 2 PEG); 3.76 (2H, d, C H 2 O); 4.37 (s, 2H, COC H 2 O); 617 (1H, s, NH); 7.3-7.6 (4 Aromatic H , m).
B. Preparation of the Emulsion of LNP-ONH-POC
The oily phase was prepared as in Example 1, by using the ingredients and proportions indicated in the Table 14 here below. A small amount of dichloromethane was added to improve the solubility in the oily phase, it was evaporated thereafter. A fluorophore (DiD) was added to the premix (80 ul, 10 mM in ethanol) in order to enable improved subsequent visual observation of the particles.
The aqueous phase was prepared as in Example 1, by using the ingredients and proportions set forth in the Table 12 here below. The surfactant SA CONH PEG100NHCO—ONH—POC was added in an amount of up to 20% by mass relative to the total mass of PEGylated surfactant. For the dissolution of surfactants, the mixture was heated to 55° C.
The emulsion was prepared by adding the aqueous phase obtained in the flask containing the oily phase (still hot at 45° C.), and then sonicating the mixture to 50° C. under the conditions indicated in the Table 2 above, but with a power Pmax of 30%.
Finally, the droplets were dialysed 2 times against PBS 1× (MW Cut off 12000-14000 Da; 500 mL; 24 hours). After dialysis, the droplets were filtered on filters of 0.2 μm.
TABLE 14
Composition of the emulsion with NPPOC group surfactant
Mass (mg)
Lipid Phase
Purified
Wax
Lecithin
Aqueous Phase
Soybean
Suppocire
Lipoid
Myrj ®
SA CONH PEG 100 -
Oil
NC
s75
S40
NCOONH-POC
PBS 1X
68
272
65
275
70
2500
C. Characterisation
The size and charge of the LNP- ONHPOC were measured by DLS (quasi-elastic light scattering) by a Nanosizer (Malvern Zetasizer).
TABLE 15
Characterisation of droplets
Mean
Polydispersity
Zeta potential
Zeta Potential
diameter
index
(mV) in water
(mv) in PBS 0.1x
3.25
54
0.119
−3.51
−3.3
mL
D. Demonstrating Evidence of the ONH-POC Functions on the Surface of the LNP
In order to clearly demonstrate evidence of the presence of oxyamine functions protected on the surface of the LNP, a sample (0.6 mL, 3.96 mM, 2.38 μmol of —ONH—POC functions) was introduced into a flask, and then a few drops of NaOH were added therein in order to make the medium more basic (pH 9), which promotes the deprotection of the oxyamines under irradiation.
The size and the zeta potential of the particles were measured after irradiation so as to determine the effect of pH and of the light on the particles. The results are provided in the Table 16 here below.
It was found that the photo-deprotection of the —ONHPOC functions was achieved without significantly altering the size and surface charge of the nanoparticles.
TABLE 16
Size and zeta potential after deprotection of the oxyamine functions
Mean
Polydispersity
Zeta Potential
Diameter (nm)
index
(mv)
SACONH-PEG100-
54
0.119
−3.3
ONHPPOC
pH 7.4
SACONH-PEG100-
55
0.161
−1.9
ONHPPOC
pH 9; hv 10 min
As the oxyamine functions (O—NH 2 ) react very quickly with the aldehyde functions, evidence of the formation of the —ONH 2 functions was demonstrated by means of reaction with the fluorescein-aldehyde having the formula given below (6.6 mM, 1.08 mL, 7.13 μmol).
The two reagents were placed into contact with each other for 2 hour with stirring on a moving stir plate and protected from light. Then, purification by size exclusion column (Sephadex G-25 Medium, GE Healthcare) was performed in order to get rid of all the fluorescein molecules that have not reacted with the LNP-ONH 2
The elution fractions collected were analysed by fluorescence spectroscopy on a Tecan plate reader (Tecan Infinite M1000). Assays were performed in two wavelength ranges: 1) with excitation at 490 nm and collecting of the emission at 520 nm (signals due to the fluorescein of the fluorescein-CHO reagent); 2) with excitation at 640 nm and collecting of the emission at 690 nm (signals due to the DiD included in the core of the particles).
The protocol was repeated with an emulsion of LNP-Myrj S100 not bearing ONH-POC functions on their surface. Furthermore, the LNP-ONHPOC that were not irradiated and therefore not deprotected were brought to be reacted with the fluorescein-aldehyde in the same proportions as before. Finally, the protocol was repeated after having inhibited the oxyamine functions (—ONH 2 ) that were deprotected with acetone before putting them in contact with fluorescein-aldehyde.
It may be noted from the elution profiles obtained with the two types of droplets that —ONH-POC functions present on the surface of the droplets, that are irradiated and thus deprotected in order to access the O—NH 2 functions, were able to react with the aldehyde function of the aldehyde fluorescein fluorophore (co-elution of the fluorescein—grafted to the surface of the nanoparticles and of the DiD included within their core). However, no reactivity with respect to the fluorescein-aldehyde has been detected for the negative controls.
E. Gelling of the LNP-ONHPOC after Photo-Deprotection and Addition of Glutaraldehyde
A quantity of 0.6 mL of the formulation of LNP-ONHPOC (3.66 mmol) as obtained here above was deprotected in the presence of NaOH (pH 9) by irradiation for 10 minutes at 365 nm (15 mW, OSRAM HBO 750MA lamp).
To this solution were added 2 .μL of a solution of glutaraldehyde 50% in water (that is 22 μmol and 10 equivalents of aldehyde functions relative to the —ONHPOC functions deprotected in —ONH 2 ). A change in colour—from blue to red- and the formation of a gel were noted.
The mechanism of the supposed gelation is illustrated in the diagram here below.
The change in colour observed during the irradiation step (deprotection of the oxyamine functions) is attributed to a degradation of the fluorophore DiD encapsulated in the core of the nanoparticles during the irradiation in basic medium.
The gel remains stable even after several hours after addition of the buffer PBS 1×, which demonstrates evidence of the production of a chemical gel.
Example 11
Formation of Gels with a Maleimide-Function Based Surfactant
A. Synthesis of SA-PEG-Maleimide
This is a PEG surfactant with 100 ethylene glycol units, one end of which is bound to the stearic acid (C18) by an amide bond, and the other end to a maleimide function by a second amide bond.
The synthesis of this compound is similar to that of the SA CONH PEG100-SPDP (or SSPyr, surfactant LII in the Example 1). As illustrated in the diagram above, the common intermediate SA CONH PEG100-NH 3 + TFA − (surfactant C in the Example 1), which is obtained in two steps (coupling of the PEG-NHBoc-NH 2 with the stearic acid and then deprotection of the Boc group), a nucleophilic substitution of the latter on the SMCC reagent (“maleimide-cyclohexane—NHS”) results in the desired product SA CONH PEG100-Malargon.
Synthesis of the Product SA com PEG100-Mal
Under argon, the SA CONH PEG100-NH 3 + TFA − (MW: 5191.44; 0.1 g; 0.02 mmol) and the diisopropylethylamine, DIEA (MW: 129.25; 5 .μL; 2 eq; 0.04 mmol.) are dissolved in dichloromethane (2 mL). After 5 minutes under stirring, SMCC (MW: 334.32; 20 mg; 0.06 mmol; 3 eq) was added in the reaction medium. The disappearance of the amine was monitored by TLC (CH 2 Cl 2 /MeOH 9/1). After 1 hour of reaction and evaporation of the solvent, the product was precipitated two times in ether in order to give after filtration mg of SA CONH PEG100-Mal (white powder).
TLC (CH 2 Cl 2 /MeOH 9/1) Rf=0.25
1 H NMR (300 MHz; CDCl 3 ): d: 0.88 (t; C H 3 —CH 2 ); 1.25 (m; C H 2 stearate); 1.50 (m; C H 2 of cyclohexane); 1.60 (m; C H 2 —CH 2 —CONH); 1.9 (m; cyclo-C H —CH 2 —); 2.20 (t; C H 2 —CONH); 3.42 (m; C H 2 —NHCO); 3.45 (m; C H 2 -Mal); 3.48-3.8 (m; ×C H 2 (PEG); C H 2 —NHCO); 6.11 (bt; NH); 6.70 (s; H C═C H of maleimide)
B. Preparation of an Emulsion of Droplets of 50 nm (LNP-Maleimide 50)
An emulsion of droplets containing the surfactant SA CONH PEG 100 -maleimide were prepared with the composition indicated in the Table 17 here below, as described in the previous Example 7 for preparation of the oily phase, of the aqueous phase, mixing of the two phases and then sonication. The particles were purified by dialysis (MWCO 12-14 KDa) against PBS and diluted so as to obtain a mass fraction of 20%.
TABLE 17
composition of the LNP-maleimide 50
Mass (mg)
Lipid Phase
Purified
Wax
Lecithin
Aqueous Phase
Soybean
Suppocire
Lipoid
Myrj ®
SA CONH PEG100-
PBS
Oil
NC
s75
S40
maleimide
1X
F
68
272
65
276
69
2500
50
C. Preparation of an Emulsion of Droplets of 120 nm (LNP-Maleimide 120)
An emulsion of droplets containing the surfactant SA CONH PEG 100 -maleimide was prepared with the composition indicated in the Table 18 here below, as described in the previous Example 7 for preparation of the oily phase, of the aqueous phase, mixing of the two phases and then sonication. The droplets were purified by dialysis (MWCO 12-14 KDa) against PBS and diluted so as to obtain a mass fraction of 20%.
TABLE 18
composition of the LNP-maleimide F120
Mass (mg)
Lipid Phase
Purified
Soy-
Wax
Lecithin
Aqueous Phase
bean
Suppocire
Lipoid
Myrj ®
SA CONH PEG100-
PBS
Oil
NC
s75
S40
maleimide
1X
F
450
150
45
172
43
1140
120
D. Formation of Gel from the LNP-Mal Emulsion and Cross-Linker SH-PEG-SH
An quantity of 100 mg of the LNP-mal emulsion prepared (500 .μL of suspension of droplets measuring 120 nm or 50 nm in diameter) is brought to be reacted with 0.9 mg of poly(ethylene glycol) dithiol (weight average molecular weight 1000 Da) at ambient temperature with a thiol/maleimide ratio of 1:1. The mixture is placed under conditions of moderate stirring.
A gel begins to form within a few minutes after the mixing of the reagents.
Example 12
Formation of Photo-Cleavable Gels
A. Synthesis of the surfactant SA CONH PEG100N—ONB-Maléimide
This is a polyethylene glycol type surfactant (100 Units) whose one end is bound to a fatty chain (C18) via an amide function and the other end has another amide function bound to a maleimide group via an ortho nitrobenzyl type (ONB) photocleavable group. Its structure and synthesis process diagram are detailed here below.
Synthesis of the Product 1
The Fmoc-Photo-Linker (950 mg, 1.82 mmol, supplier IRIS Biotech GmbH) was brought to be reacted with piperidine (237.26 .μL, 2.36 mmol) in 12 mL of dimethylformamide, DMF. Stirring conditions were maintained for a period of 3 hours under argon. The reaction medium was evaporated to dryness. The reaction was monitored by TLC using the eluent dichloromethane/methanol (9/1). The product 1 was obtained in the form of a yellow oil. The crude product was used as is in the subsequent step.
Summary of the Product 2
The product 1 was dissolved in dimethylformamide (15 mL) to which was added the 4-Maleimidobutyric acid N-hydroxysuccinimide ester (665.63 mg, 2.366 mmol). The mixture was stirred for a period of 3 hours under argon and the reaction was monitored by TLC: eluent: dichloromethane/methanol (9/1). After evaporation of the dimethylformamide, DMF, the crude product was purified by chromatography on silica gel (eluent: ethyl acetate and then dichloromethane/methanol 9/1). The product 2 was obtained in the form of a yellow oil (571.42 mg, 1.22 mmol, 67% yield from the two steps).
1 H-NMR (200 MHz, CDCl 3 ): ppm 1.51 (3H, d, CH 3 ); 1.89 (2H, m, N—CH 2 —CH 2 —CH 2 ); 2.05-2.21 (4H, m, NH—CO—CH 2 and O—CH 2 —CH 2 ); 2.51 (2H, t, COOH—CH 2 ); 3.52 (2H, t, O—CH 2 ); 3.92 (3H, s, O—CH3); 4.11 (2H, t, N—CH 2 ); 5.52 (1H, m, CH—CH 3 ); 6.69 (2H, s, 2CH maleimide); 7-7.55 (2H Ar , 2s); 8.02 (1H, NH).
MS (ESI positive mode): M calc =463.44 (C 21 H 25 N 3 O 9 ); m/z=486.2 [M+Na] +
Synthesis of the Product 3
Under argon, the SA CONH PEG100-NH 3 + TFA − (surfactant C in the Example 1, 165 mg, 0.033 mmol) and the diisopropylethylamine, DIEA (17.3 .μL, 0.1 mmol) were dissolved in dichloromethane (5 mL). After 5 minutes of stirring, the product 2 (47.62 mg, 0.1 mmol) and DCC (20 mg, 0.1 mmol) were added to the reaction medium. After a reaction period of 3 hours, the reaction mixture was precipitated in ether and purified by chromatography on silica gel. The product 3 was obtained in the form of a yellow powder.
1 H-NMR (200 MHz, CDCl 3 ): d ppm 0.88 (3H, t, CH 3 ); 1.07 (2H, m, CH 2 —CH 2 —CONH); 1.11 (2H, t, CH2-CONH); 1.19 (28H, m, 14 CH2); 1.63 (2H, m, N—CH 2 —CH 2 —CH 2 ); 1.86 (3H, d, CH 3 ); 2.1-2.2 (6H, m, NH—CO—CH 2 , O—CH 2 —CH 2 and COOH—CH 2 ); 3.46 (2H, t, O—CH 2 ); 3.5-3.70 (400H, m, CH 2 PEG); 3.96 (3H, s, O—CH3); 4.11 (2H, t, N—CH 2 ); 5.14 (1H, m, CH—CH 3 ); 5.65 (2H, s, 2CH maleimide); 6.97-7.53 (2H Ar , 2s); 8.32 (1H, NH).
B. Preparation of an Emulsion of Droplets of 50 nm (LNP ONB Maleimide 50)
An emulsion containing the surfactant SA CONH PEG 100 -ONB-maleimide was prepared with the composition indicated in the Table 19 here below, as described in the previous Example 7 for preparation of the oily phase, of the aqueous phase, mixing of the two phases and then sonication. The particles were purified by dialysis (MWCO 12-14 KDa) against PBS and diluted so as to obtain a mass fraction of 20%.
TABLE 19
composition of the LNP-ONB-maleimide 50
Mass (mg)
Lipid Phase
Aqueous Phase
Purified
Wax
Lecithin
SA CONH PEG 100 -
Soybean
Suppocire
Lipoid
Myrj ®
ONB-
PBS
Oil
NC
s75
S40
maleimide
1X
F
68
272
65
276
69
2500
50
C. Preparation of an Emulsion of Droplet of 120 nm (LNP ONB Maleimide 120)
An emulsion containing the surfactant SA CONH PEG 100 -maleimide was prepared with the composition indicated in the Table 20 here below, as described in the previous Example 7 for preparation of the oily phase, of the aqueous phase, mixing of the two phases and then sonication. The particles were purified by dialysis (MWCO 12-14 KDa) against PBS and diluted so as to obtain a mass fraction of 20%.
TABLE 20
composition of the LNP-ONB-maleimide F120
Mass (mg)
Lipid Phase
Purified
Aqueous Phase
Soy-
Wax
Lecithin
SA CONH PEG 100 -
bean
Suppocire
Lipoid
Myrj ®
ONB-
PBS
Oil
NC
s75
S40
maleimide
1X
F
450
150
45
172
43
1140
120
D. Formation of Gel from the LNP-ONB-Mal Emulsion and the Cross-Linker SH-PEG-SH
An quantity of 100 mg of the prepared emulsion (500 .μL of suspension, LNP formulation 120 nm or 50 nm) is brought to be reacted with 0.9 mg of poly(ethylene glycol) dithiol (weight average molecular weight 1000 Da) at ambient temperature with a thiol/maleimide ratio of 1:1. The mixture is placed under conditions of moderate stirring.
A gel begins to form within a few minutes after the mixing of the reagents. This gel is formed by means of the formation between particles of SA-PEG 5000 -ONB-mal-S-PEG 1000 -S-mal-ONB-PEG 5000 -SA bonds.
E. Photo-Destruction of the Gel Formed from LNP-ONB-Mal and the Cross-Linker SH-PEG-SH
The chemical gel formed earlier, which is held together by the bonds between particles of the type SA-PEG 5000 -ONB-mal-S-PEG 1000 -S-mal-ONB-PEG 5000 -SA, is photocleavable by means of irradiation at 365 nm due to the presence of the group ONB.
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A material including a continuous aqueous phase and a dispersed phase in the form of droplets containing an amphiphilic lipid and a surfactant having the following formula (I):
(L 1 -X 1 —H 1 —Y 1 ) v -G-(Y 2 —H 2 —X 2 -L 2 ) w (I),
wherein:
L 1 and L 2 independently represent lipophilic groups, X 1 , X 2 , Y 1 , Y 2 and G independently represent a linking group, H 1 and H 2 independently represent hydrophilic groups including a polyalkoxylated chain, v and w are independently an integer from 1 to 8,
wherein the droplets of the dispersed phase are covalently bonded by the surfactant having the formula (I). The invention also relating to the method for preparing the same and to the uses thereof.
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BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to photoresist compositions for a resist flow process and a process for forming a contact hole using the same. In particular, the present invention relates to a photoresist composition comprising a thermal curing agent which cures the photoresist composition at an elevated temperature; and a method for forming a contact hole using the same.
2. Description of the Background Art
Resist flow is a processing technology for forming a fine contact hole which exceeds the resolution of the exposing device.
The resist flow process has recently made remarkable developments and so that it is now used in mass production processes. The technology generally involves an exposure process and a development process. This process forms a photoresist contact hole having a resolution equal to that of the exposing device. The process also includes heating the photoresist to a temperature higher than the glass transition temperature of the photoresist which causes the photoresist to flow. The contact hole gets smaller by the flow of photoresist until a fine contact hole necessary for the integration process is obtained (see FIG. 1 ).
Thus, the resist flow process makes it possible to obtain contact holes smaller than the resolution of an exposing device. However, one major limitation of the resist flow process is that an excessive thermal flow (i.e., “overflow”) covers or destroys the contact hole pattern. The over flow can occur due to several factors including photoresist's sensitivity to heat, imprecise temperature control, and imprecise control of the flow time. Any one or more of these factors cause an excessive thermal flow, which results in the photoresist covering the contact hole. Such overflow can be seen in FIG. 2, which shows a graph of the baking temperature versus the size of final contact hole. As FIG. 2 shows, the size of a 200 nm contact hole decreases remarkably as the baking temperature increases from 100 ° C. to 140 ° C. This decrease in contact hole size is believed to be due to the photoresist undergoing a rapid thermal flow even with a slight increase in temperature.
Attempts to solve the overflow problem by improving the baking process, such as maintaining a uniform baking temperature and/or controlling the precise baking time, have been mostly unsuccessful.
SUMMARY OF THE INVENTION
Accordingly, it is an object of the present invention to provide photoresist compositions for a resist flow process.
Another object of the present invention is to provide a resist flow process for forming a photoresist pattern using such photoresist composition.
Still another object of the present invention is to provide a contact hole formation method employing the photoresist pattern formed by the above-described process.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a schematic view of a conventional resist flow process.
FIG. 2 is a graph of After Flow Critical Dimension (AFCD) versus temperature of flow bake, using the conventional photoresist composition.
FIG. 3 is a graph of AFCD versus temperature of flow bake, using the photoresist composition of the present invention.
DETAILED DESCRIPTION OF THE INVENTION
The present invention provides a photoresist composition comprising a thermal curing agent, which is capable of curing the photoresist composition when heated to a particular temperature range. Preferably, the thermal curing agent is capable of curing the photoresist composition at a temperature range where the photoresist composition becomes flowable.
In one particular embodiment of the present invention, the thermal curing agent is capable of curing the photoresist composition at temperature of 110° C. or above, preferably at 130° C. or above, and more preferably at 140° C. or above. In this manner, thermal curing agents of the present invention reduce or prevent overflow during a flow bake process (i.e., resist flow process). The amount (i.e., degree) of photoresist composition curing depends on the amount of thermal curing agent present in the photoresist composition. Typically, a higher amount of thermal curing agent in the photoresist composition provides a contact hole pattern with a higher thermal stability (i.e., able to maintain a substantially similar contact hole size). As used herein, the term “substantially similar contact hole size” refers to a contact hole size that is within about 20% of the contact hole size in the beginning of the curing stage. And conversely, a smaller amount of thermal curing agent in the photoresist composition provides a contact hole pattern with a lower thermal stability (i.e., the contact hole size decreases gradually at an elevated temperature and changes significantly relative to the contact hole size in the beginning of the curing stage).
In one aspect of the present invention, the thermal curing agent comprises a thermal acid generator and a curing compound. A thermal acid generator is a compound which is capable of generating an acidic moiety when heated, e.g., during the baking step or the resist flow process. The curing compound is selected from a group of compounds that is capable of curing the photoresist composition when contacted (i.e., reacted) with the acid that is generated by the thermal acid generator.
In one embodiment of the present invention, the thermal curing agent comprises more than one thermal acid generator. In another embodiment of the present invention, the thermal curing agent comprises more than one curing compound.
Preferably, the curing compound comprises a cross-linking moiety. Without being bound by any theory, it is believed that the cross-linking moiety present in the curing compound is responsible for curing the photoresist composition, thereby reducing or eliminating the overflow during the baking step and the resist flow process.
Exemplary thermal acid generators include alcohols comprising a leaving group, preferably located adjacent to the alcohol functional group. It has been found by the present inventors that an alcohol comprising a sulfonate group is a particularly useful thermal acid generator. Preferably, thermal acid generators include, but are not limited to, compounds of Formulas 1 to 4:
Exemplary cross-linking moieties include acetals and epoxides. Thus, curing compounds comprising a cross-linking moiety include, but are not limited to, compounds of Formulas 5 to 8:
where each of R 1 , R 2 , P4, R 5 , R 6 , and R 7 is independently substituted or unsubstituted linear or branched C 1 -C 5 alkyl; each of R 3 , R 8 , and R 9 is hydrogen or alkyl, preferably methyl; n is an integer such that the molecular weight of compound 5 is from about 1000 to about 5000; and a and b are integers such that the molecular weight of compound 7 is from about 1000 to about 5000, preferably the mole ratio of a:b is 0.75:0.25.
In one particular embodiment of the present invention, the photoresist composition comprises a photoresist resin, a photo acid generator, an organic solvent, and a thermal curing agent described above.
Typically, the, amount of thermal acid generator and the total amount of curing compound are from about 0.1 to about 50% by weight of the photoresist resin employed. Preferably, the amount of thermal acid generator is from about 0.1 to about 5% by weight of the photoresist resin employed. Preferably, the amount of curing compound is from about 1 to about 10% by weight of the photoresist resin employed.
The photoresist resin can be any currently known chemically amplified photoresist resin.
Preferred photoacid generators include sulfide and onium type compounds. In one particular embodiment of the present invention, the photoacid generator is selected from the group consisting of diphenyl iodide hexafluorophosphate, diphenyl iodide hexafluoroarsenate, diphenyl iodide hexafluoroantimonate, diphenyl p-methoxyphenyl triflate, diphenyl p-toluenyl triflate, diphenyl p-isobutylphenyl triflate, diphenyl p-tert-butylphenyl triflate, triphenylsulfonium hexafluororphosphate, triphenylsulfonium hexafluoroarsenate, triphenylsulfonium hexafluoroantimonate, triphenylsulfonium triflate and dibutylnaphthylsulfonium triflate.
While a variety of organic solvents are suitable for use in the photoresist composition of the present invention, the organic solvent selected from the group consisting of propylene glycol methyl ether acetate, ethyl lactate, methyl 3-methoxypropionate, ethyl 3-ethoxypropionate and cyclohexanone is preferred.
Another aspect of the present invention provides a method for reducing the size of contact hole on a photoresist pattern that is produced using the above described photoresist composition.
Yet another aspect of the present invention provides a process for producing a photoresist pattern comprising the steps of:
(a) coating the above described photoresist composition on a substrate to form a photoresist film;
(b) forming a first photoresist pattern using a lithography process (preferably having a lower resolution than the maximum resolution of an exposing device); and
(c) performing a flow bake (i.e., resist flow) process to allow the photoresist to undergo thermal flow to form a second photoresist pattern.
Without being bound by any theory, it is believed that during the flow bake process of step (c), the thermal acid generator produces an acid which catalyzes cross-linking reaction of the curing compound with the photoresist resin. This cross-linking of the curing compound with the photoresist resin is believed to be responsible for limiting the flow of photoresist, and therefore preservation of the photoresist pattern.
Preferably, the flow bake process is conducted at a temperature greater than the glass transition temperature of the photoresist. Typically, the cross-linking reaction occurs at a temperature range of from about 90 to about 160 ° C.
Other thermal curing agents can also be used in the present invention provided that they are capable of curing the photoresist at a particular temperature range. As stated above, the degree of curing (e.g., cross-linking) is determined by the amount of thermal curing agent used. For example, if a large amount of the curing compound comprising a cross-linking moiety is used, it will produce a very strong cross-linking such that no additional significant flow of photoresist occurs for an extended period of time even at an elevated temperature. This provides a stable contact hole pattern, i.e., the contact hole size remains substantially similar to the contact hole size as the beginning of cross-linking process. If a small amount of the curing compound comprising a cross-linking moiety is used, then it will produce a substantially weak cross-linking. This weak cross-linking causes, the contact hole size to gradually decreases at an elevated temperature as time passes. See for example, FIG. 3 .
Still another aspect of the present invention provides a method for preparing a contact hole using the photoresist composition described above. In particular, the substrate coated with a photoresist composition is etched using the second photoresist pattern (as described above) as an etching mask to form the contact hole.
Yet another embodiment of the present invention provides a semiconductor element that is manufactured using the photoresist composition described above.
The present invention will now be described in more detail by referring to the examples below, which are not intended to be limiting.
Comparative Example
A photoresist resin 402R KrF P/R (available from Shinetsu) was coated on the wafer, baked at 100° C. for 90 seconds and exposed to light using a 0.60NA KrF exposing device (Nikon S201). The photoresist composition was post-baked at 110° C. for 90 seconds, and developed in 2.38wt % aqueous TMAH solution to obtain a 200 nm L/S pattern. The resulting wafer was baked ate 100° C. for 90 seconds and subjected to a resist flow process at a temperature range of from 110 to 200° C. for 90 seconds. The size of the contact hole is shown in FIG. 2 . As can be seen, when the 200 nm-contact hole is baked at temperature in the range of from 100 to 140° C., its size diminishes significantly. It is believed that this is due to thermal flow of the photoresist.
INVENTION EXAMPLE 1
To 100 ml of photoresist 402R KrF P/R (available from Shinetsu) was added 0.4g of the thermal acid generator of Formula 4 and 2g of the curing compound of Formula 6. A 200 nm L/S pattern was obtained using this photoresist compositions and the procedure of Comparative Example. The contact hole size after subjecting the water to a baking step and a resist flow process is shown in FIG. 3 . As FIG. 3 shows, in contrast to the Comparative Example, the contact hole can be safely reduced down to 150 nm without any significant overflow at a very high temperature, e.g., even at 150° C. or above.
The foregoing discussion of the invention has been presented for purposes of illustration and description. The foregoing is not intended to limit the invention to the form or forms disclosed herein. Although the description of the invention has included description of one or more embodiments and certain variations and modifications, other variations and modifications are within the scope of the invention, e.g., as may be within the skill and knowledge of those in the art, after understanding the present disclosure. It is intended to obtain rights which include alternative embodiments to the extent permitted, including alternate, interchangeable and/or equivalent structures, functions, ranges or steps to those claimed, whether or not such alternate, interchangeable and/or equivalent structures, functions, ranges or steps are disclosed herein, and without intending to publicly dedicate any patentable subject matter.
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The present invention relates to photoresist compositions for resist flow process and processes for forming a contact hole pattern using the same. In particular, the present invention relates to photoresist composition comprising a thermal curing agent which cures photoresist composition at an elevated temperature. In one embodiment, the thermal curing agent comprises a thermal acid generator and a curing compound. Preferably, the curing compound comprises a cross-linking moiety which is capable of curing the photoresist composition when reacted with the acid that is generated by the thermal acid generator. Photoresist compositions of the present invention reduces or eliminate overflow of photoresist during a resist flow process, thereby preventing a contact hole pattern from being destroyed. In addition, photoresist compositions of the present invention allow formation of uniform sized patterns and increase in etching selection rate.
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CROSS-REFERENCE TO RELATED APPLICATIONS
[0001] The present Application is based on International Application No. PCT/EP2008/052865, filed on Mar. 11, 2008, which in turn corresponds to French Application NO. 0753933 filed on Mar. 20, 2007, and priority is hereby claimed under 35 USC §119 based on these applications. Each of these applications are hereby incorporated by reference in their entirety into the present application.
FIELD OF THE INVENTION
[0002] The present invention relates to a mixed antenna comprising a wire-plate antenna and a PIFA antenna. One of the antennas is connectable to an electric generator, the other antenna being coupled to the first by capacitive coupling. The invention applies notably in the field of telecommunications, to WiFi antennas for example.
BACKGROUND OF THE INVENTION
[0003] A digital radiological cassette makes it possible to store one or more digital images of a patient illuminated in transparency by X-rays, without necessarily having to place the patient in a strictly delimited mechanical environment, the cassette being portable and therefore easy to manipulate. If moreover this cassette is wireless, mobility and ease of use are increased. But dispensing with the wire makes it necessary to transmit the digital image to the hospital's information system by way of a transmit radio antenna. This poses practical difficulties.
[0004] On the one hand, a certain mechanical robustness of the cassette is necessary to ensure reliability in the event of a fall or knocks, as well as for protection against outside electromagnetic disturbances. This requires that the device be enclosed in a metal shell forming a Faraday cage and ensuring shielding. Whether the antenna is placed inside, this being the worst electromagnetic case, or outside, this being the worst case in respect of mechanical protection, the influence of this metal mass prevents the use of on-PCB flat antennas. The radio constraints being considered to be greater relative to the mechanical constraints, the antenna must necessarily be placed outside the metal shell. However, the space available outside is very small and defines an area rather than a volume. The antenna must also be protected from knocks and liquids frequently used in a hospital setting in order to clean the instruments.
[0005] Moreover, the medical environment requires compliance with strict medical standards from the point of view of transmitted radio power. The standard IEC 60601-1-2 limits the instantaneous power of radiation transmitted (IPRT) to a maximum of 1 milliwatt. This power restriction makes it difficult to use an off-the-shelf antenna such as an antenna of “WiFi” type, whose nominal power is generally of the order of 100 mW. They can easily be limited to 1 milliwatt, but then the metallic environment constituted by the cassette causes a critical misfit of the antenna to this power level. Off-the-shelf “WiFi” antennas are therefore definitively not fit for use in a digital radiological cassette. But making a “WiFi” antenna that is dedicated to use in a digital radiological cassette still poses numerous technical difficulties.
[0006] Indeed, such an antenna is firstly required to cover a broad frequency band or indeed several bands because of the regulatory disparities between countries. So numerous standards known commercially as “WiFi” have appeared on the scene: these standards are for example IEEE 802.11a, IEEE 802.11b, IEEE 802.11g or IEEE 802.11n. The IEEE 802.11b and IEEE 802.11g standards provide several communication channels between 2.4 and 2.5 gigahertz. The IEEE 802.11a standard provides several channels between 5 and 6 gigahertz. Thus, an almost multi-purpose WiFi link, compatible at least with the three standards IEEE 802.11a, IEEE 802.11b and IEEE 802.11g, requires the use of a multi-band antenna capable of sending and receiving information on several frequency bands. Numerous constraints arise in respect of such an antenna. First of all there are the conventional antenna constraints relating to direction of operation and power. But, above all, there are also size constraints. Indeed, the use of a WiFi link is justified essentially on a portable device offering reduced weight and size. Such is typically the case for a digital radiological cassette.
[0007] The antenna must be omnidirectional, or at the very least it must have a radiation pattern that is as uniform as possible in space. So the user does not have to worry about the relative position or the orientation of the cassette with respect to the receiving WiFi set.
[0008] The antenna must have a certain range in transmission, the range often depending on the context of use. For example, the off-the-shelf WiFi cards to be installed in portable or office computers have variable ranges, the user being able to choose his card (and the budget that he wishes to allot to it) as a function of the conditions of use such as the area to be covered, the number of stories or the thickness of the walls. Now, the range of an antenna is directly proportional to its transmission power, which is known to be subject to a regulatory limitation to 1 milliwatt in a hospital setting. Under such conditions, satisfying at one and the same time the range requirements and at one and the same time the limitation in regard to power transmitted by the antenna turns out to be complicated. Even if the problem involved is essentially that of a medical standard, neither should it be overlooked that the antenna must form an integral part of a portable device supplied from a rechargeable battery system which is therefore of limited power. The antenna must therefore have excellent efficiency, that is to say restore in the form of radiation a maximum amount of the energy provided to it by the battery.
[0009] The antenna must be multi-band, at least matched to various frequencies of the WiFi standards. Now, generally an antenna is matched to a given frequency. At this given frequency, if the antenna is supplied with energy through a cable, it must radiate a maximum amount of this energy and return a minimum amount thereof to the cable. Thus, if the power supply system has for example an impedance of 50 ohms, the antenna must also have an impedance of 50 ohms. This is easy to achieve for an antenna having to work in a single frequency band, especially a narrow band. But it is much more difficult to achieve when the antenna must work in several bands, possibly wide bands such as that of the IEEE 802.11a standard permitting heavy data throughputs.
[0010] The antenna must also have a reduced size so as to be integrated into a portable device.
[0011] Specifically, if any one of these points is not dealt with and resolved satisfactorily, it is very difficult to obtain a satisfactory link budget. The ratio between the power received by the receiving antenna and the power transmitted by the transmitting antenna is very low, resulting in a significant error rate on the line.
[0012] Similar technical problems are encountered notably in the field of portable computers comprising a WiFi antenna. The problems posed by the rechargeable power supply are amplified by the fact that a portable computer can be used away from the mains for relatively long durations. Such is not the case for a digital radiological cassette. The antennas used on portable computers are dipoles printed on a dielectric substrate, also called “2D antennas”, the antenna being encased in a plastic package insulating them from any contact with metallic elements. These antennas are particularly suitable for being integrated into varied systems. But a digital radiological cassette takes the form externally of a metallic shielding shell. If the 2D antenna is placed inside, it does not radiate outside. If it is placed outside, the metal shell considerably disturbs its radiation, rendering it ineffective.
[0013] An alternative solution which could be envisaged is the use of an antenna mounted on a ground plane, also called “3D antennas”. More voluminous, such antennas are generally used to illuminate big volumes, an entire building for example. These are for example antennas known as “PIFA” antennas (Planar Inverted F Antenna). But to obtain multi-band operation with a PIFA antenna, the latter's dimensions must be sufficient for its radiating plane to be able to comprise slots. These dimensions are incompatible with the width, length and thickness available outside a digital radiological cassette. In the volume allocated to the antenna, only a mono-band PIFA antenna could fit. Another alternative solution which could be envisaged is the use of a 3D antenna according to patent EP 0 667 984 B1. Indeed, an antenna of wire-plate type with several radiating planes according to this patent can cover several frequency bands. But it is much too big in size, notably as regards thickness, to be able to be assembled to the outside of a digital radiological cassette.
SUMMARY OF THE INVENTION
[0014] A technical problem to which the present invention proposes to respond is to provide an antenna having similar characteristics in terms of radiation to the known 3D antennas, but offering a much smaller size.
[0015] The aim of the invention is notably to provide a multi-band antenna offering a very small size. For this purpose, the subject of the invention is a mixed antenna comprising a wire-plate antenna and a PIFA antenna. One of the antennas is connectable to an electric generator. The other antenna is coupled to the first by capacitive coupling.
[0016] Advantageously, the antenna can be multi-band in frequency.
[0017] In one embodiment, the wire-plate antenna and the PIFA antenna can each comprise a radiating plate, the two plates each being able to be disposed on a radiating element and the two elements each being able to be disposed on a ground plane. The two radiating plates can be in one and the same plane and separated by a slot of constant width, the slot ensuring the capacitive coupling of the two plates.
[0018] Advantageously, the two radiating elements can be disposed on one and the same ground plane.
[0019] The slot between the two plates can form a pattern, the pattern increasing the length of the slot and its capacitance. For example, the pattern formed by the slot between the two plates can form a rectangular protrusion of one of the plates into the other plate.
[0020] In one embodiment, a central strand of a coaxial cable can be connected to one of the radiating plates and the peripheral braid of the coaxial cable can be connected to the ground plane. The central strand can link the plate to the electric generator and the peripheral braid can link the ground plane to the electrical ground. For example, the central strand of the coaxial cable can link the radiating plate of the PIFA antenna to the electric generator.
[0021] The antenna can be encased in a plastic chassis, the chassis possibly being fixed to the outside of a digital radiological cassette, the plastic chassis insulating the antenna from the disturbances caused by the metal casing of the cassette.
[0022] In addition to the fact of offering a very small size for similar performance to the known 3D antennas, the invention furthermore has the main advantages that it only requires the implementation of regular techniques for fabricating 3D antennas. Its final cost is entirely comparable with that of a PIFA antenna or of a conventional wire-plate antenna.
[0023] Still other objects and advantages of the present invention will become readily apparent to those skilled in the art from the following detailed description, wherein the preferred embodiments of the invention ae shown and described, simply by way of illustration of the best mode contemplated of carrying out the invention. As will be realized, the invention is capable of other and different embodiments, and its several details are capable of modifications in various obvious aspects, all without departing from the invention. Accordingly, the drawings and description thereof are to be regarded as illustrative in naure, and not as restrictive.
BRIEF DESCRIPTION OF THE INVENTION
[0024] The present invention is illustrated by way of example, and not by limitation, in the figures of the accompanying drawings, wherein elements having the same reference numeral designations represent like elements throughout and wherein:
[0025] FIG. 1 , through an exploded view, an exemplary mixed antenna according to the invention intended to be integrated on a digital radiological cassette;
[0026] FIG. 2 , a perspective view of the same exemplary mixed antenna according to the invention;
[0027] FIG. 3 , through a design diagram, the dimensions of the same exemplary mixed antenna according to the invention;
[0028] FIG. 4 , through a graph, the radiation pattern of the same exemplary mixed antenna according to the invention.
DETAILED DESCRIPTION
[0029] FIG. 1 illustrates through an exploded view an exemplary mixed antenna according to the invention, intended to be integrated on a digital radiological cassette. It comprises for example a radiating plate P 1 made of conducting material of rectangular shape and comprising for example a protrusion S forming a square pattern on one of its small sides. The plate P 1 is mounted for example on a radiating element E 3 made of conducting material and tile-shaped, the element E 3 supporting the plate P 1 by way of a conducting link. The element E 3 is disposed for example on a metal ground plane P 3 , in direct contact. The plate P 1 , the element E 3 and the metal ground plane P 3 form a wire-plate antenna.
[0030] The mixed antenna according to the invention comprises for example a radiating plate P 2 made of conducting material of rectangular shape and comprising for example a notch E forming a rectangle pattern on one of its small sides. The large sides of the rectangle forming the notch E are slightly larger than the sides of the square forming the protrusion S. The plate P 2 is mounted for example on a radiating element E 1 made of conducting material and cube-shaped, the element E 1 supporting the plate P 2 by way of a conducting link. The element E 1 is for example disposed on the metal ground plane P 3 , in direct contact. But a distinct ground plane could have been envisaged. A radiating element E 2 made of conducting material and tile-shaped is fixed under the plate P 2 : it is not in contact with the ground plane P 3 . The plate P 2 , the elements E 1 and E 2 , as well as the metal ground plane P 3 form a PIFA antenna. Not represented in FIG. 1 for reasons of clarity, a coaxial cable of suitable cross section can for example supply the PIFA antenna with electric current by way of the element E 2 . A hole is then drilled in the ground plane P 3 opposite the element E 2 , the diameter of the hole being substantially equal to the cross section of the cable. The central strand of the cable passes through the hole without establishing contact with the ground plane P 3 . It is soldered by its end to the element E 2 . The braided sheath of the coaxial cable can for its part be advantageously soldered at the level of the edges of the hole made in the ground plane P 3 . The central strand then provides electric current, the braided sheath being linked to the electrical ground.
[0031] The mixed antenna according to the invention achieves a coupling of the wire-plate antenna and of the PIFA antenna. Advantageously, the dimensions of the elements E 1 and E 3 are such that the plates P 1 and P 2 are in one and the same plane, the element E 1 and the element E 3 being arranged in such a way that the plates P 1 and P 2 are for example separated by a slot F. Advantageously, the protrusion S fits contactlessly into the notch E, the slot F being of small and constant width. In this way, as soon as the PIFA antenna is supplied with electric current through the central strand of the coaxial cable, induced currents appear in the wire-plate antenna. The wire-plate antenna is coupled to the PIFA antenna by capacitive coupling. It should be noted that, generally, a PIFA antenna or a wire-plate antenna are not characterized by their mode of power supply. They can equally well be powered by electrical contact or by capacitive coupling. What characterizes them is rather their mode of resonance. Indeed, the mode of resonance of a wire-plate antenna is of electrical type, the currents being concentrated rather more on the ground wire, that is to say on the radiating element E 3 supported by the ground plane P 3 in the present exemplary embodiment. The radiation of a wire-plate antenna is omnidirectional in azimuth. The antenna behaves as a monopole radiating with single vertical polarization, the polarization of the radiated field being perpendicular to the so-called “short-circuit” wire of the antenna, that is to say perpendicular to the radiating element E 3 in the present exemplary embodiment. Whereas the mode of resonance of a PIFA antenna is of electromagnetic type, the currents dispersing over the whole of the structure of the antenna. The antenna behaves as a dipole radiating as a total field uniform throughout space. This uniformity is due to the sum of the two polarizations radiated by this antenna, a horizontal polarization arising from the currents circulating on the plate P 2 and a vertical polarization arising from the so-called “short-circuit” plate of the antenna, that is to say arising from the radiating element E 1 in the present exemplary embodiment. It should also be noted that the slot F between the two antennas does not have a resonance role, but that it advantageously ensures the coupling function. Advantageously, the pattern that it forms makes it possible to increase its capacitance with respect to a straight slot without a pattern. The slot F of the mixed antenna according to the invention therefore cannot be likened to the resonant slot of a conventional PIFA antenna.
[0032] The two types of antenna therefore differ through their very operating principle. It should be noted moreover that the position of the elements E 1 and E 3 in relation to their respective radiating plate P 2 and P 1 plays a determining role in the mode of resonance of the antenna formed. To make a PIFA antenna, the element E 1 must rather be off-centered with respect to the radiating plate P 2 . To make a wire-plate antenna, the element E 3 must rather be centered with respect to the radiating plate P 1 . Incidentally, this relative position determines the function of the element in the antenna formed, the function of the element E 1 of the PIFA antenna not being at all comparable with the role of the element E 3 of the wire-plate antenna.
[0033] Including the slot F, the aggregate surface area of the thus adjoining plates P 1 and P 2 is substantially identical in width to the surface area of the ground plane P 3 on which they rest and slightly shorter in length. Blocks B 1 , B 2 , B 3 and B 4 of a dielectric material are sandwiched between the plates P 1 and P 2 , blocks B 1 and B 2 being on either side of the element E 1 , blocks B 2 and B 3 being on either side of the element E 2 , and blocks B 3 and B 4 being on either side of the element E 3 . The blocks B 1 , B 2 , B 3 and B 4 do not protrude from the sandwich formed by the plates P 1 and P 2 and by the ground plane P 3 .
[0034] The mixed antenna according to the invention for a digital radiological cassette is advantageously encased in a molded plastic chassis C. The plastic chassis C makes it possible on the one hand to fix the mixed antenna according to the invention to the exterior shielding of a digital radiological cassette, not represented in FIG. 1 . The plastic chassis C also makes it possible to isolate the antenna from the significant metal mass constituted by the shielding shell, thus preventing the radiation of the antenna from being disturbed thereby. Its role is therefore determining in the application to a digital radiological cassette. It also ensures the leaktightness of the antenna and protects it against knocks.
[0035] FIG. 2 illustrates through a perspective view the exemplary mixed antenna according to the invention, already illustrated in FIG. 1 , for a digital radiological cassette. The antenna is completely assembled. Only the radiating plates P 1 and P 2 are visible, flush with the plastic chassis C and separated by the slot F. The mixed antenna according to the invention is ready for assembly with a cassette by way of the chassis C.
[0036] FIG. 3 illustrates through a design diagram the dimensions of the mixed antenna according to the invention, already illustrated in FIGS. 1 and 2 , for a digital radiological cassette. The same diagram depicts a top view, in the upper part of FIG. 3 , and a profile view, in the lower part of FIG. 3 . All the dimensions are expressed in millimeters. The diagram attests to the very small size of the mixed antenna according to the invention.
[0037] The top view depicts the radiating plates P 1 and P 2 whose protrusion S and notch E are separated by the slot F, together with the elements E 1 , E 2 and E 3 . The profile view depicts not only the radiating plates P 1 and P 2 and the elements E 1 , E 2 and E 3 , but also the ground plane P 3 . The ground plane P 3 has a length of only 71.4 millimeters. The plates P 1 and P 2 and the ground plane P 3 have a width of only 15 millimeters. Disregarding the protrusion S and the notch E, the plates P 1 and P 2 have a length of 39 and 22 millimeters respectively. The protrusion S has the shape of a square 3 millimeters by 3 millimeters. The notch E extends over 5 millimeters in the width of the plate P 2 , and penetrates 3 millimeters into the length of the plate P 2 . Thus, the slot F between the plates P 1 and P 2 is only 1 millimeter wide. The plates P 1 and P 2 are spaced only 5 millimeters apart from the ground plane P 3 , these 5 millimeters corresponding to the height of the elements E 1 and E 3 supporting the plates P 2 and P 1 respectively. The element E 2 being only 4 millimeters in height, it is spaced 1 millimeter away from the ground plane P 3 . It should be noted that each of the elements E 1 , E 2 and E 3 has a surface area in the horizontal plane which is negligible with respect to the plate that it supports (this being the case for E 1 and E 3 ), or with respect to the plate which supports it (this being the case for E 2 ). Indeed, the elements E 1 and E 2 have respective horizontal surface areas of 3×3=9 square millimeters and 7×2=14 square millimeters, this being negligible with respect to the surface area of the plate P 2 which is 15×22=330 square millimeters. The element E 3 has a horizontal surface area of 11×5=55 square millimeters, this being negligible with respect to the surface area of the plate P 1 which is 15×39=585 square millimeters. This is why from an electromagnetic point of view, the elements E 1 , E 2 and E 3 behave similarly to conducting wires. But such elements have been preferred to conducting wires by reason notably of their mechanical robustness. The dimensions of the order of a few millimeters of the present exemplary mixed antenna according to the invention render the latter particularly suitable for portable applications, a digital radiological cassette for example.
[0038] Each of the elements E 1 and E 3 is positioned substantially in the middle of the width of the plate that it supports, E 2 is positioned substantially in the middle of the width of the plate which supports it. The element E 1 is 6 millimeters from each of the two lateral edges of the plate P 2 . The element E 2 is 4 millimeters from each of the two lateral edges of the plate P 2 . The element E 3 is 2 millimeters from each of the two lateral edges of the plate P 1 . On the other hand, because of structural constraints aimed at obtaining the characteristic radiation of a PIFA antenna, neither the element E 1 nor the element E 2 are positioned in proximity to the middle of the length of the plate P 2 . For example, the element E 1 is positioned 4 millimeters from the opposite edge of the plate P 2 from the plate P 1 , the element E 2 is positioned 3 millimeters from the other edge of the plate P 2 , adjacent to the plate P 1 , bordering the notch E. Likewise, because of structural constraints aimed at obtaining the characteristic radiation of a wire-plate antenna, the element E 3 is positioned relatively close to the middle of the length of the plate P 1 . For example, the element E 3 is positioned 21 millimeters from the opposite edge of the plate P 1 from the plate P 2 , the plate P 1 being 39 millimeters long overall.
[0039] FIG. 4 illustrates the radiation pattern of the exemplary mixed antenna according to the invention, already illustrated by FIGS. 1 , 2 and 3 , for a digital radiological cassette. The abscissa represents the frequency in gigahertz. The ordinate represents the reflection coefficient of the antenna in decibels, commonly called S 11 . An antenna is considered to be matched to a given frequency if, at this frequency, its reflection coefficient S 11 is less than −6 decibels. It is apparent that the dimensions of the wire-plate antenna formed by the radiating plate P 1 , the radiating element E 3 and the ground plane P 3 allow it to radiate effectively at a frequency f b,g of the order of 2.4 to 2.5 gigahertz, the coefficient S 11 exhibiting a minimum at almost −25 decibels at the frequency f b,g . The antenna is therefore matched to the frequency f b,g ., which corresponds to the wave range of the WiFi 802.11b and 802.11g standards. The lower dimensions of the PIFA antenna formed by the radiating plate P 2 , the element E 1 and the ground plane P 3 allow it to radiate effectively in a much higher frequency range f a of the order of 5 and 6 gigahertz, the coefficient S 11 exhibiting a minimum at almost −30 decibels at the frequency f a . The antenna is therefore matched to the frequency f a , which corresponds to the wave range of the WiFi 802.11a standard.
[0040] The mixed antenna according to the invention illustrated by FIGS. 1 , 2 , 3 and 4 of the present patent application, where the PIFA antenna and the wire-plate antenna are coupled along their widths, is given only by way of example. Examples of mixed antennas according to the invention where the PIFA antenna and the wire-plate antenna would be coupled along their lengths are entirely conceivable without deviating from the principles stated by the present invention. Varying the dimensions and the relative positions of the PIFA antenna and of the wire-plate antenna makes it possible notably to tailor the mixed antenna according to the invention to given ranges of frequencies, that is to say to optimize its reflection coefficient S 11 at the desired frequencies of use.
[0041] Multi-band and of reduced size, the mixed antenna according to the invention is particularly tailored to portable applications of the various WiFi standards, such as a digital radiological cassette for example.
[0042] It will be readily seen by one ordinary skill in the art that the present invention fulfils all of the objects set forth above. After reading the foregoing specification, one of ordinary skill in the art will be able to affect various changes, substitutions of equivalents and various aspects of the invention as broadly disclosed herein. It is therefore intended that the protection granted hereon be limited only by definition contained in the appended claims and equivalents thereof.
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The present invention relates to a mixed antenna. The antenna comprises a wire-plate antenna and a PIFA antenna, a first antenna being connectable to an electric generator and the second antenna being coupled to the first by capacitive coupling.
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TECHNICAL FIELD
[0001] The invention relates to a microfluidic device for enzymatic processing of macromolecules, more particularly for preparation of isolated single macromolecules for subsequent processing. In a further aspect, a method is provided for preparing isolated single macromolecules for subsequent processing. The invention is suited for preparing and processing ultra-long macromolecules, i.e. macromolecules with a length of about 1 million base pairs and more. An example for such macromolecules is DNA.
[0002] According to a further aspect, the present invention relates to systems, apparatus, kits, algorithms and methods for handling, preparing analysing and characterizing (in any order) biological samples. The invention also describes uses of the invention, particularly in relation to nucleic acid sequencing technologies.
BACKGROUND
[0003] In the recent decades, micro- and nanofluidic devices and methods have been developed for integrating, miniaturising and automating numerous laboratory tasks. Furthermore, due to the characteristic length scales involved, analysis tasks not previously available have been made possible.
[0004] Considerable efforts have been directed to providing a reliable, rapid and affordable analysis of very long macromolecules, such as single DNA molecules, including amplification and/or sequencing steps. However, the maximum fragment lengths analysed by existing methods, are typically limited to about 35-1000 base pairs as compared to the length of bacterial DNA of about 1-10 million base pairs, and at least 50 million base pairs of a complete human DNA molecule.
[0005] A recent article on “Single molecule linear analysis of DNA in nano-channel labelled with sequence specific fluorescent probes”, published in 2010 in Nucleic Acids Research by S. K. Das et al., discloses a nanofluidic method of analysing DNA molecules. The DNA molecules analysed have all a length less than 200 kilo base pairs. A further article on nanofluidic analysis of DNA by Reisner and co-workers, published in Proceedings of the National Academy of Sciences of the USA, vol. 107, p. 13294, 2010, discloses a method for analysing DNA applicable to long DNA molecules, where “long” refers to a length of about 100 kilo base pairs.
[0006] It is one of the merits of the present invention to recognise, that the main factor limiting the length of the fragments analysed in a nanofluidic system lies in the sample preparation and transfer steps. As a principal reason for this limitation, the fragility of isolated DNA molecules or similar long macromolecules, due to shearing forces acting on the DNA, has been identified. According to the present invention, the sample preparation and transfer steps are thus identified to be critical for increasing the fragment length that can be analysed in micro- and nanofluidic systems, and eventually being able to process, e.g. for sequencing or amplification, a complete isolated DNA molecule or similar long macromolecule.
[0007] A chromosome prior to replication comprises a single length of DNA. The ability to visualize the DNA from each chromosome, from one end to the other, would enable the native long-range organization of the genome and its variation between homologous chromosomes and between individuals to be investigated. Entropic confinement in nano-channels/grooves, as demonstrated for bacteriophage genomes (<200 Kbp length), forces DNA into an extended conformation co-linear with the information encoded therein. However, to linearize whole large genomes (e.g. Human), direct from source without cloning, two problems must be considered: Firstly, during extraction or loading into a device, genomic DNA can become fragmented due to shear forces, and secondly, DNA tends to form folded, globular states in solution rather than the extended conformation. Although methods for mapping sequence motifs and patterns (Neely et al Chem. Sci. 2010; Xiao et al Nucleic Acids Res. 35: e16 2007; Reisner et al PNAS107(30):13294-9) on linearized DNA have been developed, new approaches are needed to handle, if not whole chromosomal lengths of human DNA, then portions of chromosomes that are large enough to span the haplotype blocks and much of the structural variation found in large diploid genomes.
[0008] Moreover genome analysis methods with minimal sample preparation are needed. Direct single molecule analysis of genomic DNA can achieve this; recently a whole genome has been sequenced using single molecule technology (Pushkarov et al, Nature Biotechnology 27: 847). Even so, in current methods, DNA extraction is done off-chip and the DNA handling (e.g. pipetting) leads to reduction in size of the genome fragments due to fragmentation by shearing.
[0009] There is a pronounced need for single molecule analysis of long macromolecules. For example, there are an estimated 200 cell types in the human body. However, all cells within a seemingly homogeneous population of a given a cell type are not necessarily alike. Stochastic expression at the gene and protein level is well documented. Stochastic effects lead to widely differing responses to stimuli: fast, slow, extreme or subdued. Ensemble analysis of cell populations masks the variation that is clearly evident when individual cells from a population are analysed.
[0010] There is substantial heterogeneity between cells in a tumour biopsy, including differences in chromosome number (aneuploidy), mutational profiles, methylation profiles and expression at the RNA and protein level. Analysis of single cells within tumours is important for understanding tumour pathology and is expected to contribute to cancer diagnosis, staging, and prognosis. Biopsies may contain on the order of 10,000 cells. Systematic, high throughput and preferably automatable analysis is therefore needed to address the population cell by cell.
[0011] In addition single cell analysis is important for genetic diagnosis, particularly for pre-implantation genetic analysis, which in the future may require analysis of more than one or a few genes, as the scientific community makes increasingly more connections between genotype and phenotype.
[0012] In many cases sample material is limiting, for example from archived material or for the analysis of fetal material in a mothers circulating blood or shed tumour cells or metastatic cells in circulating blood. In these cases better methods are needed for analysis of single or a few cells or a small amount of material. In the case of analysis of material in circulating blood the task may be compared to finding a needle in a haystack because the target material is a small fraction of a complex sample.
[0013] The genome and its epigenetic modifications can be analysed by modern genomic methods, the most comprehensive approach being complete genome sequencing. However, despite the emergence of technologies that have increased throughput and spectacularly lowered sequencing cost, a number of bottlenecks remain that serve as barriers to the effective translation of genomic knowledge. Although much attention has been given to throughput/cost of the sequencing process itself, the same cannot be said of preparation of the sample for sequencing. A first bottleneck is that sequencing technologies require days of upfront sample preparation. A second bottleneck is that upfront sample processing is further increased when goal is to sequence selected parts of the genome. A third bottleneck arises because all the existing technologies produce short sequence reads and thus genome assembly relies on comparing reads to the reference genome. But since the reference sequence is a composite of several genomes, such comparisons do not reveal the phenotypically significant structural variation that exists between individual genomes (rearrangements, copy number, translocations, inversions).
[0014] As mentioned above, it is one of the merits of the present invention to recognise, that the main factor limiting the length of the fragments analysed in a micro- and/or nanofluidic system lies in the sample preparation and transfer steps.
[0015] With this insight in mind, the object of the present invention is providing an improved technique for preparing long macromolecules for subsequent processing in a micro- and/or nanofluidic device overcoming the problems of the prior art or at least providing an alternative.
DISCLOSURE OF THE INVENTION
[0016] According to a first aspect of the invention, a microfluidic device for enzymatic processing of macromolecules comprises a reaction chamber with a first manifold, a second manifold, and a plurality of reaction channels, each reaction channel extending from the first manifold to the second manifold. The device further comprises first inlet and outlet channels for filling the reaction channels via the manifolds with one or more macromolecule containers suspended in a first carrier fluid, wherein the first inlet and outlet channels are configured such that a flow established from the first set of inlets to the first set of outlets is guided through the reaction channels. The device further comprises second inlet and outlet channels for feeding an enzymatic reagent to the reaction chamber essentially without displacing the macromolecule containers trapped in the reaction channels, wherein the second set of inlets and outlets are configured such that a flow established from the second inlet to the second outlet is guided through at least one of the manifolds and bypasses the reaction channels.
[0017] The microfluidic device is filled through an input port with a sample solution containing macromolecule containers. The input port is via the one or more first inlet channels connected to the first manifold, which via the reaction channels (“isolation zones”) in the reaction chamber (“trap area”) is in fluid communication with the second manifold, which in turn via the first outlet channel is connected to an outlet port. The reaction channels are filled with the sample solution and a flow of sample solution is established from the inlet port to the outlet port. The flow of sample solution thus carries at least one macromolecule container into at least one of the reaction channels. When an isolated macromolecule is identified to be present in one of the reaction channels, the flow of sample solution is stopped and a flow of enzymatic reagent is established from the one or more second inlet channels via the manifolds to the one or more second outlet channels.
[0018] The second inlet and outlet channels are configured for feeding the enzymatic reagent to the reaction chamber without displacing the macromolecules trapped in the reaction channels. Displacement of the trapped macromolecules is avoided by carefully balancing the pressure in the first and second manifolds, i.e. the pressure applied on either end of each of the reaction channels. The reaction channels thus form a stagnant volume of the flow and only the sample solution in the manifolds is replaced by the enzymatic reagent. The enzymatic reagent diffuses from the manifolds into the reaction channels, and thus also into the reaction channel comprising the identified isolated macromolecule container. The enzymatic reagent interacts with the isolated macromolecule container, thereby producing an intact isolated macromolecule in the reaction channel. The isolated macromolecule may then by fluid handling be retrieved from the reaction channel and extracted from the reaction chamber in order to transfer the macromolecule to its destination for single molecule analysis or any other single molecule processing in one or more subsequent stages. The second inlet and outlet channels may also be used for flushing buffer solutions and/or feeding any reagents, to be applied to the macromolecule container and/or to the released macromolecule.
[0019] Preferably, the second inlet and/or outlet channels are made shallower than the microchannels in the reaction chamber. Thereby, flow of sample fluid into the reagent channels is avoided or at least kept at a minimum.
[0020] An important advantage of the device according to the invention is that sample macromolecules are provided to the input of the device in a macromolecule container. The macromolecule container protects the macromolecule from mechanical shearing during sample preparation and handling of the macromolecules, e.g. by pipetting. The macromolecule container thus acts as a “carrier” for the macromolecule. A macromolecule container may be formed by encapsulation of the macromolecule, by complexing the macromolecule with a protein scaffold or by complexing the macromolecule with polycations. A DNA molecule may, for example be encapsulated by a cell wall, in a nucleus, or carried by cell extract, preferably a metaphase chromosome. Preferably, DNA molecules are provided to the microfluidic device in a solution containing chromosomes acting as a container for the DNA molecules. In the case where cells are loaded into the device, metaphase chromosomes are obtained from the cell on-chip before releasing DNA from the chromosomes. Where cell extract is loaded, DNA can be released directly from the chromosomes. Alternatively a macromolecule container may be formed by complexing the macromolecule with a protein scaffold or in some cases with polycations, such as spermine or spermidine.
[0021] The macromolecules are released from their container on-chip where shearing forces are minimal and/or are controlled. Releasing DNA from metaphase chromosome comprises the addition of one or more enzymatic reagents. This may include the addition of proteases. The preferred protease is Proteinase K. Other protease may also be useful (e.g. Trypsin). It may also include the addition of topoisomerases before or after adding the protease. Where topoisomerase is added after protease care is taken to kill the activity of the protease and/or to remove the protease. Preferably, the proteases used are appropriate for digesting at least histones or protamine. Releasing DNA may comprise the creation of a substantially naked DNA molecule, essentially devoid of proteins. However, in some cases it may be desirable to retain binding of one or more class of proteins to the DNA. Therefore, releasing DNA may alternatively comprise the creation of chromatin fibres to which proteins are still associated.
[0022] Once released, the isolated macromolecule may be manipulated by means of on-chip fluid handling and transferred to subsequent processing/analysis stages. Thereby the mechanical forces exerted on the released macromolecule may be controlled to a level so as to avoid unintended breaking of the macromolecule. The device according to the invention may thus prepare isolated macromolecules with a length that by far exceeds the length of macromolecules prepared by known techniques.
[0023] The invention thus provides a device, system and method for releasing macromolecules, such as biomolecules, on chip from small amounts of sample material, single cells, nuclei or chromosomes in a manner that keeps the macromolecules substantially intact. In particular, in an embodiment applied to genomic DNA, megabase lengths of DNA can be kept intact. Advantageously for this embodiment, following releasing of the DNA, the DNA is linearly elongated and displayed for detection. In a further embodiment the chip design allows reagents to be flushed over the DNA and allows features of interest to be labelled and then mapped. Events along the span of the DNA region being imaged can be followed in real-time. The invention provides an unprecedentedly long-range view of the genome, which encompasses the haplotype blocks as well as the structural organization of the genome. The long-range view will facilitate the de novo identification of a significant amount of previously characterized and uncharacterised copy number/structural variation. Furthermore, the mapping can be used to barcode individual genome fragments, which enables parts of the genome, bearing specific map patterns to be selected. After analysis, individual megabase length molecules can be transported to an output port of the chip, from where they can be further processed. For example, the DNA can be isothermally amplified in- or off-chip. The amplified DNA can then be collected from the output port and subjected to further molecular analysis including sequencing by any available method. Also a DNA fragment sent to the outlet port can be a component in the assembly of artificial chromosomes or used for synthesis of complex macromolecules.
[0024] Advantageously, the method of the invention may be used at the front-end of sequencing pipelines and significantly enhances the quality and throughput of DNA sequencing. In one embodiment of the invention a micro-/nano-fluidic device processes a population of individual cells in a high-throughput manner: releasing and purifying DNA from each cell and preparing the DNA through to the final steps for sequencing. Moreover, the sample preparation is done in a highly innovative way which has the double side-benefit that the long-range haplotype map of the genome can be obtained and specific parts of the genome can be selected for sequencing. It is the downstream choice of the investigator whether to collect data separately from single cells or whether to amalgamate the data from the population of cells. If the latter, the investigator still benefits because less sample material is required.
[0025] As well as applications in the research environment the microfluidic or micro/nanofluidic devices of this invention can be used as part of point-of-care systems for medical testing as well as devices for monitoring samples in the field or in various industries (e.g. water-treatment, food processing).
[0026] In a preferred embodiment of a device according to the invention, a single pair of second inlet and outlet channels is provided and the reaction chamber is essentially symmetric with respect to a mirror axis connecting said second inlet and second outlet, a longitudinal axis of the reaction channels being oriented essentially transverse to the mirror axis.
[0027] The single pair of second inlet and outlet channels has a single second inlet and a single second outlet. The second inlet channel is via an inlet branch symmetrically connected to both the first and the second manifolds. The second outlet channel is via an outlet branch symmetrically connected to both the first and the second manifolds.
[0028] The second inlet and the second outlet are thus configured to supply enzymatic reagent symmetrically to the manifolds on either end of the reaction channels, thereby maintaining substantially equal pressure, equal flow rate, and thereby for each reaction channel a balanced reagent concentration on either end.
[0029] Alternatively, an embodiment of a device according to the invention may comprise a mirror-symmetric trap area, wherein the reaction channels extend essentially transverse to the mirror axis from a first manifold to a second manifold, and wherein each of the manifolds is provided with an inlet at a first end of the manifold and an outlet at a second end opposite to the first end. In this embodiment, the reaction channels of the trap area may be loaded with a sample fluid containing macromolecule containers by establishing a diagonal flow through the reaction chamber, i.e. from an inlet of one of the manifolds (first/second manifold) via the reaction channels to an outlet of a different manifold (second/first manifold). Once the presence of at least one target macromolecule container has been determined, i.e. the trapping of a macromolecule container in a reaction channel, the filling flow is stopped and a secondary flow of flushing agents/buffers and/or reagents may be established. Any flushing agents/buffers and/or reagents are provided by a symmetric flow bypassing the reaction channels, i.e. where a flow is driven through each of the manifolds from the respective inlet to the respective outlet without passing through a reaction channel. The pressure in the manifolds is balanced with respect to each other, such that at the same pressure is present at either end of a given reaction channel, thereby avoiding any flow/displacement of the trapped target macromolecule in the reaction channel. The reagent required for releasing the macromolecule from its container is supplied via diffusion from the manifold into the reaction channel.
[0030] In a further embodiment of a device according to the invention, the device is provided with a viewport in the region of the reaction channels, the view port allowing for the visual detection of a trapped macromolecule container in at least one of the reaction channels. The visual detection is typically performed by monitoring one or more of the reaction channels during filling of the channels.
[0031] The term “visual” comprises any form of optical observation, and in particular any microscopic imaging technique and may, advantageously be combined with a machine vision system comprising recognition modules providing target detection signals representing the presence of a target macromolecule/macromolecule container. A machine vision system may also provide further signals responsive to the visual monitoring of any process steps performed on the target following detection, including releasing the macromolecule from its container, labelling, fragmenting, de-/re-naturation and/or transferring of the released macromolecule. Alternatively, target detection signals and any further monitoring signals may be provided by other means, such as integrated or external electrical and/or magnetic sensors. Any detection and/or further monitoring signals may be used as input to a control unit for controlling the processing in an auto-mated manner.
[0032] In a further embodiment of a device according to the invention, the total effective cross-sectional area for flow through the reaction chamber in the region of the reaction channels is enlarged as compared to the first inlet channel by a ratio of at least 2:1, alternatively at least 5:1, or alternatively at least 10:1. For a given throughput this reduces the flow velocity of the sample fluid, thereby facilitating the detection of a target macromolecule.
[0033] In a further embodiment of a device according to the invention, the flow resistance of reaction channels is decreased with increasing distance from the first inlet channel. When establishing a filling flow passing through the reaction channels, a pressure drop occurs along the manifolds, wherein the pressure decreases for increasing distance from the inlet channel. Consequently different driving conditions for the flow through the reaction channels may occur. To counter this effect, and to equalize the flow through the reaction channels with respect to each other, the resistance of the reaction channels is decreased, advantageously by increasing the width of the reaction channels with increasing distance from the first inlet channel. Advantageously, the distance is increased according to a linear relationship. Equalizing the filling flow has the advantage that it facilitates detection of target macromolecule containers in any of the reaction channels.
[0034] In a further embodiment of a device according to the invention, the device only comprises passive microfluidic components. An important advantage of the device according to the invention is that it does not require any active fluidic components on chip for trapping the macromolecule container, and for releasing and retrieving the isolated macromolecule. Any flow driving and control components, such as pumps, valves or the like can thus be provided external to the device. The device only comprising passive microfluidic components can thus be provided e.g. as a chip interacting/interfacing with an analysis apparatus providing such infrastructure, whereas the chip is produced cheaply, e.g. as a disposable consumable.
[0035] In a further embodiment of a device according to the invention, the reaction chamber has a rectangular layout, the rectangle having a first edge, a second edge parallel thereto, and a third and a fourth edge essentially perpendicular to the first and second edges, the first and second manifold extending along the first and second edge, respectively, the reaction channels extending from the first to the second manifold in a direction essentially parallel to the third and fourth edge, the first inlet and outlet being arranged at diagonally opposing corners of the rectangle, and the second inlet and outlet being arranged at the third and fourth edge respectively, wherein both the second inlet and the second outlet are in symmetric fluid communication with both the first and the second manifold through edge channels extending parallel to the reaction channels along the third and fourth edge.
[0036] This configuration allows in a simple manner for establishing a diagonal filling flow, i.e. a flow passing from a first inlet via a first manifold, through essentially all reaction channels, and via a second manifold to an outlet channel.
[0037] According to a broader aspect of this embodiment, the first inlet and outlet channels are arranged at opposing edges of the rectangular reaction chamber. Preferably, at least a first inlet channel is provided at the first edge and at least a first outlet channel is provided at the second edge opposite to the first edge. Advantageously, the axis connecting the first inlet and outlet channels is not a symmetry axis of the reaction chamber. The asymmetric arrangement has the advantage of promoting distribution of the injected sample fluid over the reaction channels.
[0038] Preferably, the filling flow is injected from the first inlet into the reaction chamber at an angle that is inclined with respect to the direction of the flow barriers defining the reaction channels. Injecting the filling flow at an angle with respect to the flow barriers/reaction channels further promotes distribution of the sample fluid over the reaction channels.
[0039] Advantageously said angle of injection is selected from the range between 10 to 90 degrees, alternatively from the range between 30 to 60 degrees, preferably about 45 degrees. For reasons of disambiguation only angles between 0 and 90 degrees are recited. Angles in excess of 90 degrees are mapped back to said range between 0 and 90 degrees by always measuring the smallest angle between the direction of injection and the direction of the flow barriers defining the reaction channel walls.
[0040] The single pair of second inlet and outlet channels is in symmetric fluid communication with the first and second manifolds. This means that by injecting a fluid through the second inlet channel, a symmetric pressure distribution is established in the reaction chamber, and a balanced pressure level is established on either end of each of the reaction channels. While the pressure may drop in the manifolds along the direction of flow, the device is configured such that the pressure drop in one of the manifolds is a mirror of the pressure drop in the other manifold with respect to the symmetry axis of the reaction chamber.
[0041] Operation of the device is particularly simple and reliable, because it only requires simple actuation of external valves and/or flow driving components, yet keeping sample fluids and reagent fluids well separated. Correct establishing of the appropriate type of flow for sample fluids (diagonal flow) and for reagent fluids (symmetric flow bypassing the reaction channels) is taken care off by the geometric lay-out of the device.
[0042] In a further embodiment of a device according to the invention, the device further comprises an extraction channel connected to one of the manifolds.
[0043] Reaction products/fractioned components of the macromolecule may be collected and extracted from the reaction chamber through a suitable extraction channel connected to one of the manifolds, and either directly transferred to a subsequent processing stage or retrieved from an extraction port.
[0044] Preferably, the extraction channel is a wide, but shallow channel. In order to stretch out the macromolecule in the extraction channel, the height/depth of the extraction channel should be in the same length scale as the persistence length of the macromolecule, e.g. the characteristic length of the macromolecule representing the flexibility of the macromolecule. For double stranded DNA, this length is about 64 nm depending on salt concentration in the carrier fluid. A preferred range for the height/depth of the extraction channel is between 50 nm and 100 nm. The width of the extraction channel should be larger than this characteristic length so that the macromolecule can rearrange in order to resolve folds or similar disarrangements.
[0045] In order to facilitate high volume production of the device, defining the lateral dimensions of the device including the extraction channel should be compatible with microscale pattern transfer techniques, i.e. patterning techniques for reliably producing lateral feature widths of about 1 μm and above, such as UV-lithography, microinjection moulding or any other high volume micro-fabrication technique. In order to achieve a satisfactory yield in a laboratory scale production, the extraction channel width is typically larger than 4 μm. Furthermore, an extraction channel nanoslit with a micro-scale width is advantageous for avoiding excessive pressure build-up in the device and the associated fluidic system under operation. Therefore, the width of the extraction channel is preferably also adapted according to fluidic design considerations for a given type of application. In order to shunt a macromolecule into and through the shallow extraction channel, it is desirable to achieve a reasonable flow rate through the extraction channel, thereby avoiding excessive pressure build-up inside the device. Increasing the width of the channel is a mean to limit the maximum pressure to achieve the desired flow rate as high pressure can jeopardize the sealing of the device or the microfluidic handling system, such as pumps, valves, fluidic connectors, and the like.
[0046] As mentioned above, the device according to the invention may be integrated into an automated system for enzymatic processing and analysis of macromolecules. The automated system may comprise automated fluid handling for handling sample and reagent fluids. Any active components of the automated fluid handling system may be arranged external to the microfluidic device and interface with the microfluidic device through any known type of fluid connection technology.
[0047] A system for enzymatic processing of macromolecules comprising a device according to the invention may further comprise a machine vision system for the automated detection of a trapped macromolecule container in at least one of the reaction channels. A suitable machine vision system includes appropriate optics for imaging the macromolecule on an electronic image sensor using any known microscopic technique.
[0048] Furthermore, a system using the microfluidic device according to the present invention may comprise a nanofluidic processing/analysis portion, such as a sequencing portion or an amplification stage, arranged in direct extension of the extraction channel.
[0049] According to a further aspect of the invention, a method for preparing isolated macromolecules is provided. The method has the same advantages has mentioned above with reference to a microfluidic device for enzymatic processing of macromolecules.
[0050] A method for preparing isolated macromolecules and using a microfluidic device according to any of the above-mentioned embodiments comprises the steps of
[0051] a) at an input port connected to the first inlet, providing a first fluid containing macromolecule containers,
[0052] b) establishing a flow of the first fluid from the first inlet, via the first manifold, through the reaction channels, and via the second manifold to the first outlet,
[0053] c) stopping the flow, when a macromolecule container is detected in one of the reaction channels, thereby trapping the macromolecule container in said reaction channel,
[0054] d) at an input port connected to the second inlet, providing a second fluid containing an enzymatic reagent,
[0055] e) in at least one of the manifolds, replacing the first fluid by the second fluid by establishing a flow from the second inlet to the second outlet, wherein the flow of the second fluid essentially by-passes the reaction channels, and
[0056] f) allowing the enzymatic reagent to diffuse from the at least one manifold into the reaction channels to perform an enzymatic reaction releasing an isolated macromolecule from its container.
[0057] In a further embodiment of a method according to the invention, the macromolecule container is a metaphase chromosome and the macromolecule is a DNA-molecule.
[0058] In a further embodiment of a method according to the invention, a pre-defined level of enzyme concentration is maintained in the at least one manifold by maintaining in the at least one manifold a continuous flow of reagent with a pre-defined enzyme concentration.
[0059] In a further embodiment of a method according to the invention, in step c), trapping of the macromolecule container in one of the reaction channels is visually detected by an operator and/or by means of a machine vision system.
[0060] In a further embodiment of a method according to the invention, in step e) the first fluid is replaced by the second fluid essentially simultaneously in both manifolds, wherein at least for the reaction channel comprising the trapped macromolecule container, the hydrostatic pressures on either end of said reaction channel are balanced during said replacement.
[0061] In a further embodiment of a method according to the invention, the method further comprises the step of
[0062] g) transferring the isolated macromolecule via an extraction channel to a subsequent processing step, such as sequencing and/or amplification.
BRIEF DESCRIPTION OF THE DRAWINGS
[0063] In the following, the invention is described in detail with reference to schematic drawings, where like numerals refer to like parts. The drawings show on
[0064] FIG. 1 an embodiment of a microfluidic device according to the invention,
[0065] FIG. 2 a detail of the embodiment of the device shown in FIG. 1 ,
[0066] FIG. 3 cross-sectional view of the reaction chamber along line III-III in FIG. 2 ,
[0067] FIG. 4 cross-sectional view of the device along line IV-IV in FIG. 2 ,
[0068] FIG. 5 detail of the reaction chamber region of an alternative embodiment of a microfluidic device according to the invention in (a) a first operational state, and (b) in a second operational state,
[0069] FIG. 6 a - 6 d different operational states for a device according to another embodiment of the invention,
[0070] FIG. 7 a sequence of micrographs showing the filling of the manifolds with an enzymatic reagent and the diffusion thereof into the reaction channels,
[0071] FIG. 8 micrographs showing digestion of chromosomes in the reaction chamber,
[0072] FIG. 9 micrographs showing A) a released DNA molecule being shunted to the extraction port, and B) and C) details of the released DNA molecule in the extraction port, and
[0073] FIG. 10 a further embodiment of a device according to the invention.
DETAILED DESCRIPTION OF THE INVENTION
[0074] FIG. 1 shows schematically a microfluidic device 100 according to one embodiment of the invention. At the centre, the device 100 comprises a reaction chamber 101 (trap area) comprising reaction channels 102 defined by flow barriers 103 . A fluid sample may be loaded at a sample input port 112 and transferred to the reaction chamber 101 via a first inlet channel 110 . The sample fluid may leave the reaction chamber 101 via a first outlet channel 111 and is discharged at a sample output port 113 . Reagents may be provided in the form of a reagent fluid at a reagent input port 122 and are injected into to the reaction chamber 101 via a second inlet channel 120 . A flow of reagent fluid may leave the reaction chamber 101 via a second outlet channel 121 and is discharged through a reagent output port 123 . Processed samples may be retrieved through an extraction channel 130 and output at an extraction port 131 .
[0075] FIG. 2 shows schematically a detail of the reaction chamber portion 201 of a microfluidic device 100 according to one embodiment of the invention. Notably, the reaction chamber 201 has a square lay-out with a first edge 206 , a second edge 207 parallel thereto, and a third edge 208 and a fourth edge 209 essentially perpendicular to the first and second edges 206 , 207 . The reaction chamber 201 comprises a first manifold 204 and a second manifold 205 extending along the first edge 206 and the second edge 207 , respectively. The reaction chamber 201 further comprises reaction channels 202 defined by flow barriers 203 and extending from the first manifold 204 to the second manifold 205 in a direction essentially parallel to the third and fourth edge 208 , 209 . A first inlet 210 and outlet 211 are arranged at diagonally opposing corners of the square, wherein the principal axis of the first inlet channel 210 and the second outlet channel 213 are oriented at an angle of about 45 degrees with respect to the flow barriers 203 and thus with respect to the reaction channels 202 . This arrangement of reaction chamber layout and sample fluid inlet/outlet configuration provides for an improved distribution of the sample fluid flow throughout the reaction chamber 201 , thereby facilitating an even filling of the reaction channels 202 .
[0076] A second inlet 220 and outlet 221 are arranged at the third and fourth edge 208 , 209 , respectively. The reaction chamber is essentially symmetric with respect to a mirror axis M connecting the second inlet 220 and the second outlet 221 , and a longitudinal axis of the reaction channels 202 is oriented perpendicular to the mirror axis M. Both the second inlet 220 and the second outlet 221 are in symmetric fluid communication with both the first and the second manifold 204 , 205 through edge channels 298 , 299 extending parallel to the reaction channels 202 along the third and fourth edge 208 , 209 .
[0077] The reaction channels 202 thus act as zones for isolation of a macromolecule container (e.g. chromosome, nucleus, or cell) from which a macromolecule/polymer (e.g. Nuclear Acid) can be released. The released macromolecule can then be passed to an extraction channel 230 from where it may be retrieved for subsequent processing, for example through an extraction port 231 .
[0078] FIG. 3 shows schematically a cross-sectional view of the reaction chamber along line III-III in FIG. 2 . The microfluidic device 300 comprises a micro-structured first part 341 with access holes 342 , 343 for access to the sample input and output ports 312 , 313 , respectively. A cover part 340 is bonded to the first part 341 so as to define closed microfluidic channels. The cross-section passes from the sample inlet port 312 through the first inlet channel 310 , via the first manifold 304 , through reaction channels 302 defined by flow barriers 303 , via the second manifold 305 , and through the first outlet channel 311 to the sample output port 313 .
[0079] FIG. 4 shows schematically a cross-sectional view of the device along line IV-IV in FIG. 2 . As in mentioned above with respect to FIG. 3 , a micro-structured first part 441 defines together with a cover part 440 the fluid channels of the device. The cross-section illustrates how a released macromolecule 452 is transferred from a coiled state in the second manifold 405 to a linearized state in the extraction channel 430 and further to a recoiled state in an extraction port 431 . Note, that the first part 431 in lateral directions (i.e. in the plane of FIG. 2 ) may be patterned with micron-scale resolution techniques whereas in a vertical direction (i.e. in the plane of the cross-sections of FIG. 3 or FIG. 4 ) shallow milling may be performed to achieve nano-scale structures in some regions, and micron-scale milling may be performed to obtain deeper channels in other regions. In particular, the extraction channel 430 may have a depth c of 100 nm, whereas the depth of the manifold 405 is for example 10 μm. Also the length a of the extraction channel is chosen depending on the application, and is for example 450 μm, but may also be several millimetres or even a few centimetres.
[0080] FIG. 5 shows schematically a detail of the reaction chamber region of an alternative embodiment of a microfluidic device according to the invention. Like the embodiment of FIG. 2 , the reaction chamber 501 has a square layout with a first manifold 504 and a second manifold 505 , both manifolds 504 , 505 extending in a first direction along parallel edges of the square. Reaction channels 502 are defined by flow barriers 503 extending perpendicular thereto from the first manifold 504 to the second manifold 505 . s 502 . A shallow extraction channel 530 is centrally connected to the second manifold 505 .
[0081] The embodiment of FIG. 5 differs from the embodiment of FIG. 2 in the arrangement of fluid connection channels 510 , 511 , 514 , 515 connecting the reaction chamber to fluidic interface ports (not shown) of the device. The four fluid connection channels 510 , 511 , 514 , 515 extend outwardly from the four corners of the rectangle, one connection channel from each corner, at an angle of between 30 and 60 degrees, preferably about 45 degrees with respect to the direction of the reaction channel. As shown in the schematic drawing, the connection channels 510 , 511 , 514 , 515 have essentially the same dimensions and are arranged mirror symmetrically at least with respect to a centre axis M.
[0082] FIG. 5 a shows a first operational state, where a diagonal flow is established for filling the reaction chamber 501 with a sample fluid. Due to the symmetry of the device, any of the connection channels 510 , 511 , 514 , 515 may be chosen as a first inlet channel for injecting the sample fluid (here 510 ). A diagonal flow is established by using the connection channel at the diagonally opposing corner as the first outlet channel (here 515 ), while keeping the two other connection channels blocked/closed (here 511 , 514 ).
[0083] FIG. 5 b shows a second operational state, where parallel reagent flows are established in both manifolds 504 , 505 by simultaneously injecting reagent into the first manifold 504 and the second manifold 505 through connection channels at the same edge and discharging the reagent through corresponding connection channel at the opposite edge. In the operational state shown in FIG. 5 b , reagent is injected from connection channel 510 acting as a second inlet channel, passes through the first manifold 504 , and is discharged through connection channel 511 acting as a second outlet channel. Symmetrically thereto, reagent is simultaneously injected from connection channel 514 acting as a second inlet channel, passes through the second manifold 505 , and is discharged through connection channel 515 acting as a second outlet channel. The flow and pressure in both manifolds 504 , 505 may be controlled independently, and is adjusted to bypass the reagent channels 502 such that the macromolecule containers are fluidically immobilised in the stagnant volume of the reaction channels 502 . Typically in practice, this is done by balancing the pressure in the two manifolds 504 , 505 so as to achieve substantially equal pressures on either end of each of the reaction channels 502 .
[0084] Referring to FIG. 10 , a microfluidic device 1000 according to a further embodiment may comprise a first component for trapping/isolating macromolecule containers and releasing a single macromolecule therefrom by means of an enzymatic reaction in a reaction chamber 1001 . Advantageously, the first component may essentially correspond to the above-mentioned embodiments, e.g. as described with reference to FIG. 1-4 . The released macromolecule may be shunted to an extraction channel 1030 , and passed to a subsequent second component of the device 1000 , arranged in direct extension of the extraction channel 1030 . The second component comprises a first nanoslit 1030 a, a second nanoslit, 1030 b, and a third nanoslit 1030 c, which together with the nanoslit of the extraction channel 1030 form a cross with a longitudinal axis defined by two channels 1030 and 1030 a, and a transverse axis perpendicular thereto by the two other channels 1030 b, 1030 c. The channels 1030 a - c may be accessed through fluidic interface ports 1031 a - c. The nanoslits 1030 , and 1030 a - c have typically the same height of up to a few hundred nanometres, typically about 100 nm, depending on the actual application. The width of the channels may be between a few micrometres up to a couple of hundred micrometres, typically about 50 μm, compatible with state-of-the-art microscale pattern transfer techniques.
[0085] The longitudinal channels 1030 , 1030 a of the cross in the second component may be used to linearize, stretch, observe/sequence, label or otherwise analyse/process the single macromolecule produced in the first component. The transverse channels 1030 b, 1030 c may be used for fluidic manipulation of the macromolecule, and/or for providing additional reagents as required by the processes performed in the second component. The combination of the first and the second component in the integrated device 1000 of FIG. 10 has the advantage that the analysis/processing steps in the second component benefit from the ultra-long macromolecules that are produced in the first component.
EXAMPLE
[0086] Referring to FIGS. 6 a - 6 d, 7 , 8 and 9 , in the following, an example is given for the design, fabrication and use of a device for handling and releasing DNA from metaphase chromosomes. FIG. 6 gives a schematic view of the device used in the example and its operation. FIGS. 7-9 show micrographs visualising different aspects of the operation of the device. The device design of the example aims to immobilize a single metaphase chromosome in an isolation zone through which reagents can be exchanged by diffusion enabling proteins to be digested. The DNA thus extracted can then be shunted out of the isolation zone into a nanoslit for stretching.
[0087] FIG. 6 shows schematically a sequence of operational states for a device according to another embodiment of the invention. The device of FIG. 6 has, apart from the number of reaction channels 602 , the same configuration of the reaction chamber region, and in particular of the first inlet/outlet channels 610 , 611 , the second inlet/outlet channels 620 , 621 , and the extraction channel 630 . The sequence shows in FIG. 6 a loading of a sample 650 containing metaphase chromosomes 651 . The sample 650 is loaded at an input port 612 , which is connected to the reaction chamber 601 via first inlet channel 610 . Referring to FIG. 6 b , the reaction chamber 601 is filled with the sample 650 by establishing a diagonal sample flow through the reaction chamber 601 : a sample injection flow 660 through first inlet channel 610 transfers the sample fluid 650 to a first manifold flow 661 . The first manifold flow 661 branches into a number of reaction channel flows 662 . After passing the reaction channels 602 , the reaction channel flows 662 are collected by a second manifold flow 663 , which is leaves the reaction chamber in a sample discharge flow 664 . Single chromosomes 651 carried by the reaction channel flows 662 may be observed by optical microscopy, and the sample flow may be stopped when the presence of an isolated target chromosome 651 is determined. FIG. 6 c shows how protease is introduced in the reaction chamber 601 without displacing the chromosome 651 of interest by establishing a pressure balanced parallel flow through the manifolds 604 , 605 . A reagent injection flow 670 carrying protease splits essentially symmetrically into a first manifold flow 671 and a second manifold flow 672 , and recombines again before leaving the reaction chamber 601 in a reagent discharge flow 674 . The manifolds flows 671 , 672 essentially by-pass the reaction channels 602 . The protease enters the reaction channels 602 by diffusion 672 to act on the immobilised target chromosome 651 in order to release a DNA molecule 652 . In FIG. 6 d , the released DNA 652 is retrieved from the reaction channel 602 and shunted to the extraction port 630 by applying appropriate shunting pressures 680 , 681 , 682 , 683 through the connection channels 610 , 611 , 620 , and 621 , respectively. The released DNA 652 is stretched through a 100 nm high, 450 μm long and 50 μm wide nanoslit forming the extraction channel 630 .
[0088] The device was designed, with the aid of finite element simulations (COMSOL, USA), to have a series of isolation zones to slow down the chromosomes in the trap area while maintaining a high flow rate through the device. The parallel isolation zones increased in area with increasing distance (3000 μm 2 , 6000 μm 2 , 9000 μm 2 , etc.) from the sample entry point, in order to obtain a homogeneous flow rate into each of the zones during the introduction of the sample. This was to ensure that all chromosomes entering isolation zones were moving at the same horizontal speed in order to facilitate selection of individual chromosomes from the parade of chromosomes and cell debris flowing through the device.
[0089] The device was fabricated using UV lithography and reactive ion etching of a silicon substrate. Briefly, a 500 nm dry thermal oxide was grown on a silicon wafer. The protease inlet slit and the slit for DNA stretching were defined by UV masking and deep reactive ion etching in the oxide at the depth of 500 nm and 100 nm, respectively. The 50 μm wide microfluidic channels connecting the inlet ports and the 400×400 μm trap area were defined using a third UV lithography step and were etched in silicon at a depth of 10 μm. A thermal oxide was grown in order to later allow fusion bonding. Inlet holes were made by powder blasting from the backside of the device which was finally sealed by fusion bonding to a 500 μm thick borofloat glass wafer.
[0090] FIG. 7 visualizes the filling of the manifolds with an enzymatic reagent and the diffusion thereof into the reaction channels. The protease reagent was introduced from the second inlet port (located at the top edge of the frames) with flow occurring perpendicular to the reaction channels acting as isolation zones for the isolation of individual chromosomes. In this configuration there was no flow into the isolation zones; reagent exchange with the stagnant volume inside the isolation zones occurred by diffusion only. We used streptavidin labelled with Cy3 to visualize the diffusion of the reagent into the isolation zones to verify device operation before chromosome isolation and protease digestion was conducted. Observation of the introduction and spread of the Cy3 fluorescent marker into the isolation zones validated the device design and indicated that the reagent is able to spread quite well throughout the isolation zones by time, 300 s. The sequence of micrographs was taken with a time-lapse of 30 s between frames and shows the increasing fluorescence in the reaction chamber (“trap area”) due to the diffusion of stretavidin-Cy3 as it is injected at 0.6 nL min −1 . The diffusion constant is 60×10 −12 m 2 s −1 .
[0091] After experimental verification of the device design, the sample and reagent exchange process was applied to a sample containing metaphase chromosomes. The chromosomes were isolated from Jurkat cells (DSMZ, Germany: ACC282) in a polyamine buffer as described by Cram et al. (L. S. Cram, C. S. Bell and J. J. Fawcett, Methods Cell Sci., 2002, 24, 27-35) with some modifications. Briefly, the Jurkat cells were grown at 37° C. in a 5% CO 2 atmosphere. At exponential growth, they were arrested in metaphase with colcemide at 0.06 μg mL −1 for 12-16 hours. The cells were collected at 200 g for 10 minutes and re-suspended in a swelling buffer (55 mM NaNO 3 , 55 mM CH 3 COONa, 55 mM KCl, 0.5 mM spermidine, 0.2 mM spermine) at approximately 10 6 cells per mL and incubated for 45 minutes at 37° C. The swollen cells were collected at 200 g for 10 minutes and re-suspended in an ice-cold isolation buffer (15 mM Tris-HCl, 2 mM EDTA, 80 mM KCl, 20 mM NaCl, 0.5 mM EGTA, 0.5 mM spermidine, 0.2 mM spermine, 0.12% digitonin, and 7 mM mercaptoethanol) at approximately 8×10 6 cells per mL. The cells were lysed by vigorous vortex for 30 s. The chromosome content was estimated to be in the order of 10 7 cells per mL.
[0092] The device was mounted on a holder interfacing the inlet holes of the device with pressured air allowing movement of the solution inside the device as described elsewhere (W. Reisner, N. B. Larsen, H. Flyvbjerg, J. O. Tegenfeldt and A. Kristensen, Proc. Natl. Acad. Sci. U.S.A., 2009, 106, 79-84). Fluorescence imaging was performed using an inverted microscope (Nikon Eclipse TE2000, Japan) equipped with a 60×/1.00 water immersion objective and an EMCCD camera (Photometrics Cascade II512, USA). The temperature inside the device was controlled by a cartridge heater held in contact with the backside of the silicon device. Inlet holes were loaded with 30 mL of solution unless otherwise mentioned.
[0093] Prior to receiving the chromosomes 651 , the device was flushed by 1% sodium dodecyl sulfate, buffer solution (0.5_TBE, 3% b-mercaptoethanol (BME) and 0.5% Triton X-100) and BSA at 1 mg mL −1 for 10 minutes. A sample 650 with 1000-2000 chromosomes 651 were added to the diagonal sample inlet port 612 ; the depth of the microfluidic structure allowed the cell extract to be flushed quickly through the isolation zones formed by the reaction channels 602 while watching for the appearance of chromosomes 651 that could be isolated. A single chromosome 651 was trapped in a reaction channel 602 of the device.
[0094] Simultaneously the temperature was adjusted to 37° C. and a 100 μg mL −1 solution of protease K (1 mM of YOYO-1 is added to the protease K solution for staining the DNA strands while cut free from the chromatin in the vicinity of the bright chromosome body) was introduced. The device enabled a high flow rate of 0.6 nL min −1 allowing the protease to diffuse quickly into the stagnant volume within the isolation zone 602 .
[0095] Moreover, a continuous flow 670 , 671 , 672 , 673 , 674 through the device ensured that after 4 minutes the protease concentration around the isolated chromosome 651 was maintained above 50 μg mL −1 and that the digestion products were washed away from the isolation zone through diffusion.
[0096] The series of micrographs in FIG. 8 (A) shows the digestion of a single metaphase chromosome 651 with protease at 37° C. Subsequent frames are taken with a time-lapse of 5 minutes. As proteolysis took place, the chromosome 651 swelled and self-aligned in the plane of the device allowing reliable and reproducible fluorescence time-lapse imaging. Although no visible change of the chromosome 651 was observed after t=25 minutes, digestion was allowed to proceed for one hour as recommended by protocols for digestion in bulk solution (J. Sambrook, E. F. Fritsch and T. Maniatis, Molecular Cloning: a Laboratory Manual, Cold Spring Harbor Laboratory, 1989). FIG. 8 (B) shows different individually isolated chromosomes after 40 minutes digestion. Even after a digestion treatment that should be sufficient to remove all proteins, sister chromatids could still be clearly identified and chromosomes of different sizes and with different centromere positions could be seen. Moreover heterogeneity in the chromatin folding morphology could be observed at the micrometre scale.
[0097] The chromosomal DNA 652 could be easily manipulated by using the sample inlet/outlet microchannels 610 , 611 and the reagent inlet/outlet slits 620 , 621 as a bi-directional flow system inside the reaction chamber 601 . This enabled the chromosomal DNA 652 to be moved in front of the 100 nm high nanoslit forming the extraction channel 630 and then forced in. Although, the bi-directional flow in the reaction chamber 601 would enable DNA 652 extracted from chromosomes 651 trapped in different isolation zones 602 to each be individually manipulated and moved toward the extraction channel 630 , in the present example a dilute solution of chromosomes 651 was used and only one chromosome 651 at a time was processed.
[0098] After completion of the digestion, DNA 652 released from an individual chromosome 651 is passed through a 100 nm high nanoslit forming the extraction channel 630 . FIG. 9A shows a micrograph of a released DNA molecule 652 being shunted to the extraction channel 630 ; The post-digestion chromosomal DNA 652 was observed as a densely packed core composed of separated loops. The chromosomal DNA 652 was highly pliable: the DNA 652 stretched by increasing the flow through the nanoslit 630 and recoiled when the flow was stopped.
[0099] FIG. 9B and FIG. 9C show micrographs with details of the released DNA molecule 652 in the extraction channel 630 . FIG. 9B is a close-up of loops of DNA emanating from the core package of the chromosomal DNA. FIG. 9C is a close-up of the linear DNA strand emerging from the DNA package. A longer separate strand stretched across the whole length of the 450 μm long nanoslit and out into a microchannel ( FIG. 4C ). This corresponded to a minimal length of about 1.3 Mbp (1.3 million bases) of fully elongated DNA. Such separated DNA strands were also visible around the chromosomal DNA before the introduction to the nanoslit.
LIST OF REFERENCE NUMBERS
[0100] Throughout the application, like numerals refer to like parts, wherein x is to be replaced by the numbers 1, 2, 3 . . . 10 as appropriate.
[0101] x 00 device
[0102] x 01 reaction chamber
[0103] x 02 reaction channel
[0104] x 03 flow barrier
[0105] x 04 , x 05 first and second manifold
[0106] x 06 -x 09 first, second, third and fourth edges
[0107] x 10 , x 11 inlet/outlet channel
[0108] x 12 , x 13 connection ports
[0109] x 14 , x 15 inlet outlet channel
[0110] x 20 , x 21 inlet/outlet channel
[0111] x 22 , x 23 connection ports
[0112] x 30 extraction channel
[0113] x 31 connection port
[0114] x 40 , x 41 device parts
[0115] x 42 , x 43 connection holes
[0116] x 50 sample
[0117] x 51 macromolecule container
[0118] x 52 macromolecule
[0119] x 60 -x 64 sample flow
[0120] x 70 , x 71 reagent flow
[0121] x 72 reagent diffusion
[0122] x 73 , x 74 reagent flow
[0123] x 80 -x 83 fluidic manipulation
[0124] x 98 , x 99 edge channels
[0125] 1030 a - c nanoslits
[0126] 1031 a - c connection ports
[0127] M symmetry axis
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A microfluidic device and method for enzymatic processing of ultra-long macromolecules is accomplished using a microfluidic device a reaction chamber with a first manifold, a second manifold, and a plurality of reaction channels. Each reaction channel extends from the first manifold to the second manifold. First inlet and outlet channels fill the reaction channels via the manifolds with one or more macromolecule containers suspended in a first carrier fluid. The first inlet and outlet channels are configured such that a flow is guided through the reaction channels, and an enzymatic reagent is fed to the reaction chamber essentially without displacing the macromolecule containers trapped in the reaction channels. The second set of inlets and outlets are configured such that a flow established from the second inlet to the second outlet is guided through at least one of the manifolds and bypasses the reaction channels.
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BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates generally to multi-player board games and more particularly to a multi-player interactive board game especially adapted to effect the instruction of Biblical Christianity through Biblical teachings.
2. Description of the Prior Art
Board games for the instruction of Christian values and Biblical teachings are known in the art of multi-player board games. U.S. Pat. No. 5,377,991 issued to Olsen discloses a Game Method and Apparatus. This game includes a board on which players transit the perimeter according to a certain set of parameters. U.S. Pat. No. 5,071,133 issued to Smith discloses a Board Game for Teaching Biblical Principles. The game includes a board on which players transit the perimeter according to a certain set of parameters. U.S. Pat. No. 5,042,816 issued to Davis et al. discloses a Biblical Question and Answer Board Game. The game includes a board on which players transit the perimeter according to a certain set of parameters.
Thus, while the foregoing body of prior art indicates it to be well known to use a board game to teach Biblical principles, no known game employs the same method of play as the instant invention. The prior art does not teach the use of a unique board playing surface combined with playing pieces shaped as Bibles, the gathering and collecting of objects, the drawing of cards and the use of a timer. Nor does the prior art described above teach or suggest a board game device which may be used by individuals to teach Biblical principles according to the unique method of play provided. The foregoing disadvantages are overcome by the unique rules and gaming components of the present invention as will be made apparent from the following description thereof. Other advantages of the present invention over the prior art also will be rendered evident.
SUMMARY OF THE INVENTION
To achieve the foregoing and other advantages, the present invention, briefly described, provides an instructional board game designed to teach spiritual principles as taught in the Bible. The game is designed to be an interactive multi-player game which includes a board, player tokens, various collectable items, dice, cards and a timer. The board is generally rectangular and may fold, the board further includes a playing surface which has a number of squares and indicia printed thereon. The squares are shaped generally as to form a tree shape and and are centrally located on the board. The squares form rows, there are 14 rows on the playing board. These 14 rows form 7 pairs of rows, the first row pair is located at the bottom of the playing board and the 7th row pair is located at the top of the playing board. The second through sixth row pairs of rows are located intermediate the first row pair and seventh row pair on the playing board. Each of the seven pairs of rows are associated with a "Growth" level. The tree has seven growth levels. They are: Goodness, Knowledge, Self-Control, Perserverence, Godliness, Brotherly Kindness, and Love. Surrounding the tree are eight stacks of cards. Seven of the stacks of cards are associated with the seven aforementioned growth levels. An eighth stack of cards is located near the bottom of the board and is associated with Sin.
A player enters the playing surface through a path. A six sided dice is used which indicates the number of squares that the player may move. The path includes six squares. There are three types of squares on the path. They are "Hard Path", "Rocky Soil" and "Thorny Ground". The player must inevitably land on one of the aforementioned squares. A question is asked the player from a preprinted list which is in some fashion symbolic of the square which the player has landed on. When the player correctly responds, they would roll again in turn.
A player will enter the "Fertile Soil" squares after a certain number of plays. At this point in the player's game life, they become a Christian. At this point their token is separated in half and half of the token is placed in heaven. Heaven is defined as some location off or on the board. The token is in the shape of a Bible and may separate in half. Also, when the player enters the "Fertile Soil" square, his/her name is entered in the "Book of Life".
There are three types of squares a player may land upon during the main course of play. They are a "sin" square, a "growth" square, or a "fruit bearing" square. These squares have identifying indicia located thereon which permits the player to easily identify which square they have landed upon. When a player lands on a "growth" square a playing card from the growth card stack is drawn. The growth card drawn is from the growth card stack associated with the players position on the playing board, specifically which pair of rows the player resides in. The "growth" card includes a question related to the Biblical principle described in the stack. The answer to the question posed is written upside down at the bottom of the growth card. If the question is answered correctly, the player is granted a bonus roll of the dice. There is a maximum of one bonus roll per turn. If the question is answered incorrectly, the correct answer will be read aloud to all players. Each pair of rows is associated with a specific growth level as mentioned above. This arrangement will be more specifically addressed in the detailed description of the drawings.
When a player lands on a "Sin" square a card is drawn from the sin card deck. The sin card details the particulars of a sin committed and hands down a just chastisement, the erring player must move back five squares. Players who may have a variety of sin episodes may only backslide down to the "fertile soil" square.
The above brief description sets forth rather broadly the more important features of the present invention in order that the detailed description thereof that follows may be better understood, and in order that the present contributions to the art may be better appreciated. There are, of course, additional features of the invention that will be described hereinafter and which will form the subject matter of the claims appended hereto.
In this respect, before explaining at least the preferred embodiment of the invention in detail, it is to be understood that the invention is not limited in its application to the details of the construction and to the arrangements of the components set forth in the following description or illustrated in the drawings. The invention is capable of other embodiments and of being practiced and carried out in various ways. Also, it is to be understood, that the phraseology and terminology employed herein are for the purpose of description and should not be regarded as limiting.
As such, those skilled in the art will appreciate that the conception, upon which this disclosure is based, may readily be utilized as a basis for designing other structures, methods, and systems for carrying out the several purposes of the present invention. It is important, therefore, that the claims be regarded as including such equivalent constructions insofar as they do not depart from the spirit and scope of the present invention.
It is therefore an object of the present invention to provide a new and improved Bible board game which permits the instruction of Biblical principles in a fun and interactive manner.
It is another object of the present invention to provide a new and improved Bible board Game which may be easily and efficiently manufactured and marketed.
It is a further objective of the present invention to provide a new and improved Bible board game which is of durable and reliable construction.
An even further object of the present invention is to provide a new and improved Bible board game which is susceptible of a low cost of manufacture with regard to both materials and labor, and which accordingly is then susceptible of low prices of sale to the consuming public, thereby making such a Bible board game available to the buying public.
These together with still other objects of the invention, along with the various features of novelty which characterize the invention, are pointed out with particularity in the claims annexed to and forming a part of this disclosure. For a better understanding of the invention, its operating advantages and the specific objects attained by its uses, reference should be had to the accompanying drawings and descriptive matter in which there are illustrated preferred embodiments of the invention.
BRIEF DESCRIPTION OF THE DRAWINGS
The invention will be better understood and the above objects as well as objects other than those set forth above will become more apparent after a study of the following detailed description thereof. Such description makes reference to the annexed drawings wherein:
FIG. 1 is a top view showing the general configuration of the playing board of the instant invention.
FIGS. 2A through 2J describe the different interactive squares that the player will land on during the course of the game.
FIGS. 3A through 3F describe the specific board pieces and devices that will be utilized during the course of the game.
DESCRIPTION OF THE PREFERRED EMBODIMENT
With reference now to the drawings, a new interactive board game teaching Biblical principles in a fun and thoughtful fashion embodying the principles and concepts of the present invention will be described,
Turning initially to FIG. 1, there is shown a first exemplary embodiment of the Good News Bible Board Game of the invention generally designated by reference numeral 10. In its preferred form, the Bible board game 10 comprises a generally rectangular board 20. The board 20 may be constructed of cardboard or other suitable material. The board 20 may include a layer of lamination which has indicia and/or other figures printed thereon. The board 20 includes a centrally disposed playing surface 30. The playing surface 30 includes a variety of squares 32. The squares 32 are generally arranged in rows. The squares 32 generally form a playing surface 30 which is shaped like a tree. The playing surface 30 is entered through a path 34 which would approximate the appearance of a root and trunk of the tree shaped playing surface 30. The tree shaped playing surface 30 has a lower section and an upper section, said lower section proximal the trunk 34 and said upper section proximal the Well Done Good and Faithful Servant Square 118.
Surrounding the tree shaped playing surface 30 is a plurality of rectangles which are designed to have interactive playing cards placed atop their location. These rectangles are associated with different Biblical principles. Goodness 42, Self-Control 44, Godliness 46, Love 48, Brotherly Kindness 50, Perseverance 52, Knowledge 54, and Sin 56 surround the playing surface 30 in a counter-clockwise fashion. When a player lands on a Growth Square in a particular row, the associated interactive card is drawn from the correct deck. A growth square has a "G" designation. This designation is for the purposes of explanation of the course of the game alone, the final designation may be different. Growth squares 60 are associated with Goodness 42. Growth squares 62 are associated with Knowledge 54. Growth squares 64 are associated with Self-Control 44. Growth squares 66 are associated with Perseverance 52. Growth squares 68 are associated with Godliness 46. Growth squares 70 are associated with Brotherly Kindness 50. Growth squares 72 are associated with Love 48. Note how the growth squares 60 are located as the last right squares on the first and second rows. The growth squares 62 are located as the last left squares on the third and fourth rows. The growth squares 64 are located as the last right squares in the fifth and sixth rows. The growth squares 66 are located as the last left squares on the seventh and eight rows. The growth squares 68 are located as the last right squares in the ninth and tenth rows. The growth squares 70 are located as the last left squares in the eleventh and twelveth rows. The growth squares 72 are located as the last right squares on the thirteenth and fourteenth rows. The player will move from right to left on row 1, then from left to right on row two, then from right to left on row three and so on and so forth, alternating the direction of travel at the end of each row.
Referring now specifically to FIGS. 2A through 2J, the interactive squares that a player may land on during the course of play are described. FIG. 2A shows the "Hard Path" square designated 100. This square may be landed on in the earliest part of the game, prior to the player becoming a Christian in gamelife. FIG. 2B shows the "Rocky Soil" square designated 102. This square may be landed on during the earliest part of the game, prior to the player becoming a Christian in gamelife. FIG. 2C shows the "Thorny Ground" square designated 104. This square may also be landed on during the earliest part of the game, prior to the player becoming a Christian in gamelife. When the "Hard Path", "Rocky Soil" or "Thorny Ground" squares are landed on the player must read a sample "life application" symbolic of the type of soil square the player has landed on. FIG. 2D shows the "Fertile Soil" square designated 106. This square is landed on during the early part of play and permits the player to become a Christian during gamelife. FIG. 2F is a "Fruit Bearing" square and is designated 108. When the player lands on this square a fruit icon is gathered by the player. One of the desirable things for a player to do during the course of the game is to gather fruit icons. FIG. 2E is a "Sin" square designated by 110. When the player lands on the "Sin" square 110 during the course of the game a "Sin" card is drawn from the stack of "Sin" cards. The "Sin" cards detail real life situations concerning the avoidance of Sin, the consequences of Sin, and undesirability of Sin. FIG. 2G is a "Growth" square designated 112. "Growth" squares 112 have the letter "G" centrally disposed therein for ease of identification in this disclosure. When a player lands on a "Growth" square 112 an appropriate growth card will be drawn. The final production design may be different in regards to the indicia identifying any of the squares. FIG. 2H is a combination "Growth and Fruit" square designated 114. When a player lands on the "Growth and Fruit" square 114 both a fruit icon and an appropriate growth card will be drawn. FIG. 2J is the "Well Done Good & Faithful Servant" square designated 118. When the player transits the entire length of the board 30 the player's icon will be placed in the "Well Done Good & Faithful Servant" square 118. This is synonymous with the player going to Heaven. The specific interactions between players, movement and specific actions to be taken will become more clear during the discussion of the Rules of Play. It is to be understood that the above mentioned indicia may be changed in the final production game version.
Referring now to FIGS. 3A-3F the specific board pieces and devices are shown. FIG. 3A shows a timer 120. Timer 120 will be utilized during the game to represent Christ's Second Coming. Christ's Second Coming is a Christian belief which coincides with the end of the world where true Christian believers will ascend to Heaven. At the beginning of play, the timer 120 is set to an arbitrary time period. When the timer 120 reaches the preset time, the game ceases.
FIG. 3B shows dice 122. The dice 122 are rolled to determine the number of spaces a player may move during their turn. The dice 122 may also be utilized to determine the order of play. A pair of six sided dice 122 are shown in FIG. 3B. It is to be understood that any device which imparts a random number may be utilized to generate the number of spaces that a player may move. In the preferred embodiment a single six sided die will be employed.
FIG. 3C shows player icon 124. Player icon 124 is shaped in the form of a Bible. The Player icon 124 will come in an assortment of colors in order to differentiate between the different players. During the course of play the player icon 124 may be separated into two parts along line 126. One of these parts will be continued to be utilized as the player icon and the other will demonstrate a Biblical principle which will become apparent during the discussion of the rules of play.
FIG. 3D shows a miniature apple 128. The miniature apple 128 will be awarded to a player whose player icon 124 lands on a "Fruit Bearing" square 108. The collection of miniature apples 128 is a fundamental element of play, the number of miniature apples 128 one has collected is a good measure of how well one is doing in the game in reference to the other players.
FIG. 3E shows a miniature sapling 130. The miniature apples 128 may be traded in for a miniature sapling 130. This describes another Biblical principle which will be more evident during the discourse of the Rules of Play.
FIG. 3F shows a basket 132. Both the miniature apples 128 and the miniature saplings 130 may be collected in the basket 132 during the course of the game. The basket 132 will come in an assortment of colors as well, the player icon 124 may be the same color as the basket 132.
The previous discussion of the game board, elements, and general layout are designed only to put forth one embodiment of the instant invention. Other configurations are possible and will be covered in the scope of the appended claims.
RULES AND METHOD OF PLAY
In order to better understand the disclosed invention, a version of the rules which incorporates the major concepts of the game are presented. It is to be understood that these rules may be modified or changed within the scope of game disclosure.
The first phase of the game is known as "Genesis". In this phase of the game, the players select the player icon 124 (Bible) that they wish to use as their token for the game. The players year of birth determines the order of play. A possible alternative would be utilizing the toss of die 122 to determine the sequence of play. If possible a non-player should set the timer 120 to an undisclosed length of play time and places the timer 124 out of the view of the players. A possible alternative would be the players determining a time period that would be an agreeable time to play.
The intent of the first phase "Genesis" of the game is threefold. First to equate the game's ending with Christ's Second Coming. Second, to drive home the suddenness of Jesus's return as well as it inevitability. Thirdly, to stress the need for the Christian's diligence in their work to focus on their struggle.
The principle which is designed to be imparted to the players during the first phase "Genesis" is that Christ's second coming signals the end of the Christians struggle on Earth and heralds the Judgement which follows. The When (actual time of occurrence of Christ's Second Coming) is known to no one but God (Matthew 24:36/Mark 13:32).
The second phase of the game is known as "The Call". In this phase of the game the players will throw the die 122 to determine the number of squares their player icons 124 will move. The player inevitably lands on either a Hard Path square 100, a Rocky Soil square 102 or a Thorny Ground square 104. The player will read a sample life application determined by which square they reside on.
The intent of the second phase of the game known as "The Call" is twofold. First, to acquaint the player with the parable's symbolisms and interpretation as applied to real life situations. Second, to acquaint the players realization the he/she may have the type of infertile heart of which Jesus speaks.
The principle which is designed to be imparted to the players during the second phase "The Call" is that the Gospel often falls on unreceptive hearts where the devil can easily snatch the message away (Luke 8:12), or on eager but shallow hearts which, once beset by the world's problems and reproach, eventually fall away (Luke 8:13), or on hearts more concerned with the worries of this life and the pursuit of wealth (Luke 8:14).
The third phase of the game is called "Acceptance". The player enters this phase oil: the game when they land on the "Fertile Soil" square 106. The player then reads from a real life application having to do with repentance and acceptance. The player breaks the player icon 124 in half along line 126, placing half the icon in Heaven and half the icon on the Fertile Soil square 106 where he landed. The players name is entered in "The Book of Life". The "Book of Life" is not shown in the Figures, and may be as simple as a sheet of paper for game purposes. However, in the final game design, a more elaborate book of life may be provided.
The principles which are designed to be imparted to the players during the third phase "Acceptance" include highlighting the most important point of the Christian life, repentance and acceptance, by having the player's name entered in the "Book of Life" which assures the player of Salvation. Also, the principle of signifying a conversion, by reading aloud the application as well as reciting a sample acceptance prayer is provided. The third principle put forth in this segment of the game is to help the players realize the significance of the Christian name, that it does not come through birth or religious affinity, but at the point where he or she decides to follow Christ.
The principle which is designed to be imparted to the players during the third phase "Acceptance" is that if anyone accepts Christ into their life, that person becomes a new creation. The old self is gone; a new person has come (2 Corinthians 5:17).
The fourth phase of the game is called "Growth". The growth phase is the main phase of play and essentially includes the player transiting the board 30. The player will move the player icon 124 the number of squares indicated by the toss of the die 122. The player transits the board 30 in a square by square manner in a left to right fashion followed in the next row in a right to left fashion. When the player reaches the rightmost square in any given row, they proceed to the rightmost square in the row immediately above it, and begin traversing that row toward the left. When the player reaches the leftmost square in that row, they proceed to the leftmost square in the row immediately above it, and begin traversing that row toward the right. This zig-zag pattern is maintained throughout the game. The board 30 resembles a tree. The tree has seven growth levels, each growth level is represented by a pair of rows. The seven growth levels are Goodness, Knowledge, Self-Control, Perseverance, Godliness, Brotherly Kindness, and Love. The player icon 124 may land on several types of squares.
One type of square the player icon 124 may land on is a Growth Square 112. When the player lands on a growth square 112 they pick a card from an appropriate growth card stack. Growth squares 60 are associated with goodness growth cards 42. Growth squares 62 are associated with the knowledge growth cards 54. Growth squares 64 are associated with the self-control cards 44. Growth squares 66 are associated with perseverance growth cards 52. Growth squares 68 are associated with Godliness growth cards 46. Growth squares 70 are associated with brotherly kindness growth cards 50. Growth squares 72 are associated with love growth cards 48. The growth card drawn contains a question which the player must answer in order to advance. The correct answer is written upside down at the bottom of each card. If the question is answered correctly, the player is granted a bonus move. There is a maximum of one bonus roll per turn. If the player answers the question incorrectly, the player must remain on that growth square until the player answers the question correctly. There will be no roll of the die on the players next move, he merely picks the next card. All questions are read aloud, and if answered incorrectly, the correct answer is read aloud to edify all players.
The intent of the growth square 112 is manyfold. First, the intent is to educate players on sound Biblical principles and to reinforce through repetition the same principle through the creative structuring of the same question in different ways. Second, to build in topical studies by using different growth areas. Third, to concretely express the basic truth that one cannot grow as a Christian unless one is familiar with God's Word.
The principle which is designed to be imparted to the player by landing on the growth square includes that those who choose to follow Christ are slowly being transformed to becoming more like Him (2 Cor, 3:18). Also, that by possessing these Christlike qualities in increasing measure (2 Peter 1: 5-8) they escape the world's corruption and render the head-knowledge of Christ into one that is active and productive.
Another type of square the player icon 124 may land on is a Sin square 110. When the player lands on a sin square 110 they pick a card from the Sin card stack 56. The sin card details the occasion of sin and hands down just chastisement, that is specifically that the erring player moves back 5 spaces.
The intent of the sin square 110 is to illustrate the occasions of sin by using present day examples from the most blatant transgressions (murder, theft) to the subtlest (white lies, gossip). To stress that in God's eyes, sin is sin regardless of its nature or severity. Another intent is to instill in the player a conscious aversion to sin, the player will detest landing on the sin square. Other intents include to educate the player that succumbing to Sin hinders growth and blocks the Christians goal of pleasing God, as well as to educate the player on the different sources of sin: self, the world's system and Satan.
The principles behind the sin square 110 are as follows. Sin strains our fellowship with God because he cannot tolerate it. (Isaiah 59:1-2). He considers all sin equal in deserving punishment (Romans 3:23/James 2:10) and judges each one fairly (1 Cor 3:13-15). However, for the Christian, sin may hinder this fellowship but does not sever it. All the Christian needs to do is admit the sin, repent and draw back to God, who is always ready to forgive.
Another type of square that the player icon 124 may land on is the Fruit Bearing Square 108. When a player lands on a fruit bearing square 108 the player harvests one fruit (miniature apple) 128 and places it in the basket 132. As the game progresses and the player is able to harvest more fruits the player may trade in 5 fruits 128 for one sapling 130. No bonus turn is granted for landing on a fruit bearing square 108 as the players reward shall be in heaven.
The intent of the fruit bearing square 108 is to graphically illustrate the fruit bearing aspect of Christian life. Each fruit represents a person the player has shared with who repented and accepted Christ into their life. Another intent is to exemplify the discipleship process, that is, only 1 in 5 fertile hearts will probably grow to fruit bearing maturity. Also, the intent of the fruit bearing square 108 is to generate as much excitement in the sharing process as possible by having the player (Christian) desire to harvest as much fruit 128 as possible.
The principle behind the fruit bearing square 108 is that Christ has given the Christians the Great Commission; to go and make disciples of all the nations (Matthew 28:18-20). As one whose fertile heart the Gospel's seed had been planted, we are to eagerly look forward to bearing fruit, thirty, sixty, and even a hundredfold (Matthew 13:23).
The fifth phase of the game is called "Eternal Life". The eternal life phase is the final phase of play and essentially determines how the game ends. The game can end in two ways. First, the player reaches the last square at the top of the board 30. The game ends for that player, the other players continue to play. Secondly, the timer 120 sounds. The sound of the timer 120 heralds Christ's Second Coming. It marks the end of the game for all players. All players take inventory of their fruits and saplings and look forward to a blissful eternal life with God Almighty.
The intent of the eternal life phase is to teach the joy of having persevered, by God's grace, having been strengthened by His word. Also, to explain man's purpose in this world, specifically to please and serve the Lord. Another intent is to instill the certainty of Christ's Second Coming and the uncertainty of when it shall be.
The principles behind the eternal life phase are that we all strive to have efforts and intentions appreciated. What better acknowledgement is there that to hear God say, "Well done, Good and Faithful servant" (Matthew 25:21). This marks the culmination of the Christian's odyssey on Earth-whether it comes through physical death (Heb. 9:27) or when caught up in the clouds with Christ at His return (1 Thes 4:16-17). This too marks the start of eternity. Eternal life for those who confess that Jesus is their personal Lord and Savior (1 John 5:11-13); and eternal damnation for those who chose not to heed (Revelation 21:8).
There are several Miscellaneous Provisions of the game. For a faster game the following strategies may be employed. First, there may be no limit to the number of bonus rolls a Christian can garner and the player correctly answers questions posed. Their turn will end when the player can no longer successfully answer the questions posed. Secondly, when landing on a fruit bearing square 108, the player will be permitted one bonus turn.
A square is provided for fruit bearing combined with a growth square (FIG. 2H) 114. These are the growth squares combined with a fruit symbol. When a player lands on this square, the player reaps one bonus fruit if the question is answered correctly. An unacceptable answer voids the bonus.
If a player has a series of Sin encounters, ie: the player keeps landing on Sin squares 110, the player may only backslide to the Fertile Soil squares 106. When this happens the player picks from a special deck of cards known as the "Salvation Check" stack. The cards will ask the sinful player a question derived from key evangelism verses. Erring player will be restored if a correct answer is given by the awarding of a bonus roll. Erring player will neither regress or progress should answers to the questions be unacceptable. The player merely waits till the next turn and tries again.
The intent of the cascading sin encounter is to teach that one cannot loose their Salvation once it has been given to him by God. Also, it checks the players salvation through the review of key evangelism principles and verses. The reinforcement of one's acceptance by fellow Christians through the symbolic process of restoration is also provided. And perhaps the key intent of the cascading sin encounter is to symbolize the sad state of a Christian unfamiliar with God's words as this Christian leads an unproductive life for Christ.
The principles behind the cascading sin encounter as simply that Jesus promises to never reject those who turn to Him because it is God's will that He should not even lose one who is given to Him (John 6:37-40). However, this promise applies only to those who really belong to Christ, not all who cry "Lord!!--Lord!!" will enter the kingdom of Heaven (Matthew 7:21).
It is apparent from the above that the present invention accomplishes all of the objectives set forth by providing a new and improved Bible board game which permits the instruction of Biblical principles in a fun and interactive manner, which may be easily and efficiently manufactured and marketed, and is of durable and reliable construction.
With respect to the above description, it should be realized that the optimum dimensional relationships for the pads 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 those skilled in the art, and therefore, all relationships equivalent to those illustrated in the drawings and described in the specification are intended to be encompassed only by the scope of appended claims.
While the present invention has been shown in the drawings and fully described above with particularity and detail in connection with what is presently deemed to be the most practical and preferred embodiment(s) of the invention, it will be apparent to those of ordinary skill in the art that many modifications thereof may be made without departing from the principles and concepts set forth herein. Hence, the proper scope of the present invention should be determined only by the broadest interpretation of the appended claims so as to encompass all such modifications and equivalents.
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An instructional board game is provided which teaches spiritual principles as disclosed in the Bible to players of all ages. The game is designed to be an interactive multi-player game which includes a board, player tokens, various collectable items, dice, cards and a timer. The board includes a sequential pattern of rectangles which the players would move their tokens in response to a throw of the dice. The sequential pattern generally resembles a tree. The player will transit the board following the sequential pattern with the object of gathering "fruit", living a principled Christian life, avoiding Sin, and responding correctly to questions posed when the player lands the interactive squares. The game simulates a players journey through Christian life, with all joys, trials and tribulations therein, concluding with the timer signal which announces Christ's Second Coming. Christ's Second Coming denotes the end of the game, the player or players who have gathered the most fruit through their game life and have had their names entered in the "Book of Life" satisfy the winning conditions and thus go to Heaven. The instant game may be suitable for electronic gaming as well, that is, a computer game utilizing the method and layout may be provided.
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BACKGROUND OF INVENTION
The present invention relates generally to semiconductor device processing and, more particularly, to a method for forming a semiconductor device by uniformly etching dual, pre-doped polysilicon regions of the device.
The electronics industry continues to rely upon advances in semiconductor technology to realize higher-functioning devices in more compact areas. For many applications, realizing higher-functioning devices requires integrating a large number of electronic devices into a single silicon wafer. As the number of electronic devices per given area of the silicon wafer increases, the manufacturing process becomes more difficult.
A large variety of semiconductor devices has been manufactured having various applications in numerous disciplines. Such silicon-based semiconductor devices often include metal-oxide-semiconductor (MOS) transistors, such as P-channel MOS (PMOS), N-channel MOS (NMOS) and complementary MOS (CMOS) transistors, bipolar transistors, BiCMOS transistors, etc. Each of these semiconductor devices generally includes a semiconductor substrate on which a number of active devices are formed. The particular structure of a given active device can vary between device types. For example, in a MOS transistor, an active device generally includes a source and drain region, as well as a gate electrode for modulating current between the source and drain regions.
One important aspect of the formation of such devices, or portions thereof, relates to various photolithography and etching processes. In photolithography, a wafer substrate is coated with a light-sensitive material known as photoresist. Next, the wafer is exposed to light, wherein the light striking the wafer is passed through a mask plate. This mask plate defines the desired features to be printed on the substrate. After exposure, the resist-coated wafer substrate is developed. The desired features as defined on the mask are then retained on the photoresist-coated substrate, while unexposed areas of resist are washed away. The wafer having the desired features defined is thereafter subjected to etching. Depending upon the production process, the etching may either be a wet etch in which liquid chemicals are used to remove wafer material or a dry etch in which wafer material is subjected to a radio frequency (RF) induced plasma. One particular concern relating to the etching process is maintaining control over the etching of the features, notably in the gate electrode region of the MOS transistor.
More specifically, one of the challenges encountered during the gate etch process of submicron technologies is the control of the etch profile. In many modern submicron processes, the gate electrode is comprised of a composite of layers of materials stacked on top of one another, and is thus commonly referred to as a “gate stack.” In an exemplary process, a CMOS transistor may have a gate stack including a 1000 angstrom (Å) layer of tungsten (W), while a 500 Å of titanium nitride (TiN) provides a sheet resistance as low as 3 Ωf□ (ohms per square), and a higher breakdown voltage for the gate oxide.
A commonly used gate stack is amorphous silicon (a-Si) or polysilicon (poly-Si) on top of a thin gate oxide. The a-Si or poly-Si is typically doped with N-type carriers for NMOS or with P-type carriers for PMOS to obtain asymmetry threshold voltage between N-channel and P-channel devices for a CMOS device. As the technologies evolve, the dimensions of integrated circuits shrink. In turn, as the IC dimensions get smaller, a thinner gate oxide is needed to maintain a level of gate capacitance for the performance of the IC devices. To avoid increasing the capacitance above the desired level, it is thus necessary to maintain a high conductivity in the a-Si or poly-Si to prevent the depletion of carriers in the gate region. This depletion of carriers tends to make the a-Si or poly-Si appear as an additional “oxide thickness” contributing series capacitance component that tends to lower the overall gate capacitance.
For an exemplary process having a 100 Å oxide layer, if the gate stack contributes 5 Å of “oxide thickness,” the capacitance change would be about 5% (assuming other parameters are held constant). However, if a process has a 30 Å gate oxide layer, given a 5 Å change in thickness due to the oxide, the gate capacitance would change by about 20%. Therefore, the N-type and P-type doses required for the a-Si or poly-Si gate stack may be heavier. The thinning of the gate oxidation and the heavy doping of the a-Si and poly-Si with N-type or P-type carriers present a major challenge to the gate etch process.
Different doping types, doses, and activation level of the a-Si or poly-Si have a significant effect on the a-Si or poly-Si etch rate, as well as the etch profile. N-doped a-Si or poly-Si usually etches faster than P-doped a-Si or poly-Si in a plasma etch process. In adequately etching the P-type material, there is the possibility of etching the N-type material too much. In turn, any excessive etching may cause a localized breakthrough or “micro-trenching” of the thin gate oxidation in the bottom of the a-Si or poly-Si etch features.
In a typical a-Si or poly-Si gate plasma etching process, a main etch step with an optical endpoint is used to define the gate profile. The endpoint signal will trigger only when the a-Si or poly-Si begins clearing out of the wafer. At this point, there will be less N-doped a-Si remaining than P-doped Si. In addition, some N-doped a-Si may have been completely etched away. The etch process will break through the thin gate oxide and rapidly etch the underlying silicon substrate. After reaching the endpoint (or after the main-etch step) the process switches to a higher Si/SiO 2 selectivity over-etch step and completely removes all of the remaining a-Si (or poly-Si). The selectivity of the over-etch step is much more than that of the main-etch step. This assures a reasonable gate profile.
With a relatively thin gate oxide, micro-trenching is problematic, especially in N-doped areas. In a plasma etch process, gate etch profile is also very sensitive to the doping of a-Si or poly-Si. In addition, the doping profiles between N-doped and P-doped a-Si or poly-Si may be different. Accordingly, there is a need to maintain a good gate etch profile that is substantially free of micro-trenching and provides a consistent gate etch profile between N-type and P-type doped gate stacks, as well as good critical dimension control as the process technology approaches fractional microns in feature sizes.
SUMMARY OF INVENTION
The foregoing discussed drawbacks and deficiencies of the prior art are overcome or alleviated by a method for forming a semiconductor device, including forming a first locally doped semiconductor region of a first conductivity type and a second locally doped semiconductor region of a second conductivity type over an undoped, lower semiconductor region. A first etch is implemented to simultaneously create a desired pattern in the first and second locally doped semiconductor regions in a manner that also provides a first passivation of exposed sidewalls of the first and second locally doped semiconductor regions, wherein the first etch removes material from the first and second locally doped semiconductor regions at a substantially constant rate with respect to one another, and in a substantially anisotropic manner. A second etch is implemented to complete the desired pattern in the undoped, lower semiconductor region in a manner that protects the first and second locally doped semiconductor regions from additional material removal therefrom.
In another aspect, a method for forming a semiconductor device includes forming a locally doped N-type polysilicon region and a locally doped P-type polysilicon region over an undoped, lower polysilicon region. A first etch is implemented to simultaneously create a gate conductor pattern in the locally doped N-type and P-type polysilicon regions in a manner that also provides a first passivation of exposed sidewalls of the locally doped N-type and P-type polysilicon regions, wherein said first etch removes material from said locally doped N-type and P-type polysilicon regions at a substantially constant rate with respect to one another, and in a substantially anisotropic manner. A second etch is implemented to complete the gate conductor pattern in the undoped, lower polysilicon region in a manner that protects the locally doped N-type and P-type polysilicon regions from additional material removal therefrom.
BRIEF DESCRIPTION OF DRAWINGS
Referring to the exemplary drawings wherein like elements are numbered alike in the several Figures:
FIG. 1 illustrates a CMOS (complimentary metal oxide semiconductor) structure that may be fabricated in accordance with an embodiment of the invention;
FIGS. 2 through 4 illustrate various processing steps in forming the CMOS structure of FIG. 1 in accordance with conventional processing techniques; and
FIGS. 5-10 illustrate a method for uniformly etching dual, pre-doped polysilicon regions of a semiconductor device, in accordance with an embodiment of the invention.
DETAILED DESCRIPTION
Disclosed herein is a method for a forming semiconductor device by uniformly and simultaneously etching complementary, pre-doped polysilicon regions of the device so as to produce substantially equivalent shaped N-type and P-type gate conductors. As is described in greater detail hereinafter, locally doped N-type and P-type polysilicon regions are provided with sidewall passivation so as to enable the use of an etch chemistry that etches the N-type and P-type polysilicon at substantially the same rate, but without isotropic etching effects that would otherwise erode the sidewalls of the N-type region. Remaining undoped lower portions of the polysilicon layer may then be etched away and the structure annealed to drive the dopants into the undoped portions of the resulting poly-gate structures.
Referring initially to FIG. 1, there is shown a CMOS (complimentary metal oxide semiconductor) structure 100 that includes a substrate 102 , well regions 104 , 106 (N and P type, respectively), source/drain regions 108 , 110 , a gate oxide layer 112 , and a pair of gate conductors 114 , 116 formed over the gate oxide 112 . The gate conductors 114 , 116 are formed from a gate conductor layer, which typically includes a semiconductor material such as polysilicon with different dopants (e.g., N-doped polysilicon and P-doped polysilicon).
Conventionally, the structure 100 is formed as is shown in FIG. 2, wherein a patterned mask 118 (e.g., a hardmask of material such as TEOS, silicon nitride, CVD oxide, etc.) is used to pattern the doped regions 120 , 122 of the gate conductor layer into gate conductors. A plasma etch process is used in conjunction with the mask 118 to remove portions of the doped regions 120 , 122 of the gate conductor layer not protected by the mask 118 . Prior to gate conductor patterning and etching, the conductor layer is first deposited with non-doped polysilicon. For an NMOS device, both the gate conductor 114 and source/drain regions 108 (FIG. 1) are both doped with N-type dopant (e.g., phosphorus) by ion implantation, while for a PMOS device, the gate conductor 116 and source/drain regions 110 are both doped with P-dopant (e.g., boron).
As indicated previously, in order to improve device performance, it has become necessary to dope the gate conductor and source/drain diffusions of a MOS device with different types of dopant. For example, the N-type gate conductor 114 may be doped with phosphorus first, and thereafter the source/drain diffusions 108 are doped with arsenic to form N-type devices after the formation of the gate conductors 114 and 116 . In the case of P-type devices, it is preferable to first dope the P-type gate conductor with boron, and subsequently dope the source/drain diffusions 110 with boron difluoride (BF 2 ) after the formation of the gate conductors 114 and 116 . Moreover, it is sometimes necessary to anneal the gate conductors at higher temperature than the source/drain regions. Accordingly, because of the different dopants used for the gate conductor and the source/drain region, the gate conductor layer is pre-doped with P-type dopant in one region and N-type dopant in the remaining regions before patterning and simultaneous etching thereof.
As also indicated previously, the difficulty in simultaneously patterning the gate structures containing both N-doped and P-doped poly resides in the plasma etching thereof at similar rates and profiles. In general, N-doped poly etches faster and tends to be more isotropic than P-doped poly in plasma etching. This is illustrated in FIG. 3, where, in the un-annealed samples depicted, the N-type gate conductor 114 is shown to have excessive lateral etching in the implanted region as compared to P-type gate conductor 116 . FIG. 4 illustrates even more pronounced lateral etching in the N-type gate conductor sidewall resulting from an annealed sample. In either case, there is a strong loss of dopant in N-type poly conductor. In addition, the gate oxide 112 around the N-type poly is exposed to plasma for a longer duration than the P-type poly region since the N-type poly etches faster than the P-type poly. As a result, the thin gate oxide around the N-type poly region can easily be ruptured and is prone to punchthrough. Furthermore, the etched profile of the N-type poly is different from that of the P-type poly (as shown in FIGS. 3 and 4 ), resulting in different critical dimensions (CD).
Therefore, in accordance with an embodiment of the invention, there is disclosed a method uniformly etching dual, pre-doped polysilicon regions of a semiconductor device. Briefly stated, the present method addresses the above described concerns through a processing sequence that implants a first selected region of polysilicon with an N-type dopant, and a second selected region of the polysilicon with a P-type dopant to form locally doped regions. A hardmask is deposited and photolithographically exposed with photoresist. Then, the hard mask is etched, along with the first and second selected polysilicon regions (i.e., the locally doped regions) using the photoresist material. After this process, the photoresist material is stripped by the oxygen plasma and a passivation layer is formed on the sidewalls of the etched, implanted locally doped regions. Next, a less aggressive plasma etching is applied to remove the remaining polysilicon layer. The passivation layer prevents the N-doped region of the gate conductor from suffering sidewall etching in the less aggressive plasma etching. Thereafter, conventional processing may be continued such as, for example, annealing, doping of the source/drain regions, etc.
The present method is advantageous in that it is easier to control the profiles of the implanted layers in the presence of photoresist. In general, fluorine-type plasma etches P-type and N-type polysilicon at a similar rate, whereas N-type polysilicon is etched faster rate than P-type polysilicon in a chlorine or bromine-type plasma. On the other hand, a fluorine-type plasma tends to etch polysilicon isotropically. However, by etching in the presence of photoresist, the carbon-containing species released therefrom renders the process an anisotropic one to an extent, since the photoresist helps to passivate the initially etched sidewalls. Furthermore, the photoresist also serves to protect the hardmask.
After the locally doped regions of the polysilicon layer are etched, the photoresist used to form a passivation layer on the vertical surfaces of the partially formed gate structures of the N-doped and P-doped devices is removed. Thereafter, a less aggressive plasma etch may be used to remove the remaining undoped polysilicon layer to complete definition of the gate structure. In particular, an oxide sidewall passivation layer formed by plasma stripping of the photoresist prevents the N-doped region of the gate conductor from suffering excessive sidewall etching that is seen in conventional processing. FIGS. 5-10 illustrate in greater detail an embodiment of the present method, which utilizes this sidewall passivation.
Referring to FIG. 5, there is shown a processing stage of a CMOS structure formed upon a substrate 102 , including N-type well region 104 , P-type well region 106 , and gate oxide layer 112 formed thereupon. For ease of illustration, like elements of earlier figures are designated with the same reference numerals. An initially formed polysilicon layer 120 includes a locally doped N-type region 122 and a locally doped P-type region 124 atop the remainder of the undoped polysilicon 126 , as explained earlier. In the example illustrated, the N-type region 122 includes one or more N-type impurities implanted therein, while the P-type region 124 includes one or more P-type impurities implanted therein. However, the P-type region 124 could also simply comprise an undoped region as well. During subsequent annealing processes, any impurities contained within the locally doped regions 122 , 124 will migrate throughout the lower undoped polysilicon region 126 . The locally doped regions 122 , 124 may be formed by using well-defined ion energy during the ion implant.
It is preferable to delay the annealing process until after the gate conductors are formed so as to reduce the excessive erosion of the N-type gate conductor during the plasma process. Again, this uneven reaction is due to the fact that the N-type conductor reacts faster than the P-type conductor in conventional plasma processes. Accordingly, in addition to utilizing a vertical passivation layer to protect the sidewalls of the N-type gate conductor, the present method embodiment also delays the annealing process until the gate conductor structures are defined.
FIG. 5 also illustrates a hardmask layer 128 (e.g., TEOS, silicon nitride, CVD oxide) formed over the locally doped regions 122 , 124 . A patterned photoresist/antireflective coating (ARC) layer 130 is also shown formed over the hardmask layer 128 . As will be noted, the patterned photoresist/ARC layer 130 is used to define the gate conductor structures. Then, as shown in FIG. 6, plasma etch is utilized to etch away the exposed portions of the hardmask layer 128 with a first type of etchant. A second type of etchant is subsequently to etch away exposed portions of the locally doped regions 122 , 124 . Again, the plasma parameters used to etch the locally doped regions 122 , 124 are selected such that there will be relatively little difference in etch rates and profiles between N-type doped region 122 and the P-type doped region 124 . After the photoresist is removed, the etching process is continued such that a portion of the undoped region 126 is also removed.
A plasma etching step may be adjusted by changing a variety of properties, such as the etch rate, selectivity between different materials, and anisotropic versus isotropic nature of the etch. It is further possible to manipulate a plasma etching step to yield certain properties, by selecting a particular chemistry through choosing a combination of gases, flow rates, pressure, powers, and temperatures of the various component surfaces in contact with the plasma and semiconductor substrate. A plasma step can etch a material both laterally and vertically. Thus, depending on the particular process condition, relative etch rates along these two directions may be different and manipulated.
In the present embodiment, a fluorine-containing plasma is utilized to etch the locally doped polysilicon regions 122 , 124 , as it provides similar etch rates between N-type and P-type polysilicon. However, etching for both types of polysilicon in fluorine-based plasma tends to be isotropic, particularly for N-type polysilicon. One way to attain anisotropic polysilicon etching with fluorine-based plasma is to passivate the etched sidewalls with a polymer substance by using fluorocarbon chemistry, such as CF 4 , CHF 3 , C 4 F 8 , or C 2 F 6 , for example. As a fluorocarbon plasma also etches oxide at a fast rate, it is preferable to use photoresist as a mask material. In addition, erosion of the photoresist in fluorine-based plasma releases fluorocarbon that helps the passivation mechanism. It has been found that an NF 3 /Ar etch chemistry works well in an AME-5000 reactor, as does CF 4 /SF 6 or CF 4 /NF 3 in a LAM-2300 and TEL-SCCM reactor.
Referring now to FIG. 7, an oxygen plasma is utilized to strip away the photoresist and also remove the sidewall polymer material formed on the etched, doped-polysilicon regions 122 , 124 . At the same time, the oxygen plasma forms a passivation layer (i.e., a silicon oxide-like material) 132 on the exposed surfaces (vertical and horizontal) of the doped and undoped regions of the polysilicon. Subsequently, another etching process first removes the passivation layer 132 from the horizontal surfaces of the undoped polysilicon lower region 126 , followed by an anisotropic etching of the remaining portions of the undoped lower region 126 not protected by the hardmask 126 to define the shape of N-type and P-type conductors, as shown in FIG. 8 . The remaining vertical passivation layer 132 prevents this latest etching process from affecting the shape of the doped regions 122 , 124 . In particular, this etching process may be any known plasma process that etches undoped polysilicon, wherein there is also a native oxide layer present on the polysilicon surface. As a result, the N-type gate conductor will have substantially the same profile (i.e., shape and size) as the P-type gate conductor.
Upon completion of the undoped polysilicon etching, the vertical passivation layer 132 may be removed after cleaning the wafer in a diluted HF-solution (e.g., 200:1 DHF) that also removes the oxide hardmask 128 , as shown in FIG. 9 . Finally, after the DHF clean, annealing is performed to allow the dopants to diffuse into the previously undoped regions 126 of the polysilicon so as to define the N-type gate conductor 114 and the P-type gate conductor 116 as illustrated in FIG. 10 . In addition, the source/drain regions 108 , 110 are doped (as also shown in FIG. 10 ), and the remaining device fabrication steps may be continued in accordance with conventional processing techniques.
While the invention has been described with reference to a preferred embodiment or 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. 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 the particular embodiment disclosed as the best mode contemplated for carrying out this invention, but that the invention will include all embodiments falling within the scope of the appended claims.
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A method for forming a semiconductor device, includes forming a first locally doped semiconductor region of a first conductivity type and a second locally doped semiconductor region of a second conductivity type over an undoped, lower semiconductor region. A first etch is implemented to simultaneously create a desired pattern in the first and second locally doped semiconductor regions in a manner that also provides a first passivation of exposed sidewalls thereof, wherein the first etch removes material from the first and second locally doped regions at a substantially constant rate with respect to one another, and in a substantially anisotropic manner. A second etch is implemented to complete the desired pattern in the undoped, lower semiconductor region in a manner that protects the first and second locally doped regions from additional material removal therefrom.
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CROSS-REFERENCE TO RELATED APPLICATIONS
[0001] This application is a continuation-in-part of international patent application PCT/IB2004/004390, filed Dec. 28, 2004, the entire content of which is expressly incorporated herein by reference thereto.
FIELD OF THE INVENTION
[0002] The present invention relates to a method for configuring a process for treating a semiconductor wafer. More particularly, the invention relates to configuring a process in which a minimum layer thickness is determined for a layer to be transferred to a donor wafer to enable finishing operations to be conducted to obtain a desired layer thickness.
BACKGROUND OF THE INVENTION
[0003] Several processes and techniques for manufacturing a crystalline wafer by transferring layers are generally known. These include, for example, the layer transfer technique reported in Frontiers of Silicon - on - Insulator, J. Appl. Phys. 93, 4955 (2003) by G. K. Celler et al. and based on the “SMAT-CUT®” technology of Soitec S. A., which is known to those skilled in the art and descriptions of which can be found in a number of works dealing with wafer reduction techniques, such as U.S. Pat. No. 5,374,564. In the SMART-CUT® process, atomic species, such as ions, are implanted in a donor substrate to create a region of weakness therein before bonding of a handle substrate to the donor substrate. After bonding, the donor substrate splits or is cut at the region of weakness. What is obtained therefore is, on the one hand, a donor substrate, stripped of a layer of its structure, and, on the other hand, a wafer comprising, bonded together, a removed thin layer of the donor substrate and the handle substrate.
[0004] It is also known that a region of weakness can alternatively be formed in a donor substrate by forming a porous layer therein using the method known as the ELTRAN® process by Canon, described in U.S. Pat. No. 6,100,166. Additionally, various bonding techniques are generally known and include the method described in the reference entitled “Semiconductor Wafer Bonding: Science and Technology” (Interscience Technology) by Q. Y. Tong, U. Gösele and Wiley.
[0005] A process known as SMART-CUT®, which is described, for example, in the document “Silicon-On-Insulator Technology: Materials to VLSI, 2nd Edition”, by Jean-Pierre Colinge from Kluwer Academic Publishers, pp. 50 and 51. The SMART-CUT® process advantageously can produce structures comprising a thin layer of semiconductor material, such as SeOI (Semiconductor On Insulator) structures and the like.
[0006] Layer transfer processes, for example SMART-CUT® processes, advantageously produce crystalline wafers or other structures that preferably include a thin layer of semiconductor material, such as SeOI (Semiconductor-On-Insulator), SOI (Silicon-On-Insulator), and SGOI (Silicon-Germanium-On-Insulator) structures and the like.
[0007] Following the detachment step, the thin layer formed onto the support substrate typically has a damaged zone extending to a certain depth from the surface at which it was detached. In this damaged zone, holes may be observed on the surface of the thin layer. Some holes, which will be referred to as “shallow holes” below, are blind holes which extend part of the way into the thickness of the thin layer. In an SOI structure, for example, these shallow holes extend into the thickness of the superficial thin silicon layer but do not extend down to the buried oxide layer.
[0008] On the other hand, some holes can be fairly deep, extending completely through the thickness of the thin layer. These through holes are also referred to herein as “killing holes”. In an SOI structure for example, these killing holes can extend completely through the superficial thin silicon layer and through the buried oxide layer.
[0009] There is thus a need for a method for producing a high quality structure comprising a thin layer of semiconductor material on a substrate, which method makes it possible to minimize the density of holes within the thin layer, including the density of through holes.
SUMMARY OF THE INVENTION
[0010] The present invention relates to a method for configuring a process to treat a semiconductor wafer. The preferred embodiment includes selecting a target thickness to be obtained for a processed semiconductor layer of the semiconductor wafer, which semiconductor layer is to be transferred from a donor substrate. A target maximum density of through holes is selected, which through holes extend completely through the processed semiconductor layer. A finishing sequence of operations to be conducted on the semiconductor layer after its transfer from the donor substrate is selected for improving the surface quality of the transferred semiconductor layer to provide the processed layer. A minimum layer thickness is determined for the transfer layer, which is to be provided by providing a donor wafer than comprises the semiconductor layer and a region of weakness. The region of weakness is configured to facilitate detachment of the semiconductor layer from a remainder portion of the donor substrate. The semiconductor layer and remainder portion are disposed on opposite sides of the region of weakness. The semiconductor layer is associated with a support substrate, and the semiconductor layer is detached at the region of weakness from the remainder portion to transfer the semiconductor layer to the support substrate to provide the semiconductor wafer. This is conducted so that the transferred semiconductor layer has at least the minimum layer thickness. Additionally, the minimum layer thickness is determined such that the density of through holes is below the target maximum density after each operation in the finishing sequence. The target thickness is achieved when the finishing sequence is complete.
[0011] In the preferred embodiment, the minimum layer of thickness is determined for the transferred layer from the donor substrate. In this embodiment, the region of weakness is provided by implanting atomic species into the donor substrate. Preferably, an implantation energy is selected between about 15 keV and 120 keV for implanting the atomic species, and the implantation energy is more preferably less that 80 keV.
[0012] The finishing sequence preferably includes at least one shallow-hole reducing operation that reduces the depth of shallow holes that are present in the transferred layer, which shallow holes extend less than completely through the transferred layer. At least one shallow hole reducing operation can include a thermal annealing operation or a polishing operation. The selected finishing sequence can comprise at least one succession of a rapid thermal annealing operation and a sacrificial oxidation operation, in which the thermal annealing operation can, for example, proceed the sacrificial oxidation operation in the succession. Alternatively, the selected finishing sequence can include at least one succession of a first sacrificial oxidation operation, followed by a polishing operation, followed by a second sacrificial oxidation operation. In another finishing sequence, a succession of operations includes a first sacrificial oxidation operation, followed by a rapid thermal annealing operation, followed by a polishing operation, followed by a second sacrificial oxidation operation.
[0013] The minimum layer thickness can be determined for the transferred layer that is associated with the support, wherein an insulating layer is disposed between the transferred layer and the support substrate to provide an SOI wafer. The transfer layer can be made of silicon, the insulator layer be made of an oxide to provide the SOI wafer after detachment. In embodiments to prepare an SOI wafer, the selected finishing sequence can comprise, for example, at least two sequential successions, each succession comprising a rapid thermal annealing operation, followed by a sacrificial oxidation operation. The target maximum density of through holes can be about 0.1/cm 2 in this embodiment.
[0014] One embodiment includes determining a depth in the donor wafer in which the region of weakness is to be provided to obtain the transferred layer having the determined minimum thickness. Another embodiment includes providing the semiconductor wafer with the transferred layer of at least said determined minimum thickness and a preexisting surface quality, and conducting the selective finishing operations to obtain the processed layer. In this embodiment, the processed layer has the improved surface quality compared to the surface quality of the transferred layer, substantially the target thickness, and substantially the target maximum density of through holes or less. The region of weakness is preferably provided at a depth in the donor wafer that is substantially equal to or greater than the determined minimum thickness.
[0015] Another embodiment of a method configuring the process of treating the semiconductor wafer includes determining a minimum layer thickness of a transfer layer, which is associated with a support substrate that has a transferred surface quality, to obtain a processed layer that has a pre-selected target thickness and a target maximum density of through holes that extend completely therethrough. This processed layer has been obtained by conducting a predetermined finishing sequence of operations to improve the surface quality of the processed layer compared to the transferred surface quality. Additionally, the minimum thickness is determined such that the density of through holes is below the target maximum density after each operation in the finishing sequence.
BRIEF DESCRIPTION OF THE DRAWINGS
[0016] Other characteristics, purposes and advantages of the invention will appear to the reading of the following detailed description, with respect to the annexed drawings, given as non restrictive example, in which:
[0017] FIG. 1 schematically represents the hole density as a fimction of depth within a thin layer;
[0018] FIGS. 2 a - 2 d illustrate the effect of an RTA operation on SOI structures;
[0019] FIGS. 3 a and 3 b show the hole density within an SOI layer before and after an RTA operation, respectively;
[0020] FIGS. 4 a and 4 b illustrate the effect of a POL operation effect on an SOI structure;
[0021] FIGS. 5 a and 5 b show the hole density within an SOI layer before and after a POL operation, respectively.
[0022] FIGS. 6 a and 6 b illustrate the effect of an SOx operation on an SOI structure;
[0023] FIGS. 7 a and 7 b show the hole density within an SOI layer before and after an SOx operation, respectively;
[0024] FIGS. 8 a - 8 e show the effect of sequences RTA-SOx and Sox-RTA on an SOI structure;
[0025] FIGS. 9 a - 9 j show the effects of an embodiment of the inventive method;
[0026] FIGS. 10 a and 10 b illustrate the effect of an embodiment of the inventive method on reducing the density of killing holes; and
[0027] FIG. 11 is a flow chart illustrating an embodiment of an innovative method.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0028] The present invention relates to a method for producing a final structure comprising a thin layer of semiconductor material on a substrate. One embodiment comprises the steps of:
creating region of weakness in the thickness of a donor substrate, placing the donor substrate into close contact with a support substrate, detaching the donor substrate at the level of the region of weakness to transfer a part of the donor substrate onto the support substrate.
[0032] The invention allows production of improved properties of the thin layer, preferably by avoiding the presence of holes within the thin layer.
[0033] A layer transfer process, such as SMART-CUT®, can be used. The region of weakness can be created by implantation of atomic species within the thickness of the donor substrate. Implantation of atomic species is understood to mean any technique (such as bombardment, diffusion and the like) suitable for introducing atomic or ionic species onto the material of the implanted donor substrate, with a maximum concentration of the implanted species situated at a preset depth from the substrate relative to the surface of said implanted substrate.
[0034] When an SeOI structure is to be produced, a layer of oxide can be provided between the support substrate and the thin layer. For this purpose, the donor substrate may comprise on its top a superficial oxide layer which is to be placed, after the implantation step, into close contact with the support substrate so as to form the buried oxide layer of the final SeOI structure.
[0035] The implantation step can be performed either by implanting a single atomic species (such as hydrogen) or by co-implanting at least two different species (such as the co-implantation of both hydrogen and helium). The term “atomic species implantation” means any bombardment of atomic species, including molecular and ionic species, which can introduce the species into a material, with a maximum concentration of the species being located at a depth that is determined with respect to the bombarded surface. The molecular or ionic atomic species are introduced into the material with an energy that is also distributed about a maximum.
[0036] As indicated above, following the detachment step, the thin layer formed onto the support substrate typically has a damaged zone that can include shallow holes, which extend part of the way into the thickness of the thin layer, but do not extend down to the buried oxide layer in a typical SOI wafer, and killing holes or through holes, which extend completely through the thickness of the thin layer, and can extend through the buried oxide layer as well. The significance of the through holes is significant when the thickness of the thin layer is small (for instance less than 800 angstroms).
[0037] The resulting structures from SMART-CUT® type processes are used for applications in the fields of microelectronics, optics and/or optronics. Holes are thus to be as much as possible avoided, and fimctional components cannot be built on a through hole. Shallow hole are not as detrimental to the operation of the components built thereon, but they form defects that are desirable to be avoided.
[0038] A first embodiment of an inventive method for producing a final structure comprising a thin layer of semiconductor material on a substrate, comprises the steps of:
creating region of weakness in the thickness of a donor substrate, placing the donor substrate into close contact with a support substrate, and detaching the donor substrate at the level of the region of weakness to transfer a part of the donor substrate onto the support substrate, thus forming an intermediate structure.
The preferred method also comprises the steps of:
selecting:
a thickness that is to be reached for the thin layer of the final structure, a maximum density of through holes to be observed within the thin layer of the final structure, a finishing sequence comprising at least one operation to be performed on the intermediate structure obtained after detachment;
determining a minimum thickness of the part of the donor substrate to be transferred onto the support substrate such that the part:
presents, after each operation of the finishing sequence, a density of killing holes less than the selected maximum density, and to reach said selected thickness once the finishing sequence is completed.
[0049] Preferred embodiments of an inventive method can include the following:
the region of weakness is created in the thickness of the donor substrate at a depth substantially equal to or greater than the determined minimum thickness to be transferred; the region of weakness is created by implantation of atomic species through a face of the donor substrate from which the thin layer is made, according to implantation conditions selected for creating the region of weakness below the selected thickness; the thickness selection takes into account the selected maximum through holes density, the selected final thickness, and the effect of each operation of the finishing sequence upon the holes density; the method comprises the step of selecting implantation conditions by selecting an implantation energy between about 15 keV and about 120 keV, and preferably between about 15 keV and about 80 keV; the finishing sequence comprises at least one shallow holes depth reducing operation; the finishing sequence comprises a plurality of shallow holes depth reducing operations; the finishing step comprises at least one thermal annealing (TA) operation, as a shallow holes depth-reducing operation; the finishing step comprises at least one polishing (POL) operation, as a shallow holes depth-reducing operation; the finishing sequence comprises at least one succession of the following operations: rapid thermal annealing (RTA) followed by sacrificial oxidation (SOx); the finishing sequence comprises at least one succession of the following operations: sacrificial oxidation (SOx) followed by rapid thermal annealing (RTA); the finishing sequence comprises at least one succession of the following operations, preferably in the following order: sacrificial oxidation (SOx), polishing (POL), and SOx; the finishing sequence comprises at least one succession of the following operations, preferably in the following order: sacrificial oxidation (SOx), rapid thermal annealing (RTA), polishing (POL), and SOx; a layer of oxide is interposed between the thin layer and the support substrate, the structure thus produced being a SeOI (Semiconductor On Insulator) structure; the thin layer is formed from silicon, the structure thus produced being an SOI (Silicon On Insulator) structure.
[0064] The invention also relates to the structures obtained by the method according to the invention, such as an SeOI structure produced by the method according to the inventive method first, wherein the finishing sequence comprises an RTA/SOx/RTA/SOx sequence of operations, such that the killing holes density of the thin layer of the final structure is around 0.1/cm 2 .
[0065] The minimum thickness of the donor substrate port to be transferred to the support substrate can be selected or determined:
to have, after each operation of the finishing sequence, a density of killing holes less than said maximum density, and to reach the selected thickness once the complete finishing sequence is completed.
[0068] The present invention can help improve the quality of a structure obtained by carrying out a transfer process of the SMART-CUT® type. The structure can, in general, be any type of structure comprising a thin layer of semiconductor material on a surface exposed to the external environment. The thin layer of semiconductor material can be, for example, silicon Si, silicon carbide SiC, germanium Ge, silicon-germanium SiGe, gallium arsenide GaAs, or another suitable material. The substrate support can be made of silicon Si, quartz, or another suitable material.
[0069] As mentioned above, a layer of oxide can also be interposed in between the support substrate and the thin layer, the structure therefore formed being a SeOI (Semiconductor On Insulator) structure.
[0070] The embodiment described hereafter deals with SOI (Silicon On Insulator) structures manufacturing, but one of ordinary skill in the art will understand that the invention is can be applied to other embodiments. FIG. 1 represents the hole density as a finction of depth within an SOI transferred layer. The hole density is inversely proportional to the depth, and decreases quasi exponentially. Typically the deepest holes are between 1000 and 1400 angstroms deep, but their density is then relatively weak (typically the density of the holes deeper than 1000 angstroms is below 0.3 holes per cm 2 ). The hole density is typically similarly distributed whether the implantation step is carried out by implanting a single atomic species or by co-implanting at least two different species.
[0071] A killing hole is a hole with a depth at least equal to the thickness of the thin layer. Hence, as illustrated on FIG. 1 , the killing hole density Dk is directly related to the thin layer thickness T. This killing hole density is thus all the more significant and typically higher when the thickness of the thin layer is low. Hence, a thin SOI layer traditionally has a high killing holes density, whereas a thick SOI layer traditionally has a low killing holes density. As illustrated by FIG. 1 , an SOI layer with a thickness T greater than 1000 angstroms typically has a killing holes density Dk less than 0.3/cm 2 .
[0072] Several finishing steps of the structure obtained after detachment can be used to form a thin layer suitable for a use in the field of microelectronics, optics and/or optronics. These finishing steps generally make use of operations such as polishing (referred to as “POL” hereinbelow), thermal annealing in a neutral or reducing atmosphere (referred to as “TA” hereinbelow; such as a rapid thermal annealing (“RTA”)), sacrificial oxidation (referred to as “SOx” hereinbelow), chemical etching, etc. RTA is generally understood herein to mean rapid thermal annealing, performed over a period of several seconds or several tens of seconds, preferably at least 5 seconds, more preferably at least 10 seconds, and most preferably at least 20 seconds, preferably up to about 10 minutes, more preferably up to about 2 minutes, more preferably up to a minute, and most preferably up to about 45 seconds (RTA in a preferred embodiment is conducted for around 30 seconds). RTA is generally also understood herein to be conducted at a high temperature, for example of the order of 900° C. to 1300° C., in a controlled atmosphere, such as a mixture of hydrogen and argon, or an atmosphere of pure argon, or even an atmosphere of pure hydrogen. In one embodiment, RTA is conducted for between 20 and 40 seconds, and more preferably around 30 seconds.
[0073] SOx is a sacrificial oxidation divided into an oxidation step and a deoxidation step, a heat treatment step (typically around two hours long at 1100° C.) being preferably conducted between the oxidation and deoxidation steps. Chemical-mechanical polishing (“CMP”) is an example of a POL operation.
[0074] The following sequences of operations have for instance been proposed as finishing step of the structure obtained after detachment:
SOx-POL-SOx (refer for instance to publication FR 2 797 174); SOx-RTA-POL-SOx (refer for instance to publication FR 2 797 713); RTA-SOx-RTA-SOx (refer for instance to the Applicant's French patent application filed on Jul. 27, 2003 under n° 03 09304).
[0078] As concerns holes, the applicant has observed that the above mentioned operations can be separated into two families. A first family concerns those operations that allow reducing the depth of the shallow holes, that is those holes which depth is lower than the thickness of the thin layer being formed (such as those holes which do not extend down to the underneath buried oxide layer in the case of an SOI structure). A second family concerns those operations which do not have any curing impact on holes. RTA and POL operations are instances of the first family, whereas SOx and chemical etching operations are instances of the second family.
[0079] FIGS. 2 a - 2 d illustrate the effect of an RTA operation on SOI structures 1 a, 1 b composed respectively of a silicon layer 2 a, 2 b on top of a buried oxide layer 3 a, 3 b (the support substrates not being represented). Silicon layer 2 a of SOI structure 1 a presents a shallow hole 4 a, the depth of which is lower than the thickness of the silicon layer 2 a and thus does not extend down to the surface of the buried oxide layer 3 a. On the contrary, silicon layer 2 b of SOI structure 1 b presents a through hole 4 b which extends completely through the thickness of the silicon layer 2 b, down to the surface of the buried oxide layer 3 b.
[0080] The RTA operation has a smoothing effect that significantly decreases (by a factor two to three at least) the depth of the shallow holes (such as shallow hole 4 a ). Indeed these holes can be eliminated, in particular thanks to diffusion and recrystallization, as it is schematically represented on the right hand side of FIG. 2 in respect of structure 1 a. However an RTA operation has no effect on the through holes (such as hole 4 b ) which extend, prior to the RTA, completely through thin layer 2 b (in this case down to the surface of the buried oxide layer 3 a ). As is schematically represented in FIG. 2 d in structure 1 d through holes are not cured by an RTA operation.
[0081] FIGS. 3 a and 3 b represent the hole density within an SOI layer before (top graph) and after (lower graph) an RTA operation. Before the RTA operation, the SOI layer of thickness T presents more or less deep shallow holes, in a density, illustrated by curve Cb, which depends upon the depth of these holes. The SOI layer also presents through holes in a density Dk.
[0082] As mentioned here above, the RTA operation has no effect on through holes. The through holes density thus remains unchanged and equal to Dk. However, the RTA operation helps to cure the shallow holes by decreasing their depth and even by eliminating them. As a result of the RTA operation, the SOI layer presents shallow holes in a highly decreased density, as illustrated by curve Ca.
[0083] FIGS. 4 a and 4 b illustrate the effect of a POL operation on an SOI structure 5 composed of a silicon layer 6 on top of a buried oxide layer 7 . The silicon layer 6 presents prior to the POL operation a shallow hole 8 . As it is apparent in FIG. 4 b, by removing x angstroms of the silicon layer 6 , thus obtaining a thinned silicon layer 6 ′, the depth of the shallow hole 8 is decreased.
[0084] Furthermore, the thickness of the silicon layer 6 being removed by the POL operation can be adjusted (being more important than the shallow hole depth) in order for said shallow hole to be removed by the POL operation. However, one understands that if the silicon layer presents a through hole which extends down to the buried oxide layer, after polishing said silicon layer will still present this killing hole.
[0085] FIGS. 5 a and 5 b represent the hole density within an SOI layer before (top graph) and after (lower graph) a POL operation. Before the POL operation, the SOI layer of thickness Tb presents more or less deep shallow holes, in a density illustrated by curve Cb, which depends upon the depth of these holes. The SOI layer also presents through holes in a density Dk. As mentioned above, the POL operation has no effect on through holes. The through holes density thus remains unchanged equal to Dk.
[0086] However, the POL operation helps to cure the shallow holes, by decreasing their depth and even by eliminating them. As a result of the POL operation, the SOI layer presents shallow holes in a strongly decreased density, as illustrated by curve Cp (which is identical to curve Cb but shifted along the depth axis due to the POL thickness consumption).
[0087] FIGS. 6 a and 6 b illustrate the effect of an SOx operation on an SOI structure 9 composed of a silicon layer 10 on top of a buried oxide layer 11 . The silicon layer 10 presents prior to the SOx operation a shallow hole 12 . As is apparent in FIG. 6 b, the SOx operation reproduces the shape of the hole and does not modify its depth until it becomes a through hole when the depth equals the thickness of the material. As illustrated, if the depth of the initially present shallow hole 12 is sufficient, it is possible that this hole extends, after an SOx operation, down to the buried oxide layer (becoming a through hole 12 ′).
[0088] FIGS. 7 a and 7 b represent the holes density within an SOI layer before (top graph) and after (lower graph) an SOx operation. Before the SOx operation, the SOI layer of thickness Ti presents more or less deep shallow holes in a density, illustrated by curve Cb, which depends upon the depth of these holes. The SOI layer also presents through holes in a density Di.
[0089] As mentioned here above, the SOx operation reproduces the shape of the holes and does not modify their depth. The shallow holes density is thus unchanged, and depends upon their depth as illustrated by the unchanged curve Cb. However the thickness of the SOI layer is decreased by the SOx operation. As the new thickness Tf is lower than the initial thickness Ti, the density of through holes thus increased from Di to Df.
[0090] As is apparent from FIG. 7 a and 7 b, an SOx operation does not help to cure shallow holes, and increases the killing holes density (this increase relating directly to the consumed thickness Ti-Tf). As, for the SOx operation, a chemical etching operation reproduces the shape of the hole and does not modify its depth. As for the SOx operation, this even results in an initially relatively deep shallow-hole extending subsequently down to the buried oxide layer, and being thus “converted” to a through hole (or otherwise stated, it results in an increase of the through holes density).
[0091] As has been stated hereabove, a through hole present prior to an operation of the first family (such as an RTA or POL operation), will not be cured by said operation. Hence, as it is apparent on FIGS. 8 a - 8 e, sequences RTA-SOx and Sox-RTA with the operations conducted in the order in which they are listed, have a very different effect.
[0092] In the Sox-RTA sequence case, it is possible that the SOx operation transforms an initially (after layer transfer) shallow hole 13 into a through hole 14 . This through hole 14 will not be cured by the following RTA operation. On the other hand, in the RTA-SOx sequence case the same initially shallow hole 13 can be cured. Indeed the RTA operation will decrease its depth (see hole 15 ) while the SOx will thin the silicon layer. The resulting structure thus presents an almost entirely eliminated hole 15 ′, with greatly reduced depth. If through holes are present after transfer within the thin layer, these holes will not be cured and will remain, as killer defects in the final product.
[0093] Based on the above observations, the method according to the invention proposes to perform the steps of:
selecting a thickness which is to be reached for the thin layer of the final structure, selecting a maximum density of through holes to be observed within the thin layer of the final structure, and selecting a finishing sequence comprising at least one operation to be performed on the intermediate structure obtained after detachment.
[0097] A particular finishing sequence is generally used on the structure following the detachment step so as to improve the quality of the thin transferred layer (for instance by gummning out the roughnesses, insuring a correct thickness uniformity) and make it suitable for a use in the fields of application. This finishing sequence is notably adapted for thinning the part of the donor substrate transferred onto the support substrate (thin transferred layer) so that the thickness of the thin layer of the final structure reaches said selected thickness.
[0098] The finishing sequence may comprise at least one of the above mentioned operations (TA, POL, SOx, chemical etching) and may include any combination of these operations, such as the following sequences, which are given as non restrictive examples:
RTA-SOx; repetition of several RTA-SOx sequences (such as RTA-SOx-RTA-SOx); SOx-POL-SOx (and any repetition of this sequence); SOx-RTA-POL-SOx (and any repetition of this sequence); SOx-RTA (and any repetition of this sequence).
[0104] As mentioned above, an RTA operation (and more generally any smoothing annealing operation) helps stopping shallow holes. It is thus advantageous to make use of a sequence comprising such an RTA operation.
[0105] Moreover, under particular conditions, an RTA operation helps encapsulate the oxide layer under a Si layer, which may be favourable before performing a chemical etching or a sacrificial oxidation (see for instance WO 2004/079801). However the order (defined in terms of remaining thickness) of such an operation within a particular sequence may be important (see for instance US 2004/0151483).
[0106] Furthermore, an RTA operation is not effective for carrying out a removal of material and thinning the thin layer. On the contrary, an SOx operation is effective for thinning the thin layer, in particular for removing the zone which is damaged after detachment or for obtaining the selected thickness of the thin layer of the final structure. The thickness that can be removed by an SOx operation is typically comprised between about 100 and 1000 angstroms. However an SOx operation must be carefully performed as it may increases the through holes density. It may hence be judicious to perform an RTA operation between two SOX operations.
[0107] A POL operation also helps thinning the thin layer by material removal, but such an operation results in a degradation of the thickness uniformity and even in the thin layer being damaged. A POL operation has thus to be limited as much as possible, and to be performed after a thinning step (such as an SOx) which damages the thin layer less, or even after an RTA. Typically a POL operation is combined with an RTA so as to limit the removal of material between about 200 and 500 angstroms (which helps to limit the thickness uniformity degradation).
[0108] The method according to the invention also proposes to perform the step of determining a minimum thickness of the part of the donor substrate which has to be transferred onto the support substrate for said part to present, after each operation of the finishing sequence, a density of through holes less than the desired maximum density, and to reach said selected thickness once achieving the finishing sequence.
[0109] Hence the invention proposes to limit the density of through holes within the thin layer of the final structure by selecting an adequate thickness to be transferred onto the support substrate and taking into account:
the selected thickness which is to be reached for the thin layer of the final structure, the selected finishing sequence of operation(s) (and thus taking into account the effect upon holes density of each operation of this finishing sequence).
[0112] The above discussed graphs ( FIGS. 3 a, 3 b, 5 a, 5 b, 7 a, and 7 b ) show the effect upon holes density of each type of operation (RTA, POL and SOx). These graphs may hence be combined to evaluate the effect upon holes density of a complete finishing sequence (which may have several operations performed in a particular order, and which is adapted for thinning the thin layer to the selected thickness).
[0113] The appropriate thickness to be transferred can thus be derived from this combination of graphs so that after each operation, the through holes density is less than the selected maximum through holes density. Starting from the selected final thickness and maximum density of through holes, it is hence possible to determine, (such as by taking the operation(s) of the finishing sequence in their reverse order and starting from the last one) which minimum thickness the thin layer must present before a particular operation, and thus finally which thickness has to be transferred.
[0114] Taking the diagrams of FIGS. 8 b and 8 c as an illustrative example, the selected finishing sequence comprises an SOx operation followed by an RTA operation. Graphs of FIGS. 3 a, 3 b, 7 a, and 7 b are thus to be combined. The minimum thickness Ti to be transferred must take into account the fact that the thickness of the thin layer is decreased by the SOx operation (decreasing from Ti after transfer to Tf after the SOx operation), which results in an increase of the through holes density.
[0115] Let's consider than the selected maximum density is set to 0.3 through holes per cm 2 . The minimum thickness Ti to be transferred must then be chosen so that the thickness Tf after the SOx operation and thus before the RTA operation (which has no impact upon through holes density but helps lowering the shallow holes density) is greater than the thickness for which a through holes density of 0.3/cm 2 is obtained (that is greater than 1000 angstroms).
[0116] Turning now to the graph of FIGS. 8 d and 8 e, the selected finishing sequence now comprises an RTA operation followed by an SOx operation. Graphs of FIGS. 3 a, 3 b, 7 a, and 7 b are thus to be combined. In this case, the first operation does not reduce the thickness of the thin layer but modifies the holes density such that the subsequent SOx operation does not tend to create (a lot of) new through holes (SOx operation as illustrated on FIGS. 7 a and 7 b but starting from a reduced holes density profile after the RTA operation as illustrated by curve Ca on the graph of 3 b ). Hence, it is understood that for a selected final thickness and a selected maximum density of killing holes, the minimum thickness to be transferred in the case of an RTA-SOx finishing sequence is different (in the present case lower) than the minimum thickness to be transferred in the case of an SOx-RTA finishing sequence. The region of weakness is created in the thickness of the donor substrate at a depth substantially equal to or greater than said determined minimum thickness to be transferred. According to a possible embodiment, the region of weakness is created by implantation of species under a face of the donor substrate from which the thin layer must be made. Such an implantation can be performed by implanting a single species (such as hydrogen) or by implanting at least two different species (such as the co-implantation of helium and hydrogen). According to a preferred embodiment of the invention, implantation conditions are selected so that the implantation energy is between about 15 keV and 120 keV, and more preferably between about 15 keV and 80 keV.
[0117] According to a preferred embodiment, the finishing sequence comprises at least one operation from said first family of operations, that is an operation which allows reducing the depth of the shallow holes and helps modifying the holes density within the thin layer (see effect of an RTA and of a POL operation on FIGS. 3 a, 3 b, 5 a, and 5 b ). Said shallow holes depth reducing operation is for instance a TA operation or a POL operation.
[0118] According to an advantageous embodiment of the present invention, the finishing sequence comprises a plurality of operations from said first family of operations, that is a plurality of operations that each allows reducing the depth of shallow holes. This advantageous embodiment brings an additional benefit as it decreases the depth of the residual shallow holes, and may even help to remove these shallow holes completely.
[0119] FIGS. 9 f - 9 j give an example of the amelioration brought by a possible embodiment of the method according to the invention wherein the finishing sequence is an SOx-RTA-POL-SOx sequence of operations. Graphs of FIGS. 3 b, 5 b, and 7 b are thus to be combined to determine, taking into account the selected thickness to be reached and the selected maximum density of through holes, the minimum thickness which is to be transferred for the thin transferred layer to present, after each of these operations, a density of killing holes less than said selected density.
[0120] In FIGS. 9 a - 9 e, the implantation step is carried out classically so that a layer of thickness t is transferred onto the donor substrate. In FIGS. 9 f - 9 j, the implantation step is carried accordingly to the invention so that a layer of thickness t+500 angstroms is transferred onto the donor substrate.
[0121] In the classical case of FIGS. 9 a - 9 e, the first SOx operation does not cure shallow holes and even leads to the formation of through holes (such as hole 16 ) extending down to the buried oxide layer. These through holes can not be cured by the following RTA operation, nor by the following POL operation. The final SOx operation will lead to an SOI structure having a through hole 18 , and being thus not acceptable for manufacturing a semiconductor device.
[0122] On the other hand, in the case of the method according to a possible embodiment of the invention shown in FIGS. 9 f - 9 j, the transferred layer is thick enough for killing holes not to be formed (in a too important density exceeding the selected maximum density) by the first SOx operation. Thus, in this case the subsequent RTA operation in FIG. ___ (that is an operation allowing to reduce the depth of shallow holes, such as hole 19 ) will help to cure the present shallow holes, notably by decreasing their depth (see hole 19 ′). This RTA operation has no impact upon the through holes density, so that after this operation, the through holes density still does not exceed the selected maximum density. The POL operation will remove those shallow holes which are included within the thickness of the thin layer which is removed by this operation (in this case, those holes that are less deep than p angstroms, such as hole 19 ′). The POL operation will decrease the depth of the shallow holes that were, prior to this operation, deeper than p angstroms. As for the RTA operation, the POL operation does not impact the through holes density. Finally, at the end of the last operation (second SOx operation), a thin layer is obtained which presents the desired thickness, and a minimized density of holes, and in particular few shallow holes and a killing holes density less than said selected maximum density.
[0123] It should be noted that this second SOx operation carries out a sacrificial oxidation adapted for obtaining a final thin layer 21 whose thickness is similar to that of the thin layer 20 classically obtained. Hence this second SOx operation carries out a more important sacrificial oxidation, adapted to compensate for the thickness increase (+500 angstroms in the present case) of the transferred layer.
[0124] Moreover, the preceding example shows that a benefit is reached, in term of density of through holes, because the RTA operation (or more generally speaking an operation allowing to reduce the depth of the shallow holes) is performed on a thin layer which does not present through holes (or at least which presents through holes in a density lower than a maximum density). Furthermore, through holes density before said operation is controlled thanks to an implantation step adequately performed, notably by increasing the thickness of the layer being transferred onto the support substrate.
[0125] FIG. 10 shows that an increase of 450 angstroms of the transferred layer, when combined with a finishing RTA-SOx-RTA-SOx sequence of operations, allows to decrease the density of through holes by a factor 5 in the final thin layer (thickness 200 angstroms). Indeed the left hand side diagram drawn for a classically obtained SOI structure reveals a through holes density of 0.5 holes/cm 2 , while the right hand side diagram drawn for an SOI structure obtained as mentioned hereabove, reveals a through holes density of 0.1 holes/cm 2 only.
[0126] FIG. 11 is a flow chart illustrating a method according to a possible embodiment of the invention for determining a manufacturing process for making an SOI device. At block 110 , the specifications of the final SOI product are detailed, in particular by selecting:
the thickness Tf of the thin layer of the final structure, the finishing sequence of operation(s) of the intermediate structure obtained after transfer (in this case an RTA-SOx-RTA-SOX sequence), and the maximum density of through holes D M within the thin layer of the final structure.
[0130] At block 120 , a thickness to be transferred is selected. At block 130 , it is checked whether the density of through holes within the part of the donor substrate which has been transferred onto the support substrate is higher than the selected maximum density DM or not.
[0131] If yes, the thickness to be transferred is increased (block 140 ) and block 130 is thereafter repeated. If no, the first operation of the finishing sequence is performed. In this case, at block 150 , an RTA operation is performed. As already stated hereabove, such an RTA operation has no effect on through holes, but helps reducing the depth of the shallow holes.
[0132] At block 160 , the second operation of the finishing sequence, an SOx operation, is performed. As stated above, such an SOx operation is effective for thinning the transferred thin layer, but increases the through holes density according to the thickness consumption.
[0133] At block 170 , following the SOX operation, and similarly to block 130 , it is checked whether the density of through holes within the part of the donor substrate which has been transferred onto the support substrate is higher than the selected maximum density D M or not.
[0134] If yes, at block 180 , it is checked whether it is possible to decrease the thickness consumption of the SOx operation (performed at block 160 ). This is done by taking into account the selected particular finishing sequence, and the selected final thickness Tf. If the thickness consumption can be decreased, the SOx operation is performed (block 160 ) according to this newly set operative conditions. If the thickness consumption cannot be decreased, then block 140 is performed (that is increase of the transferred thickness).
[0135] Coming back to block 170 , if the density of killing holes after the SOx operation is lower than the maximum density D M , the next operation of the finishing sequence (here an RTA operation which does not consume thickness and does not modify the killing holes density) is performed at block 190 .
[0136] A SOx operation is thereafter performed at block 200 . At blocks 210 and 220 operations are performed which are similar to those performed respectively at blocks 170 and 180 . Following the SOx operation, and provided that (block 210 ) the through holes density is lower than the maximum density D M , the final SOI product conforms to the specifications (defined at block 110 ) is obtained at block 230 .
[0137] It will be understood that the flowchart of FIG. 11 is purely illustrative and that the present invention is by no means limited to the embodiments described and represented, but the man skilled in the art will be able to bring many alternatives or modifications there.
[0138] While illustrative embodiments of the invention are disclosed herein, it will be appreciated that numerous modifications and other embodiments can be devised by those of ordinary skill in the art. In one embodiment, a maximum thickness for the transferred semiconductor layer to obtain the desired results is also determined. Features of the embodiments described herein can be combined, separated, interchanged, and/or rearranged to generate other embodiments. Therefore, it will be understood that the appended claims are intended to cover all such modifications and embodiments that come within the spirit and scope of the present invention.
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A method for configuring a process for treating a semiconductor wafer. A minimum layer thickness of a transferred layer to be provided is determined to obtain a processed layer that has a preselected target thickness and target maximum density of through holes that extend completely therethrough, by conducting a predetermined finishing sequence of operations that improve the surface quality of the layer. The minimum thickness is determined such that the density of through holes remains below the target maximum density after each operation in the finishing sequence.
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BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to a fermentation process for preparing erythritol with high productivity using Trichosporonoides madida DS 911, more specifically, for preparing erythritol by optimizing the culture conditions such as pH, temperature, aeration rate and agitation speed, and by developing the process of fed-batch culture such as feeding strategy of substrate and composition of feeding substrate.
2. Description of Prior Art
Erythritol, a four carbon sugar alcohol, is a naturally occurring substance and is widely distributed in nature. Like most of the other polyols, it is a metabolite or storage compound for seaweeds and mushrooms. Fruits like melons, grapes and pears also contain erythritol. As it is often produced by bacteria, fungi, and yeasts, erythritol also occurs frequently in fermented food like wine, beer and soy sauce.
Erythritol is a moderately sweet bulking agent with 70˜80 percent of the sweetness of sucrose in a 10 percent solution. Its high negative heat of solution provides the crystalline material with a strong cooling effect. As it has a taste which is very close to sucrose and with no bitter aftertaste, it is ideal to improve the taste in combination with intensive sweetener like aspartame.
Erythritol production from natural sources such as fruits and vegetables is not practical due to their relative small amounts. Erythritol can be chemically produced by reduction of meso-tartarate, oxidation and reduction of 4,6-o-ethylidene-D-glucose, hydrolysis of dealdehyde starch, or hydrogenation process. Since erythritol production by the chemical methods has been found to be expensive, it is worthwhile to explore an alternative method for the effective production of erythritol using microorganisms.
Erythritol can be biologically produced by microorganisms, especially genus of Candida (U.S. Pat. No. 3,756,917); genus of Aureobasidium (JP Pat. No. 2,626,692 and U.S. Pat. No. 4,923,812); genus of Trichosporonoides (Y. K. Park, Biotechnology Letters 15 (1993) pp 383-388) and genus of Moniliela (Hajiny, Applied Microbiology 12 (1964) pp 240-246).
However, the methods using such microorganisms have a few drawbacks in large scale production. More specifically, the method disclosed in U.S. Pat. No. 3,756,917 using the genus of Candida has low productivity due to its long cultivation period, even though the conversion ratio from n-paraffin is so high.
In the case of the genus of Aureobasidium, the method shows high fermentation yield of erythritol in the concentrated glucose medium compared to other microorganisms. However, the low production rate causes low productivity of erythritol in the case of batch mode fermentation (JP Pat. No. 2,626,692). Even though the productivity is highly increased in the case of cell-recycled continuous culture, there is no successful application in the large scale more than 50 m 3 in industry (U.S. Pat. No. 4,923,812).
On the other hand, the method using the genus of Trichosporonoides shows low productivity due to its long cultivation period even though the conversion ratio is comparatively high. Even though the method using the genus of Moniliela shows high conversion ratio in the high cencentrated glucose medium, the foam vigorously occures during the fermentation, which has to be removed using lots of xanthan gum.
SUMMARY OF THE INVENTION
The object of the present invention is to provide novel cell of Trichosporonoides madida DS 911, which was deposited to Korea Research Institute of Bioscience and Biotechnology, Korean Collection for Type Cultures (Address: KCTC, KRIBB #52, Oundong, Yusong-ku, Taejon 305-333, Republic of Korea), with accession number KCTC-0496BP on Jun. 18, 1998 under Budapest treaty, for preparing erythritol with high productivity.
The other object of the present invention is to provide the optimal culture conditions for maximum productivity of erythritol using Trichosporonoides madida DS 911 deposited to Korea Research Institute of Bioscience and Biotechnology with accession number KCTC-0496BP comprising the step of:
i) fermenting glucose medium with cells wherein
a) composition of medium for maximum production of erythritol consists of 30˜45 (w/v)% of glucose, 0.1˜0.3 (w/v)% of yeast extract, 3˜6 (w/v)% of corn steep liquor and 0.1˜0.2 (w/v)% of phytic acid;
b) pH of culture medium is 3˜4;
c) temperature of cultivation is 30˜35° C.;
d) aeration rate of the medium is 0.5˜1.0 volume of air per volume of medium per minute; and
e) agitation speed of the medium is 300˜400 rpm;
ii) removing cells and other residue from the fermentation medium; and
iii) separating and recovering erythritol from the fermentation medium of step (ii).
The further object of the present invention is to provide a fed batch fermentation process, wherein the glucose and corn steep liquor are fed together after the bleeding of culture broth from the fermentor, when the glucose was exhausted in the culture broth such as; wherein the fermentation is fed batch fermentation which characterizes
i) feeding 10˜40% culture broth when glucose is wholly depleted in culture broth;
ii) supplying the same volume of substrate, after feeding the culture broth; on condition that the composition of feeding substrate is glucose and corn steep liquor, and glucose concentration in culture broth is adjusted to 10˜30%, and corn steep liquor to 0.05˜2%.
DETAILED DESCRIPTION OF THE INVENTION
The present invention concerns a method for obtaining erythritol with a high yield and a high volumetric productivity using Trichosporonoides madida DS 911.
The novel cells used for the present invention are isolated by following method.
The material collected from honey comb is inoculated in a liquid medium consisting of 38˜42% of glucose, 0.9˜1.1% of yeast extract et al., suspended and cultivated for 5 days at 30° C. in a shaking incubator. The cultivated solution is spreaded in a plate medium consisting of 38˜42% of glucose, 1.8˜2.2% of yeast extract et al. and cultivated for 3 days at 30° C. The single colony is selected and cultivated in a medium consisting of 28˜32% of glucose, 0.4˜0.6% of yeast extract, 0.09˜0.11% of urea et al. and cultivated for 5 days at 30° C. Then, Trichosporonoides madida DS 911 is isolated as the most erythritol producer compared to those of other cells by HPLC analysis.
This cell was named Trichosporonoides madida DS 911 and deposited to Korea Research Institute of Bioscience and Biotechnology with accession number KCTC-0496BP under Budapest Treaty.
The followings are biochemical properties of novel cell Trichosporonoides madida DS 911.
1. Morphological property
Colonies are usually restricted, and their surface is smooth or cerebriform, and initially cream colored, often finally olivaceous-brown in the PCA medium.
Budding cells often present, and their shapes are ellipsoidal, frequently composing a pseudomycelium in the PCA medium.
Hyphae is infrequently formed on malt agar with 40% additional saccharose, and it is hyaline, smooth and thin-walled, 2.5-3 μm wide, soon changing over into conidial chains.
Conidia is arising in terminal or lateral, unbranched or once branched, and acropetal chains from undifferentiated hyphae. Each chain is comprising up to 6 conidia, which are globose or ellipsoidal, and 6.5-15×3.5-7 μm on average, with inconspicous scars; terminal conidia is the shortest, and lower conidia is arthroconidium-like, and cylindrical with rounded ends.
2. Physiological properties
TABLE 1______________________________________Fermentation property of sugar (*1)______________________________________ D-glucose + D-galactose v Sucrose - Maltose - Lactose - Raffinose -______________________________________ (note) *1: The fermentation property was measured by the method of J. Lodder et al. using Wickerham preparation medium. v: variable
TABLE 2______________________________________Availability of sugar (*2)______________________________________D-glucose + D-galactose - L-solbose - Sucrose + Maltose v Cellobiose - Trehalose - Lactose - Melibiose - Raffinose - Melezitose - Inulin - D-xylose + L-arabinose + D-arabinose v D-ribose + L-rhamnose - Glycerol - Erythritol v D-mannitol v α-methyl-D-glucoside - Salicin - Inositol -______________________________________ (note) *2: The availability of sugar was measured by Biolog kit. v: variable
TABLE 3______________________________________Other properties______________________________________Availability of nitrate + growth at 36° C. + necessity of vitamin - urea decomposition + DBB (*3) +______________________________________ (note) *3: Diazonium Blue B
The microorganism of present invention has pseudohyphae, arthrospore and blastospore, and the shape of its colony is restricted and cerebriform. Therefore, the novel cell is classified as the species of Trichosporonoides madida. The inventors named this cell Trichosporonoides madida DS 911.
The followings are culture method using Trichosporonoides madida DS 911 for preparing erythritol with the maximum productivity.
Seed culture
The frozen (-70° C.) cells of Trichosporonoides madida DS 911 are cultivated in growth medium [30˜50 (w/v)% of glucose, 0.9˜1.1 (w/v)% of yeast extract and 1.9˜2.1 (w/v)% of agar] at 32˜38° C. for 3 days. And, the obtained cells are cultivated in growth medium [30˜50 (w/v)% of glucose, 0.09˜0.11 (w/v)% of yeast extract and 4˜6 (w/v)% of corn steep liquor and 0.1˜0.2 (w/v)% of phytic acid] at 32˜38° C. for 2 days in a shaking incubator. This seed culture is transferred to a main fermentor for the erythritol production.
Main Culture
Experiments with fermentation medium are performed at 30˜35° C. and 300˜400 rpm in a 50L fermentor. The fermentation medium consists of 30˜45 (w/v)% of glucose, 0.1˜0.5 (w/v)% of yeast extract, 3˜6 (w/v)% of corn steep liquor and 0.1˜0.2 (w/v)% of phytic acid as carbon source and nitrogen sources. Aeration rate is in the range of 0.5˜1.0 vvm.
The fermentation process is preferably by fed-batch process. When the glucose is completely consumed in the medium, the concentration of erythritol is measured by high performance liquid chromatography equipped with carbohydrate analysis column (YMC pack polyamine II, Japan).
The conversion yield of erythritol is 40˜50% and volumetric productivity is 1.5˜2.0 g/L-hr in fed-batch cultures, which correspond to 5˜15% increase compared with simple batch fermentation. The culture time includes the time that used for the prepartion of culture medium.
Finally the fermentation medium is centrifuged for removing cells and other residues, and the supernatant is filtered and purified for obtaining erythritol crystal.
The present invention can be explained more specifically by following examples.
EXAMPLE 1
The frozen (-70° C.) cells of Trichosporonoides madida DS 911 are cultivated in the medium [40 (w/v)% of glucose, 1.0 (w/v)% of yeast extract and 2.0 (w/v)% of agar] at 35° C. for 3 days. Thereafter, the obtained cells are cultivated in growth medium [30 (w/v)% of glucose, 0.1 (w/v)% of yeast extract, 5 (w/v)% of corn steep liquor and 0.1 (w/v)% of phytic acid] at 35° C. for 2 days in a shaking incubator. This seed culture broth is transferred to a main fermentor for the production of erythritol.
Experiments with fermentation medium are performed at 35° C. and 300 rpm, 1.0 vvm for 3 days in a 50L fermentor. The fermentation medium consists of 30 (w/v)% of glucose, 0.1 (w/v)% of yeast extract, 4 (w/v)% of corn steep liquor and 0.1 (w/v)% of phytic acid as carbon source and nitrogen sources.
After 72 hours fermentation, the final concentration of erythritol is 14.1% and a small amount of glycerol is obtained. Finally the fermentation medium is centrifuged for removing cells and other residues, and the supernatant is filtered and purified by active carbon and ion exchange resin for obtaining the crystal of erythritol. The melting point of obtained crystal is 122° C. and by HPLC and NMR analysis, it is identified as meso-erythritol.
EXAMPLE 2
Experiments with fermentation medium are performed at 35° C. and 200 rpm for 5˜8 days in a shaking incubaor. The fermentation medium consists of 30˜45 (w/v)% of glucose, 0.1 (w/v)% of yeast extract, 4 (w/v)% of corn steep liquor and 0.1 (w/v)% of phytic acid as carbon source and nitrogen sources. Table 4 shows the results of the fermentation.
TABLE 4______________________________________Concentration Fermentation of glucose period Erythritol Glycerol Yield (%) (day) (g/L) (g/L) (%)______________________________________30 5 141 2 47 35 6 165 6 47 40 7 184 14 46 45 8 189 25 42______________________________________
EXAMPLE 3
Experiments with fermentation medium are performed at 35° C. and 200 rpm for 5 days in a shaking incubator. The fermentation medium consists of 40 (w/v)% of glucose, 0.1 (w/v)% of yeast extract, 4 (w/v)% of corn steep liquor and 0.1 (w/v)% of phytic acid as carbon source and nitrogen sources. The pH is adjusted to 3.5˜5.0. Table 5 shows the results of the fermentation.
TABLE 5______________________________________ Erythritol Glycerol Yield pH (g/L) (g/L) (%)______________________________________3.0 136 5 45 3.5 141 2 47 4.0 142 3 47 5.0 140 3 47______________________________________
EXAMPLE 4
Experiment with fermentation medium is performed at 35° C. and 300 rpm, 1.0 vvm for 84 hours in a 50L fermentor. The fermentation medium consists of 40 (w/v)% of glucose, 0.1 (w/v)% of yeast extract, 4 (w/v)% of corn steep liquor and 0.1 (w/v)% of phytic acid. The pH is adjusted to 3.5. After 84 hours of fermentation, the final concentration of erythritol is 18.9% and the productivity of erythritol is 2.25 g/L-h which corresponds to more than 10% higher productivity compared with that in the genus of Aureobasidium (JP Pat. No. 2,626,692).
EXAMPLE 5
Experiments with fermentation medium are performed at 35° C. and 300 rpm, 1.0 vvm in a 50L fermentor. The fermentation medium consists of 40 (w/v)% of glucose, 0.1 (w/v)% of yeast extract, 4 (w/v)% of corn steep liquor and 0.1 (w/v)% of phytic acid as carbon source and nitrogen sources. The pH is adjusted to 3.5. When the glucose was used up, 5L of culture broth is bleeded and the same volume of glucose syrup (720 g/L) and 175 g of corn steep liquor are inserted to the fermentor. After 21 hours of fermentation, glucose is exhausted. The final concentration of erythritol is 21.1% and the erythritol concentration of bleeded culture broth is 18.7%. The productivity of erythritol is 1.84 g/L-h.
EXAMPLE 6
Experiments with fermentation medium are performed at 35° C. and 300 rpm, 1.0 vvm in a 50L fermentor. The fermentation medium consists of 40 (w/v)% of glucose, 0.1 (w/v)% of yeast extract, 4 (w/v)% of corn steep liquor and 0.1 (w/v)% of phytic acid as carbon source and nitrogen sources. The pH is adjusted to 3.5. When the glucose is used up, 10L of culture broth is bleeded and the same volume of glucose syrup and 350 g of corn steep liquor are fed into the fermentor. After 42 hours of fermentation, glucose is completely exhausted. The final concentration of erythritol is 23.3% and the erythritol concentration of bleeded culture broth is 18.5%. Volumetric productivity is 1.91 g/L-hr which correspond to 10% increase compared with the simple batch fermentation (Example 4).
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The present invention relates to a fermentation process for preparing erythritol with high productivity using Trichosporonoides madida DS 911, more specifically, for preparing erythritol by optimizing the culture conditions such as pH, temperature, aeration rate and agitation speed, and by developing the process of fed-batch culture such as feeding strategy of substrate and composition of feeding substrate.
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PRIOR RELATED PROVISIONAL AND PATENT APPLICATIONS
[0001] This Application is related to and claims the benefit of the filing date of prior filed U.S. Provisional Patent Application No. 60/267,657, file Feb. 9, 2001. This application is a continuation-in-part of U.S. patent application Ser. No. 10/074,543, filed Feb. 11, 2002, and a continuation-in-part of U.S. patent application Ser. No. 09/971,539 filed Oct. 2, 2001, and a continuation-in-part of U.S. patent application Ser. No. 09/918,999, filed Jul. 31, 2001 and a continuation-in-part of U.S. patent application Ser. No. 09/844,818 filed Apr. 27, 2001.
BACKGROUND OF THE INVENTION
[0002] 1. Field of the Invention
[0003] The present invention relates to the field of power generation using thermoelectric devices.
[0004] 2. Description of the Related Art
[0005] Although it has long been understood that thermoelectric devices can be used to generate power, thermoelectric power generation has been little utilized because the efficiency of present generator design and the power density of such generators are too low.
[0006] Historically, solid-state electrical power generating systems are constructed from TE Modules or stand-alone TE elements placed between a source of heat and a heat sink. The parts are designed with no moving parts in the power generator its self. Generally, systems that use hot and cold working fluids as the hot and cold sources employ fans to transport the fluids to the assembly.
[0007] In other applications, pressurized air and fuel are combusted within the generator. Still in other applications, such as automotive exhaust waste power converters, heat is transported to the generator by the exhaust system. In these devices, the waste heat is removed either by external fans supplying coolant or by free convection through finned radiators.
[0008] In applications such as generators that employ nuclear isotopes as the heat source, individual TE elements are configured to produce electrical power. Each TE element is attached to an isotope heat source on the hot side, and to a waste heat radiator on the cold side. No parts move during operation.
SUMMARY OF THE INVENTION
[0009] New hetrostructure thermoelectric, quantum tunneling, very thin plated, and deposited thermoelectric materials operate at substantially higher power densities than typical of the previous bulk materials and offer the potential for higher system efficiency.
[0010] Successful operation of thermoelectric devices with high power density requires high heat transfer rates both on the cold and hot side of TE Modules. One way to achieve this is through rotary designs that lend themselves to high fluid flow rates, and hence, high thermal power throughput. In one preferred embodiment, rotary systems in which a portion of the heat exchanger acts as fan blades, and thereby contributes to working fluid flow, can reduce power into the fan, simplify system design and reduce size.
[0011] Further, the heat transfer rate in many systems can be increased by employing heat pipes, as is well known to the art. Such devices use two-phase (liquid and vapor) flow to transport heat content from one surface to another. Where heat is to be removed at a heat source surface, the fluids' heat of vaporization is utilized to extract thermal power. The vapor flows to a surface at a lower temperature at the heat sink side where it condenses and thus gives up its heat of vaporization. The condensed fluid returns to the heat source side by capillary action and/or gravity.
[0012] Properly designed heat pipes are very efficient and transport large thermal fluxes with very low temperature differential. Some keys to efficient operation are that the liquid return process be efficient and that the entire heat source side be wetted at all times, to make liquid always available to evaporate and carry away thermal power. Similarly, it is important that the cool, sink side does not accumulate liquid since heat pipe working fluids are usually relatively poor thermal conductors. Thus, the sink side should shed liquid efficiently, to maintain effective thermal conductance surface.
[0013] In one embodiment, discussed herein, properly oriented heat pipes are combined with rotating heat exchange members, to utilize the centrifugal forces induced by rotation of the heat exchangers to improve performance. Rotary acceleration produced by fans and pumps can be up to several thousand Gs, so that with proper design, the liquid phase can be transported from the heat sink side to the heat source side very efficiently. Designs in which the colder end is closer to the axis of rotation than the hotter end, can exhibit very desirable heat transport properties because the centrifugal forces advantageously increase liquid phase flow when. As a result, such designs have increased power density, and reduced losses.
[0014] Finally, power generators that are combined with thermal isolation as described in U.S. patent application Ser. No. 09/844,818, entitled Improved Efficiency Thermoelectrics Utilizing Thermal Isolation can further increase performance.
[0015] One aspect described involves a thermoelectric power generator having at least one rotary thermoelectric assembly that has at least one thermoelectric module. The at least one rotary thermoelectric assembly accepts at least one working fluid and converts heat from the working fluid into electricity. Advantageously, the at least one rotary thermoelectric assembly comprises at least one hotter side heat exchanger and at least one cooler side heat exchanger. In one embodiment, the at least one hotter side heat exchanger has at least one hotter side heat pipe in thermal communication with the at least one thermoelectric module and a plurality of heat exchanger fins in thermal communication with the at least one hotter side heat pipe. In one embodiment, the at least one cooler side heat exchanger has at least one cooler side heat pipe in thermal communication with the at least one thermoelectric module and a plurality of heat exchanger fins in thermal communication with the at least one cooler side heat pipe. In one embodiment, the least one working fluid is at least one hotter and at least one cooler working fluid.
[0016] Preferably, the heat pipes contain a fluid, and the heat pipes are oriented such that centrifugal force from the rotation of the rotary thermoelectric assembly causes a liquid phase of the fluid to gather in a portion in said heat pipes. For example, the fluid in the cooler side heat pipes is in a liquid phase at at least a portion of an interface to the at least one thermoelectric module, and the fluid in the hotter side heat pipes is in a vapor phase at at least a portion of an interface to the at least one thermoelectric module.
[0017] In one embodiment, a motor coupled to the at least one rotary thermoelectric assembly spins the at least one rotary thermoelectric assembly. In another embodiment, the least one working fluid spins the at least one thermoelectric assembly. Preferably, the spinning pumps the working fluid through or across the heat exchangers, or both through and across the beat exchangers.
[0018] In one preferred embodiment, the at least one rotary thermoelectric assembly has a plurality of thermoelectric modules, at least some of the thermoelectric modules thermally isolated from at least some other of the thermoelectric modules. In another embodiment, the at least one hotter side heat exchanger has a plurality of portions substantially thermally isolated from other portions of the hotter side heat exchanger.
[0019] Another aspect described herein involves a method of generating power with at least one thermoelectric assembly having at least one thermoelectric module. The method involves rotating the at least one thermoelectric assembly, passing at least one first working fluid through and/or past a first side of the at least one thermoelectric assembly to create a temperature gradient across the at least one thermoelectric module to generate electricity, and communicating the electricity from the at least one thermoelectric module. In one embodiment, the method also involves passing at least one second working fluid through and/or past a second side of the at least one thermoelectric assembly. The rotation may be obtained in any number of ways, such as with a motor, with the working fluid itself, and in any other feasible manner to spin the thermoelectric assembly.
[0020] Preferably, the at least one thermoelectric assembly has at least one first side heat exchanger and at least one second side heat exchanger, and the step of passing the at least one first working fluid involves passing the at least one first working fluid through and/or past the first and/or second side heat exchanger.
[0021] As with the apparatus, in one embodiment, the at least the at least one first side heat exchanger has at least one first side heat pipe in thermal communication with the at least one thermoelectric module and a plurality of heat exchanger fins in thermal communication with the at least one first side heat pipe. Advantageously, the heat pipes contain a fluid and are oriented such that centrifugal force from the rotation of the at least one thermoelectric assembly causes a liquid phase of said fluid to gather in a portion in said heat pipes. The configurations for this method are as with the apparatus.
[0022] Another aspect described involves a thermoelectric power generation system having a source of at least one hotter working fluid, a source of at least one cooler working fluid, and at least one rotary thermoelectric assembly having at least one thermoelectric module, wherein the rotary thermoelectric assembly accepts the at least one hotter working fluid and converts heat from the hotter working fluid into electricity. Preferably, the system also has an exhaust for the at least one hotter and the at least one cooler working fluids, and at least one electrical communication system to transfer electricity from the rotary thermoelectric assembly.
[0023] In one embodiment, the at least one rotary thermoelectric assembly comprises at least one hotter side heat exchanger and at least one cooler side heat exchanger. As with the previous method and apparatus discussion, in one embodiment, at least the at least one hotter side heat exchanger has at least one hotter side heat pipe in thermal communication with the at least one thermoelectric module and a plurality of heat exchanger fins in thermal communication with the at least one hotter side heat pipe. Similarly, in one embodiment, at least the at least one cooler side heat exchanger may have at least one cooler side heat pipe in thermal communication with the at least one thermoelectric module and a plurality of heat exchanger fins in thermal communication with the at least one cooler side heat pipe. Thermal isolation may also be utilized.
[0024] These and other aspects and benefits of the present description will be apparent from the more detailed description of the preferred embodiments below.
BRIEF DESCRIPTION OF THE DRAWINGS
[0025] FIGS. 1 A- 1 C depict a general arrangement of a thermoelectric generator that hot and cold fluids a motor and heat exchanger fins to create a temperature differential across a TE Module. Electrical power is produced from the thermal power within the hot side fluid stream.
[0026] [0026]FIG. 1G further depicts a general arrangement of a thermoelectric generator in which the flow and pressure of a working fluid spins the generator assembly, thus eliminating the need for the electric motor shown in FIGS. 1C and 1D
[0027] [0027]FIG. 2A depicts a TE Module, heat pipes and heat exchanger assembly for generally axial fluid flow in a rotary solid-state power generator.
[0028] [0028]FIG. 2B gives a detailed cross sectional view of the assembly of FIG. 2A
[0029] [0029]FIG. 2C gives a second view of a segment of the assembly of FIG. 2A.
[0030] [0030]FIG. 3A depicts a sectional view of a TE Module, heat pipes and heat exchanger assembly for generally radial fluid flow in a rotary power generator.
[0031] [0031]FIG. 3B shows a detailed, cross-sectional view of the assembly of FIG. 3A.
[0032] [0032]FIG. 4 depicts an axial flow power generator wherein the hot and cold fluids flow generally parallel to one another in the same general direction. The generator utilizes thermal isolation and heat pipes to improve energy conversion efficiency.
[0033] [0033]FIG. 5 depicts a radial flow power generator wherein the hot and cold fluids flow generally parallel to each other in the same direction. The generator utilizes thermal isolation and heat pipes to improve efficiency.
[0034] [0034]FIG. 6 depicts an axial flow generator with hot and cold fluids flowing in generally opposite directions to one another. Advantageously, the TE Modules and heat exchangers are thermally isolated to improve efficiency and increase power density.
[0035] [0035]FIG. 7 depicts a radial flow generator with the hot and cold fluids flowing generally in opposite directions. Advantageously, the TE Modules are thermally isolated. Heat pipes are employed to both increase efficiency and power density.
[0036] [0036]FIG. 8 depicts a power generator with both generally radial and axial flows. A solid conductive heat transfer member is utilized to transfer heat between the TE Module and the hot side fin.
[0037] [0037]FIG. 9 depicts a portion of an axial flow power generator in which current flows through TE elements or modules and heat pipes in a circular direction about the axis of rotor rotation.
[0038] [0038]FIG. 10 depicts a system block diagram of a thermoelectric power generator.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
[0039] In the context of this description, the term Thermoelectric Module or TE Module are used in the broad sense of their ordinary and customary meaning, which is (1) conventional thermoelectric modules, such as those produced by Hi Z Technologies, Inc. of San Diego, Calif., (2) quantum tunneling converters (3) thermoionic modules, (4) magneto caloric modules, (5) elements utilizing one, or any by combination of, thermoelectric, magneto caloric, quantum, tunneling and thermoionic effects, (6),) any combination, array, assembly and other structure of (1) through (6) above.
[0040] In this description, the words cold, hot, cooler, hotter and the like are relative terms, and do not signify a temperature range. For instance, the cold side heat exchanger may actually be very hot to the human touch, but still cooler than the hot side. These terms are merely used to signify that a temperature gradient exists across the TE Module.
[0041] In addition, the embodiments described in this application are merely examples, and are not restrictive to the invention, which is as defined in the claims.
[0042] FIGS. 1 A- 1 F depict a general arrangements for a rotary thermoelectric power generator 100 . FIG. 1A is a perspective view. FIG. 1B is a view of a rotor assembly 135 as visible through the slots 126 of FIG. 1A. FIG. 1C is a cross section through the rotary thermoelectric power generator 100 . FIGS. 1 D- 1 F provide additional detail for various portions of the generator. A rotor assembly 135 (best seen in FIGS. 1B and 1C) is comprised of TE Module 101 , in good thermal contact with hot side heat exchanger 102 , such as heat transfer fins, on one side and a cold side heat exchanger 103 , such as heat transfer fins, on the other. Insulation 109 separate hot and cold sides. Insulation 109 rigidly connects the rotor parts to a motor rotor 110 . The TE Module 101 is depicted here for explanatory purposes and is comprised of TE elements 104 and circuitry 129 . At contact points 124 , 125 , wires 123 electrically connect TE Module 101 to portions 117 , 119 of shaft assembly 130 that are electrically isolated from each other, TE Module 101 , hot side heat exchanger 102 , cold side heat exchanger 103 , insulation 107 , 109 , wiring 123 , circuitry 129 and shaft portions 117 , 119 all form a rigid rotatable unit.
[0043] Motor assembly 111 is connected to motor rotor 110 by bearings 144 (FIG. 1F). Slip ring contact 118 is in electrical communication with shaft member 119 , and slip ring contact 120 is in electrical communication with shaft member 117 . Wiring 122 connects to slip ring contacts 118 and 120 through circuitry 132 and other circuitry not shown, such as traces on a circuit board or other conventional circuit connections. Wiring 122 also connects to motor assembly 111 , through a circuit board 112 and other circuitry not shown.
[0044] Spokes 113 (best seen in FIG. 1A) mechanically attach inner wall 114 (of FIG. 1 C) to motor base 116 and thereby to the motor assembly 111 . Hot side fluid filter 128 is attached to outer housing 131 , and cold side fluid filter 127 is supported by vanes 115 and attached to an extension 133 of outer housing 131 . Openings 126 in the outer housing, such as slots, allow fluid 106 , 108 passage through outer housing 131 . A hot working fluid 105 , 106 (FIGS. 1C and 1D) is confined to a chamber defined by outer wall 131 , openings 126 , insulation 109 , filter 128 and TE Module 101 . Cold working fluid 107 , 108 is confined by inner wall 114 , vanes 115 , outer housing extension 133 , motor base 116 and filter 127 .
[0045] Hot fluid 105 passes through the hot side filter 128 and transfers heat to the hot side heat exchanger 102 . The interface between the hot side heat exchanger 102 and TE Module 101 is thus heated. Similarly, cold fluid 107 passes through cold side filter 127 and absorbs heat from cold side heat exchanger 103 . Thus, the interface between the cold side heat exchanger 103 and TE Module 101 is cooled. The temperature gradient (heat flow) across the TE Module 101 generates electrical power. The electrical power is transferred through wires 123 , to conduct points 124 , 125 , to shaft portions 117 , 118 and through slip ring contacts 118 , 120 and to wires 122 (best seen in FIG. 1F).
[0046] Motor assembly 111 acting on motor rotor 110 spins the rotor assembly. In one embodiment, the heat exchangers 102 , 103 are configured as fins oriented longitudinally away from the axis of rotation of the rotor assembly. In this configuration, the heat exchangers 102 , 103 advantageously act as fan blades of a centrifugal fan or blower and thereby continuously pump working fluids 105 , 107 in order to maintain a temperature differential across TE Module 101 . A portion of the heat flow across TE Module 101 is continuously converted to electrical power. Hot working fluid 105 is cooled as it passes through the hot side heat exchanger 102 and exits as waste fluid 106 through openings 126 . Similarly, cold working fluid 107 is heated as it passes through cold side heat exchanger 103 and exits as waste fluid 108 through openings 126 .
[0047] The benefits of this rotational thermoelectric power generator will be explained in detail with specific configurations for the rotary assembly 135 in the following figures. The rotation of the heat exchanger thermoelectric module as a unit allows one or more heat exchangers to be used as fan blades for pumping the working fluid. In addition, other benefits and uses for rotation may be obtained in increasing the efficiency of the power generation system and increasing power density, as further explained below.
[0048] [0048]FIG. 1D depicts a closer view of cold and hot side working fluid movements for the power generator 100 . The TE Module 101 is in good thermal communication with the hot side heat exchanger 102 and a cold side heat exchanger 103 . The two sides are separated by insulation 109 . Hot side fluid 105 and 106 is contained by an outer wall 131 and insulation 109 . Similarly, cold side fluid 107 , 108 is contained by the inner wall duct 114 and insulation 109 . Motor rotor 110 is rigidly attached to insulation 109 so that insulation 109 , TE Module 101 and heat exchangers 102 , 103 move as a unit. Wires 123 connect TE Module 101 to rotary slip rings 118 , 120 as described in more detail in the discussion of FIG. 1F. Motor rotor 110 is connected through bearings 144 (FIG. 1F) to motor driver 140 and shaft 130 (shown in detail in FIG. 1F). Electrical wires 123 connect to TE Module 101 and shaft 130 .
[0049] A temperature gradient is produced across TE Module 101 by hot fluid 105 heating heat exchanger 102 and cool fluid 107 , cooling heat exchanger 103 . Hot fluid 105 cools and exits and cool fluid 107 is heated and exits. The movement of hot fluid 105 is created by the rotation of heat exchanger 102 componentry which act as vanes of a blower or radial fan. Motor rotor 110 and motor driver 140 produce the rotation. Fluid flow is guided by the outer housings and the insulation.
[0050] [0050]FIG. 1E shows a cross section of TE Module 101 and heat exchangers 102 , 103 . Heat exchangers 102 , 103 are shown as folded fins as is known to the art, but may be of any other suitable heat exchanger design, as an example, any advantageous designs found in Kays, William M., and London, Alexander L., Compact Heat Exchangers, 3 rd Edition, 1984, McGraw-Hill, Inc. Heat pipes and any other technology may be incorporated to enhance heat transfer.
[0051] [0051]FIG. 1F illustrates additional details of an embodiment of a slip ring assembly for transferring the electric power created TE Module 101 to external systems. The assembly consists of wires 123 in insulation 109 , one of which is electrically connected to inner shaft 119 , and a second to outer shaft 117 . Electrical insulation 142 mechanically connects inner and outer shafts 117 , 119 . Advantageously, outer shaft 119 is mechanically connected to motor rotor 110 and bearing 144 . Slip ring contact 118 is electrically connected to inner shaft 119 and slip ring contact 120 is electrically connected to outer shaft 117 .
[0052] [0052]FIG. 1G depicts an alternate configuration of a thermoelectric generator that uses flow and pressure of a working fluid to spin the generator assembly, thus eliminating the need for the electric motor shown in FIGS. 1C and 1D.
[0053] As depicted in FIG. 1G, the TE 101 , heat exchangers 102 , 103 and related parts comprising the rotatable parts of the thermoelectric generator are as identified in FIG. 1D, except that a fan 150 and insulation 109 are attached to form a rotatable unit. Bearings 152 , shaft 130 , and spokes 116 , 151 form the suspension for the rotatable parts.
[0054] In operation, working fluid 105 propels fan 150 . Power from the fan spins the rotatable parts. In this embodiment, the rotation acts to draw in cold working fluid 107 , as well as provide other benefits from rotation discussed in the description of FIGS. 2 to 7 and 9 .
[0055] The fan 150 is shown as a separate part. The same function can be achieved by using other designs that have heat exchangers or yet other parts shaped and positioned as to utilize power available in the hotter, colder and/or exhaust fluid streams to cause rotation. For Example, such a system could be used in the exhaust stream of a combustion engine, such as with an automobile. In such an example, what would otherwise simply be waste heat, is converted to electricity, and the exhaust flow spins the rotary thermoelectric assembly.
[0056] Motor rotor 110 , insulators 109 , 142 , and shafts 117 , 119 rotate as a unit and are supported by bearing 144 . Slip rings 118 , 120 transmit the electrical power produced within the rotating unit to an external electrical circuit. The slip rings 118 , 120 can be of any design known to the art, and the shafts 117 , 119 can be of any viable configuration that are conductive or contain conductive wires or members. The electrical power transmission parts and configuration can be of any design that conveys power from the rotating unit to external circuitry.
[0057] It should be understood that although FIG. 1 depicts a single rotary assembly, multiple rotary assemblies are also contemplated.
[0058] [0058]FIG. 2A depicts a cross-sectional view of rotor assembly 200 for a thermoelectric power generator of the form illustrated generally in FIG. 1. The rotor assembly 200 consists of a ring-shaped TE Module 201 in good thermal contact with a circular array of outer heat pipes 202 and a circular array of inner heat pipes 203 . A hot side heat exchanger 204 is in good thermal contact with outer heat pipes 202 , and a cold side heat exchanger 205 is in good thermal contact with inner heat pipes 203 . The rotor assembly 200 is generally symmetrical about its axis of rotation 211 .
[0059] In operation, the rotor assembly 200 spins about its axis of rotation 211 . Hot fluid (not shown) is in contact with the hot side heat exchanger 204 , which transfers heat flux to the outer heat pipes 202 , and to the outer surface of the TE Module 201 . A portion of the heat flux is converted to electrical power by the TE Module 201 . The waste heat flux passes through the inner heat pipes 203 , then to the cool side heat exchanger 205 and finally to a cooling fluid (not shown) in contact with the cool side heat exchanger 205 .
[0060] [0060]FIG. 2B presents a more detailed view of a cross-section of rotor assembly 200 through a heat pipe. As in FIG. 2A, the heat pipes 202 and 203 are in thermal contact with TE Module 201 . The TE elements 208 and electrical circuitry 209 complete the TE Module 201 . In one preferred embodiment, the heat pipes 202 , 203 are comprised of sealed shells 214 , 215 containing a heat transfer fluid. In operation, while the rotor assembly 200 spins about the axis 211 , the rotational forces push a liquid phase of heat transfer fluid away from the axis of rotation of the particular heat pipes 202 , 203 . The direction of the outward force induced by rotation is shown by arrow 210 . For example, in the heat pipe 202 , a liquid phase 206 forms an interface 212 with the vapor phase. The hot side heat exchanger 204 is in good thermal contact with the hot side heat pipe shell 214 . Similarly, the cool side heat pipes 203 , 215 , have heat transfer fluid 207 in a liquid phase and an interface 213 with the vapor phase. The cooler side heat exchanger 205 is in good thermal communication with the cool side heat pipe shells 215 .
[0061] The outward force 210 induced by rotor assembly 200 rotation acts to force the liquid phases 206 and 207 to the positions shown in FIG. 2B. Hot gas (not shown) transfers heat from the outer heat exchanger fins 204 to outer heat pipe shells 214 . The heat flux causes a portion of the liquid phase 206 on the hot side to vaporize. The vapor moves inward in the opposite direction to that indicated by arrow 210 , since it is displaced by denser liquid phase 206 . Vapor phase fluid in heat pipes 202 in contact with the interface of TE Module 201 and hot side heat pipe shells 214 transfers a portion of its heat content to the TE Module 201 , and condenses to the liquid phase. The rotation-induced force drives the dense liquid-phase in the direction indicated by the arrow 210 . The fluid cycle repeats as more heat is absorbed by the hot side heat exchanger 204 , transferred to the outer heat pipe shells 214 , and then to the outer surface of TE Module 201 .
[0062] Similarly, waste heat from the inner side of TE Module 201 causes the liquid phase 207 of the inner heat pipe fluid to boil and be convected inward to the inner portions of the inner heat pipe shells 215 . The cold working fluid (not shown) removes heat from the cooler side heat exchanger 205 , and adjacent portions of cooler side heat pipe shells 215 . This causes condensation of the fluid 207 . The liquid phase is driven by centrifugal force in the direction indicated by the arrow 210 , and accumulates against the TE Module 201 and the inner heat pipe shells 215 interface. This cycle constantly repeats, with the fluid constantly evaporating at one location, condensing at another, and being transported back to the first by centrifugal force.
[0063] The forces produced by the rotor assembly 201 rotation can be several times to thousands of times that of gravity, depending on rotor dimensions and rotational speed. Such centrifugal forces can enhance heat pipe heat transfer, thus allowing the rotor assembly 200 to operate with less heat transfer losses and at higher heat fluxes.
[0064] [0064]FIG. 2C shows a sectional view of the rotor assembly 200 of FIG. 2A viewed along the axis of rotation 211 . The TE Module 201 is in good thermal contact with the outer heat pipes 202 and the inner heat pipes 203 . The heat exchangers 204 , 205 , such as fins as shown, are in good thermal contact with the heat pipes 202 , 203 .
[0065] [0065]FIG. 2C shows individual heat pipe segments 202 , 203 and the TE Module 201 . The hot working fluid (not shown) flows through passages 216 between the outer heat exchanger fins 204 and the outer heat pipes 202 . Similarly, the cold working fluid (not shown) flows through the inner passages 217 between the inner heat exchanger fins 205 and the inner heat pipes 203 .
[0066] [0066]FIG. 3 depicts an alternative thermoelectric power generator rotor assembly 300 , in which, working fluids flow in a generally radial direction. The cross section view shows a disk-shaped TE Module 301 in good thermal contact with hot side heat pipes 302 and cold side heat pipes 303 . In good thermal contact with the hot side heat pipes 302 is a heat exchanger 304 , and with the cooler side heat pipes 303 is a cool side heat exchanger 305 . The rotor assembly 300 rotates about and is generally symmetrical about a centerline 310 .
[0067] In operation, the rotor assembly 300 spins about the centerline 310 , driven by a motor such as in FIG. 1. Hot working fluid (not shown) passing generally radially outward between the hot side heat exchanger 304 (fins in this depiction) and the hot side heat pipes 302 , transfers heat to the heat exchanger 304 and the outer heat pipes 302 and then to the TE Module 301 . Similarly, cold working fluid (not shown) passing generally radially outward through the center side heat exchanger 303 and the cooler side heat pipes 305 removes heat convected by the cooler side heat pipes 303 from the TE Module 301 . A portion of the thermal flux passing from the hotter side heat pipes 304 to the TE Module 301 and out through the cooler side heat pipes 305 is converted by TE Module 301 to electric power.
[0068] Rotation of the heat pipes 302 , 303 (configured as flattened tubular sections in this embodiment) advantageously act as fan blades that pump hot and cold working fluids (not shown) outward. Advantageously, the heat exchangers 304 , 305 and the heat pipes 302 , 303 are configured to maximize both heat transfer and fan fluid pumping action. Thus, the rotor assembly 300 functions both as the power generator and working fluid pump.
[0069] [0069]FIG. 3B shows a more detailed, cross-sectional view 311 through a heat pipe of the rotor assembly 300 depicted in FIG. 3A. The TE Module 301 is comprised of TE elements 309 and circuitry 310 . The TE Module 301 is in good thermal contact with heat pipes 302 , 303 . As with the FIG. 2 configuration, the hotter side heat pipes 302 are comprised of sealed shells 312 with a fluid having a liquid phase 306 and vapor phase, with an interface 314 . Similarly, the cooler side heat pipes 303 are comprised of sealed shells 313 , containing fluid with liquid phase 307 and vapor phase, with an interface 315 . The heat exchanger fins 304 , 305 are in good thermal communication with the heat pipes 302 , 303 . An arrow 308 points in the direction of an outward force generated as the rotary assembly rotates about the axis 310 .
[0070] In operation, the outward forces push the liquid phases 306 , 307 of the heat transfer fluids within the heat pipes 302 , 303 outward, forming the liquid phases 306 , 307 and the interfaces 314 and 315 . Heat flux from the hot side working fluid (not shown) flowing past the hot side heat exchanger 304 evaporates portions of the fluid 306 , which condenses at the hotter side heat pipe shells 312 at the TE Module 301 interface. Similarly, a portion of the heat flux passes through the TE Module 301 to its interface with cooler side heat pipe shells 313 , and into the cooler side heat pipe fluid 307 , causing the fluid 307 to boil. The vapor phase condenses on the inner portion of the cool side heat pipe shell 313 as heat is removed by transfer to the cooler side heat exchanger 305 , and to the cooler side working fluid (not shown). This heat transfer process is analogous to that described in more detail in the descriptions of FIGS. 2A, 2B and 2 C.
[0071] [0071]FIG. 4 depicts one side of another rotating power generator 400 in cross-section. A TE Module 401 is connected thermally to a cooler side heat exchanger 402 and a hotter side heat exchanger 403 . In the depicted embodiment, the cooler side heat exchanger 402 has segments of heat pipes 404 and fins 406 . Similarly, hotter side heat exchanger 403 has segments of heat pipes 405 and fins 407 . A cooler working fluid 408 , 410 is confined to a chamber formed by insulators 416 , 423 , 424 and a duct 412 . Similarly, a hotter working fluid 414 and 415 is confined by the insulators 423 , 424 and an outer duct 411 . Rotor insulation 416 is connected rigidly to a motor rotor 417 , the inner portion of the exchanger 402 , and thereby to the TE Module 401 and heat exchanger 403 . Wires 420 and a shroud 425 are connected rigidly to the TE Module 401 . Similarly, a fan blade assembly 413 is rigidly attached to the TE Module 401 . A shaft assembly 419 is attached to the motor rotor 417 , and to bearings 418 . A slip ring assembly 421 is in electrical communication to a shaft assembly 419 . The insulators 423 and 424 are configured to form a labyrinth seal 422 . Spokes 409 connect the left most bearing 418 to insulation 424 and to duct 411 .
[0072] The assembly formed by the motor rotor 417 , the insulators 416 , 423 , the heat pipes 402 , 403 , the TE Module 401 , the fan blades 413 , the wires 420 , the shaft 419 and the shroud 425 rotate as a unit. Rotation of the fan blades 413 provides motive force for the hot and the cold working fluids 408 , 410 , 414 , 415 .
[0073] The hot working fluid 414 enters from the left and transfers thermal energy to the hot side heat exchanger 402 and then, to TE Module 401 . The flow of the hot working fluid 414 is driven by the rotation of the fan blades 413 . Similarly, the cooler working fluid 408 enters from the left and extracts waste thermal energy from the cooler side heat exchanger 403 and the TE Module 401 . The electrical power created passes through the wires 420 and out of the rotating portion through the shaft assembly 419 and the slip ring assembly 421 , as was described in more detail in the discussion of FIG. 1F.
[0074] The heat pipes 402 , 403 are segmented to thermally isolate one portion from another for the purposes taught in U.S. patent application Ser. No. 09/844,818 filed Apr. 27, 2001, entitled Improved Efficiency Thermoelectrics Utilizing Thermal Isolation, which application is incorporated by reference herein. Heat transfer within the heat pipes 402 , 403 is enhanced by the centrifugal acceleration as discussed above, and thereby, increases efficiency of thermal power transport and the allowable power density at which the system can operate. By utilizing centrifugal force to enhance the heat transfer, the overall device can be more compact and employ thermoelectric materials that advantageously operate at high thermal power densities.
[0075] The seal 422 is representative of any seal configuration that suitably separates hot fluid 414 from cold fluid 408 with a moving to stationary boundary. In some configurations, the pumping power of the fan 413 in combination with the inlet geometry may negate the need for the seal 422 . Alternately, seal 422 may serve the function of providing separation of the hotter and cooler working fluids 408 , 422 if an external, alternate mechanism (not shown) to fan blades 413 provides the force to pump the working fluids 408 , 422 through the heat exchangers 402 , 403 . In such an embodiment, the fan 413 may be omitted or its function supplemented by an alternate fluid pump mechanism.
[0076] [0076]FIG. 5 depicts a power generator configuration in which the heat exchangers act as fan blades. The TE Module and heat exchanger are similar in concept to the configuration depicted in FIG. 3. The rotor assembly 500 consists of TE Modules 501 , cooler fluid heat exchanger 502 , a hotter fluid heat exchanger 503 , insulation 515 , 517 , spokes 508 and a motor rotor 509 , all of which are connected rigidly to one another to form a rigid unit that rotates about a shaft 510 . The cooler fluid heat exchanger 502 has heat pipes in good thermal contact with fins 504 . Similarly, the hotter fluids heat exchanger 503 has heat pipes in good thermal contact with fins 505 . Insulation 515 , 517 and a duct 507 form a chamber that confines a hotter working fluid 511 , 512 . Similarly, insulation 515 , 517 and a duct 506 form a chamber, which confines a cooler working fluid 513 , 514 . A seal 516 is formed in the insulation 515 , 517 to separate the hotter 511 and the colder working 513 fluids.
[0077] The assembly 500 operates by the motor rotor 509 providing motive force to rotate the heat exchangers 502 , 503 , which, in turn, creates a pumping action to pull hot and cold fluid through the heat exchangers 502 , 503 to produce a temperature gradient across the TE Module 501 . Electrical power generated thereby is extracted and transferred to external circuitry by the design shown in FIGS. 1 A- 1 E, or by any other transfer method acceptable in the environment.
[0078] Advantageously, several working fluids may be used within a single assembly. A generator such as that of FIG. 4 may have several sources of hot side working fluids each with a different composition and/or temperature. This condition can arise, for example, with waste electrical power generation systems that have several sources of exhaust gas to be processed with waste heated fluid from a boiler, dryer or the like. Such multiple sources of working fluids may be introduced through wall 411 at a position along the axis of rotation where the hot side working fluid 422 has been cooled to a temperature that when combined with an added working fluid, advantageously generates electrical power. In this circumstance, the heat flux may vary in some of the heat pipes 402 , 407 and fins 405 , 409 so that TE Modules 101 , heat pipes 402 , 207 and fins 405 , 409 may differ in their construction, size, shape, and/or materials from one section to the next in the direction of fluid flow. Also, insulation and fin structure can be used to separate different fluids. Finally, more than one cold side working fluid 409 , 410 can be utilized in combination with at least one hot side working fluid.
[0079] The design of FIG. 6 also utilizes heat pipes as described in FIG. 4. The assembly 600 of FIG. 6 utilizes counter-flow as taught in U.S. patent application Ser. No. 09/844,818, which is incorporated by reference herein. FIG. 6 depicts a cross-section of yet another rotary thermoelectric power generator. Advantageously, this embodiment also utilizes thermal isolation. The generator assembly 600 has a rotating assembly formed of a TE Module 601 , pairs of thermally isolated heat exchangers 602 , 603 , fan assemblies 610 , 613 with shrouds 607 , 614 , insulation 615 , 616 , 619 , 620 , 624 , a motor rotor 617 and a shaft assembly 618 .
[0080] Hotter side working fluid 611 , 612 is confined by insulation 609 , 615 , 619 , 620 , 621 . Cooler side working fluid 604 , 606 is confined by insulation 609 , 615 , 616 , 619 , 621 , and a duct 608 . Spokes 605 connect a bearing 622 to the insulation 615 .
[0081] Cooler side working fluid 604 enters from the left, absorbs thermal power from heat exchangers 602 , thereby cooling them, and is pumped radially outward by the centrifugal action of fan blades 610 . The fan blades 610 may or may not contain an inner shroud 607 which can be employed to provide structural support and act as a partial seal to keep hotter working fluid 611 separate from the cooler working fluid 606 , and help guide the cooler working fluid's 606 flow. The hotter working fluid 611 enters in a radially inward direction, conveys thermal power to hotter side heat exchangers 603 and then is pumped radially outward by the action of the rotating fan blades 613 . The shroud 614 may be employed to add structural rigidity to the fan blades 613 , act as a partial seal to separate cooler working fluid 604 from the exiting hotter working fluid 612 , and help guide the hotter working fluid's 612 flow.
[0082] [0082]FIG. 7 depicts a cross-section of yet another rotary thermoelectric power generator. The design of FIG. 7 is configured to operate in counter flow. The heat exchangers may or may not contain heat pipes to enhance heat transfer.
[0083] [0083]FIG. 7 depicts a radial flow power generator 700 . A rotating assembly consists of a TE Module 701 , heat exchangers 702 , 703 , with fins 704 , 705 , insulation 720 , fan blades 723 , a motor rotor 718 and a shaft 719 . Bearings 721 attach the shaft assembly 719 to a non-rotating duct 717 inner support 707 , spokes 722 and a duct 710 . The hotter working fluid 706 , 709 is confined by an inner support 707 , the duct 710 , insulation 720 , the TE Module 701 and an exhaust duct 711 . The cooler working fluid 712 , 713 , 714 is confined by exhaust ducts 711 , 716 , insulation 720 . the TE Module 701 and a duct 717 . A seal 715 separates the hotter working fluid 709 from the cooler working fluid 712 .
[0084] The assembly 700 operates using counter-flow of the same general type discussed in the description of FIG. 6. It operates in a generally radial direction with the hot side heat exchanger 702 with its fins 704 acting as rotating fan blades to pump hotter working fluid 706 , 709 . Cooler working fluid 712 , 713 , 714 responds to the net effect of a radially outward force produced by heat exchanger heat pipes 703 and fins 704 and a larger radially outward force produced by the rotation of fan blades 723 acting on the cooler side working fluid 713 , 714 . The net effect of the counteracting forces is to cause fluid 712 , 713 , 714 to flow in the directions shown in FIG. 7. Since, the larger blade force is generated by the position of fan blades 723 , being longer than, and extending radially outward farther than the heat exchangers 703 with its fins 705 . Alternately, any portion of the fluids' 706 , 709 , 712 , 713 , 714 motion could be generated by external fans or pumps. In such configurations, the fan 723 may be, but need not be, deleted.
[0085] Electrical power is generated and transmitted by methods and design described in FIGS. 1 and 5- 6 , or any other advantageous way.
[0086] [0086]FIG. 8 depicts a power generator that combines radial and axial geometries. The general arrangement 800 has a rotational portion consisting of a TE Module 801 , heat exchangers 802 , 803 , a thermal shunt 804 , insulation 811 , a fan assembly 808 and 809 , a duct 807 , a motor rotor 817 and a shaft assembly 818 . Cooler working fluid 805 , 815 is confined by a shroud 807 , insulation 811 , a fan duct 808 , and a wall 810 . Hotter working fluid 812 , 813 is confined by a shunt 804 , a shroud 807 , insulation 811 , 816 and a wall 814 . A bearing 819 connects rotating shaft assembly 818 to spokes 806 and wall 810 .
[0087] Operation is similar to that previously described in FIG. 7, except that the cooler working fluid 805 flows through heat exchanger 802 in a generally axial direction. As depicted herein, the thermal shunt 804 and the heat exchangers 802 , 803 may or may not contain heat pipes. Further, the heat exchangers 802 , 803 , the TE Module 801 and the thermal shunt 804 may or may not be constructed so as to be made up of thermally isolated elements as taught in U.S. patent application Ser. No. 09/844,818, entitled Improved Thermoelectrics Utilizing Thermal Isolation, filed Apr. 27, 2001, which patent application is incorporated by reference herein.
[0088] [0088]FIG. 9 depicts an integrated TE Module and heat exchanger. An assembly 900 is a segment of a ring-shaped array of TE Modules 901 with a center of rotation 909 a heat exchanger 902 with fins 904 , heat exchanger 903 with fins 905 and thermal insulation 908 . Gaps 906 , 907 electrically isolate sections of the fins 904 , 905 that are connected to the individual heat exchanger parts 902 , 903 . When operating, one heat exchanger 903 , for example, is cooled and the other heat exchanger 902 is heated creating a thermal gradient across TE Modules 901 . Electrical power is produced by the resultant heat flow.
[0089] In this configuration, the TE Modules 901 may be individual TE elements 901 with a current 910 flowing in a generally circular direction around the ring of which assembly 900 is a portion. In a portion where the TE Modules 901 are individual thermoelectric elements, for the current 910 to flow as shown, the elements 901 are alternately of N-and P-type. Advantageously, heat exchangers 902 , 903 are electrically conductive in that portion between the adjacent TE elements 901 . If the fins 904 , 905 are electrically conductive and in electric contact with heat exchangers 902 , 903 , adjacent fins must be electrically isolated from on another as indicated by gaps 906 , 907 . Electric power can be extracted by breaking the circular current flow at one or more locations and connecting, at the breaks, to electrical circuitry as discussed in FIG. 7.
[0090] Alternately, groups of elements can be between adjacent heat exchangers 903 , 902 , thus forming TE Modules 901 . Such TE Modules 901 can be connected electrically in series and/or parallel and may have internal provisions for electrical isolation so that gaps 906 , 907 are not needed. Thermal isolation between hot and cold sides may be maintained by insulation 1008 .
[0091] If the heat exchangers 902 , 903 contain heat pipes, advantageously, working fluids cool the inner heat exchangers 903 and heat the outer heat exchangers 902 .
[0092] [0092]FIG. 10 illustrates a block diagram of a thermoelectric power generator system 1000 . As illustrated, the system has a hotter working fluid source 1002 , a colder working fluid source 1004 , a generator assembly 1006 , exhaust fluid outputs 1008 , and electrical power output 1010 . The generator assembly 1006 is configured with any of the embodiments disclosed above, or any similar embodiment using the principals taught herein. A source of hotter fluid 1002 provide a heat source for the generator assembly 1006 . A source of colder fluid 1004 provide a source of working fluid sufficiently cooler in temperature to create an advantageous temperature gradient across the thermoelectric in the generator assembly 1006 . The waste working fluid exits the generator assembly at an output 1008 . Electrical power from the generator assembly 1006 is provided at a power output 1010 . This system 1000 is merely a generally exemplary system, and is not restrictive of the manner in which the generator assemblies of the present invention would be incorporated into a power generation system.
[0093] The individual teachings in this application may be combined in any advantageous way. Such combinations are part of this invention. Similarly, the teachings of U.S. application Ser. No. 09/844,818 entitled Improved Efficiency Thermoelectrics Utilizing Thermal Isolation, and U.S. application Ser. No. 09/971,539, entitled Thermoelectric Heat Exchanger related to rotary heat exchangers can be used in combination with this application to create variations on the teachings herein, and are part of this invention. For example, the heat exchangers of the hot and/or cold sides, in one embodiment, are configured in portions that are substantially thermally isolated from other portions of the heat exchanger. Similarly, portions of the thermoelectric module, in one embodiment, are thermally isolation from other portions of the thermoelectric module.
[0094] Accordingly, the inventions are not limited to any particular embodiment, or specific disclosure. Rather, the inventions are defined by the appended claims, in which terms are presented to have their ordinary and customary meaning.
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An improved thermoelectric power generation system utilizes rotary thermoelectric configurations to improve and increase thermal power throughput. These systems are further enhanced by the use of hetrostructure thermoelectric materials, very thin plated materials, and deposited thermoelectric materials, which operate at substantially higher power densities than typical of the previous bulk materials. Several configurations are disclosed.
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BACKGROUND OF THE INVENTION
Computed transaxial tomography techniques have recently been disclosed and developed. In particular there has recently been disclosed and claimed apparatus for producing circularly scanned charged-particles which, when striking a target, produce a rotating x-ray beam suitable for use in computed transaxial tomography. Such devices can operate using any one of a variety of beam scanning apparatus which are well known in connection with cathode-ray oscilloscopes, radar, etc. However, a major use of circularly scanned beams is for the production of fast x-ray scans, as in the case of taking x-ray "pictures" of moving objects, such as a human heart. Such fast x-ray scans require a rapidly scanned charged-particle beam, and if such a beam is to produce x-rays of adequate intensity, high beam currents must be employed. Because of space charge effects and other phenomena, the need for high beam currents automatically requires that the beam have a relatively large cross-section at the place where it is deflected. The beam must then be focused so as to converge strongly at the target in at least one dimension, so as to provide high resolution. The deflection and focusing of such high-current, large-cross-section beams requires a radically different approach from those taught by the prior art.
SUMMARY OF THE INVENTION
In one embodiment of the invention the objectives of high beam current and optimum focus in a circularly scanned x-ray device are accomplished through the use of a rotating dipole field. While such a field can be produced by mechanically rotating a simple dipole (i.e. a beam-deflecting magnet), in a preferred embodiment of the invention the rotating field is produced electrically using stationary coils.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
The invention may best be understood from the following detailed description thereof, having reference to the accompanying drawings in which:
FIG. 1 is a vertical central section showing somewhat schematically a circularly scanned x-ray device with which the rotating dipole field of the invention may be employed;
FIG. 2 is a diagrammatic view in longitudinal central section of one of a pair of pole pieces which may be rotated mechanically in accordance with the invention;
FIG. 3 is a section along the line 3--3 of FIG. 2;
FIG. 4 is a transverse section taken through coils embodying a second form of the invention;
FIG. 5 is a view similar to that of FIG. 4 except that the coils and magnetic material are folded out in a straight line from their actual annular position so as to show the arrangement of the windings;
FIG. 6 is a perspective view of the coils of FIGS. 4 and 5.
Referring to the drawings and first to FIG. 1 thereof, the apparatus therein shown is adapted to produce a circularly scanned x-ray beam. The x-rays are produced at a circular target 1, and x-ray collimators 2 collimate the emergent x-rays so that they are directed towards a patient 3 supported near the axis of the annular target 1. An annulus of detectors 4 is arranged as close as possible to the annular target 1. The output of the detectors 4 is delivered in a well-known manner to computer apparatus which provides the desired x-ray picture of a cross-sectional slice of the patient's body. The x-rays are produced at the target 1 by bombarding the same with a charged-particle beam 5. The charged-particle beam 5 is produced in a conventional particle accelerator 6 and is directed into a focusing ion lens arrangement 7 which may consist of quadrupoles or a solenoid. The charged-particle beam 5 is circularly scanned about the annular target 1 and simultaneously focused thereat by a deflector-focuser 8 constructed in accordance with the invention. The simplest form of deflector focuser 8 will now be described.
Referromg now to FIGS. 2 and 3, the deflector focuser therein shown comprises a simple pair of magnetic poles flanking the beam 5. One such magnetic pole is shown at 9 in FIG. 2, and the pair of pole pieces 9, 10, is shown in FIG. 3. As is well known, a uniform magnetic field such as that produced by pole pieces 9, 10 deflects a charged-particle beam into a circular path having a radius of curvature R. Because of the fringing fields, the effective length of the magnet is somewhat larger than the physical length of the pole pieces. Thus, in FIGS. 2 and 3 the incident effective field boundary is shown at 11 and the exit effective field boundary is shown at 12. Each charged particle in the beam 5 approaches the entrance effective boundary 11 in a rectilinear path, travels between boundaries 11 and 12 in a circular path of radius R, and emerges from the exit effective boundary 12 in a rectilinear path which is at an angle φ with respect to the incident path. The field strength and size of the pole pieces 9, 10 are so chosen that the angle φ will direct the charged-particle beam onto the annular target 1. The pole pieces 9, 10 are connected, in accordance with well-known techniques, by a yoke (not shown) and are energized by suitable coils (not shown). The charged-particle beam is then scanned over the target by simple mechanical rotation of the pair of pole pieces 9, 10. It will be appreciated that since both the size of the pole pieces and the strength of the magnetic field are variable parameters for the designer, the angle φ may be fixed and yet the radius of curvature R may still be varied if desired. This now permits adjustments in the design stage of the focusing of the charged-particle beam 5 in addition to deflection thereof.
The exit-fringing field of a simple dipole as shown in FIGS. 2 and 3 gives focusing in the transverse plane, and the focal length is a function of the exit angle β, which is the angle between the normal to the exit effective boundary 12 and the emergent ray. In general, β should not be less than φ/2, and the strength and dimensions of the magnetic field are chosen such that the focusing action for azimuthal focusing is as close to the target as possible. In the case of a beam which crosses the incident effective field boundary as parallel trajectories, if β = φ the exit fringing field does not produce any focusing in the median plane and the focusing action in the transverse plane has a focal length equal to or slightly greater than R/tan β. In accordance with usual terminology, the median plane is the plane of the drawing in FIG. 2 and is the plane perpendicular to the drawing which lies midway between the pole pieces 9 and 10 of FIG. 3. Again in accordance with the usual terminology, the transverse "plane" is the plane perpendicular to the plane of the drawing in FIG. 2 which is aligned with the axis of the charged-particle beam. Thus the transverse plane is perpendicular to the plane of the drawing of FIG. 2, and lies in the plane of the drawing of FIG. 3. In a representative circularly scanned device such as that shown in FIG. 1, the angle φ is 30°, and if the pole pieces 9, 10 are now adjusted with respect to size and strength of magnetic field so as to produce a radius of curvature R of 100 centimeters, and if one assumes a parallel beam and an exit angle β = φ, the resultant focal length f is approximately 200 centimeters, which is appropriate for a circularly-scanned x-ray device of the type shown in FIG. 1.
In circularly scanned tomography, it is important that the charged particle beam be focused in the azimuthal direction. The azimuthal direction corresponds to the circumferential dimension of the annular target. If the spot on the target is narrow in this direction, the x-rays fan out in the planar slice of the object being "photographed" from a "point" source. The focus of the charged particle beam in the radial or "spot length" direction is not critical, and the spot length can be reduced by altering the target angle so that it is more nearly perpendicular to the axis of the beam. However, under certain circumstances it may be desirable to provide focusing in the radial or "spot length" direction as well as in the azimuthal direction.
Most of the focusing effect is provided by the solenoid or other focusing device, which focuses in both planes. The solenoid or other focusing device may thus provide adequate focusing in the radial direction. However, if additional focusing in the radial direction is desired, the deflector-focuser may be adjusted to provide such focusing by arranging the orientation of the exit effective boundary 12 so that it is not parallel to the entrance effective boundary 11, but at an angle thereto so that β is a little less than φ, as shown in FIG. 2.
The device producing azimuthal focusing should be as close to the target as possible, in order to produce the smallest possible magnification in the azimuthal direction. It is possible that in the radial direction one may not want a true image. This is because space charge effects may be reduced by stretching the image in this plane.
While a device such as that shown in FIGS. 2 and 3 is operable, it involves moving parts which are generally to be avoided. In a preferred embodiment of the invention, such moving parts are avoided by adapting the principles of the induction motor so as to produce a rotating dipole field electrically with stationary coils.
Referring now to FIGS. 4, 5 and 6, the appropriate rotating field may be produced, by analogy to the induction motor, by a pair of windings each of which produces a uniform magnetic field, the two uniform magnetic fields being disposed at right angles to each other. If each of the two coils is excited by a sinusoidal input, and if the sinusoidal inputs are 90° out of phase with each other, a rotating magnetic field is produced. The windings may be identical except that they are arranged so that their configuration is displaced 90° with respect to each other. One of the windings is shown in FIGS. 4 and 5. As shown most clearly in FIG. 5, the turns of the winding therein shown are all directed into the paper in the left half of section A and in the right half of section B, and are directed out of the paper in the remaining portions. The result is to produce a south pole at section A and a north pole at section B so that the field pattern shown in FIG. 4 is produced. The simplest arrangement is of course to have a plurality of loops arranged as shown in FIG. 6. However, more sophisticated arrangements are of course possible in accordance with induction motor techniques and other well-known techniques. It can be shown that for the production of the uniform field the number of turns should vary sinusoidally as shown in FIG. 5.
The focusing effect of the deflector-focuser shown in FIGS. 4, 5 and 6 is quite similar to that of the rotating simple dipole of FIGS. 2 and 3, with β approximately equal to φ. However, there may be some modification of the simple pattern associated with FIGS. 2 and 3. For example, the field lines will bulge at the entrance and exit of the coil. This means that after being deflected through 30°, the effective value of β is somewhat less than φ.
While the foregoing description of the deflector-focuser shown in FIGS. 4, 5 and 6 refers to a two-phase arrangement, it is to be understood that three-phase circuitry (with 60° or 120° displacement as in a three-phase induction motor) and multi-phase arrangements are also comprehended within the scope of my invention.
Having thus described the principles of the invention together with illustrative embodiments thereof, it is to be understood that although specific terms are employed they are used in a generic and descriptive sense and not for purposes of limitation, the scope of the invention being set forth in the following claims.
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Various optical devices for use with circular-scanning techniques in computed transaxial tomography are disclosed. In essence such devices produce a rotating dipole field so as simultaneously to provide a circular scan and to focus the charged particle beam on the circular target.
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CROSS-REFERENCE TO RELATED APPLICATION
This application claims priority to U.S. Provisional Application No. 61/593,083, filed Jan. 31, 2012.
BACKGROUND OF THE INVENTION
This application relates to a gas turbine engine, wherein the size and number of core inlet stator vanes at an upstream end of a compressor section are positioned to minimize icing concerns.
Gas turbine engines are known, and typically include a fan delivering air into a compressor section as core flow, and also to a bypass path. The air entering the compressor section typically passes across inlet stator vanes, and towards a compressor rotor. The air is compressed in the compressor section, delivered into a combustion section, mixed with fuel and ignited. Products of this combustion pass downstream over turbine rotors, driving the rotors to rotate, and in turn drive the compressor and fan sections.
In one traditional type of gas turbine engine, a low pressure turbine drives a low pressure compressor, and a high pressure turbine drives a high pressure compressor. The low pressure turbine typically also drives the fan blade through a low spool. In such engines, the fan blade and low pressure compressor were constrained to rotate at the same speed as the low pressure turbine.
More recently, it has been proposed to incorporate a gear reduction between the low spool and the fan blade such that the fan blade may rotate at a distinct speed relative to the low pressure turbine. Such engines have a gear reduction typically positioned inwardly of a core engine gas flow.
One concern with gas turbine engines when utilized on airplanes is that ice may be passed downstream into the core flow. The ice may accumulate on an outer housing, known as a splitter, which defines an outer periphery of the core flow, and on the stator vanes. When the ice builds up, this is undesirable. The problem becomes particularly acute with a geared turbofan, as the core flow tends to be across a smaller cross-sectional area then in the prior systems.
SUMMARY
In a featured embodiment, a gas turbine engine has a fan, a turbine operatively connected to the fan, an inner core housing having an inner periphery, and a splitter housing having an outer periphery. The inner periphery of the inner core housing and the outer periphery of the splitter housing define a core path. A plurality of inlet stator vanes is located in the core path. The inner periphery of the inner core housing, the outer periphery of the splitter housing and the plurality of inlet stator vanes define a flow area having a hydraulic diameter. The hydraulic diameter of the flow area is greater than or equal to about 1.5 inches.
In another embodiment according to the previous embodiment, the hydraulic diameter is greater than or equal to about 1.7 inches.
In another embodiment according to the previous embodiment, the turbine is a low pressure turbine which also drives a low pressure compressor, and the fan as a low spool.
In another embodiment according to the previous embodiment, the low spool drives the fan through a gear reduction.
In another embodiment according to the previous embodiment, the gear reduction is positioned inwardly of the inner core housing.
In another embodiment according to the previous embodiment, the gear reduction has a gear reduction ratio greater than 2.3.
In another embodiment according to the previous embodiment, the gear reduction has a gear ratio of greater than 2.5.
In another embodiment according to the previous embodiment, the fan also delivers air into a bypass duct.
In another embodiment according to the previous embodiment, a bypass ratio of the amount of air delivered into the bypass duct compared to the amount of air delivered into the core path is greater than about 6.
In another embodiment according to the previous embodiment, the bypass ratio is greater than 10.
In another embodiment according to the previous embodiment, the fan has an outer diameter that is larger than an outer diameter of the rotors in the low pressure compressor.
In another embodiment according to the previous embodiment, the low pressure turbine has a pressure ratio that is greater than about 5:1.
In another featured embodiment, a gas turbine engine has a fan that delivers air into a core path and into a bypass duct as bypass air. The air in the core path reaches a low pressure compressor, and then a high pressure compressor. The air that is compressed by the high pressure compressor is delivered into a combustion section where it is mixed with fuel and ignited. Products of the combustion pass downstream over a high pressure turbine and then a low pressure turbine. The low pressure turbine drives the low pressure compressor as a low spool. A gear reduction is driven by the low spool to in turn drive the fan at a rate of speed lower than that of the low spool. The gear reduction is positioned inwardly of an inner core housing which defines an inner periphery of the core path. A splitter housing defines an outer periphery of the core path. A plurality of inlet stator vanes extend between the splitter and the inner core housing. There is a flow area between adjacent stator vanes, wherein a hydraulic diameter is defined as: Hydraulic diameter=(4×A)/(O+L+I+L), where A is the area between the trailing edge of one vane, the leading edge of an adjacent vane, the inner periphery of the splitter, and the outer periphery of the inner core housing. L is the length of the leading edge of each vane. I is the length of the inner periphery of the vanes and O is the length of the outer periphery between adjacent vanes. The hydraulic diameter is greater than or equal to about 1.5 inches.
In another embodiment according to the previous embodiment, the hydraulic diameter is greater than or equal to about 1.7 inches.
In another embodiment according to the previous embodiment, the gear reduction is positioned inwardly of the inner core housing.
In another embodiment according to the previous embodiment, a bypass ratio of the amount of air delivered into the bypass duct compared to the amount of air delivered into the core path is greater than about 6.
In another embodiment according to the previous embodiment, the bypass ratio is greater than 10.
In another embodiment according to the previous embodiment, the gear reduction has a gear reduction ratio greater than 2.3.
In another embodiment according to the previous embodiment, the low pressure turbine has a pressure ratio that is greater than about 5:1.
In another embodiment according to the previous embodiment, the gear reduction has a gear reduction ratio greater than 2.3.
In another featured embodiment, a compressor module has a compressor rotor, a plurality of inlet stator vanes adjacent the rotor, a flow area defined between leading edges of two adjacent stator vanes, and an outer boundary and an inner boundary. The hydraulic diameter is greater than or equal to about 1.5 inches.
In another embodiment according to the previous embodiment, the hydraulic diameter is greater than or equal to about 1.7 inches.
These and other features may be best understood from the following drawings and specification.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 shows a gas turbine engine somewhat schematically.
FIG. 2 is a cross-sectional view through an upstream end of a gas turbine engine.
FIG. 3 is a forward view of a portion of the FIG. 2 gas turbine engine.
FIG. 4 is a schematic view.
DETAILED DESCRIPTION
FIG. 1 schematically illustrates a gas turbine engine 20 . The gas turbine engine 20 is disclosed herein as a two-spool turbofan that generally incorporates a fan section 22 , a compressor section 24 , a combustor section 26 and a turbine section 28 . Alternative engines might include an augmentor section (not shown) among other systems or features. The fan section 22 drives air along a bypass flow path while the compressor section 24 drives air along a core flow path for compression and communication into the combustor section 26 then expansion through the turbine section 28 . Although depicted as a turbofan gas turbine engine in the disclosed non-limiting embodiment, it should be understood that the concepts described herein are not limited to use with turbofans as the teachings may be applied to other types of turbine engines including three-spool architectures.
The engine 20 generally includes a low speed spool 30 and a high speed spool 32 mounted for rotation about an engine central longitudinal axis A relative to an engine static structure 36 via several bearing systems 38 . It should be understood that various bearing systems 38 at various locations may alternatively or additionally be provided.
The low speed spool 30 generally includes an inner shaft 40 that interconnects a fan 42 , a low pressure compressor 44 and a low pressure turbine 46 . The inner shaft 40 is connected to the fan 42 through a geared architecture 48 to drive the fan 42 at a lower speed than the low speed spool 30 . The high speed spool 32 includes an outer shaft 50 that interconnects a high pressure compressor 52 and high pressure turbine 54 . A combustor 56 is arranged between the high pressure compressor 52 and the high pressure turbine 54 . A mid-turbine frame 57 of the engine static structure 36 is arranged generally between the high pressure turbine 54 and the low pressure turbine 46 . The mid-turbine frame 57 further supports bearing systems 38 in the turbine section 28 . The inner shaft 40 and the outer shaft 50 are concentric and rotate via bearing systems 38 about the engine central longitudinal axis A which is collinear with their longitudinal axes.
The core airflow is compressed by the low pressure compressor 44 then the high pressure compressor 52 , mixed and burned with fuel in the combustor 56 , then expanded over the high pressure turbine 54 and low pressure turbine 46 . The mid-turbine frame 57 includes airfoils 59 which are in the core airflow path. The turbines 46 , 54 rotationally drive the respective low speed spool 30 and high speed spool 32 in response to the expansion.
The engine 20 in one example is a high-bypass geared aircraft engine. In a further example, the engine 20 bypass ratio is greater than about six (6), with an example embodiment being greater than ten (10), the geared architecture 48 is an epicyclic gear train, such as a planetary gear system or other gear system, with a gear reduction ratio of greater than about 2.3 and the low pressure turbine 46 has a pressure ratio that is greater than about 5. In one disclosed embodiment, the engine 20 bypass ratio is greater than about ten (10:1), the fan diameter is significantly larger than that of the low pressure compressor 44 , and the low pressure turbine 46 has a pressure ratio that is greater than about 5:1. Low pressure turbine 46 pressure ratio is pressure measured prior to inlet of low pressure turbine 46 as related to the pressure at the outlet of the low pressure turbine 46 prior to an exhaust nozzle. The geared architecture 48 may be an epicycle gear train, such as a planetary gear system or other gear system, with a gear reduction ratio of greater than about 2.5:1. It should be understood, however, that the above parameters are only exemplary of one embodiment of a geared architecture engine and that the present invention is applicable to other gas turbine engines including direct drive turbofans.
A significant amount of thrust is provided by the bypass flow B due to the high bypass ratio. The fan section 22 of the engine 20 is designed for a particular flight condition—typically cruise at about 0.8 Mach and about 35,000 feet. The flight condition of 0.8 Mach and 35,000 ft, with the engine at its best fuel consumption—also known as “bucket cruise Thrust Specific Fuel Consumption (‘TSFC’)”—is the industry standard parameter of lbm of fuel being burned divided by lbf of thrust the engine produces at that minimum point. “Low fan pressure ratio” is the pressure ratio across the fan blade alone, without a Fan Exit Guide Vane (“FEGV”) system. The low fan pressure ratio as disclosed herein according to one non-limiting embodiment is less than about 1.45. “Low corrected fan tip speed” is the actual fan tip speed in ft/sec divided by an industry standard temperature correction of [(Tambient deg R)/518.7)^0.5]. The “Low corrected fan tip speed” as disclosed herein according to one non-limiting embodiment is less than about 1150 ft/second.
FIG. 2 shows a portion of the gas turbine engine 20 . In particular, an outer housing, known as a splitter 80 defines an outer periphery for the core flow path C. A row of stator vanes 82 is positioned at a forward end. Air from the fan blade is divided into the bypass flow path B, and into the core flow path C, as mentioned above. The gear reduction 48 is positioned inwardly of an inner housing 83 .
As shown in FIGS. 3 and 4 , the spacing and number of stator vanes 82 is selected such that the total flow area A between the vanes 82 is selected to reduce the likelihood of icing. As shown, a pair of spaced vanes 82 are circumferentially spaced by area A. The area A is defined by a leading edge L of one vane 82 , a leading edge L of an adjacent vane 82 , the inner periphery O of the splitter 80 , and the outer periphery I of the inner housing 83 . A perimeter is defined by the sum of L, O, L and I. The hydraulic diameter may be defined as 4 times the area A divided by the perimeter. This would be equation 1 as follows:
Hydraulic diameter=(4× A )/( O+L+I+L ) Equation 1
The hydraulic diameter is desirably greater than or equal to about 1.5 in (3.8 cm). In preferred embodiments, it would be greater than or equal to about 1.7 in (4.3 cm).
The hydraulic diameter can be calculated for a compressor module in a similar manner by measuring the leading edges and measuring the distances along the outer and inner boundaries of the flow area, even though the module is not mounted in a splitter or outward of an inner housing.
Of course, FIG. 3 shows a small circumferential segment, and it should be understood that the spacing would typically be equal across the entire circumference.
Although an embodiment of this invention has been disclosed, a worker of ordinary skill in this art would recognize that certain modifications would come within the scope of this invention. For that reason, the following claims should be studied to determine the true scope and content of this invention.
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A gas turbine engine is defined wherein the inlet guide vanes leading into a core engine flow path are sized and positioned such that flow paths positioned circumferentially intermediate the vane are sufficiently large that a hydraulic diameter of greater than or equal to about 1.5 is achieved. This will likely reduce the detrimental effect of icing.
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BACKGROUND
[0001] Pay-as-you-go business models have been used in many areas of commerce, from cellular telephones to commercial laundromats. In developing a pay-as-you go business, a provider, for example, a cellular telephone provider, offers the use of hardware (a cellular telephone) at a lower-than-market cost in exchange for a commitment to remain a subscriber to their network for a period of time. In this specific example, the customer receives a cellular phone for little or no money in exchange for signing a contract to become a subscriber for a given period of time. Over the course of the contract, the service provider recovers the cost of the hardware by charging the consumer for using the cellular phone. In addition to implementing the pay-as-you-go business model via subscriptions, another implementation of the pay-as-you-go business model allows the customer to pre-pay for a block of service units, i.e., “pay-per-use.” Using the cellular phone example, the customer may pre-pay for a block of 300 minutes. At the end of the 300 minutes, the customer may purchase additional blocks of service time or may return the phone to the service provider. The service provider may then contract out the phone to a different user.
[0002] The pay-as-you-go business model may incorporate a model of perpetual ownership. As part of a user agreement or contract, a service provider may allow the customer to take full unfettered ownership of the device after certain contractual conditions have been met. For example, the customer may take perpetual ownership of the device after a subscription period of so many years, or after having purchased so many blocks of service units. At the time of perpetual ownership, the service provider may turn off or disable pay-as-you-go features in the device and the customer may take possession of the device in a non-pay-as-you-go configuration.
[0003] The pay-as-you-go business model is predicated on the concept that the hardware provided has little or no value, or use, if disconnected from the service provider. To illustrate, should the subscriber mentioned above cease to pay his or her bill or the pay-per-use customer does not purchase additional blocks of time, the service provider deactivates the account, and while the cellular telephone may power up, calls cannot be made because the service provider will not allow them. The deactivated phone has no “salvage” value, because the phone will not work elsewhere and the component parts are not easily salvaged nor do they have a significant street value. In most cases, however, even though the phone has been deactivated it is still capable of connecting to the service provider in order to arrange restoration of the account. When the account is brought current, the service provider will re-authorize the device on its network and allow calling.
[0004] This model works well when the service provider, or other entity taking the financial risk of providing subsidized hardware, is able to enforce the terms of the contract as above. Because an electronic device, such as a computer, may have useful functions even when not connected to a network or server, a pay-as-you-go device may be responsible to self-administer contract enforcement. When the electronic device is responsible for self administration, a clock circuit may become a prime target for tampering because many business models are time based. For example, a subscription good for one calendar month may never expire if the clock is tampered with to keep the time within the valid month.
[0005] The communication between entities in the pay-as-you-go system requires a unified schema to support the various forms of packets. The schema needs to be elegant and robust to support provisioning, metering, and other types of configuration messages as well as to provide a foundation for any future messages needed for product evolution. The schema also needs to have security at multiple levels to guard against malicious users who may try to hook into the system to fraudulently use and/or configure the electronic devices for their own use and gain.
SUMMARY
[0006] This Summary is provided to introduce a selection of concepts in a simplified form that are further described below in the Detailed Description. This Summary is not intended to identify key features or essential features of the claimed subject matter, nor is it intended to be used to limit the scope of the claimed subject matter.
[0007] A system supporting pay-as-you-go electronic devices requires that all communication from the electronic devices include the current time at the electronic device initiating the communication. The communication may be a request to add value to a timed usage or subscription account. If the current time at the electronic device is not within an allowable limit, a response message may include an updated time. The original request may be deferred or denied until the electronic device communicates a message with an acceptable current time. If repeated communications from the electronic device contain invalid current times, the electronic device in question may be blocked from being sent further responses until an appropriate service action may be taken to determine if tampering or a hardware failure have occurred.
[0008] If the current time at the electronic device is within the allowable limit, processing may proceed normally. To discourage fraudulent messages, application-level security may be applied to communications by encrypting and signing messages between a secure module in the electronic device and a trusted server. The trusted server may also communicate other information to the electronic device, such as how to configure to enforce terms of a service contract, any changes to contract terms, if the end-user has fulfilled the ownership requirements and has unfettered use of the electronic device, if the end-user has returned the electronic device back to the service provider and the device is not associated with any end-user, and other such provisioning information. Additionally, the service provider may also communicate with the electronic device locally to (re)configure the pay-as-you-go configuration (e.g., after end-user A has ended his/her contract and turned in the device and before it is contracted out to end-user B) or to disable pay-as-you-go altogether (e.g., if the service provider wishes to sell the electronic device in a non-pay-as-you-go mode).
[0009] Methods and a program of instruction for communicating between elements in a pay-as-you-go system may utilize a provisioning packet schema. This packet schema may be used for defining the communication from a provisioning server to an electronic device adapted for use in a pay-as-you-go system by the addition of a local provisioning system, from the electronic device to the provisioning server, or from a local service provider to the electronic device. The packet schema may take the form of a four-level schema, and may comport with XML, TLV, other such languages or combinations thereof.
[0010] The first level of the four level schema may contain the actual packet content data to be consumed by an entity in the pay-as-you-go system and additional administrative information such as but not limited to: pre-paid card/subscription, sender, sequence and tracking identifiers; creation date; conversation thread sequence numbers; and the like. The packet content data may consist of a provisioning instruction with a specific content type and any other additional data needed to process that specific content type. Examples of content types may include information from the provisioning server to the electronic device adapted for use in a pay-as-you-go environment such as an indication of the contract type and length (whether pre-paid or subscription), an indication that the end-user has fulfilled the contract obligations and fully owns the electronic device, an indication that the end-user has returned the electronic device to the service provider and provisioning needs to be suspended until the next end-user, and a desired configuration of metering and other electronic device behavior to enforce contract terms. Other content types and their associated fields are also possible.
[0011] For communication generated at an electronic device adapted for use in a pay-as-you-go environment, the packet schema may define a request content type that may contain information on the metering state, last sequence number, platform and software version indicators, pay-as-you-go contract balance, debugging code fields and state information. The packet schema may also define the packet content data received and interpreted by the electronic device. These content types may include all of the aforementioned provisioning instruction content types able to be generated by the provisioning server, as well as provisioning instructions able to be generated locally by the service provider, including but not limited to an indication to disable local service provisioning and an indication of the desired pay-as-you-go configuration.
[0012] The second level of the four level schema may contain the packet content of the first level, a version identifier of the schema, and a signature which may be RSA or may be another public-key encryption algorithm. The security at the second level may ensure that the packet content data is signed by the required source.
[0013] The third level of the four level schema may contain the encrypted data of the first and the second layers to prevent the communicated packet data from being exposed. Additional security may be provided by including the sender's identifier and the session identifier for use as keys to decrypt the data.
[0014] The fourth level of the four level schema may contain the data of the first three levels, the version of the schema, and a hash to prevent tampering. The hash may use a MAC (message authentication code) for the first, second, and third layers, or it may use another cryptographic hashing mechanism to authenticate the message.
DRAWINGS
[0015] FIG. 1 is a block diagram of a computing system that may operate in accordance with the claims;
[0016] FIG. 2 is a simplified and exemplary block diagram of a system supporting a pay-as-you-go business model;
[0017] FIG. 3 illustrates a packet-defining schema that may be used for communicating from a provisioning system to an electronic device adapted for use in a pay-as-you-go system;
[0018] FIG. 4 illustrates details of other layers in the packet schema shown in FIG. 3 ;
[0019] FIG. 4 a describes a method for communicating between a provisioning server system and an electronic device in a pay-as-you-go system;
[0020] FIG. 5 illustrates a packet-defining schema that may be generated by an electronic device adapted for use in a pay-as-you-go system;
[0021] FIG. 6 illustrates a packet-defining schema that may be received at an electronic device adapted for use in a pay-as-you-go system, and
[0022] FIG. 7 shows a method for receiving a provisioning packet in a pay-as-you-go system.
DESCRIPTION
[0023] Although the following text sets forth a detailed description of numerous different embodiments, it should be understood that the legal scope of the description is defined by the words of the claims set forth at the end of this patent. The detailed description is to be construed as exemplary only and does not describe every possible embodiment since describing every possible embodiment would be impractical, if not impossible. Numerous alternative embodiments could be implemented, using either current technology or technology developed after the filing date of this patent, which would still fall within the scope of the claims.
[0024] It should also be understood that, unless a term is expressly defined in this patent using the sentence “As used herein, the term ‘______’ is hereby defined to mean . . . ” or a similar sentence, there is no intent to limit the meaning of that term, either expressly or by implication, beyond its plain or ordinary meaning, and such term should not be interpreted to be limited in scope based on any statement made in any section of this patent (other than the language of the claims). To the extent that any term recited in the claims at the end of this patent is referred to in this patent in a manner consistent with a single meaning, that is done for sake of clarity only so as to not confuse the reader, and it is not intended that such claim term by limited, by implication or otherwise, to that single meaning. Finally, unless a claim element is defined by reciting the word “means” and a function without the recital of any structure, it is not intended that the scope of any claim element be interpreted based on the application of 35 U.S.C. §112, sixth paragraph.
[0025] Much of the inventive functionality and many of the inventive principles are best implemented with or in software programs or instructions and integrated circuits (ICs) such as application specific ICs. It is expected that one of ordinary skill, notwithstanding possibly significant effort and many design choices motivated by, for example, available time, current technology, and economic considerations, when guided by the concepts and principles disclosed herein will be readily capable of generating such software instructions and programs and ICs with minimal experimentation. Therefore, in the interest of brevity and minimization of any risk of obscuring the principles and concepts in accordance to the present invention, further discussion of such software and ICs, if any, will be limited to the essentials with respect to the principles and concepts of the preferred embodiments.
[0026] Many prior-art high-value computers, personal digital assistants, organizers, and the like, are not suitable for use in a pre-pay or pay-for-use business model as is. The device must be adapted to support the business model by having the ability to meter time, enforce contract conditions, communicate with a provisioning system, and other such behaviors. In the pay-as-you-go business model, a service provider owns the adapted physical device (computer, PDA, organizer, etc.) and enters into a contract or service agreement for device usage with an end-user. The service agreement may be a subscription with a fee to be paid at a regular interval, it may be a pre-paid card or account with a fixed amount of usage time that may be replenished by the end-user, or it may be some other similar pay-as-you-go arrangement. When certain terms of the service agreement have been fulfilled by the end-user (e.g., paid subscription over a pre-defined length of time or paid for a pre-defined number of minutes), the service provider may transfer full ownership of the device to the end-user and the device would enter a perpetual non-metered state for unfettered use.
[0027] The ability to enforce a contract requires a service provider, or other enforcement entity, to be able to affect a device's operation even though the device may not be connected to the service provider, e.g. connected to the Internet. A first stage of enforcement may include a simple pop up warning, indicating the terms of the contract are nearing a critical point. A second stage of enforcement, for example, after pay-per-use minutes have expired or a subscription period has lapsed, may be to present a system modal user interface for adding value and restoring service. A provider's ultimate leverage for enforcing the terms of a subscription or pay-per-use agreement is to disable the device. Such a dramatic step may be appropriate when it appears that the user has made a deliberate attempt to subvert the metering or other security systems active in the device.
[0028] Uses for the ability to place an electronic device into a limited function or hardware locked mode may extend beyond subscription and pay-per-use applications. For example, techniques for capacity consumption could be used for licensing enforcement of an operating system or individual applications.
[0029] FIG. 1 illustrates a logical view of a computing device in the form of a computer 110 that may be used in a pay-per-use or subscription mode. For the sake of illustration, the computer 110 is used to illustrate the principles of the instant disclosure. However, such principles apply equally to other electronic devices, including, but not limited to, cellular telephones, personal digital assistants, media players, appliances, gaming systems, entertainment systems, set top boxes, and automotive dashboard electronics, to name a few. Components of the computer 110 may include, but are not limited to a processing unit 120 , a system memory 130 , and a system bus 121 that couples various system components including the system memory to the processing unit 120 . The system bus 121 may be any of several types of bus structures including a memory bus or memory controller, a peripheral bus, and a local bus using any of a variety of bus architectures. By way of example, and not limitation, such architectures include Industry Standard Architecture (ISA) bus, Micro Channel Architecture (MCA) bus, Enhanced ISA (EISA) bus, Video Electronics Standards Association (VESA) local bus, and Peripheral Component Interconnect (PCI) bus, front side bus, and Hypertransport™ bus, a variable width bus using a packet data protocol.
[0030] The computer 110 may include a security module 125 . The security module 125 may be enabled to perform security monitoring, pay-per-use and subscription usage management, and policy enforcement related to terms and conditions associated with paid use, particularly in a subsidized purchase business model. The security module 125 may be embodied in the processing unit 120 , as a standalone component, or in a hybrid, such as a multi-chip module. A clock 126 may be incorporated into the security module 125 to help ensure tamper resistance. To allow user management of local time setting, including daylight savings or movement between time zones, the clock 126 may maintain its time in a coordinated universal time (UTC) format and user time calculated using a user-settable offset. The security module 125 may also include a cryptographic function (not depicted).
[0031] Computer 110 typically includes a variety of computer readable media. Computer readable media can be any available media that can be accessed by computer 110 and includes both volatile and nonvolatile media, removable and non-removable media. By way of example, and not limitation, computer readable media may comprise computer storage media and communication media. Computer storage media includes volatile and nonvolatile, removable and non-removable media implemented in any method or technology for storage of information such as computer readable instructions, data structures, program modules or other data. Computer storage media includes, but is not limited to, RAM, ROM, EEPROM, flash memory or other memory technology, CD-ROM, digital versatile disks (DVD) or other optical disk storage, magnetic cassettes, magnetic tape, magnetic disk storage or other magnetic storage devices, or any other medium which can be used to store the desired information and which can accessed by computer 110 .
[0032] The system memory 130 includes computer storage media in the form of volatile and/or nonvolatile memory such as read only memory (ROM) 131 and random access memory (RAM) 132 . A basic input/output system 133 (BIOS), containing the basic routines that help to transfer information between elements within computer 110 , such as during start-up, is typically stored in ROM 131 . RAM 132 typically contains data and/or program modules that are immediately accessible to and/or presently being operated on by processing unit 120 . By way of example, and not limitation, FIG. 1 illustrates operating system 134 , application programs 135 , other program modules 136 , and program data 137 .
[0033] The computer 110 may also include other removable/non-removable, volatile/nonvolatile computer storage media. By way of example only, FIG. 1 illustrates a hard disk drive 140 that reads from or writes to non-removable, nonvolatile magnetic media, a magnetic disk drive 151 that reads from or writes to a removable, nonvolatile magnetic disk 152 , and an optical disk drive 155 that reads from or writes to a removable, nonvolatile optical disk 156 such as a CD ROM or other optical media. Other removable/non-removable, volatile/nonvolatile computer storage media that can be used in the exemplary operating environment include, but are not limited to, magnetic tape cassettes, flash memory cards, digital versatile disks, digital video tape, solid state RAM, solid state ROM, and the like. The hard disk drive 141 is typically connected to the system bus 121 through a non-removable memory interface such as interface 140 , and magnetic disk drive 151 and optical disk drive 155 are typically connected to the system bus 121 by a removable memory interface, such as interface 150 .
[0034] The drives and their associated computer storage media discussed above and illustrated in FIG. 1 , provide storage of computer readable instructions, data structures, program modules and other data for the computer 110 . In FIG. 1 , for example, hard disk drive 141 is illustrated as storing operating system 144 , application programs 145 , other program modules 146 , and program data 147 . Note that these components can either be the same as or different from operating system 134 , application programs 135 , other program modules 136 , and program data 137 . Operating system 144 , application programs 145 , other program modules 146 , and program data 147 are given different numbers here to illustrate that, at a minimum, they are different copies. A user may enter commands and information into the computer 20 through input devices such as a keyboard 162 and pointing device 161 , commonly referred to as a mouse, trackball or touch pad. Other input devices (not shown) may include a microphone, joystick, game pad, satellite dish, scanner, digital camera, or the like. These and other input devices are often connected to the processing unit 120 through a user input interface 160 that is coupled to the system bus, but may be connected by other interface and bus structures, such as a parallel port, game port or a universal serial bus (USB). A monitor 191 or other type of display device is also connected to the system bus 121 via an interface, such as a video interface 190 .
[0035] The computer 110 may operate in a networked environment using logical connections to one or more remote computers (not depicted) over a network interface 170 , such as broadband Ethernet connection or other known network.
[0036] FIG. 2 is a simplified and exemplary block diagram of a system 200 supporting pay-as-you-go usage of a computer or other electronic device. A provisioning server 202 may serve as a trusted endpoint for provisioning requests from one or more electronic devices participating in the pay-as-you-go business ecosystem, and may be similar to the computer of FIG. 1 . The provisioning server 202 may include the secure clock 126 of FIG. 1 adapted to support pay-as-you-go metering purposes. An electronic device 204 may be similar to the computer 110 of FIG. 1 . The electronic device 204 may be configured for use in a pay-as-you-go system by including a local provisioning system 212 for metering time, enabling/disabling pay-as-you-go functionality, and communicating with the provisioning server 202 . A secure clock 126 of computer 110 may reside in the local provisioning system 212 to assist with time metering. Other electronic devices 206 may perform substantially the same as the exemplary device 204 . Communication between the provisioning server 202 and the electronic device 204 may be accomplished through a network 208 that may include landline, wireless, or broadband networks, or other networks known in the art.
[0037] An accounting server 210 may be linked to the provisioning server 202 and may maintain account data corresponding to the electronic device 204 . The accounting server 210 may also serve as a clearinghouse for financial transactions related to the electronic device 204 , such as replenishing or adding value to a pay-as-you-go account maintained on the electronic device 204 . For example, an end-user may transfer funds to an account maintained on the accounting server 210 for use in an add-value or subscription transaction. The accounting server 210 itself may have a link to a scratch card system (not depicted) allowing the end-user to purchase a card at retail and use a hidden number to replenish his or her account. Other prepaid account funds transfer systems are well known, for example, with respect to prepaid cellular phones, and are equally applicable in this business model.
[0038] The architecture and functionality of the provisioning server 202 are discussed in detail in U.S. patent application Ser. No. 11/668,439. To paraphrase here for the reader's context, the provisioning server 202 may accept an authentication packet, or request, from an electronic device 204 206 adapted for use in a pay-as-you-go system and may determine whether to process the request or reply with related information or instructions. Operations of the electronic devices 204 206 adapted for use in a pay-as-you-go system are also discussed in more detail in U.S. patent application Ser. No. 11/668,439. Briefly, the metered-use electronic devices 204 206 may receive a packet from a provisioning server 202 through a network 208 that may include landline, wireless, or broadband networks, or other networks known in the art. The electronic devices 204 206 may also receive a packet/message from a local on-site service provider 214 via a USB, Ethernet, or other such connection known in the art. The electronic devices 204 206 may determine how and if to process the message, including potentially replying with a response. The packing and unpacking of packets/messages and related subsequent processing, actions, and responses are disclosed by U.S. patent app. Ser. No. 11/668,439.
[0039] FIG. 3 illustrates an embodiment of a schema defining a provisioning packet 300 that may be used for communicating from a provisioning system 202 to an electronic device adapted for use in a pay-as-you-go system 204 206 . The schema 300 may comport with a four-layer schema 302 305 308 310 which may be of the form XML (Extensible Mark-Up Language), TLV (Type-Length-Value), other languages commonly known in the art, or combinations thereof. The first layer 310 of the schema may contain one or more fields such as: the hardware identification (HWID) of the sender 320 which may be identification of the provisioning system 202 or may be identification of the electronic device 204 206 , the creation date 322 of the packet, a sequence number 324 to keep track of the conversation between entities, a tracking identification 326 that may be implemented as a GUID (Globally Unique Identifier) or may be implemented with a different tracking identification mechanism, a transaction identification 328 that may contain an identifier of a pre-paid card purchased by the end-user or may contain a subscription identifier, an identification of the service provider for the electronic device 204 206 which may take the form of a universal product identifier (UPID) 330 or may take a different form, and a provisioning instruction 332 . Of course, other additional fields may also be used to support communication between the provisioning server 202 and the electronic device 204 206 .
[0040] The provisioning instruction 332 may have a content type 340 . This content type 340 may be one of many different types with unique meanings. FIG. 3 illustrates the various content types that may be defined by the schema for provisioning packet 300 , however, as stated above, the operations of the provisioning system 202 and the electronic device 204 206 with relation to the content types are disclosed by U.S. patent application Ser. No. 11/668,439. A pre-paid content type 350 may indicate the total time purchased 352 by the end-user using a scratch-off card, access code, or other such means. A subscription content type 354 may indicate that an end-user has paid for an interval of subscription time (which may be daily, monthly, etc.) and may further indicate the subscription end date 356 . A refurbish content type 358 may indicate that a pay-as-you-go electronic device 204 206 has been returned to the service provider by an end-user and is temporarily in a dormant/inactive mode. A perpetual content type 360 may indicate that an end-user has fulfilled the criteria for ownership and has unlimited use of the pay-as-you-go electronic device 204 206 .
[0041] A provisioning instruction 332 with a configuration content type 362 may indicate a desired configuration of the pay-as-you-go electronic device 204 206 . The fields defining the desired configuration may include one or more of the following: an enforcement level 364 that may inform the local provisioning system 212 of desired action(s) (e.g., reboot, add grace time, etc.) to take when pay-as-you-go conditions expire, a maximum reserve tank time 366 to indicate a borrowed amount of time from a future pre-paid card or subscription purchase to use to when an end-user's pay-as-you-go conditions expire, an indication of time to perpetual ownership 368 , and a session identification timeout value 372 to inform the local provisioning system 212 how to adjust a timeout value for a session. Other fields may also be included with configuration content type 362 to support configuring of the pay-as-you-go electronic device 204 206 .
[0042] Of course, the range of content types 340 in the provisioning instruction 332 is not limited to the content types listed here, but may include other types to support necessary communication between a provisioning server 202 and an electronic device adapted for use in a pay-as-you-go system 204 206 .
[0043] FIG. 4 illustrates the details of other levels of the schema defining the provisioning packet 300 . The second layer 308 may contain the content of the first layer 410 , an indicator of the schema version 415 , and a signature of the first layer 420 to ensure the data is being signed by the required source. The signature 420 may be an RSA algorithm or it may be another public key encryption algorithm. The third layer 305 may contain an encryption of the first and second layers 420 , a session identification 425 , and a hardware identification (HWID) 435 of the sender. The fourth layer 302 may contain the third layer data 435 , an indicator of the schema version 440 , and a cryptographic hash function for the other three layers to prevent tampering. This cryptographic hash function may be a message authentication code (MAC) 445 or it may be another cryptographic hash algorithm commonly known in the art. Other embodiments of the packet schema are also possible.
[0044] FIG. 4 a illustrates an embodiment of a method 450 for communicating between a provisioning server system 202 and an electronic device 206 that may comport with a four-level schema. At the start 453 , a provisioning instruction is generated 457 which may contain a content type 340 and associated fields. The range of the content type 340 and associated fields may be a content type and fields as described by FIG. 3 and FIG. 5 . Next, a first layer of a four-layer schema may be generated 460 that may contain the provisioning instruction and associated fields. A second layer may be generated 463 that may include the content of the first layer, a version indicator of the schema, and an RSA signature. A third layer may be generated 467 that may consist of an encryption of the first and second layers, a session identification value, and a hardware identification of the sender. The fourth layer may be generated 470 that may contain the third layer data, an indicator of the schema version, and a cryptographic hash function of the other three layers. Lastly, the provisioning packet may be transmitted 473 , and the method may end 477 . Of course, other embodiments of method 450 may be possible.
[0045] FIG. 5 shows an embodiment of a schema defining a provisioning packet 500 generated by an electronic device adapted for use in a pay-as-you-go system 204 206 . The schema 500 may comport with a four-layer schema 502 505 508 510 which may be of the form XML (Extensible Mark-Up Language), TLV (Type-Length-Value), other languages commonly known in the art, or combinations thereof. The first layer 510 of the packet 500 may contain a provisioning instruction 512 and may also contain other fields (e.g., HWID, tracking ID, etc.) similar to those of packet 300 . The provisioning instruction 510 may be of a request content type 515 , and may additionally contain one or more of the following fields: a metering state 518 to signify the state of metering of the local provisioning system 212 , a last sequence number 520 to keep track of the conversation between entities, a hardware lock mode counter 523 to indicate how many times the electronic device 204 206 has entered limited function or hardware locked mode, a platform indicator 526 to signify whether the local provisioning system 212 hardware or local provisioning system 212 software initiated the request content type 515 packet, a balance of time 530 if the pay-as-you-go conditions are implemented with a pre-paid account, the end date of the subscription 533 if the pay-as-you-go conditions are implemented with a subscription account, a software version indicator 536 for the local provisioning system 212 , a debugging code field 540 , and a set of state flags 543 . As stated above, these summary of field definitions are to provide context; the operations of the provisioning system 202 and the electronic device 204 206 with relation to the fields defined by schema 500 are disclosed by U.S. patent application Ser. No. 11/668,439. Of course, other content types and other fields may also be defined by this schema 500 as needed to support packet/message communication generated by an electronic device adapted to operate in a pay-as-you-go environment.
[0046] FIG. 6 illustrates an embodiment of a provisioning packet schema 600 used by an electronic device adapted for use in a pay-as-you-go system 204 206 to interpret packets that it receives. The provisioning packet 600 may comport with a four-layer schema 602 605 608 610 which may take the form of XML (Extensible Mark-Up Language), TLV (Type-Length-Value), other languages commonly known in the art, or combinations thereof. The first layer 610 of the packet 600 may contain a provisioning instruction 612 and may also contain other fields (e.g., HWID, tracking ID, etc.) similar to those fields defined in packet 300 of FIG. 3 . The provisioning instruction 612 may have a content type 614 . This content type 614 may be one of many different types with unique meanings. FIG. 6 illustrates the various content types that may be defined by the schema for provisioning packet 600 , however, as stated above, the operations of the provisioning system 202 and the electronic device 204 206 with relation to the content types are disclosed by U.S. patent application Ser. No. 11/668,439. A provisioning instruction 612 with a disable local provisioning content type 620 may be an indication to disable the local provisioning system 212 at the electronic device 204 206 , for instance, when the service provider wishes to sell the electronic device 204 206 in a non-pay-as-you-go mode.
[0047] A pre-paid content type 623 may indicate that an end-user has purchased a set amount of time using a scratch-off card, access code, or other such means. A subscription content type 626 may indicate that an end-user has paid for an interval of subscription time (which may be daily, monthly, etc.) and may further indicate the expiration date of the subscription. A refurbish content type 630 may indicate that a pay-as-you-go electronic device 204 206 has been returned to the service provider by an end-user and is temporarily in a dormant/inactive mode. A perpetual content type 633 may indicate that an end-user has fulfilled the criteria for ownership and has unlimited use of the pay-as-you-go electronic device 204 206 .
[0048] A provisioning instruction 612 with a configuration content type 637 may be interpreted as communicating a desired configuration of the pay-as-you-go electronic device 204 206 . With the configuration content type 637 , additional fields used to specify the desired configuration may be similar to those defined in packet 300 of FIG. 3 , and may include one or more of the following: an enforcement level that may inform the local provisioning system 212 of desired action(s) (e.g., reboot, add grace time, etc.) to take when pay-as-you-go conditions expire, a maximum reserve tank time to indicate a borrowed amount of time from a future pre-paid card or future subscription extension to use to when an end-user's pay-as-you-go conditions expire, an indication of time to perpetual ownership, and a session identification timeout value to inform the local provisioning system how to adjust a timeout value for a session. Of course, other additional fields may also be used as needed.
[0049] A provisioning instruction 612 with an OEM configuration content type 638 may indicate a desired configuration of the electronic device adapted for a pay-as-you-go system 204 206 . The fields defining the desired configuration may include one or more of the following: an initial balance of time 640 , an enforcement level 643 that may inform the local provisioning system 212 of desired action(s) (e.g., reboot, add grace time, etc.) to take when pay-as-you-go conditions expire, a maximum reserve tank time 646 to indicate a borrowed amount of time from a future pre-paid card or subscription purchase to use to when an end-user's pay-as-you-go conditions expire, a service provider identification 650 , a hardware lock mode image 653 , and a session identification timeout value 656 .
[0050] FIG. 7 illustrates an embodiment of a method 700 for receiving a provisioning packet 707 that may comport with a four-level schema. At the start 703 , the fourth layer may be interpreted 710 as having the third layer data, a schema version indicator, and a message authentication code for the other three layers. If the MAC is validated successfully 712 , the third layer may be interpreted 713 . The third layer may contain an encryption of the first and second layers to be decrypted, a session identification value, and a hardware identification of the sender. The second layer may then be interpreted 717 that may include the content of the first layer, a version indicator of the schema, and an RSA signature. If the RSA signature is validated successfully 718 , the first layer may be interpreted 720 . The first layer may include a provisioning instruction and associated fields. A content type and associated fields may be obtained from the provisioning instruction 723 , where the content type may be one of the types illustrated by FIGS. 5 and 6 . When the provisioning packet has been interpreted in its entirety, the method 700 may end 727 . Of course, other embodiments of method 700 may be possible.
[0051] An exemplary implementation of the packet schema may be represented by the following:
[0000]
<?xml version=“1.0” encoding=“utf-8” ?>
<xs:schema xmlns:xs=“http://www.w3.org/2001/XMLSchema” elementFormDefault=“qualified”
attributeFormDefault=“qualified”>
Layer 1 : Payasyougo Packet Content
<xs:complexType name=“PrepaidContentType”>
<xs:sequence>
<xs:element name=“Minutes” type=“xs:int” minOccurs=“1” maxOccurs=“1” />
<xs:element name=“TotalMinutesBought” type=“xs:int” minOccurs=“1” maxOccurs=“1” />
</xs:sequence>
</xs:complexType>
<xs:complexType name=“SubscriptionContentType”>
<xs:sequence>
<xs:element name=“EndDate” type=“xs:dateTime” minOccurs=“1” maxOccurs=“1” />
</xs:sequence>
</xs:complexType>
<xs:complexType name=“TimeSyncContentType”>
<xs:sequence>
<xs:element name=“UTCTime” type=“xs:dateTime” minOccurs=“1”maxOccurs=“1” />
</xs:sequence>
</xs:complexType>
<xs:complexType name=“RefurbishContentType”>
<xs:sequence>
<xs:element name=“Refurbish” type=“xs:string” minOccurs=“1” maxOccurs=“1” />
</xs:sequence>
</xs:complexType>
<xs:complexType name=“PerpetualContentType”>
<xs:sequence>
<xs:element name=“Perpetual” type=“xs:string” minOccurs=“1” maxOccurs=“1” />
</xs:sequence>
</xs:complexType>
<xs:complexType name=“ConfigurationContentType”>
<xs:sequence>
<xs:element name=“EnforcementLevel” type=“xs:int” minOccurs=“1” maxOccurs=“1” />
<xs:element name=“MaxReserveTankTimeInMinutes” type=“xs:int” minOccurs=“1” maxOccurs=“1”
/>
<xs:element name=“SessionIDTimeoutInSeconds” type=“xs:int” minOccurs=“1” maxOccurs=“1” />
<xs:element name=“MaxAllowedBitmapUpdates” type=“xs:int” minOccurs=“1” maxOccurs=“1”
/>
<xs:element name=“TotalHoursToPerpetual” type=“xs:int” minOccurs=“1” maxOccurs=“1” />
</xs:sequence>
</xs:complexType>
<xs:complexType name=“OEMConfigurationContentType”>
<xs:sequence>
<xs:element name=“EnforcementLevel” type=“xs:int” minOccurs=“1” maxOccurs=“1” />
<xs:element name=“MaxReserveTankTimeInMinutes” type=“xs:int” minOccurs=“1”
maxOccurs=“1” />
<xs:element name=“MaxAllowedBitmapUpdates” type=“xs:int” minOccurs=“1” maxOccurs=“1”
/>
<xs:element name=“SessionIDTimeoutInSeconds” type=“xs:int” minOccurs=“1” maxOccurs=“1”
/>
<xs:element name=“InitialBalanceInMinutes” type=“xs:int” minOccurs=“1” maxOccurs=“1” />
<xs:element name=“UPID” type=“xs:string” minOccurs=“1” maxOccurs=“1” />
<xs:element name=“HLMImage” type=“xs:hexBinary” minOccurs=“0” maxOccurs=“1” />
</xs:sequence>
</xs:complexType>
<xs:complexType name=“PacketDownloadContentType”>
<xs:sequence>
<xs:element name=“PacketDownloadComplete” type=“xs:int” minOccurs=“1” maxOccurs=“1” />
</xs:sequence>
</xs:complexType>
<xs:complexType name=“DisableLPMContentType”>
<xs:sequence>
<xs:element name=“DisableLPM” type=“xs:string” minOccurs=“1” maxOccurs=“1” />
</xs:sequence>
</xs:complexType>
<xs:complexType name=“RequestContentType”>
<xs:sequence>
<xs:element name=“State” type=“xs:int” minOccurs=“1” maxOccurs=“1” />
<xs:element name=“StateFlags” type=“xs:int” minOccurs=“1” maxOccurs=“1” />
<xs:element name=“LSN” type=“xs:int” minOccurs=“1” maxOccurs=“1” />
<xs:element name=“HLMCount” type=“xs:int” minOccurs=“1” maxOccurs=“1” />
<xs:element name=“Platform” type=“xs:string” minOccurs=“1” maxOccurs=“1” />
<xs:element name=“Minutes” type=“xs:int” minOccurs=“0” maxOccurs=“1” />
<xs:element name=“EndDate” type=“xs:dateTime” minOccurs=“0” maxOccurs=“1” />
<xs:element name=“BugCheckCode” type=“xs:int” minOccurs=“0” maxOccurs=“1” />
<xs:element name=“PlatformID” type=“xs:int” minOccurs=“1” maxOccurs=“1” />
</xs:sequence>
</xs:complexType>
<xs:element name=“PayasyougoPacketContent”>
<xs:complexType>
<xs:sequence>
<xs:element name=“HWID” type=“xs:string” minOccurs=“0” maxOccurs=“1” />
<xs:element name=“CreationDate” type=“xs:dateTime” minOccurs=“1” maxOccurs=“1” />
<xs:element name=“SequenceNumber” type=“xs:int” minOccurs=“0” maxOccurs=“1” />
<xs:element name=“TrackingID” type=“xs:string” minOccurs=“0” maxOccurs=“1” />
<xs:element name=“TransactionID” type=“xs:string” minOccurs=“0” maxOccurs=“1” />
<xs:element name=“UPID” type=“xs:string” minOccurs=“0” maxOccurs=“1” />
<xs:element name=“LPMBuildNumber” type=“xs:string” minOccurs=“0” maxOccurs=“1” />
<!-- ========================================================= -->
<!-- Packet type definitions -->
<!-- ========================================================= -->
<xs:element name=“PacketType” minOccurs=“1” maxOccurs=“1”>
<xs:simpleType>
<xs:restriction base=“xs:string”>
<xs:enumeration value=“PREPAID_PROVISION_PACKET_TYPE” />
<xs:enumeration value=“SUBSCRIPTION_PROVISION_PACKET_TYPE” />
<xs:enumeration value=“CONFIGURATION_PACKET_TYPE” />
<xs:enumeration value=“OEM_CONFIGURATION_PACKET_TYPE” />
<xs:enumeration value=“TIMESYNC_PACKET_TYPE” />
<xs:enumeration value=“REFURBISH_PACKET_TYPE” />
<xs:enumeration value=“PERPETUAL_PACKET_TYPE” />
<xs:enumeration value=“NO_MORE_PACKETS_PACKET_TYPE” />
<xs:enumeration value=“LPM_AUTHENTICATION_PACKET_TYPE” />
<xs:enumeration value=“DISABLE_LPM_PACKET_TYPE” />
</xs:restriction>
</xs:simpleType>
</xs:element>
<xs:element name=“ContentChoice”>
<xs:complexType>
<xs:choice>
<xs:element name=“PrepaidContent” type=“PrepaidContentType” />
<xs:element name=“SubscriptionContent” type=“SubscriptionContentType” />
<xs:element name=“TimeSyncContent” type=“TimeSyncContentType” />
<xs:element name=“RefurbishContent” type=“RefurbishContentType” />
<xs:element name=“PerpetualContent” type=“PerpetualContentType” />
<xs:element name=“ConfigurationContent” type=“ConfigurationContentType” />
<xs:element name=“OEMConfigurationContent” type=“OEMConfigurationContentType” />
<xs:element name=“PacketDownloadContent” type=“PacketDownloadContentType” />
<xs:element name=“LPMRequest” type=“RequestContentType” />
<xs:element name=“DisableLPMContent” type=“DisableLPMContentType” />
</xs:choice>
</xs:complexType>
</xs:element>
</xs:sequence>
</xs:complexType>
</xs:element>
<xs:element name=“PayasyougoPacket”>
<xs:complexType>
<xs:sequence>
<xs:element name=“SchemaVersion” type=“xs:int” minOccurs=“1” maxOccurs=“1”
default=“2” />
<xs:element name=“PacketContent” type=“xs:hexBinary” minOccurs=“1” maxOccurs=“1” />
<xs:element name=“Signature” type=“xs:hexBinary” minOccurs=“0” maxOccurs=“1” />
</xs:sequence>
</xs:complexType>
</xs:element>
</xs:schema>
Layer 2 : Payasyougo Packet
<xs:element name=“PayasyougoPacket”>
<xs:complexType>
<xs:sequence>
<xs:element name=“SchemaVersion” type=“xs:int” minOccurs=“1” maxOccurs=“1”
default=“2” />
<xs:element name=“PacketContent” type=“xs:hexBinary” minOccurs=“1” maxOccurs=“1” />
<xs:element name=“Signature” type=“xs:hexBinary” minOccurs=“0” maxOccurs=“1” />
</xs:sequence>
</xs:complexType>
</xs:element>
</xs:schema>
<?xml version=“1.0” encoding=“utf-8” ?>
<xs:schema xmlns:xs=“http://www.w3.org/2001/XMLSchema” elementFormDefault=“qualified”
attributeFormDefault=“qualified”>
Layer 3 : Payasyougo Protocol Packet Content
<xs:element name=“PayasyougoProtocolPacketContent”>
<xs:complexType>
<xs:sequence>
<xs:element name=“HWID” type=“xs:string” minOccurs=“1” maxOccurs=“1” />
<xs:element name=“SessionID” type=“xs:hexBinary” minOccurs=“1” maxOccurs=“1” />
<xs:element name=“PayasyougoPacket” type=“xs:hexBinary” minOccurs=“1” maxOccurs=“1”
/>
</xs:sequence>
</xs:complexType>
</xs:element>
Layer 4 : Payasyougo Protocol Packet
<xs:element name=“PayasyougoProtocolPacket”>
<xs:complexType>
<xs:sequence>
<xs:element name=“SchemaVersion” type=“xs:int” minOccurs=“1” maxOccurs=“1”
default=“2” />
<xs:element name=“MAC” type=“xs:hexBinary” minOccurs=“1” maxOccurs=“1” />
<xs:element name=“ProtocolData” type=“xs:hexBinary” minOccurs=“1” maxOccurs=“1” />
</xs:sequence>
</xs:complexType>
</xs:element>
</xs:schema>
[0052] Although the forgoing text sets forth a detailed description of numerous different embodiments, it should be understood that the scope of the patent is defined by the words of the claims set forth at the end of this patent. The detailed description is to be construed as exemplary only and does not describe every possible embodiment because describing every possible embodiment would be impractical, if not impossible. Numerous alternative embodiments could be implemented, using either current technology or technology developed after the filing date of this patent, which would still fall within the scope of the claims.
[0053] Thus, many modifications and variations may be made in the techniques and structures described and illustrated herein without departing from the spirit and scope of the present claims. Accordingly, it should be understood that the methods and apparatus described herein are illustrative only and are not limiting upon the scope of the claims.
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Methods and a program of instruction provide a packet schema framework for communication between elements of a pay-as-you-go business model including a provisioning server, an adapted electronic device, and a service provider. The packet schema defines provisioning instructions and content types to support service provisioning, including electronic device configuration and state, time-metering, and other types of functional and administrative tasks as well as to provide a foundation for any future messages needed for product evolution. The schema also defines security at multiple levels to guard against malicious users who may try to hook into the system to fraudulently use and/or configure the electronic devices for their own use and gain.
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FIELD OF THE INVENTION
This invention concerns a drill chuck for a drill that is to be used particularly for surgical purposes.
BACKGROUND OF THE INVENTION
A drilling device for surgical proposes is described in EPO application EP-A 90109556.2. It consists essentially of drive means, for example a compressed air turbine or an electrical motor, an angle attachment that can be connected with the drive means via a coupling, and a drill bit connected to the angular attachment. The angular attachment is made of a material that, at least as regards its components adjacent the drill bit, is X-ray permeable. This gives the surgeon unhindered image converter control, so that the operating field is visible to him on an X-ray screen without dark areas of any kind being created by the drilling device. This makes this device suitable for various osteosynthetic procedures, including the positioning of locking holes during intramedullary nailing. Particularly in intramedullary nailing, because of the anatomical-geometrical conditions, angle gear attachments of this type are used. The drill bit in this case can be connected, permanently or via a suitable coupling, with the drive shaft of the angle attachment. However, during an operation, it may be necessary to change one drill bit for another, for example one with a large diameter, as quickly as possible. Drilling devices according to this prior design are not well adapted to this.
SUMMARY OF THE INVENTION
In accordance with the present invention, a drill chuck is provided, especially for surgical purposes, which permits simple and rapid handling, particularly when a drill bit is being changed, while at the same time maintaining perfect and continuous screen monitoring of the drilling procedure by X-rays.
In accordance with the invention, the drill chuck is designed as a quick-change chuck, and is preferably made entirely of a material that is permeable by X-rays. The X-ray permeability creates optimum conditions for screen monitoring of the drilling by a surgeon, and also guarantees a very simple and rapid drill handling, especially when a drill bit is being changed.
The drill chuck, designed as a quick-change chuck, is preferably removably attached to an angle attachment of a drilling device, so that a drill bit can be changed or inserted easily. Advantageously, the chuck is connected to an angular attachment because for the aforementioned drilling purposes angular attachments are preferably used. However, the quick-change chuck can also be attached to a drill not having an angular attachment.
The quick-change chuck according to the invention consists of retaining means which holds a drill bit, a gripper sleeve that envelops the retaining means and can be slid in the direction of the drilling axis, and at least one locking pin that can be slid cross-wise to the drilling axis, which locking pin holds or releases the drill bit in response to longitudinal sliding of the gripper sleeve, whereby the desired ease of use is achieved to the maximum degree.
BRIEF DESCRIPTION OF THE DRAWINGS
Other details and advantages of the invention are explained in greater detail by means of the drawings in which:
FIG. 1 is a vertical section, partly in side elevation, of drilling device with a drill chuck according to the invention;
FIG. 2 is a vertical section, partly in side elevation, of the drill chuck of FIG. 1 in a position that releases the drill bit; and
FIG. 3 is a vertical section, partly in side elevation, of the drill chuck of FIG. 1 in the position of holding the drill.
DETAILED DESCRIPTION OF THE INVENTION
The drilling device 10 shown in FIG. 1 consists essentially of a partially illustrated drive means 11, an angular attachment 12 having an angle gear 13 which angle gear 13 is rotationally connected with the drive 11, and a quick-change chuck 30, which is linked on the drive side to the angle gear 13. The drive means 11 can, for example, be an electric motor or a compressed air turbine, and it has a chuck 16 that is detachedly coupled with a drive shaft 18 of angle gear 13. By means of a bearing 19 that consists, for example, of two anti-friction bearings, the drive shaft 18 is rotationally held in a housing 15 of angle attachment 12, which housing is attached to drive 11. For stabilization purposes, drive shaft 18 is additionally supported at its front end 18' in housing 15. Shaft 18 has attached to its forward section a bevel gear 17, which engages a bevel gear 21 to form the angle gear 13, which is also housed in housing 15.
The driven-side bevel gear 21 is rotationally linked, by means of a pin 29, with a coupling shaft 32 connected to the drive shaft 18 at a 90° angle. This coupling shaft 32 is a component of the quick-change drill chuck 30 according to the invention. The drill chuck 30 consists of a retainer 31 permanently screwed to housing 15, a gripper sleeve 33 that envelops the retainer 31 and may be slid back and forth in the direction of drilling axis A, and three locking pins 34 positioned to slide transversely to drilling axis A and offset from each other at 120° angles. The coupling shaft 32 is rotationally housed in retainer 31, and together they form an opening 36 into which a drill bit 50 can be inserted. The quick-change chuck 30 is made entirely of a material that is permeable by x-rays. Materials such as polyetheretherketone (PEEK), polyamidimide (known, for example, under the name TORLON), and polyoxymethylene (POM) have in particular proven to be very suitable. Their advantage is that in addition to being permeable by x-rays they are also self lubricating and can be sterilized at temperatures up to 140° C. Composite plastics, preferably reinforced by fiber, cloth, or pellets, or special ceramic materials, can also be used.
FIG. 2 shows the quick-change chuck 30 in the position of having released a drill, and FIG. 3 shows the same chuck in a position of holding a drill 50. In the position of FIG. 2, the gripper sleeve 33 is slid over the retainer 31 to a stop 35 at the drill side of the chuck. The locking pins 34, positioned in the chuck 31 in such manner as to slide crossways to drill axis A, are thereupon in pushed-back position, that is, they do not extend into the opening 36 that accepts the drill 50. This is achieved by means of a guide track 37 inside gripper sleeve 33 and running in the direction of drill axis A which permits the locking pin 34 to move radially outward. For this particular embodiment, though only one is shown, there are three locking pins 34 on the circumference of the chuck 31, spaced circumferentially from one another at angles of 120° each. However, it is possible to use only a single pin, or more than three pins.
In FIG. 3 in which the quick-change chuck 30 holds the drill 50, the gripper sleeve 33 is pushed against a stop 41 at the drive side of the chuck. The locking pins 34 project into the opening 36, and thus into an annular groove 52 of a drill shank 53 in which the drill bit 50 is gripped. By means of the sliding of gripper sleeve 33, locking pin 34 is moved in the guide track 37 radially inward to a stop 42 in the retainer 31. The semi-spherical head of the locking pin 34 permits accurate guiding of the said pin in guide track 37. An annular groove 52 in drill shank 53 has a tapered groove surface 52', which is in contact with the rounded tip of locking pin 34, with drill shank 53 striking frontally against a rear frontal surface 36' in opening 36, whereupon drill bit 50 is fixed in its axial direction. Drill shank 53 further has a contact surface 53', and is thus held solidly in opening 36 inside coupling shaft 32 and is moved by said coupling shaft 32. In contrast to drill bit 50, drill shank 53 is made of a material that is permeable by x-rays, and thus the exact drill path can be determined and followed on a screen, for according to the invention, the components of the quick-change chuck 30 transmit the x-rays practically without any loss. On the other hand, for wear resistance, it is possible to make the locking pins 53 of a material not permeable by x-rays.
It should further be mentioned that gripper sleeve 33 consists of the sleeve proper as well as an additional ring 54 that grips the retainer 31, with the gripper sleeve 33 being screwed onto and secured by the ring 54. Between the sleeve and the retainer, on the end facing the drill, there is an O-ring 39 that acts as a seal and in particular as a stop when the gripper sleeve is slid.
The retainer and the coupling shaft housed in it may also consist of a single unit. This is then housed rotationally in housing 15 and rotationally connected with bevel gear 21. Consequently, the entire drill change chuck 30 rotates, whereas in the embodiment described it does not move, and only the coupling shaft 32 and drill bit 50 turn with shaft 53.
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A drill chuck is provided for surgical drilling machines in which the entire chuck is made of material permeable to X-radiation.
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CROSS-REFERENCE TO RELATED APPLICATIONS
[0001] This application is a continuation of International Application No. PCT/FR2012/052583, filed on Nov. 9, 2012, which claims the benefit of FR 11/60277, filed on Nov. 10, 2011. The disclosures of the above applications are incorporated herein by reference.
FIELD
[0002] The present disclosure relates to the manufacture of cellular core panels, and more particularly, to a device allowing the implementation of a method for brazing such panels.
BACKGROUND
[0003] The statements in this section merely provide background information related to the present disclosure and may not constitute prior art.
[0004] The use of acoustic attenuation panels, for example in the nacelles of aircraft engines and nacelle elements equipped with such a panel to reduce noise emissions of turbojet engines, is known from the prior art.
[0005] In the case of an exhaust cone (plug), these acoustic attenuation panels generally have a sandwich structure comprising:
a perforated skin which is permeable to air, external (oriented towards the noise source), called “resistive” or “acoustic” skin, the role of which is to dissipate the acoustic energy, a cellular core structure of the honeycomb type and, an inner skin formed by a solid skin (opposite to the noise source), called structuring skin.
[0009] In some cases, the acoustic attenuation panels are designed to be installed in a hot area of the nacelle of the aircraft turbojet engine, and particularly in the downstream part of this nacelle through which exhaust gases are expelled.
[0010] The use of acoustic attenuation panels in this exhaust area allows for significantly reducing the sound emissions situated in the range of high frequencies.
[0011] For these particular applications at high temperature, acoustic attenuation panels whereof the outer skin is formed by a perforated metal sheet are generally used, the cellular core structure is metallic, and the inner skin is a solid metal sheet.
[0012] The cellular core structure can then be joined by brazing the solid metal sheet and the perforated metal sheet.
[0013] By definition, brazing is a method for assembling two elements using a filler metal having a melting temperature lower than that of the base metal of the elements. By bringing the filler metal to its melting temperature, the filler metal melts and wets the base metal with which it is in contact and then diffuses within the latter. Then, by cooling the assembly, the filler metal solidifies and provides bonding between the different elements in contact.
[0014] Such assembling operations of acoustic attenuation panels are delicate operations insofar as there is a risk that the acoustic and structural qualities of the panel are affected by these operations such as affecting the mechanical strength of the panel or even a loss of panel acoustic absorption.
[0015] A bad relative positioning of the constitutive elements of the panel after brazing can have an impact on the acoustic and structural qualities of the panel.
[0016] It is thus desirable to be able to best control the relative positioning of the pieces involved during brazing and the braze joint, namely the contact between the brazed elements.
[0017] Moreover, the assembling operations can affect metallurgical properties of the treated panel and have an impact on the surface properties of the latter, which can reduce the aerodynamic performances thereof.
[0018] Devices for assembling pieces to be brazed, in which stress forces are exerted on the pieces to be brazed in order to provide a sufficient contact pressure between the pieces and compensate for the expansions of the latter, are already known.
[0019] These forces tend to avoid deformations of pieces during brazing and to maintain them in their relative shape and positioning.
[0020] These deformations, if not controlled, generate brazing defects such as a poor quality of the braze joints or a local lack of the joint.
[0021] A known device provides for the use of tie rods to apply a mechanical pressure on the elements to be brazed, during brazing. The mechanical pressure may be insufficient during the brazing cycle, particularly during melting of the filler material. The defects of the braze joint may persist.
[0022] Another known device can provide for using means providing a gas pressure on the elements to be brazed, a more easily adjustable pressure to compensate for a decrease in the pressure applied on the pieces and prevent deformations and defects of the braze joints.
[0023] Moreover, such a device can further be used to stretch a piece if necessary while it is brazed, such as, for example, bending it such that it takes the shape of a matrix.
[0024] However, such devices face sealing problems that affect the quality of the pressure during brazing, and the properties of the braze joints that result from the brazing cycle.
[0025] Moreover, these problems multiply the maintenances of devices and the associated costs.
[0026] Furthermore, a risk of telegraphing is encountered, which is a phenomenon wherein, under gas pressure, an acoustic panel skin, for example, would be unintentionally deformed upon its installation on the device.
SUMMARY
[0027] The present disclosure provides an assembly device by brazing of a composite panel comprising at least two parts separated by a filler material and intended to be joined together by a braze joint characterized in that it comprises:
[0028] a furnace allowing to reach a temperature for brazing the panel,
[0029] an assembly device comprising a form having a shape similar to the final shape of the panel to be brazed,
[0030] pressing means designed to exert a mechanical pressure on at least part of the surface of said panel along a direction allowing to permanently deform the panel into a shape, the configuration of which complies with that of a form,
[0031] these pressing means being designed to move under the action of elastic forcing means, the forces exerted by said elastic forcing means being determined so that, at the brazing temperature, they exert the forces necessary for deforming the panel against the form.
[0032] Thanks to the present disclosure, there is provided a mechanical assembly device by brazing a panel, easy to implement, which allows for controlling the thermal deformations and expansions of the elements constituting the panel and the braze joint.
[0033] Indeed, such a mechanical device allows to control the stress forces exerted on the panel in order to, on the one hand, provide a proper relative position of the different parts to be brazed, in spite of their respective expansions, throughout brazing, providing therefore a good quality braze joint while allowing to perform, during these expansions, a controlled deformation of the panel into a predetermined final shape.
[0034] According to particular forms of the present disclosure, a device according to the present disclosure can comprise one or several of the following technically feasible features, taken separately or in combination.
[0035] Advantageously, the forces exerted by said elastic forcing means are determined so that, throughout the thermal cycle, they exert the forces necessary to the deformation of the panel against the form.
[0036] Advantageously, the pressing means are movably mounted in translation on a support structure by means of a sliding connection.
[0037] In one form, such pressing means comprise at least one ring formed of a plurality of bearing pads distributed over the surface of the panel on which a mechanical pressure is exerted.
[0038] In another form, the pressing means are provided with at least one travel stop.
[0039] Advantageously, the pressing means are indexed on the support structure.
[0040] In one form, the elastic forcing means comprise leaf springs and/or springs.
[0041] Advantageously, the mechanical pressure exerted by each pressing means is defined independently from the other pressing means.
[0042] In another form, the elastic forcing means are each associated to a locking system defining the tensioning of elastic forcing means.
[0043] As one form, the locking system comprises a wedge system.
[0044] In still another form, the elastic forcing means are designed to become deformed in the direction of the slide.
[0045] In one form according to the present disclosure, the device is made of carbon-carbon material—and in one form is the Sepcarb® brand material, which allows to overcome the effects of flow and deformations generated by the thermal cycles of brazing.
[0046] In one form, the panel is a metal sandwich panel.
[0047] As another form, the panel is a sandwich panel of a cellular core structure.
[0048] The present disclosure also relates to an assembly method by brazing of a composite panel comprising at least two parts separated by a filler material and intended to be joined together by a braze joint implemented by the setup according to the present disclosure wherein:
[0049] the panel is docked on the tooling device;
[0050] the assembly device is placed in the heating means allowing to achieve a brazing temperature of the panel,
[0051] during the thermal cycle and at the brazing temperature, a pressure is exerted by the pressing means on at least part of the surface of said panel in a direction allowing to permanently deform the panel into a shape whereof the configuration conforms to that of the form, these pressing means being designed to move under the action of elastic forcing means, the forces exerted by said elastic forcing means being determined so that, at the brazing temperature, they exert the necessary forces for the deformation of the panel against the form.
[0052] 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
[0053] In order that the disclosure may be well understood, there will now be described various forms thereof, given by way of example, reference being made to the accompanying drawings, in which:
[0054] FIG. 1 is a schematic vertical cross-sectional representation of an assembly device by brazing of an acoustic panel according to the present disclosure, in a position in which the panel is brazed and deformed against a form; and
[0055] FIG. 2 is a schematic cross-sectional representation of the assembly device by brazing of an acoustic panel of FIG. 1 , seen from above.
[0056] The drawings described herein are for illustration purposes only and are not intended to limit the scope of the present disclosure in any way.
DETAILED DESCRIPTION
[0057] The following description is merely exemplary in nature and is not intended to limit the present disclosure, application, or uses. It should be understood that throughout the drawings, corresponding reference numerals indicate like or corresponding parts and features.
[0058] FIG. 1 schematically illustrates an assembly device 1 in accordance with the present disclosure for the implementation of a method of brazing.
[0059] Such a device 1 is arranged inside a brazing furnace, not shown.
[0060] The following examples will be described with respect to an operator requiring to assemble by brazing an acoustic attenuation panel 100 .
[0061] The present disclosure is obviously neither limited to this field of application nor to the types of associated materials.
[0062] An acoustic attenuation panel, designated by the reference 100 on FIG. 1 , includes, on the opposite side to the origin of the acoustic excitement, an inner skin consisting of a structuring skin formed in a sheet.
[0063] On this structuring skin, a structure of acoustic absorption material is brought, which, in a non-limiting manner, is a structure of honeycomb type.
[0064] An external acoustic skin formed, in a non-limiting manner by a perforated sheet can be brought onto the honeycomb structure.
[0065] This acoustic attenuation panel 100 is designed to be used in high temperature areas, in particular on an aircraft nacelle (in particular the area of expulsion of turbojet exhaust gas).
[0066] Thus, the structuring skin and the acoustic skin may be formed from metallic materials.
[0067] These materials can be selected from metals and/or metal alloys such as titanium, Inconel and all their grades.
[0068] The cellular structure may be formed, for its part, of metallic, polymer, ceramic or composite materials, available on the market.
[0069] The cellular structure can be fixed on the acoustic skin and on the inner skin by a brazing method, with an assembly device according to the present disclosure.
[0070] For this, a filler material interposed between the sheets and the cellular core structure is provided. It can be formed by a strip of braze joint or any other filler material of brazing, such as for example, a powder.
[0071] The melting point of this filler material should be lower than the melting temperature of the base metal of the skins and of the acoustic structure.
[0072] The device is designed to apply to this panel 100 , during brazing, forces which tend to permanently deform from an initial shape of preform to a final shape after brazing.
[0073] More particularly, according to the present disclosure, the device 1 comprises pressing means 30 designed to exert mechanical pressure on at least part of the surface of said panel 100 in a direction allowing to permanently deform the panel 100 into a shape the configuration of which conforms to that of a form 20 during brazing.
[0074] These pressing means 30 are designed to move under the action of elastic forcing means 210 , the forces exerted by said elastic forcing means 210 being determined so that throughout the assembly (of the brazing cycle(s) in particular), and more particularly at brazing temperature, they exert the necessary forces to the deformation of the panel 100 against the form 20 .
[0075] More specifically, with reference to FIGS. 1 and 2 , the assembly device 1 includes a frame 10 having a basic base 11 and a lid 12 , the base 11 and the lid 12 being connected by a support structure 13 .
[0076] This support structure 13 perpendicular to the base 11 and to the lid 12 is exhibited, according to a non-limiting example a conical framework with a double wall 13 a , 13 b.
[0077] The base 11 and the lid 12 are designed to allow a docking of the panel 100 to be brazed using clamping means (not shown).
[0078] These clamping means may include, but are not limited to, clamping screws.
[0079] The device 1 further comprises several deformation units 200 of the treated panel, in one example by the number of 96, designed to apply forces to the treated panel 100 , still in the preform phase, during brazing, which tend to deform the panel 100 against the form 20 thus, so that the panel 100 espouses the mark of said form 20 .
[0080] The number 96 of units is given for illustrative purposes and is in no way limiting.
[0081] Each unit 200 is implemented within the brazing furnace facing the form 20 the shape and dimensions of which are complementary to the final shape of the brazed panel 100 .
[0082] This form 20 is a rigid external shell, stationary, integral with the frame 10 and, more particularly, the base 11
[0083] In one form, it consists of two upper and lower parts, this in order to facilitate the unmolding of the panel 100 at the end of the brazing cycle(s).
[0084] Each deformation unit 200 is mounted permanently on the support structure 13 in order to cooperate with the pressing means 30 , themselves indexed, in part, by suitable means on the support structure 13 .
[0085] This support structure 13 is associated, along the panel 100 to be brazed, to one or several superposed rings, each provided with several pressing means 30 providing forces that tend to apply the panel against the form 20 .
[0086] These pressing means 30 may be distributed over the surface of the panel 100 on which each pressing means 30 exerts a local mechanical pressure.
[0087] Specifically, each pressing means 30 comprises at least one pressing sector 32 designed to contact the panel 100 , this pressing sector 32 being slidably mounted relatively to the support structure 13 by means of a sliding connection.
[0088] Each pressing means 30 can move to apply a pressure to the panel 100 to be brazed, this movement being defined as cited above, by the elastic forcing means 210 to which they are associated.
[0089] Each of these is associated with end-of-travel stops limiting their movement and that, as a result, of the panel 100 to be brazed.
[0090] Thus, in one form mode of the present disclosure, illustrated in FIGS. 1 and 2 , the rings of the pressing sector 32 are superposed by a suitable system, for example of a basket type, along the panel 100 and independently from the conical framework 13 .
[0091] The pressing means 30 may come in the form of a pad 32 driven by a retainer rod 33 provided at its end opposite to the pad 32 , with a supporting head 31 , in simple contact on the corresponding pad 32 and, at the opposite end, a head forming an end-of-travel stop 34 of the rod 33 .
[0092] This retainer rod 33 is mounted permanently in the support structure 13 crossing both walls 13 a , 13 b.
[0093] As for the heads forming end-of-travel stop 34 , they allow to prevent any exit of the retainer rod 33 from its housing in the support structure 13 .
[0094] They further participate in the locking/unlocking of the corresponding pressing means 30 , as will be described later in the description.
[0095] In one form, the pressing means 30 have an axial stroke, radially with respect to the support structure 13 , of the order of 3 mm in radius.
[0096] It is also to be considered to vary the stroke in an interval of 3 to 10 mm in radius.
[0097] Pertaining to the units of deformation 200 , they include thrust systems of the pressing means 30 of the panel 100 , namely the elastic forcing means 210 but also the locking means 220 providing the tensioning of the elastic forcing means 210 and used to support the latter.
[0098] The elastic forcing means 210 are fixed on the support structure 13 and more particularly, each in a particular concavity formed between the double wall 13 a , 13 b by a suitable maintenance system.
[0099] It may be mentioned, as non-limiting example of maintenance system, a ring providing the maintenance of the corresponding elastic forcing means 210 in the framework 13 .
[0100] Furthermore, each elastic forcing means 210 is mounted on the circumference of the retainer rod 33 of the corresponding pressing means 30 , between the supporting head 31 and the locking means 220 .
[0101] The elastic forcing means 210 may come in a non-limiting manner, in the form of a leaf spring or a spring.
[0102] The locking means 220 are also supported by this support structure 13 and arranged in the axis of the sliding connection, opposite the corresponding support pad 32 , between the elastic forcing means 210 and the head forming an end-of-travel stop 34 of the retainer rod 33 .
[0103] The locking means or tapered wedges 220 as will be seen below allow the withdrawal of elastic forcing means 210 so as to provide the placing of the cone of the support structure 13 .
[0104] The tapered wedges 220 are removed after locking the expansion plug on the frame 13 so that the elastic forcing means 210 exert a force on each pad 32 , throughout the assembly and the thermal cycle of the panel 100 and particularly at brazing temperature.
[0105] This force is such that it provides the maintenance of the relative position of the constitutive elements of the panel 100 during their dilatation, while directing the deformation of the panel 100 so that it espouses the shape of the form 20 , resulting in a plastic deformation of the panel 100 into its final shape.
[0106] Experiments, tests, routines, or calculations allow finding the calibration of the elastic forcing means 210 , compared with their relative position on the panel 100 to be heat conformed.
[0107] More particularly, each elastic forcing means 210 is compressed to exert on the corresponding pressing means 30 a force in the direction of the slide, causing a radial displacement of the pressing means 30 which exert as such a compression force perpendicular to the panel surface 100 on the latter.
[0108] In one form, these locking or withdrawal means 220 include wedge systems 221 , each of which defining the clamping force by biasing the corresponding elastic forcing means 210 .
[0109] As illustrated in FIG. 1 , in an alternative form, each wedge system 221 comprises two complementary beveled corner sections 222 , 223 , mounted between the inner side (opposite the elastic forcing means 210 ) of the inner wall 13 a of the support structure 13 and the stop 34 of the retainer rod 33 , on the circumference of the latter.
[0110] The relative movement of these two corner sections 222 , 223 along the inner side of the inner wall 13 a of the support structure 13 defines the associated movement of the retainer rod 33 .
[0111] Any other known withdrawal system 220 may be provided.
[0112] During the temperature rise, the skins/sheets and the cellular core structure of the panel 100 are subjected to expansion forces and their relative position may change as they tend to become spaced apart from each other.
[0113] The device 1 according to the present disclosure allows to apply evenly distributed forces of adapted intensity on the panel 100 to maintain the relative position of the parts to be assembled according to their expansions by the movement of the pressing means 30 along the corresponding slide, while allowing a permanent monitored plastic deformation of the panel 100 against the form 20 .
[0114] In one form, the pressure exerted in a range in the order of 6 Mpa to 18 Mpa.
[0115] Furthermore, the device 1 is at least partially of carbon-carbon material (in one for is the Sepcarb® brand material).
[0116] In another form, the elastic forcing means 210 are made of carbon-carbon material.
[0117] Such a material has low thermal inertia.
[0118] It is resistant at high temperatures and light, and thus reduces the mass of the device and can extend the service life of the device to about 20 years.
[0119] In a non-limiting example, the elastic forcing means 210 are formed by the methods described in French patent application FR 2 772 748, which is incorporated herein by reference in its entirety.
[0120] Furthermore, the device 1 allows a significant economic gain on the service life of an aircraft program on the investment as well as on the production time.
[0121] It also allows brazing several components at the same time as furnaces are limited in tonnage.
[0122] Its low mass also allows reducing the brazing cycle owing to the low thermal inertia of the tooling.
[0123] Furthermore, such a device may be placed in a brazing furnace provided with means designed to carry out a vacuum brazing.
[0124] A method of assembly by brazing using a device 1 according to the present disclosure is now described.
[0125] First, various points of attachment between the skins and acoustic structure of the panel 100 , are carried out, preferably at each end of the jointing of one of the skins.
[0126] In a non-limiting example, these points may be welding points.
[0127] Thereafter, the panel to be brazed 100 is docked on the base 11 provided with the lower part of the form 20 (cut at the apex to allow its implementation and unmolding).
[0128] The panel 100 in place, it can then be installed the second part of the form 20 around the panel 100 .
[0129] In a non-limiting example, six rings of 16 pads 32 are superimposed by a suitable system, facing the support structure 13 and independent from the latter.
[0130] These pad rings 32 are distributed radially opposite to an internal side of the panel 100 to be brazed.
[0131] Mounting of the expansion system 13 with the elastic forcing means 210 in the retracted position by the wedge systems 220 and 221 , is then performed.
[0132] At this stage, the elastic forcing means 210 are compressed and biased by the withdrawal means 220 and 221 . Once the expansion system 13 is locked by screwing on the upper part of the base 12 , the wedge systems 220 to 223 may be removed to release the pressure from the pads 32 .
[0133] At this stage, each deformation unit 200 exerts a pressure on the internal wall of the corresponding pad ring 32 .
[0134] It is worth noting that the elastic forcing means 210 are in cold and hot compression throughout the brazing thermal cycle.
[0135] This allows preventing a detachment of the panel 100 with the tooling during the cooling phase of the cycle.
[0136] Furthermore, the compression of the panel 100 by the pressing means 30 is permanent, continuous and exerted before the beginning of the brazing cycle; during the whole brazing cycle until the withdrawal of the panel 100 from the form 20 .
[0137] It is worth noting that, at room temperature (20° C.), the panel 100 to be brazed is not pressing on the form 20 . Contact only occurs once the brazing temperature is reached.
[0138] Thus, prior to the brazing cycle, the locking means 220 are unlocked, the biasing of the elastic forcing means 210 is released for compressing each pad 32 on the panel 100 .
[0139] In a following step, at least one brazing cycle is started after having emptied the furnace chamber.
[0140] The furnace temperature is thus raised to the brazing temperature.
[0141] During the rise in temperature, differential expansions between the elements of the panel 100 to be brazed, the filler material and the device 1 are present.
[0142] Each elastic forcing means 210 applied to the corresponding pressing means 30 causes the retainer rod 33 and the associated pad 32 in a displacement providing a pressure on the panel 100 such as to compensate the phenomena of differential expansion of the elements.
[0143] At the brazing temperature at the same time higher than the melting temperature of the filler metal and lower than the melting temperature of each of the three materials, the mechanical pressure exerted by each elastic forcing means 210 on the corresponding pressing means 30 is calibrated to move by sufficient axial stroke the related pressing means 30 to stretch the panel 100 , so that it espouses the shape of the form 20 .
[0144] The forces applied to the panel 100 extending beyond the forces related to the thermal expansion of the various elements thereof and providing to maintain these elements providing in contact throughout the brazing cycle, not only is the mechanical pressure applied adapted to form uniform braze joints for the brazed panel 100 but also to heat form the panel 100 .
[0145] The following step consists in cooling the treated panel 100 by decreasing the temperature by suitable means, so as to solidify the filler metal which thus makes a connection between the two materials.
[0146] It is worth noting that, in one form, the brazing operation is carried out under vacuum.
[0147] At this stage, an acoustic panel 100 is obtained whereof the acoustic structure and the skins are brazed and the panel 100 conformed to its final shape.
[0148] Hence, a panel 100 brazed and conformed in one single operation with good brazing quality is obtained.
[0149] Thanks to the present disclosure, the differential expansions of the panel 100 , the tooling and the filler material are monitored throughout the brazing cycle in order not to change the relative position of the latter and in a precise manner, the deformation of the panel 100 to a particular shape of a form 20 is guided, by a simple and rapid to implement mechanical device.
[0150] Such a device finds a non-limiting application in the brazing of panels 100 having to present one or several bends in their profile.
[0151] Advantageously, the geometry of the parts to be brazed and to be conformed can be a geometry of revolution.
[0152] Such a device allows reducing the brazing cycle time. In fact, the device 1 makes it possible to braze two pieces simultaneously since thanks to its low mass, it is possible to place two pieces in the same furnace. This can go as far as not needing to invest in a vacuum furnace.
[0153] Furthermore, it avoids problems of sealing that may occur in the assembly devices of the prior art where gas pressure is required.
[0154] It also reduces the phenomena of “telegraphing” resulting from a depression of the skins of the panels during their docking in the assembly devices of the prior art in which a gas pressure device is required
[0155] Such a tooling has an improved service life (no flow) and the maintenance, due to the simplicity of the device, is lesser and cheap.
[0156] Although the present disclosure has been described with specific form, it is obvious that it is in no way limiting and that it includes all technical equivalents of the means described as well as the combinations thereof if these fall within the scope of the present disclosure.
[0157] Thus, it can be considered to exert different or not local stress forces according to their position on the panel to be treated.
[0158] An alternative form may also provide to exert stress forces on either side of the panel 100 to be treated rather than on the same side of the latter.
[0159] Furthermore, an alternative form may provide a brazing cycle under a monitored atmosphere.
[0160] The present disclosure may also find a non-limiting application in brazing acoustic attenuation panels used in ejection cone/primary turbojet nozzle setups.
[0161] In addition, each panel may be conformed and brazed by a device according to the present disclosure with the front and rear flanges thereof welded with finished lugs. This provides the hold of the eject section and performing a thermal releasing treatment after the brazing while enjoying a hold of the setup throughout the cycle.
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A setup for assembling, by brazing, a composite panel including at least two parts separated by a filler material and joined together by brazing. The setup includes a furnace to achieve a brazing temperature for brazing the panel, and an assembly device which has a form having a shape similar to the final shape of the panel to be brazed. In particular, the assembly device further includes a pressing device to apply mechanical pressure to at least part of the surface of the panel in a direction allowing the panel to be permanently deformed into a shape which matches that of the form. The pressing device is moved under the action of a spring, and the forces applied by the spring being determined so that, at the brazing temperature, the spring applies the force necessary for deforming the panel against the form.
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CROSS REFERENCE TO RELATED APPLICATIONS
[0001] This application is a divisional application of application Ser. No. 10/192,639, filed Jul. 11, 2002, which is a divisional application of Ser. No. 09/962,271, filed Sep. 26, 2001.
BACKGROUND OF THE INVENTION
Field of the Invention
[0002] The present invention concerns a signal for synchronizing base stations in a mobile radio telecommunication system. More particularly, the present invention concerns a signal for synchronizing base stations for a telecommunication system of the time division duplex (TDD) type. The telecommunication system is for example the system for which a standard is at present being drawn up, normally referred to as 3GPP W-CDMA TDD.
[0003] FIG. 1 depicts a radio frame of such a telecommunication system. It consists of fifteen time slots, some of which, for example the slots IT 0 , IT 1 , IT 2 , IT 5 , IT 6 and IT 8 , are intended for conveying data (in the broad sense of the term) in the downlink direction (base station to mobile terminal) whilst others, the slots IT 3 , IT 4 , IT 7 , IT 9 , IT 10 , IT 11 , IT 12 , IT 13 and IT 14 , are intended for conveying data in the uplink direction (mobile station to base station). During a transmission slot, the data (D) are transmitted in the form of a sequence of symbols. The slot also includes a midamble (M) comprising pilot symbols enabling the channel to be estimated, a power control word (TPC) and a guard period (GP′). In such a system, several mobile terminals or base stations can transmit or receive data in the same time slot. The connections are differentiated by code division multiplexing (Code Division Multiple Access=CDMA). The symbols transmitted by or for the different users are spectrally spread, approximately at a “chip” frequency 1/T c where Tc is the elementary transmission period.
[0004] Because the same frequency can be used both in the uplink direction and in the downlink direction, it is essential to ensure synchronization of the base stations. This is because, if such were not the case, a first mobile terminal transmitting at high power in an uplink channel could interfere with a second mobile channel, close to the first, receiving data over a downlink channel. The synchronization constraint between adjacent base stations is around a few microseconds (approximately 5) in the WCDMA TDD system.
[0005] To effect synchronization between base stations, several methods have been proposed in the state of the art. According to a first method, the synchronization is achieved by virtue of GPS receivers equipping the base stations. According to a second method, first of all, in an initial phase, for example during the phase of setting up the network or a new base station, an approximate synchronization is carried out (of around a few tens of ms, that is to say a few tens of thousands of “chips”). This rough initial synchronization is provided by the network, or more precisely by the radio access controller (RNC) controlling several adjacent base stations (also referred to as “B nodes”). A fine synchronization is then effected regularly by the radio interface between adjacent base stations. The purpose of this fine synchronization is notably to correct any difference in the sequencing clocks between adjacent base stations. To do this, certain time slots are reserved for the transmission and reception of a synchronization signal. A time slot dedicated to synchronization comprises essentially a synchronization signal (Sync) and a guard period (GP). Synchronization is obtained, in a manner known per se, by correlation of the received sequence with a sequence which is a replica of the one transmitted. The correlation is effected on a time window with a length given by the margin of accuracy of the approximate synchronization. Thus, when a base station receives a synchronization signal and detects a correlation peak in this window, it can synchronize its sequencing with that of the adjoining base stations.
[0006] The synchronization signal generally used is lengthy (a few thousands of “chips”) in order to obtain good accuracy of correlation for an acceptable power per symbol. The guard period must be greater than the propagation time from a base station to an adjacent station so as to avoid, on reception, an encroachment of the synchronization signal on an adjacent time slot. The distance between two base stations being greater than the radius of a cell, the guard period (GP) is chosen so as to be greater than the normal guard period (GP′). The guard period (GP) must also take account of the difference between the frame clocks.
[0007] The synchronization signal is chosen so as to have good autocorrelation properties, namely a very pronounced autocorrelation peak. Generally the synchronization signals used are obtained from primitive polynomials on GF(2), a Galois field of cardinal 2. Such a sequence has a length L which is an N th power of 2 minus 1, that is to say L=2 N −1. This is the case notably for so-called Gold sequences proposed in the report TSGR1#15(00)0946 entitled “Sequences for the cell sync burst” of the Working Group TSG-RAN of the ETSI for synchronizing adjacent base stations.
[0008] Gold sequences have good periodic autocorrelation properties (the correlation of a sequence consisting of the repetition of a Gold sequence with a replica of the sequence of the latter does not have significant secondary peaks). On the other hand, these sequences unfortunately do not have such good aperiodic autocorrelation properties (correlation of an isolated Gold sequence with a replica). What is more, the correlator generally used operates in the time domain in the form of a conventional adapted FIR filter having a complexity in terms of O(L) which can be very high. In addition, the choice of the lengths of such sequences is reduced, since they can, as has been seen, take only values 2 N −1 and a truncation would lead to a substantial loss of autocorrelation properties.
SUMMARY OF THE INVENTION
[0009] One purpose of the present invention is to propose a signal for synchronizing adjacent base stations by virtue of the transmission of a correlation sequence having very good autocorrelation properties and a wide choice of possible lengths, and this for a low degree of complexity of the correlator.
[0010] The present invention is defined by a signal for synchronizing base stations in a mobile radio telecommunication system in which a first base station transmits a synchronization signal having a first sequence followed by a second sequence, the first and second sequences being obtained from polyphase complementary sequences, and at least one second base station effects the correlation of the synchronization signal with a replica of the first sequence and a replica of the second sequence, the correlation results then being added in order to provide synchronization information.
[0011] Advantageously, the first and second sequences are Golay complementary sequences.
[0012] According to a first embodiment, the synchronization signal comprises guard times around the first and second sequences.
[0013] According to a second embodiment, the synchronization signal comprises a periodic extension of the first sequence followed by a periodic extension of the second sequence.
[0014] According to a third embodiment, the first sequence is generated by means of a first Golay sequence and a first ancillary sequence by successively multiplying the first Golay sequence by the bits of the first ancillary sequence.
[0015] Likewise, the second sequence can be generated by means of a second Golay sequence, complementary to the first Golay sequence, and a second ancillary sequence by successively multiplying the second Golay sequence by the bits of the second ancillary sequence.
[0016] Advantageously, the first ancillary sequence and the second ancillary sequence are Golay complementary sequences.
[0017] According to a variant embodiment, the correlation is effected by a trellis filtering.
BRIEF DESCRIPTION OF DRAWINGS
[0018] The characteristics of the invention mentioned above, as well as others, will emerge more clearly from a reading of the following description given in relation to the accompanying figures, amongst which:
[0019] FIG. 1 depicts schematically a transmission frame of a transmission system of the W-CDMA TDD type;
[0020] FIG. 2A depicts a first embodiment of the invention;
[0021] FIG. 2B depicts a second embodiment of the invention;
[0022] FIG. 2C depicts a third embodiment of the invention;
[0023] FIG. 3 depicts a correlator useful to the third embodiment of the invention.
DETAILED DESCRIPTION
[0024] The general idea at the basis of the invention is to use, for synchronizing adjacent base stations, a pair of complementary polyphase codes and more particularly a pair of Golay complementary codes. In the remainder of the description, mention will be made not of polyphase codes but of Golay codes. It is clear, however, that the invention applies to polyphase codes in general.
[0025] These complementary codes, known as such, have the remarkable property that the sum of their aperiodic autocorrelation functions is a Dirac function. In other words, if a pair of such complementary codes is denoted (A,B), this gives a□AA(m)+□BB(m)=□(m) where m is the time index, □ the Kronecker symbol, and □ the aperiodic autocorrelation function.
[0026] In addition, as described notably in the article by S. Z. Budisin, entitled “Efficient pulse compressor for Golay complementary sequences”, published in Electronics Letters, Vol. 27, N□3, pages 219-220 in January 1991, the correlator can be produced by virtue of a trellis filter having a complexity in terms of O(logL) rather than in terms of O(L) as in a conventional adapted FIR filter. This trellis filter is also referred to as an EGC filter, standing for Efficient Golay Correlator. An example of an embodiment of an EGC filter is given in the article by B. M. Popovic entitled “Efficient Golay Correlator”, published in IEEE Electronics Letters, Vol. 35, N□ 17, January 1999.
[0027] In addition, for a given authorized length, there are several possible Golay sequences. This is because, Golay sequences being generated by generator codes, it can be shown that two distinct generator codes with the same length generate Golay sequences which are also distinct and have the same length. These sequences have good intercorrelation properties (that is to say low intercorrelation values), enabling, for example, groups of base stations to use distinct codes or again to effect a synchronization of the base stations at different times of their sequencing.
[0028] A first embodiment of the invention is illustrated in FIG. 2A . According to this embodiment, a synchronization signal consists of two Golay complementary sequences A and B multiplexed in time, each sequence being preceded and followed by a guard time, as described in the French application FR-A-9916851 filed on 30/12/99 in the name of the applicant. This synchronization signal is transmitted by a base station and is received by an adjacent base station. On reception, the synchronization signal is correlated with a replica of the sequence A and a replica of the sequence B, and the result of correlation with the sequence A is delayed so as to be aligned in time with the result of correlation with the sequence B before they are added, the Dirac peak being obtained when the replicas of A and B are aligned with the corresponding sequences. The presence of the guard times GP 1 , GP 2 and GP 3 ensures that, at the time of correlation, the sequences A and B do not overlap the corresponding complementary replicas, namely B and A respectively, in a time window centered on the time alignment position. Thus secondary correlation peaks can result from the intercorrelation between sequences and complementary replicas are ejected out of this window. More precisely, if GP 2 =2.GP 3 =2.GP 1 =2.GP, the sum of the two correlation results has an isolated Dirac peak in a window of width 2.GP around the time alignment position. The correlations are advantageously effected by EGC correlators, as mentioned above.
[0029] A second embodiment of the invention is illustrated in FIG. 2B . According to this embodiment, a synchronization signal consists of two Golay complementary sequences multiplexed in time, each sequence being preceded and followed by a periodic extension, as explained in the French application entitled “Channel estimation sequence and method of estimating a transmission channel using such a sequence” filed in the name of the applicant. The periodic extension of a given sequence is a truncation of the periodic sequence obtained by repetition of the sequence. To do this, it suffices to concatenate with the sequence to be extended a prefix corresponding to the end and a suffix corresponding to the start of the sequence. FIG. 2B indicates schematically the concatenation of prefixes and suffixes for two Golay complementary sequences A and B. The synchronization signal itself consists of two sequences thus extended ext(A) and ext(B). The periodic extensions produce the same advantages as the guard times, namely the absence of secondary correlation peaks around the Dirac peak in a certain time window. More precisely, if the suffixes and prefixes are of identical size and equal to E, the sum of the correlation results will have an isolated Dirac peak in a window of width 2.E around the time alignment position. This will easily be understood if the case is considered where the synchronization signal comprises completely periodised sequences A and B. The correlation with replicas of A and B then produces a series of Dirac peaks of period L. A periodic extension of size E amounts to truncating this series by a window of width 2.E around the time alignment peak. The advantage of this embodiment compared with the previous one is not to cause abrupt variations in signal power between the sequences A and B, at the transmitter amplifier. Such abrupt variations may generate high frequencies and intersymbol interference and consequently degrade the correlation results on reception.
[0030] A third embodiment of the invention is illustrated in FIG. 2C . According to this embodiment, a composite sequence ( 10 ) is generated from a Golay code sequence A or B and an ancillary sequence X ( 20 ), according to the mode of constructing the hierarchical sequences. More precisely, the first bit of the ancillary sequence X ( 20 ) is multiplied successively by all the bits of the sequence A, and then the second bit of the second sequence by all the bits of the sequence A, and so on, and he sequences obtained are concatenated. Such a composite sequence will be noted below A*X ( 30 ), A being the base sequence and X being the generator ancillary sequence ( 20 ). The Golay complementary sequences A and B can thus be multiplied by ancillary sequences X, Y, identical or distinct, the latter also being able themselves to be Golay sequences
[0031] Let A*X and B*X be composite sequences obtained from a pair A, B of Golay complementary sequences, of length L, extended by prefixes and suffixes of size E. A*X and B*X are multiplexed in time and separated by an interval W. The signal received is correlated with the sequence A on the one hand and with the sequence B on the other hand.
[0032] The result of the first correlation is delayed by (L+2E)+W and is summed with the result of the second correlation. The sum obtained is a sequence R having a series of Dirac peaks of period L′=L+2E modulated by the values x 0 , x 1 , . . . ,x K where K is the length of the sequence X, each peak being surrounded by a window of width 2.E containing only zeros. The sequence R is then subjected to a filtering by means of a linear response filter:
H ( z )= x 0 +x 1.z −L′ + . . . +x k.z −K.L′ .
[0033] The filtered sequence R includes a Dirac peak of height 2.K.L in the middle of a zero window of width 2.E which makes it possible to detect it easily. In addition, the total sequence consisting of the sequences A*X and B*X multiplexed in time is of total length 2.(L+2.E).K+W, which offers a wide choice of lengths of permitted sequences.
[0034] According to another variant embodiment, four composite sequences A*X, A*Y, B*X, B*Y are generated, where A, B form a first pair of Golay complementary sequences, extended or not, and X, Y form a second pair of Golay complementary sequences serving as generator ancillary sequences.
[0035] The composite sequences are multiplexed in time and separated by intervals which will be assumed to be equal and of width W. The sequences A and B are of length L′=L+2.E where L is the length of the basic sequence and E the size of the extension, the sequences X, Y being of length K. The total sequence length is therefore 4(L+2E)K+3W, which offers a wide choice of permitted sequence lengths.
[0036] The present variant takes advantage of the fact that there are L′ pairs of complementary sequences (X,Y) in the form of sub-sequences S m and S′ m with S m (n)=(A*X) n.L′+m and S′ m (n)=(B*X) n.L+m , m= 0 , . . . ,L′−1 obtained by decimation of the initial total sequence. Instead of effecting a correlation with an EGC correlator, a “hierarchical” correlator is used, the first stage of the EGC function correlator modified as depicted in FIG. 3 .
[0037] It will be assumed that the pair of sequences X and Y has been generated conventionally by an elementary sequence s 0 , . . . ,s k−1 , where K=2 k −1, and delays D′ 0 , D′ 1 , . . . ,D′ k−1 with D′ i =2 Pi where (P 0 , P 1 , . . . ,P k−1 ) is a permutation on the set (0, 1, . . . ,k−1), recursively as follows:
X 0 ( i )=□( i ); Y 0 ( i )=□( i );
X n ( i )= X n−1 ( i )+ s n−1 .X n−1 ( i−D′i ); Y n ( i )= Y n−1 ( i )− s n−1 .Y n−1 ( i−D′ i );
Likewise, it will be assumed that the pair of sequences A, B was generated by the elementary sequence t 0 , . . . ,t l−1 , where L=2 1 −1, and delays D 0 , D 1 , . . . ,D k−1 with D i =2 Pi where (P 0 , P 1 , . . . ,P l−1 ) is a permutation on the set (0,1, . . . ,l−1).
[0038] The first correlation stage effects a correlation with the pair of sequences X, Y, but differs from a conventional EGC correlator in that the delays have been multiplied by a factor L′ in order to take account of the scattering in the samples. The two correlation results are added after time alignment by a delay D XY , the delay D XY separating the sequences A*X and A*Y, on the one hand, the sequences B*X and B*Y, on the other hand. The second stage of the correlator effects the correlation with the pair of sequences A, B and is conventional per se. The correlation results are aligned in time by a delay D AB and added, the delay D AB corresponding to the difference in time between the sequences A*X and B*X on the one hand and the sequences A*Y and B*Y on the other hand.
[0039] The correlator thus formed first of all effects a rough correlation with a step L′ and then a fine correlation to the sampling step. Its complexity is low since the number of operations performed is in O(log(K)+log(L)).
[0040] Although the example described above has only two sequence levels and two correlation levels, the invention can be extended in an immediate manner to any number of levels of sequences and corresponding stages of the hierarchical correlator.
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A synchronization signal used to synchronize base stations in a mobile radio telecommunication system having a first sequence followed by a second sequence, the first and second sequences being polyphase complementary sequences configured such that when the synchronization signal is correlated with a replica of the first sequence and a replica of the second sequence, and the correlation results are added exemplary synchronization results are obtained.
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This is a continuation of application Ser. No. 365,958 filed 5/31/73 now abandoned.
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to time-division switching networks for transmitting PCM (Pulse Coded Modulation) speech signals and, more particularly, to means and processes for propagating speech samples and space-division switching cross-point addresses through large size networks including, at least, one time-division switching stage and one space-division multistage switch.
2. Description of the Prior Art.
Such time-division switching networks are well known and may be parts of local or toll exchanges. They are designed for handling a great number of ingoing or outgoing time-division channels. Every time-division stage includes separate time-division groups, each group being respectively connected to a separate individual link of the space-division switch.
In a known manner, the purpose of the space-division switch is to extend network capacity over limits resulting from present pure time-division switching network technology, and utilization of a space-division switch together with ingoing and outgoing time-division groups makes it possible to attain very large size networks.
In high-traffic large size networks, the space-division switch advantageously comprises several cascaded stages. The resulting drawback is that speech sample transfer time, via the space-division switch, increases as the number of stages. Transferring a sample through the space-division switch during a single network elementary time becomes difficult, whereas it may be performed readily in networks having smaller capacity.
Furthermore, the various cross-points contributing to a sample propagation path must be addressed. Due to the large number of time-division channels connected to networks of this kind, memory capacity reserved in the network for cross-point addresses is particularly important.
SUMMARY OF THE INVENTION
A purpose of the present invention is then to provide means and processes permitting, on the one hand, to design large capacity time-division switching networks including a space-division multistage switch through which speech sample transmission is longer than the considered time-division network elementary time, and, on the other hand, to substantially reduce the memory capacity reserved for cross-point addresses with respect to that needed in known means and processes.
According to a feature of this invention, there is provided a time-division network with, at least, a time-division stage and a space-division multistage switch, which incudes means for sequentially propagating step-by-step, through a speech sample propagation path as it is established, at least part of addresses of cross-points pertaining to that path and to the considered speech sample, each step leading through a predetermined number of cross-points of the considered path either at least part of the following cross-point addresses, if any, or the speech sample which follows them on that path.
The time-division switching network also comprises means for simultaneously propagating addresses of the various cross-points of a path.
According to another feature of this invention, within a time-division network having an input time-division stage which comprises separate time-division groups, each time-division group having a speech memory connected, via a separate so-called outgoing register, to a separate input link of the first space-division switch stage, network propagating means include hereunder defined space-division address memories, transfer registers, space-division address memory output registers and addressing registers.
In each time-division group, a space-division address memory is associated to the speech sample memory and has as many rows as in the speech sample memory and a number of columns at least equal to the number of bits needed for addressing the various crosspoints of any sample propagation path.
In each input link of each space-division switch stage, a transfer register is mounted which has a capacity at least equal to the number of speech sample bits.
A crosspoint addressing register is associated to each input link of each space-division switch stage, and it is so connected and designed as to be able to receive the binary address of any one of the crosspoints capable to connect the considered associated input link to an output of the stage reached by that link.
A process for propagating crosspoint addresses and speech samples in a switching network according to this invention comprises the following steps:
addresses of crosspoints determining a sample propagation path through the space-division switch stages are associated to the corresponding speech sample;
at the beginning of one of the two portions of each time-division network elementary time, hereinafter defined as first elementary half-time, the transfer of all crosspoint addresses contained in input time-division group output registers is triggered toward next registers;
at the beginning of the other portion of each time-division network elementary time, hereinafter defined as second elementary half-time, the transfer of speech samples contained in input time-division group outgoing registers is triggered toward next registers;
at the beginning of each elementary half-time, the transfer of binary data (samples or addresses) contained in transfer registers located at space-division stage inputs -- save those of the last space-division stage -- is triggered toward the next registers;
at the beginning of one elementary half-time out of two, the transfer of binary data contained in transfer registers located at last space-division stage inputs is triggered toward next registers, such an elementary half-time being the first half-time if space-division stage number is even and being the second half-time if space-division stage number is odd.
BRIEF DESCRIPTION OF THE DRAWINGS
Other features of the present invention will appear more clearly from the following description of an embodiment, the said description being made in conjunction with the accompanying drawings, wherein:
FIG. 1 is a schematic diagram of an embodiment of a network according to this invention, and
FIG. 2 is a time diagram concerning the propagation process according to this invention and relating to two successive samples from a same time-division group.
DESCRIPTION OF PREFERRED EMBODIMENTS
The embodiment shown in FIG. 1 relates to a time-space-time division network, but may apply to any combination of time- and space-division stages without limitation. Attention is directed to co-pending applications Ser. No. 291,995 filed Sept. 25, 1972 and Ser. No. 350,053, filed Apr. 11, 1973 for additional information respepcting related systems.
The network shown in FIG. 1 comprises an input stage including a plurality of separate identical time-division groups, such as 1a and 1b, a cascaded three-stage space-division switch 2 and an output stage including a plurality of separate identical output time-division groups, such as 3a and 3b.
Each input time-division group having an identical structure, only the group 1a will be described which conventionally includes a speech memory 7a supplied by an input time-division circuit 12a.
Each row of the memory 7a can contain a speech sample, such a sample being made of eight bits.
Each speech sample received from circuit 12a is then stored in a given row of speech memory 7A under control of the time monitor circuit 8a. The address of each given row is conventionally stored in a row of the control memory 4a, to the corresponding storage being performed by a network processing computer 5 which may be selected from among conventional processors used for switching systems. Exemplary computers are the ITT 1600 and ITT 3200 which were designed specifically for use with switching systems, as demonstrated in Pat. Nos. 3,557,315 and 3,562,716 as well as in the literature, as described in Electrical Communication, volume 46, number 4, 1971, pages 233 - 245. Addresses are sequentially read from memory 4a under control of pulse supplied from network clock 6, via a connection indicated by "h".
Memories 4a and 7a are respectively provided with output registers 9a and 10a controlled by clock 6, via connections h. Register 9a and circuit 12a actuate memory 7a, via an OR-type circuit 11a.
Any address read from control memory 4a is transferred to register 9a which addresses the corresponding row of memory 7a. The sample, which arbitrarily may be designated "E", contained in the addressed row of 7a, is transmitted via the register 10a to be transferred again, via the space division network 2 towards the concerned output time-division group, for instance to group 3a.
In this respect, it is necessary to find a propagation path connecting register 10a to input register 21b of group 3b, via the three stages of switch 2.
In a conventional manner, addresses of concerned crosspoints which determine the sample propagation path, are provided from the concerned computer 5. Those crosspoint addresses are stored in a space-address memory pertaining to each input time-division group, such as 13a for group 1a.
Memory 13a is associated to speech memory 7a and comprises as many columns as bits needed for addressing sample propagation path crosspoints through space-division network 2.
In the described embodiment, the first space-division stage of network 2 includes sixteen matrices, each matrix having eight input links and sixteen output links. The second space-division stage includes sixteen matrices, each matrix having sixteen input links and sixteen output links. The third space-division stage includes sixteen matrices, each matrix having sixteen input links and eight output links. Each input link of the first stage is associated to an input time-division group 1a, so that there may be, for example, 128 input time-division groups, which corresponds to half the number of time-division network elemetary times that in this example would be 256.
Thus, each input link of the first stage may be connected to sixteen output links of the same stage through sixteen crosspoints, so that four bits are needed for use in addressing one crosspoint out of sixteen available for establishing such a connection. Likewise, each input of the second stage may be connected to sixteen output links and crosspoint addressing needs four bits. However only three bits are needed for addressing crosspoints in the third stage, or for use in connecting one input link to one output link out of eight.
Therefore, each row of crosspoint address memory 13a may contain 4 + 4 + 3 = 11 bits.
To each row of speech memory 7a there is associated a row of the space address memory 13a. Memory 13a contains addresses of crosspoints determining the propagation path for a speech sample such as E above stored in the corresponding row of memory 7a.
Any time-division address provided from control memory 4a triggers simultaneous transfers, on the one hand, of the sample stored in the row designated by that address in speech memory 7a and, on the other hand, of space addresses stored in the corresponding row of the associated memory 13a. Then, the speech sample is written in output register 10a and corresponding crosspoint addresses written in a register 14a, which is divided in three portions, which are respectively alloted to addresses, which are not illustrated in the Figures but may be designated AS 1 , AS 2 and AS 3 , for each of the three space-division stages, respectively.
The two registers 10a and 14a are sequentially controlled by clock 6, via connections h, clock 6 delivering control signals particularly at times t spaced by T/2, T being the network elementary time duration.
In the described embodiment, network elementary times T are then divided into two operation times. Register 14a is first controlled at the beginning of a time t n corresponding to the beginning of a network elementary time T n (FIG. 2). Bits contained in register 14a are transmitted through eleven outputs. The four first outputs corresponding to address AS1 of the first crosspoint 27a involved in the propagation of sample E, supply the four inputs of an addressing register 18a associated to the input link which group 1a is connected to. Thus, register 18a receives the four bits corresponding to the address of that crosspoint 27a and triggers its operation controlled by clock 6.
Since each input link of the first stage is associated to an addressing register, that first stage includes 128 addressing registers 18, each being respectively connected by four inputs to one of the output registers 14 of one of the 128 input time-division groups.
Simultaneously, during time t n , addresses AS2 and AS3 of crosspoints in the second and third stages are transmitted to a transfer register 15a associated to the considered input link. Thus, there are also 128 transfer registers for the 128 input links of the first stage in the described embodiment.
Transfer register 15a has a capacity equal, at least, to speech sample bit number. It has seven of its eight inputs connected to the seven remaining outputs of register 14a, so as to receive the seven bits corresponding to second and third stage crosspoint addresses.
At time t n +1 , speech sample E is in register 10a, the first concerned crosspoint 27a is activated and addresses of the two other concerned crosspoints are stored in registr 15a (FIG. 2).
Then, clock 6 simultaneously triggers, during time t n +1 , on the one hand, the transfer of addresses AS2 and AS3 of the two unoperative concerned crosspoints, via the first crosspoint 27a, and, on the other hand, the transfer of sample E to register 15a.
In this respect, register 15a has its eight inputs connected to the eight outputs of register 10a.
At time t n +2 (FIG. 2), sample E is stored in 15a, the first crosspoint 27a is still operative, addresses AS2 and AS3 of the two further crosspoints are stored in a second transfer register 16a connected to outputs of crosspoint 27a. Moreover, the four bits of the address of the second stage crosspoint are also stored in an addressing register 19a connected to the corresponding outputs of crosspoint 27a.
In this respect, each first stage crosspoint has, on the one hand, four outputs connected to an addressing register 19 and, on the other hand, its eight outputs connected to the eight inputs of a transfer register 16.
Thus, the second stage includes 256 input transfer registers and 256 addressing registers.
During time t n +2 , addresses AS2 and AS3 are transferred via the second concerned operative crosspoint, i.e. 28a, and sample E is transferred to register 16a, via 27a.
At time t n +3 (FIG. 2), sample E is stored in 16a, the second crosspoint 28a is activated, addresses AS2 and AS3 are stored in a third transfer register 17a connected to the eight outputs of crosspoint 28a and, in addition, address AS3 is stored in an addressing register 20a connected to the three concerned outputs of crosspoint 28a.
Thus, the third stage includes 256 input transfer registers and 256 addressing registers.
During time t n +3 , sample E is transferred, via crosspoint 28a, to register 17a and the third concerned crosspoint 29b is activated. Conversely, addresses AS2 and AS3 are expelled from register 17a by sample E and are not further transmitted because register 21a is not controlled by clock 6.
At time t n +4 or T n +2 , sample E is stored in 17a, the third point 29b is being activated, clock 6 triggers the transfer of sample E to transfer register 21b connected to the eight outputs of crosspoint 29b. Thus, the third stage has also 128 output transfer registers.
During time t n +5 , sample E is transferred from register 21b to input register 30b of output time-division group 3b.
Outgoing groups, such as 3b, are conventional and, for instance the group 3b basically includes a control memory 22b with its output register 23b, a speech memory 24b with its input registers 30b and output registers 25b, and an output time-division circuit 26b.
Transmission operations through that group are conventional and will not be further described hereinafter, as being well known to those skilled in the art.
In a conventional manner, each time-division group operates in a separate manner, under the control of the network clock 6 and, as a result, simultaneous transfers of 128 speech sample may occur at the same time and at the same propagation step, i.e. transfers of 128 samples from input time-division group outgoing registers to first space stage input transfer registers.
Likewise, as shown in the diagram of FIG. 2, the transfer of the binary data comprising a speech sample and concerned crosspoint addresses may be initiated at the beginning of each elementary time T.
Furthermore, the memory capacity needed for addressing crosspoints is reduced if compared to that of a network including a memory for crosspoint addresses per output stage link. Indeed, according to this invention, in the described embodiment, each of the 128 ingoing time-division groups includes a crosspoint address memory with 128 rows, each row having 11 bits. The necessary memory capacity is then of 128 2 (4+4+3) = 180(10) 3 bits or of 360(10) 3 bits, if speech sample memories are duplicated for safety reasons.
In the case of a network including a crosspoint address memory per output stage link, the need would be in fact:
16 × 16 × 256 × 3 No. 197(10).sup. 3 bits for the first stage comprising 16 16-output 8-input matrices, that is therefore 256 memories with 256 memories with 256 3-bit rows;
16 × 16 × 4 No. 262(10) 3 bits for the second stage comprising 16 16-output 16-input matrices, that is therefore 256 memories with 256 3-bit rows;
16 × 8 × 256 × 4 No. 131(10) 3 bits for the third stage comprising 16 8-output 16 input matrices, that is therefore 128 memories with 256 4-bit rows;
that is a total address memory capacity of more than 590(10) 3 bits, instead of 360(10) 3 bits.
While the principles of the present invention have hereabove been described in relation with a specific embodiment, it must be clearly understood that the said description has only been made by way of example and does not limit the scope of this invention.
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In a large time-space-time division switching network, particularly one employing a multistage space-division switch, one time-division elementary time is too brief to enable transmission of addresses of crosspoints to be completed through all the stages of the multistage switch, and also provide for transmission of the speech sample. To cope with this situation, two successive network elementary times are used, each elementary time being divied into two half-times, i.e., a first half-time and a second half-time. First half-times are used for transmitting addresses of crosspoints to be closed immediately. Second half-times are used for storing data concerning further crosspoint addresses plus a speech sample. Addresses are propagated through a speech sample path according to a "staggered operation", thereby reducing the requirements for memory dedicated to crosspoint addresses.
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CROSS-REFERENCES TO THE RELATED APPLICATIONS
This application is a division of application Ser. No. 08/247,240, filed May 23, 1994, now abandoned, which is a continuation-in-part of U.S. patent application Ser. No. 08/021,333 filed on Feb. 23, 1993.
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to a semiconductor device, such as a thin-film transistor, having in its main part a polysilicon thin film for transferring carriers.
2. Description of the Related Art
A technique of forming a thin-film transistor on an insulating substrate is known in the field of active matrix liquid crystal displays (LCDs). The technique allows a semiconductor integrated circuit to be formed on a transparent insulating substrate formed of, for example, glass, or a large insulating substrate which cannot be formed of a monocrystalline semiconductor. At present, a thin-film transistor generally includes an active layer made of amorphous silicon o r polysilicon. Since amorphous silicon can be formed at a low temperature, it is applicable to an active matrix LCD which must be formed on a glass substrate having a low melting point.
However, since amorphous silicon has a low electron mobility, it has been used only as a switching element for charging a pixel capacitor electrode to apply an electric field to a liquid crystal. An active layer made of polysilicon must be used in a circuit element, e.g., a driver circuit, a ROM, a RAM or a CPU, which must be driven at a high speed. For example, a driver circuit of a high-quality, large-screen liquid crystal TV or a high-definition office automation (OA) liquid crystal display panel is driven at a clock frequency of about 10 MHz. If such a driver circuit is formed of a semiconductor device, a field effect mobility μ FE of 50 cm 2 /V·sec or more, preferably 80 cm 2 /V·sec or more is required. However, the field effect mobility μ FE of a polysilicon thin-film transistor known to the public at present is at most 30 cm 2 /v·sec.
SUMMARY OF THE INVENTION
It is accordingly an object of the present invention to provide a semiconductor device which allows the mobility of carriers to greatly increase. To achieve the object, the semiconductor device of the present invention has a polysilicon thin film in its main part, wherein a grain size is substantially the same as a crystallite size on the (111) plane and the crystallite size is greater than a thickness of the polysilicon thin film (EPC: 180 nm or greater).
Additional objects and advantages of the invention will be set forth in the description which follows, and in part will be obvious from the description, or may be learned by practice of the invention. The objects and advantages of the invention may be realized and obtained by means of the instrumentalities and combinations particularly pointed out in the appended claims.
BRIEF DESCRIPTION OF THE DRAWINGS
accompanying drawings, which are incorporated in and constitute a part of the specification, illustrate presently preferred embodiments of the invention, and together with the general description given above and the detailed description of the preferred embodiments given below, serve to explain the principles of the invention.
FIGS. 1 to 6 are enlarged cross-sectional views showing the steps of manufacturing a field effect thin-film transistor as an embodiment of a semiconductor device according to the present invention;
FIG. 7 is a schematic diagram for explaining the definition of a grain size;
FIG. 8 is a diagram for explaining crystallography by an X ray diffractor;
FIG. 9A is a graph showing the grain size-field effect mobility characteristic of the thin-film transistor shown in FIG. 6;
FIG. 9B is a graph showing the crystal size-field effect mobility characteristic of the thin-film transistor shown in FIG. 6;
FIG. 10 is a graph showing the grain size-crystallite size characteristic of the thin-film transistor shown in FIG. 6;
FIG. 11 is a graph showing the surface anisotropy of the intensity of an X-ray diffraction; and
FIG. 12 is a graph showing the peak intensity of an X-ray diffraction and intensities near the peak of a specified plane.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
Basic Concept of the Invention
It has been considered that the field effect mobility μ FE of a polysilicon thin-film transistor is determined by grain sizes of silicon crystals constituting an active layer, i.e. a polysilicon thin film. Although there is another determinant such as a trap of carriers which may be caused depending on the state of an interface between the polysilicon thin film and a gate insulating film, it has been considered important to form large and uniform grains, as far as the crystal structure is concerned. Under these circumstances, techniques for an enhancement of the electron mobility by increasing the size and the uniformness of grains have been studied. However, the present inventor discovered throughout his research that it is difficult to enhance the electron mobility only by increasing the grain size of a polysilicon thin film. According to the inventor's research, the electron mobility was not increased beyond a predetermined value however the grain size is increased, whereas it was satisfactorily increased even when the grain size was not very large.
As a result of the research, the inventor found that the crystallite size, as well as the grain size, must be increased to enhance the field effect mobility μ FE of a thin-film transistor having a polysilicon thin film as an active layer. It is desirable that the grain size and the crystallite size are substantially the same. In addition, the mobility was further increased when the grain size and the crystallite size were greater than the thickness of the polysilicon thin film. This appears to result from the monocrystallization effect due to the state that crystallites having a size regarded as a substantially perfect monocrystal region occupy the main region of the grain and decrease the crystal defects in the grain.
An embodiment of the present invention will be described in detail.
Embodiment
FIGS. 1 to 6 show the steps of manufacturing a thin-film transistor according to an embodiment of the present invention. The structure of the thin-film transistor and a method of manufacturing the same will now be described with reference to these drawings in sequence.
First, as shown in FIG. 1, an amorphous silicon thin film 2 is deposited on the upper surface of an insulating substrate 1 made of quartz or the like by an LP-CVD (Low Pressure Chemical Vapor Deposition) method at a temperature of 550° C. Thereafter, as shown in FIG. 2, XeCl excimer laser beams are applied to the substrate, thereby polycrystallizing the amorphous silicon thin film 2 into a polysilicon thin film 3 by a liquid-phase growth. The crystal structure of the poly-silicon thin film 3 in this state will be described later. Then, as shown in FIG. 3, a photoresist film 5 is formed on the upper surface of the polysilicon thin film 3, and patterned not to leave on the regions of film 3 which correspond to source and drain forming regions 4. Using the photoresist film 5 as a mask, impurities such as phosphorus ions or boron ions are injected to a high concentration into the source and drain forming regions 4 of the polysilicon thin film 3, thereby forming impurity-injected regions 6. Thereafter, the photoresist film 5 is removed. Next, as shown in FIG. 4, XeCl excimer laser beams are applied to the polysilicon thin film 3 again to activate the impurities injected in the regions 6. Then, as shown in FIG. 5, an unneeded peripheral portion of the poly-silicon thin film 3 is removed. A central portion of the polysilicon thin film 3 serves as a channel region 3a, and side portions thereof a source and drain regions 3b formed of activated impurity regions. Subsequently, as shown in FIG. 6, a gate-insulating film 7 formed of a silicon oxide film and the like is formed on the upper surface of the assembly. Thereafter, a gate electrode 8 made of chrome and the like is formed on the upper surface of a portion of the gate insulating film 7 which corresponds to the channel region 3a, by means of a depositing and a patterning. Thereafter, a passivating insulating film 9 made of silicon nitride or the like is formed on the entire upper surface of the assembly. Then, contact holes 10 are formed in those portions of the passivating insulating film 9 and the gate-insulating film 7 which correspond to the source and drain regions 3b. Subsequently, source and drain electrodes 11 made of aluminum and the like are patterned on the passivating insulating film 9 and connected to the source and drain regions 3b through the contact holes 10 are formed on the passivating insulating film 9 and in the holes 10. Thus, a field effect thin-film transistor of a coplanar type is obtained.
The crystal structure of the polysilicon thin film 3 shown in FIG. 2 will now be described with reference to Table 1.
TABLE 1______________________________________Sample: LPCVDThickness of silicon film: 500Å GrainPolycrystal- Mobility size Crystallitelizing method (μ.sub.FE) (C) B size (hkl)______________________________________Embodiment of Present InventionLaser anneal 90 cm.sup.2 /V · sec 246 nm (111)XeCl excimer 202 nmlaser (220)250° C., 144 nm300 mJ/cm.sup.2 Liquid-phase (311)growth! 103 nmPrior ArtHeat 30 cm.sup.2 /V · sec 1.2 μm (111)treatment 37 nm600° C. (220)48 hours 23 nm Solid-phase (311)growth! 36 nm______________________________________
As shown in Table 1, a polysilicon thin film according to an embodiment of the present invention was prepared in the following manner: an amorphous silicon thin film having a thickness of about 500Å was deposited on the upper surface of a quartz substrate, and XeCl excimer laser beams were applied twice to the amorphous silicon thin film at a temperature of about 250° C. under an energy density of about 300 mJ/cm 2 , so that the amorphous silicon thin film was polycrystallized in a liquid-phase growth, to obtain a polysilicon thin film. To compare the present embodiment with a conventional device, a polysilicon thin film according to conventional art was prepared in the following manner: an amorphous silicon thin film having a thickness of about 500Å was deposited on the upper surface of a quartz substrate; the substrate was heated in a nitrogen atmosphere at a temperature of about 600° C. for 48 hours, so that the amorphous silicon thin film was polycrystallized in a solid-phase growth, to obtain a polysilicon thin film.
The crystal structure were analyzed by using a (Transmission Electron Microscope) and an XD (X-ray Diffractor analysis). In case of the TEM, grain size was measured with JEM-2010 of JEOL (acceleration voltage: 200 kV, magnification: 5×10 5 to 1.5×10 6 ). The grain size of the embodiment was 246 nm, whereas the grain size of the prior art was 1.2 μm, which is 5 times greater than the grain size of the embodiment. The grain size refers to the size of a grain in the top view of the polysilicon thin film, and is represented by an average value of the total of average values c of size of grains obtained by the following equation: c=(a+b)/2, where a denotes the length of a grain along the major axis and b denotes the length of the grain along the minor axis, for example, as shown in FIG. 7. Each grain size C indicated in Table 1 is an average calculated based on the measured values at 30 points.
The crystallite size by use of the XD was measured by detecting a diffraction intensity by using a low angle incidence method, wherein θ'=1°. The crystallite size was measured with RU-200 of Rigaku Denki Company (radiation source: CuKa, maximum output: 12 kW) under the conditions of the incident X-ray intensity of 50 kV and the power of 180 mW. FIG. 11 is a graph showing the X-ray intensity in a range of 2θ between 20° and 120°. As clearly shown in FIG. 11, the peak intensities on the (111), (220) and (311) planes are greater than those on the other planes. The peak intensities on the (620), (533), (444), (711), (642) and (731) planes in a range of 2θ between 120° and 159° were also measured. However, a definite peak on each of these planes was not detected and the peak intensity on the (111) plane was the greatest.
As shown in FIG. 11, the peak intensities on the planes other than the (111), (220) and (311) planes were very weak and greatly influenced by noise. Therefore, the intensity was measured three times by step scanning for 2 seconds with a rotational angle of 0.01° within a range of ±1.5° on each of the peak planes. the result of this measurement is shown in FIG. 12. As clearly shown in FIG. 12, the volume of the (111) plane is the greatest.
The crystallite size was calculated from the peak width at half height by use of the following equation of Scherrer.
D.sub.hkl =λ/(B·cos θB)
where D hkl denotes a crystallite size in a direction perpendicular to the (hkl) plane; λ, a wavelength of an X-ray beam; B, a half width; and θB, a Bragg's angle. The results of the measurement are shown in Table 1. In the conventional device, the average values of the crystallite size measured in the three-time measurement were 37 nm on the (111) plane, 23 nm on the (220) plane, and 36 nm on the (311) plane, whereas in the present embodiment, the average values were much greater than in the conventional device, i.e., 202 nm on the (111) plane, 144 nm on the (220) plane, and 103 nm on the (311) plane.
Coplanar type field effect thin-film transistors as shown in FIG. 6 were manufactured using the thin films of the embodiment and the conventional art, and the field effect mobilities μ FE thereof were measured. As shown in Table 1, the mobility in the conventional thin-film transistor was 30 cm 2 /V·sec, whereas the mobility in the thin-film transistor of the present embodiment was 90 cm 2 /V·sec, which is three times greater than that of the conventional transistor. The measurement result represents that the field effect mobility μ FE is correlated to the crystallite size rather than the grain size. This appears to be based on the fact that a thin-film transistor wherein the grain size is large and the crystallite size is small includes a number of crystal defects, while a thin-film transistor wherein the crystallite size is substantially the same as the grain size includes few crystal defects, even if the grain size is small, since the crystallite is regarded as a complete monocrystal region.
To confirm this, a similar measurement was performed with respect to a number of samples according to the embodiment. FIGS. 9A, 9B, and 10 show results of the measurement. Although the sample indicated in Table 1 includes an amorphous silicon film deposited on the substrate to a thickness of 500Å by a LPCVD method, some of the samples indicated in FIGS. 9A, 9B, and 10 are formed by a plasma CVD method or have various thicknesses (500 to 3000Å). FIG. 9A shows the relationship between grain size C and field effect mobility μ FE , and FIG. 9B shows the relationship between crystallite size and field effect mobility μ FE on the (111) plane. FIG. 10 shows the relationship between a grain size and a crystallite size on the (111) plane. Although a crystal size measured by a low-angle incidence method must be corrected, the values of the crystallite size indicated in FIGS. 9B and 10 are calculated by the equation of Scherrer and uncorrected. As shown in FIG. 9A, there is a specific correlation between the grain size C and the field effect mobility μ FE - Further, as shown in FIG. 9B, there is a specific correlation between the crystallite size on the (111) plane and the field effect mobility μ FE . Conditions for the correlations can be understood from FIG. 10. The broken line in FIG. 10, which makes an angle of 45° with the abscissa, represents a characteristic that the ratio of a crystallite size to a grain size is 1:1. As is obvious from FIG. 10, crystallite size approximates the grain size. In the range that the grain size is 100 nm or smaller, it is substantially the same as the crystallite size. In the range that the grain size is greater than 100 nm, the ratio of the crystallite size to the grain size is slightly smaller than 1. In case that the size is about 300 nm, the crystallite size is about 60 to 70% of the grain size. If a thin film having the crystallite size the same as the grain size in the range of 200 to 300 nm or greater of the grain size by improving the manufacturing method is obtained, the field effect mobility μ FE can be further increased.
It is clear from FIGS. 9A and 9B that the crystallite size of about 180 nm (measured value) or greater and the grain size C of about 200 nm or greater suffice to obtain a field effect mobility μ FE of about 80 cm 2 /V·sec. If these conditions are satisfied, a field effect thin-film transistor having a field effect mobility μ FE of about 80 cm 2 /V·sec can be obtained. Accordingly, it is possible to form, using a semiconductor device, a driver circuit which is operated with a clock frequency of about 10 MHz. Conventionally, it has been considered that the field effect mobility μ FE increases in proportion to the grain size C. However, the conventional idea, in which the crystallite size is not taken into account, is clearly incorrect in view of Table1.
Further, referring to Table 1, the crystallite sizes on the (111), (220), and (311) planes of the embodiment are respectively 202 nm, 144 nm, and 103 nm, which are all greater than the thickness of the polysilicon thin film, i.e., 500Å. In contrast, in the conventional device, the crystallite size on the (111) plane, i.e. the maximum peak plane, is 37 nm which is smaller than the thickness of the polysilicon thin film, 500Å. This proves that the field effect mobility μ FE can be more greatly increased than in the conventional device, if the crystallite size of the polysilicon thin film is greater than the thickness of the polysilicon thin film. According to the embodiment, since the thickness of the polysilicon thin film is 500 to 3000Å, the field effect mobility μ FE of at least 50 cm 2 /V·sec is ensured.
The polysilicon thin film can have a thickness of 500 to 1500Å.
The present invention is not limited to a field effect thin-film transistor, but is applicable to any type of semiconductor device having a polysilicon thin film as its main part to transfer carriers.
As has been described above, if a polysilicon thin film has a grain size and a crystallite size which are substantially the same, the field effect mobility μ FE can be greatly increased, accordingly, a driver circuit which is operated with a clock frequency of about 10 MHz can be formed using a semiconductor device. Note that when the crystallite size is 60 to 70% or greater of the grain size, these sizes are considered to be "substantially the same".
Additional advantages and modifications will readily occur to those skilled in the art. Therefore, the invention in its broader aspects is not limited to the specific details, and representative devices, shown and described herein. Accordingly, various modifications may be made without departing from the spirit or scope of the general inventive concept as defined by the appended claims and their equivalents.
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A method of preparing a semiconductor device, comprising: forming an amorphous silicon layer on a substrate, and applying shots of an excimer laser beam to the amorphous silicon layer to convert the amorphous silicon layer into a polysilicon layer having a plurality of silicon grains, each of the grains having a grain size and including a crystallite having a crystallite size on the (111) plane, an average value of the crystallite sizes on the (111) plane of the crystallites included in the polysilicon layer being sixty percent or greater of an average value of the grain size.
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RELATED APPLICATION
The present-application is a continuation application of U.S. Ser. No. 13/804,000, filed Mar. 14, 2013, which claims the benefit of U.S. Provisional Application No. 61/613,770, filed Mar. 21, 2012, and entitled “AUTOMATED IMPLANTABLE PENILE PROSTHESIS PUMP SYSTEM”, which are incorporated herein by reference in their entireties.
FIELD OF THE INVENTION
The present invention is generally directed to a pump system for an implantable penile prosthesis. Specifically, the present invention is directed to a suction poppet assembly for an implantable penile prosthesis pump system.
BACKGROUND OF THE INVENTION
Implantation of an implantable penile prosthesis (IPP) is a common surgical procedure for treating erectile dysfunction and other penile ailments. An IPP comprises an inflatable cylinder connected by a pump to a separate reservoir for holding the quantity of fill liquid via kink resistant tubing. This version of the IPP is available under the trade name AMBICOR from American Medical Systems of Minnetonka, Minn. Typically, the entire IPP is implanted into the patient's body with the inflatable cylinder being placed in the corpus cavernosum and the pump being placed within the scrotum. The reservoir can also be placed within the scrotum or placed elsewhere within the pelvic region. To operate the IPP, the pump is manually actuated to transfer fill liquid from the integrated or implanted reservoir into the inflatable cylinder to fill and pressurize the inflatable cylinder.
A typical pump system for an IPP comprises a pump bulb that can be compressed to draw fluid from a reservoir and push the inflation fluid into the inflatable cylinder. Generally, the pump is compressed and released to draw fluid from the reservoir into the pump. The pump is compressed again to force fluid from the pump into the inflatable cylinder. Two selective poppet valves are positioned along the flow path between reservoir and inflatable cylinder to control the direction of the fluid flow through the pump system.
Typically, the IPP and the pump system are provided to the medical personnel without any working fluid within the system. Prior to implantation, each component of the IPP is filled or nearly filed with the working fluid by the medical personnel. The medical personnel also often test the operation of the IPP to insure that the all the components of the IPP are functioning properly prior to implantation. However, if too much air remains in the IPP when the pump system is operated by the medical personnel or the patient, the air within the system can cause pump to lock up. Specifically, the pump bulb can remain compressed after being actuated rather than re-expanding to draw additional fluid into the pump bulb.
Another drawback of the pump system is that the poppet valves can become misaligned during filling and operation of the IPP and pump system. If the poppet becomes misaligned, uncontrolled leakage can occur allowing fluid to travel through the fluid pathway. Similarly, the misaligned poppet can become stuck preventing any operation of the poppet.
As such, there is a need for a pump system for an IPP that can be operated by medical personnel with a reduced risk of damage or malfunction during test operation.
SUMMARY OF THE INVENTION
The present invention is directed to an IPP having a valve assembly comprising a dual poppet design. The valve assembly is integrated into a pump assembly comprising a pump bulb that can be actuated to transfer working fluid from a reservoir to at least one inflatable cylinder. The valve assembly defines a valve flow path, for example, a generally linear flow path, between the reservoir and the inflatable cylinder. The valve flow path intersects the opening to the pump bulb such that actuating the pump bulb moves fluid along the flow path. In one aspect, the valve flow path also defines a suction annulus positioned in the valve flow path between the reservoir and the pump bulb. Similarly, the valve flow path can also define a cylinder annulus positioned between the pump bulb and the cylinder.
In one aspect, the valve assembly comprises a suction poppet engagable to the suction annulus and a cylinder poppet engagable to the cylinder annulus. Each poppet is movable along a central axis defined by the flow path between an engaged position in which the poppet is engaged to its corresponding annulus to prevent the flow of working fluid through the annulus and a disengaged positioned wherein the poppet is positioned to allow working fluid to pass through the corresponding annulus. In one aspect, the poppets are both biased to the engaged position to prevent flow of working fluid until the pump bulb is actuated. The suction poppet is positioned on the pump bulb side of the suction annulus such that releasing the compressed pump bulb creates a suction that pulls the suction poppet into the disengaged position and draws a quantity of working fluid through the suction annulus into the pump bulb. In contrast, the cylinder poppet is positioned on the opposite side of the cylinder annulus from the pump bulb, wherein compressing the pump bulb creates a positive pressure pushing the cylinder poppet into the disengaged position and a forcing a quantity of working fluid through the cylinder annulus into the inflatable cylinder.
In one aspect, the flow path further defines an annular ring positioned between the suction annulus and the pump bulb opening. If the pump bulb is actuated too quickly and/or air is present within the pump bulb opening such as, for example, during the initial installation, the suction poppet can become wedged against the annular ring blocking all flow and creating a vacuum condition essentially locking the pump bulb in the compressed state. In one aspect, the suction poppet can further comprise a head extending through the suction annulus. The head can define a lip engagable by a plurality of fingers extending from the suction annulus. The fingers engage the lip when the suction poppet is slid into the disengaged position to prevent the suction poppet from engaging the annular ring and creating vacuum lock up. The fingers allow for a controlled travel distance of the suction poppet preventing vacuum lock up of the pump bulb.
In one aspect, the suction puppet can further comprise an elongated suction poppet shaft extending through the cylinder annulus. In this configuration, a cylinder poppet can define defines a cylinder poppet bore for slidably receiving the elongated suction poppet shaft. If the suction poppet becomes misaligned, the suction poppet may not properly engage the suction annulus allowing working fluid to leak through the suction annulus. The cylinder poppet bore guides the suction poppet to maintain an axial alignment of the suction poppet along a valve chamber axis as the suction poppet moves between the engaged position and the disengaged position relative to suction annulus.
In one aspect, the valve assembly can further comprise a release button that can be pressed against an elongated head of the suction poppet to push the suction poppet to the disengaged position along the valve chamber axis without operating the pump bulb. The elongated suction poppet shaft can be used to push against an end of the cylinder poppet bore such that both the suction poppet and the cylinder poppet are positioned in the disengaged position allowing free flow through the valve flow path. The release button can be used to return the working fluid to the reservoir from the inflatable cylinder. The release button can also be used to reset the operation of the valve assembly.
A method of preventing vacuum lock up of the pump bulb, according to an aspect of the present invention, can comprise providing a suction poppet positioned between the suction annulus leading to the reservoir and the pump bulb, wherein the suction poppet further comprises an elongated head extending through the suction annulus. The method can further comprise defining a plurality of fingers extending from the suction annulus to limit the travel distance of the suction poppet and prevent uncontrolled engagement of the suction poppet to other features within the valve assembly.
The above summary of the various representative embodiments of the invention is not intended to describe each illustrated embodiment or every implementation of the invention. Rather, the embodiments are chosen and described so that others skilled in the art can appreciate and understand the principles and practices of the invention. The figures in the detailed description that follow more particularly exemplify these embodiments.
BRIEF DESCRIPTION OF THE DRAWINGS
The invention can be completely understood in consideration of the following detailed description of various embodiments of the invention in connection with the accompanying drawings, in which:
FIG. 1 is a top view of a implantable penile prosthesis according to an embodiment of the present invention.
FIG. 2 is a partial cross-sectional view of a valve assembly according to an embodiment of the present invention.
FIG. 3 is a side view of a suction poppet according to an embodiment of the present invention.
FIG. 4 is a perspective view of a suction annulus with a head of the suction poppet extending through annulus according to an embodiment of the present invention.
While the invention is amenable to various modifications and alternative forms, specifics thereof have been shown by way of example in the drawings and will be described in detail. It should be understood, however, that the intention is not to limit the invention to the particular embodiments described. 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.
DETAILED DESCRIPTION
As shown in FIG. 1 , an implantable penile prosthesis (IPP) 2 , according to an embodiment of the present invention, comprises at least one inflatable cylinder 4 , a reservoir 6 , a pump 8 and a valve assembly 10 . The pump 8 can further comprise a pump bulb 12 that can be compressed and released to draw and pump working fluid. The IPP 2 generally operates by actuating the pump bulb 12 to draw a quantity of working fluid from the reservoir 6 and pumping the working fluid into the inflatable cylinder 4 . The valve assembly 10 is generally adapted to prevent back flow of the working fluid during operation of the pump 8 to inflate inflatable cylinder 4 .
As shown in FIGS. 1-2 , the valve assembly 10 defines a valve flow path 14 and comprises a suction poppet 16 and a cylinder poppet 18 . The valve flow path 14 is defined between a reservoir inlet 20 from the reservoir 6 and a cylinder outlet 22 leading to the cylinder 4 . The valve flow path 14 also further comprises a linear valve chamber 24 extending along a central valve chamber axis a-a. The linear valve chamber 24 defines a pump bulb opening 26 providing fluid communication between the pump bulb 12 and the linear valve chamber 24 . The linear valve chamber 24 also defines a suction annulus 28 and an annular ring 30 positioned between the reservoir inlet 20 and the pump bulb opening 26 . Similarly, the linear valve chamber 24 also defines a cylinder annulus 32 positioned between the pump bulb opening 26 and the cylinder outlet 32 . In one aspect, the suction annulus 28 further comprises a plurality of fingers 34 as shown in FIG. 4 that extend radially toward the central valve chamber axis a-a.
As shown in FIGS. 2-3 , the suction poppet 16 defines a sealing surface 36 and is linearly movable along the central valve chamber axis a-a between an engaged position and a disengaged positioned. In the engaged position, the sealing surface 36 is engaged to the suction annulus 28 preventing flow of working fluid through the suction annulus 28 . In the disengaged positioned, the sealing surface 36 is disengaged from the suction annulus 28 allowing working fluid to pass through the suction annulus 28 . As shown in FIGS. 2-3 , the suction poppet 16 is positioned on the pump bulb opening 26 side of the suction annulus 28 such that the suction poppet 16 is biased to maintain flow in a single direction during inflation of the cylinders 4 . In one aspect, the suction poppet 16 further comprises a suction poppet spring 38 maintaining the suction poppet 16 in the engaged position to prevent flow through the valve flow path 14 without operation of the pump bulb 12 .
In one aspect, the suction poppet 16 further comprises an elongated head 40 extending through the suction annulus 28 and defining a lip 42 engagable by the plurality of fingers 34 when the suction poppet 16 moves toward the disengaged position limiting the travel distance of the suction poppet 16 and preventing the suction poppet 16 from engaging the annular ring 30 .
As shown in FIG. 2 , the cylinder poppet 18 also defines a sealing surface 44 engagable to the cylinder annulus 32 . The cylinder poppet 18 is also movable along the central valve chamber axis a-a between an engaged position in which the sealing surface 44 is engaged to the cylinder annulus 32 preventing flow of working fluid through the cylinder annulus 32 and a disengaged positioned allowing working fluid to pass through the annulus 32 . As shown in FIG. 2 , the cylinder poppet 18 is positioned on the cylinder outlet 22 side of the cylinder annulus 32 such that the cylinder poppet 18 is biased to maintain a flow direction from the reservoir 6 to the cylinder 4 during normal operation. In one aspect, the cylinder poppet 18 further comprises a cylinder poppet spring 45 to maintain the suction poppet 16 in the engaged position to prevent flow through the valve flow path 14 without operation of the pump bulb 12 .
In one aspect, the cylinder poppet 18 further comprises an elongated cylinder poppet shaft 46 and defines a lip 48 . In this configuration, the valve flow path 14 further defines a cylinder journal 50 defining a journal bore 52 for receiving the elongated cylinder poppet shaft 46 . The journal bore 52 guides the cylinder poppet 18 along the central valve chamber axis a-a during movement of the cylinder poppet 18 between the engaged and disengaged position such that the cylinder poppet 18 is prevented from moving along an axis transverse to the central valve chamber axis a-a. The cylinder journal 50 also engages the lip 48 of the cylinder poppet 18 when the poppet 18 moves to the disengaged position to limit the travel of the cylinder poppet 18 .
In one aspect, the suction poppet 16 can further comprise an elongated suction poppet shaft 54 extending through the cylinder annulus 32 . In this configuration the cylinder poppet 18 further defines a cylinder poppet bore 56 for receiving the elongated suction poppet shaft 54 . The cylinder poppet bore 56 guides the elongated suction poppet shaft 54 along the central valve chamber axis a-a during movement of the suction poppet 16 between the engaged and disengaged position such that the suction poppet 16 is prevented from moving along an axis transverse to the central valve chamber axis a-a. The elongated suction poppet shaft 54 can also be used to engage the end of the cylinder poppet bore 56 to push the cylinder poppet 18 into the disengaged position.
In operation, compressing the pump bulb 12 creates a positive pressure pushing working fluid and/or air within the pump bulb 12 out of the pump bulb opening 26 into the valve flow path 14 . The positive pressure also pushes against the cylinder poppet 18 moving the cylinder poppet 18 into the disengaged position forcing the fluid and/or air into the inflatable cylinder 4 . Releasing the compressed pump bulb 12 allows the pump bulb 12 to expand and creates a vacuum pulling the cylinder poppet 18 into the engaged position and the suction poppet 16 into the disengaged position allowing working fluid to be drawn from the reservoir 6 into the pump bulb 12 . The process can be repeated to continuously draw working fluid from the reservoir 6 to inflate the inflatable cylinder 4 .
In one aspect, the valve assembly 10 can further comprise a release button 58 for allowing fluid to flow in reverse through the valve flow path 14 . The release button 58 can be actuated to push against the elongated head 40 to push the suction poppet 16 into the disengaged position. In this configuration, the elongated suction poppet shaft 54 is adapted to engage the end of the cylinder poppet bore 56 to push the cylinder poppet 18 into the disengaged position. With both the suction poppet 16 and the cylinder poppet 18 are in the disengaged position with respect to the their corresponding annulus, the pressure of the working fluid within the inflatable cylinder 4 pushes working fluid through the valve flow path 14 back to the reservoir 6 .
As shown in FIG. 2 , a method of preventing vacuum lock up of the pump bulb 12 comprises positioning the suction poppet 16 positioned between the suction annulus 28 and the pump bulb 12 , wherein the suction poppet 16 further comprises an elongated head 40 extending through the suction annulus 28 . The method further comprises defining a plurality of fingers 34 extending from the suction annulus 28 to limit the travel distance of the suction poppet 16 to prevent uncontrolled engagement of the suction poppet 16 to other features within the valve assembly 10 .
While the invention is amenable to various modifications and alternative forms, specifics thereof have been shown by way of example in the drawings and described in detail. It is understood, however, that the intention is not to limit the invention to the particular embodiments described. 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.
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A dual poppet valve assembly for a pump assembly of an implantable penile prosthesis having a suction poppet engagable by a plurality of fingers allowing free travel of the poppet and to prevent vacuum lockup of the pump assembly. The suction poppet can also include an elongated shaft receivable within a corresponding bore of a cylinder poppet to prevent the suction poppet from becoming misaligned during the operation of the pump assembly.
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BACKGROUND OF THE INVENTION
The present invention relates to a flat gasket with filter elements.
In order to fulfil the increased requirements with respect to cleanliness, there is an increased demand for the integration of filter elements in flat gaskets. The corresponding filter elements mainly serve for picking of impurities accrued during production as well as other residues circulate via the operational fluids, especially during the initial period of operation of an internal combustion engine or a vehicle.
Such flat gaskets are already known from the state of the art, e.g. from DE 200 19 040 U1 or DE 20 2010 006 768 U1. They are mainly used as gaskets for parts which guide water, air and/or oil. This can be gaskets in transmissions, cylinder head gaskets or other gaskets in internal combustion engines and especially gaskets in the exhaust line of internal combustion engines.
DE 20 2010 006 768 U1 teaches a flat gasket with a metallic mesh material being installed between two metallic layers. The mesh material extends between the metallic layers and also spans the area of the passage openings in the metallic layers. In and for these passage openings, the mesh layer acts as a filter. According to DE 20 2010 006 768 U1, the mesh material is not compressed in these filter areas, while it is compressed in the bridge areas where it is covered by the material of the metallic layers. This compression causes a transverse impermeability of the mesh material in the respective areas, whereas the non-compressed mesh material in the filter areas shows a reduced flow resistance for the fluid which passes through the passage openings in the metallic layers.
It is disadvantageous that the mesh material has to be compressed with a demanding process in the areas to be covered by the metallic layers, namely the sealing areas, while the filter areas have to be protected from any compression. Such a structured and local compression method is demanding and causes considerable cost of production.
BRIEF SUMMARY OF THE INVENTION
It is therefore the object of the present invention to overcome this problem. It is thus the object of the present invention to provide for a metallic flat gasket as well as to its use, which gasket can easily be passed by the fluid in its filter regions, has a high transversal impermeability in the sealing areas and at the same time can be produced with low effort.
This object is solved by the metallic flat gasket according to claim 1 . The claims depending on claim 1 represent advantageous embodiments of the invention.
Claim 19 provides for advantageous uses of the metallic flat gasket according to the invention. These are especially given if the gasket is used as a transmission plate or a gasket for a transmission and in general as a gasket for parts which pass water, air, pressurized gas and/or oil, or other gaskets of an internal combustion engine, especially in the exhaust line of an internal combustion engine.
The invention thus provides for a flat gasket which comprises at least two metallic layers, thus two layers comprising a metal sheet or consisting of metal sheet. These metallic layers show passage openings which upon assembly of the gasket layers correspond to each other and are arranged adjacent to each other in a direction perpendicular to the planes of the gasket layers. Adjacent here means that the passage openings can be arranged directly one upon the other or indirectly, thus distanced to each other by at least one intermediate layer. These gaskets allow for the passage of fluids from one side of the passage opening to the opposite one, e.g. of hydraulic oil in a transmission or of air in pneumatic transmission actuator, of exhaust gases in gaskets in the exhaust gas recirculation area or of water in the supply gasket of a water pump. Apart from that, the gasket usually also shows passage openings for fastening means, especially for bolts and/or screws.
In both metallic layers, several passage openings are arranged vicinal to each other in the respective plane of the gasket layer with the respective passage openings in the different layers preferably being flush with each other or at least being continuous in the passage direction. These passage openings may be provided with a filter or may be designed in such a way that they allow for non-filtered passage of media. The present invention relates to a flat gasket with a mesh material which forms the filter element for such passage openings with filter.
Between the two metallic layers, a further, thus a third layer, is arranged according to the invention, which third layer in the area of the passage openings for the passage of fluids does not comprise a passage opening of its own but which spans these passage opening(s). In order to nevertheless allow for the passage of fluids, this third layer is designed as a sieve layer, which comprises a mesh material or consists of mesh material.
The mesh material comprises threads which cross each other while forming crossings. Preferably, the mesh material is a woven mesh material.
According to the invention, the height of the mesh material is reduced both in the filter regions and in the adjacent regions already covered by the metallic layers in such a manner that for all crossing points, the total height of two threads crossing each other in the centre of a crossing point is less than the 1.4 fold, preferably less than 1.2 fold of the height of an individual thread at half the distance between two neighbouring crossing points. In an advantageous embodiment, the entire mesh material of the sieve layer is formed in this way.
This means that the mesh material in the region of the passage openings and in the regions encircling the passage openings is compressed to 70%, preferably to 60%, of its initial thickness or less, with the compression preferably being realized over the complete area of the mesh material. This applies for the cases where the mesh material at least in the centre area between the crossing points of the threads is not compressed meaning that the threads at least in the centre area show their initial thickness. In case the mesh material is compressed to a higher degree, thus with the threads also being compressed in the centre area between the crossing points, the total height of two threads of the mesh at a crossing point equals the height of a thread in the centre area between two neighbouring crossing points.
Advantageously, the compressed mesh material shows a degree of compression of more than 30%, preferably more than 35%, preferably more than 40%, especially preferably more than 45% compared to the non-compressed initial material. For some mesh materials, especially the ones with larger original mesh widths or partitions, even higher degrees of compression are recommended, namely more than 50% or even 55%. These values apply for non-compressed mesh thread with an essentially round cross section, which are usually used for mesh materials.
In an advantageous embodiment, two threads crossing each other at a crossing point as a consequence of the compression show a ratio of their width (extension in the plane of the mesh material and essentially orthogonal to the extension direction of the thread) to their height (extension perpendicular to the plane of the mesh material) of between 1.5 and 4, preferably between 2 and 4, preferably between 2 and 3, further preferably between 2.5 and 3.
In an ordinary mesh material, thus a non-compressed, initial material, it is obvious that there is considerable free interspace in the mesh when considering the mesh material from above or from the bottom side. This interspace provides for the permeability of the mesh material in a direction perpendicular to the plane of the mesh. Within the plane of the crossings, each crossing point of two threads is surrounded by an alternating sequence of four free interspaces and four continuations of the threads crossing each other. In a mesh with a plain weave, each thread rises between a first pair of threads and descends between the next pair which causes that even in a very densely woven material, there is quite some interspace. In an intersection through the mesh, which is taken exactly at half the width of a particular thread, when following this thread along its course through the plurality of crossing threads, the thread is covered by crossing threads only in short sections, namely at the crossing points. Especially in the immediate neighbourhood of a crossing point between a longitudinal and a transversal thread, interspaces are present between these two threads both to the left and to the right side of the transversal thread. These interspaces in the cross-sectional view often have a shape which can be considered approximately triangular. These interspaces allow fluid to pass transversely through the mesh, e.g. along the thread. In the gasket according to the invention, a sufficient transversal impermeability is achieved by a compression of the initial mesh material, thus by a shift of material of the thread mainly from the upper and lower surfaces of the mesh into these interspaces, which results in a reduction of the thickness of the mesh material compared to the initial mesh material. When considering a comparable cross-sectional view through the mesh at half the width of a particular thread, the remaining free areas between this, e.g. transversal thread and the longitudinal threads crossing the former are much smaller compared with the interspaces in the initial material. In the cross-section which is taken at half the width of the thread, a remaining free area—thus a continuous free area—is of ≦0.008 mm 2 , preferably ≦0.006 mm 2 , preferably ≦0.004 mm 2 , most preferably ≦0.002 mm 2 per crossing point. With the described design, some or all of the remaining free areas in the sieve layer formed by the mesh material become so small that the sieve is sufficiently impermeable in its transversal direction.
The remaining free areas are thus defined as the respective continuous area, which when considering the sieve area along the middle of a mesh thread is not intersected or covered by a mesh thread. The remaining free areas are present on both sides of a thread at each crossing point. It can also be referred to as remaining transversal free area.
The metallic flat gasket according to the invention provides for a metallic flat gasket which allows for the intended passage of fluids through the filter area. At the same time, the transversal impermeability of the mesh material outside of these filter areas is sufficient in order to prevent fluid from permeating through the mesh material from one passage opening to another, vicinal passage opening.
According to the invention, it is especially advantageous if the metallic layers arranged adjacent to the mesh layer comprise a sealing bead which encircles at least one of the passage openings at least in sections. Such a sealing bead further improves the transversal impermeability.
It is also advantageous if the metallic layers arranged adjacent to the mesh layer on their surface facing the mesh layer are coated at least in sections. Elastomers, such as fluoropolymers, e.g. FKM (e.g. vinylidene-fluoride-hexafluoropropylene copolymer) are particularly suited for such coatings. Other suitable coating materials are silicone rubber, NBR rubber (acryl-butadiene rubber), HNBR (hydrated acryl-butadiene rubber), PUR (polyurethane), NR (natural rubber), FFKM (perfluoro rubber), SBR (stryrene-butadiene rubber), BR (butadiene rubber), IIR (butyl rubber), FVSQ (silicone rubber), CSM (chlorosulfonated polyethylene), as well as silicone or epoxide resins as such or in a mixture of at least of the materials mentioned. With this coating, the transversal impermeability is further increased as the remaining free areas of the mesh material are further sealed by the coating material, which enters into the interspaces between the treads.
With non-coated surfaces of the sealing layer arranged adjacent to the sieve layer, it is preferred if the sieve material is compressed to a larger degree, e.g. to more than 50%, preferably to more than 55%, while with coated surfaces of the sealing layers which coatings face the sieve layer, smaller degrees of compression are usually sufficient, e.g. between 30% and 50%—including the limits mentioned.
The two metallic layers, which are arranged adjacent to the mesh material, advantageously consist of stainless steel, spring steel, spring-hard steel or carbon steel. Such layers may comprise sealing beads as mentioned above, which sealing beads provide for an additional sealing in the direction of the plane of a gasket layer or parallel to this plane.
The threads of the mesh advantageously consist of metal, for example steel, e.g. austenitic steel, ferritic steel, stainless steel or carbon steel or they comprise these metals. If an austenitic steel is used for the initial mesh material, martensite formation during compression causes this material to become magnetic. This mesh material then can be used in the same way as a ferritic steel. It is thus possible to use a magnetic grab for such a compressed magnetic mesh material, which is a considerable advantage during production and handling. The thread diameter of the initial mesh material is usually between 0.04 and 0.12 mm.
As an alternative, the mesh threads can also consist of a thermoplastic or a thermoset material or comprise such. It is advantageous to use a polyester or a polyamide material.
It is advantageous to use a woven material as the thread material, in particular a woven material with a plain weave or with a twill weave. The mesh material may advantageously show a height of 10 μm to 1400 μm, preferably of 60 μm to 400 μm, and/or a width of the mesh of 80 μm to 250 μm, preferably 100 μm to 225 μm, preferably 100 μm to 200 μm. These magnitudes relate to the compressed material, which is reduced in its height.
If the mesh material is reduced in its thickness over its entire area, e.g. by compression, this allows for a particularly simplified production of metallic flat gaskets according to the invention. Such a completely compressed mesh material can be produced in an easy and cost-efficient manner from an initial mesh material, e.g. by calendaring. Both the weight per area and the partition remain essentially the same during compressing, with calendaring, the partition in the longitudinal direction may slightly increase.
During calendaring, only one line over the width of the material is compressed at a time, which means that calendaring requires considerable less pressure force is required than for a entire area compression of the mesh material. With an increasing degree of compression, the transversal spacings in the mesh material become smaller, which facilitates a sealing of the remaining free areas with a coating, e.g. with a coating of the adjacent metallic layers. The sieve layer itself remains uncoated.
Particularly high degrees of compression with remaining free areas of less than 0.004 mm 2 are possible without any damage to the mesh material if the material is calendared, intermediately annealed and again calendared. It is possible to anneal the mesh material once more at the end of the process.
From a production point of view, it is preferred to use a uniform piece of sieve material as the sieve layer. Some particular application may however require the use of mesh materials with different properties.
To this end, it is in principle possible to use a pair of graded calendar rolls or a pair of rolls each with a sequence of calendar rolls with different heights, these rolls being arranged one after another along the axis of each composed roll with the same sequence to be used for the upper and the lower composed roll. This allows to using a sieve layer with areas of different heights and therefore different magnitudes of the remaining free area. However, the zones run with a constant width which means that this variation of different mesh properties can only be used in particular applications.
As an alternative, it is possible, to combine different calendared materials in such a way to the sieve layer that this layer is composed of different pieces of different calendared material which are connected to each other either by adhesion or by form-locking. The connection needs to be performed in the plane of the sieve layer, thus without overlap and without any thickening. It is particularly preferred if laser welding is used for this connection.
The mesh width is generally selected depending of the size of particles of the particles to be filtered and the maximum admissible flow resistance. The initial material is selected from mesh materials with a ratio between mesh width and thread diameter of 2:1 to 4.5:1, preferably 7:5 to 9:2. With an increase of this ratio, compression of the mesh material becomes easier, but with a ratio higher than the maximum value specified above, the sealing beads usually used in metallic flat gaskets and the typical bolt forces would not suffice to achieve a sufficient sealing effect of the flat gasket.
To summarize, one can state that the mesh material according to the invention, especially when its entire area has been compressed, allows for a simplified and cost-efficient production of a flat gasket with filter areas. This flat gasket at the same time provides for a good passage of the fluids through the passage openings and a sufficient transversal impermeability. Together with the advantageous gasket, an advantageous method for the production of such a gasket is presented.
Apart from the mesh material layer and the top and bottom layers from relatively thin metal sheets, a distance layer which allows to adapting the thickness of the gasket, may be arranged between one of the top and bottom layers and the sieve layer, respectively. While the thickness of the bottom and top layer is usually between 0.1 and 0.25 mm, the thickness of the distance layer is at least 0.3 mm. The distance layer usually shows the same distribution of passage openings as the top and bottom layer, their magnitude may however be different.
In the following, some examples of a flat gasket according to the invention are explained in detail. Elements described for an individual example at the same time represent elements of the invention as such. In the following, identical or similar elements are referred to with identical or similar reference numbers. All multi-layer cross-sections show the gasket layers in an exploded representation relative to each other.
BRIEF DESCRIPTION OF THE DRAWINGS
It is shown in
FIG. 1 : A gasket for a transmission control unit;
FIG. 2 : A cross-section through a transmission gasket according to the state of the art;
FIG. 3 : Cross-sections through three transmission gasket as examples for flat gaskets according to the invention;
FIG. 4 : Two cross-sections through mesh materials, once in the non-compressed and once in the compressed state, respectively;
FIG. 5 : A cross-section through a mesh material of a flat gasket according to the invention, corresponding to FIG. 4 ;
FIG. 6 : A polished cut section of a mesh material; and
FIG. 7 : In two partial figures the ratio of the transverse leaking area to the compression of the material, for three different initial materials.
DETAILED DESCRIPTION OF THE INVENTION
FIG. 1 shows a gasket, namely a gasket 20 for a transmission control unit, in a plan view. This plan view shows a first metallic layer 1 with a multitude of passage openings 6 , 7 , but where only some of the passage openings are explicitly marked with a reference number. The passage openings are openings for a passage through the transmission gasket 20 , in a direction perpendicular to the plane of the drawing sheet. The passage openings 6 here are passage openings for bolts or the like; in these passage openings, no filter is arranged. The passage openings 7 are passage openings for fluids, e.g. for hydraulic oil. In these passage openings 7 , a filter is arranged, which according to the invention is formed by a sieve layer 3 consisting of a mesh material. The sieve layer in FIG. 1 is referred to with reference number 3 , only in the area of the passage openings 7 , it is not covered by the gasket layer 1 and therefore only visible in this area.
Around the passage openings 7 and the bolt passage openings 6 , sealing beads 11 are arranged in the first metallic layer 1 . They form sealing lines around the circumferential edges of the passage openings 6 and 7 and as a consequence improve the transversal impermeability between these passage openings 6 and 7 . The transversal impermeability is defined as the impermeability for the passage of fluids within the plane of the layer of the transmission gasket 20 ; it expresses the ability to seal against the permeation of fluids within the plane of the layer, namely the sieve layer, from a passage opening 6 , 7 to another, vicinal passage opening 7 , 6 .
FIG. 2 now shows in a cross-section the assembly of a transmission gasket 20 according to the state of the art. Such a transmission gasket comprises two metallic gasket layers 1 and 2 , between which a further layer 21 is arranged. In the area of a passage opening 7 , the intermediate layer 21 comprises an opening with a mesh sieve 22 being arranged in this passage opening. This mesh sieve 22 at its outer edge is connected to the layer 21 , e.g. clipped. The mesh sieve 22 now forms a filter for a fluid, which passes through the mesh sieve 22 in a direction perpendicular to the plane of the mesh sieve. However, the production of such a gasket with a composed layer 21 , 22 is extremely demanding.
FIG. 3 therefore shows three embodiments of metallic flat gaskets according to the invention, for example transmission gaskets, comparable to FIG. 1 . FIG. 3 shows three cross-sections which all correspond to line A-A in FIG. 1 .
FIG. 3 -A shows in a cross-section including passage openings 6 ( 6 a , 6 b , 6 c ) and passage openings 7 ( 7 a , 7 b , 7 c ) with the filter area. In the layers 1 and 2 made of spring steel, all these passage openings 6 a , 6 b , 6 c and 7 a , 7 b , 7 c are surrounded by elastic sealing beads 11 a to 11 f.
The central layer 3 according to the invention in its entirety consists of a woven mesh, which shows a degree of compression of more than 30%, thus a thickness which corresponds to less than 70% of its initial thickness. The woven mesh here is shown along the extension direction of a transversal thread 5 in a sectional view, so that the longitudinal threads 4 a , 4 b , 4 c in turn are only shown as short sections in their cross section. Only some of the longitudinal threads in FIG. 3 -A are referred to with an individual reference number.
The mesh material in the present example consists of metal threads, namely of a stainless steel of the type 1.4306 and is compressed over its entire area, thus over its complete width and its complete length by calendaring. Such a compression is particularly advantageous if it is accomplished with a calendar. A conventional press would require pressure forces which make a compression of the entire area with a degree of compression of more than 40% extremely laborious.
As already mentioned, the layer 3 mesh material spans the passage openings 7 a , 7 b and forms a filter area for fluid passing through these passage openings 7 a , 7 b , e.g. hydraulic oil. At the same time, the mesh material with such high degrees of compression is sufficiently impermeable in its transversal direction as to not allow hydraulic oil at all or in a quantity higher than admissible to pass from a passage opening 7 a , 7 b through the sieve layer 3 , thus in the plane of the sieve layer 3 to the passage openings 6 a , 6 b , 6 c.
In the passage openings 6 a , 6 b , 6 c , no mesh material is arranged, as these openings, for example as bolt holes, do either not need or not allow a filter area.
As can be appreciated from FIGS. 1, 3A -C, 4 A-B, 5 A-B and 6 , the mesh material comprises a weave of threads. The weave comprises at least a first set of threads all oriented in a first direction and a second set of threads all oriented in a second direction different than the first direction. The first direction may be transverse to the second direction. The threads of the first set are spaced from one another at regular intervals. The threads of the second set are spaced from one another at regular intervals.
In FIG. 3 -B, a comparable embodiment as in FIG. 3 -A is illustrated. In addition, both the gasket layers 1 and 2 on their surface facing the central layer 3 are covered with an elastomeric, FKM-based coating 9 , 10 with a coating thickness of about 40 μM. This elastomeric coating seals interspaces which may exist in the sieve layer 3 in between individual threads 4 a to 4 c , 5 . Advantageous coating thicknesses are between 20 μm and 50 μm. It is preferred that both surfaces of gasket layers which face to the mesh layer be coated. The sieve layer 3 itself is uncoated.
FIG. 3 -C shows a further embodiment of a metallic flat gasket according to the invention. As a difference to the embodiment of FIG. 3 -A, here, the direction of the sealing beads is inverted. They now do not point away from the sieve layer 3 , but point towards the latter. This arrangement of the beads also allows for a good sealing in the transversal direction, thus in the plane of the layer and with respect to the permeation of a fluid from a passage openings 7 a , 7 b to the passage openings 6 a , 6 b , 6 c.
FIG. 4 in drawing 4 -A shows a sectional view through a mesh material, with the cross section taken at the middle of a thread 5 and representing its longitudinal extension. The same material is shown drawing 4 -B but now in a compressed state according to the invention. For this material, it is obvious, that at the crossing points, 12 a , 12 b , 12 c , the total thickness of the two threads 4 a , 5 crossing each (e.g. at the crossing point 12 a ) other is approximately the same than the thickness of the thread 5 between the two vicinal crossing points, e.g. between the two crossing points 12 a and 12 b or 12 b and 12 c . In FIG. 4 -B, the mesh material is thus shown with a degree of compression of about 50%. The degree of compression compared to the initial material shown in FIG. 4 -A is 50% as well. The distance between the threads 4 a and 4 c in both subfigures 4 -A and 4 -B corresponds to twice the partition of the weave. The width of a mesh in contrast corresponds to the distance between the right edge of thread 4 a and a vertical projection of the left edge of thread 4 b.
FIG. 5 in subfigure 5 -A again shows the cross section through a mesh material, which has already been shown in FIG. 4 -B. In addition, FIG. 5 -B shows an increased section of crossing point 12 b . It is obvious that remaining free areas 8 a , 8 b remain in the vicinity of the longitudinal thread 4 a up to the area in which the transversal thread 5 reaches its full thickness. These remaining free areas in the cross section of the mesh material are not completely covered by threads 4 a and 5 . Such remaining free areas 8 a , 8 b allow fluid to permeate along the thread 4 a also in the transversal direction, thus in the direction of the plane of the mesh material 3 . With a sufficient reduction of these remaining free areas, the transversal permeability is extremely limited and thus the transversal impermeability becomes so good that the mesh material is not only suited as filter material in the passage openings 7 a , 7 b , but also as a sealing material in the areas between these passage openings. Based on this, it is sufficient to compress the mesh material 3 over its entire area in a uniform way and without providing any particular local structuring. While it is not possible to compress material with local structures in a calendar, it is possible to produce a uniformly compressed material with a calendar. This use of a calendar allows for a cost-efficient and simple production of compressed mesh material with the extremely high degree of compression required for the sealing purpose described.
FIG. 6 represents a polished cut section of a calendared mesh material of the steel type 1.4301, the cut has been performed in the middle of a thread 5 . As a consequence of the situation of the cut, the threads 4 a , 4 b , . . . running perpendicularly to the cut thread 5 are visible as well as the crossing points 12 a , 12 b , . . . . The cut representation illustrates the conditions in a wire mesh, which has been compressed by about 55%, which has been calendared from a wire mesh with a wire thickness of 80 μm and a mesh width of 125 μm. The total thickness of the woven mesh H is at an average of the two positions marked with an arrow 74.5 μm and therefore 46.5% of the initial thickness. Analogously, the height of the individual threads HD with an average of 37.7 μm at the three positions marked is less than 50% of the thickness of the initial thread. The width B of the threads at the crossing points in the compressed sieve material therefore has changed considerably less, it amounts at an average of the two positions marked 106.4 μm and is thus ⅓ larger than the initial diameter of the thread. The ratio of width B to height HD of the compressed individual threads at the crossing points is between 2.7 and 2.8. It is obvious that only very small remaining free areas F are left between the threads 4 a , 4 b , 5 which cross with each other and the calendared woven mesh therefore shows a high transversal impermeability.
As tests involving hot oil are difficult and too dangerous to set up with standard size test specimens, suitability for practice of materials has been tested on few real examples at the test bench and under the conditions of a producer of automatic transmission units with testing conditions being secret know-how of this company. The decisive factors were whether the transmission unit did actuate an oil pump at the frequency to be expected under the test conditions and that only the correct switching operations took place. Tests were performed with the sieve layer being arranged between top and bottom layers 1 , 2 made from beaded carbon steel DC 01 C 490 with a thickness of 0.250 mm.
The conditions set by the producer of the automatic transmission units were for instance achieved with a stainless steel 1.4301 sieve layer of 0.224 mm and 0.08 mm thread diameter at 55% percent of compression even though the top and bottom layers were not coated. With an FKM coating with a thickness of 40 μm on both surfaces of the layers 1 , 2 a sieve layer with 0.125 mm mesh width and 0.08 mm thread diameter and a degree of compression of 30% did also fulfil the requirements. However, apart from the properties of the top and bottom layers, it is mainly the remaining free area which decides on whether a sieve material leads to the required impermeability.
FIG. 7 shows two diagrams which illustrate the magnitude of the remaining free areas 8 a , 8 b of the compressed mesh material once in 10 −3 mm 2 (per remaining free area) and once as a relative value of the initial transverse leaking area for three different initial materials, all corresponding to the steel type 1.4301, which is rather similar to the 1.4306 type considered in the context of FIG. 3 . Two materials have initial thread diameters of 0.08 mm but different initial mesh width, namely 0.224—indicated with diamond labels—and 0.125, marked with triangular labels. The measurement points with the circular labels relate to an initial material with a higher thread width of 0.09 mm and a mesh width of 0.200 mm.
Both partial FIGS. 7 -A and 7 -B at first sight show what is expected, namely that the remaining free areas become smaller with an increasing degree of compression of the mesh material. As follows from FIG. 7 -A, at a degree of compression of 30%, the two materials with the smaller mesh width have transverse leaking areas which are less than 40% of the corresponding values of the initial sieve, the sieve material with 0.224 mm mesh width showing a slightly larger value. With 45% compression, the transverse leaking are is reduced to less than 10% of the initial value of all materials considered.
If one considers the absolute values in FIG. 7 -B, the sieve material which in combination with coated top and bottom layers lead to the expected result shows a remaining transverse leaking area of 2.5 10 mm 2 . Corresponding values are achieved with the material having 0.200 mm mesh width and 0.09 mm tread diameter at 40% of compression. A remaining transverse leaking area of less than 1 10 −3 mm 2 is obtained at 45% compression.
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The present invention relates to a flat gasket with filter elements. In order to fulfill the increased requirements with respect to cleanliness, there is an increased demand for the integration of filter elements in flat gaskets. The corresponding filter elements mainly serve for picking of impurities accrued during production as well as other residues circulate via the operational fluids, especially during the initial period of operation of an internal combustion engine or a vehicle.
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BACKGROUND AND SUMMARY OF THE INVENTION
This invention relates generally to shim material and more particularly to a plastic shim adapted for application between two spaced surfaces.
Shims have been used for many years to provide proper spacing between two surfaces, provide a seal between two mating surfaces, or to adjust the height or position of a particular object spaced from another object. Shims are used in a variety of manufacturing operations to fill unwanted gaps or spaces in assembled articles caused by imperfectly fitting components. For example, in the automotive industry, steel shims are commonly used to fill gaps during the assembly of various components where subassemblies are bolted together. In other industries shims are used to compensate for alignment irregularities between mating surfaces and to adjust the orientation of a structure.
In large machinery mounting applications, a bed plate is typically formed and the machine is mounted on the bed plate via studs or bolts. The machine is leveled by placing shims of appropriate thicknesses between the machine base and the bed plate. A worker mounting a large piece of machinery such as a generator or an air conditioning unit, must place various sizes of shims between the unit base and the foundation. In situations where the foundation does not have upwardly projecting studs, positioning a shim between the mating surfaces may be difficult and possibly dangerous to the worker. If the piece of machinery is particularly heavy, positioning a loose shim correctly on the foundation is difficult. Often the shim moves from the desired position as the components are mated together requiring several attempts at proper placement of the shims. These conventional shims are usually metal and are relatively heavy, expensive and often prone to corrode.
In manufacturing situations where shims are required, it is desirable to be able to place a shim against one surface such that the shim remains against the surface until the other mating surface is joined. However, when using conventional shims the first surface must generally be upwardly facing with projecting pins or studs projecting upward so that when the shim is placed over the studs and onto the surface gravity retains the shims in position. Otherwise, if this first surface is slanted or downwardly facing, a conventional shim placed thereon will simply fall off.
Accordingly, it is a principal object of this invention to provide a plastic shim to overcome this disadvantage and to provide shims that are lightweight, rust free, simple to install, and will retain their position against a surface having a projection outward therefrom in any orientation until the two mating surfaces are joined.
A self retaining plastic shim according to the present invention has a generally flat plate shape with an aperture therethrough. The shim has integral opposing tabs projecting inward from the wall of the aperture. These tabs are preferably of decreasing thickness as the tab extends inward of the aperture. The tabs elastically deflect when a shim having these tabs is placed onto a surface having a projection such as a stud pushed through the aperture in the shim. The deflection of the tabs against the stud holds the shim in place against the surface of the first body until the first body with the shim attached is placed against a second body having a corresponding aperture to receive the bolt or stud.
Thus when the shim is simply applied to one surface having projecting studs, bolts or pins, it is unnecessary to manually hold the shim in place while the two surfaces are joined.
Further objects, features and advantages of the invention will become evident from a consideration of the following detailed description when taken in conjunction with the accompanying drawing and the appended claims.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is an exploded perspective view of a first and second body having a self retaining molded shim according to a first embodiment of the present invention therebetween;
FIG. 2 is an enlarged perspective view of the embodiment of the self retaining shim according to the present invention shown in FIG. 1;
FIG. 3 is a partial sectional view through the shim shown in FIG. 2 taken along the line 3--3;
FIG. 4 is a partial plan view of a second embodiment of the present invention;
FIG. 5 is a partial sectional view taken along line 5--5 in FIG. 4 of the second embodiment of the shim according to the present invention with the shim mounted against a surface having a stud protruding through the aperture;
FIG. 6 is a plan view of a third embodiment of the shim according to the present invention illustrating a bolt suspended by the shim by the projecting tabs gripping the threads of the bolt; and
FIG. 7 is a sectional view of the shim and bolt shown in FIG. 6 taken along the line 7--7.
DETAILED DESCRIPTION OF THE INVENTION
Turning now to the drawing, a shim 10 according to a preferred embodiment of the present invention is shown placed between block 12 and base 14. Block 12 and base 14 are merely representative of two objects to be mated to simplify the explanation of the invention. Block 12 has studs 16 protruding downward from the bottom surface 18. Bottom block 14 has corresponding holes 20 for receiving studs 16 when blocks 12 and 14 are mated together with shim 10 sandwiched between them.
Lightweight shim 10 in this embodiment, is a generally C-shaped flat body 22 which has a slot 24 in each leg of body 22. The general shape of body 22 is merely illustrative. Other shapes may also be formed depending on the particular installation and the particular shapes of the surfaces to be mated.
Spaced along slot 24 and projecting from sidewall 26 are deflectable tabs 28 which project inward of slot 24. As shown in FIG. 3, deflectable tabs 28 have tapered cross sections narrowing from sidewall 26 in a concave taper 30 to terminating edge 32. Because of this taper, tabs 28 are increasingly elastically deflectable as terminating edge 32 is approached.
An alternative embodiment of the present invention is shown in FIG. 4. In this embodiment, instead of slots 24 being formed in the body, square apertures 34 are provided with convex arcuate inward tabs 36 projecting inward from each of the sidewalls of square apertures 34. Once again, tabs 36 are integral with body 33 and perform the same function as in the previous embodiment.
FIG. 5 shows a partial sectional view of the shim body 33 of FIG. 4 applied adjacent to block 12. Tab 36 will deflect as shown when passed over stud 16 and exert a retaining force against stud 16 sufficient to retain the lightweight shim 10 against surface 18.
Other embodiments may be visualized depending on the particular application of the shims having the self retaining tab feature integral to the shim body. For example, in the shim design shown in FIGS. 1 and 3, the tabs on opposite sides of the slots could be directly opposing one another rather than being partially off-set as shown. Other apertures and tab formations may also be used. This feature is purely a matter of detailed design and does not depart from the spirit of the present invention.
A third embodiment of the shims according to the present invention is shown in FIGS. 6 and 7. A bolt 38 is shown in FIG. 6 gripped by shim 40. Threads 42 on bolt 38 engage tabs 44 to hold bolt 38 on shim washer 40. As shown in FIG. 7, in this embodiment, tabs 44 are preferably slightly narrower in cross section then the angle 46 formed between threads 42. Thus full engagement of tabs 44 to threads 42 is achieved compared to the partial engagement with the treads as shown in the embodiment illustrated in FIG. 5.
The shim washer 40 illustrated in FIGS. 6 and 7 is shown holding the bolt 38 in place so that bolt 38 does not fall out of shim washer 40. Similarly, if bolt 38 were inverted, shim washer 40 would remain on bolt 38. An extension of the embodiment shown in FIGS. 6 and 7 then would be a ring shaped shim with a plurality of spaced apart apertures, each having a bolt 38 held in place by tabs similar to tabs 44 shown in FIGS. 6 and 7.
Typical plastic polymeric materials that are appropriate for shims according to the present invention may be of various compositions such as ABS, acetyl, polyamide, or other thermoplastic materials which have the structural strength necessary to accommodate compressive loads and have other physical characteristics desirable for the particular service application, such as being suitable for temperature, humidity, other environmental conditions, resistant to vibration, etc..
Self retaining plastic shims according to the present invention may be formed by the injection molding process. This process can provide simple and inexpensive shims of various thicknesses having integral tabs projecting into the apertures. The tabs may be of various shapes, two of which are shown in FIGS. 3 and 4. Many other shapes of the tabs are possible depending on the particular detailed application and the particular plastic material being utilized.
The self retaining plastic shims according to the present invention simplify a component assembly process where shims are required as well as provide an inexpensive inherent means of temporarily positioning a shim on one surface until the opposing surfaces can be mated. As these shims are made of plastic, they are also rust free, eliminating potential long term corrosion problems found with conventional metal shims.
The invention has been described above in an illustrative manner and it is to understood that the terminology that has been used is intended to be in the nature of words and description rather than that of limitation. Obviously many other modifications and variations of the present invention are possible in light of the above teachings. It is therefore to be understood that within the scope of the appended claims the invention may be practiced other than what is specifically described.
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A self retaining shim for mounting between two surfaces is made of plastic and engages a projection from one of the surfaces on which the shim is to be mounted. The shim has inwardly directed deflectable tabs projecting into an aperture for engaging the projection to hold the shim in place while the two surfaces are joined.
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Botanical/commercial classification: Rosa hybrida /Hybrid Tea Rose Plant.
Varietal denomination: cv. Meimarkize.
SUMMARY OF THE INVENTION
The new variety of Rosa hybrida Hybrid Tea rose plant was created by artificial pollination wherein two parents were crossed which previously had been studied in the hope that they would contribute the desired characteristics. The female parent (i.e., the seed parent) was the ‘Meisatex’ variety (non patented in the United States). The male parent (i.e., the pollen parent) was the product of the cross of the ‘Meikola’ variety (U.S. Plant Pat. No. 5,607) and the ‘Keidargo’ variety (non-patented in the United States).
‘Meisatex’×(‘Meikola’בKeidargo’).
The seeds resulting from the above pollination were sown and small plants were obtained which were physically and biologically different from each other. Selective study resulted in the identification of a single plant of the new variety.
It was found that the new Hybrid Tea rose plant of the present invention:
(a) forms strong vegetation, (b) forms substantially globular-shaped buds, (c) forms at mid-season abundantly and substantially continuously attractive yellow-green blossoms suffused with pink possessing a light fragrance wherein the numerous petals are positioned in a quartered manner, (d) displays attractive green foliage, (e) forces well under greenhouse growing conditions, and (f) is particularly well suited for cut flower production under greenhouse growing conditions.
The new variety well meets the needs of the horticultural industry and performs well under greenhouse growing conditions. No disease problem has been observed during observations to date when the new variety was being grown in greenhouses.
The new variety can be readily distinguished from its ancestors. For instance, the blossom coloration is considerably different from that of the ‘Meisatex’, ‘Meikola’, and ‘Keidargo’ varieties. More specifically, the ‘Meisatex’ variety forms orange-red blossoms, the ‘Meikola’ variety forms Venetian pink blossoms, and the ‘Keidargo’ variety forms dark red blossoms.
The new variety has been found to undergo asexual propagation in France by a number of routes, including budding, grafting, and the use of cuttings. Asexual propagation by the above-mentioned techniques in France has shown that the characteristics of the new variety are stable and are strictly transmissible by such asexual propagation from one generation to another.
The new variety has been named ‘Meimarkize’.
BRIEF DESCRIPTION OF THE PHOTOGRAPH
The accompanying photograph shows that as nearly true as it is reasonably possible to make the same, in a color illustration of this character, typical specimens of the plant parts of the new variety. The rose plants of the new variety were approximately one year of age and were observed during May while growing on Rosa indicia Major understock and growing in greenhouses at Le Cannet des Maures, Var, France. Dimensions in centimeters are indicated at the bottom of the photograph, as is a standard color comparison.
FIG. 1 illustrates a specimen of a young shoot;
FIG. 2 illustrates a specimen of a floral bud before the opening of the sepals;
FIG. 3 illustrates a specimen of a floral bud at the opening of the sepals;
FIG. 4 illsutrates a specimen of a floral bud at the opening of the petals;
FIG. 5 illustrates a specimen of a flower in the course of opening;
FIG. 6 illustrates a specimen of an open flower— plan view— obverse;
FIG. 7 illustrates a specimen of an open flower— plan view— reverse;
FIG. 8 illustrates a specimen of a fully open flower— plan view— obverse;
FIG. 9 illustrates a specimen of a fully open flower— plan view— reverse;
FIG. 10 illustrates a specimen of a floral receptacle showing the arrangement of the stamens and pistils;
FIG. 11 illustrates a specimen of a floral receptacle showing the arrangement of the pistils (stamens removed);
FIG. 12 illustrates a specimen of a flowering stem;
FIG. 13 illustrates a specimen of a main branch;
FIG. 14 illustrates a specimen of a leaf with three leaflets— plan view— upper surface;
FIG. 15 illustrates a specimen of a leaf with five leaflets— plan view— under surface; and
FIG. 16 illustrates a specimen of a leaf with seven leaflets— plan view— upper surface.
DETAILED DESCRIPTION
The chart used in the identification of the colors in that of The Royal Horticultural Society (R.H.S. Colour Chart). The description is based on the observation of one-year-old plants during May which were budded on Rosa indicia Major understock and growing in greenhouses at Le Cannet des Maures, Var, France.
Class: Hybrid Tea. Plant:
Height. —When pruned to a height of 0.85 cm, floral stems having lengths of approximately 60 to 70 cm on average are produced. Width. —Approximately 80 cm on average.
Branches:
Color. —Young stems: near Yellow-Green Group 144A. Adult wood: near Green Group 143A. Thorns. —On young stems: Small Prickles: Quantity: none. Long prickles: Quantity: none. On adult stem: Small prickles: Quantity: Approximately 10 on average on a stem length of 10 cm. Length: approximately 0.2 cm. average. Color: near Greyed-Yellow Group 160D with some Greyed-Orange Group 166A. Base: Obovate. Long prickles: Configuration: rather slightly, very longish pointed and curved downwards on the upper surface, and concave on the under surface. Quantity: approximately 1 on average on a stem length of 10 cm. Length: approximately 0.4 cm on average. Color: near Yellow-Green Group 160D with Greyed-orange Group 166A. Base: obovate.
Leaves:
Stipules. —Adnate, pectinate and narrow, smooth, approximately 1.8 cm in length on average, approximately 0.2 cm in width on average, near Green Group 138A no the upper side, and near Green Group 138B on the under surface. Petioles. —Upper surface: near Green Group 143A in coloration. Under surface: near Green Group. 143B in coloration. Length: approximately 2.8 cm for the terminal leaflet. Rachis. —Upper surface: Near Green Group 143A in coloration. Under surface: near Green Group 143B in coloration. Leaflets. —Number: 3, 5 and 7 (most often). Shape: generally elliptical with a pointed tip and an obtuse base. Size: the terminal leaflet commonly are approximately 9.6 cm in length on average and approximately 5 cm in width on average. Serration: small and single (as illustrated). Texture: physically firm and thick. Color (young foliage): Upper surface: near Green Group 138A. Under surface: near Green Group 136B. Color (adult foliage): Upper surface: near Green Group 139A. Under surface: near Green Group 138B.
Inflorescence:
Number of flowers. —Commonly approximately 5 to 7 blossoms per stem. Peduncle. —Smooth, approximately 2.5 cm in length on average, approximately 0.6 cm in diameter on average, and near Yellow-Green Group 144A in coloration. Sepals. —Upper surface: smooth and near Yellow-Green Group 146B in coloration. Under surface: glandular and near Yellow-Green Group 144A in coloration. Size. —Approximately 3.6 cm in length on average, and approximately 1.2 cm in width at the widest point on average. Shape: longish-pointed and new at the top and somewhat straight at the base. Extensions: two sepals commonly possess no extensions and three sepals commonly possess very weak extensions. Buds. —Shape: substantially globular. Size: medium. Length: approximately 3 cm on average. Width: approximately 2.3 cm on average. Color as calyx breaks: Upper surface: near Red Group 56C, and amply suffused with near Red group 49A, and with a spot at the base of the near Green-Yellow Group 1C. Under surface: near Red Group 56C, and amply suffused with Red Group 49A and margined with Red Group 54A, and with a spot at the base of near Green-Yellow Group 1C more or less suffused with Yellow-Green Group 149A. Flower. —Shape: cup-shaped. Diameter: approximately 8 cm on average. Color (in the course of opening): Upper surface: near Red Group 56C suffused with near Red Group 49A. Under surface: near Red Group 56C suffused with near Red Group 49A and more or less margined with Red Group 54A. Spot at base: near Green-Yellow Group 1C on both surfaces. Upper side: possesses external whorls of near Red Group 56C and 56D, and internal whorls of near Red Group 56C and 56D, more or less suffused with Red Group 49A. Under surface: near Yellow-Green 150D with suffused with Yellow-Green Group 144B and 144D on the external petals. External whorls are near Green-Yellow Group 1C margined with near Red Group 56C, and internal whorls are near Green-Yellow Group 1C and one more or less suffused with near Red Group 56C and near Red Group 49A. Spot at base: bear Green-Yellow Group 1A. Color stability: slight change with age. Fragrance: light. Lasting quality: the blossoms commonly last approximately 14 to 16 days on the plant on average, and approximately 9 or 10 days on average when cut and placed in a vase. Petal number: approximately 97 on average under normal growing conditions. Petal shape: with a substantially rounded tip and base. Petal texture: consistent and somewhat firm. Petal length: approximately 5.4 cm on average. Petal width: approximately 5.7 cm on average. Petal arrangement: imbricated, without petaloids, and commonly quartered. Petal drop: good with the petals commonly detaching cleanly before drying. Stamen number: approximately 57 on average. Anthers: regularly arranged around the styles, approximately 0.3 cm in size on average, and near Orange Group 26B in coloration. Pollen: present. Filaments: approximately 0.5 cm in length on average and near Group 1A in coloration. Pistils: approximately 172 on average. Stigmas: approximately 0.8 cm in size on average and near Green-Yellow Group 1D in coloration. Styles: approximately 0.1 cm in length on average, and near Red-Purple Group 58A in coloration. Receptacle: smooth, funnel-shaped in longitudinal section, approximately 1.5 cm in length on average, approximately 1.7 cm in width on average at the widest point, and near Yellow-Green Group 144A in coloration. Hips: none observed to date when grown under greenhouse growing conditions.
Development:
Vegetation. —Strong. Blooming. —Mid-season, abundant and substantially continuous. Tolerance to diseases. —No diseases have been observed during observations to date when grown in greenhouses. Aptitude to bear fruit. —None observed during observations to date. Aptitude to to forcing. —Good.
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A new and distinct variety of Hybrid Tea rose plant is provided that forms at mid-season abundantly and substantially continuously attractive yellow-green blossoms suffused with pink processing a light fragrance wherein the numerous petals are positioned in a quartered manner. The buds are substantially globular-shaped. The vegetation is strong and attractive green foliage is formed. The plant forces well and is particularly well suited for cut flower production under greenhouse growing conditions.
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CROSS-REFERENCE TO RELATED APPLICATIONS
This application is the U.S. national phase of the International Patent Application No. PCT/FR2011/050607 filed Mar. 22, 2011, which claims the benefit of French Application No. 1052659 filed Apr. 8, 2010, the entire content of which is incorporated herein by reference.
FIELD
The invention relates to the field of computer file storage management on multiple interconnected storage devices. It more particularly relates to the management of these files in a context of sharing them to enable access from any of these devices to the files stored on the devices.
BACKGROUND
With the proliferation of home devices able to store computer files, users of these devices are encountering difficulties in managing all the stored files.
Today it is common to have one or more personal computers, a storage device that streams media over a distribution network (“Set Top Box”), or other devices. The user then has an assortment of files distributed across different equipments.
To access the files stored on a specific device, the user must adapt to the file system of the device. Even when the devices are networked to allow using one device to access a file stored on another device, the user must adapt to the specific organization of the files on each device.
As a result, it is difficult for the user to keep a simple and consistent view of all the computer files (text, audio, video, images, etc.) on the assorted devices the user has.
A need therefore exists for a management of computer files stored on different communicating devices that is both effective and transparent to the user.
SUMMARY
The present invention aims to improve the management of files on these devices.
For this purpose, a first aspect of the invention proposes a method for managing computer files in a first device able to store computer files and able to be connected with at least a second device in order to exchange at least computer files, said first device storing the files according to a first data structure representing a first file tree enabling access to files stored in memory of the first device, the children of the root of the first tree corresponding to a first level of the tree, the children of the first level nodes corresponding to a second level of the tree, and so on,
said method comprising the following steps:
for a current level of the first tree, receiving data representative of a level of the same rank in a second data structure representing a second file tree enabling access to files stored in the second device, the children of the root of the second tree corresponding to a first level of the tree, the children of the first level nodes corresponding to a second level of the tree, and so on, comparing the current level with the level of the same rank, in the second structure, represented by the data received, in order to determine the presence in the second tree, at the rank level of the current level, of an element that is not found in the first tree at the current level, and if an element of the second tree is not found in the first tree, incorporating a descriptor for this element into the first tree data structure at the current level, said descriptor enabling access to said element from the first tree.
An element of the tree corresponds, for example, to a file or a folder (or sub-folder).
A descriptor may additionally contain one or more pieces of information such as the name, type, or size of the stored item.
The descriptor is incorporated, for example, by adding a leaf to the first tree.
It is also possible to add a node, in order to describe a folder for example.
In the first aspect of the invention, a unique document space is created for the user of the first device, enabling access to the elements present in both the first and second devices. When the method is implemented in every device the user has (or group of users, such as a family), the same view of the document space (or portion of the document space) is obtained on each device, meaning the same tree (or sub-tree) of folders and the same content files.
The method of the invention simplifies the actions the user must perform to access files stored on different devices. In effect, the user is given a single consistent view of all his/her files and folders, with transparent file sharing and optimal management (changes or saves for example).
For example, the comparison of levels is done element by element, using at least one from among the name, size, or content of the element.
The content of an element corresponds, for example, to the binary content of a file.
In some embodiments, during the comparison of levels, it is also determined whether a first element of the first tree and a second element of the second tree are identical according to a first comparison criterion, and in this case the following steps are applied:
comparing the first and second elements using a second criterion to determine whether the first and second elements are different according to the second criterion, and if the first and second elements are different according to the second criterion, incorporating a descriptor for the second element into the first tree data structure at the current level, said descriptor enabling access to said second element from the first tree.
A low-level verification of the presence of two identical elements within the first and second devices can therefore be performed. For example, the first criterion may correspond to comparing the names of the elements, and the second criterion may correspond to comparing the size or the content of the elements.
In some embodiments, during the comparison of levels, it is also determined whether a third element of the first tree and a fourth element of the second tree are identical according to a third comparison criterion, and in this case the following steps are applied:
accessing the content of the third element, sending a request to the second device to obtain data representative of the content of the fourth element, comparing the content of third and fourth elements to determine whether the two elements differ in content, and if the third and fourth elements differ in content, incorporating a descriptor for the fourth element into the first tree data structure at the current level, said descriptor enabling access to said fourth element from the first tree.
This reduces the amount of data initially sent to describe the level of the second tree. Additional data are only received if there is a need to discriminate between two identical elements using the third criterion.
It may additionally be arranged so that the first and second trees are respectively associated with a first piece of version information and a second piece of version information respectively representing a change in state over time of the first and second trees, the method then additionally comprises the steps of:
sending a request to the second device in order to receive data representative of the second piece of version information, comparing the first and second pieces of version information to determine whether the version of the first tree is earlier than the version of the second tree, and if the version of the first tree is earlier than the version of the second tree, sending a request to obtain the data representative of the level in the second data structure of the same rank as the current level in the first tree.
In this manner, each device knows how up to date its information concerning the elements present in the other devices is.
For example, if the first device is disconnected from the second device followed by a reconnection, the first device can use the version information to find out whether the second tree has changed and whether a new comparison of trees is required in order to update the first tree.
The method may additionally comprise the steps of:
comparing the current level with the level of the same rank, in the second structure, represented by the data received, in order to determine the presence in the first tree, at the rank level of the current level, of a descriptor for an element of the second tree, this element no longer being present in the second tree at the current level in the second version, and if the element is no longer present in the second tree, deleting the descriptor for this element from the first tree data structure at the current level.
It is thus possible to keep the first tree consistent with changes made in the elements of the second tree.
In some embodiments, the elements of the first and second trees are associated with a third piece of version information representing the version of the tree to which they belong which was the current version when they were last modified; the comparison of the current level with the level of the second structure represented by the data received is made by comparing the third pieces of information associated with the elements.
This simplifies and accelerates the comparison of the trees. The comparison criterion enables rapid comparison and allows processing only those elements that have a later version than the version of the first tree.
In order to keep the trees of a set of devices synchronized, it can be arranged so that, when a file is updated on the first device, the first piece of version information is updated and then sent out to the other devices in a version modification notification message.
For example, the request to the second device to receive data representative of the second piece of version information is sent after a message is received from the second device indicating a change of version for the second tree.
In order to access an element of the second device from a descriptor in the first tree, the first device may additionally:
send a query to at least one other device to ask whether the element is present on said at least one other device, and if the element is present on a device, the first device obtains a copy of the element in order to store it in the first device.
In this manner, file copies can be made to synchronize the content of the first and second trees.
Other aspects of the invention provide for:
a computer program containing instructions for implementing a method according to the first aspect of the invention when the program is executed by a processor; a computer-readable medium on which such a computer program is stored; a device configured to implement the method according to the first aspect of the invention; and a system comprising devices for implementing a method according to the first aspect of the invention.
Such a system comprises:
a first device able to store computer files and exchange them with at least a second device, a second device able to store computer files and exchange them with at least the first device, and
the first device stores the files in a first data structure representing a first file tree enabling access to files stored in memory of the first device, the children of the root of the first tree corresponding to a first level of the tree, the children of the first level nodes corresponding to a second level of the tree, and so on, and
for a current level of the first tree: the first device receives data representative of a level of the same rank in a second data structure representing a second file tree enabling access to files stored in the second device, the children of the root of the second tree corresponding to a first level of the tree, the children of the first level nodes corresponding to a second level of the tree, and so on; the first device compares the current level with the level of the same rank, in the second structure, represented by the data received, in order to determine the presence in the second tree, at the rank level of the current level, of an element which is not found in the first tree at the current level; and if an element of the second tree is not found in the first tree, the first device incorporates a descriptor for this element into the first tree data structure at the current level, said descriptor enabling access to said element from the first tree.
For example, the devices comprise:
a communication unit for sending and receiving messages in order to exchange computer files with at least a second device, a storage unit for storing computer files, and a processing unit for managing computer files according to a first data structure representing a first file tree enabling access to files stored in the storage unit, the children of the root of the first tree corresponding to a first level of the tree, the children of the first level nodes corresponding to a second level of the tree, and so on, said processing unit being configured, for a current level of the first tree, to: receive data representative of a level of the same rank in a second data structure representing a second file tree enabling access to files stored in the second device, the children of the root of the second tree corresponding to a first level of the tree, the children of the first level nodes corresponding to a second level of the tree, and so on; compare the current level with the level of the same rank, in the second structure, represented by the data received, in order to determine the presence in the second tree, at the rank level of the current level, of an element which is not found in the first tree at the current level; and if an element of the second tree is not found in the first tree, incorporate a descriptor for this element into the first tree data structure at the current level, said descriptor enabling access to said element from the first tree.
The advantages provided by the computer program, the computer-readable medium, the device, and the system, as briefly described above, are at least identical to those mentioned further above in relation to the method according to the first aspect.
BRIEF DESCRIPTION OF THE DRAWINGS
Other features and advantages of the invention will be further apparent from reading the following description. This description is purely illustrative and is to be read with reference to the attached drawings, in which:
FIG. 1 illustrates a general context for the implementation of some embodiments of the invention;
FIG. 2 is a general flow chart representing the steps followed to update a common file tree according to one embodiment;
FIGS. 3 a and 3 b illustrate two file trees and the result of updating a tree with information from the other tree according to one embodiment;
FIG. 4 illustrates accessing an element, in a tree of a device according to one embodiment, corresponding to a file or a folder which is not found locally;
FIG. 5 illustrates a synchronization of the trees of interconnected devices according to one embodiment;
FIG. 6 schematically illustrates a system and devices according to one embodiment.
DETAILED DESCRIPTION
FIG. 1 illustrates a general context for implementing some embodiments of the invention. In this context, a set of devices able to store and exchange computer files are connected to each other, for example via a network 10 . In another context (not represented), the devices could be directly connected to each other. The set of devices includes, for example, two PC-type personal computers 11 and 12 , a digital camera 13 , a set top box 14 , and a NAS (Network Attached Storage) file storage device 15 .
Each device can store computer files such as text, audio, image, video, or other files. In addition, the devices interconnected by the network 10 can exchange files.
For example, computer 11 can send a file stored on its drive to computer 12 so that the latter can store it on its own drive.
We propose offering the user a unified view of a file tree 16 grouping all the files stored on the interconnected devices, and doing so from any device.
Each device displays a tree which shows files and folders, independently of whether it actually has stored locally all the files and folders shown in the tree. In order to indicate that a file or folder of the tree is not stored locally on a device, this file or folder may, for example, be displayed in gray.
Thus, whether the user is looking at files on the computer 11 or on the set top box 14 (or other device), the user can find a file stored on any of the devices. The user can find a file in the tree, regardless of its actual storage location and regardless of the device from which the user wishes to access it.
Updating the tree on each device is described below, with reference to FIGS. 2 , 3 a and 3 b . FIG. 2 is a general flowchart representing the steps applied to update the tree, and FIGS. 3 a and 3 b illustrate updating the tree of a device with data representing another tree of a second device.
The tree creation method can be carried out by any of the interconnected devices 11 , 12 , 13 , 14 , and 15 .
The device carrying out the method, for example device 11 , has a data structure representing a tree 30 . This tree has a root RTA from which all the files and folders are accessible in the device. From the root RTA, it is possible to access folder F 1 , folder F 2 , and file F 3 as represented in FIG. 3 . Folder F 1 contains a file F 11 and a folder F 12 . Folder F 2 contains folder F 21 , which itself contains other folders and files (not represented), and folder F 22 containing file F 221 .
During a first initialization step S 20 , device 11 visits the first level in the tree RTA, meaning the level of the direct children of the root, which in this case is folders F 1 and F 2 , and file F 3 . The goal is to compare this first level with the first level of the tree 31 of another device with which it is sharing files, for example device 12 .
Tree 31 represents the files available in device 12 . This tree contains a root RTB from which it is possible to access two folders F 4 and F 5 . Folder F 4 contains folder F 41 which in turn contains folders and files (not represented), file F 42 , and another folder F 43 containing two files F 431 and F 432 . Folder F 5 contains folder F 51 which in turn contains files and folders (not represented), and file F 52 .
During step S 21 , device 12 receives data representative of the level in tree 31 of the same rank as the current level in tree 30 . For example, if device 11 is at the rank level N in tree 30 , it receives the representative data for rank level N in tree 31 . The device receives, for example, a list of elements (files, folders, and sub-folders), with attributes such as the size, file type, or others.
The data may be received after a message is sent to device 11 to that effect, or after a synchronization of the tree 30 as described below.
Device 11 then performs the comparison of levels of the same rank during step S 22 . For example, device 11 performs an element by element comparison of the name, size, or content of the elements. This comparison aims to determine the presence of elements in that level of tree 31 that are not present in that level of tree 30 .
For example, device 11 begins by verifying, in the first level of tree 30 , whether a folder exists named “F 4 ”, then whether a folder exists named “F 5 ”.
During step T 23 , it is then decided whether tree 30 is to be updated.
In a first example, it is assumed that elements F 4 and F 5 do not have the same name as elements F 1 , F 2 , and F 3 . Tree 30 is then modified during step S 24 by incorporating into the current level a descriptor for elements F 4 and F 5 which enables accessing these elements on the second device 12 . The new tree 30 obtained in this manner is illustrated in FIG. 3 b . This descriptor contains a name to designate the element, a storage indicator (for example an identification of the device storing it), a backup mode, a version number (as described below), or some other information.
In a second example, it is assumed that element F 4 has the same name as element F 1 . A new comparison is then performed according to another known criterion, such as, for example, the size of these elements. Based on the result of this second comparison, if the elements are of different sizes, it is decided to add a descriptor for element F 4 . If such a descriptor is added, it may for example bear a different name than the name of element F 1 , to avoid confusing them.
In a third example, it is assumed that element F 4 has the same name as element F 1 . It is then attempted to determine whether these elements differ in content, and therefore a second level of tree 30 is accessed, which contains elements F 11 and F 12 as children of element F 1 of the first level. At the request of device 11 , data is then obtained from device 12 , describing elements F 41 , F 42 , F 43 of the corresponding level in tree 31 . Next a comparison of the content of elements F 1 and F 4 is made and it is decided whether or not to incorporate a descriptor for element F 4 in tree 30 .
Once the elements of the current level of the tree 31 are incorporated, the device advances to the next level during step S 25 .
The number of levels to be visited can be adjusted according to how deep the tree 30 is to be modified. The greater the desired modification depth in the tree, the more levels are visited.
Alternatively, it may be decided to visit a level only if a user of the second device has accessed this level.
Also alternatively, the different levels of the tree may be accessed according to automatic updates.
With a tree updated in this manner, a user can use any device to access the files stored on another device.
As illustrated in FIG. 4 , when accessing an element in a device tree that corresponds to a file or a folder that is not present locally, the device can send requests to other devices in order to copy the file or folder locally for subsequent access.
In this example, device 12 wants to access file D 1 which is not stored on device 12 . Device 12 sends requests 40 to all the devices 11 , 13 , 14 , and 15 in order to poll them to find out whether they have this file stored.
In this example, device 15 sends a response message 41 saying that it does not have the file, devices 11 and 14 do not answer, and device 13 sends a message indicating that it has the file.
The device then sends a message 43 to device 13 to obtain a copy of file D 1 . Device 13 then sends a message 44 containing the data of file D 1 .
If several devices can provide D 1 , a choice can be made on where to send the message 43 according to the transfer speed or some other criterion.
Once file D 1 has been copied locally, it can be opened on device 12 .
After each device has updated its own tree to show the elements present on the other devices, mechanisms for updating and synchronizing these trees as a function of events on the network of these devices can additionally be provided.
In order to manage such synchronization, the concept of tree versions and the elements that compose them can be introduced. For example, each tree of each device is associated with a version number.
This version information can be used for the comparison in step S 22 , described above. In this case, it can be decided to incorporate only the elements of tree 31 which have a later version than the version of tree 30 .
When an element is saved after modification, a change notification can be sent out to the other devices so that each device of the set of interconnected devices can update its tree. In the case of a device reconnecting to the network after being disconnected for a certain period of time, a synchronization phase can allow updating its tree to reflect changes that may have occurred in the organization of the files and folders of the other devices. In addition, to incorporate changes made to files on the other devices as quickly as possible, each device may have an implemented listening mechanism (such as a loop) that watches for change notifications on the network, refresh mechanism that triggers (periodically, upon detection of predefined events, or other) a synchronization action, or some other mechanism.
A version (or revision) number is associated with each element of a tree. On each device, a general revision number is assigned to the tree. FIG. 5 illustrates a synchronization of the trees of interconnected devices. An identifier indicating the device which created the latest revision is associated with it as well. For example, “Id_ 15 : V 1 ” indicates revision V 1 created on device 15 . In the example, after a state where all devices were in revision Id_ 15 : V 1 , a change made to device 12 has caused it to advance to state Id_ 12 : V 2 .
After modifying a file D 2 on device 12 , the user saves his/her changes. This document then has revision number Id_ 12 : V 2 , which is propagated up the tree of folders to the root of the tree. This new revision number is assigned to all folders in the path to the document.
Next, device 12 broadcasts a message 50 to inform the other devices of the creation of the new revision Id_ 12 : V 2 .
Synchronization is then performed between device 12 and the other devices, so that the other devices can update their tree to reflect the change made to file D 2 .
The same type of synchronization can be performed for the creation or deletion of a file or folder.
As an alternative to broadcasting the message 50 , each device, for example device 15 , could periodically send a request to the other devices to receive the version number of their current tree. Then, upon receipt of the version number for the other devices, device 15 compares these version numbers to the version of its current tree. If the device determines that its tree has an earlier version than the tree version of a device which has returned its version number, it begins updating its tree as described above. In the example shown in FIG. 5 , device 15 determines that version V 1 of its tree is older than version V 2 of the tree of device 12 .
During the update, the device may detect that its current tree contains a descriptor for an element which in version V 1 is stored on device 12 but is not present on device 12 in version V 2 . In this case, this descriptor is deleted to bring the tree of device 15 into agreement with that of device 12 .
A computer program comprising instructions for implementing the method of the invention can be written by a person skilled in the art, according to a general algorithm deduced from the general flow chart of FIG. 2 and from the present detailed description.
FIG. 6 schematically illustrates a system according to an embodiment of the invention. The system comprises a device 60 connected to another device 61 via a communication network 62 .
Device 60 comprises a processing unit 601 for creating and/or updating a data structure representing a file tree enabling access to files stored in the storage unit 602 of the device according to a method of the invention. The storage unit 602 may contain different types of memory storage. For example, the storage unit also contains memory for storing computational data. The storage unit may also contain memory for storing a computer program according to the invention, for execution by a processor of the processing unit. The device additionally comprises a communication unit 603 for communicating in particular with device 61 via the network 62 in order to execute a method of the invention and exchange computer files. Device 61 has a structure similar to that of device 60 and comprises a processing unit 610 , a memory unit 611 , and a communication unit 612 .
The invention is not limited to the embodiments presented. Other variants and embodiments can be deduced and implemented by a person of the art upon reading the present description and the attached drawings.
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A method for managing computer files in a first device storing the files according to a first file tree, comprising the following steps: for a current level of the first file tree, receiving data representing a level of the same rank of a second data structure representing a second file tree of a second device communicating with the first device; comparing the current level with the level of the same rank of the second file tree, in order to determine the presence in the second file tree, at the rank level of the current level, of an element that is not found in the first file tree at the current level; and, in the event that an element of the second file tree is not found in the first file tree, adding a descriptor of said element to the first file tree at the current level, wherein the descriptor enables access to said element from the first file tree.
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BACKGROUND OF THE INVENTION
The invention relates to a method of recovering linear polyester, such as PET and PBT, from the waste of same, and a device for carrying out the method.
Unlike many other meltable thermoplastic plastics such as polyethylene, polypropylene or polystyrene, linear polyesters such as polyethylene terephthalate cannot be processed by simple melting and regranulation to make a reusable raw material for higher quality requirements, because polyesters are hydrolytically degraded during melting by the moisture which always adheres, unless they have been previously dried. On the other hand the breakdown of the polymer chains by hydrolysis is reversible on polyesters, by polycondensation being carried out through suitable reaction conditions such as vacuum, high temperature and stirring, and the reaction water formed being removed. In contrast to the other plastics mentioned, in polyesters even the breakdown of the molecule chains caused by thermal or oxidative degradation can be repaired.
Polyethylene terephthalate (PET) as waste is frequently marked by an increased concentration of carboxyl terminal groups in relation to intact PET and a depletion of glycol ester terminal groups. The cause of this is first and foremost the thermal degradation which is unavoidable during melting and during the processing from the melt. This leads to the fact that in usual regranulating processes the chain length of the PET, measured by the intrinsic solution viscosity (i.v.) decreases; if the behaviour of the PET in repeated regranulation and reuse is observed, as can be expected in intensive recycling, it can be ascertained that after roughly the third regranulation, the intrinsic solution viscosity has sunk so far, that the material is unusable. The intrinsic solution viscosity can be raised again by solid-phase postcondensation of the PET, this measure coming up against limits, however, since the carboxyl terminal groups have in the meantime increased and the glycol ester terminal groups have decreased. The greater the COOH/OH ratio, the lower the intrinsic solution viscosity which may be achieved through postcondensation, and the higher the COOH concentration of the postcondensation product.
Methods of recycling PET are known, in which the irregular waste is crushed and compacted in such a way that the parts of the waste so treated can be led continuously through shaft or other dryers, in order to achieve complete drying of the parts. Thereafter the melting and postcondensation are carried out. This method has the disadvantage that the drying of the waste is very expensive as a result of the extent of the plant and the energy consumption, and that hydrolytic degradation cannot be completely avoided, even if the waste is dried.
With these methods, the degree of polycondensation which may be obtained in the end product depends on the quality of the polyester waste used as raw material, in particular on its intrinsic solution viscosity (i.v.) and its COOH concentration. The end product from this method is therefore excluded from many applications which require a certain degree of polycondensation. Such products must therefore be described as inferior.
These methods are moreover not in the position to compensate for the loss of glycol ester terminal groups which increases with time and which is unavoidable in the repeated recycling of polyester, especially in the practically closed circuit.
The purpose underlying the invention is to create a method and a device for recovering linear polyester with simultaneous hydrolytic and glycolytic degradation, by means of which a recycled polyester of high quality should be obtained, and so that recycling is possible even in the closed circuit, it being intended that the plant size and the energy consumption should be kept small. In particular, it is the purpose of the invention to produce a polyester with exactly the degree of polycondensation which is necessary for the respective application, independently of the quality (i.v., concentration of carboxyl terminal groups) of the raw polyester.
SUMMARY OF THE INVENTION
The present invention addresses and solves the above-mentioned problems and meets the enumerated objects and advantages, as well as others not enumerated.
Corresponding to the present invention, undried waste is led into an extruder by being melted, hydrolytic degradation occurring in the melt. The waste only needs to be precrushed sufficiently for it to be able to pass without any problem through the inlet aperture of the shredding device connected upstream of the extruder. To the melt is added diol, for example ethylene glycol, corresponding to the basic constitutional unit for the polymer to be treated, for example PET, and then the melt is further condensed in a reactor, similar to the end reactors in continuous polyester polycondensation plants to the degree of polycondensation desired for processing. Thus the hydrolytic degradation of the polyester is acceptable and diol additives are added in the stoichiometrically necessary amount to obtain in a melt postcondensation the desired polyester with its molecular weight raised again. The partial glycolysis of the polymer, for example PET, caused by the addition of diol, for example ethylene glycol, lowers the ratio of the concentration of COOH/OH terminal groups such that in the following melt postcondensation, the desired intrinsic solution viscosity can be unreservedly achieved. Thus the end product maybe used for the usual applications such as threads, films and bottles and is comparable with a polyester produced from the original monomers.
As a result of the purposeful control and the temperature of the degradation regarding the degree of polymerization, together with the glycolytic degradation to limit values of between 15 and 35, adaptation to the desired parameters of the end product can be undertaken.
Advantageously, the diol is metered in such a way that the ratio of the COOH/OH terminal groups at the entrance of the postcondensation reactor lies between 0.3 and 0.1, which makes possible an optimisation of the process conditions.
In an advantageous manner, the melt is filtered before and/or after the metered addition of diol, since the melt at that point in time has the lowest relative molar mass and thus the lowest viscosity, and this results in lower outlay on filter pressure and filter area, i.e. the energy and apparatus costs can be reduced.
BRIEF DESCRIPTION OF THE DRAWINGS
An embodiment, given by way of example, of the device according to the invention is shown in the drawing and is explained in greater detail, together with the method, in the following description. The only FIGURE shows a diagrammatic construction of the device according to the invention.
DESCRIPTION OF THE PREFERRED EMBODIMENT
The method according to the invention for recovering linear polyesters, for example PET, can be used for carefully sorted waste in the most varied form, i.e. the waste can be present in the form of bottle scrap, fibres and threads, films and spunbonded nonwovens, with trimmings or whole webs, and as lumps of melt. Dirty waste can be washed before processing and larger pieces of polymer can be coarsely precrushed. Also suitable as raw material are coarsely precrushed drinks bottles made of PET which have been freed of paper and adhesive residue through the sorting of extraneous substances and other polymers and through washing with water. The water adhering to the surface as a result of washing can be removed in simple dryers, without the drying going so far that moisture diffuses from the interior of the polymer.
The plant shown in the figure has as essential components a single-screw degasifying extruder 2 downstream of a shredding device 1, into which the precrushed waste is fed via a conveyor belt. The shredding device here consists preferably of a rotatable disc received in a housing, on the upper surface of which disc erected cutters are disposed transversely. The precrushed pieces of waste are homogenised, warmed up and compacted in this device, the necessary centrifugal force for tangential charging of the extruder screw being generated simultaneously as a result of the rotation of the disc. Downstream of the extruder 1, in which the waste material is melted, is connected a filter unit 3 with a mesh width of between 40 and 150 μm. The melt emerging from the filter unit 3 passes through a special static mixer 6 and then a metering pump unit 7 which guides the melt via a further filter unit 8 with a mesh width of between 20 and 30 μm into the postcondensation reactor 9. A metering pump 5 with a variable drive system meters ethylene glycol and reaction additives from a reservoir 4 into the flow of melt to the static mixer 6.
The reactor 8 is configured as a horizontal cylinder, in which is disposed a rotor fitted with discs and/or spokes. The vacuum necessary for the reaction in the end reactor is produced via a vacuum system 10 containing spray condensers and pumps. A discharge pump 12 conveys the postcondensed melt to a further processing location at which a granulator 13 and/or a spinning device 14 and/or some other treatment device 15, for example a film casting device, is provided.
The precrushed and compacted undried waste is delivered into the extruder 2, in which the waste is melted, hydrolytic degradation taking place in the melt. This degradation is carried out deliberately via the process conditions and settings. These refer to the degree of moisture in the waste and/or the temperature and/or the height of the vacuum in the extruder 2. Since the extruder 2 is a degasifying extruder, the volatile impurities emerging during the melting process can be extracted. In hydrolytic degradation, the melt reduces its molecular weight, i.e. the degree of polymerization decreases, resulting in the melt becoming less viscous and thus being able to be coarsely filtered with low outlay on pressure or filter area in the filter unit 3 with a filter strength of between 40 and 150 μm.
Ethylene glycol and other additives such as optical brighteners, colouring agents, colour pigments, stabilizers, catalysts are added to the melt via the metering pump 5, good intermixing taking place in the static mixer 6. Then, once the melt has been metered for the reactor 9, it is finely filtered (filter unit 8). By the addition of ethylene glycol, glycolytic degradation also occurs. The combined hydrolytic and glycolytic degradation, controlled via the process conditions and settings in the extruder and via the metered amount of ethylene glycol added, is carried out in a range predetermined by a lower and an upper limit, the lower limit for the degree of polymerization being 15, since below this value there is no longer any reason in using the postcondensation or end finishing reactor 9. The upper limit of the degree of polymerization lies approximately at 35, preferably 30, since otherwise the advantage of the favourable filtration would be lost.
Furthermore, a desired state of the carboxyl terminal groups COOH and of the hydroxyl terminal groups OH should be present at the entrance of the postcondensation reactor 9. The ratio of the terminal groups COOH/OH should be between 0.3 and 0.1 at the entrance of the end reactor 8. Preferably, there is provided before the end reactor 9 a melt viscosimeter, not shown, which measures the viscosity, the addition of the ethylene glycol and/or the other process parameters being controlled in dependence on the measurement result.
In the postcondensation reactor 8 a final polymerization degree of approximately 105 is achieved, by a vacuum of between 3 hPa and 1 hPa and temperatures of between 285° C. and 290° C. being provided; inside the end reactor 9, the final molecular weight is set by the melt being exposed to the vacuum in forming large surfaces, by which means the ethylene glycol easily evaporates out of the product with increasing viscosity. The melt is conveyed through the postcondensation reactor 9 by the inclination of the discs on the rotor and the dwell time is set by the rotational speed and the level. The reaction conditions are controlled in dependence on the results of the measurement of the viscosity by the viscometer 12.
At the end of the reactor, the melt leaves the reactor 9 via a discharge line which is connected to the pump 12. It can be further processed into threads in the spinning device 14 or into films in the casting device 15, or fed into a granulating unit 13.
In a special embodiment of the postcondensation reactor 8, a final polymerization degree of between roughly 150 and roughly 200 can be set. This is achieved by a vacuum of between 0.5 and 1.0 hPa, the rotor of the reactor being realised with greater material strength, such that it withstands the forces occurring with high melt viscosity. A degree of polymerization (DP) of approximately 150 permits the production of PET-bottles, whilst the product with approximately DP 200 is suitable for the manufacture of industrial yarn with high stability, high modulus and low shrinkage. Both bottles and industrial yarn can be produced from the granulated polyester by remelting in the extruder and subsequent injection moulding of the bottle preforms or spinning of the threads. Particularly economic is, however, the direct processing of the melt from the end reactor into preforms or threads, without interim processing of the melt into granules. This last way, which is known for virgin polyester, is accessible also for recycled polyester through the method according to the invention.
EXAMPLE 1
The raw material in the form of coarsely crushed, clean and carefully sorted polyester waste is fed into the extruder at a feed rate of 1300 kg/h and melted there.
The vapours are extracted from the degasifying zone of the extruder at a pressure of 200 mbar.
The electric heating of the extruder is set in such a way that the emerging melt has a temperature of 285° C.
The melt having a viscosity of 20 to 100 Pas is filtered by automatic reversible flow filters with a pore size of 130 μm. All melt lines are heated with a temperature of 290° C.
In a specially designed mixing section, 20 kg/h pre-heated glycol is then metered into and intensively mixed with the melt. By means of a controlled gear pump, the melt is filtered again in an exact amount via an easy-change filter with a pore size of 25 μm and led into the reactor.
The disc reactor has a length of 4.0 m, a diameter of 1.8 m and is fitted with altogether 21 discs of varied perforation and design. The discs are driven at a rotational speed of 1.5 min -1 . In the reactor, the level of the melt is measured and kept constant. The temperature of the reactor is 288° C. and the pressure is controlled around an average value of 1.0 mbar via the viscosity of the end product.
The vapour mixture from 17.1 kg/h EG, 1.6 kg/h water, 0.12 kg/h DEG and oligomers is condensed and led back into a recovery process.
The melt is drawn out of the reactor by means of a special wide-mouthed gear pump at a constant speed and pressed into further processing via a melt viscosimeter; the temperature is 286° C., the pressure 150 bar, the viscosity 260 Pas.
EXAMPLE 2
In a pilot plant, 25 kg/h PET granules having an intrinsic viscosity (i.v.) of 0.636 dl/g and carboxyl terminal groups of >33 mmol/kg are melted in an extruder at temperatures of 270-290° C. Then, the polymer stream is mixed with 190 g/h ethylene glycol and led to the end reactor. The end reactor has a diameter of 0.6 m and a length of 1.2 m. With a melt temperature of approx. 285° C., a vacuum of approx. 3 mbar and a rotor speed of 0.5 min -1 , an intrinsic solution viscosity in the product of i.v.=0.65 dl/g is achieved. The carboxyl terminal groups are here less than 25 mmol/kg. The liquid polymer is solidified into strands and granulated.
The PET granulate with i.v.=0.65 dl/g, produced in this manner, is melted again in a spunbonded nonwoven installation in an extruder. The polymer throughput amounts to approximately 42 kg/h. The liquid polymer is fed in by means of gear pump through nozzles having hole diameters of 0.4 mm and processed into spunbonded nonwoven with filament speeds of 4000 m/min. The titre is 3 dtex, the area weight 30 g/m 2 . The spunbonded nonwoven is 660 mm wide.
While preferred embodiments, forms and arrangements of parts of the invention have been described in detail, it will be apparent to those skilled in the art that the disclosed embodiments may be modified. Therefore, the foregoing description is to be considered exemplary rather than limiting, and the true scope of the invention is that defined in the following claims.
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A method and device for recovering linear polyesters, such as PET and PBT, from polyester waste of the most varied form, in a continuous manner, in which undried or not dried-through waste is melted, the polymer chains being hydrolytically degraded by adhering moisture, and in which diol, corresponding to the basic constitutional unit of the polymer, is added to the melt resulting in glycolytic degradation, and the melt so treated is further condensed to the desired degree of polymerization.
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This invention concerns the preparation of pure zirconium from ore which may be, for example, zircon or baddeleyite, etc., and which typically also contains varying amounts, e.g., about 2-3% by weight, of hafnium containing materials.
In the processing of zircon ore to recover pure zirconium, it is conventional to comminute zircon with petroleum coke, chlorinate the products thereof and separate the crude zirconium tetrachloride (ZrCl 4 ) containing hafnium values from by-products such as carbon monoxide and silicon tetrachloride, and then complex the zirconium and hafnium values with ammonium thiocyanate (NH 4 SCN), and extract from an acidic aqueous solution the hafnium complex from the zirconium complex with an organic solvent such as methyl isobutyl ketone (MIBK). This process is described in the literature and, more particularly, in U.S. Pat. Nos.: 2,938,769; 3,069,232; 3,006,719; and 4,202,862; and the references cited therein, the disclosure of which are incorporated herein by reference.
In the operation of such a process, it is conventional practice to recover the extracting solvent and NH 4 SCN which are expensive materials, and which are employed in large quantities in this process. Exemplary apparatus, process, and conditions for carrying out such solvent and NH 4 SCN recovery is described in the aforesaid U.S. Pat. No. 3,006,719; wherein, in the present process as described hereinafter in detail, separation columns 3, 4 and 5 thereof and their operating parameters substantially as described therein may be employed. However, as described in the aforesaid U.S. Pat. No. 4,202,862, the regeneration of solvent and NH 4 SCN, has been attended with the problem of producing objectionable odors from the process apparatus.
In general in such separation procedures for isolating zirconium and hafnium values, the zirconium and hafnium raffinates are subsequently treated with regenerated solvent to remove thiocyanic acid (HSCN), then steam-stripped to recover dissolved and entrained solvent, then treated with ammonium sulfate to precipitate zirconium or with ammonia (NH 3 ) to precipitate hafnium. The precipitated metal values are recovered by filtration and calcined to produce oxides. When certain organic sulfur compounds, produced in the solvent and NH 4 SCN regeneration step, contact the acid raffinates, they are converted to noxious odiferous compounds, and can then easily escape into the atmosphere, since filtration, calcination and the like, are typically not conducted in sealed equipment.
It is a principal object of the present invention, therefore, to provide a process for separating zirconium and hafnium values wherein a thiocyanate complexing agent is employed, and wherein the odor problems caused by certain sulfur compounds formed in the NH 4 SCN/solvent regeneration procedures, are essentially eliminated.
BRIEF DESCRIPTION OF THE INVENTION
These and other objects hereinafter appearing have been attained in accordance with the present invention which is defined in its general sense as the process for separating zirconium values from hafnium values comprising the steps:
(A) forming a solvent extraction system comprising an organic solvent phase and an acidic aqueous phase;
(B) feeding to or forming in-situ in said system thiocyanate complexes of zirconium and hafnium;
(C) maintaining a concentration of HSCN in said system;
(D) separating the solvent phase containing the hafnium values and HSCN from the aqueous zirconium raffinate;
(E) stripping the hafnium values from the solvent phase from (D) to produce an aqueous hafnium raffinate;
(F) returning a major portion of the stripped solvent from (E) to the extraction system of (A);
(G) separating the thiocyanate (SCN - ) values from the minor portion of stripped solvent from (E);
(H) removing from the solvent from (G) essentially all thiazolines;
(I) scrubbing said zirconium and hafnium raffinates with the purified solvent from (H) to remove essentially all HSCN values therefrom;
(J) stripping with steam dissolved and entrained solvent from the scrubbed raffinates (I); and
(K) returning said recovered solvent (J) to (G).
BRIEF DESCRIPTION OF THE DRAWING
FIG. 1 is a partial schematic of the zirconium-hafnium separation process of the present invention.
DETAILED DESCRIPTION OF THE INVENTION
Referring to the schematic in FIG. 1, crude ZrCl 4 containing the hafnium material, or as stated in U.S. Pat. No. 3,006,719, the oxychloride (oxide-chloride) of the metals, dissolved in water and adjusted to an acidity of about 5 normal with aqueous ammonia (NH 4 OH) is introduced via line 11 to the NH 4 SCN stream line 12. In a manner substantially described in said U.S. Pat. No. 3,006,719, the resultant material is fed into the extraction column 10 containing the liquid-liquid extraction media MIBK and thiocyanate. It is noted that thiocyanate complexes of the zirconium and hafnium may also be formed in the extraction column.
Hydrochloric acid (HCl) and sulfuric acid (H 2 SO 4 ) are passed to the top of column 10 via line 13 from column 40 while MIBK and thiocyanate recycle are added at the bottom via line 14. At the top of column 10, an organic phase comprising MIBK, hafnium thiocyanate complex, and other compounds, is recovered and passed via line 15 to column 40 where it is countercurrently contacted with downwardly flowing H 2 SO 4 and HCl entering via line 16. At the bottom of column 10, a zirconium oxychloride (ZrOCl 2 ) solution or raffinate is recovered via line 17. In addition to ZrOCl 2 , the recovered raffinate will contain ammonium chloride (NH 4 Cl) and HSCN, which may be recovered by scrubbing, in column 20, with the purified MIBK via line 18 in accordance with the present invention as more fully described hereinafter. From the bottom of column 50, the acid-scrubbed hafnium material is recovered via line 19 and will comprise primarily hafnium oxysulfate and H 2 SO 4 ; MIBK and HSCN are recovered at the top of column 50 and passed via lines 20 and 24 to thiocyanate regeneration mixer settler 80 wherein the HSCN is reacted with NH 3 and NH 4 OH entering the mixer settler via lines 22, 23, and 24. The NH 4 SCN recovered from the mixer settler 80 is passed via line 12 for admixture in with the zirconium and hafnium oxychloride solution to column 10. MIBK is recovered from mixer settler 80 and passed via line 25 to distillation column 90. Distilled MIBK passes via lines 26 and 18 to the thiocyanate recovery column 20. Distilled MIBK also passes via lines 26 and 27 to column 50 for thiocyanate recovery. It is contemplated that from about 60 to 80% of the MIBK and HSCN recovered at the top of column 50 is recycled directly via line 14 into column 10.
The above description of the basic structural elements and material flow patterns are, as stated above, substantially as described in U.S. Pat. No. 3,006,719, except for distillation column 90. As will now be described, the present invention utilizes additional and uniquely placed equipment and flow patterns.
Referring further to the schematic, in Applicants' process, a distillation column 90 is placed in line 25 and is operated to essentially completely purify all the solvent from the thiocyanate regeneration mixer-settler 80. It is particularly noted that this unit 90 is operated as a pure distillation unit and not merely a partial steam stripping unit, with the result that all sulfur-containing compounds such as the thiazolines which are precursors for the formation of odiferous mercaptoketones in the acidic aqueous phase are removed. The bottoms or tars, containing the sulfur compounds and the precursor thiazolines, are continuously removed via line 30. The distillation eliminates these precursors from the recycle regenerated solvent system. It is also noted that the point of entry of this purified recycle solvent into the extraction columns 20 and 50 are such as to intimately scrub essentially all of the residual thiocyanate from the zirconium and hafnium raffinates and thus further insure a thiocyanate-free raffinate for use in subsequent processing. The purified MIBK will also scrub odiferous mercaptoketones from the raffinates and therefore insure that subsequent processing does not release the odiferous mercaptoketone compounds to the atmosphere. The point of contact of the raffinate with the purified solvent may, of course, be outside of the extraction columns 20 and 50. There are substantial advantages in retaining solvent and scrubbed-out thiocyanate within the column for use therein.
Useful and typical operating feed rates and conditions for the basic process in which the present invention is utilized are described in detail in the aforesaid U.S. Pat. No. 2,938,769, and are specifically enumerated in Example 1 thereof, with the modification, of course, of there being essentially zero concentration of thiazolines in the purified MIBK stream from the present distillation unit going to the raffinate scrubbers. The distillation unit 90 can be of conventional design and construction and may be plate or packed column or the like and sized according to the throughput of a particular system design. If properly sized the distillation unit should readily accommodate the solvent feed rates as described, for example, in the aforesaid U.S. Pat. No. 2,938,769, or even scaled up to commercial quantities on the order indicated in the aforesaid U.S. Pat. No. 4,202,862. It is noted that multiple apparatus units and multiple purification passes may be utilized as is well known to the art and illustrated, for example, in U.S. Pat. No. 2,938,769, wherein a supplemental HCl stripping operation is employed for improving zirconium values recovery. Any separation technique which removes sulfur-containing compounds, such as the thiazoline precursors, from the regenerated solvent may be utilized as well.
In addition to the odiferous mercaptoketone compounds being removed by the purified MIBK in columns 20 and 50, the raffinates from columns 20 and 50 feed steam stripper columns 30 and 60 respectively to remove dissolved and entrained MIBK. The MIBK-free raffinates are further processed into oxides. The MIBK removed from the raffinates is captured and passed via lines 28, 29 and 24 to the thiocyanate regeneration mixer-settler 80. This mercaptoketone-containing MIBK enters mixer-settler 80 and when it leaves via line 25 the odiferous mercaptoketones have been converted into sulfur-containing thiazoline compounds, which are subsequently removed in distillation column 90. This recycle of MIBK to the thiocyanate regeneration mixer-settler 80 is a precaution to remove odiferous mercaptoketone compounds should the distillation column not achieve complete removal of the odor precursor thiazolines or experience an upset condition.
In certain preferred embodiments of the invention, the SCN - values of (G) are converted to NH 4 SCN prior to or during separation thereof from the solvent, the NH 4 SCN is used to form the thiocyanate complexes of (B), the zirconium and hafnium raffinates are essentially isolated from the extraction system before scrubbing with purified solvent from (H) in (I), solvent from (G) for scrubbing is purified in (H) by distillation, the scrubbed raffinates are steam-stripped to recover solvent in (J), and the recovered solvent is returned to (G).
In the present process, the HSCN-free solvent from (G) is treated in step (H) to remove other materials, particularly elemental sulfur and sulfur compounds dissolved or suspended in it. Of particular importance is the removal in this step of certain thiazolines, which on contact with aqueous acid in steps (I) and (J) are hydrolyzed to produce odiferous mercaptoketones.
It has been demonstrated by F. Asinger et al, Annalen der Chemie, Vol 672, (1964), pages 156-178, that reaction of MIBK with sulfur and NH 3 at 20 degrees C to 40 degrees C for eight hours produces a mixture of 2-methyl-2,4-diisobutyl-Δ 3 -thiazoline (i) and 2,4-dimethyl-2-isobutyl-5-isopropyl-Δ 3 -thiazoline (ii). In the publication and in a subsequent one (ibid, pages 179-193), they show that these Δ 3 -thiazolines are hydrolyzed by aqueous acid to give, in the case of (i), 1-mercapto-4-methyl-2-pentanone (iii), and in the case of (ii), 3-mercapto-4-methyl-2-pentanone (iv). These mercaptoketones are detected by the human nose at concentrations in air in the range below one part per billion (ppb), and have a highly unpleasant odor which has been compared by some to that of the urine of the domestic cat. Asinger et al also show, as reported in their above-cited first publication, that mercaptoketones (iii) and (iv) will react with NH 3 and MIBK to yield, respectively, the Δ 3 -thiazolines (i) and (ii).
The presence of the thiazolines (i) and (ii) and of the mercaptoketones (iii) and (iv) in zirconium-hafnium separation process streams was established as follows.
Before step (H) was instituted, an impinger trap containing dilute H 2 SO 4 was used to sample a particularly odiferous discharge, that from the exhaust of a pump used to generate the vacuum required for the filters with which zirconium sulfate is recovered after precipitation from the zirconium raffinate of (I). The H 2 SO 4 was extracted with chloroform, and the chloroform extract submitted to gas chromatography, with mass spectroscopic analysis of each material eluted from the chromatography column. In this way it was shown that a chromatogram peak previously associated with the mercaptoketone odor was a mixture of the two isomeric mercaptoketones (iii) and (iv). Positive identification of these compounds by gas chromatography was henceforth possible.
Again before step (H) was instituted, a sample of zirconium raffinate was taken from the process after step (I), that is, after contact with regenerated solvent for the purpose of removing HSCN. This sample was extracted with chloroform, and the chloroform extract submitted to gas chromatography, with mass spectroscopic analysis of each material eluted from the chromatography column as before. The mercaptoketones (iii) and (iv) were found in this sample too, but also found were the two 3 -thiazolines (i) and (ii). The chromatographic peaks associated with the thiazolines were now identified, so that subsequently these materials could be detected chromatographically.
By these expedients, the odiferous compounds were positively identified, the presence of thiazolines in the process stream was demonstrated, and the exact nature of the compounds responsible for certain gas-chromatographic peaks established.
In the following, we show that sulfur is always present in the equipment in which step (G) is carried out. We show that reaction of NH 3 , sulfur and MIBK indeed results in formation of the Δ 3 -thiazolines (i) and (ii) as claimed by Asinger et al, and that hydrolysis of these Δ 3 -thiazolines with aqueous HCl indeed produces the mercaptoketones (iii) and (iv), again in agreement with the findings of Asinger et al. We show that the Δ 3 -thiazolines (i) and (ii) are always detectable in the solvent from step (G), and that mercaptoketones (iii) and (iv) are always detectable in the zirconium raffinates from step (I) and especially in the recovered solvent from step (J) unless the solvent from step (G) has been subjected to purification by use of step (H). Further, we show that the mercaptoketones (iii) and (iv) found in the recovered solvent from step (J), when solvent from step (G) has not been purified by step (H), are converted to the Δ 3 -thiazolines (i) and (ii) by treatment with NH 3 . Finally, we show that the Δ 3 -thiazolines (i) and (ii) are essentially completely removed when the solvent is subjected to a treatment such as, for example, fractional distillation, as in step (H).
Samples of solid materials from the equipment used to carry out step (G) were submitted for X-ray powder-diffraction examination. The angular positions of the X-ray diffraction-peaks, taken with CuK radiation, were converted to d-spacing values and compared with those tabulated by the Joint Committee on Powder Diffraction Standards (JCPDS), Card No. 24-733, for orthorhombic sulfur, as shown in Table 1. It is seen that the correspondence is conclusive evidence that the solids are orthorhombic sulfur.
TABLE 1______________________________________d-Spacings and peak intensities for solids from thio-cyanate regeneration equipment and for orthorhombic sulfuras given by JCPDS, 24-733.Solids fromthiocyanate regeneration Orthorhombic sulfurd, A I/I.sub.o d, A I/I.sub.o______________________________________4.07 15 4.060 123.93 22 3.918 163.86 100 3.854 1003.59 11 3.570 73.46 37 3.447 373.35 46 3.336 223.23 49 3.219 413.12 26 3.113 203.10 18 3.084 152.86 22 2.848 172.63 17 2.625 112.58 5 2.569 32.51 15 2.502 72.43 11 2.426 122.38 7 2.378 42.30 6 2.289 62.12 19 2.113 111.992 5 1.9892 31.905 11 1.9038 81.823 5 1.8236 51.786 12 1.7824 121.757 6 1.7563 71.726 9 1.7271 71.702 7 1.6785 8______________________________________
Sulfur (24 g) was added to MIBK (187 ml) in a four-neck flask fitted with an inlet tube reaching to the bottom of the flask, an outlet tube starting well above the liquid level, a stirrer, and a thermometer. The temperature was raised to 40 degrees C and NH 3 gas bubbled through the stirred mixture at a rate of a few bubbles per second for eight hours. The reaction mixture was cooled to room temperature, the liquids decanted away from the settled solids, the aqueous layer rejected and the organic layer diluted with ether, washed neutral with water, dried with anhydrous sodium sulfate (Na 2 SO 4 ), separated from the Na 2 SO 4 , and the ether distilled away. The residue left after ether removal was distilled under vacuum, and following Asinger et al, the fraction boiling at 60 degrees C to 70 degrees C at a pressure of 0.3 mm of mercury (Hg) was collected. This was analyzed by gas chromatography, and the presence of the thiazolines (i) and (ii) established.
Following further the procedures of Asinger et al, the fraction boiling at 60 degrees C to 70 degrees C and 0.3 mm Hg (4 gm) was added to a mixture of 1N HCl (200 ml) with dioxane (50 ml) in a flask fitted with a reflux condenser and boiled under total reflux for five hours. The flask and its contents were cooled, extracted with ether and the ether solution washed with dilute sodium bicarbonate solution, then with water, until neutral, then dried with anhydrous Na 2 SO 4 . The ether was then distilled away, and the residue fractionally distilled at a pressure of 11.5 mm of Hg. Two fractions were recovered, one boiling at 62 degrees C to 68 degrees C and another boiling at 72 degrees C to 74 degrees C. These boiling ranges are consistent with those given by Asinger et al for mercaptoketones (iii) and (iv). The presence of mercaptoketones (iii) and (iv) in the samples was confirmed by gas chromatography.
Acid hydrolysis of the thiazoline mixture to yield the mercaptoketones (iii) and (iv) was demonstrated without the presence of dioxane.
Samples of solvent from step (G) were repeatedly analyzed by gas chromatography, and peaks characteristic of the Δ 3 -thiazolines (i) and (ii) identified routinely.
Before operation of step (H) for purification of regenerated solvent, samples of solvent recovered by steam-stripping aqueous raffinates that had been treated for removal of HSCN invariably showed high levels of mercaptoketones when analyzed by gas chromatography. When this solvent was treated with NH 4 OH, analysis by chromatography showed conversion of the mercaptoketones to thiazolines.
Samples of regenerated solvent from step (G) were subjected to laboratory-scale, batchwise fractional distillation and early, middle and late fractions analyzed for thiazolines by subjecting them to acid hydrolysis then analyzing for mercaptoketones. The results of this were that mercaptoketones were undetectable in the products of acid hydrolysis of the first third of the solvent to be distilled, and this was sufficiently encouraging to test a continuous, pilot-scale distillation of regenerated solvent. This was done as described in the following example.
EXAMPLE
A pilot-scale distillation system was designed and assembled to remove odiferous mercaptoketone precursors from regenerated solvent. The system consisted primarily of a 50-liter glass reboiler, a 6" ID ×9 ft high packed column, and a stainless-steel water-cooled condenser. The reboiler was equipped with an internal steam coil constructed of 3/4" zirconium tubing and having a heat-transfer surface area of approximately 30 ft 2 . The column section was packed with nearly nine feet of 5/8" ceramic saddles supported by a bottom sieve plate. The overhead condensate product was collected in a 20-gallon stainless steel storage tank; some of this material was refluxed to the top of the column as required to achieve the desired mass-transfer efficiency. All process equipment, except for the condenser, was insulated to minimize heat losses.
A 56-hour distillation run was performed using this system. Regenerated solvent, having an average total solids concentration of 1.75 g/l, was continuously introduced to the column at a feedrate of about six gallons per hour, and distilled solvent was continuously withdrawn as product. The reboiler temperature was maintained at 135 degrees C by adding 28 pounds per hour of saturated steam at 57-58 psig. Three gallons per hour of distilled solvent were refluxed back to the column, giving a reflux ratio of 0.5.
Pressure drop across the packing and support plate was 3/8 inch of water. The condenser cooling water flowrate was 1.3 gallons per minute; the water inlet and outlet temperatures were 19 and 25 degrees C, respectively. The heavy liquid in the reboiler, containing sulfur, high-boiling "tars" and the thiazoline precursor compounds, exhibited a total solids concentration of approximately 500 g/l. A half liter of this material was tapped as bottoms every eight hours, resulting in a solids concentration factor of roughly 300:1.
The overhead distillate product obtained during this run was water-clear, and subsequent chromatographic analysis did not detect the presence of odiferous mercaptoketone precursors (the chromatogram only showed the peak for MIBK and some instrument noise). Distillate samples were also subjected to acid hydrolysis at elevated temperature in the laboratory in an attempt to generate odiferous mercaptoketones from any residual thiazoline precursor compounds which may have been present. In this procedure, solvent, 20 ml, was intimately contacted with sufficient 2N HCl to give a total volume of two liters. One liter of the resulting aqueous solution was then refluxed for 90 minutes at 103-105 degrees C. After any floating solvent was removed, the sample was submitted for analysis. No odiferous mercaptoketones were detected, confirming that precursor-free solvent had indeed been produced. Therefore, fractional distillation is an acceptable technique for removing thiazolines from regenerated solvent and thereby substantially eliminating odiferous mercaptoketone emissions.
The invention has been described in detail with particular reference to preferred embodiments thereof, but it will be understood that variations and modifications will be effected within the spirit and scope of the invention.
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A process for separating zirconium values from hafnium values wherein an aqueous solution of ZrCl 4 and HfCl 4 is contacted with NH 4 SCN, feeding the resultant solution into a solvent extraction system containing aqueous HCl and MIBK, separating off the solvent phase containing MIBK, HSCN, hafnium thiocyanate complex, and any decomposition products of HSCN to leave the aqueous phase raffinate containing NH 4 Cl, zirconium oxide-chloride and low concentrations of HSCN, scrubbing the hafnium values from the separated solvent phase, treating the scrubbed solvent phase containing MIBK and HSCN with NH 4 OH to convert the HSCN to NH 4 SCN, separating the NH 4 SCN from the treated solvent phase, treating the separated solvent phase to remove essentially all thiazolines, and scrubbing residual HSCN from the raffinate with the desulfurized solvent phase.
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This is a continuation, application Ser. No. 655,044, pending filed Feb. 4, 1976, which is a continuation of application Ser. No. 503,538, filed Sept. 5, 1974, now abandoned.
BACKGROUND
This invention relates to certain polyamide copolymers prepared from unbranched aliphatic dicarboxylic acids and a diamine mixture. More particularly, this invention relates to such polyamide copolymers which are useful as melt adhesives, especially for textiles.
It is known that certain polyamides can be applied as melt adhesives for textiles. The use of a polyamide for this purpose requires a good washing resistance to warm washing suds and a special melting characteristic that allows for processing in a technical important temperature range of about 120°-160° C.
It is also known that the melting behavior of a polyamide can be adjusted by copolymerization.
A further demand for textile melt adhesives is a high water absorption so that the vapor diffusion is not affected in the glued materials.
Up to the present, all polyamides, which have been used as textile melt adhesives, have shown, when in powder form, a tendency to bake or fuse together, especially when they contain aminocarboxylic acids. Therefore, additives are regularly mixed to these powders in order to improve the trickling ability. If the aminocarboxylic acids are omitted at mean average molecular weight (Mn), the fusion is decreased, but the range of melting temperatures is so small, that the polyamide cannot be processed in the common machines.
There is a need to transfer the good effect realized by use of branched diamines to compounds free of amino acid.
SUMMARY
The present invention provides polyamides of certain composition and a special range of molecular weight which polyamides in powder form do not fuse together, but show all advantages of the suitable polyamides known as melt adhesives.
The present invention thus relates to a polyamide copolymer of unbranched, aliphatic dicarboxylic acids with 6 to 20 C-atoms and a diamine mixture consisting of
(a) 20-80 mol percent, preferably 20-70 mol percent unbranched aliphatic diamines with 6-20, preferably 6-12 C-atoms and
(b) 80-20 mol percent, preferably 80-30 mol percent, branched, aliphatic and/or cycloaliphatic diamines
with a molecular weight of 2000-40000, preferably 6000-25000, as melt adhesive, especially for textile materials.
DESCRIPTION
Smaller quantities of aminocarbonic acids and their lactames can also be used, in this case, however, the molar ratio of dicarboxylic acid: aminocarboxylic acid may not fall below>9:1.
For preparing copolyamides unbranched aliphatic dicarboxylic acids with 6-20 C-atoms, as adipic-, pimelic-, suberic-, azelaic- and sebacic acid as well as undecane-, dodecane-, octadecanedicarbonic acid and others are suitable.
If desired, it is also possible to use smaller quantities of others than unbranched dicarbonic acids in order to control the melting viscosity.
As suitable unbranched aliphatic diamines with 6-20, preferably 6-12 C-atoms, hexamethylene-, heptamethylene-, octamethylene-, nonamethylene-, decamethylene-, undecamethylene-, dodecamethylene diamine and others can be mentioned for example.
As branched aliphatic and cycloaliphatic diamines the following compounds with 3-15 C-atoms can be mentioned especially for example: 1,2-propylene diamine, 2-and 3-methylhexamethylene diamines, 3-isopropyl-hexamethylene diamine, 2-tert, butyl-hexamethylene diamine, 2,3-, 2,4-, 2,5-, 3,3- and 3,4-dimethylhexamethylene diamine, 3-isooctyl-hexamethylene diamine, 3-iso-dodecylhexamethylene diamine, 2-methyl-4-ethylhexylmethyl diamine, 2,2,4- and 2,4,4-trimethylhexamethylene diamine, 2,2,5,5-tetramethylhexamethylene diamine, 2,4-diethyl-octamethylene diamine and others as well as the cycloaliphatic diamines, like 3,6-diamino-2-methylcyclohexane, 3-aminomethyl-3,5,5-trimethylcyclohexylamine, 4,4'-bis-aminomethyl-2,2'-dimethyl-dicyclohexylmethane and the like. Thereby especially those diamines which have 3 alkyl radicals, are preferred as the 1:1 mixture of 2,2,4- and 2,4,4-trimethylhexylene diamine and the 3-aminomethyl-3,5,5-trimethylcyclohexylamine. Naturally, also mixtures of these compounds can be applied. Advantageously are those which contain as well aliphatic as cycloaliphatic diamines.
As suitable aminocarboxylic acids and their lactams especially those with 4-12 C-atoms are to mention, as the ε-aminobutane-, ε-aminocaproic-, ε-aminododecane acid (ε-aminolaurine acid) and others.
It is preferred to manufacture the copolyamides by prior art methods, whereby the starting materials are heated from 150°-250° C. until the desired molecular weight is reached. This takes in general 2-5 hours, whereby the reaction time depends on the magnitude of the condensation. In known manner the molecular weights can be adjusted by using a slight excess of diamine- or dicarboxylic acid or by adding monofunctional amines or car acids.
The advantages of the copolyamides with respect to their use as melt adhesives, especially for textiles, is shown by the examples.
The use of mono- and dibranched diamines of the invention results in a decrease of the baking.
The subject of the present invention is illustrated by the following examples. In order to show the applicability of the manufactured copolyamides, a so-called baking-test is performed, which test is described follows.
Baking test
In a cylindrical form of 5 cm interior diameter a tablet of the testing material is pressed at a pressure of 0.12 kg/cm 2 . The form is divided in the plain into two parts, which forms with the axis of the cylinder an angle of 90°. Both parts of the form are pulled apart in a testing machine in radial direction. The necessary power is related to the cross-section of the tablet and serves for the estimation of the baking of the material.
EXAMPLE 1
A polyamide of 1.0 mol adipic acid, 0.4 mol hexamethylene diamine, 0.3 mol 3-aminomethyl-3,5,5-trimethylcyclohexylamine (IPD), 0.3 mol of a 1:1 mixture of 2,4,4- and 2,2,4-trimethylhexamethylene diamine (TMD) and 0.03 mol caprolactam is produced by melt condensation according to known methods (5 hours at from 150° to 250° C. increasing temperature). The molecular weight was approximately 8000. The melt flow index had a value of approximately 12 at 160° C. and under a load of 2.16 kg. The product was reduced to a granular size of 80-200 μ and was subjected to a baking test. Thereby a value of 44 g/cm 2 was measured.
If the caprolactam part in the above mentioned composition is increased to 0.2 mol, the value of the baking goes up to 90 g/cm 2 .
EXAMPLE 2
A polyamide of 1.0 mol adipic acid, 0.2 mol dodecamethylene diamine and 0.8 mol TMD was produced by melting condensation according to example 1. The molecular weight was approximately 10000. The melting index at 160° C. and a load of 2.16 kg was 7. Reduced to a granular size of 80-200 μ the product showed at the baking test a value of 38 g/cm 2 .
EXAMPLE 3
A polyamide of 1.0 mol adipic acid, 0.2 mol dodecamethylene diamine and 0.8 mol 3-methylhexamethylene diamine was produced by melt condensation according to example 1. The molecular weight was approximately 10000. The melt flow index at 160° C. and under a load of 2.16 kg was 10.
Reduced to a granular size of 8-200 μ, the product showed at the baking test a value of 60 g/cm 2 .
EXAMPLE 4
A copolyamide of 1.0 mol azelaic acid, 0.6 mol hexamethylene diamine, 0.2 mol IPD and 0.2 mol TMD was produced according to example 1. The molecular weight was approximately 12000. At 160° C. and a load of 2.15 kg the melt flow index was 8. The value of the baking test measured at a powder of the granular size of 80-200 μ, was 30 g/cm 2 .
EXAMPLE 5
A copolyamide of 0.8 mol dodecane dicarbonic acid (1,12), 0.2 mol azelaic acid, 0.7 mol hexamethylene diamine, 0.15 mol IPD and 0.15 mol TMD was produced according to example 1 and mixed with 10 weight percent N-methylbenzene sulfonamide. The molecular weight was approximately 18000. At the pulverized material the following values were measured:
______________________________________granular size 80-200 μmelt flow index at160° C. and a loadof 2.16 kg 13baking test 42 g/cm.sup.2______________________________________
EXAMPLE 6
A copolyamide of 0.8 mol octadecanediacid-(1.18), 0.2 mol adipic acid, 0.7 mol 1.18-diaminooctadecane, 0.15 mol 3.3-dimethylpentane diamine-(1.5) and 0.15 mol 1-methyl-3,6-diaminocyclohexane was produced according to example 1. The molecular weight was approximately 12000. It had a melting index of 11 at 160° C. and a load of 2.16 kg. The value of the baking test, measured at a powder of the granular size of 80-200 μ, was 64 g/cm 2 .
The datas mentioned in the foregoing examples can be conformed by small modifications of the composition also to other demands. Therefore they do not mean a limitation. The molecular weights were stabilied in common manner.
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A polyamide copolymer, useful as a melt adhesive especially for textiles, produced from the following monomers
1. An unbranched aliphatic dicarboxylic acid with 6-20 C-atoms;
2. A diamine mixture consisting of
(a) 20-80 mol percent, unbranched aliphatic diamines with 6-20 C-atoms; and
(b) 80-20 mol percent branched aliphatic and/or cycloaliphatic diamines;
said copolymer having a molecular weight of 2000-40000.
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BACKGROUND OF THE INVENTION
The field of the present invention relates to small-sized vehicles such as motorcycles, motor tricycles and the like.
In the above-referred small-sized vehicles, normally there is provided a fairing for covering a front portion of a vehicle body over its front surface as well as its both left and right side surfaces. And in a vehicle provided with such fairing rear view or, back-mirrors are mounted at the upper side portions of the fairing via arm members projecting from the side portions as disclosed for example, in Japanese Utility Model Publication No. 60-17429. Also, in Laid-Open Japanese Patent Specification No. 58-49538 is disclosed a back-mirror device which is constructed in such manner that when on external load is applied thereto it may turn to avoid the external load. In these back-mirror devices, the above-mentioned arm member becomes thick and has a large wind pressure area because it must rigidly support the back-mirror so as not to induce rocking or vibration, and moreover, as it project to the side of the vehicle body, an air resistance upon running of the vehicle would be increased by this arm member.
A back-mirror device having a structure in which the arm member is made of two parts taking into consideration an aerodynamic characteristic, is known by Laid-Open Japanese Patent Specification No. 59-32534. In this back-mirror device, an arm member for supporting a mirror is formed of two thin arm portions. However, this cannot fully prevent vibration of a mirror resulted from running of a vehicle.
SUMMARY OF THE INVENTION
The present invention relates to improvements in the heretofore known back-mirror device as described above, and has it as an object to provide a back-mirror device in which a back-mirror is rigidly supported by an arm member that has a small air resistance but yet has sufficient rigidity, and has excellent external appearance.
To that end, according to the present invention, in a back-mirror device for small-sized vehicles of the type that a rear view mirror is mounted to an upper side portion of a fairing which covers a front portion of a vehicle body by the intermediary of an arm member projecting from the side portion, the above-mentioned arm member is provided with an opening which penetrates through the arm member in the direction of running of the vehicle.
According to the present invention, since running wind striking the arm member would smoothly flow backwards through an opening at a central portion, an air resistance is reduced. Moreover, this opening would not largely affect the rigidity of the arm member, and the arm member holds a high rigidity owing to arm portions respectively formed above and below the opening and spaced from each other, and can firmly support a back-mirror.
In addition, according to the present invention there is provided a back-mirror device which can effectively avoid an external load in the event that the external load has been applied to a mirror, which comprises an aerodynamically excellent arm member, and which can prevent vibration of a mirror caused by vibration of a vehicle body as such as possible.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a side view of a motorcycle provided with a back-mirror device according to a first preferred embodiment of the present invention;
FIG. 2 is a front view of the same motorcycle;
FIG. 3 is a perspective view of an upper fairing of the same motorcycle;
FIG. 4 is a cross-section view taken along line IV--IV in FIG. 3 as viewed in the direction of arrows;
FIG. 5 is a cross-section view taken along line V--V in FIG. 3 as viewed in the direction of arrows;
FIG. 6 is a cross-section view taken along line VI--VI in FIG. 2 as viewed in the direction of arrows;
FIG. 7 is a perspective view of a back-mirror device according to a second preferred embodiment of the present invention;
FIGS. 8 and 9 are perspective views for explaining operations of the same back-mirror device;
FIG. 10 is a perspective view of a back-mirror device according to a third preferred embodiment of the present invention;
FIG. 11 is a partial enlarged perspective view of FIG. 10;
FIG. 12 is a perspective view for explaining an operation of the same back-mirror device;
FIG. 13 is a plan view, partly cut away, of a back-mirror device according to a fourth preferred embodiment of the present invention;
FIG. 14 is a rear view, partly cut away, of the same back-mirror device; and
FIG. 15 is a cross-section view taken along line XV--XV in FIG. 13.
DETAILED DESCRIPTION OF PREFERRED EMBODIMENTS
FIG. 1 is a side view of a motorcycle to which the present invention has been applied, and FIG. 2 is a front view of the same. A front wheel 1 is suspended by a front fork 2, and this front fork 2 is connected at its top end to a handle bar 3 via a handle rotary shaft. A rear wheel 4 is rotatably supported at a rear end of a rear fork 5 that is rockably supported from a vehicle body frame. At the rear of the handle bar 3 are sequentially disposed a fuel tank 6, a seat 7 and a rear-seat 8 along a center line of the vehicle body. A front portion of the vehicle body is covered by a fairing 9. The fairing 9 extends over the front surface and the left and right side surfaces of the vehicle body, and an opening 10 is formed in the lower portion of its front surface. The above-mentioned front wheel 1 and the front fork 2 are led out to the exterior through this opening 10. Upon running, running wind would flow into the interior of the fairing 9, and would cool a radiator 11 and an engine mounted at the rear lower position of the radiator.
The fairing 9 is divided into an upper fairing 9a and a lower fairing 9b at a severing line 12, and they are respectively mounted to the vehicle body. At the front central portion of the upper fairing 9a is provided a head light 13, and at the lower edge portion of the upper fairing 9a are provided a pair of left and right front winkers 14 in the front surface portions along the severing line 12 as positioned on the opposite sides of the opening 10, as shown in FIGS. 3 and 5. In addition, at the upper portion of the upper fairing 9a are mounted rear view or back-mirrors 15 as projecting sidewards via arm members 16. FIG. 3 is a perspective view of the upper fairing 9a.
Each of the front winkers 14 is mounted to the front portion at the lower edge of the upper fairing 9a by placing mount pieces 17 and 18 projecting from its upper edge and its rear edge along the inner surface of the upper fairing 9a and fastening them with bolts 19 and 20, respectively. In the upper fairing 9a are formed notches 21 each of which conforms to the profile of the front surface of the front winker 14, and when the front edge portion of the front winker is fitted in this notch 21, and outer surface of a lens of the front winker 14 forms a surface that is flush with the outer surface of the upper fairing 9a, that is, an extension surface that is smoothly continuous to the outer surface of the upper fairing 9a. At the lower edge portion of the front winker 14 is provided a plug piece 23 as projected therefrom, and by inserting this insert piece 23 into a forked receptacle 24 formed at the upper edge of the lower-fairing 9b, the lower edge of the front winker 14 can be detachably supported from the lower fairing 9b. The outer surface of the lower fairing 9b and the outer surface of the lens 22 also form a smoothly continuous single surface.
The back-mirror 15 is provided at the upper side portion of the upper fairing 9a via the arm member 16 as projected therefrom as described above, an opening 25 penetrating through the arm member 16 in the back and forth direction, that is, from the forward to the rear side of the mirror housing is formed in the arm member 16, and the arm member 16 is divided into upper and lower arm portions 26, 26 by this opening 25. As shown in FIG. 6, the respective arm portions 26, 26 have a transverse cross-section of stream line shape that expands gradually from the forth towards the rear, and hence, upon running, running wind striking this arm member 16 would favorably pass through the outside of the arm member 16 and through the opening 25 as guided by the arm portions 26, 26. Accordingly, it can be avoided that either a large wind pressure acts upon the arm member 16 due to the running wind or vortexes are generated behind the arm member 16 and a resistance force due to these vortexes is exerted upon the arm member. Furthermore, since this arm member 16 consists of two arm portions 26, 26 disposed above and below as spaced from each other, the arm member 16 has a large rigidity and can firmly support the back-mirror 15. Moreover, the above-mentioned two arm portions 26, 26 are formed by providing the opening 25 in the arm member 16, the back-mirror is mounted to the upper fairing 9a by the intermediary of this integral arm member 16, and so, the external appearance is improved. The cross-section configuration of the arm portion 26 could be modified into a shape contracting gradually from the forth towards the rear.
FIGS. 7 to 9 show a back-mirror device 27 according to a second preferred embodiment of the present invention. This back-mirror device 27 consists of a mirror 28, a housing 29 for holding the mirror 28, and an arm member for connecting the housing 29 with the above-mentioned upper fairing 9a. The arm member 30 is provided with an opening 31 that is similar to the above-described opening 25, and by this opening 31, a main arm portion 32 at the below and an auxiliary arm portion 33 at the above are formed.
The above-mentioned main and auxiliary arm portions 32 and 33 are respectively divided into housing side arm parts 32a and 33a formed integrally with the above-mentioned housing 29 and fairing side arm parts 32b and 33b mounted to the side portion of the upper fairing 9a. On the housing side arm part 32a of the main arm portion 32 is provided a mushroom-shaped protrusion 32c, and on the fairing side arm part 32b is provided a fitting bore 32d into which the protrusion 32c is to be fitted. The housing side arm part 32a and the fairing side arm part 32b are coupled together by fitting the mushroom-shaped protrusion 32c into the fitting bore 32d. However, it is to be noted that they are constructed in such manner that if an external load exceeding a predetermined amount is applied to the side of the mirror 28, the protrusion 32c is disengaged from the fitting bore 32d, and thereby the external load can be avoided.
Between the housing side arm part 33a of the auxiliary arm portion 33 and the fairing side arm part 33b is provided a member 34 having flexibility and a vibration absorbing characteristic, and therefore, vibration of the mirror 28 caused by vibration of the vehicle body can be prevented and the mirror 28 would not be disengaged from the vehicle body owing to the auxiliary arm portion 33, even if the protrusion 32c is disengaged from the fitting bore 32d. The auxiliary arm portion 33 is constructed in such member that if an external load exceeding a predetermined amount is applied to the side of the mirror 28, the external load can be avoided by the flexibility of the member 34 similarly to the case of the above-described main arm portion 32.
The arm member 30 constructed in the above-described manner is mounted to the side portion of the upper fairing 9a in such fashion that the main arm portion 32 may be positioned at the forth or forward and lower location and the auxiliary arm portion 33 may be positioned at the rear and upper location. Consequently, in the event that during running an external load exceeding a predetermined amount is applied to the side of the mirror 28 from the forth (in the direction of arrow A in FIG. 8), the arm member 30 can immediately avoid the external load by the main arm portion 32 positioned at the forth being separated or bent, and therefore, a response characteristic to the external load applied from the forth is excellent. In addition, when the vehicle sinks such as upon getting on, in the event that an external load exceeding a predetermined amount is applied to the side of the mirror 28 from the below (in the direction of arrow B in FIG. 9), also the arm member 30 can immediately avoid the external load by the main arm portion 32 positioned at the below being saparated or bent, and therefore, a response characteristic to the external load applied from the below is also excellent.
FIGS. 10 to 12 show a third preferred embodiment of the present invention which has a nearly similar construction to the above-described second preferred embodiment, hence with respect to component parts common to the second preferred embodiment, they are given like reference numerals in the drawings, and detailed description thereof will be omitted. Only difference from the second preferred embodiment exists in that the housing side arm part 32a, and the fairing side arm part 32b are respectively provided with notched portions 32c and 32d, and these notched portions 32c and 32d are overlapped and coupled by means of a bolt 35 and a nut 36 so that the housing side arm portion 32a and the fairing side arm portion 32b may be freely rotatable relative to each other. In this case also, the arm member 30 is mounted to the side portion of the upper fairing 9a similarly to the second preferred embodiment, in the event that during running of the vehicle an external load exceeding a predetermined amount is applied to the side of the mirror 28 from the forth, the arm member 30 can immediately avoid the external load by the main arm portion 32 positioned at the forth being bent, hence a response characteristic to the external load applied from the forth is excellent, and the housing 29 can be firmly held by the arm member 30 similarly to the second preferred embodiment. Moreover, since a member 34 having a vibration absorbing characteristic is provided in the auxiliary arm portion 33, vibration of the mirror 28 caused by vibration of the vehicle body can be prevented.
FIGS. 13 to 15 show a fourth preferred embodiment of the present invention. A back-mirror device 37 according to this fourth embodiment also consists of a housing 39, and an arm member 40 for connecting the housing 39 with the above-described upper fairing 9a. The arm member 40 is made of rubber and has a boot-shape. In the arm member 40 is formed an opening 41 which penetrates through the arm member in the forth and back direction, and by this opening 41 are formed a forth or forward lower main arm portion 42 and a rear upper auxiliary arm portion 43. In FIG. 13, arrow FR indicates the direction of the forth of the vehicle body.
A bar 44 extends within the main arm portion 42, one end of the bar 44 is threadedly secured to the housing 39 by means of a nut 45, and the other end is connected to a click mechanism 46. The click mechanism 46 is fixedly secured to a small protrusion 48 of a base member 47, and it is positioned very close to the base member 47. The base member 47 is firmly secured to the upper fairing 9a and a front cowl stay 50 at the inside thereof by means of a plurality of bolts 49. It is to be noted that the housing 39 can be adjusted in inclination in every direction by well-known means (not shown).
FIG. 14 is a rear view, partly in cross-section, of the back-mirror device 37 (as viewed by a driver), and it clearly shows that the bar 44 is accommodated in the main arm portion 42 of the arm member 40.
Returning now to FIG. 13, the click mechanism 46 for coupling the base member 47 and the bar 44 is positioned very close to the upper fairing 9a. The position of an external force (arrow F) exerted upon the housing 39 from the lateral direction is spaced by a distance l from a line X in the lateral direction which passes through the center of the click mechanism. Consequently, if the force F in the lateral direction is exerted upon the back-mirror device, the entire back-mirror device would easily tilt backwards at its foot portion. This tilting state is shown by double-dot chain lines in FIG. 13.
The auxiliary arm portion 43 has a cylindrical shape as shown in FIG. 14 and support the back-mirror device 37 from the rear by making use of a resilient effect of rubber. Since a large wind pressure is applied to the back-mirror device 37 during running, the support by the auxiliary arm portion 43 is important. The reason is because if the auxiliary arm portion 43 is not present, the click mechanism 46 must be made stiff by the corresponding amount and hence the swingability in the horizontal direction is degraded.
FIG. 15 is a cross-section view taken along line XV--XV in FIG. 13 as viewed in the direction of arrows, which shows details of a rachet or click mechanism 46. The click mechanism itself could be of any known structure. Briefly explaining, a pin 51 of the click mechanism 46 is fixedly secured to the protrusion 48 of the base member 47, and the bar 44 is connected via a bottom plate 53 to a cylinder 52 surrounding the pin 51. A spring 54 is accommodated in a compressed state within the space between the pin 51 and the cylinder 52, and the top end of the spring 54 is pressed by a stopper 55 that is fixedly secured to the pin 51. In addition, on the contact surfaces between the protrusion 48 and the bottom plate 53 are respectively formed recesses, and a ball 56 is accommodated in these recesses. Since this ball 56 is resiliently pressed between the protrusion 48 and the bottom plate 53, under a normal condition the bar 44 is fixed to the base member 47. However, if a force F in the lateral direction is applied to the back-mirror device 37, then a torque about the pin 51 is applied to the bar 44, hence when the force F exceeds the resilient resistance force of the spring 54, the bottom plate 53 would rise up, and the bar 44 would be rotated up to the point where the force F is not exerted upon the back-mirror device 37. In this way, the force F in the lateral direction is absorbed and mitigated by the click mechanism 46. In addition, by adjusting the spring 54 of the click mechanism, the initial movable torque can be set at any arbitrary value.
In the last-mentioned embodiment, since a rotatable coupling device, that is the click mechanism 46 is provided on the base member 47 and the housing 39 is disposed at the tip end of the bar 44 fixedly secured to that coupling device, when an external force in the lateral direction has been exerted upon the back-mirror device 37, the back-mirror device can tilt easily.
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A back-mirror device for small-sized vehicles of the type that a back-mirror is mounted to an upper side portion of a fairing which covers a front portion of a vehicle body by the intermediary of an arm member projecting from the side portion. The arm member is provided with an opening which penetrates through the arm member in the direction of running of the vehicle, hence upon running of the vehicle, running wind blows through the opening from the forth to the rear, and thereby an air resistance is reduced. Among two arm portions separated to the above and the below by the opening, one arm portion is may be made to be able to avoid an external load by separation or bending in the event that an external load exceeding a predetermined amount is applied thereto, and the other arm portion could be provided with a flexible vibration-absorptive member.
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BACKGROUND OF THE INVENTION
[0001] The present invention relates to a sheet handling device comprising a sheet support plate having at least one internal fluid cavity; and a temperature control system containing a temperature controller and a closed circulating system for circulating a temperature control liquid through the cavity and through the temperature controller, the circulating system including expansion means for at least partially absorbing the expansion and contraction of the temperature control liquid.
[0002] In the copying and printing industry, a sheet handling device with a temperature controlled sheet support plate is frequently used for supporting an image receiving sheet and at the same time controlling the temperature thereof. For example, in a hot melt ink jet printer, a sheet, e. g. a sheet of paper, is advanced over a sheet support plate while the image is being printed. At room temperature, the hot melt ink is solid, and it is therefore necessary that the ink is heated in the printer above its melting point before it can be jetted onto the paper. The ink droplets that are jetted onto the paper tend to spread-out, more or less, before the ink solidifies. In order to obtain a suitable and constant amount of spreading of the ink droplets, the temperature of the sheet support plate and hence the temperature of the paper should be controlled such that the ink cools down at an appropriate rate.
[0003] In an initial phase of the print process, when a new sheet has been supplied, it is generally desirable to heat the sheet and to keep it at a suitable operating temperature. However, in the further course of the print process, it is necessary to dissipate the heat of the ink that solidifies on the paper. To that end, a temperature control fluid, e. g. a liquid, may be passed through the cavity in the plate in order to control the temperature of the plate.
[0004] For reasons of power consumption, it is required that the printer enters into a so-called sleep mode, when the printer is not operating for a certain length of time, and in the sleep mode, among others, the heating system for the sheet support plate is switched off. After a period of time, the temperature of the temperature control fluid and the sheet support plate will drop noticeably and may even reach room temperature. As a result, when a new image is to be printed, it will take a certain amount of time for the sheet support plate to be heated to its operating temperature.
[0005] Frequently, an incompressible liquid is used as the temperature control fluid. When the temperature control liquid is heated from room temperature to the operating temperature, it will expand, although it will remain in the liquid state. When the temperature falls again, the liquid will contract. Therefore, in order to avoid the build-up of a high pressure due to a temperature rise of the temperature control liquid, an expansion tank has been provided for absorbing the expansion and/or contraction of the liquid. However, such an expansion tank increases the amount of material that has to be heated when a new image is to be printed after a period of inactivity.
SUMMARY OF THE INVENTION
[0006] Accordingly, it is an object of the present invention to provide a sheet handling device which allows to quickly bring the sheet support plate to its operating temperature, and to provide a printer containing such a sheet handling device.
[0007] According to the present invention, this object is achieved by a sheet handling device of the type indicated above, wherein that the expansion means includes at least one hose for connecting the cavity and the temperature controller which is adapted to flexibly expand and contract.
[0008] Because the expansion means consists of one or more hoses that are also used to connect the cavity and the temperature controller, the number of structural elements is reduced. This is advantageous, because it involves a reduction of the heat capacity of the temperature control system. Thus, the time that is needed to heat the sheet support plate from room temperature to its operating temperature is reduced, with a corresponding savings in energy. The present invention is also advantageous in that production costs are reduced. Furthermore, when a rigid metal tube is replaced by a flexible hose made of, e.g., an elastomeric polymer, the heat capacity of the temperature control system is further reduced.
[0009] For example, the length, diameter, material, and wall thickness of the hose are adapted to enable the hose to flexibly expand and contract. The larger the length of the hose is, the larger is the increase in volume that is produced by a certain expansion of the hose wall. Also, the larger the diameter of the hose, the larger is the increase in volume for a certain amount of expansion of the wall of the hose, because the increase of the cross section of the hose is proportional to its diameter. The expansion of the hose can also be increased by choosing a suitable material and by reducing the wall thickness of the hose. At the same time, the chosen material has to be compatible with the temperature control liquid.
[0010] Preferably, the hose is adapted to flexibly expand and contract in accordance with the volume changes that correspond to the expected temperature changes of the liquid, e. g., between room temperature and the operating temperature of the sheet support plate.
[0011] The present invention is particularly useful for a hot-melt ink jet printer.
BRIEF DESCRIPTION OF THE DRAWINGS
[0012] A preferred embodiment of the invention will now be described in conjunction with the drawings, in which:
[0013] FIG. 1 is the schematic perspective view of a hot melt ink jet printer; and
[0014] FIG. 2 is a partial top view of a sheet support plate in the printer shown in FIG. 1 .
DETAILED DESCRIPTION OF THE INVENTION
[0015] As is shown in FIG. 1 , a hot melt ink jet printer includes a platen 10 which is intermittently driven to rotate in order to advance a sheet 12 , e. g. a sheet of paper, in a direction indicated by an arrow A over the top surface of a sheet support plate 14 . A plurality of transport rollers 16 are rotatably supported in a cover plate 18 and form a transport nip with the platen 10 , so that the sheet 12 , which is supplied from a reel (not shown) via a guide plate 20 , is paid out through a gap formed between an edge of the cover plate 18 and the surface of the sheet support plate 14 .
[0016] A carriage 22 which includes a number of ink jet printheads (not shown) is mounted above the sheet support plate 14 so as to reciprocate in the direction of arrows B across the sheet 12 . In each pass of the carriage 22 , a number of pixel lines are printed on the sheet 12 by means of the printheads which eject droplets of hot melt ink onto the sheet in accordance with image information supplied to the printheads. For the sake of simplicity, guide and drive means for the carriage 22 , ink supply lines and data supply lines for the printheads, and the like, have not been shown in the drawing.
[0017] The top surface of the sheet support plate 14 has a regular pattern of suction holes 24 which pass through the plate and open into a suction chamber 26 that is formed in the lower part of the plate 14 . The suction chamber is connected to a blower 28 which creates a subatmospheric pressure in the suction chamber, so that air is drawn-in through the suction holes 24 . As a result, the sheet 12 is pulled against the flat surface of the support plate 14 and is thereby held in a flat condition, especially in the area which is scanned by the carriage 22 , so that a uniform distance between the nozzles of the printheads and the surface of the sheet 12 is established over the entire width of the sheet and thus a high print quality can be achieved.
[0018] The droplets of molten ink that are jetted out from the nozzles of the printheads have a temperature of 100° C. or more and cool down and solidify after they have been deposited on the sheet 12 . Thus, while the image is being printed, the heat of the ink must be dissipated at a sufficient rate. On the other hand, in the initial phase of the image forming process, the temperature of the sheet 12 should not be too low because if otherwise, the ink droplets on the sheet 12 would be cooled too rapidly and would not have sufficient time to spread-out. For this reason, the temperature of the sheet 12 is controlled via the sheet support plate 14 by means of a temperature control system 30 . The temperature control system includes a temperature controller 31 and a circulating system with hoses 32 that are connected to opposite ends of the plate 14 .
[0019] As shown in FIG. 2 , a plurality of elongated cavities 34 are formed in the interior of the sheet support plate 14 , so as to extend in parallel with one another and in parallel with the direction (B) of travel of the carriage 22 between opposite ends of the plate 14 , where the cavities are connected to the hoses 32 through suitable manifolds. Each cavity 34 is delimited by a top wall 36 , a bottom wall 38 and two separating walls 40 and is thereby separated from the suction holes 24 and the suction chamber 26 . The top walls 36 , together, define the top surface 42 of the plate 14 which is machined to be perfectly flat. Between each pair of two separating walls 40 , which delimit to adjacent cavities 34 , a hollow space 44 is formed, through which the suction holes 24 pass through into the suction chamber 26 .
[0020] It will be understood that the temperature controller 31 may include a heater, a temperature sensor, a heat sink and the like for controlling the temperature of the liquid, as well as a pump 45 or other displacement means for circulating the liquid through the cavities 34 of the sheet support plate 14 .
[0021] The material of hoses 32 and their wall thickness are adapted to enable the hose to flexibly expand and contract in response to expansion and contraction of the temperature control liquid. The material of hoses 32 may be, for example, an elastomeric polymer. In FIG. 1 , expanded hoses 32 are schematically indicated by dashed lines.
[0022] While minimum values for the length and the diameter of hoses 32 are imposed by the dimension of the sheet support plate 14 and the required flow rate of the liquid, the length and diameter of the hoses may be selected somewhat larger in order to cope with the expected temperature and volume changes of the liquid. For example, the temperature changes of the liquid may be in the order of magnitude of the temperature change of the sheet support plate 14 between room temperature T 1 and an operating temperature T 2 , which is for example in the range of 30° C. to 40° C. The optimal length and diameter of the hoses 32 depend on the ability of the hose wall material to expand, and also depend on the volume of cavities 34 and the volume of temperature control liquid contained in the temperature controller 31 . The larger the length and the diameter of the hoses 32 , the larger will be the increase in volume obtained by expansion of the hoses 32 . At the same time, the volume ratio of hoses 32 as compared to the overall volume of temperature control liquid that is contained in the system will also increase. However, the smaller the overall volume, the smaller is the heat capacity of the liquid. Thus, it is possible to determine an optimal length and diameter of the hoses, for example, by experiment, so that the expansion of the liquid is at least partially absorbed by the expansion of the hoses, while at the same time the heat capacity of the temperature control system is maintained at an economic level.
[0023] The wall thickness of the hoses 32 may be optimized in order to ensure, on the one hand, a sufficient stability of the hoses and a sufficiently small diffusion rate of the liquid and, on the other hand a sufficient elasticity, so that the elastic restoring forces of the expanded hoses will only lead to a minor increase in the pressure of the liquid. At any rate, the pressure increase in the cavities 34 should be small enough to avoid a deformation of plate 14 . Of course, fittings (not shown) for connecting the hoses 32 to the pressure controller 31 and to the cavities 34 are pressure-tight to ensure that liquid does not leak from the circulating system due to the pressure that remains when the hoses 32 expand.
[0024] Thanks to the expandability of the hoses 32 , a dedicated expansion tank for absorbing the expansion or contraction of the liquid can be dispensed with. As a result, the temperature control system can be assembled from a low number of parts in the production process, thereby decreasing production costs. Due to the low number of parts and the flexibility of the hoses 32 , equipment maintenance is also facilitated.
[0025] The invention being thus described, it will be obvious that the same may be varied in many ways. Such variations are not to be regarded as a departure from the spirit and scope of the invention, and all such modifications as would be obvious to one skilled in the art are intended to be included within the scope of the following claims.
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A sheet handling device including a sheet support plate having at least one internal fluid cavity; and a temperature control system containing a temperature controller and a closed circulating system for circulating a temperature control liquid through the cavity and through the temperature controller, the circulating system including expansion means for at least partially absorbing expansion and contraction of the liquid, the expansion means provided with at least one hose connecting the cavity and the temperature controller and adapted to flexibly expand and contract with the temperature control liquid.
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BACKGROUND OF THE INVENTION
Sheets which are conveyed rhythmically one after another with respect to their rear edges are produced, for example, by rotational cutters. Using a known cutter which cooperates with a device for stacking, the sheets pass between high-speed upper and lower conveyor belts after having been cut. A low-speed conveyor belt is arranged in a conveying direction behind the lower high-speed conveyor belt, and the upper side of the low-speed conveyor belt is displaced downwards opposite a joint conveying plane of the high- and low-speed lower and upper conveyor belts. A deflecting member is arranged above the conveying plane in the transitional zone between the high- and low-speed lower conveyor belts. The deflecting member is controlled rhythmically with the on-coming rear edges of the sheets, and thus deflects the rear edges of the sheets downwards from the conveying plane onto the lower slower conveyor belt. The downward deflection is carried out in order to obtain space for the leading edge of the next sheet, which is to be separated from the previous sheet. Control of the compressed air by the deflecting member, however, causes difficulties as it is impossible, especially upon a quick succession of sheets (the sensing elements, the relay control, valve, and the air all need more time than the interval between the sheets allows) to keep the compressed air, which deflects the sheet, away from the leading edge of the next sheet. A clean separation is therefore not possible, at least with sheets which follow each other in quick succession. However, when overlapping occurs, the overlapped sheets which have been deposited on the lower low-speed conveyor belt are further transported to the stacking point. Further separation only takes place to a limited extent on this stretch. This means that the front edge of the sheet collides with a stop of the stack at a considerably high speed, dependent on the speed at which the sheets are fed and the degree of overlapping. In the case of thin sheets having a large format, such a collision may lead to crushing of the sheet, setting up a relationship between the stiffness of the sheet and the kinetic energy of the sheet which is unfavorable. (German Offenlegungsschrift No. 1,245,702).
In a different type of separation device, which does not have pneumatic conveyor and braking means, but operates with rollers which come into contact with the material to be conveyed, a pair of rollers is provided as braking means. One of the rollers has a projection, and the other of the rollers has a recess which rotates in synchronization with the former. Whilst one sheet entering the roller gap is not affected by the other area of the two rollers, the sheet end is affected by the projection and the recess. The sheet can consequently be conveyed without any interference by the pair of rollers only until its end, and is then affected by the projection and the recess. As the speed of rotation of the pair of rollers is less than the speed at which the sheet is conveyed, the sheet is decelerated. As the periphery of the projection and the recess are downwardly displaced opposite the conveying plane, the end of the sheet is also deflected downwards at the same time as the braking occurs, so that the leading edge of the next sheet, which is conveyed at a higher speed than the decelerated sheet, can be dropped on top of the decelerated sheet.
In this known device the end of the sheet is indeed also deflected downwards from its conveyance plane by means of the projection; however, this deflection merely serves for sheet separation; no transfer into the effective area of the braking means occurs. The conveyor means remain fully effective. (German Auslegeschrift No. 2,032,800).
OBJECT OF THE INVENTION
It is an object of the present invention, therefore, to produce a device in which the deflecting member is in the form of a conveyor means, whereby it is possible to ensure without any special sensing and control means that the end of a sheet is brought into the effective range of the braking device, and which provides a safe treatment for sheets having a lower than normal degree of inherent stiffness.
SUMMARY OF THE INVENTION
The above object is attained, according to the invention, by the deflecting member being a suction conveyor roller which has projections on its periphery, and which rotates rhythmically with the ends of the sheets in such a manner that the ends of the sheets are laid on the projections.
Transfer from a conveying to a braking effect on the sheets is accomplished merely by moving the ends of the sheets out of the effective area of the suction conveyor roller into an effective range of the suction braking means by means of projections formed on the rollers, i.e., by mechanical and not pneumatical means. Consequently no special means for controlling the suction air is needed. This type of reversal of the conveying effect to the suction effect is achieved exactly, so that the sheets may be fed sheet-by-sheet (i.e., overlapping each other) by the device in quick succession.
The suction conveyor roller is only perforated in the area outside the projections, so that the end of the sheet deflected downwards from the suction conveyor roller can be removed from the suction conveyor roller as easily as possible.
The rollers of the suction table can be coated on their surfaces with a material having a high friction coefficient, in order to achieve a defined conveyance speed upon decelerating the sheet by means of the suction table. The slippage between the sheet and the rollers is thereby kept at a low level.
A risk exists especially in the case of thin sheet material for it to be drawn into spaces between the rollers which are formed closely one next to another. This risk exists particularly in relation to the beginning of the sheet. To avoid disadvantageous consequences in spaces formed between closely spaced rollers, filler members, particularly threaded rods disposed loosely thereupon, may be provided. The threaded rods are preferably coated with an anti-adhesive means on their surfaces.
A better solution for preventing the critical points of a sheet (the leading edge and/or gumming area) from being pulled into a space between two adjacent rollers, is for the rollers to have axially spaced raised rings on their periphery, by means of which the adjacent rollers intermesh with each other.
The intervening roller space is decreased on selecting the diameter of the rollers by means of the intermeshing of the rollers of the suction table in such a way that the filler member is no longer necessary to prevent the sheet from being pulled into that space. Due to the filler member not being required, a possible source of malfunction does no longer exist, and the device, according to the invention, is consequently made safer.
So that the suction force of the suction table can be applied as directly as possible, the rings of the rollers are perforated for exposure to at least a part-vacuum.
One embodiment of the invention provides that the roller of the suction table positioned opposite the suction conveyor roller has a substantially larger diameter than the other rollers, in order to directly increase the braking effect after the end of the sheet has been deflected due to the flat curving of this roller. The sheets can then follow one another more closely and form a larger contact surface.
The suction table is preferably exposed to a part-vacuum by a two-section suction box arranged underneath the suction table, so that the part of the suction box in the area of the large roller is exposed to a substantially higher vacuum than the second part of the suction box. This measure also serves to increase the braking effect.
The part-vacuum in the second part of the suction box can be easily produced by connecting that part of the suction box to the first part of the suction box by means of an opening which is provided with a throttle flap. The part-vacuum in the second part can then be controlled by means of the throttle flap.
BRIEF DESCRIPTION OF THE DRAWING
The invention is explained in further detail as follows by means of a drawing showing preferred embodiments of the invention. Specifically,
FIG. 1 shows a side view of a device for feeding sheet-by-sheet in schematic form;
FIG. 2 shows an enlarged section of FIG. 1;
FIG. 3 shows the conveying and separation of the sheets so that the alignment with FIG. 1 is maintained and the height scale is greatly enlarged;
FIG. 4 shows a side view of a modified device for separating sheets in schematic form;
FIG. 5 shows an enlarged section of FIG. 4;
FIG. 6 shows the conveying of overlapping sheets to be stacked so that alignment with FIG. 4 is maintained and the height scale is greatly enlarged, and
FIG. 7 shows a top view of an enlarged section of FIG. 4.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
As comparison of the device of FIGS. 1 and 2 with FIGS. 4, 5 and 7 shows the basic structure of the two devices to be the same. Therefore the construction elements which are the same are also given the same reference numbers.
A roll 1 of paper is conveyed between lower and upper conveyor rollers 2 and 3 to a cutter which is composed of a lower fixed blade 4 and a rotating upper blade 5. The cutting edge of the upper blade 5 has a slightly spiral form so that during rotation and cooperation with the lower blade 4 it cuts the roll 1 into a plurality of sheets.
The cut sheets are conveyed from the cutter 4, 5 to a suction conveyor roller 7 by means of a table 6, which is composed of floating bars operated by compressed air, and is arranged below the conveying plane. The suction conveyor roller 7 is perforated with the exception of an area 17. The suction conveyor roller 7 has crescent-shaped projections 16 in this area 17, best shown in FIG. 5, which extend in a circumferential direction and peak radially at the end on the rear side; the projections 16 are axially spaced from one another. A fixed comb 21 meshes with the spaces between the projections 16. The suction conveyor roller 7 rotates around a suction tube 8 arranged therein so as to be secured against rotation, which suction tube 8 has sealing bars 9 disposed in a lower area on the suction conveyor roller 7, the latter being smooth on the inside. The sealing bars 9 permit the suction effect of the perforated suction conveyor roller 7 to be effective only in the lower area.
A group of floating bars 10 operated by compressed air is arranged in a conveying direction behind the suction conveyor roller 7 and above the conveying plane. A suction table comprising several rollers 11-15 and 31-39 arranged closely next to one another, and a suction box 13, 30 arranged thereunder, is disposed below the conveying plane in the area of the suction conveyor roller 7 and the group of floating bars 10. The rollers 11-15 and 31-38 form an upper cover section of the suction box 13, 30.
In the embodiment of FIGS. 1 and 2 all rollers 11-15 are perforated so that the suction of the suction box 13 can become effective due to the perforation. The rollers 11-14f have the same diameter, whereas the roller 15 is somewhat smaller in diameter in comparison to the former. Threaded rods 22-28 are disposed in the space formed between the equal-sized rollers 11-14f, the threaded rods 22-28 being disposed loosely on the rollers 11-14f. The construction of the rods 22-28 in the form of threaded rods additionally permits suction air to pass through the threads.
In the embodiment of FIGS. 4, 5 and 7 the roller 31, which is disposed first in the conveying direction and below the suction conveyor roller 7, has a substantially larger diameter than the rollers 32-39 positioned behind the roller 31, as seen in the conveying direction. All rollers have axially spaced and raised rings 40, 41 and 42 on their periphery, which are produced by milling out annular grooves in the shell surface of the rollers. The space between the rings 40, 41, 42 and adjacent rollers is formed in such a way in relation to the width of the rings 40, 41 and 42 that adjacent rollers intermesh, as can be seen most clearly in FIG. 7. The shell of the roller 32 is composed of metal, whereas the shells of rollers 31 and 33-39 are composed of hard rubber. The roller 31 operates as a suction roller by means of its perforation and connection to a box 30a of high vacuum, whereas the roller 32 and the subsequent rollers 33-39 operate as a suction table by means of gaps existing between the rings and grooves of respective adjacent rollers and their connection to the vacuum-source box 30b. Thus perforation of rollers 32-39 is unnecessary. In contrast to the homogeneous suction box 13 provided in the embodiment of FIGS. 4 5 and 7, the suction table is subdivided into a part 30a positioned rearwardly in the conveying direction of the sheets, and a part 30b positioned forwardly thereof. A cover plate 40 is also provided which is disposed parallel to the rollers 31-39, one end of the plate meshing in the manner of a comb into the shell surface of the roller 32. A throttle flap 41 is connected to the plate 40. An opening formed in part 30a of the suction box, which is exposed to high vacuum, and communicating with part 30b of the suction box can be adjusted in size by a throttle flap 41. A particularly strong braking effect can be exerted on the sheet with this device at a location where the roller table is least curved.
All the rollers 11-15 and 31-39 have a defined rotational speed which is produced and determined by a belt drive 44 which is only portrayed in FIG. 7 for the embodiment of FIGS. 4, 5 and 7. The rotational speed of the first roller 11, 31 in the conveying direction is substantially lower than the rotational speed of the suction conveyor roller 7. The rotational speed of the next roller 12, 32 is, in contrast, equal to that of the first roller 11, 31. The rotational speed of the subsequent rollers 14a-15, and 33 to the last roller which is acted on by suction air, decreases gradually in the conveying direction.
So that the two first rollers 11, 12, 31, 32 can effectively decelerate the sheets, and so that no relative speed between the sheets and the surface of the roller can occur between the rollers 14a-15 and 33-39 conveying sheets at progressively decreasing speeds, the surface of the rollers may be provided with a coating having a high friction coefficient. If threaded rods 32-38 are provided in the respective spaces between the rollers 11-14f, the threaded rods 22-28 being rotated by the rollers 14-14f against the conveying direction of the sheets and coated with anti-adhesive means, they do not then disturb the conveying of sheets, and do not erase any print on the sheets which may possibly not yet be dry enough to prevent erasure thereof.
The device according to the invention operates in the following way:
The sheet, which is cut from the roll 1 by the cutter 4, 5, and which is conveyed by the floating-bar table 6 of the suction conveyor roller 7, has the leading edge thereof exposed to the suction conveyor roller 7 effectively in the lower area of the latter. As the suction conveyor roller 7 rotating rhythmically in concert with the rotating blade 5 of cutter 4, 5 has a slightly larger diameter than the periphery of the blade 5, its rotational speed is very slightly greater than that of the rotating blade 5 or the speed of the roll 1 which is conveyed to the cutter 4, 5. Consequently the sheet which is picked up by the suction conveyor roller 7 is slightly accelerated, so that a small space is created between the rear edge of the sheet and the leading edge of the next sheet. The leading edge of the sheet picked up by the suction conveyor roller 7 is transferred to the upper floating edges 10. This transfer is made by means of the comb 21, and is facilitated by the suction air of the suction tube 8 not being effective in the transfer area due to the sealing bar 9. Since the cutter 4, 5 and the suction conveyor roller 7 are time correlated with one another, the end of the sheet reaches the projections 16, the latter having the form of bars or preferably small brushes, which deflect the end of the sheet downwards into the effective area of the suction brake roller 11, 31, the latter rotating at a substantially lower rotational speed. This suction brake roller 11, 31 takes up the end of the sheet, declerates its rotational speed, and by so doing provides room above the end of the sheet for the next leading sheet edge. The suction brake roller 11, 31 decelerates the sheet to a conveying speed of only a fraction of the speed at which the sheet is conveyed to the cutter 4, 5. The conveying speed decreases, for example, by 1/10 so that the next sheet overlaps by 90%, i.e., at a much higher percentage than previously known. If the sheet is only decelerated at the end, and the rest of the area of the sheet, particularly the leading edge, remains under the action of the floating bars 10, which are operating in the conveying direction, this ensures that the sheet is held straight. The particular advantage of the floating bars 10 is due to the fact that a new leading edge of a sheet is pulled in between the bars and the rear portion of the preceding sheet remaining suspended on the bars without being crushed.
The overlapping portrayed schematically in FIGS. 3 and 6 occurs as soon as the end of the sheet leaves the suction brake rollers 11, 12, 31 and 32 and reaches the effective area of the suction rollers 14a-15 and 33-39, the speed of conveying of the latter being decreased in stages. As a result the sheet being transported reaches such a low speed directly before striking against the stop 8 in the stack 19, that harmful crushing thereof cannot occur. During the whole of the conveying process over the suction table 11-15 and 31-39 it is ensured that the individual sheets are further conveyed at a defined speed, which speed is decreased in stages, so that the rear edges of the sheets are pushed closer and closer together. However, as a consequence of this overlapping effect, the front edges of the sheets also become more closely spaced, so that the remaining free length thereof, when coming to a stop, is so small that harmful bulging, distortion and the like is prevented.
Consequently, the device according to the invention, performs sheet separation and sheet distribution without jamming at high speed, such jam-free separation and distribution being effected and ensured at low cost even when the inherent stiffness of the sheet is low. This is so because the deflecting means, which deflect the rear edges of the sheets ryhthmically downwards into the effective area of the braking means due to the rear edges of the sheet being conveyed, does not disturb the leading edges of the respective next sheets, and the latter can consequently be conveyed with maximum overlapping into the vacated space provided above the previously deflected sheet. The active rear edge conveying of the sheets at progressively lower speeds until the front edge of a sheet practically strikes the stop of the stack ensures that the sheets hit the stop of the stack at a very low speed. Further auxiliary means above the stack, such as conveyor means, are no longer necessary; the stack therefore remains freely accessible from above. This is a requirement which is valued above all by printers.
The sheets, especially the leading edges thereof, their ends and any gumming areas are prevented from being drawn into the space between the individual rollers by the threaded rods provided in that space in the embodiment of FIGS. 1 and 2, and by the intermeshing rollers in the embodiment of FIGS. 4, 5 and 7. In both embodiments a relatively flat conveyor surface is achieved for the sheets even where relatively large roller diameters are employed.
The last roller 15, 39 does not have to exert any braking effect on the sheets as the speed of conveying of the sheets has, at this point already become very low. For this purpose the last roller may be arranged outside the suction box, as shown in the embodiment of FIGS. 4, 5 and 7. The object of that roller, the latter no longer having a braking effect, is then to directly ensure a clean transfer of the sheet before its final position in the stack. A clean transfer can possibly also be achieved by means of a stripping comb which meshes with the grooves of the last rollers. Blowing elements can also be mounted on the device to ventilate the sheets.
While there has been shown what is considered to be the preferred embodiment of the invention, it will be obvious that modifications may be made which come within the scope of the disclosure of the specification. Accordingly,
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The invention relates to a device for sheet-by-sheet feeding and placing the sheets on a stack, the sheets being conveyed rhythmically one after another, including a conveyor means and a suction braking means disposed below a conveying plane, for transporting the sheets into an effective range of the suction braking means; the ends of the sheets may be held and transported by a deflecting member which is arranged above the conveying plane.
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FIELD OF THE INVENTION
The present invention relates to a spinfinish material which is applied on fiber during production of polymer fibers used as reinforcement material in tire technology, both improves the physical properties of the fiber and cord-rubber adhesion, and a production method thereof.
BACKGROUND OF THE INVENTION
Today, the polyethyleneterephthalate (PET) with high tenacity decreases the deformation of the composite structure it forms with the rubber significantly with its high strength and low elongation properties, thus material with higher performance can be produced. The PET fiber is most commonly used in tire, hose, components such as conveyor band and belt as rubber reinforcement material.
The synthetic fibers are hard to adhere to rubber without binding agents in between them because they have a very smooth surface and low reactivity. The low surface activity of the fibers stems from the low polarity and low reactivity of the polymer molecules. Therefore, adhesives are used in intermediate surfaces since the physical and chemical bonding between the rubber and cord fabric used in the tire production technology is very low. Adhesives vary according to the type of the polymer used in cord fabric.
Since the elongation of cord fabric material is low and its strength is high, and the elongation of the rubber material is high and its strength is low; the adhesive which is used should provide an excellent intermediate surface in order to provide the best performance. Increasing adhesiveness provides better compatibility between the rubber and the cord fabric, and enables the properties of both rubber and cord fabric to be revealed better in the final product.
As it is in reinforcing materials such as nylon, rayon, aramide; an adhesive should be applied in order that the PET cords are adhered to the rubber. In cord fabric production, water based Resorcinol-Formaldehyde-Latex (RFL) adhesive solutions enabling the cord fabric to rubber have been used for over fifty years. In RFL adhesive solutions, caustic and ammoniac are the most commonly used catalysts. In the said solutions, different Formaldehyde/Resorcinol (F/R) mol ratios, resin/latex ratios, solid ratios and additional activating chemicals are used for especially PET fiber.
Whereas the adhesion of fibers such as nylon and rayon are easy to adhere to the rubber with RFL, there are difficulties in adhesion of PET fiber to the rubber. The main reason for this is that functional groups such as carboxyl (COOH) and hydroxyl (OH) forming bonds with the RFL are only present on chain ends of PET molecule in structure of PET fiber. In nylon and rayon material, the density of the functional groups is much higher than in the PET fiber. For this reason, the adhesive systems of PET fibers are continuously developed. One of the said methods is to develop spinfinish materials that will increase the surface activity of PET fiber with RFL applied during yarn production.
Spinfinish materials are mostly liquid compositions which are comprised of more than one components and wherein all components are in equilibrium. Applying spinfinish material which is a very important part of fiber production procedure provides various properties to the fibers, as well as provides ease by forming intermediate surface between the fiber surface and the metal and/or ceramic components present in the production procedure.
The main functions of the spinfinish material are to provide lubrication by greasing the fiber surface, to prevent abrasions by minimizing the friction between filament-filament, filament-metal and filament-ceramic, to provide antistatic properties to the fiber, and to prevent the fiber from falling apart by keeping the hundreds of filaments forming the fiber. During the production of synthetic fibers used as rubber reinforcing material and produced in high speeds, spinfinish is applied on the fibers coming out of spinnerets in order to drawability of the fiber. It is not possible to produce fiber with high performance in high speeds without spinfinish. The said spinfinish material is used for providing drawability in nylon 6.6 fibers, whereas it is also used to activate the surface of the fiber besides the said property in PET fiber production.
The spinfinish which has a very important role in production of fibers with high performance causes many problems in spinning, drawing and twisting processes when they are not compatible with the system it is used with. These can be breakage in fiber, filamentation, winding in drawing cylinders and irregularity in reel form, being smoked, tar forming which cannot be cleaned, unevenness in the reel form, deteriorations in twisting quality and ruptures. For this reason, the spinfinish material used for producing fiber with high quality should have some main properties.
High decomposition temperature, high smoking temperature, optimum viscosity, antistaticity, not leaving residue on the metal/ceramic components, low volatility are among the expected major properties. Besides, the spinfinish which is used being harmless to the environment and human's health, providing emulsion quality in aqueous solution, being resistant to the temperature in process conditions, not experiencing chemical reactions, not being oxidized in storage conditions and being low cost also provide advantage in production of fibers.
U.S. Pat. No. 4,348,517, an application known in the state of the art, discloses a spinfinish composition applied in two stages on PET fiber. The said composition is stated to be comprised of triglycidyl glycol ether and epoxy silane.
U.S. Pat. No. 3,803,035, another application known in the state of the art, discloses a spinfinish composition comprised of lubricant, antistatic agent, emulsifier and polyepoxy.
U.S. Pat. No. 3,793,425, another application known in the state of the art, discloses coating PET fiber with a solution comprised of epoxy resin buffered with potassium carbonate sodium carbonate or ammonium hydroxide.
U.S. Pat. No. 4,054,634, another application known in the state of the art, discloses a two stage spinfinish application. Spinfinish applied in first stage comprises polyethyleneoxide-polypropyleneoxide (EO-PO) monoethers, whereas in spinfinish composition applied in second stage compositions comprising catalysts such as epoxy silane and sodium hydroxide, potassium hydroxide, sodium carbonate, potassium carbonate, sodium acetate, potassium acetate are disclosed.
The compositions disclosed in the said methods are high cost and/or harmful to environment. Most part of them cannot provide the desired adhesion between the fiber and rubber and the strength. Furthermore, there is no study for applying spinfinish on fiber in single stage during the production of fiber.
SUMMARY OF THE INVENTION
The objective of the present invention is to provide a spinfinish material which can be applied in single stage on fiber and which can be applied as water based emulsion.
Another objective of the present invention is to provide a spinfinish material which has a high smoking temperature and is applied on fiber.
A further objective of the present invention is to provide a spinfinish material which does not leave residue when it is applied on fiber.
Another objective of the present invention is to provide a spinfinish material which improves the adhesion between cord-rubber in tire technology when it is applied on fiber used in cord production.
Yet another objective of the present invention is to provide a production method of a spinfinish material which is low cost, applied on fiber and have the properties mentioned above.
BRIEF DESCRIPTION OF DRAWINGS
A spinfinish material applied on fiber and a production method thereof developed to fulfill the objective of the present invention is illustrated in the accompanying figure, in which;
FIG. 1 is the view of the flowchart of the method.
FIG. 2 is the view of the FITR spectrums of the samples taken from the reaction medium in different times during the synthesis of active component, and comprising EO-PO and IPTS in ratio of 1:2.
DETAILED DESCRIPTION OF THE INVENTION
The production method for the spinfinish material applied on fiber ( 10 ) developed to fulfill the objective of the present invention comprises the steps of
synthesis of the active component ( 11 ),
heating the polymer ( 111 ), adding initiator ( 112 ), adding catalyst ( 113 ), performing the reaction ( 114 ),
preparing the improving material ( 12 ), adding the improving material to the active component ( 13 ), obtaining the spinfinish material ( 14 ).
In the inventive production method for a spinfinish material applied on fiber ( 10 ), first the active component is synthesized ( 11 ). For this purpose, first the polymer is placed inside the reactor and preheated in there ( 111 ). In the preferred embodiment of the invention, ethyleneoxide-propyleneoxide copolymer (EO-PO) (block and/or graft copolymers) the number-average molecular weight of which is between 1000 and 5000 g/mole is used. In the preferred embodiment of the invention, the process of heating the polymer ( 111 ) is performed when the reactor temperature is in the range of 60-100° C.
When the temperature of the reactor reaches the desired value, the initiator is added dropwise ( 112 ). In the present invention, 3-isocyanatopropyl-triethoxy silane (IPTS) is used as initiator. The ratios of EO-PO copolymer and IPTS added inside the reactor can be between 1:1 and 1:2.
After the initiator is added ( 112 ), the catalyst which will catalyze the reaction is added inside the reactor ( 113 ). In the present invention, tin 2-ethylhexanoate is used as catalyst. The reaction started with adding the catalyst ( 113 ) continues for 9-24 hours under nitrogen atmosphere ( 114 ).
Then the improving materials are added to the active component ( 13 ) formed as a result of the reaction ( 114 ), and the spinfinish material is obtained in this way ( 14 ). The improving materials are prepared with lubricant in ratio of % 30-60 by weight, emulsifier in ratio of % 30-50, antistatic agent in ratio of % 1-10, wetting agent in ratio of % 1-10, antioxidant in ratio of % 0-2, surface activating agents in ratio of % 1-5, bacteria preventing agents, corrosion inhibitors and anti-foams ( 12 ).
In the preferred embodiment of the invention, the ratio of the active component in the spinfinish material which is obtained is between % 20 and % 60 by weight. When the spinfinish material obtained after all the steps, the adhesion between the cords used in tire technology with the rubber is reinforced.
The inventive method for producing spinfinish material applied on fiber ( 10 ) is performed in bulk medium and the product formed as the reaction proceeds with FTIR analysis. EO-PO copolymer, the water of which is previously removed and the number-average molecular weight of which is between 1000 and 5000 g/mole, is placed into the reaction balloon, and 3-isocyanatopropyl-triethoxy silane (IPTS) is added dropwise when the ambient temperature reaches 80° C. After that, tin 2-ethylhexanoate is added and the reaction is performed under nitrogen atmosphere. The schematic view of the reaction is as follows:
After the reaction started, samples were taken from the reaction medium after 9, 12, 15 and 24 hours, it was followed with FTIR analysis whether the reaction was completed. The FTIR spectrums of the samples taken in different times from the reaction medium are as in FIG. 2 : When the reaction is completed, the band of the isocyanate group at 2200 and 2353 cm −1 present in the IPTS (N═C═O) completely disappears, instead a band belonging to urethane group at 1718 cm −1 (NHCOO) wavelength is seen. As a result of the optimizations, reaction times are determined as 24 hours for 1:2 ratio (the ratio of the polymer to the initiator), and 9 hours for the ratio of 1:1.
3 different spinfinish materials comprising active component in ratios of % 20, % 40, and % 60 by mass (respectively spinfinish-1, spinfinish-2, spinfinish-3) were prepared, and all used materials and the ratios in the composition are given below in Table 1.
TABLE 1 The Compound of Spinfinish compositions Spinfinish Formula Spinfinish-1 Spinfinish-2 Spinfinish-3 Name of the Weight % Weight % Weight % component Function 20 40 60 AB Active component 26 22 18 Emulgin RT40 Lubricant (Castor oil) and emulsifier 11 7 3 Dehydol LS6 Emulgator (5 mol ethoxylated alcohol C12-C14) 11 7 3 Dehydol LT7 Emulgator (7 mol ethoxylated alcohol C12-C14) 21 17 13 Rinalit SMO Cohesion (Sorbitan agent monooleate) 11 7 3 Crafol 56 Antistat (phosphate ester) Spinfinish-1: spinfinish with 20% active component Spinfinish-2: spinfinish with 40% active component Spinfinish-3: spinfinish with 60% active component
some physical properties of these 3 different prepared spinfinish material were measured and the said values are given below in Table 2.
TABLE 2
Some physical properties of spinfinish compositions
Properties
Spinfinish-1
Spinfinish-2
Spinfinish-3
Viscosity (cP) (at 25° C.)
390
990
1040
Smoking point (° C.)
152
152
172
Degradation temperature
362
376
392
(T 1/2 ) (a)
Residue (%) (at 600° C.)
5
7
8
TGA measurements were performed at range of 25° C.-600° C. in oxygen environment at 20° C./min heating rate.
The inventive spinfinish material can also be applied on fibers such as polyethylene terephthalate, polyethylene naphthalate, and other fibers that can bond with RFL similar to these in terms of surface properties.
In order to apply the inventive spinfinish material comprising active component, first the water based emulsion of the material is prepared. The concentration of the water based emulsions which are prepared is 5% by weight, is applied after the 1100 dtex synthetic, continuous, high modulus, low shrinking (HMLS) PET fibers go out of the spinnerets at high speeds.
After the fibers on which spinfinish material is applied are prepared in certain structures (dtex*layer*twist), dipping process is performed, and they are used in cord production. In order to adhere the said cords to the rubber, they should be dipped into water based adhesive solutions. Dipping solution is comprised of two different solutions. First solution comprises polyepoxy and/or blocked polyisocyanate. The solid amount of the first adhesive dipping solution varies between 0.5% and 5%. The second is comprised of Resorcinol-Formaldehyde-Latex (RFL). The latexes which are used are VP (vinyl pyridine-styrene-butadiene ter polymer) and SBR (styrene-butadiene copolymer) latexes. The solid amount of the water based RFL solution can vary between 3% and 30%. pH range of RFL is kept between 8 and 12. After the cords are dipped, drying and curing processes are performed. Drying is performed at 100-150° C., and curing is performed at 210-250° C. The cords which are dipped are pressed with unvulcanized rubber compositions. The said composite material is cured under press for 20 minutes at 170° C.
The preparation of an exemplary spinfinish material and application on fiber is explained below.
EXAMPLE
In a medium not comprising solution (bulk), after the 60 g Synalox EO-PO copolymer, the water of which is removed previously and the molecular weight of which is 1000 g/mole, is placed into the reactor, when the ambient temperature reaches 80° C., 31.24 g IPTS is added dropwise, and then the reaction is performed in nitrogen atmosphere by adding a drop of tin 2-ethylhexanoate. The synthesized active component can be prepared with different ratios given in Table 1 with other components of the spinfinish.
While applying the material on the fiber, water based emulsion solution is prepared with spinfinish material comprising 40% active component. The concentration of the emulsion solutions which are prepared is 5%, they are applied on 1100 dtex HMLS PET fiber at high speeds in one stage. 1100 dtex PET fibers which are treated with spinfinish material, the adhesion activating component of which is 40% in the formulation, are twisted in sizes of 1100×2 470×470, and the cord is produced. The twisted cords first were treated with adhesive comprising 3% epoxy-blocked isocyanate, and then treated with 20% solid standard RFL solution, dried at 140° C. for 110 seconds, and then cured at 235 and 225° C. for 55 seconds for each. Some physical properties of the obtained yarn are given in Table 3.
TABLE 3
The physical properties of PET fiber treated with exemplary spinfinish
material comprising active component in ratio of 40% by weight.
Reference
Properties
Product
Spinfinish-2
Yarn/Ceramic friction coefficient
0.49
0.46
@100 m/min
Yarn/Yarn friction coefficient
0.38
0.33
@100 m/min
Yarn-Breaking strength (kg)
8.03
8.08
Twisted Cord-Breaking strength (kg)
14.72
14.70
% conversion (a)
92
91
Produced cord breaking.strength (kg)
14.5
14.8
H-adhesion (kg) (b)
100
111
(b) conversion calculation:
Raw yarn strength: 8.03 kg
Twisted cord strength: 14.72 kg
% conversion: 14.72/(2×8.03)×100=92
(b) Dipping solution-1: Comprising adhesion improving activator (epoxy-isocyanate)
Dipping solution-2: RFL solution
The reference product is an oil product used in the state of the art, it is in the know-how scope of the oil producers.
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The present invention relates to a spinfinish material and a production method thereof which comprises the steps of synthesizing the active compound ( 11 ), heating polymer ( 111 ), adding initiator ( 112 ), adding catalyst ( 113 ), performing the reaction ( 114 ), preparing the improving material ( 12 ), adding the improving material into the active component ( 13 ), obtaining the spinfinish material ( 14 ); which is applied on fiber during production of polymer fibers used as reinforcing material in tire technology, both improves the physical properties of fiber and makes the cord-rubber adhesion easier.
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CROSS-REFERENCE TO RELATED APPLICATIONS
[0001] This application claims the benefit of U.S. Provisional Application No. 60/525,973.
STATEMENT REGARDING FEDERALLY SPONSORED RESEARCH OR DEVELOPMENT
[0002] None.
BACKGROUND OF THE INVENTION
[0003] 1. Field of the Invention
[0004] This invention relates to the field of roof shingle designs and methods of applying shingles. More specifically, the present invention relates to an improved configuration for a cedar shake shingle, a chemical treatment of this shingle, and the installation of a plurality of such shingles.
[0005] 2. Description of the Related Art
[0006] Cedar shake shingles have been used for roofing houses for a long time. Shakes are a favorite choice among many homeowners, more for ornamental reasons than for practical ones. Practically speaking, shake shingles have many disadvantages.
[0007] One of these disadvantages is in terms of wind resistance. The conventional cedar shake roof will have a difficult time withstanding excessive winds. A typical prior art shingle which would be used on a conventional shake roof is shown in prior art FIGS. 1 and 2 . As can be seen in FIG. 1 , the prior art shake 10 is relatively thin. It has an upper surface 12 , an exposed portion 14 , a covered portion 16 , a termination and 18 , a butt-end 20 , an underside 22 and side surfaces 24 . The shingle is secured to the conventional roof using 2 fasteners 28 , which may be staples or nails. The conventional nails or staples used for such a purpose are typically constructed of electro or hot-dipped galvanized steel.
[0008] As will be known to one skilled in the art, shingles are laid in rows, one row over the other, this results in the exposed 14 and covered 16 portions. Portion 16 will be covered by the next row of shingles up the roof, whereas portion 14 is exposed to the elements. The exposed 14 and covered 16 portions are divided by a transition line 26 which is formed by the butt-end 20 of the shingle immediately above it.
[0009] The dimensions of the conventional shingle are typically as follows. They typically have a length of 24″, and a butt-end thickness of {fraction (1/2)}″. As maybe seen in FIG. 1 , the shingle is tapered towards a termination end 18 which is typically around {fraction (1/8)}″ thick. These dimensions make the ratio of butt-end thickness (about {fraction (1/2)}″), versus termination end thickness (about {fraction (1/8)}″) about 4-1. The distance of the transition line from termination end 18 is typically 10″. Because of the thinness of shingle 10 and its fastener positioning, it is made somewhat vulnerable to excessive winds.
[0010] A second disadvantage in a shake roof is in hail resistance. Impact testing of such roofs reveal that even moderate sized hail can create significant damage to the roof's shakes. Similarly, walking on the roof is often avoided because even careful stepping on the roof may resulting damage to the shakes. One of the reasons for this vulnerability of the conventional shake is that its exposure area is very great relative to its overall thickness. It is spread out too thin, in other words.
[0011] A third disadvantage present in the prior art shake roof is that its shakes tend, over time, to prematurely curl upwards away from the roof. This makes the overall appearance of the roof somewhat unsightly.
[0012] A fourth disadvantage in the conventional shake roof is that it may degrade. This degradation may take the form of dry rot, algae, insect problems, or combinations thereof. These forms of degradation are the result of exposure to the elements, such as rain. The exposed surfaces of the shingles are typically the most affected. This is because they are bare and thus, not barred off from environmental factors.
[0013] Because of these four disadvantages, there is a need in the art for a shake, and method of applying that shake, which (i) results in wind and impact resistance, (ii) has better insulation properties, and (iii) forms a barrier between the cedar and the environment to prevent dry rot, algae and insect problems.
SUMMARY OF THE INVENTION
[0014] The present invention overcomes these disadvantages in the conventional shake roof by providing a shingle that is thicker with a less dramatic taper, thinner, has a minimized exposure area relative to thickness, and is chemically treated to form a barrier between the cedar and the environment.
BRIEF DESCRIPTION OF THE SEVERAL VIEWS OF THE DRAWINGS
[0015] The present invention is described in detail below with reference to the attached drawing figures, wherein:
[0016] FIG. 1 is a side view of the conventional cedar shake used in the prior art methods.
[0017] FIG. 2 is a perspective view of the prior art shake.
[0018] FIG. 3 is a side view of the wood shake of the present invention.
[0019] FIG. 4 is a perspective view of the wood shake of the present invention.
[0020] FIG. 5 is a drawing showing, from a side view, the way in which the shingles of the present invention may be disposed on a roof.
[0021] FIG. 6 shows, from a perspective view, how the shingles in the present invention are laid on the roof.
DETAILED DESCRIPTION OF THE INVENTION
[0022] The shingle design of the present invention are shown in FIGS. 3 and 4 . The manner in which these shingles are laid on a roof are shown in FIGS. 5 and 6 .
[0023] Referring first to FIG. 3 , the shingle of the present invention 30 has an upper surface 32 . Upper surface 32 is divided into two portions. The first of these is an exposed portion 34 which will be exposed to the elements. When shingle 30 is nailed on the roof as part of a first row of shingles, a second row of shingles will be laid above it (as shown in FIGS. 5 and 6 ). The part of upper surface 32 that is not covered by the shingles of the second row creates exposed portion 34 . Accordingly, covered portion 36 is the portion of upper surface 32 which is covered by the shingle in the row immediately above it. These two portions 34 and 36 are divided by a transition line 36 . Referring to FIG. 6 , transition line 36 exists where the butt-end 60 of the shingle in the row above ends, thus exposing portion 34 of shingle 30 .
[0024] Shingle 30 is configured as follows. From butt-end 40 it may be seen in FIG. 3 that the shingle is tapered until it reaches a termination and 38 . The preferred shingle thickness at butt-end 40 is about {fraction (7/8)}″, however, the thickness could fall any where within the {fraction (1/2)}″ to 1″ range—and might even be thicker—and still fall within the parameters of the present invention. The preferred thickness at termination end 38 is approximately {fraction (1/4)}″. These preferred dimensions make the ratio of butt-end thickness ({fraction (7/8)}″), versus termination end thickness, ({fraction (1/4)}″), about 7-2. Comparing this ratio to that of the conventional shingle shown in FIG. 1 , which was 4-1, reveals that the shingle of the present invention has a taper that is less extreme, ensuring more longitudinally consistent durability.
[0025] Another difference present in shingle 30 from that of shingle 10 is in its overall length. It will be recalled the length of conventional shingle 10 is about 24″. The approximately 18″ shingle of the present invention 30 is significantly shorter.
[0026] These differences in taper and thicknesses may be easily observed by comparing the profile of conventional shake's side-surface 24 in FIG. 1 with the side surface 44 of the shake of the present invention shown in FIG. 3 . The FIG. 3 profile formed by underside 42 , butt-end 40 , upper surface 32 , and tapered end 38 , is much different that that defined by underside 22 , butt-end 20 , upper surface 12 and tapered end 18 of the conventional shake.
[0027] The method of fastening shake 30 to the roof is done using fasteners 48 . Fasteners 48 may be electro-galvanized staples or nails. Alternatively, they could be constructed of stainless steel to make them more weather resistant. The fasteners 48 are driven through shake 30 at points approximately one inch up from the transition line 46 and approximately one inch in from the sides 44 of the shake on both sides.
[0028] It will now be described the manner in which the shingle is to be chemically treated. The chemical used in applicant's process if known as chromated-copper-arsenate (CCA). CCA is widely used to preserve wooden things. It has most often conventionally been used to preserve wooden articles that are produced from soft woods. Some examples of soft woods might be lodge pole white, jack and red pines. Because pine tends to rot, the CCA is applied in these conventional methods to provide a barrier between the environment and the wood. It has typically been applied to the article on which it is being deposited under pressure. This is so that it penetrates well below the surface of the wood. The chromium component in the CCA bonds with the cellulose in the wood and undergoes a valence change from the hexavalent to the trivalent state. Once this change in states has occurred, the CCA, over a relatively short period of time, under pressure, will not leach out of the wood over the course of time.
[0029] The methods of the present invention involve using this CCA method which has already been well-established in the art in terms of being used on pines, to treat cedar for use on shake roofs. Though a different recipient (cedar) is used for the CCA, the process for administering the CCA is the same. It is administered to the shakes, and allowed to impregnate the wood (under pressure) over time. These methods of administering the CCA will be known to those skilled in the art. The only significant difference from that which is conventional is that the CCA is being used to treat shakes instead of the types of wood, and types of products described as conventional above.
[0030] Once the cedar shingles for use in the present invention methods have been appropriately CCA treated, they will be ready for installation on a roof.
[0031] FIG. 5 shows how the shingles are installed from a side view. In the figure, it may be seen that in upper shingle 50 , is disposed on top of shingle 30 . Also seeing in this figure is that the butt-end 60 of shingle 50 is what defines the transition line between exposed surface 34 and covered surface 36 on shingle 30 . In FIG. 4 , it may also be seen that transition line 46 along with the edges of the shingle define an exposed surface ( 34 ) which is much smaller than the exposed surface 14 of the conventional shake.
[0032] This different in exposure area is significant when coupled with the concept that shake 30 is significantly thicker and less tapered than is conventional. This aspect of the present invention provides numerous advantages. For one, the shingle will be held more tightly to the roof. This is because the shingle in the row immediately above it 50 is thicker, and thus more steady, and has more weight. This helps secure shingle 30 (referring to FIG. 5 ) better because the bottom of shingle 50 is pressing down harder. This greatly improves the wind resistance and other durability aspects of the shingle 30 . The wind resistance will also be improved by the aerodynamics of shingle 30 . When conventional shingles become slightly loosed, as will occur over time, they are more easily blown off because of their thinness. There is also more potential lift area that makes the shingle vulnerable to wind that might enter under and lift up on the shingle.
[0033] Another advantage created by minimizing the exposure area 34 of the shingle versus the shingles thickness is that there is less surface per shingle that is exposed to the elements. This will minimize environmental degradation.
[0034] Also advantageous in shingle 30 over conventional shingle 10 , which is thinner, wider, and longer, is that the shingle of the present invention is more durable to hail and to workers stepping on it. Like a pencil is more easily broken than a baseball bat, so is prior art shingle 10 more easily broken than present invention shingle 30 . Because of the more uniform thickness of shingle 30 along its length. These factors in combination with the more gradual taper of shingle 30 , make it much more durable than the conventional shingle.
[0035] A further advantage in the shingle of the present invention is due to the application of CCA. The application of this CCA in combination with the durability improvements caused by the present invention shingles configurations make it even more durable and weather resistant. This is because of the barrier the chemical creates. The combination of all these factors in combination provide a shingled roof which is capable of withstanding winds exceeding 130 mph. Additionally, it may be walked on without the fear of causing significant damage to the shingles. Users will also be added the benefit of improved insulation. The shingles will keep the home cooler in the summer and warmer in the winter. A roof constructed of the methods of the present invention will also be able to withstand extreme temperatures and freeze-thaw conditions found in various climates. Insect, dry rot and algae problems will also be greatly reduced.
[0036] Although the invention has been described with reference to the preferred embodiment illustrated in the attached drawing figures, it is noted that substitutions may be made and equivalents employed herein without departing from the scope of the invention as recited in the claims.
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Disclosed is a shingle configuration and method of deploying shingles both of which provide improved durability and element resistance. With respect to how the shingles are configured, they are made shorter, thicker, less wide, and have a less dramatic taper than do conventional shingles. Additionally, these shingles are pressure treated with a chemical that provides a barrier making them resistant to wood rot and other elemental maladies. The shingles are then applied to the roof in such a manner that the exposed surface of each individual shingle will be reduced.
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RELATED APPLICATIONS
[0001] This application claims priority to U.S. Provisional application Ser. No. 61/426,584 filed Dec. 23, 2010 and incorporated herein in its entirety.
BACKGROUND OF THE INVENTION
[0002] A. Field of Invention
[0003] This invention pertains to a bracket system for window treatments configured and structured to accept and support several window shades and other types of treatments.
[0004] B. Description of the Prior Art
[0005] Most window treatments consist of an elongated member that supports one or more decorative elements to cover a window, a door, some other openings, or purely for decorative purposes. Controls are added that are normally at least partially in, or attached to the elongated member and used to selectively , open or close the treatment and/or perform various other operations thereon.
[0006] The elongated member is mounted either within the opening or on a vertical wall just adjacent to the opening using various types of brackets. FIG. 1 shows an end view of a conventional elongated member having an end bracket 10 with a conventional L-shaped fascia 12 disposed between the end brackets (such as 10 ) and arranged to protect and hide various interior elements of the window treatment. The bracket 10 is formed with a plurality of holes 14 for mounting the bracket. The fascia 12 is made from a sheet of metal, plastic or other relatively light but strong material.
[0007] The bracket 10 holds a clutch mechanism 16 operated by a chain cord 20 having ends 20 A, 20 B. The clutch mechanism 16 includes a pulley 18 operated by a chain chord 20 having cord ends 20 A, 20 B pulling on one end 20 A or the other 20 B causes the pulley to rotate in one direction or another thereby performing a predetermined function for the window treatment.
[0008] The fascia is made with a thin lip 22 bent inwardly. The bracket 10 is made with a corner opening 24 having at its front edge a tongue 26 sized and shaped to fit into the lip 22 . The fascia 12 has a generally L-shaped cross-section with a major portion 30 terminating with lip 22 and a minor portion 32 .
[0009] The window treatment is installed as follows. The bracket 10 and another similar bracket are mounted. The window treatment is mounted between the brackets. The fascia 12 is then positioned with its major portion being orientated essentially horizontally and the lip 22 is inserted into opening 24 . The fascia 12 is then rotated around tongue 26 clockwise causing the minor portion 32 to come into contact with and snap unto bracket 10 reaching the position shown.
[0010] This arrangement has several disadvantages. First, a different-shaped bracket must be provided for each kind of window treatment. This can expensive and problematical for small distributors who cannot be fiscally burdened by requiring them to carry a large number of different types of brackets. Second, in some instances, the bracket must be mounted on horizontal wall W (using some other openings that have been omitted in FIG. 1 ). However, as can be seen in FIG. 1 , tong 26 has to be disposed below the wall W by several millimeters to accommodate the fascia 12 and allow it to be secured to the bracket. As a result, the upper-most edge of the fascia 12 is always slightly below and not flush with the wall W. This feature is found objectionable by many persons because it leaves a very narrow gap between the fascia 12 and the wall W which allows some light to be seen above the fascia that is not pleasing esthetically.
[0011] Furthermore, existing brackets in general are sized and constructed to accommodate only window dressings of certain preselected configurations, and must be customized for each configuration.
SUMMARY OF THE INVENTION
[0012] The present invention addresses the problems discussed above and provides solutions to solve the problems. More specifically, a bracket system is provided that includes two brackets receiving ends of a window dressing. The brackets have a generally rectangular or square base with two side edges, a top edge and a bottom edge. Some of the edges are provided with panels disposed perpendicularly to the base.
[0013] The system further includes a fascia that is preferably L-shaped with a vertical member and a horizontal member. In one embodiment of the invention, the vertical member is mounted on the brackets so that a small portion of the fascia extends above the bracket thereby providing a neater look by blocking light from passing through above the fascia.
[0014] In another aspect of the invention, the panels or edges of the brackets are configured to accept the fascia in either a first configuration in which the horizontal part is on top of the brackets and a second configuration in which the fascia horizontal part is attached to the bottom of the brackets.
[0015] Plates may be mounted or attached to the brackets for accepting the ends of window shades. Adapters are attached to the plates, if necessary, various plates having different configurations to conform to or receive window dressings of different kinds. In some configuration, two or more parallel window dressings are supported by a single pair of brackets.
BRIEF DESCRIPTION OF THE DRAWINGS
[0016] FIG. 1 shows an end view of a prior art window dressing and its end bracket;
[0017] FIG. 2 shows an orthogonal exploded view of a bracket system for a window treatment constructed in accordance with this invention;
[0018] FIG. 3 shows a front view of the bracket system;
[0019] FIG. 4 shows an end view of the bracket system;
[0020] FIG. 5 shows an elevational view of a bracket with a plate;
[0021] FIG. 5 AA shows a side view of the plate;
[0022] FIG. 5 BB shows a side view of the bracket;
[0023] FIG. 5A shows a side view of the facie for the bracket system;
[0024] FIG. 5B shows an elevational view of the bracket used in the system;
[0025] FIG. 5C shows top view of the bracket of FIG. 5B ;
[0026] FIG. 6 shows a side sectional view of the fascia attached to a bracket;
[0027] FIG. 7 shows an enlarged side view of the fascia attached to the bracket;
[0028] FIG. 8 shows an orthogonal view of a bracket of FIGS. 2-5 supporting some of the components of a window covering;
[0029] FIG. 9 shows an orthogonal view of the invention configured to receive and support two window dressings attached to a single bracket;
[0030] FIG. 10 shows an orthogonal view of the some of the components of the window dressing of FIG. 9 ;
[0031] FIG. 11 shows an orthogonal view of the invention configured to receive and support a window dressing having a large diameter;
[0032] FIG. 12 shows an orthogonal view of the invention configured with an adapter plate shaped to receive and support a motor-driven a window dressing;
[0033] FIG. 13 shows an orthogonal view of the invention configured with an adapter having three holes;
[0034] FIG. 14 shows an alternate embodiment of the bracket having a plate three holes in a row;
[0035] FIG. 15 shows an alternate embodiment of the bracket receiving a clutch plate; and
[0036] FIG. 16 shows an alternate embodiment of the bracket receiving a plate adapted to receive a motorized window shade.
DETAILED DESCRIPTION OF THE INVENTION
[0037] The major elements of bracket system constructed in accordance with this invention are shown in FIGS. 2-5B . The bracket system 100 includes two, preferably identical, end brackets 102 , 104 . The end brackets are 102 , 104 preferably are made of a conventional metallic alloy using conventional techniques, such as stamping.
[0038] Each end bracket includes a flat rectangular base 106 and three panels 108 , 110 , 112 disposed along three sides of the base 106 . The fourth side has a tab 114 . The three panels and the tab are substantially perpendicular to the base 106 . Panels 108 , 110 are preferably identical and the panel 112 is configured so that it is symmetrical about a vertical axis of the brackets 102 , 104 . The three panels have a plurality of slots and perforations as described in more detail below.
[0039] Attached to the two brackets is a fascia 116 . As shown in detail in FIG. 5A , the fascia 116 is L-shaped and has two sections 118 , 120 . Section 118 is provided with an intermediate lip 122 shaped to form a channel 124 . Section 120 is terminated with a lip 126 forming a channel 128 . It should be understood that the dimensions of the lips 122 and 126 and channels 124 and 128 are somewhat exaggerated in FIG. 5A for the sake of clarity but in actuality there are shaped so that the channels are about the same cross-sectional width as the thickness of bracket 102 to form an interference therewith. The length of the fascia 116 is dependent on the width of the window dressing. Its total height HF is equal to H 1 +H 2 , where H 1 is the distance from the free edge of section 118 to the lip 122 . The fascia has a width W. The fascia 116 can be extruded aluminum or other similar material.
[0040] Details of the bracket 102 are shown in FIGS. 5A and 5B . Panel 110 is formed of three sections. Two of the sections 130 , 134 are mirror images and include apertures 136 for mounting the brackets and to make the brackets lighter. The central section 132 has essentially the shape of an elongated tongue. Panel 110 has several dimensions that have special importance.
[0041] The distance between the side edge SE of section 132 and the outer surface of panel 108 is equally to the width W of fascia 116 . The distance between side edge SE 2 of section 134 and the outer surface of panel 108 is at least H 1 . The length of panel 108 is H 2 . The distance between the top edge TE of panel 102 and the outer surface of panel 110 is at least H 1 . The distance between the side edge SE 3 of tab 114 and the outer surface of panel 108 is W. The distance between the bottom edge BE of panel 108 and the bottom surface of tab 114 is at least H 1 . As a result of these dimensions, the fascia 116 can be mounted on to the brackets 102 , 104 in two configurations. In one configuration, the section 120 is attached to the bottom of the bracket as shown in FIG. 5A . In the second configuration, the section 120 is attached to the top of the bracket. In either case, the section 118 is attached to the panel 108 (or 112 ). Moreover, the portion 131 of section 118 extends vertically further then the panel 110 of bracket 102 by amount sufficient to insure that imperfections in the window seal or installing the bracket 102 slightly below the window seal does not result in a gap of light seen above the window dressing. For example, the portion 132 may exceed the top surface of section 110 by about 1/32-⅜″. Moreover, the bracket and its panels are shaped so that fascia 116 is installed by first inserting its portion 131 into either zone Z or Y (see FIG. 5B ) and then pivoting it to snap onto the brackets 102 , 104 . The final position of the facie is shown in FIGS. 6 and 7 .
[0042] In addition, the plate 230 also has on one side a plurality of tabs 135 and on the other side a panel 137 . As seen in FIG. 5 AA, the panel 137 is formed of three sections 137 A, 137 B, 137 C. Each tab 135 is shaped so that it is angled slightly to permit the plates 230 to be press-fit into the brackets 102 , 104 with the tabs 135 engaging the inner surfaces of slots 113 A, 113 B, 113 C (these slots are shown in FIG. 5 BB) of section 108 .. Both sections 108 and 110 further include a slot 113 D which is somewhat longer then the slots just described. Section 137 B is bent slightly outwardly and is sized and shaped to engage slot 113 D on section 110 . In other words, panel 137 and tabs 135 cooperate to maintain the plate 230 in place within the bracket 102 , 104 .
[0043] Completing the system, there are two end caps 130 (shown in detail in FIGS. 3 and 4 ). Each end cap may be sized to cover one of the brackets 102 , 104 and serve mostly a decorative purpose. On their inner surface, caps 130 may be provided with fingers 132 ( FIG. 2 ) that form an interference fit with holes 134 to mount and keep the end caps 130 on the brackets. Typically, end caps may be about 5.12×5.14 in and may be molded plastic or other materials.
[0044] The sizes specified herein is particularly useful for various configurations, such as one large shade, two or more smaller shades, a shade with a clutch, a shade with a wound spring or other mechanisms. Various plates, adapters, etc. are mounted (temporarily or permanently) on the brackets to accommodate various sizes, numbers and types of window shades. This modular design allows the bracket system to be used in a large variety of uses and applications. The remaining figures show some exemplary configurations for the bracket system illustrating just some of the configurations that may be used to support various window coverings.
[0045] Getting back to FIG. 5 , bracket 102 is shown with a plate 230 formed with a set of five slots and holes arranged to receive the ends of respective window coverings, either directly, or via adapters.
[0046] Each set includes a circular hole 240 and two rectangular slots 242 arranged on either side of the hole 240 . This is a standard configuration and can be used to accept a window covering at each set of slots and holes. (Note to Joe—is this true?) For example, in FIG. 5 , adapters 140 are provided that mount on plates 230 . The adapters are shaped and sized to receive and a standard clutch 144 at one end and a plain idler end (not shown) on the other bracket. FIG. 8 shows an enlarged isometric view of the bracket 104 with a plate 230 , an adapter 140 and a clutch 144 .
[0047] FIGS. 9 and 10 show configuration in which two parallel window shades 150 , 152 with respective clutches 154 , 156 are mounted on the same bracket 104 and plate 230 . Each of the shades can be operated on its own and can be replaced independently.
[0048] FIG. 11 shows bracket 104 , plate 230 and adapter 140 supporting a clutch 160 for receiving a window dressing having a relatively large diameter.
[0049] FIG. 12 shows bracket 104 with a plate 170 and an adapter 171 . Adapter 171 has two lateral horizontal pins 173 sized and shaped to receive and support the ends of a known motorized window shade (not shown). for supporting the pin end of a motorized window shade (not shown). In this figure, an intermediate support 172 is also shown that may be mounted on the wall, a window well, etc., and then couple to the fascia of the bracket system. This intermediate bracket is necessary for very long window dressings that may be too heavy to be supported by only two brackets and may sag in the middle.
[0050] FIG. 13 shows a bracket 104 with plate 170 and adapter 178 having three holes 173 A aligned horizontally. This adapted is useful for supporting another line of known window dressings.
[0051] FIG. 14 shows details of the plate 170 used in FIGS. 12 and 13 .
[0052] FIG. 15 shows details of a plate 180 for a different kind of clutch.
[0053] FIG. 16 shows a bracket 104 with a plate 180 for supporting a SOMFY ST-50 motor.
[0054] Numerous modifications may be made to the invention without departing from its scope as defined in the appended claims;
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A bracket system for window dressing includes two brackets configured to be attached to an architectural member, such as a window well, a wall or a ceiling and receive the ends of window dressings. The brackets have edges adapted to receive a fascia designed to hide the window dressing. Preferably, the fascia has a front wall designed to snap onto the brackets and is sized so that it extends above the brackets to provide a neater and cleaner look. The fascia may be L-shaped with a vertical and a horizontal member and the brackets may be configured so that the horizontal member attaches either to the top or to the bottom of the brackets.
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This application is a continuation of application Ser. No. 07/858,071 filed Mar. 26, 1992, now abandoned.
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to a wireless communication device for transmitting and receiving data, for example, by radiowaves, and to a printing system employing such a device.
2. Description of the Related Art
In a network of conventional wireless communication devices, the transmission power of each device is set strong enough to be received by the farthest device. A network of wireless communication devices is illustrated in FIG. 5, in which a symbol "0" indicates a wireless communication device. The transmission power of a device 10 is set so that a device 1 farthest from the device 10 can receive the data sent by the device 10. The transmission power of a device 4 can be set lower than that of the device 10, since the device 4 is located substantially at the center of the network so that the distance from the device 4 to the farthest device therefrom is shorter than the distance from the device 10 to the device 1.
Thus, in a network, different devices may have different transmission power levels, according to their locations in the network.
Such a network or device, however, has problems as described below.
Devices located in the peripheral area of the network, such as the device 10 in FIG. 5, use significantly more power than devices located in the central area of the network, such as the device 4. For example, the device 10 always uses the same high power to transmit data to any device, whether to the farthest device 1 or to the neighboring devices 4, 7 and 8. Also, the high power radiowaves sent out by the device 10 naturally reach the area outside the network (e.g., the area below the unit 10 in FIG. 5) as well, so that communication between the devices in the network can be received by a device outside the network. This becomes a significant problem when confidential data is communicated in the network. As a result, security protection becomes difficult.
SUMMARY OF THE INVENTION
An object of the present invention is to solve the above problems by providing a wireless communication device which changes its transmission power according to a current receiver, for example, to a level just high enough to communicate with the current receiver device. Thus, a device according to the present invention requires less total power and contributes to network security.
Another object of the present invention is to provide a printing system which uses such a device and thus does not require high power.
Other objects, features and advantages of the present invention will become apparent in the attached drawings, the detailed description of the preferred embodiments and the claims.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a block diagram of a communication device according to one embodiment of the present invention.
FIGS. 2 and 3 show a flowchart illustrating the operation of the device shown in FIG. 1.
FIG. 4 is a time chart of transfer data.
FIG. 5 illustrates a network of devices according to the present invention.
FIG. 6 is a block diagram of a communication device used in a printer of a printing system according to another embodiment of the present invention.
FIG. 7 is a block diagram of a communication device used in a host computer of the above mentioned printing system.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
The preferred embodiments of the present invention will be described hereinafter with reference to the drawings.
[Embodiment 1]
FIG. 1 shows a communication device comprising: an antenna 101 for transmitting and receiving radiowaves; a sending unit 102 for sending out data; a receiving unit 103 for receiving data; a control unit 104 having an environment setting unit 107; a memory 105 for storing data; and operation unit 106. Each of such devices in a network (FIG. 5) has an identification code.
Referring to FIG. 2, when a communication device in a network is powered to transmit data in Step S1, a receiver is selected from the other communication devices in the network (Step S2). Then, the sender device determines in Step S3 the minimum transmission power required for the transmission of the data to the receiver device. This operation may be carried out either serially for all the other devices when powered, or specifically for the receiver device when data is to be transmitted.
In detail, the sender device sends the receiver device the command to sense its own state(Step S4), and judges whether the transmission power is proper or not based on the status which the receiver sends to the sender (Steps S5 and S6). When it is judged to be improper, such as when the sender receives a status signal indicating that the reception has been failed or when the sender does not receive a status signal from the receiver, the sender changes the level of transmission power to send the command again in Step S3. Alternatively, the sender may send, together with the command, data regarding the transmission power level to transmit the command, and the receiver changes its transmission power level, according to the received data, for example, to send a status signal to the sender.
When the transmission power level is judged to be proper in Step S6, the control unit 104 of the sender device stores the data regarding the transmission power level (Step S7), in association with the ID code of the receiver device. On the other hand, the control unit 104 of the receiver also stores the data regarding the own transmission power level of the sender, in association with the ID code of the sender (Step S8). The transmission power level is stored in the control unit 104 of the receiver, based on, for example, the above-mentioned data regarding the transmission power received, together with the command, from the sender. In such a way, the environment setting unit 107 included in the control unit 104 of each device stores a table containing the transmission power levels corresponding to the other devices.
Referring to FIG. 3, the sender device examines whether the receiver device is ready for receiving or not (Step S10). When the receiver is not ready, the sender waits for the receiver to be ready (Step 11). When the receiver is ready, the sender sends out the start bit to the receiver (Step S12) so that data transmission will start. Then, the sender transmits the data to the receiver (Step S13) and then, sends out the stop bit (Step S14). Data may be sent out by the unit of a character or a block of several characters, as shown in FIG. 4.
Next, the sender device judges whether any reception errors have occurred in Step S15. For this judgment, various methods can be used, such as, a parity check in which a parity bit is added to each of the data, a successive sending check in which data is sent twice for error detection, an inverse check in which data and the inverse of such data (each bit, "1" or '0", of the data is inverted) are used as the check codes, etc.
Only when it is judged that there is no reception error, does the receiver send the ACK signal to the sender (Step S16). When a reception error is found, the receiver requests the resending of the data in Step S17, and the sender sends the data again via Step S12. In such a case, the transmission power level may be changed. If it is changed, the data of the transmission power level stored in the environment setting unit 107 is updated accordingly and the operation illustrated in FIG. 2 may be omitted. The procedure as described above is repeated for data transfer (If the data transfer is performed by the unit of a character, data transfer operation is performed several times according to the amount of data to be transferred).
[Embodiment 2]
To handle a state where a plurality of communication devices simultaneously transmit data to one device in a network, a wireless communication device according to this embodiment is equipped with a function such as interruption or polling; thereby, the receiver device receives data successively from the sender devices according to the priority of each sender device, or the receiver accesses to a sender in order to request a data transfer when the receiver idles. Further, the polling enable devices may be equipped with a function such that a receiver remotely controls (on radiowaves) the transmission power of a sender during the setting of the transmission power.
If a wireless communication device is added to a network of such wireless communication devices, each existing device stores the data of the distance to the added device and the ID code of the added device, and the added device stores the data of the distance to each of the existing devices and the ID code thereof. The ID codes and the distance data are stored in the environment setting unit 107 (e.g. an E 2 PROM) of the control unit 104 of each device. As an alternative, to transmit data to an uncataloged device (newly added to the network), a sender device and the uncataloged device (the receiver) may carry out the operation shown by the flowcharts in FIGS. 2 and 3, starting with the lowest transmission power level, and the sender and/or the receiver automatically catalog each other.
As described above, since a wireless communication device according to the present invention uses a transmission power level specific to a receiver device, such a device requires less total power and makes it difficult for an outside device to receive a communication of the network. Also, since the transmission power is kept relatively low, wireless interference is substantially prevented.
Since the proper transmission power level varies in proportion to the distance to receivers, the initial value for the transmission power can thus be set. Also, since a device according to the present invention adjusts the transmission power to a proper level which varies depending on external noises, location factors, weather conditions, etc., the reliability or quality of communication is upgraded.
[Embodiment 3]
A wireless communication device according to the present invention can be employed in a communication system to transmit print data from a host computer to a printer. According to this embodiment, one host computer (the sender) transmits print data to a plurality of printers (the receivers) on radiowaves. In FIG. 5, the host computer may be the device 10, and the printers may be the other devices 1 to 9.
Referring to FIG. 6, the printer having an interface for wireless communication comprises: an antenna 601; a receiving unit 602; a sending unit 603; a page memory 604; a bit map memory 605; a font memory 606; a main control unit 607; an environment setting unit 608; an operating panel 609; a printer engine interface 610; and a printer engine 611.
Data transmitted from the host computer is received by the antenna 601 and sent through the receiving unit 602 to be temporarily stored in the page memory 604. When data for one page is accumulated in the page memory 604, the main control unit 607 reads from the font memory 606 the bit map data corresponding to the character data stored in the page memory 604 and develops the bit map data as a dot pattern in the bit map memory 605. Then, the main control unit 607 reads the developed dot pattern data from the bit map memory 605 and sends the data to the printer engine interface 610. The printer engine 610 converts the word (16 bits) or byte (8 bits) data to serial data (P-S conversion) and outputs the converted data as a VIDEO signal to printer engine 611. Printing is thus started. Also, the main control unit 607 sends the status of the printer (e.g. READY, PAPER OUT, WARMING UP) through the sending unit 603 to the host computer. Paper size, the attributes of the print characters (typeface, size, etc), the number of copies, etc. can be determined according to the preferences of a user by operating the operating panel 609. The ID code of the printer and data of the distance to the host computer are stored in the environment setting unit 608. Usually, a nonvolatile memory is used to keep data even if the printer is switched off.
Referring to FIG. 7, the host computer having a wireless communication interface comprises: an antenna 701; a receiving unit 702; a sending unit 703; a main control unit 704; a CPU (e.g. a microprocessor) 705; ROM 706 storing a bootstrap program of the host computer; RAM (e.g. DRAM) 707 for the work area (RAM is memory into which data can be written and from which data can be read); an environment setting unit 708 including a memory, e.g. a nonvolatile memory, to store the printer's ID code and the distance data, both of which are required by the wireless communication device of the present invention; a hard disk unit 709; a display interface 711; a CRT 710; a keyboard interface 712; and a keyboard 713.
To transmit the print data of a document composed by using document composition application software (e.g. an editor), the main control unit 704, referring to the information stored in the environment setting unit 708, selects a printer in the network, and sends the print data to the sending unit 703. The print data is accordingly transmitted as serial data from the antenna 701 on radiowaves to the selected printer. The receiving unit 702 receives a status signal from the printer and sends the received signal to the main control unit 704.
In the above-described embodiments, radiowaves are used, but infrared rays, ultrasonic waves or light rays may also be used.
It is to be understood that the present invention is not limited to the disclosed embodiments but intended to cover various modifications and equivalent arrangements included within the spirit and scope of the appended claims.
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In a network of wireless communication devices, each device has a unit for transmitting information, a unit for variably controlling the transmission power for transmission of information, a unit for receiving information transmitted, and a unit for controlling the other units. Each device shifts the transmission power to a level proper to a current receiver device.
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CROSS-REFERENCE TO RELATED APPLICATION
This application claims the benefit of U.S. Provisional Application No. 60/406,072 filed Aug. 26, 2002, which is hereby incorporated by reference in its entirety.
BACKGROUND OF THE INVENTION
1. Field of the Invention
This invention is generally directed to a novel polymorph of N-methyl-N-(3-{3-[2-thienylcarbonyl]-pyrazol-[1,5-α]-pyrimidin-7-yl}phenyl)acetamide which has activity over a wide range of indications, and is particularly useful for the treatment of insomnia, and to related processes, compositions and methods.
2. Description of the Related Art
The term “insomnia” is used to describe all conditions related to the perception of inadequate or non-restful sleep by the patient (Dement, International Pharmacopsychiatry 17:3-38, 1982). If left untreated, insomnia may result in disturbances in metabolism and overall body function including reduced productivity and significant changes in mood, behavior and psychomotor function, and a higher incidence of morbidity and mortality.
Traditionally, the management of insomnia includes treatment and/or mitigation of the etiological factors, improving sleep hygiene and the administration of hypnotic agents. The early hypnotic agents, such as barbiturates, while effective, elicited a spectrum of unwanted side effects and longer-term complications. For example, barbiturates have the potential to result in lethargy, confusion, depression and a variety of other residual effects many hours post dosing, as well as having a potential for being highly addictive.
During the 1980's, the pharmaceutical treatment of insomnia shifted away from barbiturates and other CNS depressants toward the benzodiazepine class of sedative-hypnotics. This class of sedative-hypnotic agents showed substantial effectiveness in producing a calming effect which results in sleep-like states in man and animals (Gee et al., Drugs in Central Nervous Systems, Horwell (ed.), New York, Marcel Dekker, Inc., 1985, p. 123-147) and had a greater safety margin than prior hypnotics, barbiturates or chloral hydrate (Cook and Sepinwall, Mechanism of Action of Benzodiazepines, Costa and Greengard (eds.), New York, Raven Press, 1975, p. 1-28). As with barbiturates, however, many benzodiazepines also possess side effects that limit their usefulness in certain patient populations. These problems include synergy with other CNS depressants (especially alcohol), the development of tolerance upon repeat dosing, rebound insomnia following discontinuation of dosing, hangover effects the next day, and impairment of psychomotor performance.
More recently, a new class of agents has undergone development. These agents are non-benzodiazepine compounds, which bind selectively to a specific receptor subtype of the benzodiazepine receptor. This receptor selectivity is thought to be the mechanism by which these compounds are able to exert a robust hypnotic effect, while also demonstrating an improved safety profile relative to the non-selective, benzodiazepine class of agents. The first of these agents to be approved by the United States Food and Drug Administration (FDA) for marketing in the United States was Ambien (zolpidem tartrate), which is based on the imidazopyridine backbone (see U.S. Pat. Nos. 4,382,938 and 4,460,592). In addition to Ambien, another compound known as Sonata (zaleplon), which is a pyrazolopyrimidine-based compound, has received FDA approval (see U.S. Pat. No. 4,626,538). Other non-benzodiazepine compounds and/or methods for making or using the same have also been reported (see, e.g., U.S. Pat. No. 4,794,185, 4,808,594, 4,847,256, 5,714,607, 4,654,347; 5,891,891).
While significant advances have been made in this field, there is still a need in the art for compounds that are effective as sedative or hypnotic agents generally, particularly in the context of treating insomnia. One such compound is N-methyl-N-(3-{3-[2-thienylcarbonyl]-pyrazol-[1,5-α]-pyrimidin-7-yl}phenyl)acetamide (referred to herein as “Compound 1”). Compound 1 is disclosed in U.S. Pat. No. 6,399,621 and has the following chemical structure:
In addition, U.S. Pat. Nos. 6,384,221 and 6,544,999 are directed to polymorph Form I and Form II of Compound 1, while U.S. Pat. Nos. 6,472,528 and 6,485,746 are directed to synthesis and controlled release, respectively, of Compound 1.
While Compound 1 has proven particularly promising for the treatment of insomnia, improved forms of this compound are desired, particularly with regard to enhanced solubility, oral bioavailability, ability to be readily formulated, ease of synthesis, and/or physical stability. The present invention fulfills one or more of these needs and provides further related advantages.
BRIEF SUMMARY OF THE INVENTION
The present invention is generally directed to a novel polymorphic form of Compound 1, referred to herein as “polymorph Form III”. Polymorph Form III exhibits a predominant endotherm peak at about 191° C. (as measured by a TA 2920 Modulated Differential Scanning Calorimeter (DSC) at a scan rate of 10° C. per minute). Polymorph Form III also exhibits an X-ray Powder Diffraction pattern with characteristic peaks (expressed in degrees 2θ (+/−0.2°θ) at one or more of the following positions: 10.2, 13.3, 18.9, 20.7, 22.2, 28.1 and 30.8. More specifically, such characteristic peaks are at 18.9 and 28.1, and further at 10.2, and further at 13.3, 20.7, 22.2 and 30.8.
Polymorph Form III has utility over a wide range of applications, including utility as a sedative and/or hypnotic agent generally and, more specifically, for the treatment of insomnia. Thus, in another embodiment, methods are disclosed for treating various conditions, including insomnia, by administering an effective amount of polymorph Form III to an animal or subject in need thereof (referred to herein as a “patient”), and typically to a warm-blooded animal (including a human).
In one embodiment, polymorph Form III is substantially pure—that is, containing less than 2% by weight total impurities, less than about 1% by weight water, and less than 0.5% by weight residual organic solvent; or, in a more specifically embodiment, less than 1% by weight total impurities, less than about 0.75% by weight water, and less than 0.4% by weight residual organic solvent.
In another embodiment, Compound 1 is in the form of a composition or mixture of polymorph Form III along with one or more other crystalline, solvate, amorphous, or other forms of Compound 1. For example, such a composition may comprise polymorph Form III along with one or more other polymorphic forms of Compound 1, such as polymorph Form I and/or Form II. More specifically, the composition may comprise from trace amounts up to 100% polymorph Form III, or any amount in between—for example, the composition may comprise less than 0.1%, 0.5%, 1%, 2%, 5%, 10%, 20%, 30%, 40% or 50% by weight of polymorph Form III based on the total amount of Compound 1 in the composition. Alternatively, the composition may comprise at least 50%, 60%, 70%, 80%, 90%, 95%, 97%, 98%, 99%, 99.5% or 99.9% by weight of polymorph Form III based on the total amount of Compound 1 in the composition.
Prior to administration, and in further embodiment, polymorph Form III may be formulated as a pharmaceutical composition that contains an effective dosage amount of polymorph Form III in combination with one (or more) pharmaceutically acceptable carrier(s). Such compositions may assume a variety of forms, including pills, tablets and capsules for oral administration.
In still another embodiment, the pharmaceutical composition comprises an effective dosage amount of Compound 1, wherein Compound 1 comprises at least a certain percentage of polymorph Form III (based on the total amount of Compound 1 present in the composition—that is, the total amount of Compound 1 being 100%). In other words, at least a certain percentage of Compound 1 present within the pharmaceutical composition exists as polymorph Form III, with the remainder of Compound 1 being in a different form, including (but not limited to) polymorph Form I, polymorph Form II, or any other crystalline, solvate or amorphous form(s).
In yet a further embodiment, this invention provides processes for making polymorph Form III. For example, polymorph Form III may be made by (a) providing a heated crystallization solvent comprising Compound 1, (b) adding water and a nucleating agent (such as carbon or crystals of polymorph Form III) thereto in amounts sufficient to induce crystallization of polymorph Form III, and (c) collecting crystallized polymorph Form III. Optionally, the crystallization solvent can be cooled after step (b). In an alternative embodiment, polymorph Form III may be made by (a) providing a heated crystallization solvent comprising Compound 1, (b) adding the heated crystallization solvent to a co-solvent or mixture of co-solvents, (c) adding a nucleating agent thereto in amounts sufficient to induce crystallization of polymorph Form III, and (d) collecting crystallized polymorph Form III. Further, polymorph Form III made according to one or more of the processes of this invention is also disclosed.
These and other aspects of this invention will be apparent upon reference to the following detailed description and attached figures. To that end, certain patent and other documents are cited herein to more specifically set forth various aspects of this invention. Each of these documents is hereby incorporated by reference in its entirety.
BRIEF DESCRIPTION OF THE FIGURES
FIG. 1 is a Differential Scanning Calorimetry (DSC) thermogram of polymorph Form III.
FIG. 2 is an X-ray powder diffraction spectrum of polymorph Form III.
FIG. 3 is an Raman FT Infrared spectrum of polymorph Form III.
DETAILED DESCRIPTION OF THE INVENTION
As mentioned above, the present invention is generally directed to a novel polymorphic form of Compound 1, referred to herein as “polymorph Form III”, as well as to compositions containing the same. Also disclosed are methods relating to the use of polymorph Form III by administration to a patient in need of the same, and to processes for making polymorph Form III.
Solids exist in either amorphous or crystalline forms. In the case of crystalline forms, molecules are positioned in 3-dimensional lattice sites. When a compound recrystallizes from a solution or slurry, it may crystallize with different spatial lattice arrangements, a property referred to as “polymorphism,” with the different crystal forms individually being referred to as a “polymorph”. Different polymorphic forms of a given substance may differ from each other with respect to one or more physical properties, such as solubility and dissociation, true density, crystal shape, compaction behavior, flow properties, and/or solid state stability. In the case of a chemical substance that exists in two (or more) polymorphic forms, the unstable forms generally convert to the more thermodynamically stable forms at a given temperature after a sufficient period of time. When this transformation is not rapid, the thermodynamically unstable form is referred to as the “metastable” form. In general, the stable form exhibits the highest melting point, the lowest solubility, and the maximum chemical stability. However, the metastable form may exhibit sufficient chemical and physical stability under normal storage conditions to permit its use in a commercial form. In this case, the metastable form, although less stable, may exhibit properties desirable over those of the stable form, such as enhanced solubility or better oral bioavailability.
In the case of Compound 1, two polymorphic forms (i.e., Form I and Form II) have previously been reported (see U.S. Pat. Nos. 6,384,221 and 6,544,999). Compound 1 is presently undergoing clinical trials for treatment of insomnia. In anticipation of potential large-scale production, significant effort has been directed to the commercial-scale production of Compound 1. During one such production run, an impurity was discovered within the end product. In an effort to remove the impurity, carbon was added, followed by recrystallization. As a result of this subsequent work up, it was surprisingly discovered that a new polymorph (i.e., polymorph Form III) was obtained. While not intending to be limited by theory, it is believed that the added carbon served as a nucleation site for formation of polymorph Form III.
The novel and surprising polymorph of this invention, polymorph Form III, may be characterized by, for example, melting point and/or X-Ray powder diffraction spectrometry. As shown in FIG. 1 , polymorph Form III exhibits a predominant endotherm peak at about 191° C. as measured by a TA 2920 (TA Instruments, New Castle, Del.) Modulated Differential Scanning Calorimeter (DSC) at a scan rate of 10° C. per minute with an Indium standard. As used herein, the term “about 191° C.” means a range of 190 to 192.5° C. In this regard, it should be understood that the endotherm measured by a particular differential scanning calorimeter is dependent upon a number of factors, including the rate of heating (i.e., scan rate), the calibration standard utilized, instrument calibration, relative humidity, and upon the chemical purity of the sample being tested. Thus, an endotherm as measured by DSC on the instrument identified above may vary by as much as ±1° C. or even ±1½° C. Accordingly, the term “about 191° C.” is intended to encompass such instrument variations.
The X-Ray powder diffraction spectrum for polymorph Form III is presented in FIG. 2 , and is set forth in tabular form in Table 1 below. The X-Ray powder diffraction was measured by a Siemens D500 Automated Powder Diffractometer equipped with graphite monochromator and a Cu (λ=1.54 Angstrom) X-ray source operated at 50 kV, 40 mA. Two-theta calibration is performed using an NBS mica standard. The sample was analyzed using the following instrument parameters: measuring range=4-40° 2θ; step width=0.050°; and measuring time per step=1.2 sec.
TABLE 1
X-Ray Powder Diffraction Spectral Lines
d value
2-θ°
Intensity
Intensity %
9.15587
9.652
1388
7.0
8.91589
9.912
7718
39.1
8.65670
10.210
19744
100.0
8.16181
10.831
572
2.9
7.88947
11.206
1398
7.1
6.85166
12.910
765
3.9
6.64840
13.306
4690
23.8
6.29329
14.061
396
2.0
5.24469
16.891
1398
7.1
5.19705
17.047
1731
8.8
5.05094
17.544
1170
5.9
4.76647
18.600
1567
7.9
4.69634
18.880
4865
24.6
4.34978
20.400
1131
5.7
4.29694
20.654
4611
23.4
4.12546
21.522
758
3.8
4.00186
22.195
2281
11.6
3.87889
22.908
1046
5.3
3.72796
23.849
321
1.6
3.56593
24.950
752
3.8
3.51637
25.307
716
3.6
3.40208
26.172
781
4.0
3.34446
26.631
1738
8.8
3.30597
26.947
764
3.9
3.23885
27.516
544
2.8
3.17029
28.124
4022
20.4
3.01819
29.572
480
2.4
2.97878
29.973
264
1.3
2.89811
30.827
2802
14.2
2.79651
31.977
890
4.5
2.77443
32.238
354
1.8
2.60380
34.415
407
2.1
2.53630
35.360
1434
7.3
2.41973
37.124
262
1.3
2.38437
37.695
253
1.3
The crystal structure of polymorph Form III was determined by single crystal X-ray diffraction analysis. A colorless plate of polymorph Form III having dimensions of 0.30×0.20×0.13 mm was mounted on a glass fiber in random orientation. Preliminary examination and data collection were performed with Mo K α radiation (λ=0.71073 Å) on a Nonius KappaCCD diffractometer. Data relating to the single crystal X-ray crystallography of polymorph Form III is presented in the following Tables 2-6.
TABLE 2
Crystal Parameters
Space Group
P2 1 /n
a, Å
9.5887(3)
b, Å
10.3985(4)
c, Å
17.5807(7)
α
90
β
96.8044(14)
γ
90
Z (molecules/unit cell)
4
Calculated Density (g/cm)
1.436
Temperature (K)
150
TABLE 3
Positional Parameters and Their Estimated Standard Deviations
Atom
x
y
z
U (Å 2 )
S(1)
0.46180(7)
−0.27982(8)
0.14578(4)
0.0384(2)
O(6)
0.62938(19)
−0.0547(2)
0.18402(10)
0.0382(6)
O(122)
0.8323(3)
0.2180(3)
−0.36178(12)
0.0643(8)
N(8)
0.7964(2)
0.1011(2)
0.09047(13)
0.0405(7)
N(9)
0.8076(2)
0.1723(2)
0.15438(12)
0.0317(6)
N(14)
0.8428(2)
0.0463(2)
−0.03115(11)
0.0286(6)
N(12A)
0.9717(5)
0.2278(5)
−0.2546(3)
0.0282(12)
N(12B)
0.9122(5)
0.3116(5)
−0.2521(3)
0.0319(14)
C(2)
0.3830(3)
−0.3736(3)
0.07383(18)
0.0420(9)
C(3)
0.4087(3)
−0.3309(3)
0.00378(17)
0.0391(8)
C(4)
0.4960(3)
−0.2230(3)
0.00787(16)
0.0331(7)
C(5)
0.5358(2)
−0.1829(3)
0.08160(14)
0.0294(7)
C(6)
0.6305(2)
−0.0805(3)
0.11554(13)
0.0280(7)
C(7)
0.7219(2)
−0.0121(2)
0.06857(13)
0.0264(7)
C(10)
0.8880(3)
0.2745(3)
0.15515(15)
0.0333(7)
C(11)
0.9616(3)
0.3131(3)
0.09337(14)
0.0311(7)
C(12)
0.9484(2)
0.2422(3)
0.02666(14)
0.0269(6)
C(13)
0.8667(2)
0.1337(2)
0.02781(11)
0.0154(5)
C(15)
0.7574(3)
−0.0389(3)
−0.00555(14)
0.0289(7)
C(121)
1.0127(3)
0.2801(2)
−0.04226(14)
0.0272(7)
C(122)
1.1408(2)
0.3451(2)
−0.03341(14)
0.0278(7)
C(123)
1.2019(3)
0.3852(3)
−0.09671(14)
0.0292(7)
C(124)
1.1380(3)
0.3615(3)
−0.17015(16)
0.0412(8)
C(125)
1.0100(4)
0.2988(4)
−0.17857(16)
0.0614(11)
C(126)
0.9462(3)
0.2586(3)
−0.11575(16)
0.0453(8)
C(12A)
0.8662(6)
0.2827(7)
−0.3016(3)
0.0324(17)
C(12B)
0.9236(7)
0.2085(7)
−0.2969(4)
0.0361(17)
C(13A)
1.0305(3)
0.1070(3)
−0.27368(17)
0.0446(9)
C(13B)
0.8135(3)
0.4141(3)
−0.27623(17)
0.0430(9)
H(2)
0.328
−0.447
0.082
0.050
H(3)
0.371
−0.370
−0.043
0.047
H(4)
0.525
−0.182
−0.036
0.040
H(10)
0.898
0.326
0.200
0.040
H(11)
1.020
0.387
0.098
0.037
H(15)
0.723
−0.112
−0.034
0.035
H(122)
1.186
0.362
0.016
0.033
H(123)
1.289
0.430
−0.090
0.035
H(124)
1.181
0.388
−0.214
0.049
H(126)
0.857
0.217
−0.123
0.055
U eq = (1/3) Σ i Σ j U ij a* i a* j a i · a j
Hydrogens included in calculation of structure factors but not refined.
TABLE 4
Anisotropic Temperature Factor Coefficients
Name
U(1, 1)
U(2, 2)
U(3, 3)
U(1, 2)
U(1, 3)
U(2, 3)
S(1)
0.0396(4)
0.0424(5)
0.0333(4)
−0.0081(3)
0.0048(3)
0.0054(3)
O(6)
0.0505(11)
0.0416(12)
0.0240(10)
−0.0064(9)
0.0105(8)
−0.0006(8)
O(122)
0.0705(15)
0.096(2)
0.0248(11)
−0.0246(14)
−0.0014(10)
−0.0111(12)
N(8)
0.0482(14)
0.0424(15)
0.0313(13)
0.0033(11)
0.0067(10)
0.0017(11)
N(9)
0.0430(12)
0.0308(13)
0.0220(11)
0.0035(10)
0.0067(9)
−0.0032(9)
N(14)
0.0346(11)
0.0299(12)
0.0215(10)
−0.0007(9)
0.0039(8)
−0.0037(9)
N(12A)
0.035(2)
0.035(3)
0.013(2)
0.000(2)
−0.0042(19)
0.0008(19)
N(12B)
0.035(2)
0.036(3)
0.024(3)
0.005(2)
0.0010(19)
0.006(2)
C(2)
0.0354(14)
0.0386(18)
0.0512(19)
−0.0088(12)
0.0014(12)
0.0004(14)
C(3)
0.0359(15)
0.0408(18)
0.0386(16)
−0.0010(12)
−0.0037(11)
−0.0033(13)
C(4)
0.0315(13)
0.0382(17)
0.0288(14)
0.0034(11)
−0.0002(10)
−0.0007(12)
C(5)
0.0295(13)
0.0312(15)
0.0275(13)
0.0042(10)
0.0036(10)
0.0036(11)
C(6)
0.0314(13)
0.0292(14)
0.0233(13)
0.0033(10)
0.0030(9)
0.0025(10)
C(7)
0.0336(13)
0.0252(14)
0.0208(12)
0.0038(10)
0.0043(9)
0.0018(10)
C(10)
0.0452(15)
0.0324(16)
0.0228(13)
−0.0004(12)
0.0061(11)
−0.0033(11)
C(11)
0.0396(14)
0.0300(14)
0.0236(12)
−0.0006(11)
0.0038(10)
−0.0019(11)
C(12)
0.0291(12)
0.0308(14)
0.0208(12)
0.0034(10)
0.0029(9)
0.0023(10)
C(13)
0.0207(10)
0.0169(11)
0.0089(9)
0.0014(8)
0.0030(7)
−0.0004(8)
C(15)
0.0358(13)
0.0282(14)
0.0227(12)
0.0010(10)
0.0031(9)
−0.0011(10)
C(121)
0.0317(13)
0.0290(15)
0.0211(12)
0.0031(10)
0.0034(9)
0.0017(10)
C(122)
0.0331(13)
0.0258(14)
0.0237(12)
0.0014(10)
−0.0005(9)
−0.0012(10)
C(123)
0.0303(13)
0.0273(14)
0.0298(13)
−0.0024(10)
0.0030(10)
0.0004(11)
C(124)
0.0424(15)
0.056(2)
0.0253(14)
−0.0174(13)
0.0041(11)
0.0038(13)
C(125)
0.058(2)
0.106(3)
0.0183(15)
−0.043(2)
−0.0035(13)
0.0069(16)
C(126)
0.0371(15)
0.074(2)
0.0232(14)
−0.0218(14)
−0.0028(11)
0.0084(13)
C(12A)
0.029(3)
0.049(4)
0.019(3)
−0.001(3)
0.002(2)
0.004(3)
C(12B)
0.038(3)
0.047(4)
0.024(3)
−0.001(3)
0.006(3)
−0.001(3)
C(13A)
0.0548(18)
0.0415(18)
0.0357(16)
0.0079(13)
−0.0024(12)
−0.0088(13)
C(13B)
0.0461(16)
0.048(2)
0.0341(15)
0.0134(13)
0.0017(12)
0.0084(13)
The form of the anisotropic temperature factor is: exp[−2π {h 2 a* 2 U(1, 1) + k 2 b* 2 U(2, 2) + l 2 c* 2 U (3, 3) + 2hka*b*U(1, 2) + 2hla*c*U(1, 3) + 2klb*c*U(2, 3)}], where a*, b*, and c* are reciprocal lattice constants.
TABLE 5
Bond Distances
Atom 1
Atom 2
Distance
S(1)
C(2)
1.702(3)
S(1)
C(5)
1.727(3)
O(6)
C(6)
1.235(3)
O(122)
C(12A)
1.263(7)
O(122)
C(12B)
1.357(8)
N(8)
N(9)
1.339(3)
N(8)
C(13)
1.400(3)
N(8)
C(7)
1.406(3)
N(9)
C(10)
1.312(4)
N(14)
C(15)
1.321(3)
N(14)
C(13)
1.377(3)
C(2)
C(3)
1.359(4)
C(3)
C(4)
1.396(4)
C(4)
C(5)
1.372(4)
C(5)
C(6)
1.478(4)
C(6)
C(7)
1.460(3)
C(7)
C(15)
1.413(3)
C(10)
C(11)
1.421(4)
C(11)
C(12)
1.378(4)
C(12)
C(13)
1.375(3)
C(12)
C(121)
1.477(3)
C(121)
C(126)
1.390(4)
C(121)
C(122)
1.394(3)
C(122)
C(123)
1.382(3)
C(123)
C(124)
1.384(4)
C(124)
C(125)
1.383(4)
C(125)
C(126)
1.389(4)
C(125)
N(12B)
1.510(5)
C(125)
N(12A)
1.533(6)
N(12A)
C(12A)
1.355(7)
N(12A)
C(13A)
1.432(6)
C(12A)
C(13B)
1.540(8)
N(12B)
C(12B)
1.343(8)
N(12B)
C(13B)
1.454(5)
C(12B)
C(13A)
1.494(8)
Numbers in parentheses are estimated standard deviations in the least significant digits.
TABLE 6
Bond Angles
Atom 1
Atom 2
Atom 3
Angle
Atom 1
Atom 2
Atom 3
Angle
C(2)
S(1)
C(5)
91.67(14)
C(126)
C(121)
C(122)
118.9(2)
C(12A)
O(122)
C(12B)
42.2(4)
C(126)
C(121)
C(12)
122.0(2)
N(9)
N(8)
C(13)
121.9(2)
C(122)
C(121)
C(12)
119.1(2)
N(9)
N(8)
C(7)
132.9(2)
C(123)
C(122)
C(121)
120.5(2)
C(13)
N(8)
C(7)
105.3(2)
C(122)
C(123)
C(124)
121.0(2)
C(10)
N(9)
N(8)
116.5(2)
C(125)
C(124)
C(123)
118.2(3)
C(15)
N(14)
C(13)
103.91(19)
C(124)
C(125)
C(126)
121.7(3)
C(3)
C(2)
S(1)
112.0(2)
C(124)
C(125)
N(12B)
120.2(3)
C(2)
C(3)
C(4)
112.8(3)
C(126)
C(125)
N(12B)
114.9(3)
C(5)
C(4)
C(3)
113.0(3)
C(124)
C(125)
N(12A)
116.0(3)
C(4)
C(5)
C(6)
133.6(2)
C(126)
C(125)
N(12A)
117.8(3)
C(4)
C(5)
S(1)
110.5(2)
N(12B)
C(125)
N(12A)
40.2(2)
C(6)
C(5)
S(1)
115.89(18)
C(125)
C(126)
C(121)
119.6(3)
O(6)
C(6)
C(7)
121.4(2)
C(12A)
N(12A)
C(13A)
120.9(5)
O(6)
C(6)
C(5)
118.3(2)
C(12A)
N(12A)
C(125)
114.4(5)
C(7)
C(6)
C(5)
120.3(2)
C(13A)
N(12A)
C(125)
124.5(4)
N(8)
C(7)
C(15)
104.4(2)
O(122)
C(12A)
N(12A)
112.7(6)
N(8)
C(7)
C(6)
124.9(2)
O(122)
C(12A)
C(13B)
130.8(5)
C(15)
C(7)
C(6)
130.7(2)
N(12A)
C(12A)
C(13B)
116.4(5)
N(9)
C(10)
C(11)
124.4(2)
C(12B)
N(12B)
C(13B)
120.6(6)
C(12)
C(11)
C(10)
119.7(3)
C(12B)
N(12B)
C(125)
110.2(5)
C(13)
C(12)
C(11)
114.9(2)
C(13B)
N(12B)
C(125)
129.1(4)
C(13)
C(12)
C(121)
121.7(2)
N(12B)
C(12B)
O(122)
110.2(6)
C(11)
C(12)
C(121)
123.4(2)
N(12B)
C(12B)
C(13A)
120.3(6)
C(12)
C(13)
N(14)
125.07(19)
O(122)
C(12B)
C(13A)
129.5(5)
C(12)
C(13)
N(8)
122.6(2)
N(12A)
C(13A)
C(12B)
33.8(3)
N(14)
C(13)
N(8)
112.3(2)
N(12B)
C(13B)
C(12A)
37.9(3)
N(14)
C(15)
C(7)
114.1(2)
Numbers in parentheses are estimated standard deviations in the least significant digits.
In addition, FIG. 3 shows the FT-Raman spectra of polymorph Form III as acquired on a Raman accessory module interfaced to a Magna 860® Fourier transform infrared (FT-IR) spectrophotometer (Thermo Nicolet). This module uses an excitation wavelength of 1064 nm and an indium gallium arsenide (InGaAs) detector. Approximately 0.5 W of Nd:YVO 4 laser power was used to irradiate the sample. The samples were prepared for analysis by placing the material in a glass tube and positioning the tube in a gold-coated tube holder in the accessory. A total of 256 sample scans were collected from 3600-100 cm −1 at a spectral resolution of 4 cm −1 , using Happ-Genzel apodization. Wavelength calibration was performed using sulfur and cyclohexane.
Polymorph Form III may be prepared by crystallization from a crystallization solvent containing Compound 1. As used herein, the term “crystallization solvent” means a solvent or combination of solvents from which Compound 1 is preferentially crystallized as polymorph Form III. Representative crystallization solvents include polar solvents, nonpolar solvents, protic solvents and aprotic solvents, and more specifically include acetic acid, methylene chloride, acetone, methanol, ethanol, propanol, butanol, ethyl acetate, THF, DMF, diethyl ether, acetonitrile, toluene, water, and combinations thereof. In one embodiment, the crystallization solvent comprises acetic acid, to which water is gradually added.
Compound 1 may be introduced into the crystallization solvent in either a solid or liquid form. When added as a solid, Compound 1 may be in the form of a solid powder or any other solid form that aids its dissolution within the crystallization solvent. When added as a liquid, Compound 1 may first be dissolved in a co-solvent to yield a co-solvent solution, which is then combined with the crystallization solvent. The concentration of Compound 1 within the co-solvent solution may range from 0.1% by weight to the saturation point. This concentration will, of course, vary depending upon the temperature at which the co-solvent solution is held, with warmer temperatures generally allowing for the preparation of more concentrated solutions of Compound 1. In general, the co-solvent should aid in the dissolution of Compound 1, but not negatively interfere with the formation of polymorph Form III from the resulting crystallization solvent. Suitable co-solvents include the same solvents as identified above for the crystallization solvent. Further, the co-solvent and the crystallization solvent may be the same or different. For example, both the crystallization solvent and the co-solvent may be acetic acid, or they may be different solvents (or combinations thereof).
In one embodiment, the co-solvent solution containing Compound 1 is added to the crystallization solvent or, alternatively, the crystallization solvent is added to the co-solvent solution. In still another embodiment, the co-solvent solution may be at or above ambient temperature (e.g., heated), while the temperature of the crystallization solvent may be below (e.g., chilled), above (e.g., heated) or at ambient temperature. Alternatively, the co-solvent solution can undergo a solvent exchange and form a solution or heterogeneous mixture of the crystallization solvent and Compound 1. For example, Compound 1 may be dissolved in a first solvent, followed by addition to a second solvent, and then followed by removal of all or part of the first solvent (e.g., by distillation).
Crystallization of polymorph Form III may be achieved by addition of carbon or other nucleating agent to the crystallization solvent containing Compound 1. As used herein, a “nucleating agent” means a substance that aids in the formation of “nuclei” around which a crystal grows. Such nuclei may occur spontaneously in a supersaturated crystalline solvent and then will grow into larger crystals. Formation of the nuclei may also be induced by addition of a seed crystal or by the incidental or purposeful addition of some foreign solid matter such as dust or activated carbon. In a specific example (see Example 1 below), addition of a small amount of activated carbon to a heated solution of Compound 1 in acetic acid (60 mL) and water (70 mL), followed by subsequent cooling steps, yields polymorph Form III. The carbon may be added either before or after the addition of the water to result in formation of polymorph Form III.
Once obtained, crystals of polymorph Form III may be used as the nucleating agent or “seed” crystals for subsequent crystallizations of polymorph Form III from the crystallization solvent. In one embodiment, the crystallization solvent is formed by dissolving Compound 1 in hot acetone or other suitable crystallization solvent. The crystallization solvent is then seeded with crystals of polymorph Form III, cooled and filtered, resulting in polymorph Form III. In another embodiment, a crystallization solvent is formed by slurrying Compound 1 in acetone or other appropriate solvent. The crystallization solvent is then seeded with crystals of polymorph Form III and filtered, resulting in polymorph Form III. Such seeding with crystals of polymorph Form III may take place at any time during the slurrying process. Alternatively, seeding with crystals of polymorph Form III may take place prior to, or simultaneously with, addition of Compound 1 to the crystallization solvent.
Crystals of polymorph Form III may also be used as the nucleating agent or seed crystals in the conversion of a suspension or slurry of Compound 1 to produce polymorph Form III. Depending upon factors such as temperature, solvent and time, the resulting Compound 1 may be predominantly polymorph Form III, or may be polymorphic mixtures of Compound 1.
For purposes of administration to a patient, polymorph Form III may be formulated as a pharmaceutical composition. Such pharmaceutical compositions comprise polymorph Form III and one or more pharmaceutically acceptable carriers, wherein the polymorph is present in the composition in an amount that is effective to treat the condition of interest. Typically, the pharmaceutical compositions of the present invention include polymorph Form III in an amount ranging from 0.1 mg to 250 mg per dosage depending upon the route of administration, and more typically from 1 mg to 60 mg. Appropriate concentrations and dosages can be readily determined by one skilled in the art.
Pharmaceutically acceptable carriers are familiar to those skilled in the art. For compositions formulated as liquid solutions, acceptable carriers include saline and sterile water, and may optionally include antioxidants, buffers, bacteriostats and other common additives. The compositions can also be formulated as pills, capsules, granules, or tablets which contain—in addition to polymorph Form III—diluents, dispersing and surface-active agents, binders, lubricants, and/or delayed releases agents. One skilled in this art may further formulate the polymorph in an appropriate manner, and in accordance with accepted practices, such as those disclosed in Remington's Pharmaceutical Sciences, Gennaro, Ed., Mack Publishing Co., Easton, Pa. 1990 (incorporated herein by reference in its entirety).
In another embodiment, the invention provides a method for treating conditions that benefit from administration of agents that possess anxiolytic, anti-anoxic, sleep-inducing, hypnotic, anticonvulsant, and/or skeletal muscle relaxant properties. Such conditions include insonmia specifically, as well as sleep disorders generally and other neurological and psychiatric complaints, anxiety states, vigilance disorders, such as for combating behavioral disorders attributable to cerebral vascular damage and to the cerebral sclerosis encountered in geriatrics, epileptic vertigo attributable to cranial trauma, and for metabolic encephalopathies.
The methods of this invention include systemic administration of polymorph Form III, preferably in the form of a pharmaceutical composition. As used herein, systemic administration encompasses both oral and parenteral methods of administration. For oral administration, suitable pharmaceutical compositions include powders, granules, pills, tablets and capsules, as well as liquids, syrups, suspensions and emulsions. These compositions may also include flavorants, preservatives, suspending, thickening and emulsifying agents, and other pharmaceutically acceptable additives. For parental administration, the compounds of the present invention can be prepared in aqueous injection solutions that may contain buffers, antioxidants, bacteriostats and/or other additives commonly employed in such solutions.
The following examples are offered by way of illustration, not limitation.
EXAMPLE 1
Representative Synthesis of Polymorph Form III
Compound 1 (10 g) made according to the procedures of U.S. Pat. No. 6,399,621 (incorporated herein by reference) was dissolved in 60 mL of acetic acid. The solution was then filtered and heated to 70-75° C. Water (70 mL) and carbon (Darco G-60, 5 mg) were added to the heated solution, and the resulting solution was then cooled 5° C. every 30 minutes. At 55° C., crystallization began and the temperature was held steady for 30 minutes. The mixture was then cooled to 45-50° C. and 40 mL of water was added. The mixture was further cooled to 25° C. over a 1 hour period and the resulting solid was filtered and washed with 40 mL of water and dried to yield 9 g of polymorph Form III as a yellow solid (see FIGS. 1 and 2 for characterization of Polymorph Form III by DSC and X-ray powder diffraction).
EXAMPLE 2
Representative Synthesis of Polymorph Form III
Compound 1 (10 g) made according to the procedure of U.S. Pat. No. 6,399,621 was dissolved in 60 mL of acetic acid. The solution was then filtered and heated to 70-75° C. Water (70 mL) was added to the heated solution. After cooling to 67° C., polymorph Form III seed crystals (as obtained by the procedure described in Example 1 above) were added and the mixture was cooled to 50° C. over 2 hours. 40 mL of water was added and the mixture was cooled to room temperature. The resulting solid was filtered and washed with 40 mL of water to yield 9 g of polymorph Form III as a yellow solid (DSC endotherm peak at 191.86° C.).
EXAMPLE 3
Representative Synthesis of Polymorph Form III
Compound 1 (10 g) was prepared according to the procedure of U.S. Pat. No. 6,399,621 and dissolved in 60 mL of acetic acid. The solution was then filtered and heated to 70-75° C. Water (70 mL) was added to the heated solution. After cooling to 52° C., polymorph Form III seed crystals (as obtained by the procedure described in Example 1) were added and the mixture was stirred for 30 minutes. The mixture was then cooled to 47° C. over 30 minutes followed by addition of 40 mL of water. Following cooling to room temperature, the resulting solid was filtered and washed with 40 mL of water to yield 9 g of polymorph Form III as a yellow solid (DSC endotherm peak at 191.68° C.).
EXAMPLE 4
Interconversion of Compound 1
Interconversion experiments were carried out to evaluate the thermodynamic stability of Compound 1 at room temperature. Three slurries were prepared by making saturated isopropanol solutions of Compound 1, filtering the solutions through 0.2 μm filters, and then adding an amount (in the form of crystals) of a polymorphic form of Compound 1. To the first slurry, equal amounts of both polymorph Form II and polymorph Form III (i.e., approximately 25 mg each) were added; to the second slurry, equal amounts of polymorph From I and polymorph Form III (i.e., approximately 25 mg each) were added; and to the third slurry, approximately 25 mg of polymorph Form III was added. The slurries were then agitated for 16 days. The resulting solids were collected by vacuum filtration, air-dried, and analyzed using XRPD. By the above technique, the first slurry seeded with polymorph Forms II and III yielded exclusively polymorph Form III. On the other hand, the second slurry seeded with polymorph Forms I and III yielded polymorph Form III as the predominant product, with only a minor amount of polymorph Form I. The third slurry seeded with polymorph Form III alone yielded exclusively polymorph Form III. These results indicate that Compound 1, when in a slurry form, will convert to polymorph Form III when seeded with crystals of the same, and under such conditions is the favored polymorph.
The above is a detailed description of particular embodiments of the invention. It will be appreciated that, although specific embodiments of the invention have been described herein for purposes of illustration, various modifications may be made without departing from the spirit and scope of the invention. Accordingly, the invention is not limited except as by the appended claims.
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Polymorph Form III of N-methyl-N-(3-{3-[2-thienylcarbonyl]-pyrazol-[1,5-α]-pyrimidin-7-yl}phenyl)acetamide, and use thereof as a sedative-hypnotic, anxiolytic, anticonvulsant, and/or skeletal muscle relaxant agent. Related compositions and methods are also disclosed, particularly with regard to treatment of insomnia.
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FIELD OF THE INVENTION
[0001] The present invention relates to elevator group control methods and control devices, and aims, in particular, to provide a group control method and a group control device capable of efficiently control the operation of the elevators in diversified traffic situations and under a variety of specific conditions required for a group management system.
BACKGROUND OF THE INVENTION
[0002] In general, the objective of operation control of conventional group management systems is to reduce the average waiting time of passengers in elevators by efficiently controlling the operation of a plurality of elevators within a building.
[0003] Therefore, what the group management system must truly evaluate in its control operation is that the waiting time of passengers, including prospective passengers, and the significance of waiting time of individual passengers should be basically considered to be equivalent. However, a group management system has difficulty in directly figuring out the waiting time of individual passengers. Accordingly, the control operation is conventionally performed by evaluating the waiting time of a hall call as an alternative, that is, evaluating a time period as waiting time from a hall call is registered until an elevator arrives in response to the call.
[0004] Further, when evaluating, a focus of the evaluation is placed on the waiting time of a newly registered hall call as a target of assignment, and the waiting time of individual hall calls is not treated equivalently. In addition, as an assignment of a hall call affects, not only a call that has already been made but also a hall call that is possibly made in the near future, it is essential that the evaluation includes any hall call that may be made in the future. However, even if a hall call that is possibly made in the future is evaluated, an evaluation value for the call is usually treated only as a correction term (e.g., Patent Publication 1).
[0005] On the other hand, the conventional group management system is typically based on an “immediate assignment method” which determines a car to respond instantly upon registration of a hall call, and an “immediate prediction method” of which announces an assigned car instantly at an elevator hall. In a group management system employing the “immediate prediction method”, as any change in an assignment of a hall call that has been made may cause confusion among passengers waiting for an elevator, it is desirable not to change the assignment if circumstances allow. Accordingly, the assignment change is limited to a case satisfying specific conditions, such as changing an assignment of a potentially long waiting hall call to a different car (e.g., Patent Publication 2).
[0006] Further, the conventional group management system is provided with controlling means for moving a car to a random floor by assigning a pseudo call (virtual call) to the car. However, such means are used only under limited traffic situations such as distributed waiting during down peak and reference floor recalling when people arrive before working hours (e.g., Patent Publication 3).
[0007] Moreover, development of the conventional group management systems has been promoted in the policy of reducing waiting time of the hall call as much as possible with the application of artificial intelligence technologies such as “fuzzy” and “neuro” (e.g., Patent Publication 4).
CITATION LIST
Patent Publication
[0000]
Patent Publication 1: Japanese Examined Patent Publication No. H06-62259
Patent Publication 2: Japanese Unexamined Patent Publication No. 2006-124075
Patent Publication 3: Japanese Examined Patent Publication No. H06-2553
Patent Publication 4: Japanese Unexamined Patent Publication No. H08-225256
SUMMARY OF THE INVENTION
Problems to be Solved by the Invention
[0012] As described above, what a group management system must truly evaluate in its control operation is the waiting time of passengers including prospective passengers. However, when the control operation is performed by evaluating the waiting time of a hall call as an alternative as described in Patent Publication 1, only the waiting time of a person who first registers a hall call is evaluated when a plurality of waiting passengers are present on one floor, and it is not possible to appropriately evaluate the waiting time of a plurality of passengers waiting after this hall call. In addition, unless considering all, not just a part, of the hall calls (waiting passengers) that are possibly made in the future, the waiting time of passengers as a result of control operation of a group management system cannot be appropriately evaluated. Consequently, in a traffic situation in which waiting passengers are concentrated on a plurality of unspecified floors, it is a difficult challenge to reduce long waiting periods by adequately evaluating the waiting time and controlling the operation of elevators. For example, if it is presumed that passengers are concentrated only on a specific floor such as in the case when people arrive before working hours in an office building, it is relatively easy to prepare a control method suitable for such a traffic situation. However, it is difficult to flexibly control the operation of elevators by appropriately evaluating waiting time in complicated and diversified traffic situations such as a case where the traffic is concentrated on a plurality of unspecified floors.
[0013] Further, according to Patent Publication 2, an assignment is changed only when a specific event such as a long waiting occurs. However, the “immediate prediction method” on which a typical group management system is based may not be necessary in the first place depending on the country or region the system is employed or on the clients' view. In addition, immediate prediction is often not applicable in the case in which a number of elevators in a group management system is small. In such a case, while an assignment of a hall call can normally be changed freely as long as the waiting time of passengers can be reduced if only a little, as different evaluative criteria are used in an assignment of a hall call and an assignment change of a hall call, an assignment change of a hall call is not exactly used to the best effect in the reduction of waiting time of passengers.
[0014] Similarly, while Patent Publication 3 is provided with the controlling means for assigning a pseudo call (virtual call) to an empty car (car stopping without a traveling direction) and moving the car to any floor, such means are still used only under limited traffic situations such as distributed waiting during down peak and reference floor recalling when people arrive before working hours. Accordingly, although there is the possibility that waiting time can be reduced by assigning a pseudo call in any traffic situation, as different evaluative criteria are used in an assignment of a hall call and an assignment of a pseudo call, an assignment of pseudo call is not exactly used to the full extent in the reduction of waiting time at an elevator hall.
[0015] Moreover, an acceptable degree of repetition of an assignment change and an assignment of a pseudo call varies depending on the group management specification, the elevator specification, the user interface of an elevator hall, the use of the building, clients' needs, or traffic situation, and it is difficult to perform group control to reduce waiting time of passengers while conducting an assignment change or an assignment of a pseudo call at an adequate degree of repetition according to various requirements and specific conditions.
[0016] Furthermore, when it is intended to reduce the waiting time of a hall call as much as possible with applying artificial intelligence technologies as described in Patent Publication 4, while a highly advanced control can provide some effects, this also increases complexity and size of the system, making the system a black box. Therefore, it is difficult to respond to tasks such as adding a new control function within a limited development period, in addition to the problems as described above, and it is extremely difficult to analyze, explain, and adjust a problem in the control even if it is pointed out.
Means of Solving the Problems
[0017] The present invention has been made in order to address the various problems described above, and to provide an elevator group control method, including: placing a plurality of elevators in service for a plurality of floors; calculating an evaluation index for a newly made hall call; and selecting and assigning the best suited car to the hall call based on the evaluation index, wherein a waiting time expectation value of all passengers on all floors for each direction either that have already occurred or that is expected to occur within a predetermined time period is taken as the evaluation index, the waiting time expectation value being the expected value the sum or the average of the waiting time.
[0018] Further, according to the present invention, other than the assignment of the new hall call is performed using the waiting time expectation value as the evaluation index, an assignment change of a hall call or a pseudo call assignment to an empty car is performed based on the same evaluation index every predetermined time period or at the same time with the assignment of the new hall call.
[0019] Moreover, according to the present invention, the waiting time expectation value is calculated by using an estimated value of the passenger arrival rate on each floor and for each direction, an estimated value of hall call occurrence rate for an entire group, and an estimated time of arrival for each car, for each floor and in each direction.
Effects of Invention
[0020] According to the present invention, employing a method of stochastically evaluating the waiting time of passengers, instead of the waiting time of a hall call as in a conventional example, allows appropriate evaluation of a bias of the passenger arrival rate on each floor and the waiting time of prospective passengers, and it is possible to reduce the waiting time of passengers as originally desired in complicated and diversified traffic situations.
[0021] Further, according to the present invention, as the evaluation of the waiting time of a hall call is not necessary, it is possible to evaluate a situation as needed even when there is no new hall call. Therefore, the same evaluation index (waiting time expectation value of the all passengers) can be applied in a versatile manner for controlling means other than means for assigning a hall call, that is, an assignment change of a hall call or an assignment of a pseudo call to an empty car that is stopping without a traveling direction, and thus it is possible to facilitate optimization of the control as a whole.
[0022] Moreover, according to the present invention, when the group management system does not employ the immediate prediction, by constantly and effectively utilizing an assignment change of a hall call without restricting to a limited traffic situation, it is possible to reduce the waiting time of passengers.
[0023] Furthermore, according to the present invention, by constantly and effectively utilizing a pseudo call assignment without restricting to a limited traffic situation, that is, by moving an empty car that is stopping without any traveling direction to an appropriate position as needed, it is possible to reduce the waiting time of passengers.
[0024] Further, according to the present invention, a degree of repetition of an assignment change or a pseudo call assignment can be adjusted according to diverse needs and specific conditions that vary depending on individual buildings, and it is possible to reduce the waiting time of passengers under adjusted conditions.
[0025] Moreover, according to the present invention, a group control method based on a unified evaluation index of the waiting time of passengers can be realized, and consequently it is possible to simplify the control structure as compared to the group control to which conventional artificial intelligence is applied. Therefore, it is possible to facilitate addition of a new control function, and to easily analyze, explain, and adjust a problem in the control when it is pointed out.
BRIEF DESCRIPTION OF DRAWINGS
[0026] FIG. 1 is a diagram showing an entire configuration of a group management system of elevators according to a first embodiment of the present invention.
[0027] FIG. 2 is a diagram showing a relation between the position of a car and a call for explaining the estimated arrival time of the car.
[0028] FIG. 3 is a table illustrating one example of a table for estimated time of arrival according to the present invention.
[0029] FIG. 4 is a main flowchart showing an entire procedure according to the first embodiment of the present invention.
[0030] FIG. 5 is a chart showing a variation in the estimated time of arrival of each car at one station position.
[0031] FIG. 6 is a chart showing a part of FIG. 5 by dividing the shaded region.
[0032] FIG. 7 is a flowchart explaining a specific procedure of the new hall call assignment process in Step S 2 in FIG. 4 .
[0033] FIG. 8 is a flowchart explaining specific steps of the waiting time expectation value calculation process for all passengers at all station positions in Step S 24 in FIG. 7 .
[0034] FIG. 9 is apart of a flowchart explaining specific steps of the waiting time expectation value calculation process for all passengers at a station position “s” in Step S 204 in FIG. 8 .
[0035] FIG. 10 is a part of the flowchart explaining specific steps of the waiting time expectation value calculation process for all passengers at a station positions in Step S 204 in FIG. 8 .
[0036] FIG. 11 is a part of a flowchart explaining specific steps of the hall call assignment change process in Step S 4 in FIG. 4 .
[0037] FIG. 12 is a part of the flowchart explaining specific steps of the hall call assignment change process in Step S 4 in FIG. 4 .
[0038] FIG. 13 is a part of the flowchart explaining specific steps of the hall call assignment change process in Step S 4 in FIG. 4 .
[0039] FIG. 14 is a part of a flowchart explaining specific steps of the pseudo call assignment process in Step S 5 in FIG. 4 .
[0040] FIG. 15 is a part of the flowchart explaining specific steps of the pseudo call assignment process in Step S 5 in FIG. 4 .
[0041] FIG. 16 is a part of the flowchart explaining specific steps of the pseudo call assignment process in Step S 5 in FIG. 4 .
[0042] FIG. 17 is a part of a flowchart showing steps of a process of assigning a new hall call and changing the assignment according to a second embodiment of the present invention.
[0043] FIG. 18 is a part of the flowchart showing steps of the process of assigning a new hall call and changing the assignment according to the second embodiment of the present invention.
[0044] FIG. 19 is a part of the flowchart showing steps of the process of assigning a new hall call and changing the assignment according to the second embodiment of the present invention.
DETAILED DESCRIPTION OF PREFERRED EMBODIMENTS
First Embodiment
[0045] In general, the car position in a group control cannot be judged only by a floor level, the traveling direction of the car should be included in the judgment. Therefore, in the description hereinafter, the term “station position” is used as a concept for expressing the stop position of a car including both floor and direction to simplify explanation.
[0046] Now, one embodiment of the present invention will be described with reference to FIG. 1 through FIG. 16 .
[0047] FIG. 1 is a diagram showing an entire configuration of a group management system of elevators according to a first embodiment of the present invention. Here, the description is given taking an example in which three elevator cars including a first car to a third car are controlled as a group. However, it should be appreciated that the number of the elevators is not limited to three.
[0048] Referring to FIG. 1 , reference number 11 represents an elevator control device configured to perform elevator control operation of the first car, reference numbers 12 and 13 similarly represent elevator control devices configured to perform elevator control operation respectively of the second car and the third car, a reference number 20 represents a hall call registration device that is common to all elevators and configured to register a hall call, and a reference number 30 represents a group control device configured to control the operation of the elevators as a group while communicating with the elevator control devices 11 - 13 .
[0049] Reference number 31 represents passenger arrival rate estimating means configured to estimate a passenger arrival rate at a station position. The passenger arrival rate estimating means estimates the passenger arrival rate using a conventional method such as, for example, stochastic estimation of the passenger arrival rate based on learned data relating to a time period during which no hall call is made by presuming the arrival of a passenger who uses an elevator to be Poisson arrival. It is also possible to correct the passenger arrival rate according to variations in a number of car calls and a live load of a car.
[0050] Reference number 32 represents hall call occurrence rate estimating means configured to estimate the rate of occurrence of hall calls in an entire group. This also can be easily obtained using a conventional method such as division of the number of hall calls occurring per a predetermined time, this time period is based on a short-term learning or a long-term learning by the predetermined time.
[0051] Reference number 33 represents car arrival time estimating means configured to estimate time at which each car can arrive at each station position, and it is possible to use various methods of conventional hall call waiting time estimation as the method to estimate the time of arrival. However, while estimation of waiting time for a single entire loop of car is sufficient in the conventional hall call waiting time estimation, as the present invention is also required to estimate waiting time of prospective passengers, it is necessary to estimate waiting time for a single entire loop and a half considering a farthest car call that is set off from an assigned hall call on a back side as shown in FIG. 2 , and to estimate for two entire loops and a half at maximum, considering the necessity of estimating waiting time of passengers that may occur after responding to all the calls that can be assumed.
[0052] One example of a table for estimated time of arrival produced by the car arrival time estimating means is shown in FIG. 3 . Here, while calculation is made by assuming that time required for a car to travel a single floor is 2 seconds and that the time required for a car to make a single stop is 10 seconds to simplify an explanation, traveling time and such are calculated based on learned data of group management in practice.
[0053] Referring back to FIG. 1 , a reference number 34 represents waiting time expectation value calculating means configured to stochastically calculate, as a general evaluation index, an expectation value of a sum or an average of the waiting time of all the passengers (including passengers that have already appeared) estimated to appear at all of the station positions within predetermined time (hereinafter, the expectation value of the sum or the average of waiting time is simply referred to as a waiting time expectation value). A concept and a method of calculation of the waiting time expectation value of all passengers will be described later.
[0054] A reference number 35 represents hall call assigning means configured to evaluate a newly registered hall call taking the waiting time expectation value as an evaluation index, or holistically in conjunction with other evaluation indices, and to assign the call to the best suited car. The hall call assigning means performs an assignment process every time a new hall call is made.
[0055] A reference number 36 represents hall call assignment changing means configured to change an assignment of a hall call that has been assigned based on the waiting time expectation value. The hall call assignment changing means calculates, every predetermined time, the waiting time expectation value assuming that the assignment is changed, compares the calculated waiting time expectation value with the waiting time expectation value before the assignment change is made, and performs the assignment change of the hall call if a difference between the two values satisfies a predetermined condition.
[0056] A reference number 37 represents pseudo call assigning means configured to assign a pseudo call to an empty car based on the waiting time expectation value. The pseudo call assigning means calculates, every predetermined time, the waiting time expectation value assuming that a pseudo call is assigned, compares the calculated waiting time expectation value with the waiting time expectation value before the assignment of a pseudo call is made, and assigns a pseudo call to the empty car if a difference between the two values satisfies a predetermined condition.
[0057] A reference number 38 represents learning means configured to perform statistical processing of data received from the elevator control devices 11 - 13 and the hall call registration device 20 and accumulates the data. The learning means is configured by, similarly to those used in conventional group control, such as short-term learning means for learning about current traffic situation, and long-term learning means for learning about traffic situation in each time period on weekday, weekend, or the same day.
[0058] A reference number 39 represents communicating means configured to communicate with each of the elevator control devices 11 - 13 .
[0059] Next, a procedure of an elevator group control method according to the present invention of the above configuration is described with reference to flowcharts in FIG. 4 through FIG. 16 .
[0060] FIG. 4 is the main flowchart of the entire procedure, showing that the assignment process is performed every time when a new hall call is made, and a hall call assignment change process and a pseudo call process are performed every predetermined time. This procedure is constantly and repeatedly performed.
[0061] First, in Step S 1 , it is determined whether or not a new hall call is present, and if present, awaiting time expectation value of all passengers at all station positions is calculated in Step S 2 , and the hall call is assigned to the best suited car based on a result of the calculation. Further, separately from the assignment of the new hall call, every time a predetermined time passes (Step S 3 ), the current waiting time expectation value of all the passengers and the waiting time expectation value assuming that an assignment change is performed, are compared in Step S 4 , and the assignment change is performed if a difference between the two values satisfies a predetermined condition. Similarly, the current waiting time expectation value and the waiting time expectation value assuming that a pseudo call is assigned to an empty car are compared in Step S 5 , and the assignment process of a pseudo call is performed if a difference between the two values satisfies a predetermined condition. Details of these processes will be described later. As described above, according to the first embodiment, the waiting time expectation value of all the passengers is calculated when a new hall call is made and every predetermined time, the assignment change of a hall call and the assignment of a pseudo call to an empty car, in addition to the assignment of a new hall call are performed based on the same evaluation index every predetermined time so that the value is as small as possible, that is, so that the waiting time of all the passengers is reduced.
[0062] Here, before describing the details of the processes, an idea of the waiting time expectation value of all the passengers at all of the station positions as a general evaluation index and how to calculate this value according to the present invention are described.
[0063] First, when evaluating the waiting time of all the passengers, how to evaluate arrival time of an empty car (car stopping without a traveling direction) must be considered. Unless the arrival time of an empty car can be appropriately evaluated, it is not possible to obtain a general evaluation index that can be applied to every traffic situation. In particular, as the pseudo call assignment control is in principle performed for an empty car, it is important to appropriately evaluate the arrival time of an empty car.
[0064] However, there are many uncertain elements regarding a time point and a direction at and in which an empty car starts traveling, and it is not possible to estimate the arrival time of an empty car to each station position in the same manner as a traveling car. For example, when a hall call is made at one station position in the future, the empty car may have responded to a different hall call and may not be present at an original position. Therefore, based on a hall call occurrence rate and the number of cars in an entire group, a probability P(t) that an empty car is present at an original position in a standby state is expressed as an exponential function of time t in equation 1 listed below, and it is assumed that the empty car can arrive at any station position in response to a call from this station position if the car is in the standby state, and that the empty car is removed from evaluation targets when the car is not in standby state.
[0000] P ( t )=exp(−α t ) [Equation 1]
α: A hall call occurrence rate per car
[0066] In this manner, by expressing the standby probability of an empty car in an exponential function, and using this in the calculation of the waiting time expectation value, as will be described later, it is possible to stochastically evaluate an influence of the presence of an empty car to the waiting time of prospective passengers although in a simplified manner.
[0067] Next, the calculation of “the waiting time expectation value of all the passengers expected to occur within predetermined time T” at one station position is described by schematizing as shown in FIG. 5 .
[0068] FIG. 5 is a graphic chart showing variation in estimated time of arrival of each car at one station position, in which a horizontal axis represents time and a vertical axis represents the estimated time of arrival. Here, the chart shows that the first car is always traveling within the time T, and passes once by a station position as a target. The chart also shows that the second car currently stops as an empty car, and that the third car is currently traveling but stops at time t 4 and becomes an empty car.
[0069] In FIG. 5 , the waiting time expectation value of all the passengers is obtained by the integration of the shaded area and multiplication of a passenger arrival rate λ. However, when there is an empty car present closer than a traveling car, the expectation value of the waiting time is calculated assuming that this empty car responds at the probability P(t) expressed by the equation 1.
[0070] Regions in the shaded area are divided by time that satisfies conditions as listed below.
[0000] (a) Time at which estimated time of arrival of the traveling car becomes equal to estimated time of arrival of the empty car.
(b) Time at which the traveling car becomes an empty car in a stopped state.
(c) Time at which the traveling car arrives at the target station position.
[0071] As the region divided in this manner shows a simple shape as shown in FIG. 6 , it is possible to perform integral calculation easily, and to obtain the waiting time expectation value of all the passengers that occur in a time period represented by the divided region.
[0072] For example, the waiting time expectation value of all the passengers in a region E 5 shown in FIG. 5 can be obtained by equation 2 listed below.
[0000] E =∫ λ ( w 1 P ( t )+ w 2 P ( t )(1 −P ( t ))+( w 0 −( t−t 4 ))(1 −P ( t )) 2 ) dt [Equation 2]
[0073] λ s : A passenger arrival rate at the station position s
[0074] Similarly, where a number of empty cars that can influence the waiting time of passengers at a station position as a general target is m, a waiting time expectation value E Z of all the passengers in time periods t a −t b can be obtained by equation 3 listed below.
[0000]
E
z
=
∫
t
a
t
b
λ
(
∑
k
=
1
m
(
w
k
P
(
t
)
(
1
-
P
(
t
)
)
k
-
1
)
+
(
w
0
-
(
t
-
t
a
)
)
(
1
-
P
(
t
)
)
m
)
t
[
Equation
3
]
[0075] w 0 : Estimated time of arrival at time t a of a car that arrives at a target station position in the shortest time out of all traveling cars
[0076] w 1 , w 2 , . . . : Estimated time of arrival of cars whose estimated time of arrival at target station position is shorter than w 0 out of empty cars, where w 1 , w 2 , . . . are in ascending order of estimated time of arrival.
[0077] In this manner, by summing up the waiting time expectation values of the passengers obtained for the respective regions, a waiting time expectation value Es of all the passengers that appear at a station position s within a predetermined time T is obtained by equation 4 listed below.
[0000]
E
s
=
∑
k
=
1
n
E
z
[
Equation
4
]
[0078] n: A number of divided regions
[0079] It should be noted that there must be a single passenger at hall call registration if a hall call has already been made at this station position, and it is possible to ignore the presence of an empty car until a car assigned to this hall call arrives. Therefore, the waiting time expectation value of the passengers in this case can be obtained by equation 5 listed below.
[0000]
E
z
=
h
c
w
t
+
λ
·
h
c
w
t
2
2
[
Equation
5
]
[0080] Then, the waiting time expectation value ET of all the passengers that have appeared or may appear within the predetermined time T at all the station positions can be finally obtained by equation 6 listed below.
[0000]
E
T
=
∑
s
∈
S
E
s
[
Equation
6
]
[0081] S: A class representing all station positions
[0082] E T is “the waiting time expectation value of all the passengers at all the station positions” used as a general evaluation index in the group control method according to the present invention.
[0083] Based on what has been described above, the steps for calculating the waiting time expectation value of all the passengers at all the station positions, and the procedure for assigning a new hall call based on the result of the calculation are described with reference to flowcharts in FIG. 7 through FIG. 10 .
[0084] FIG. 7 is a flowchart explaining a specific procedure in Step S 2 in FIG. 4 , showing the steps for calculating the waiting time expectation value of all the passengers at all the station positions assuming that a new hall call is tentatively assigned to each car, and assigning the new hall call to a car whose waiting time expectation value is the smallest.
[0085] First, in Step S 21 , the initial value of a variable eval representing the waiting time expectation value is set to be the maximum value, and based on Step S 22 and Step S 27 , the process between these steps is repeated for all of the cars.
[0086] In Step S 23 , a table for estimated time of arrival for a case in which a new hall call HC is tentatively assigned to an “i” car is generated for each car as shown in FIG. 3 . Then, in Step S 24 , the waiting time expectation value of all the passengers at all the station positions, assuming that the hall call is tentatively assigned to the “i” car, is calculated based on the generated table for estimated time of arrival (detailed steps will be described later), and stored as variable e.
[0087] In Step S 25 , the variable e is compared with the variable eval. If e<eval, a waiting time expectation value e at this time is substituted for the variable eval, and a car number “i” is substituted for “car” in Step S 26 . Similarly, Step S 23 through Step S 26 are repeated for all of the cars, and the smallest value out of the waiting time expectation values of all the passengers at all the station positions assuming that the new hall call is tentatively assigned to the respective cars is stored as eval, and the car that is tentatively assigned at this time is stored as “car”. Then, in Step S 28 , the new hall call HC is actually assigned to the “car” car whose waiting time expectation value is the smallest.
[0088] Next, a specific procedure in Step S 24 for calculating the waiting time expectation value of all the passengers at all the station positions, assuming that the new hall call is tentatively assigned to one car, is shown in the flowchart in FIG. 8 .
[0089] First, in Step S 201 , the initial value of the variable E T representing the waiting time expectation value of all the passengers at all of the station positions is set to be 0. In Step S 202 , the hall call occurrence rate shown by equation 1 is obtained as α, and based on Step S 203 and Step S 206 , the process between these steps is repeated for all station positions. Specifically, in Step S 204 , the waiting time expectation value of all the passengers at the station position is calculated as E S , and in Step S 206 , the value obtained by adding E S to E T is newly stored as E T by updating. In this manner, Step S 204 and Step S 205 are repeated for all of the station positions, and the waiting time expectation value of all the passengers at all the station positions, assuming that the new hall call is tentatively assigned to one car, is obtained as E T . Then, in Step S 207 , the value of E T is returned to Step S 24 in FIG. 7 and substituted for e.
[0090] Next, a specific procedure in Step S 204 for calculating the waiting time expectation value of all the passengers at one station position s is shown in flowcharts in FIG. 9 and FIG. 10 . The procedure is divided into two flows at a connecting sign G for convenience sake.
[0091] First, in Step S 251 , a passenger arrival rate at the station position s is obtained as λ, and in Step S 252 , the predetermined time T (e.g., about 60 seconds) is divided into a plurality of time periods that can be subjected to the integral calculation of the waiting time expectation value, as described with reference to FIG. 5 . In Step S 253 , a number of the divided time periods is taken as n, and in Step S 254 , the initial value of E S is set to be 0 and the initial value of t a is set to be the current time.
[0092] Then, based on Step S 255 and Step S 269 , the process between these steps is repeated for all of the time periods. Specifically, in Step S 256 , the end time of a time period z is set to be t b , and in Step S 257 , it is determined whether or not the time period z is a leading time period. If the time period z is the leading time period, then, in Step S 258 , it is determined whether or not there is a hall call at station position s. If there is no hall call at station position s, only the passengers that possibly appear within the predetermined time are considered, and the waiting time expectation value is calculated based on equation 3. Then, the process proceeds to Step S 259 .
[0093] In Step S 259 , the estimated time of arrival of a car that can arrive at the station position s in the shortest time out of all cars with a traveling direction during the time period z is substituted for w 0 . In Step S 260 , arrival time of all cars whose estimated time of arrival at the station position s is shorter than w 0 out of cars without any traveling direction during the time period z is substituted for w 1 -w m in ascending order, and the number of the cars is substituted for m. Then, in Step S 261 , based on equation 3, the waiting time expectation value E Z during time period z is calculated.
[0094] On the other hand, if the time period z is the leading time period in Step S 257 , and if there is a hall call at the station position s in Step S 258 , the passengers that have already appeared are considered, and the waiting time expectation value is calculated based on equation 5. Then, the process proceeds to Step S 262 .
[0095] In Step S 262 , a car to which the hall call at the station position s is assigned is taken as “acar”. Then, hall call occurrence time at the station position s is taken as t a in Step S 263 , estimated time of arrival of the “acar” carat the station position s is taken as t b in Step S 264 , estimated time of arrival hcwt is obtained based on the difference between t a and t b in Step S 265 , and the waiting time expectation value E Z is calculated during time period z based on equation 5 in Step S 266 .
[0096] Then, in Step S 267 , the value obtained by adding E Z obtained in Step S 261 or Step S 266 to the original value of E S is newly taken as E S , and in Step S 268 , t b is newly stored as t a by updating. In this manner, the steps from Step S 256 to Step S 268 are repeated for all of the time periods, and the waiting time expectation value E S of all the passengers at the station position s is obtained. Then, in Step S 270 , the value of E S is returned to Step S 204 in FIG. 8 , and newly stored as E S by updating.
[0097] The above described is the new hall call assignment process taking the waiting time expectation value of all the passengers at all the station positions as the evaluation index.
[0098] Next, the hall call assignment change process that is performed every predetermined time is described similarly by taking the waiting time expectation value of all the passengers at all the station positions as the evaluation index.
[0099] FIG. 11 through FIG. 13 are flowcharts explaining specific steps of the hall call assignment change process in Step S 4 in FIG. 4 . The process shown is divided into three flows at connecting signs C and D for convenience sake. In this process, the waiting time expectation value of all the passengers at all of the station positions, assuming that an assignment of a hall call that has been performed to one car, is changed to a different car is calculated, the calculated waiting time expectation value is compared with the waiting time expectation value before the assignment change, and the assignment change is performed if a difference between the two values satisfies a predetermined condition.
[0100] First, in Step S 401 , the current table for estimated time of arrival is generated for each car, and the generated tables are stored as Tab. In Step S 402 , the current waiting time expectation value of all the passengers at all the station positions is calculated based on the tables for estimated time of arrival, and stored as eval 0 . The calculation steps of the waiting time expectation value of all the passengers in Step S 402 is the same as the process in Step S 24 in FIG. 7 as described above, and therefore an explanation is omitted. In Step S 403 , the initial value of the variable eval representing the waiting time expectation value when the assignment change is performed is set to be the maximum value.
[0101] Then, based on Step S 404 and Step S 415 , the process between these steps is repeated for all of the station positions. Specifically, in Step S 405 , it is determined whether or not there is an assigned hall call at the station position s. If there is an assigned hall call, the assigned car is taken as “acar” in Step S 406 .
[0102] Further, based on Step S 407 and Step S 414 , the process between these steps is repeated for all of the cars from the first car. In Step S 408 , it is determined whether or not the “i” car is the “acar” car. If the “i” car is not the “acar” car, that is, not the car assigned for the station position s, it is determined whether or not the “i” car can service the station position s in Step S 409 . Then, if the “i” car can service, in Step S 410 , a table for the estimated time of arrival, assuming that the assigned car for the station position s is tentatively changed to the “i” car, is generated as shown in FIG. 3 , and in Step S 411 , the waiting time expectation value of all the passengers is calculated based on the generated table for estimated time of arrival, and stored as variable e. The calculation steps of the waiting time expectation value of all the passengers in Step S 411 is performed in the same manner as the process in Step S 24 in FIG. 7 as described above, and therefore an explanation is omitted.
[0103] Then, in Step S 412 , the value of e and the value of eval are compared, and if e is smaller, e is newly stored as eval by updating, and the car number “i” of the assigned car at this time is stored as “car”. Subsequently, the same process is repeated for all of the cars in Step S 414 , and then for all the station positions in Step S 415 , and the minimum value out of the waiting time expectation values, assuming that the assignment change is performed, is stored as eval, and the car to which the assignment is changed to this time is stored as “car”.
[0104] Then, in Step S 416 , it is determined whether or not a difference between the current waiting time expectation value eval 0 (before the tentative assignment change) and the minimum value eval after the tentative assignment change is greater than the set value ReasParam 1 . Further, in Step S 417 , it is determined whether or not the reduction rate of the waiting time expectation value (a value obtained by dividing the difference between the current waiting time expectation value eval 0 and the minimum value eval after the tentative assignment change by eval 0 and then multiplying by 100%) is no smaller than the set value ReasParam 2 . If the reduction rate is no smaller than the set value, in Step S 418 , the assignment of the hall call at the station position s is changed to the “car” car, and the hall call assignment change process is terminated. Specifically, in this example, in order to prevent unnecessary confusion due to the assignment change, the assignment change is performed only when the waiting time expectation value of all the passengers at all the station positions decreases by an amount of the set value or more and when the reduction rate is no smaller than the set value.
[0105] Next, a pseudo call assignment process that is performed every predetermined time is described similarly by taking the waiting time expectation value of all the passengers at all the station positions as the evaluation index.
[0106] FIG. 14 through FIG. 16 are flowcharts explaining specific steps of the pseudo call assignment process in Step S 5 in FIG. 4 . The process shown is divided into three flows at connecting signs E and F for convenience sake. In this process, the waiting time expectation value of all the passengers at all of the station positions assuming that a pseudo call at one station position is tentatively assigned to an empty car is calculated, the calculated waiting time expectation value is compared with the waiting time expectation value before the tentative assignment, and the pseudo call assignment is performed if a difference between the two values satisfies a predetermined condition.
[0107] First, in Step S 501 , the current table for estimated time of arrival is generated for each car, and the generated tables are stored as Tab. In Step S 502 , the current waiting time expectation value of all the passengers at all of the station positions is calculated based on the tables for estimated time of arrival, and stored as eval 0 . The calculation steps of the waiting time expectation value of all the passengers at all of the station positions in Step S 502 are performed in the same manner as the process in Step S 24 in FIG. 7 as described above, and therefore an explanation is omitted. In Step S 503 , the initial value of the variable eval is set to be the maximum value.
[0108] Then, based on Step S 504 and Step S 513 , the process between these steps is repeated for all of the cars from the first car. Specifically, in Step S 505 , it is determined whether or not the “i” car is an empty car. If the “i” car is an empty car, based on Step S 506 and Step S 512 , the process between these steps is repeated for all of the station positions s.
[0109] In Step S 507 , it is determined whether or not the “i” car can service the station positions. If the “i” car can service, in Step S 508 , a table for estimated time of arrival assuming that a pseudo call at the station position s is tentatively assigned to the “i” car is generated as shown in FIG. 3 , and in Step S 509 , the waiting time expectation value of all the passengers is calculated based on the generated table for estimated time of arrival, and stored as the variable e. The calculation steps of the waiting time expectation value of all the passengers in Step S 509 are performed in the same manner as the process in Step S 24 in FIG. 7 as described above, and therefore an explanation is omitted.
[0110] Then, in Step S 510 , the value of e and the value of eval are compared, and if e is smaller, in Step S 511 , e is newly stored as eval by updating, and the car number “i” of the assigned car at this time is stored as “car” by updating. Subsequently, the same process is repeated for all of the station positions, and then for all of the cars, and the minimum value out of the waiting time expectation values assuming that the pseudo call assignment is performed is stored as eval, and the car to which the pseudo call is tentatively assigned is stored as “car”.
[0111] Then, in Step S 514 , it is determined whether or not the difference between the current waiting time expectation value eval 0 (before the tentative pseudo call assignment) and the minimum value eval after the tentative pseudo call assignment is greater than the set value PseudoParam 1 . Further, in Step S 515 , it is determined whether or not the reduction rate of the waiting time expectation value (a value obtained by dividing the difference between the current waiting time expectation value eval 0 and the minimum value eval after the tentative pseudo call assignment by eval 0 and then multiplying by 100%) is no smaller than the set value PseudoParam 2 . If the reduction rate is no smaller than the set value, in Step S 516 , the pseudo call at station position s is assigned to the “car” car, and the pseudo call assignment process to an empty car is terminated. Specifically, in this example, similarly to the case of the assignment change, in order to prevent unnecessary movement due to the pseudo call assignment, the pseudo call is assigned only when the waiting time expectation value of all the passengers decreases by the set value or more and the reduction rate is no smaller than the set value.
Second Embodiment
[0112] According to the first embodiment, the assignment of a new hall call is performed at a different timing from the assignment change of the hall call or the assignment of a pseudo call. However, the two processes can be performed at the same time.
[0113] FIG. 17 through FIG. 19 are flowcharts showing a specific procedure for assigning a new hall call and changing an assignment of a hall call at the same time. The process shown is divided into three flows at connecting signs A and B for convenience sake.
[0114] This process is an example in which the waiting time expectation value of all the passengers at all of the station positions assuming that a new hall call is assigned to each car is compared with the waiting time expectation value of all the passengers at all of the station positions assuming that the assignment of an assigned hall call is changed to a different car at the same time, and the new hall call assignment and the assigned hall call assignment change are performed at the same time if a difference between the two values satisfies a predetermined condition. The process is performed when a new hall call is made.
[0115] First, in Step S 601 , a variable evalA representing the waiting time expectation value, assuming that a new hall call is tentatively assigned and a variable evalB representing the waiting time expectation value, assuming that the assignment change is performed at the same time with the tentative assignment of the new hall call, are respectively set to be maximum values, and based on Step S 602 and Step S 617 , the process between these steps is repeated for all of the cars. Specifically, in Step S 603 , a table for estimated time of arrival assuming that a new hall call HC is tentatively assigned to an “i” car is generated, and then, in Step S 604 , the waiting time expectation value of all passengers at all station positions is calculated based on the generated table for estimated time of arrival, and set as a variable e. The calculation steps of the waiting time expectation value of all the passengers in Step S 604 are performed in the same manner as the process in Step S 24 in FIG. 7 as described above, and therefore an explanation is omitted.
[0116] Then, in Step S 605 , the value of e and the value of evalA are compared, and if e is smaller, in Step S 606 , e is newly stored as evalA by updating, and the car number “i” of the tentatively assigned car at this time is stored as “acarA” by updating.
[0117] Subsequently, based on Step S 607 and Step S 616 , the process between these steps is repeated for all hall calls AHC that are assigned to the tentatively assigned car “i”. Specifically, in Step S 608 , it is determined whether or not HC and AHC are calls made on the same floor, and if not med on the same floor, based on Step S 609 and Step S 615 , the process between these steps is repeated for all cars “j”. The reason why it is determined whether or not HC and AHC are calls for the same floor here is not to consider a hall call that is made on the same floor as a new hall call, but as a target of the assignment change when assigning the new hall call, because performing the assignment of a hall call and the assignment change on the same floor at the same time may confuse waiting passengers when a hall call in an opposite direction has already been registered on the floor on which the new hall call is made.
[0118] Then, in Step S 610 , it is determined whether or not i=j. If i≠j, in Step S 611 , a table for the estimated time of arrival assuming that HC is tentatively assigned to the “i” car and the assignment of AHC is tentatively changed to the “j” car is generated. In Step S 612 , the waiting time expectation value of all the passengers at all station positions is calculated based on the table for estimated time of arrival, and the obtained value is set as the variable e. The calculation steps of the waiting time expectation value of all the passengers in Step S 612 are performed in the same manner as the process in Step S 24 in FIG. 7 as described above, and therefore an explanation is omitted.
[0119] In Step S 613 , the value of e and the value of evalB are compared, and if e is smaller, in Step S 614 , e is newly stored as evalB by updating, the tentatively assigned car “i” assigned to HC is stored as “acarB” by updating, and the car whose assignment is tentatively changed to AHC is stored as “rcarB” by updating. The tentatively assignment change is repeated for all the cars in Step S 615 , and for all of the hall calls AHC in Step S 616 , and the minimum value out of the waiting time expectation values assuming that the tentative assignment of the new hall call is performed at the same time as the tentative assignment change of the assigned hall call is stored as evalB, the tentatively assigned car at this time is stored as “acarB”, and the car whose assignment is tentatively changed is stored as “rcarB”.
[0120] Furthermore, this process is repeated for all the cars in Step S 617 , and the minimum value out of the waiting time expectation values assuming that the tentative assignment of the new hall call is performed is stored as evalA, and the tentatively assigned car at this time is stored as “acarA”.
[0121] In Step S 618 , it is determined whether or not the difference between evalA and evalB is greater than the set value ReasParam 1 . Further, in Step S 619 , it is determined whether or not the reduction rate of the waiting time expectation value (a value obtained by dividing the difference between evalA and evalB by evalA, and then multiplying by 100%) is no smaller than the set value ReasParam 2 . If the reduction rate is no smaller than the set value, HC is assigned to the “acarB” car in Step S 620 , and the assignment of AHC is changed to the “rcarB” car in Step S 621 . Moreover, when even one of Step S 618 and Step S 619 is not satisfied, HC is assigned to the “acarA” car in Step S 622 , and the assignment of the assigned hall call is not changed. Specifically, in this example, in order to prevent unnecessary confusion due to the assignment change, the assignment of a new hall call and the assignment change are performed at the same time only when the waiting time expectation value of all passengers at all of the station positions decreases by the amount of the set value or more and when the reduction rate is no smaller than the set value, and only the assignment of a new hall call is performed when not.
[0122] While, in this example, the case in which the assignment change is performed at the same time with the assignment of a new hall call is described, it is also possible to perform the assignment of a pseudo call to an empty car at the same time with the assignment of a new hall call, instead of or along with the hall call assignment change.
Other Embodiments
[0123] It should be appreciated that, while in the above embodiments, the difference and the reduction rate from the current waiting time expectation value is compared with a set value as criteria for performing the hall call assignment change and the assignment of a pseudo call, such set value is not required to be a fixed value. The value can be set to be any value according to the group management specifications and conditions of the building; for example, the set value regarding the assignment change can be set to be closer to 0 when the immediate prediction is not performed, and the hall call assignment change is performed if there is possibility of improvement in the waiting time expectation value if only a little, or the set value regarding the pseudo call assignment can be set to be a greater value when energy saving is considered to be important, and standby operation using a pseudo call is performed only in a situation in which it is expected to reduce the waiting time to a large extent.
[0124] Further, in the above embodiments, as the waiting time expectation value of all passengers at all the station positions is taken as the general evaluation index, it is not necessarily possible to assign a car that can arrive in the shortest time to individual hall calls, and there is a case in which the car can pass without responding to a hall call. In such a case, if the group management system is provided with only a hall lantern as a guiding device in the elevator hall, then there is no problem as waiting passengers cannot see whether or not a car passes by without responding to the hall call. However, in the case that the group management system is provided with a hall indicator indicating the floor at which the car is currently in as the guiding device in an elevator hall, the waiting passengers at the elevator hall can see the car passing without responding to the hall call. Further, a car passing without responding to the hall call can also be recognized in the case in which doors at the hall has a window. Therefore, in a group management system of such specifications, there is a problem where the waiting passengers seeing the car passing without responding to the hall call may feel that their requests are unduly ignored or that the passengers are given a low priority, and thus dissatisfy with the group management system.
[0125] In order to address such a problem, it is possible to provide means for converting the car passing without responding to the hall call (including changing the direction of an approaching car) contrary to the expectation of the waiting passenger as a penalty value into waiting time.
[0126] For example, where the time of passage of the car is t p and the time at which the hall call is serviced by the car is t s , the penalty value can be calculated by equation 7 listed below.
[0000] Penalty Value= A+B ( t s −t p ) [Equation 7]
[0127] Here, A is an invariable for converting customers' dissatisfaction with passage of the car into time, and B is a coefficient representing dissatisfaction of the customers that increases in proportion to the time elapsed after the passage. Further, t s and t p can be obtained in the table for estimated time of arrival described above.
[0128] In the case in which the waiting passengers can recognize the passage of the car due to installation of the hall indicator or such, the evaluation can be made by adding the penalty value to the waiting time expectation value of all the passengers as the general evaluation index according to the present invention, or comprehensive evaluation can be performed by further adding other evaluation indices.
[0129] In addition, the present invention is not limited to the above embodiments, and various modifications can be made without departing the spirit of the present invention.
REFERENCE MARKS IN THE DRAWINGS
[0000]
11 - 13 Elevator Control Device
20 Hall Call Registration Device
30 Group Control Device
31 Passenger Arrival Rate Estimating Means
32 Hall Call Occurrence Rate Estimating Means
33 Car Arrival Time Estimating Means
34 Waiting Time Expectation Value Calculating Means
35 Hall Call Assigning Means
36 Hall Call Assignment Changing Means
37 Pseudo Call Assigning Means
38 Learning Means
39 Communicating Means
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Provided are a group control method and a group control device capable of efficiently controlling the operation of elevators in diversified traffic situations and under a variety of specification conditions required for a group management system. A plurality of elevators are placed in service for a plurality of floors, an evaluation index for a newly made hall call is calculated, and the best suited car is selected and assigned to the hall call based on the evaluation index in the group control method of elevators. A waiting time expectation value of all passengers on all floors for each direction, either that have already occurred or that are expected to occur within a predetermined time period, is taken as the evaluation index, the waiting time expectation value being the expectation value for the sum or the average of waiting time.
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BACKGROUND OF THE INVENTION
The invention is based on a generic hydraulic unit for a vehicle brake system. From European Patent Disclosure EP 0 621 836 B1, one such generic unit is known that is embodied as immersion-proof. The hydraulic unit has at least one pump that has a piston, and the piston is indirectly drivable by an electric motor via an eccentric that is rotatable inside an eccentric chamber. Because it cannot be precluded that the moving piston may entrain pressure fluid into the eccentric chamber through a sealing ring or the like on the occasion of pump operation, a conduit extends downward from the eccentric chamber and opens to the atmosphere through a housing block that receives the at least one pump; a check valve that can open toward the atmosphere is built into the conduit. Pressure fluid that has been entrained into the eccentric chamber and drips from the piston enters the conduit and stresses the check valve, causing it to open, and finally flows out of the housing block. As a result, filling of the eccentric chamber with pressure fluid is averted, so that pressure fluid remains far away from the electric motor, or in other words does not penetrate the electric motor and impair the operability thereof.
In a hydraulic unit known from International Patent Disclosure WO 96/13416, the electric motor is located above an eccentric chamber, in which the eccentric acting on at least one piston of a pump is rotatable. Once again, a conduit leads downward from the eccentric chamber, directly or indirectly to a so-called central venting point, where an element is installed that is permeable to air but not to water from the environment, so as to equalize the pressure of the eccentric chamber, for instance, relative to the ambient atmosphere and on the other hand to prevent at least splashing water from entering the unit. As an additional provision, the central venting point may have a check valve mentioned in this aforementioned patent disclosure. For instance, a check valve disclosed in the first reference cited, EP 0 629 836 B1, could be used. The unit also has at least one reservoir intended for temporarily receiving pressure fluid; it comprises a cylindrical hollow chamber closed off from the ambient atmosphere, a piston displaceable in the chamber that divides the hollow chamber into a variable storage chamber and a spring chamber, and a spring acting on the piston. The spring is braced on a cap that tightly closes off the hollow chamber. Extending from the spring chamber, adjacent to the cap, a pressure equalization conduit, which leads either upward to an inner hollow chamber in the electric motor or downward to a hollow chamber in a covering hood. The covering hood covers electromagnets of valves of the unit, as well as electrical components that are disposed on a circuit board. In operation of the unit, pressure fluid entrained into the eccentric chamber by a piston of the pump drips directly into the covering hood, for instance, so that it cannot be precluded that electrically operative components will become moistened with the pressure fluid.
OBJECT AND SUMMARY OF THE INVENTION
The characteristics set forth herein offer the advantage that pressure fluid entrained into a cam element chamber, which for instance may be an eccentric chamber, by motions of the piston pump piston, are delivered to the at least one spring chamber, far from electrical components, and collected in that chamber. Because the entrained pressure fluid is collected in the spring chamber, permeable elements at a central venting point as in the prior art, or a check valve as in the prior art, can conditionally be dispensed with. To this extent, the invention yields cost savings as well as the advantage of a hermetic seal of the unit from the environment. The housing block together with the at least one pump can be immersed and submerged, for instance in salty water, without the risk of damage.
With the provisions recited herein, advantageous refinements of and improvements to the hydraulic unit defined are possible.
The characteristics set forth offer the advantage that because of dual utilization of conduit portions, the housing block can be produced economically, on the one hand having fewer conduits and on the other by cleaning these fewer conduits after they have been produced.
The characteristics set forth herein offer the advantage that a housing block, known from EP 0 699 571 A1, for a hydraulic unit of a vehicle brake system can be used without changing its size or its basic internal design, so that the only provision necessary is the disposition of the characteristics set forth hereinafter. The engineer can decide how much pressure fluid entrained by the at least one piston of the at least one pump should be stored. If the hydraulic unit is intended merely to avoid the danger of wheel locking, then the at least one container will be made smaller than if the hydraulic unit is additionally designed for automatic braking and for traction control of driven wheels or for stabilization while driving. This is because automatic braking can involve more-frequent activation of the at least one pump.
The characteristics defined herein offer a practical exemplary embodiment for such containers with recourse to deep-drawing techniques known per se. The characteristics set forth herein offer the advantage that in a favorable way from a production standpoint, the invasion of water between a fastening portion of the container and the housing block is averted.
The features set forth offer the advantage on the one hand that the motor can be delivered complete to an assembly line, along which the motor is moved toward the housing block and fixed to it, and as a further advantage at the same time an intended sealing off against the invasion of water from the environment into the motor and into the cam element chamber located in the housing block is avoided. The characteristics set forth also offer the advantage that the seal can be made in a favorable way from a production standpoint, and because of the resultant geometrical design of the seal, less sealing material is consumed. Since the sealing material can be mounted in the form of a worm of closed circular-annular shape, both the aforementioned sealing and sealing off of the pressure-equalizing conduit relative to the environment are attained by means of such a worm.
The characteristics defined herein bring about a pressure equilibrium between the motor and a covering hood, which contains such electrically operative components as relays or semiconductor elements and which thus also protects electromagnets of valves of the hydraulic unit from the harmful effects of the environment by sealing them off from the environment. Pressure equalization of both the motor interior and the covering hood with regard to the atmosphere is done in a way that is gentle to the unit, by making use of a cable sheath, joined in sealed fashion to the covering hood, and this sheath is terminated at the highest possible point in the vehicle, to avert the risk that water can enter a partially immersed vehicle. To this extent, it is possible to avoid the provision of a pressure equalization hose, which begins at a lowest point of the hydraulic unit and then rises, as disclosed in WO 96/13416, a hose that serves the sole purpose of pressure equalization.
The invention will be better understood and further objects and advantages thereof will become more apparent from the ensuing detailed description of preferred embodiments taken in conjunction with the drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 shows a first exemplary embodiment of the hydraulic unit according to the invention in a side view and partially cut away;
FIG. 2 shows a cross section of the unit of FIG. 1 along line II--II;
FIG. 3 shows a component of the hydraulic unit in an oblique view;
FIG. 4 shows a detail of the hydraulic unit of FIG. 1 in an end view;
FIG. 5 shows an electrical component in a cutaway view for the unit of FIG. 1;
FIG. 6 shows a second exemplary embodiment of the unit of the invention, partly cut away; and
FIG. 7 shows a third exemplary embodiment of the unit of the invention, again partly cut away.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
First Exemplary Embodiment
The hydraulic unit 2 of the invention includes as its essential components a housing block 3 and, mounted against the housing block 3, a motor 4, which is shown only in FIG. 3, as well as a housing 5 and a covering hood 6. Because the hydraulic unit 2 to this extent largely agrees with the hydraulic unit of EP 0 699 571 A1, a relatively brief general description will suffice, so that characteristics essential to the invention will be more apparent.
A securing face 7 for the motor 4 is located on a face end A of the housing block 3, as shown in FIGS. 1 and 4. Extending vertically to this securing face 7 in the housing block 3 is a stepped bore 8, which defines an eccentric chamber 9. A shaft trunnion 10, which by means of a ball bearing 11 that is supported by the stepped bore 8, determines a pivot axis 12 for an eccentric 13 that is embodied integrally with a shaft 14. The shaft 14 extends from the eccentric 13 into the motor 4. The motor may be embodied in a manner not shown as a direct current motor, with an armature and collector that are not shown and may be equipped with contact brushes, also not shown, that are associated with the collector. In addition, it will be noted here that the eccentric 13 shown is a cam element known per se, as well as known swash plates and other cam curves. Accordingly, to avoid unnecessary limitation here, the eccentric is also understood to be a cam element, and correspondingly in an expanded sense a cam element chamber is intended in place of an eccentric chamber 9.
A cross section through the eccentric 13 is shown in FIG. 2. In FIG. 2, the shaft 14 adjoining the eccentric 13 behind it can also be seen. In FIG. 3, the sequence of a shaft trunnion 10, eccentric 13 and shaft 14 is clearly shown. Disposed around the eccentric 13 is for instance a needle bearing 15, which is held together by a bearing ring 16. Axial stop means 17, 18 for the bearing ring 16 are provided on both sides of the bearing ring 16. The bearing ring 16 is rotatable relative to the eccentric 13 between these axial stop means 17 and 18. The stop means 17 has a hub 19, which is seated fixedly on the shaft 14. The axial stop means 18 is in the form of an outer conical ring and is press-fitted, firmly seated, onto the eccentric 13. These individual parts are shown in FIG. 1. In FIG. 2, crosswise to the pivot axis 12 of the eccentric 13 and thus coaxially and in mirror symmetry with the eccentric 13, two pump pistons 20, 21 are provided. The pump pistons 20, 21 are displaceable in pump cylinder bores, not shown, that are located in pump cylinders 22 and 23. The pump cylinders 22 and 23 are combined with outlet valves 24 and 25, respectively, thus forming two piston pumps that are operative independently of one another and have inlets 24a and 25a. In a manner known per se, these inlets 24a and 25a are assigned inlet check valves, not shown, inside the piston pumps. The piston pumps 22, 23 are fixed in the housing block 3, for instance by means of caulked features 26, 27. To generate pressure, the pump pistons 20 and 21 are displaceable longitudinally by means of the eccentric 13, which has earlier also been called a cam element, with the interposition of the needle bearing 15 and its bearing ring 16. For displacement in the respective opposite direction, a C-shaped spring clip 28 firmly hooked onto the pump pistons 20 and 21 is used.
In FIG. 2, first cylindrical bores 30, 31, which are drilled vertically from below into the housing block 3 in the manner of blind bores, are located below the elements 20, 22, 24 and 21, 23, 25 of the respective piston pumps 22, 23. In the bores 30 and 31, pistons 34 and 35, so-called storage pistons, that are loaded by springs 32, 33 are provided. Sealing rings 36 and 37, respectively, assure that sealed-off storage chambers 38 and 39 are available, above the pistons 34, 35, for receiving pressure fluid. Connecting conduits 30a and 31a extend upward from the cylindrical bores 30 and 31 and connect the storage chambers 38 and 39 to the inlets 24 and 25a of the two piston pumps 24 and 25. Below the pistons 34 and 35, the cylindrical bores 30 and 31 form spring chambers 30b and 31b. The springs 32 and 33 are retained inside the cylindrical bores 30 and 31 by means of spring plates 32a and 33a, which in turn are braced rigidly in the housing block 3 by means of spring wire rings 32b and 33b. The connecting conduits 30a and 31a communicate with lower stepped bores 52, located above the piston pumps 24, 25, which bores serve to receive multiposition valves 53, shown schematically in FIG. 1, that are actuatable by means of electromagnetic coils 55. The multiposition valves 53 in the exemplary embodiment are so-called brake pressure reduction valves. Also shown in FIG. 2 are upper stepped bores 50, to which in FIG. 1 multiposition valves 51 with electrical coils 54 are assigned. Because the subject of the invention does not pertain to the hydraulic interconnection of multiposition valves with wheel brake cylinders and a master cylinder, further details need not be addressed here.
In a manner according to the invention, first conduit portions 101, 102 and 103 extend downward, beginning at the eccentric chamber or cam element chamber 9. The conduit portion 101 is made in the manner of a bore that intersects the stepped bore 8 at its lowest point and thereby forms a kind of channel and in its further course extends in the form of a cylindrical bore, for instance parallel to the pivot axis 12 of the eccentric 13. The conduit portion 101 ends in the manner of a blind bore. Intersecting the conduit portion 101 and in the process discharging into this conduit portion 101 is the conduit portion 102, which is drilled in from an underside of the housing block 3 and is closed off, adjoining the underside, by means of a ball 104 press-fitted into place. The conduit portion 103 in turn is made in the form of a bore that begins at one side of the housing block 3, intersects the cylindrical bore 30, discharges into the conduit portion 102 and intersecting the latter extends onward, finally discharging into the bore 31. The conduit portions 101-103 form a conduit oriented downward from the cam element chamber 9 and discharging into the spring chambers 30b and 31b. It can be seen that pressure fluid dripping from the ends, visible in FIG. 2, of the pistons 20 and 21 find a path out of the cam element chamber 9 and into the spring chambers 30b and 31b. The pressure fluid dripping off is the same pressure fluid mentioned in the description of the prior art, which on the occasion of the operation of the piston pumps 22 and 23 passes through sealing rings, not shown, or in other words has been entrained between sealing faces.
To prevent dirt and water from penetrating the bores 30, 31 from below, these bores are closed by means of closure elements 106 and 107. In the exemplary embodiment, the closure elements 106 and 107 perform the task both of a cap as in the prior art and the task of catching pressure fluid according to the invention, fluid that has been diverted out of the eccentric chamber 9 by means of the first conduit portions 101, 102 and 103.
The respective closure element 106 and 107 is produced here in the form of a substantially cup-shaped deep-drawn part, next to whose free edge 108 a bead 108 is first disposed, the bead subsequently being upset to form a flangelike axial stop as shown. With the free edge 108 leading, the closure element 106 and 107 is press-fitted into the respective spring chamber 30b and 31b. This already creates a certain sealing, which is supplemented by a sealing element 110, which in a manner that can be selected from the prior art for instance be a prefabricated sealing ring, or a worm of initially liquid silicon rubber, applied before the closure elements 106 and 107 are built in, which over the course of time, changes into a rubber-elastic state. It is shown in FIG. 2 that the upper free edges 108 and these closure elements 106 and 107 are located below the conduit portion 103. To this extent, pressure fluid from the conduit portion 103, for instance, can get into the two bores 30, 31 along the sealing rings 32b, 33b and flow downward into the closure elements 106 and 107. It will be appreciated that the greater the axial length of the closure elements 106 and 107, the more pressure fluid can be received before collected pressure fluid reaches the level at which the conduit portion 103 is disposed. In order that no pressure fluid will reach the outside even from a beginning of a bore portion that belongs to the conduit portion 103, a ball 105 is press-fitted as a closure piece into the housing block 3.
In addition it will be noted that the respective closure elements 106 and 107, each assigned to one of the bores 30 and 31, can be exchanged for a common cap in the manner of a cap shown in European Patent Disclosure EP 0 662 891 B1, which according to FIG. 2 thereof is embodied in substantially tub-shaped fashion and is braced against the housing block with the interposition of a seal. If such a cap is used, then the disposition of the ball 104, the conduit portion 103, and the ball 105 that seals off the conduit portion 103 from the outside, as shown in FIG. 2 of the present application, may be dispensed with.
A generic pressure equalization conduit between at least one spring chamber 30b, 31b and the interior 111 of the motor 4 includes the first conduit portions 101, 102 and 103 and the eccentric chamber or cam element chamber 9 and finally two conduit portions 112 and 113. The conduit portion 113 is embodied as a hole in an end wall 114 of the motor facing toward the housing block 2. The conduit portion 112 is embodied in the manner of a bore cut halfway open, for instance, which intersects the contour of the stepped bore 8 and is embodied in comparable fashion to a portion of the conduit portion 101 that has been described above. Located between the conduit portions 112 and 113 is a conduit portion 115, which is located radially inside a sealing element 116 that is located between the end wall 114 of the motor and the securing face 7 furnished by the housing block 3. In FIG. 4, this sealing element 116 is embodied as extending annularly and is either stamped out of a sealing material or injection molded from it, or preferably, as described for the sealing element 110 of the closure elements 106 and 107, made from an initially liquid sealing material such as silicone rubber by being poured or sprayed onto the securing face 7. A sealing element produced in this way is sometimes also called a sealing worm and here has a thickness, measured in the axial direction of the motor 4, of substantially 2 mm, for instance. Radially inside this sealing element 116, it is possible to dispose support elements 117, which for instance are four in number and for instance are elastic.
It can now be appreciated that beginning at the eccentric chamber 9, the conduit portion 112 extends radially outside a centering attachment 118, which receives a ball bearing not shown and originates at the end wall 114 of the motor extending toward the eccentric 13, between the end wall 114 and the securing face 7 located on the housing block 3 and thus radially inside the sealing element 116, and finally continues in the form of the conduit portion 113 that is formed by a hole in the end wall 114 of the motor. This brings about a pressure equilibrium between the interior 111, that is, a hollow chamber of the motor 4, and the eccentric chamber 9. Together with the first conduit portions 101, 102 and 103 that were described first, a pressure equalization conduit exists between the at least one spring chamber 30b, 31b and the interior 111 of the motor 4; when at least one of the two pistons 34, 35 moves counter to the force of the respective spring 32, 33, the pressure equalization conduit allows air to escape from the respective spring chamber 30b, 31b into the interior 111, the purpose of which is that a displacement resistance of the respective piston 34 or 35 is determined essentially by the force of the respective spring 32, 33. It can be seen that to divert pressure fluid out of the eccentric chamber 9 and for equalizing pressure between the spring chambers 30b and 31b and the interior 111 of the motor, first conduit portions 101, 102 and 103 are utilized in two ways. This provides a cost savings compared with two separately embodied conduits, of which one would be used to carry away pressure fluid and the other would be used for pressure equalization.
Shown in FIG. 1 is a cable 64, which originates at the housing 5 and leads to the motor 4 to supply current to it. The housing 5 is a housing in which a relay, for instance, for switching the electric current for the motor 4 is disposed. In a manner according to the invention, a pressure equilibrium is created between the interior 111 of the motor 4 and the housing 5, which is sealed off relative to the housing block 3. The purpose of pressure equalization is served here by a pressure equalization conduit, which is formed by interstices between wires 120 of the cable 64 and a tubular cable sheath 121 that sheathes the wires 120.
Oriented toward the housing 5, the cable sheath 121 is surrounded by a sealing sleeve 122, which is inserted sealingly into a plug portion 123. The plug portion 123 in turn has a further sealing sleeve 124 on its outside, which becomes operative upon insertion of the plug part 123 into a socket that is located in the housing 5. Contact clips 125 are provided inside the plug part 123 and are electrically connected to the wires 120 by digging into them. It can be seen that because of the embodiment of the contact clips 125 as a bent sheet-metal part with a central portion 126, a flow is possible through the plug part 123, from the contact clips 125, to in between the wires 120 shown and from there on between the wires through the cable sheath 121.
In a comparable way, the cable sheath 121 is introduced into a further sealing sleeve 127, which is located inside a second plug part 128. Instead of the contact clips 125 already described, a plug prong 129 is electrically connected to the wires that extend inside the cable sheath 121. The electrical connection can once again be made in a manner known per se by digging action, to which end the plug prong 129, protruding into the sealing sleeve 127, has a tubular prolongation that is crimped toward the wires 120. To allow a flow of air around the plug prong 129, this prong is aligned by means of centering ribs 130 inside the plug part 128. A contact bush, not shown, is associated with the plug prong 129 inside the motor 4, and a brush holder, also not shown, is for instance connected to the contact bush. The centering ribs 130 extend radially outward from a tubular portion 131. A sealing element 132 that has sealing ribs 133 oriented toward the motor 4 is slipped over this tubular portion 131. To enable the sealing ribs 133 to be pressed sufficiently firmly against the motor 4, fastening tabs 134 with screw holes 135 are formed onto the plug part 128. One fastening tab can be seen in FIG. 1. The screw hole 135 is not visible, because it is covered by the head 136 of a fastening screw.
The cable sheath 121 is connected at least indirectly to the connection cable 140 in a way that equalizes pressure; the connection cable 140 likewise comprises a cable sheath 141 and in this case a plurality of sheathed connection strands 142.
By means of elements 143 and 144, not described in detail, which can be learned from the prior art in electrical connection technology, a connection is made with a sealed plug base 145 located on the housing 5. This prevents water from entering between an end of the cable sheath 141--this end is not visible in the drawing--and the housing 5. In a manner according to the prior art, contact elements not shown are disposed in the plug base 145 and the connection part 144 in such a way that beginning at the connection strands 142, once again air flow possibilities are present, which can be from the cable sheath 141 into the housing 5 or in the opposite direction. The connection cable 140 is extended upward inside the vehicle to the highest possible point, of which it can be assumed that no water will get into it. As a consequence, in an intended way, the cable sheath 141 acts as a pressure equalization conduit between the ambient atmosphere and the interior of the housing 5 and indirectly through the cable sheath 121 for the motor 4 as well.
The provisions described in detail thus directly prevent the invasion of water to the hydraulic unit 2 yet nevertheless provide a pressure equalization of interiors of the hydraulic unit 2 with the ambient atmosphere, and they moreover bring about the diversion of pressure fluid, entrained by pump pistons, into a region of the unit that is located far from vulnerable electrical parts of the hydraulic unit. This prevents electrolytically active ingredients that may be present in the pressure fluid from attacking electrical components or rendering them inoperative.
Second Exemplary Embodiment
The second exemplary embodiment of an anti-lock brake system 2a of FIG. 6 is embodied identically, in terms of the diversion of pressure fluid entrained by pump pistons, to the first exemplary embodiment shown in FIGS. 1, 2, 3 and 4. In FIG. 6, therefore, of the first conduit portions only the conduit portion 101 originating at the cam element chamber 9 and a portion of the length of the conduit portion 102 extending downward from the conduit portion 101 are shown. In a distinction from the first exemplary embodiment, the component 118 here serves the purpose of centrally receiving a ball bearing, not shown. This ball bearing, not shown, is intended to embrace the shaft 14 and thus support it centrally with respect to the motor 4. In the region of the component 118, the stepped bore 8 is therefore embodied such that an annular second conduit portion 112a opens up between this bore and the component 118. In the direction toward the interior 111 of the motor, a further, second conduit portion 115 adjoins it; as in the first exemplary embodiment, this conduit portion extends inside a sealing element 116, between a securing face 7 of a housing block 3a and an end wall 114 of the housing. Once again, a further, second conduit portion 113, which is embodied as a hole in the end wall 114 of the motor, connects the second conduit portion 115 to the interior 111 of the motor 4.
An upper screw head 150 and a lower screw head 151 of two screws 150a and 151a are shown in fragmentary form in FIG. 1, and FIG. 3 they are shown passed through the motor 4 in order to secure it by being screwed into the housing block 3a. To that end, as shown in FIG. 4, two threaded holes 152 and 153 are provided in the housing block. To prevent entrained pressure fluid, which may possible escape from the cam element chamber 9 through the second conduit portion 112a between the securing face 7 and the end wall 114 of the motor, from reaching the threaded hole 115 and thus from flowing along the lower screw 151a to reach the interior of the motor 4, a sealing strip 116a, extending for instance with a uniform curvature, also extends around the threaded hole 153 from the sealing element 116.
In the second exemplary embodiment of FIG. 6, the motor has two bearings for the shaft 14 on either side of an armature, not shown. One of the two bearings is the ball bearing, already mentioned, in the component 118. When such a motor 4 is mounted on the housing block 3a, the centering of the motor relative to the cam element chamber 9 is accomplished when the shaft trunnion 10 is plugged into the ball bearing 11 located in the housing block 3a.
As described for the first exemplary embodiment, here as well the sealing element 116 and the sealing strip 116a can selectively be poured or sprayed from sealing medium or stamped out from a plate.
Third Exemplary Embodiment
The third exemplary embodiment of the hydraulic unit 2b of the invention as shown in FIG. 7 takes over the housing block 3a of the second exemplary embodiment shown in FIG. 6, for instance, so that entrained pressure fluid, which originates in pump elements 22, 23 and is to be diverted out of the cam element chamber 9, can flow downward through conduit portions 101, 102, far away from the interior 111 of the motor 4.
The pressure equilibrium between the cam element chamber 9 and the interior 111 of the motor is provided by an opening in the component 118 that discharges as a second conduit portion into the cam element chamber 9; this opening forms an annular second conduit portion 113a that surrounds the shaft 14. This second conduit portion 113a is adjoined by a further second conduit portion 113b, which extends between an inner ball bearing ring 118b, embracing the shaft 14 and an outer ball bearing ring 118a that is horizontal relative to the housing block 3a, and in the process extends between bearing balls 118c. Since on the other hand in a manner already described the cam element chamber 9 communicates with the spring chambers 30b and 31b through first conduit portions 101, 102 and 103, a pressure equilibrium between the spring chambers 30b and 31b and the interior 111 of the motor 4 is again possible through the cam element chamber. This third exemplary embodiment makes do without openings, shown in FIGS. 1, 2, 3 and 6, each of them forming one second conduit portion 113, and this makes production cheaper.
In addition it will also be noted that in the third exemplary embodiment of FIG. 7, the second conduit portions 112a, 115 and 113 of the second exemplary embodiment shown in FIG. 6 can also be adopted, for the sake of promoting a pressure equilibrium between the spring chambers 30b, 31b and the interior 111 of the motor 4.
The foregoing relates to preferred exemplary embodiments of the invention, it being understood that other variants and embodiments thereof are possible within the spirit and scope of the invention, the latter being defined by the appended claims.
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A hydraulic unit for a vehicle brake system that enables limiting wheel brake slip is known. To that end, the hydraulic unit has at least one piston pump, which is drivable by an electric motor and empties a reservoir that is filled on the occasion of the limitation of wheel brake slip. This reservoir comprises a cylinder, embodied in the manner of a blind bore, as well as a piston that divides a storage chamber from a spring chamber in the cylinder, a spring, and a closure element that prevents water from entering the cylinder if the hydraulic unit should become immersed in water. A pressure equalization conduit begins at the spring chamber and leads into the interior of the motor, so that a displacement of the piston for taking up pressure fluid in the storage chamber is effected essentially only by friction of the piston and forces of the spring. A conduit is also provided, by means of which pressure fluid that emerges from the piston pump at the eccentric can be carried away. The invention proposes connecting the spring chamber of the reservoir to the conduit that carries the pressure fluid away. The spring chamber forms a collection container for pressure fluid, as a result of which the collection of the pressure fluid takes place far away from electrical components of the hydraulic unit, and especially of the motor, thus avoiding electrical defects.
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BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to a method and device for the production of solid particles from a liquid and the separation of solid particles contained in a bath of refrigerating liquid. The method of producing and separating solid particles is intended for example for obtaining balls of ice for surface cleaning by projection of the particles, or for constituting solid products from aqueous mixture. Finally, the method of production and separation is provided for obtaining solid particles from liquids of which the latent heat of solidification is less than that of pure water.
2. History of the Related Art
French Patent 2 630 668 discloses a method and a device for producing balls of ice for surface treatments. The method consists in dispersing by gravity a spectrum of droplets of water in a column of cold gas, so that the droplets of water pass through said column of cold gas by gravity and cool, solidifyig superficially before dropping in a bath of refrigerating liquid where they are solidified entirely in the form of balls of ice. The device for carrying out the method comprises an exchange column supplied with cold gas and droplets of water which are regularly distributed via an injector to create a spectrum of droplets. The device also comprises a receptacle secured to the exchange column comprising a spray pipe for feeding the refrigerating liquid, a cone for receiving the balls of ice and an orifice for evacuating the balls of ice at the bottom of the cone.
The receptacle has a cylindro-conical form in which a refrigerating liquid such as liquid nitrogen is introduced with a view to completely solidifyig the droplets of water which pass therethough.
A phenomenon of heating will be noted, when the partially solidified droplets of water reach, at the end of their free fall, the surface of the refrigerating liquid, said phenomenon due to the evaporation of the liquid nitrogen. The phenomenon of heating retains each ball of ice in lift until it has attained the temperature of the gaseous nitrogen coming from the change of phase of the liquid nitrogen.
It will be noted that it is only after complete solidification of the ball of ice that it starts its descent by gravity to the bottom of the cylindro-conical receptacle the phenomenon of heating also provokes a high rate of occupation of the surface of the bath of liquid nitrogen, risking constituting either out-of-calibre balls or agglomerates which are highly detrimental to the manufacture of the balls of ice and to the extraction thereof at the Archimedean screw.
A second phenomenon which is detrimental in the manufacture of the balls of ice is noted, which is induced by the slight difference in density between the ice at -196° and that of the liquid nitrogen, viz. respectively about 0.850 and 0.8068. The slight difference in density influences the dynamics of descent by gravity of the balls of ice, hence a strong tendency to constitute agglomerates at the surface of the bath of liquid nitrogen.
DE-A-2 805 676 discloses a method and a device for producing solid balls comprising a supply of cold gas, an agitator with blade, a receptacle and an Archimedean screw belonging to an extraction device. In this device, the movement of the liquid in the bottom of the receptacle is not directed downwardly, this resulting in risks of turbulences and choking.
SUMMARY OF THE INVENTION
It is a more particular object of tile invention to overcome these drawbacks, by proposing a method and a device in which the circulation of the balls towards the extraction device is facilitated.
In this spirit, the invention relates to a method for producing and extracting solid particles in the form of balls consists in dispersing by gravity a spectrum of droplets of particles in a column of cold gas, so that the droplets pass through said cold gas column by gravity and cool, solidifyig superficially before falling into a bath of refrigerating liquid, and in continuously extracting the balls from the bath of refrigerating liquid, characterized in that it future consists in displacing the bath of refrigerating liquid in a slow movement in the sense of a vortex in a cone of asymmetrical profile constituted by an assembly of inclined walls shaped to produce two distinct zones of progressive and different inclination, so as to create a wave whose forces are directed downwardly in order to allow descent of the droplets of particles so that they solidify entirely in the form of balls.
The invention also relates to a device for carrying out the method and more specifically, a device for producing and extracting solid particles in the form of balls, of the type comprising an exchange column supplied with cold gas, an injector of particles to be solidified and a receptacle supporting the column and whose bottom comprises an orifice for evacuating the solidified particles in the form of balls, said orifice communicating with a pipe in which is rotated an Archimedean screw of an extraction device for continuously evacuating the solid particles, characterized in that said bottom has the form of a cone of asymmetrical profile constituted by an assembly of inclined walls shaped to produce two distinct zones of progressive and different inclinations, a blade of an agitator being introduced inside said asymmetrical cone to displace, in a slow movement, a bath of refrigerating liquid contained in the receptacle.
BRIEF DESCRIPTION OF THE DRAWINGS
The accompanying drawings, given by way of example, will enable the invention, the characteristics that it presents and the advantages that it is capable of procuring, to be more readily understood.
FIG. 1 is a view in perspective illustrating the device according to the invention for carrying out the method of producing and extracting solid particles.
FIG. 2 is a schematic section showing the receptacle of the device for producing/extracting solid particles.
FIG. 3 is a plan view along III--III of FIG. 2, showing the profile of the receptacle in the form of an asymmetrical cone.
DESCRIPTION OF THE PREFERRED EMBODIMENT
FIG. 1 shows a device 1 for producing and extracting solid particles, comprising an exchange column 2 mounted to its lower part with a receptacle 3 which abuts by means of brackets 3a on a chassis (not shown). The whole of the device 1 is made of stainless steel enveloped in an insulating material 4 such as polyurethane, shown in dashed and dotted lines.
The exchange column 2 is shaped like the one described in French Patent 2 630 668, with the result that it comprises, towards it upper end, i.e. opposite the receptacle 3, the inlet of an injector 2a. This injector is provided with a large number of holes trough which the spectrum of droplets intended to produce the balls of solid particles is formed. The diameter of the droplets of particles may be adjusted as a function of the diameter of the holes.
The exchange column 2 also supports an agitator 5 whose shaft 5a is secured to a blade 5b which is placed inside the receptacle 3.
The receptacle 3 has a spray pipe 3b arranged just below the level of fixation of the exchange column 2 to feed the refrigerating liquid inside the device 1. The spray pipe 3b is pierced with a multitude of holes to diffuse the refrigerating liquid which is constituted for example by liquid nitrogen. It will be noted that the spray pipe 3b has the form of a C in order to constitute inside the receptacle 3 a passage for the drive shaft 5a of the agitator 5 (FIGS. 2 and 3).
The receptacle 3 has in its upper part a cylindrical profile 3c extending to the exchange column 2 and inside which is placed the injection spray pipe 3b. The cylindrical profile 3c extends, to form the lower part of the receptacle 3, in an asymmetrical cone 3d (FIG. 2).
The asymmetrical cone 3d is constituted by an assembly of inclined walls which are shaped to produce two distinct zones of progressive and different inclinations. The first zone 3e comprises a plurality of walls assembled on one another, of which at least the end one 3f is inclined by an angle included between 40° and 45° with respect to the vertical axis (A--A) of the cone 3d. On the other hand, the second zone 3g extending from the first comprises a plurality of walls of which at least the end one 3h is inclined by an angle included between 3° and 10° with respect to the vertical axis of the cone 3d (FIGS. 2 and 3).
It will be noted that the variation in the inclination of the walls constituting the first zone 3e must be sufficient to allow the blade 5b of the agitator 5 to be placed in position.
The asymmetrical cone 3d comprises in its lower part an orifice 3i located in the vicinity of the wall 3h of the second zone 3g, i.e. offset laterally with respect to the principal axes locating the widest base of the cone 3d. The orifice 3i opens out in an inclined pipe 3j extending upwardly and in which is rotated an Archimedean screw 6a of an extraction device 6 for continuously evacuating the solid particles located in the bottom of the asymmetrical cone 3d.
The pipe 3j comprises in its upper part a spout 3k of cylindrical profile for evacuating the balls of solid particles inside a sealed container for conserving the balls.
It is observed that the pipe 3j is arranged in a vertical plane substantially perpendicular to that containing the drive shaft 5a of the agitator 5.
Operation of the device for producing the solid particles is identical to that described in French Patent 2 630 668. In fact, the injector 2e disperses at the top of the exchange column 2 a spectrum of droplets of liquid particles falling by gravity in the exchange column. Upon direct contact of the cold gas, the droplets freeze partially. They fall by gravity in the exchange column 2 and thus drop in the bath of refrigerating liquid located in the asymmetrical cone 3d of the receptacle 3 where they solidify completely.
The wide, flat blade 5b of the agitator 5 provokes a slow movement of the bath of liquid nitrogen in the sense of a vortex. This movement, associated with the shape of the asymmetrical cone 3d, makes it possible to create a wave whose forces are directed downwardly. The orifice 3i is positioned with respect to the point of convergence of the forces mentioned above in order to accelerate extraction of the solid particles located at the bottom of the cone 3d by means of device 6.
It will be noted that the speed of rotation, which is slow and fairly precise, of the blade 5b, avoids a turbulent breaking of the wave against the walls of the asymmetrical cone 3d. Under these conditions, it is ascertained that the consumption of liquid nitrogen is very close to the theoretical one.
It will be noted that the solid particles pass through the bath of liquid nitrogen in quite satisfactory manner without creating any choking at the level of the surface of said bath of liquid nitrogen. In fact, as soon as the particles in the course of solidification arrive on the surface of the bath of nitrogen, said particles are directly entrained by the wave effect of said bath so that they pass therethrough as far as the orifice 3i of the asymmetrical cone 3d.
It will be noted that the solid particles may be constituted from any aqueous mixture of any liquid of which the latent heat of solidification is less than that of pure water.
Moreover, it must be understood that the foregoing description has been given only by way of example and that it in no way limits the domain of the invention which would not be exceeded by replacing the details of execution described by any other equivalents.
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The device for implementing the method comprises a receptacle (3) whose internal profile has the shape of an asymmetric cone (3d) inside which is arranged a blade (5b) of an agitator (5) to agitate with a slow motion the bath of refrigerating liquid contained in the receptacle (3), an orifice (3i) being provided at the bottom of the cone (3d) and communicating with a pipe (3j) wherein is rotationally driven an Archimedean screw (6b) of an extractor device (6) to evacuate continuously the solid particles.
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TECHNICAL FIELD OF THE INVENTION
This invention relates generally to the field of composite materials and more particularly to a method for composite material repair.
BACKGROUND OF THE INVENTION
Many manufacturing processes today call for the fabrication of components from “composite” materials, also known as fiber-reinforced polymers. Fiber-reinforced polymers are comprised of reinforcing fibers that are positioned in a polymer matrix. Commonly, the reinforcing fibers are fiberglass, although high strength fibers such as aramid and carbon are used in advanced applications, such as aerospace applications. The polymer matrix is typically a thermoset resin, such as polyester, vinyl ester, or epoxy. Specialized resins, such as, phenolic, polyurethane and silicone are used for certain applications.
Composite materials may be formed using numerous types of fabrication process. One such process is a wet lay-up process. In a wet lay-up process, layers of dry reinforcing fiber are laid on a mold by hand or by a placement machine. Liquid resin is then poured on the fiber materials such that the resin fills the spaces between the fibers. The materials may then be cured at room temperature or in an autoclave and the liquid resin turns into a solid thermoset. The fibers are thus embedded in the solid thermoset resin and reinforce the resin. Alternatively, layers of fibers can be pre-impregnated with resin and then partially cured to form layers of “prepreg” material. After this partial curing, the resin has not completely set and the prepreg layers are flexible and can be shaped in or around a mold or forming tool. Once the prepreg layers are so shaped, the prepreg is then completely cured in an autoclave to form a fiber-reinforced laminate.
A common defect associated with composite structures is air inclusions or voids located inside the composite material. Such voids weaken the composite material and sometimes must be repaired. Another scenario requiring repair is when the composite material is impacted during service, resulting in delamination or delaminations between layers of the material. Such damage is typically referred to as interlaminar defects or interlaminar damage.
One type of repair for voids and interlaminar defects is resin injection. During one type of resin injection repair, two holes are drilled through the composite material to the void or delamination inside the composite material. The two holes are typically drilled at opposite ends of the defect. Resin is then either driven into one hole using pressure until it exits the second hole, or resin is drawn into one hole by applying a vacuum to the second hole. When using such a two-hole process, air entrapment in the void is common and therefore the resin does not completely fill the void. In addition, since two holes must be drilled in the structure, the already weak structure is further weakened.
SUMMARY OF THE INVENTION
In accordance with the present invention, a method for composite material repair is provided that substantially eliminates or reduces disadvantages or problems associated with previously developed methods. In particular, the present invention contemplates a method of repairing a void in a composite material using a repair material injected into the void through a single channel.
In one embodiment of the present invention, a method for repairing a composite material having an internal void includes identifying the location of the internal void and forming a single channel extending from a surface of the composite material to the internal void. The method further includes pulling a vacuum in the internal void and inserting a repair material through the channel into the internal void.
Technical advantages of the present invention include a method for composite material repair that provides an improved method of repairing voids in composite materials over the prior art. Unlike the prior art, the present invention only requires the formation of one hole or channel in the composite material, and thus minimal additional damage is caused by the repair process. Furthermore, the method of the present invention allows the creation of a complete or almost complete vacuum in the void, causing most of the air molecules to be removed from the void before the repair material is injected. Therefore, the amount of air remaining in the void after the repair material has been injected is minimized and the void is entirely or almost entirely filled with the repair material.
Other technical advantages are readily apparent to one skilled in the art from the following figures, descriptions, and claims.
BRIEF DESCRIPTION OF THE DRAWINGS
For a more complete understanding of the present invention, and for further features and advantages, reference is now made to the following description, taken in conjunction with the accompanying drawings, in which:
FIG. 1 is a cross-section of a composite material repair set-up according to teachings of the present invention;
FIG. 2 is a plan view of portions of the composite material repair set-up of FIG. 1; and
FIG. 3 is a flowchart illustrating a method of composite material repair according to teachings of the present invention.
DETAILED DESCRIPTION OF THE INVENTION
The present invention and its advantages are best understood by referring now in more detail to FIGS. 1 through 3 of the drawings.
FIGS. 1 and 2 illustrate cross-sectional and plan views, respectively, of a composite material repair set-up 10 according to one embodiment of the present invention. FIG. 3 is a flowchart illustrating a method of composite material repair according to one embodiment of the present invention. FIGS. 1-3 will be described together. Set-up 10 includes a composite material 12 having an internal void 14 . Void 14 may have been formed during the formation of composite material 12 . For example, void 14 may have been formed due to the failure of two layers of composite material to bond together in the area at which void 14 is located. Alternatively, void 14 may have been formed due to delamination between two layers of composite material 12 . Such delamination may be caused by impact to composite material 12 . The term “void” indicates any type of defect forming a cavity in composite material 12 , whether it be an air inclusion formed during the fabrication of material 12 , a interlaminar defect formed due to impact or other stress, or any other cause of a cavity within material 12 . In addition, the present invention may be used in conjunction with composite materials formed using any appropriate fabrication process.
The presence of void 14 in composite material 12 causes weakness in material 12 and may lead to a failure of material 12 . Therefore, it is preferable that void 14 be filled to strengthen material 12 . Before void 14 is repaired by filling, the location thereof is identified at step 100 of the method illustrated by the flowchart of FIG. 3 using ultrasonic equipment or any other appropriate method. After the location of void 14 is identified, a channel 16 is formed at step 102 that extends from a surface 18 of material 12 to void 14 . Channel 16 is typically formed by drilling through material 12 or by any other appropriate method. Channel 16 intersects void 14 at any point; however, it is preferable that channel 16 intersects void 14 near the center thereof.
When appropriate, channel 16 is cleaned to remove any loose material. The location of channel 16 is then identified by drawing lines 19 (illustrated in FIG. 2) on surface 18 of composite material 12 that intersect with the channel 16 . Lines 19 are needed to identify the location of channel 16 when the channel cannot be seen through the bleeder material 22 as described below. The channel locations lines 19 should be long enough to extend past the area of surface 18 that will be covered by bleeder material 22 . Alternatively, any other appropriate method of marking or otherwise determining the location of channel 16 are also included within the scope of the present invention.
After channel 16 has been formed through composite material 12 , preparations are made to create a vacuum in void 14 . In the illustrated embodiment, a vacuum bag setup is used to create a vacuum in void 14 . In this setup, bleeder material 22 is placed over channel 16 on surface 18 at step 104 . Bleeder material 22 is a thick, felt-like cloth that absorbs excess repair material 32 , described below. Bleeder material 22 also functions as a breather, providing a continuous air path for creating the vacuum in void 14 . Overlaying the bleeder material 22 is a vacuum hag 20 . Bag sealant tape 24 is placed around bleeder material 22 at step 106 . Sealant tape 24 is a putty-like material that is used to create a seal between vacuum bag 20 and surface 18 .
Vacuum bag 20 , which is typically a thick plastic material, is placed over bleeder material 22 at step 108 and is pressed in contact with sealant tape 24 at step 110 . By pressing vacuum bag 20 against sealant tape 24 , a seal is formed between bag 20 and surface 18 . Alternatively, sealant tape 24 is attached to vacuum bag 20 , and then the bag and sealant tape 24 are pressed against surface 18 . Although the present invention encompasses using any thickness of material for the vacuum bag, the vacuum bag 20 preferably has a thickness of at least 0.5 millimeters.
As illustrated in FIGS. 1 and 2, a vacuum hose 26 is inserted through vacuum bag 20 . Vacuum hose 26 is inserted through vacuum bag 20 by means of a vacuum port or any other appropriate method. A vacuum pump 27 (illustrated in FIG. 2) is attached to the vacuum hose 26 to draw or pull a vacuum through bleeder material 22 in void 14 and channel 16 at step 112 .
To locate channel 16 (either before or after forming the vacuum) a straight edge is aligned with lines 19 such that the parts of the lines obscured by the bleeder material 22 can be re-drawn on top of the vacuum bag. The point at which these re-drawn lines intersect should indicate the location of channel 16 , which is not visible through the vacuum bag and the bleeder material. Again, any other appropriate method of locating channel 16 is encompassed by the present invention.
After locating channel 16 , a syringe 28 is used to inject a repair material 32 , such as a resin or any other appropriate material, through channel 16 into void 14 at step 114 . A needle 30 attached to the syringe is inserted into the channel 16 to inject the repair material. The needle 30 is long enough to pierce bag 20 and bleeder material 22 and enter channel 16 , and has an inside diameter sufficient to allow the flow of repair material 32 into the void 14 . In one embodiment of the invention, a needle having an inside diameter of 1.0 millimeters is used, however the invention is not limited to any one needle diameter.
Before inserting needle 30 through vacuum bag 20 and bleeder material 22 , a small amount of repair material 32 may be ejected through the needle to ensure that no air bubbles are contained in the repair material inside the syringe 28 . In addition, it is preferable that a small amount of repair material 32 be ejected on top of vacuum bag 20 at the point at which needle 30 is to be inserted through the vacuum bag. This forms a small bead 34 of repair material on the surface of vacuum bag 20 thereby providing a seal to prevent air leakage around the needle 30 when inserted through bag 20 .
To fill void 14 , needle 30 is inserted through bead 34 , vacuum bag 30 and bleeder material 22 into channel 16 . As a result of the previously pulled vacuum in void 14 and channel 16 , repair material 32 is drawn into void 14 from syringe 28 . When the repair material begins to fill channel 16 after filling void 14 , vacuum pump 27 may be shut off at step 116 , allowing the vacuum head to release gradually. Slight pressure is applied to a plunger 36 of syringe 28 until repair material 32 overflows into the bleeder material 22 . Pressure is applied to overcome the friction of plunger 36 in syringe 28 and to cause repair material 32 to flow into void 14 and channel 16 . When the vacuum head is released, atmospheric pressure drives the resin into any remaining unfilled regions of void 14 . If a sufficient vacuum has been pulled in void 14 and channel 16 , these areas will be completely filled with repair material 32 .
When the vacuum head has been released, the injection process is complete. Needle 30 is removed from channel 16 , and vacuum bag 20 , bleeder material 22 and tape 24 are removed from surface 18 at step 118 . If appropriate, the repair material 32 that fills void 14 and channel 16 may be hardened by curing. Furthermore, any excess repair material 32 coming out of channel 16 onto surface 18 , may be sanded or otherwise removed from surface 18 at step 120 .
The method of the present invention results in a very high percentage of void 14 being filled with repair material 32 . It has been found through experimentation that there is an approximately one-to-one correlation between the percentage of air evacuated from void 14 and the percentage of the void volume that is filled with repair material when using the present invention. Therefore, if a sufficient vacuum is drawn in void 14 and channel 16 , these areas will be almost completely filled with repair material 32 . For example, a typical two-stage vacuum pump will evacuate more than 99.9% of the air inside of void 14 and channel 16 . In this example, since 99.9% of the air is evacuated from void 14 and channel 16 , approximately 99.9% of void 14 and channel 16 will be filled with repair material after the process is complete. Since virtually all of the air molecules are removed from void 14 and channel 16 before repair material injection begins, there is virtually no air entrapment in void 14 and channel 16 . This ensures that composite material 12 will regain the greatest possible amount of strength after the repair process is complete. In addition, since the process described above requires only one channel 16 , the loss of material strength caused by the repair process is minimized.
Although the present invention has been described with selected embodiments, a myriad of changes, variations, alterations, transformations, and modifications may be suggested to one skilled in the art, and it is intended that the present invention encompass such changes, variations, alterations, transformations, and modifications as fall within the spirit and scope of the appended claims.
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A method for repairing a composite material having an internal void includes identifying the location of the internal void and forming a single channel extending from a surface of the composite material to the internal void. The method further includes pulling a vacuum in the internal void and inserting a repair material through the channel into the internal void.
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CROSS-REFERENCE TO RELATED APPLICATIONS
The present application claims priority of 10 2014 005 533.7, filed Apr. 16, 2014, the priority of this application is hereby claimed and this application is incorporated herein by reference.
BACKGROUND OF THE INVENTION
The invention relates to a method for holding together a blow mold of multipiece design of a blowing station. Furthermore, the invention relates to a blowing station for a blowing machine, and also to a blowing machine.
Blowing machines for the blow molding of containers consisting of a thermoplastic material have been known for quite some time in the prior art. The containers are molded by the action of blowing compressed air in so-called blow molds. The cavity inside a blow mold forms the female mold for the container which is to be produced. In blowing machines, which work according to the principle of rotary machines, the blow molds are arranged at blowing stations which are located in the region of blowing wheels. In order to blow a container inside a blow mold, the blow mold is first of all opened and a so-called preform inserted in the blow mold. Blow molds usually consist of a plurality of segments, especially three segments, specifically typically consisting of a mold bottom and two side halves with a semi-cylindrical base contour. These blow mold segments are as a rule detachably fastened on stable blow mold carriers. The detachability enables an exchange of molds if a change is to be made from one bottle type to another bottle type which is to be produced.
For opening and closing the blow mold, the blow mold segments are moved. Typically, it involves the capability of opening up the side sections in the manner of a book and a lifting and lowering of the mold bottom. Other movements are also possible. The basic construction of a blowing station with blow mold carriers and a multipiece blow mold is described in EP 1 919 690 B1, for example.
On account of the high pressures which prevail inside the blow mold during a blow molding process, there is a necessity for locking mechanisms for the closing and clamping of the blow mold, which ensure a lock which is tight and secured against inadvertent opening of the blow mold. Such locking mechanisms are known under the term mold clamp, for example.
It is known to pressurize a mold clamp for the clamping of the blow mold with a blowing pressure, which is provided for the blowing of the containers, in parallel with the pre-blowing and final blowing of a container. That is to say, if compressed air flows into the preform, then compressed air also flows into the mold clamp. It is also known that the mold clamp is pressurized with compressed air independently of the pressurizing of the preform, retained in the blow mold, with pre-blowing air or final blowing air. To this end, provision is made, for example, for a separate valve which is electromagnetically actuated, for example. Via the actuating of this electrically operated valve, the duration of blowing pressure application to the mold clamp can be freely selected. This is preferably used in the case of blowing methods in which the duration and the force of the clamping has to be controlled independently of the blowing pressure.
If the mold clamp is pressurized with blowing pressure in parallel with the pre-blowing and final blowing, it is disadvantageous that the development of force which is generated via the blowing air in the mold clamp lags behind a rapidly developing container bubble in the blow mold. In this case, the container material can be squeezed into not yet fully closed mold gaps between the segments of the blow mold and a so-called parting line is created, which corresponds to a material surplus on the outer wall of the blown container in the region of the mold gaps. Containers with a parting line are usually treated as scrap or considered to be defective.
In the case of conventionally operated mold clamps, it has been shown to be disadvantageous that with an unfavorable ratio of the holding volume of the mold clamp in relation to the volume of the container which is to be produced frequently leads to the occurrence of parting lines. The introduction of blowing air into the preform with simultaneous introduction of the blowing air into the mold clamp occasionally leads to the preform quickly expanding and already butting against the walls of the blow mold before the mold clamp closes the mold gaps between the segments of the blow mold. It occurs for example because the feed line cross section for the introduction of the blowing air into the preform is considerably larger for constructional reasons than the feed line cross section of the mold clamp. The different feed line cross sections, with equal inlet pressure, lead to different volumetric flows and therefore to filling of the preform or of the mold clamp at a different rate. This especially makes itself felt in the case of blow molding of small containers in which the holding volume is small compared with the volume of the mold clamp.
A blowing station with a pneumatic mold clamp is known from DE 10 2011 110 962 A1, in which a supply pressure for the mold clamp is tapped from a pneumatic supply line of the blowing station.
SUMMARY OF THE INVENTION
The invention is based on the object of disclosing a method and a device by means of which the holding together of a closed blow mold in a simple and robust form is made possible. A reliable mold clamp is to be ensured and the occurrence of parting lines is to be counteracted.
The method according to the invention is distinguished by the fact that the mold clamp is pressurized at least at times with compressed air from a control compressed air line. Previously, it was customary to extract the compressed air required for the mold clamp from the blowing compressed air supply and to introduce it into the mold clamp either at the same time with the pressurizing of the preform or using a separate control valve. Before introducing blowing compressed air into the preform, control compressed air can already be directed into the mold feed line, however, without a separate switching valve necessarily being used because before commencement of the introduction of blowing pressure a vent valve is first of all to be closed as a rule by the control compressed air and in the process it can also be directed into the mold clamp. According to the invention, it is therefore made possible in a simple manner to pressurize the mold clamp with compressed air at an early stage.
In accordance with the invention is a method for holding together, in its closed state, a blow mold of multipiece design of a blowing station using a compressed air-operated mold clamp exerting a holding-together force, wherein the mold clamp is pressurized with compressed air for the purpose of and for the duration of the generation of the holding-together force, wherein the blowing station has a relief valve which can be controlled by means of control compressed air from a control compressed air line, wherein the mold clamp is pressurized at least at times with control compressed air from the control compressed air line.
The relief valve can serve for the pressure relief of the mold clamp, of a compressed air line supplying the blowing station and/or of the blow mold or of the container produced in the blow mold. Compressed air lines supplying the blowing station can be a control compressed air line or a blowing air pressure line, for example.
The mold clamp in this case is advantageously pressurized at least at times with blowing compressed air from the blowing compressed air line. This can be advantageous or even necessary if the pressure of the blowing compressed air is higher than the control pressure and, for example, an attempt is made to pressurize the blow mold in the final blowing phase. It is then possible to additionally or alternatively direct blowing compressed air into the mold clamp.
Preferably, the pressurizing is first carried out with the control compressed air and then with the blowing compressed air. The control compressed air in this case is to counteract the risk, existing at the beginning, of pressurizing the blow mold by the initially flowing-in pre-blowing air, whereas the blowing compressed air which is introduced into the mold clamp counteracts the later risk that the pressure inside the blow mold exceeds the clamping force which is applied by the mold clamp.
The pressurizing of the mold clamp with the control air is advantageously carried out at the latest at the point in time —preferably even with a time interval in advance—at which the blowing compressed air flows into a preform which is accommodated in the blow mold. The lagging behavior of the clamp which is described for the prior art can consequently be reliably avoided. In this case, the pressurizing with control compressed air and with blowing compressed air is preferably not carried out at the same time but one after the other in respect to time, e.g. first of all with control compressed air, then with blowing compressed air.
The switching between the pressurizing with control air and the pressurizing with blowing compressed air can be conducted in different ways, e.g. using at least two control valves which control the respective feeds of the control compressed air and of the blowing compressed air into the mold clamp. Preferably, however, this is carried out via a changeover valve which minimizes the circuitry cost and enables a simple retrofit capability of existing systems in a constructionally simple manner.
In this case, for example the changeover valve on a first inlet side is advantageously connected in a communicating manner to a control compressed air line, on a second inlet side to the blowing compressed air line, and on the outlet side to the mold clamp. In this way, a changeover is automatically carried out at the point in time at which the blowing compressed air exceeds the pressure of the control compressed air.
The invention furthermore relates to a blowing station for a blowing machine for the blow molding of containers from preforms consisting of a thermoplastic material, with a blow mold of multipiece design and with a compressed air-operated mold clamp for holding together the blow mold in its closed state, wherein the mold clamp is designed for implementing a method according to one of the preceding claims. That is to say, provision is made for the necessary actuating elements and pipelines to implement the method according to the invention. The advantages are gathered from the advantages according to the method and described above.
The method according to the invention and the device according to the invention are designed in such a way that after the closing of an especially multipiece blow mold they hold the segments of the blow mold in a closed position by exerting a clamping force. As a result of the clamping force, development of gaps between reciprocally movable parts of the blow mold is prevented or avoided. During the clamping of the blow mold, the effect of high pressure forces—which arise during the blowing of a container from a preform inside the blow mold—pushing apart the blow mold segments is also avoided. The clamping of a blow mold therefore especially includes the exertion of a clamping force upon a closed blow mold. The clamping force is created by the mold clamp and especially by the feed of compressed air into the mold clamp.
Also in accordance with the invention is a blowing station for a blowing machine for the blow molding of containers from preforms consisting of a thermoplastic material, with a blow mold of multipiece design and with a compressed air-operated mold clamp for holding together the blow mold in its closed state, wherein the blowing station has a relief valve which can be controlled by means of control compressed air from a control compressed air line, wherein the mold clamp is connected, or can be connected, to the control compressed air line in a communicating manner.
According to the invention, the mold clamp can be operated with blowing compressed air and with a retention air which is provided independently from the blowing compressed air. This is exemplified based on the control compressed air. If alternative compressed gas sources should be available, these alternative compressed gas sources may also be used.
Also in accordance with the invention is a blowing machine for the blow molding of containers from preforms consisting of a thermoplastic material with a blowing station of the aforesaid type according to the invention. The advantages of the blowing machine are gathered from the advantages according to the method and mentioned in relation to the blow mold.
The invention has the added advantage that at least two fluids which are independent of each other can be used for the operation of the mold clamp. By using a fluid which is independent of the blowing air an early development of force of the mold clamp can be initiated in a simple manner, especially if blowing air for the molding of a container is not yet directed into the blow mold or into the preform contained therein. For the adjustable feed of fluids to the mold feed line for the purpose of its operation, an actuating element of the subsequently described type can be used. Such an actuating element has at least two inlets and one outlet in a preferred design. The inlets can preferably be pressurized with blowing air on one side and with retention air on the other side. This retention air can be control compressed air, for example, as described previously. For feeding a fluid to the mold clamp, the outlet of the actuating element is connected to the mold clamp.
It is conceivable that the mold clamp can be operated with other fluids in addition to a blowing air and a retention air, e.g. the control compressed air. For this, the actuating element can have more than two inlets so that in addition to a blowing air and/or to a retention air another fluid, with which the mold clamp can be operated, can also be directed to said mold clamp.
The actuating element is preferably designed so that it connects one of the inlets in each case to the outlet for the passage of a fluid. In the case of this embodiment, the inlets are discretely connected to the outlet. Alternatively or additionally, the actuating element can be designed to connect the outlets in a continuous manner to the outlet. This continuous principle of operation leads to the advantage that a fluid mixture with an adjustable ratio of the fluids applied to the inlets of the actuating element can be directed to the outlet of the actuating element and therefore to the mold clamp. Both in the case of the discrete connection and in the case of the continuous connection, first inlets, or a first inlet, can be connected to the outlet and the remaining inlets can be shut off in a fluidtight, especially gastight, manner. The shutting off of inlets prevents an undesirable drain of a fluid via an inlet. In one simple embodiment, check valves can be provided in the actuating element for shutting off the inlets.
The actuating element is preferably designed so that it directs only one of the fluids to the mold clamp, especially either blowing air or control compressed air, which are applied to its inlets. More preferably, the actuating element is designed so that of the fluids being applied to its inlets it directs the fluid with the highest pressure level to the mold clamp. Alternatively or additionally, the actuating element can be designed to direct blowing air or retention air, especially at the same pressure level or only slightly different pressure levels, to the mold clamp at the same time.
The retention air is preferably extracted from a fluid source in the pneumatic system of a blowing machine, especially in the proximity of the blowing station.
In a preferred embodiment, the retention air is a control air which is provided for the actuation of valves which are arranged in the region of the blowing station. This control air can, for example, be a fluid which is provided for the switching of a vent valve which is arranged in the region of a blowing station. To be more precise, use can therefore be made of a compressed air for the mold clamp which can be tapped in the proximity of a blowing station in an early phase of the blowing process or even before the blowing process, specifically especially before the blowing passage provided for the introduction of blowing air into the blow mold is pressurized with blowing air.
An advantageous point in time for the operation of the mold clamp is, for example, when a pilot valve is switched in order to introduce a control air, provided for the switching of a vent valve, into a fluid line in the region of a blowing station.
In an especially preferred embodiment, the actuating element is a changeover valve. A changeover valve is known from the prior art as a pneumatic or hydraulic valve with at least two inlets and one outlet. If at least one of the inlets is pressurized with a fluid, this fluid is directed to the outlet of the changeover valve and therefore to the mold clamp. It can especially be provided that in dependence upon the respective pressure level of the fluids being applied to the inlets of the actuating element, the fluid with the higher pressure level is directed to the outlet of the actuating element and therefore to the mold clamp.
In a more preferred embodiment, the actuating element has a non-electrical drive. This has the advantage that a blowing station can be equipped with the mold clamp according to the invention in a simple manner. If an electrically operated actuating element is dispensed with, the adaptation or adjustment of the electric control of the blowing machine or of the blowing station can especially be dispensed with. An actuating element with mechanical drive is robust, inexpensive and low on maintenance.
The previously described blowing station according to the invention and/or the blowing machine according to the invention is, or are, especially designed for implementing the method according to the invention described in the introduction.
The various features of novelty which characterize the invention are pointed out with particularity in the claims annexed to and forming a part of the disclosure. For a better understanding of the invention, its operating advantages, specific objects attained by its use, reference should be had to the drawings and descriptive matter in which there are illustrated and described preferred embodiments of the invention.
BRIEF DESCRIPTION OF THE DRAWING
In the drawing:
FIG. 1 shows a block diagram of a compressed gas supply in the region of a blowing station and a device according to the invention for closing off a blow mold, and
FIG. 2 shows a schematic view of a mold clamp according to the invention.
DETAILED DESCRIPTION OF THE INVENTION
FIG. 1 schematically shows a block diagram of a compressed gas supply in the region of a blowing station and a device 10 according to the invention for closing a blow mold 12 . The device 10 according to the invention is equipped with a mold clamp 14 which is connected via a fluid line to an actuating element 16 .
The actuating element 16 preferably has three ports. Via a first port, the actuating element 16 is connected to the mold clamp 14 , as described. Via a second port, the actuating element 16 can be connected to a blowing air line 24 . The blowing air line 24 conducts the blowing compressed air P 1 , P 2 which is provided for the blowing of a container from a preform. The mold clamp 14 can therefore be pressurized with blowing compressed air P 1 , P 2 via the actuating element 16 . In an end region, the blowing air line 24 can be connected to a blow mold 12 . Via this connection, the blowing compressed air P 1 , P 2 can be directed into the blow mold 12 for the blowing of a container. Via a third port, the actuating element 16 can be connected to a valve 36 via which it can be pressurized with a control air S which is independent of the blowing compressed air P 1 , P 2 . It is conceivable that alternatively or additionally a retention air, which is independent of the control air S and of the blowing compressed air P 1 , P 2 , is fed to the actuating element and is provided for continuing to the mold clamp and for its operation (not shown).
A pressure transducer 18 for measuring the pressure level of the blowing compressed air P 1 , P 2 can be connected to a fluid line between the actuating element 16 and the blowing air line 24 .
Via the valve 28 shown in FIG. 1 , blowing compressed air P 2 can be introduced into the blowing air line 24 . The valve 28 can be switched for example via the switching valve 30 between an open position and a closed position. To this end, the switching valve 30 is first of all opened. The fluid which is directed through the valve 30 is directed to the valve 28 and switches this into the open position. According to the aforesaid principle, the valve 26 can also be switched via a switching valve 34 . Via the valve 26 , blowing air P 1 can be directed into the blowing air line 24 . A restrictor device 32 for regulating the gas flow is preferably provided upstream of the valve 26 .
In FIG. 1 , it is apparent at the designation 20 that the blowing air line 24 can be connected to a vent valve 22 . Via the vent valve 22 , the blowing compressed air P 1 , P 2 can preferably be discharged to the environment via a silencer 38 . The blowing air line 24 can be vented in this way. A vent valve is also referred to as a relief valve.
The blowing cycle usually starts with the closing of the vent valve 22 . This can be achieved by the opening of the valve 36 . With the opening of the valve 36 , the valve 22 is pressurized with control compressed air, as a result of which the vent valve 22 is operated into its closed position. In a following step, the control air S, which can be used especially for the switching of the vent valve 22 , preferably flows via the actuating element 16 to the mold clamp 14 of the device 10 . By means of this pressure application, force can be applied to the blow mold 12 early, that is to say, for example, before or at the commencement of a pressure buildup in the blowing air line 24 . After commencement of the blow molding process, that is to say after introducing blowing compressed air P 1 , P 2 into the blowing air line 24 , the actuating element 16 preferably switches over from control air S or retention air to blowing compressed air P 1 , P 2 . The actuating element 16 especially switches over when the pressure level of the blowing compressed air P 1 , P 2 at the actuating element 16 is higher than the pressure level of the control air S or retention air being applied at the actuating element 16 .
The pressure level of the control air S or retention air, at the commencement of container bubble development in the blow mold 12 —e.g. when the blow mold 12 is pressurized with the blowing compressed air P 1 —can be higher than the pressure level of the blowing compressed air P 1 in the blowing air line 24 . It is therefore assumed that the changeover of the actuating element 16 from control air S or retention air to blowing compressed air P 1 , P 2 is carried out only, or at the earliest, with the introduction of blowing compressed air P 2 into the blowing air line 24 .
For the sake of completeness, it may be mentioned that connecting points between fluid lines for the distribution of the compressed gas which is conducted in the lines are shown in FIG. 1 as diamonds—as identified by the designation 20 , for example. Intersecting lines without a connection are shown with a break in a cutting line—as identified by the designation 40 , for example.
It is understood that the supply lines and connecting points between the components are preferably of a gastight construction. A device 10 with a mold clamp 14 and an actuating element 16 can be in accordance with the invention. Also in accordance with the invention can be a system which consists of a device 10 with a mold clamp 14 and a selection of components of FIG. 1 .
FIG. 2 shows a schematic view of a mold clamp 10 according to the invention from FIG. 1 in simplified form. As shown, the mold clamp 14 , designed as a working cylinder, of the device 10 is connected by means of a fluid line 44 to an actuating element 16 . The actuating element 16 preferably has a feed for a retention air S and a feed for a blowing compressed air P 1 , P 2 . If the mold clamp 14 is pressurized with a fluid via the fluid line 44 , it can be provided that the mold clamp 10 tensions segments 46 , 48 of a blow mold 12 against each other or presses the segments 46 , 48 of the blow mold against each other. Pressing the segments 46 , 48 against each other ensures a tight closure of the blow mold 12 so that the blow mold 12 , under the load of high blowing air pressures inside the blow mold 12 , is not inadvertently opened during the blow molding process and development of a gap between segments 46 , 48 of the blow mold 12 is prevented or avoided. Naturally, the blow mold 12 can consist of additional segments, e.g. two mold halves and a bottom segment (not shown).
The arrows A and B in FIG. 2 schematically show the displacement of a first segment 46 of a blow mold 12 in relation to a second segment 48 . In the direction of the arrow A, the blow mold 12 is closed. In the direction of the arrow B, the blow mold is opened. The bridge 42 schematically shows a stationary arrangement of the segment 48 in relation to a housing of the mold clamp 14 . By means of the bridge 42 , the segment 48 can therefore be connected to a housing of the device 10 or of a mold clamp 14 in a form-fitting and/or force-applied manner. As especially shown in FIG. 2 in a simplified manner, the device 10 in a simple variant can have a mold clamp 14 , designed as a working cylinder, with a pressure cylinder and a piston for displacement of a segment 46 of the blow mold 12 . Other embodiments, which fall within the concept of the subjects requiring protection, are conceivable.
While specific embodiments of the invention have been shown and described in detail to illustrate the inventive principles, it will be understood that the invention may be embodied otherwise without departing from such principles.
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A method for holding together, in its closed state, a blow mold of multipiece design of a blowing station for the blow molding of containers from preforms made of a thermoplastic material using a compressed air-operated mold clamp exerting a holding-together force. The mold clamp is pressurized with compressed air for the purpose of and for the duration of the generation of the holding-together force. The blowing station has a relief valve which can be controlled by control compressed air from a control compressed air line. The mold clamp is pressurized at least at times with control compressed air from the control compressed air line.
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This application claims priority to German Patent Application DE 10 2004 030 597.8 filed Jun. 24, 2004, the entirety of which is incorporated by reference herein.
BACKGROUND OF THE INVENTION
The present invention relates to a turbomachine in accordance with the features described below.
More particularly, this invention relates to a turbomachine with at least one stator and at least one downstream rotor, with the stator being provided with stationary stator blades and the rotor comprising several rotor blades attached to a rotating shaft. A casing exists which confines the passage of fluid through the rotor and the stator in the outward direction.
The aerodynamic loadability and the efficiency of turbomachines, for example, blowers, compressors, pumps and fans, is limited especially by the growth and the separation of boundary layers in the rotor tip area near the casing wall. The state of the art only partly provides solutions to this problem. While various concepts for the fluid supply on turbine blades exist, these are not applicable to turbomachines since they primarily serve for surface cooling, not for boundary layer energization. For rotors, a concept exists for the supply of air on the hub and casing via axially symmetrical slots to influence the wall boundary layers there. Finally, publications exist showing concepts in which rotors are blown by individual nozzles near the casing to favorably influence the radial gap flow there. Accordingly, the general concept of influencing the boundary layer by blowing in or supplying fluid is provided in the state of the start, but the known solutions are trivial, only partly effective and very limited in their practical applicability.
FIG. 1 shows a schematic representation of the state of the art of in-service turbomachinery in the example of a multi-stage configuration. The figure schematically shows a hub 1 and a casing 2 between which a fluid flow passes from the left-hand side, as indicated by the arrow 3 . Furthermore, the figure illustrates two and a half stages of a multi-stage turbomachine in cutout view, here beginning with a stator 4 and ending with a stator 6 . Arranged between the stators are the rotors 7 and 8 . The first stators 4 , 5 shown are variable ( 10 ) to provide for an adequate operating range of the turbomachine. In support of this and serving the same purpose, a fluid bleeding device 9 is provided between the stages. These design features incur high cost and constructional effort.
The state of the art is disadvantageous in that realizable turbomachines involve considerable cost and constructional effort to ensure an adequately wide operating range, in particular, at partial load. Simple existing concepts for blowing rotor tips are not compatible with a multi-stage design since they require additional space and do not satisfy the demands of operational safety.
BRIEF SUMMARY OF THE INVENTION
A broad aspect of the present invention is to provide a turbomachine of the type specified above which, while avoiding the disadvantages of the state of the art, is characterized by exercising a highly effective influence on the boundary layer due to a controlled and well-positioned creation of a peripheral jet and by high efficiency.
It is a particular object of the present invention to provide solution to the above problems by a combination of the characteristics described herein. Further advantageous embodiments of the present invention will become apparent from the description below.
The present invention accordingly provides means for the creation of a peripheral jet in the area of at least one stator vane by way of at least one nozzle issuing fluid at the radially outer boundary of a main flow path.
The present invention therefore relates to turbomachines, such as blowers, compressors, pumps and fans of the axial, semi-axial and radial type. The working medium or fluid may be gaseous or liquid.
The turbomachine according to the present invention can comprise one or several stages, each with one rotor and one stator.
According to the present invention, the rotor includes a number of blades which are connected to the rotating shaft of the turbomachine and impart energy to the working medium. The rotor can feature a free blade end or be provided with a shroud on the casing. According to the present invention, the stator includes a number of stationary blades with fixed blade ends on the casing side.
According to the present invention, the turbomachine may be provided with a special type of stator upstream of the first rotor, a so-called inlet guide vane assembly.
In accordance with the present invention, at least one stator or inlet guide vane assembly, instead of being fixed, can be rotatably borne to change the angle of attack. A shaft accessible from the outside of the annulus can, for example, accomplish such a variation.
The turbomachine may, in a special form, also be provided with at least one row of variable rotors.
In accordance with the present invention, the turbomachine may alternatively also have a bypass configuration, with the single-flow annulus dividing into two concentric annuli behind a certain blade row, with each of these annuli housing at least one further blade row.
More particularly, the present invention provides for a turbomachine which comprises means for the creation of a peripheral jet in the area of at least one vane of a stator row such that the exit opening (nozzle) required for the creation of the jet at the outer boundary of the main flow path is embedded in a stator component or is at least partly confined by a stator component.
BRIEF DESCRIPTION OF THE DRAWINGS
The present invention is more fully described in light of the accompanying drawings showing preferred embodiments. In the drawings,
FIG. 1 is a schematic representation of the state of the art,
FIG. 2 is a schematic representation of the basic concept in accordance with the present invention,
FIGS. 3-6 show different variants and configurations of the turbomachine in accordance with the present invention,
FIGS. 7 a - 7 b show an arrangement in accordance with the present invention with stator-embedded nozzle (wall-flush) and fluid supply via the stator root, meridional view and perspective view of the stator,
FIGS. 8-11 show an arrangement in accordance with the present invention with stator-embedded nozzle (wall-flush) and fluid supply via the stator root, view A-A in FIG. 7 a,
FIGS. 12-15 show an arrangement in accordance with the present invention with stator-embedded nozzle (protruding) and fluid supply via the stator root, meridional view and perspective view of stator variants,
FIG. 16 shows an alternative arrangement in accordance with the present invention with stator-embedded nozzle (protruding) and fluid supply via the stator root, meridional view,
FIGS. 17-20 show an alternative arrangement in accordance with the present invention with stator-embedded nozzle (protruding) and fluid supply via the stator root, view A-A in FIG. 16 ,
FIGS. 21-22 show an alternative arrangement in accordance with the present invention with stator-embedded nozzle (protruding) and fluid supply via the stator root, perspective view of stator variants,
FIGS. 23-24 show an arrangement in accordance with the present invention with stator-embedded nozzle (wall-flush) and fluid supply via the actuating shaft of the stator, meridional view and perspective view of the stator,
FIGS. 25-26 show an arrangement in accordance with the present invention with stator-embedded nozzle (protruding) and fluid supply via the actuating shaft of the stator, meridional view and perspective view of the stator,
FIGS. 27-29 show an arrangement in accordance with the present invention with stator-adjacent nozzle (wall-flush) and fluid supply via the stator root, meridional view and perspective view of stator variants,
FIG. 30 shows an arrangement in accordance with the present invention with stator-adjacent nozzle (protruding) and fluid supply via the stator root, meridional view,
FIGS. 31-32 show an arrangement in accordance with the present invention with stator-adjacent nozzle (wall-flush) and fluid supply via the casing periphery, meridional view and perspective view of the stator,
FIG. 33 shows an arrangement in accordance with the present invention with stator-adjacent nozzle (protruding) and fluid supply via the casing periphery, meridional view,
FIG. 34 shows a wall-flush type of nozzle with direct mouth at the main flow path,
FIG. 35 shows a wall-flush type of nozzle with overshooting mouth at the main flow path.
DETAILED DESCRIPTION OF THE INVENTION
FIG. 2 shows a highly simplified illustration of the inventive solution by way of a cutout of a multi-stage turbomachine. The core of the inventive solution is the device for the creation of a fluid jet which originates at the periphery of the main flow path and essentially parallels the casing, with this device being provided in the area of at least one stator 4 and constructionally integrated into the design of the stator (stator-integrated peripheral jet creation 11 ). This functional unit may, in a particular form according to the present invention, connect to, and be fed from, a point located further downstream in the main flow path (e.g. a chamber 13 for interstage bleed) via a flow passage (line 12 ). In a further particular form, a freely designable filter device 14 is provided in the route of the return line. In another particular form, a throttling device 15 or a controllable valve is provided in the route of the return line. This can be actuated by a mechanism of existing variable stators, as indicated by the broken arrow. In still another particular form, control of the valve 15 is provided by way of a freely designable, mechanical or hydraulic connection to an existing mechanism 16 for the actuation of variable stators. Thus, control can be effected in a simple way in dependence of the rotor speed.
FIGS. 3-6 show four of a multitude of possible configurations of the turbomachine according to the present invention. Shown is an annulus which is flown from the left to the right-hand side and the machine axis 18 around which a rotor drum (hub 1 ) rotates. In the examples shown in FIGS. 4 and 6 , a further rotor drum (hub 1 ) is provided. The rotors, stators and the inlet guide vane assembly are each shown in schematic representation.
FIGS. 7 a and 7 b show an inventive arrangement of a stator 4 with a subsequent rotor 7 , surrounded by a casing 2 . Accordingly, the figure shows an arrangement with stator-embedded nozzle (wall-flush) and fluid supply via the stator root in meridional view and a three-dimensional view of the stator. The stator 4 is firmly connected to the casing 2 . In the representation selected, the rotor 7 has a running gap between its blade tips and the casing 2 , however, the present invention also provides for rotor designs with tip-shrouded blades. The stator root 19 and the casing 2 form a fluid supply chamber 20 which issues into the main flow path via a flow passage and a nozzle 21 . Here, the nozzle 21 is completely embedded into the stator component and has a wall-flush configuration with particularly low flow disturbance. Accordingly, fluid flows from the supply chamber 20 via the vane root (stator root 19 ) into the main flow path and towards the tip of the rotor 7 . For further clarification, a stator vane is shown in perspective view on the right side of the figure. The leading edge is designated with reference numeral 22 . In this and the following illustrations, the individual blade with root is to be considered either as a separate component or as part of a larger vane assembly.
FIGS. 8-11 show various nozzle arrangements enabled by the present invention in meridional section A-A (a plane formed by meridional direction m and circumferential direction u) with view onto the vane root (stator root 19 ). Accordingly the figure shows an arrangement with stator-embedded nozzle (wall-flush) and fluid supply via the stator root, according to the sectional view A-A of FIG. 7 a . The upper left representation applies to a meridional nozzle orientation, the upper right representation to an oblique nozzle orientation, both bottom representations apply to a sheared nozzle orientation. The nozzle 21 can a have a rectangular or a sheared layout, be positioned on the pressure side or the suction side of the profile, and be inclined in the meridional direction or against the meridional direction by the angle beta. No specification is made with regard to the root platform of the stator 4 , with a rectangular platform and an obliquely stepped platform being shown as examples. Preferably, the exit of the nozzle 21 is to be arranged near the trailing edge plane of the stator 4 . The position of the nozzle is confined by the rims of the stator root 19 . It extends over part of the circumference. In accordance with the present invention, the wall-flush nozzle 21 can either be mechanically or electrochemically machined directly into the material of the stator 4 or be created by means of inserts in the vane root (stator root 19 ).
FIGS. 12-15 show an alternative arrangement according to the present invention of a stator 4 with a downstream rotor 7 . The figure details an arrangement with stator-embedded nozzle (protruding) and fluid supply via the stator root in meridional view as well as perspective views of stator variants. As in the examples described above, fluid is supplied into the fluid supply chamber 20 . Again, the nozzle 21 is fully embedded into the stator component, but has a protruding, aerodynamically safely controllable configuration. The nozzle exit is here on the side of the vane root (stator root 19 ) looking into the main flow direction. For further clarification, various variants of a stator vane provided by the present invention are shown in perspective view on the right-hand side of the figure. Here, an elevation of the platform required for the nozzle protrusion may occur on the entire circumference or only on part of the circumference. In particular, the nozzle can be open towards one side of the stator platform (stator root) to enable connection to the root (and nozzle, if applicable) of an adjacent stator vane or stator vane assembly.
FIG. 16 shows an alternative arrangement according to the present invention in which the nozzle 21 is again fully embedded into the stator component, has a protruding configuration, but is arranged within the stator passage. Specifically, an arrangement with stator-embedded nozzle (protruding) and fluid supply via the stator root is shown in meridional view.
In correspondence with the meridional view A-A in FIG. 16 , FIGS. 17-20 shows a view (a plane formed by meridional direction in and circumferential direction u) onto the vane root (stator root 19 ) of various nozzle arrangements enabled by the present invention. More particularly, an arrangement with embedded nozzle (protruding) and fluid supply via the stator root is shown. The upper left view shows a meridional nozzle orientation, the upper right view an oblique nozzle orientation, and the two bottom views show a sheared nozzle orientation. The nozzle 21 can have a symmetrical or non-symmetrical layout, be positioned on the pressure side or the suction side of the profile, and be inclined in or against the meridional direction by the angle beta. No specification is made with regard to the root platform of the stator 4 , with a rectangular platform and an obliquely stepped platform being shown as examples.
FIGS. 21-22 shows two variants of the solution according to the present invention with adjacency of nozzle exit to the suction side or to the pressure side of the stator vane. The left-hand illustration shows pressure-side adjacency, while the right-hand illustration shows suction-side adjacency of the nozzle exit. The trailing edge of the stator is indicated with the reference numeral 23 , with the arrowhead 24 showing the pressure side and the arrowhead 25 the suction side.
FIGS. 23-24 shows an inventive arrangement of a variable stator with a downstream rotor, surrounded by a casing. The figure details an arrangement with stator-embedded nozzle (wall-flush) and fluid supply via the actuating shaft of the stator in meridional view as well as a three-dimensional view of the stator. Also in this example, fluid is supplied to the fluid supply chamber 20 . In the perspective representation, reference numeral 22 designates the leading edge and reference numeral 23 the trailing edge of the Stator 4 . The stator is rotatably borne within the casing. For further clarification, a stator vane is shown in perspective representation on the right-hand side of the figure. Adjacent to the actuating shaft, a fluid supply chamber is provided by the casing which issues into the main flow path via a flow passage extending through the hollow actuating shaft, the round stator root and a nozzle. Here, the nozzle is completely embedded into the stator component and has a wall-flush configuration with particularly low disturbance. Accordingly, fluid flows from the supply chamber via the vane root (stator root 19 ) into the main flow path and towards the tip of the rotor. Preferably, the nozzle exit is arranged near the trailing edge plane of the stator. Nozzle position is confined by the rims of the stator root. It extends over a part of the circumference. In accordance with the present invention, the nozzle can either be machined directly into the material of the stator by a mechanical or electrochemical process or be formed by inserts in the vane root (stator root 19 ).
FIGS. 25-26 show an arrangement with protruding nozzle of a variable stator with a subsequent rotor according to the present invention. Clarity is provided by the three-dimensional representation of the variable stator in the right-hand half of the figure. Accordingly, the figure shows an arrangement with stator-embedded nozzle (protruding) and fluid supply via the actuating shaft of the stator in meridional view.
FIGS. 27-29 shows an arrangement according to the present invention of a stator 4 with a downstream rotor 7 , surrounded by a casing. The arrangement shows a wall-flush, stator-adjacent nozzle and a fluid supply via the stator root, also in meridional view. The stator 4 is firmly connected to the casing 2 . The stator root 19 and the casing 2 form a fluid supply chamber 20 which initially connects, via an opening, to a cavity formed jointly by the stator 4 and the casing 2 . A subsequent nozzle 21 is also partly confined by the stator 4 . The nozzle 21 has a wall-flush configuration with particularly low disturbance. Accordingly, fluid flows from the supply chamber via the vane root (stator root 19 ) and the stator-adjacent nozzle 21 into the main flow path and towards the tip of the rotor 7 . For further clarification, two possible variants of the stator vane are shown on the right-hand side of the figure in three-dimensional representation. As can be seen, the opening in the stator root 19 required for feeding the stator-adjacent nozzle 21 is realizable either by a hole in the flank of the root or by a partial recess of the flank itself.
FIG. 30 shows an arrangement according to the present invention for the case of a protruding nozzle 21 which is arranged adjacent to the stator and is supplied with fluid via the stator root.
FIGS. 31-32 shows an arrangement according to the present invention for the case of a wall-flush, stator-adjacent nozzle 21 which is fed via a fluid supply chamber in the casing periphery.
FIG. 33 shows an arrangement according to the present invention for the case of a protruding, stator-adjacent nozzle 21 which is fed via a fluid supply chamber in the casing periphery.
It is particularly advantageous if the wall-flush nozzle 21 is designed to further rules. FIG. 34 shows a highly enlarged representation of the nozzle mouth at the main flow path. Accordingly, the left-hand contour of the nozzle should be inclined to the annulus contour by an angle gamma <80°. The resultant tip 26 can be left sharp-edged, be chamfered or rounded. The right-hand contour 27 of the nozzle 21 should, towards the fluid-wetted side, be completely convex between the point Q on the throat of the nozzle 21 and the point of transition into the annulus contour R. It can be particularly favorable to provide a small duct 28 , small if compared to nozzle 21 , for fluid extraction in close vicinity of point R. Reference numeral 28 indicates the nozzle throat at the end of the upstream nozzle wall.
As shown in FIG. 35 , it can be particularly favorable to allow the right-hand contour of the nozzle 21 to overshoot beyond the annulus contour to a certain degree before it connects to point R. In this case, the completely convex contour section 27 ends at point A, which is located before point R. In the case of an overshooting entrance of the nozzle 21 , a possible extraction point could be located in close vicinity of point A of the curvature change.
The inventive turbomachine accordingly provides a yet unequalled degree of space-saving peripheral flow influencing, which, moreover, enables the constructional effort and cost (less variable stators and interstage bleed) to be significantly reduced beyond a level that would required with state-of-the-art machinery to provide adequate operational safety. This is possible for various types of turbormachines, such as blowers, compressors, pumps and fans. Depending on the degree of utilisation of the concept, a reduction in cost and weight of the turbomachine between 10 and 20 percent is achievable. Furthermore, the improvement in efficiency provided by the present invention is estimated at 0.2 to 0.5 percent.
LIST OF REFERENCE NUMERALS
1 Hub
2 Casing
3 Main flow direction
4 Stator
5 Stator
6 Stator
7 Rotor
8 Rotor
9 Fluid bleeding device
10 Actuating shaft of the stator
11 Stator-integrated peripheral jet creation
12 Line
13 Chamber
14 Filter device
15 Throttling device/valve
16 Mechanism
17 Annulus
18 Machine axis
19 Stator root
20 Fluid supply chamber
21 Nozzle
22 Leading edge
23 Trailing edge
24 Pressure side
25 Suction side
26 Tips
27 Contour section
28 Duct
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A turbomachine has at least one stator ( 4 ) and at least one downstream rotor ( 7 ), with the stator ( 4 ) being provided with stationary stator blades and the rotor ( 7 ) comprising several rotor blades attached to a rotating shaft. A casing ( 2 ) confines the passage of fluid through the rotor ( 7 ) and the stator ( 4 ) in the outward direction. A mechanism for peripheral jet creation is provided in the area of at least one vane of the stator ( 4 ), with at least one nozzle ( 21 ) issuing fluid at the radially outer boundary of a main flow path.
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FIELD OF THE INVENTION
This invention relates to a toner and a developer for developing an electrostatic latent image in an electrophotographic process, an electrostatic recording process and the like, and also relates to an image forming method using the same.
BACKGROUND OF THE INVENTION
In an electrophotographic image formation process, an image is formed by developing an electrostatic latent image formed on a photoreceptor with a toner containing a colorant, transferring the toner image onto transfer paper, and fixing the toner with a heat roll, etc. The photoreceptor is cleaned for the next cycle of electrostatic image formation. Dry developers used in such electrophotography are divided into a one-component developer that is a toner itself comprising a binder resin having a colorant dispersed therein and a two-component developer comprising such a toner and a carrier mixed therewith. Upon carrying out copying operations using these developers, excellent fluidity, transportability, fixability, chargeability, transfer properties, and cleanability are required for ensuring process suitability.
To meet the demand for compact equipment for space saving, an image formation system in which a residual toner is recovered simultaneously with development to omit a cleaning step has been proposed recently (hereinafter referred to as a "cleanerless system") (see JP-A-5-94113, the term "JP-A" as used herein means an "unexamined published Japanese patent application"). This system has the disadvantage that the recovered toner is different from the other part of the toner in charging characteristics so that it is not transferred and remain in the developing unit. Therefore, the cleanerless system has been demanded to have improved transfer efficiency.
Separately, it has been proposed to make toner particles almost spherical in order to improve the fluidity, chargeability, and transfer properties. However, use of spherical or nearly spherical toner particles causes the following problems. A developing unit is equipped with a transport control plate, and the amount of a developer to be transported can be controlled by adjusting the distance between the transport control plate and a magnetic roll. The problem is that the rate of the change in the transported developer amount to the change in the distance between the magnetic roll and the transport control plate for adjusting the transported developer amount increases as the shape of toner particles approach spheres. As a result, the transported amount becomes unstable. Such a problem can be suppressed by making all toner particles shapeless, but this causes reductions in fluidity and transfer efficiency and changes in chargeability and fluidity with time due to external additive's migrating and embedding into depressions of the toner particles.
Proposals have been made to obtain a developer satisfying all the requirements for fluidity, chargeability, transportability, and transfer properties by regulating the range of the shape of toner particles. For example, JP-A-61-279864 discloses a toner, shape of which is limited so that the median of the shape index may fall within a specific range. However, even with the regulated median of the shape index, sufficient transfer efficiency cannot be secured if shapeless toner particles exceed a certain proportion. Where the shapeless particles have small size, transfer becomes more difficult.
JP-A-1-185654 teaches that the rise in toner charging and charge distribution can be sharpened by regulating the relationship between the median of the shape of a toner and that of a carrier. Taking into account the distribution of the particle diameter and particle shape, however, sufficient transfer efficiency applicable to a cleanerless system cannot be obtained if the content of small and shapeless toner particles exceeds a certain proportion. In addition, insufficient cleaning and transport are caused.
Hence, it has been proposed to regulate the proportion of nearly spherical particles in number and the proportion of shapeless particles in number to improve cleanability, developing properties, and image quality (see JP-A-6-148926 and JP-A-6-148941). Further, JP-A-8-328312 proposes achieving both desired transfer properties and image quality by making black toner particles more shapeless than the other three color toners while making the other three color toners spherical. However, transfer properties change depending not only on shape but also on size. That is, small diameter toner particles and shapeless toner particles are hard to transfer due to strong electrostatic adhesion to a photoreceptor. Therefore, if the shapeless particles have a small diameter, sufficient transfer efficiency for application to a cleanerless system cannot be obtained even though the proportion of the number of the shapeless particles is reduced.
On the other hand, in order to cope with high-speed and large number of sheets copying systems while fulfilling the recent demand for color printing, especially on-demand color printing, a system comprising forming a multi-color image on a transfer belt and transferring and fixing the multi-color image onto an image fixing material at a time has been reported (see JP-A-8-115007).
Taking the step of transferring a toner image from a photoreceptor to a transfer belt as first transfer and the step of transferring the multi-color image from the transfer belt to an image fixing material as second transfer, there remains an untransferred toner in both the first and second transfer steps, which reduces the overall transfer efficiency and, of course, necessitates a cleaning step.
Particularly in the second transfer step, where a multi-color image is transferred all at once, and the image fixing material varies, for example in the case of paper, in terms of its thickness and surface properties, it has now been an outstanding subject to improve transfer properties and cleanability of an untransferred remaining toner. In this connection, the shape of a toner has been attempted to be controlled in order to improve its fluidity, chargeability, transportability, transfer properties, and cleanability. For example, to make toner particles spherical or nearly spherical has been proposed so as to improve fluidity, chargeability, and transfer properties, but cleanability is reduced as toner particles approach spheres. While a cleanerless system has been proposed as described above, in which a residual toner is recovered simultaneously with development while bringing the transfer efficiency as close to 100% as possible, this system is difficult to apply to full color printing because four color toners would be mixed with each other.
Further, with the spread of color printers based on electrostatic latent image development, it has been desired for the printers to be applicable to not only specific paper for exclusive use but a variety kinds of paper. When common paper is used, there are tendencies that paper dust remains on a photoreceptor to interfere with latent image formation or enters a developing unit to reduce the developing performance, leading to image missing.
Since sufficient cleanability cannot be secured simply by regulating the median of a shape index, regulating the proportion of nearly spherical particles in number has been proposed (see JP-A-6-148926 and JP-A-6-148941). However, transfer properties change not only with shape but also with size as previously stated. Therefore, a toner should be designed with due consideration for both of particle shape and size in order to obtain sufficient cleanability while securing satisfactory transfer properties.
SUMMARY OF THE INVENTION
An object of the present invention is to provide a toner for electrostatic latent image development which satisfies the requirements of fluidity, chargeability, developing properties and transfer properties over an extended period of time and, which eliminates the disadvantages particularly associated with a system where a cleaning step is omitted and an untransferred remaining toner is recovered simultaneously with development.
Another object of the present invention is to provide a developer for electrostatic latent image development which contains the above toner.
A further other object of the present invention is to provide a toner for electrostatic latent image development which eliminates the disadvantages associated with a multi-color image simultaneous transfer system adopted to development, transfer and cleaning so as to cope with the demands for high-speed and large number of sheets copying and high image quality.
A still other object of the present invention is to provide a developer for electrostatic latent image development which contains the above toner.
A yet further object of the present invention is to provide an image forming method which makes it possible to produce a large number of high quality prints at a high speed.
As a result of extensive investigation, the inventors of the present invention have found that the above objects are accomplished by a toner and a developer in which toner particles have a number average particle diameter of from 3 to 10 μm, and the size distribution and the shape index of the toner particles fulfill a specific relationship. The present invention has been completed based on this finding.
That is, the present invention relates to a toner for electrostatic latent image development, which comprises toner particles comprising a binder resin and a colorant,
wherein said toner particles have a number average particle diameter of from 3 to 10 μm and satisfy relationship (1) or (2):
M.sub.50 (b)>M.sub.50 (a)>M.sub.50 (c) (1)
M.sub.50 (b)<M.sub.50 (a)<M.sub.50 (c) (2)
wherein M 50 (a) is an average shape index at a number average particle diameter D 50 which is calculated from cumulative 50% particles counting from the larger diameter side, M 50 (b) is an average shape index at a number average particle diameter D 16 which is calculated from cumulative 16% particles counting from the larger diameter side, and M 50 (c) is an average shape index at a number average particle diameter D 84 which is calculated from cumulative 84% particles counting from the larger diameter side.
The toner according to the present invention, in a first aspect, is for use in an apparatus adopting a cleanerless system, and said toner particles satisfy relationship (1). The toner in the first aspect preferably has an average shape index of 105 to 145.
The toner according to the present invention, in a second aspect, is for use in an apparatus adopting a blade cleaning system, and said toner particles satisfy relationship (2). The toner in the second aspect preferably has an average shape index of 110 to 145.
The present invention also relates to a developer for electrostatic latent image development, which comprises:
a carrier; and
a toner which comprises toner particles comprising a binder resin and a colorant,
wherein said toner particles have a number average particle diameter of from 3 to 10 μm and satisfy relationship (1) or (2):
M.sub.50 (b)>M.sub.50 (a)>M.sub.50 (c) (1)
M.sub.50 (b)<M.sub.50 (a)<M.sub.50 (c) (2)
wherein M 50 (a) is an average shape index at a number average particle diameter D 50 which is calculated from cumulative 50% particles counting from the larger diameter side, M 50 (b) is an average shape index at a number average particle diameter D 16 which is calculated from cumulative 16% particles counting from the larger diameter side, and M 50 (c) is an average shape index at a number average particle diameter D 84 which is calculated from cumulative 84% particles counting from the larger diameter side.
The developer according to the present invention, in a first aspect, is for use in an apparatus adopting a cleanerless system and said toner particles satisfy relationship (1).
The developer according to the present invention, in a second aspect, is for use in an apparatus adopting a blade cleaning system and said toner particles satisfy relationship (2).
The carrier used in the first and second aspect developers preferably has a resin coat.
The present invention further relates to an image forming method comprising the steps of:
(i) forming a latent image on a latent image holding member;
(ii) developing said latent image with a developer comprising a toner to form a toner image; and
(iii) transferring said toner image to a receiving member,
wherein said toner comprises toner particles comprising a binder resin and a colorant, and
wherein said toner particles have a number average particle diameter of from 3 to 10 μm and satisfy relationship (1) or (2):
M.sub.50 (b)>M.sub.50 (a)>M.sub.50 (c) (1)
M.sub.50 (b)<M.sub.50 (a)<M.sub.50 (c) (2)
wherein M 50 (a) is an average shape index at a number average particle diameter D 50 which is calculated from cumulative 50% particles counting from the larger diameter side, M 50 (b) is an average shape index at a number average particle diameter D 16 which is calculated from cumulative 16% particles counting from the larger diameter side, and M 50 (c) is an average shape index at a number average particle diameter D 84 which is calculated from cumulative 84% particles counting from the larger diameter side.
In a first aspect of the image forming method according to the present invention, said toner particles satisfy relationship (1), and an untransferred remaining toner is recovered simultaneously with the development.
In a second aspect of the image forming method according to the present invention, said toner particles satisfy relationship (2), and a toner remaining on the latent image holding member is cleaned off by blade cleaning.
The toners according to the present invention satisfy all the requirements of fluidity, chargeability, developing properties, and transfer properties over an extended period of time. In particular, the first aspect toner for use in a cleanerless system eliminates the outstanding problems arising from untransferred remaining toner particles, and the second aspect toner eliminates the outstanding problems associated with blade cleaning when applied to a multi-color image transfer system of development, transfer and cleaning which meets the demands for producing a large number of copies and for high image quality. Therefore, the developer of the present invention comprising the toner of the present invention makes it possible to form a large number of prints with high image quality at a high speed.
DETAILED DESCRIPTION OF THE INVENTION
The terminology "average shape index" used for toner particles means a value, ML 2 /A, calculated according to the following equation:
ML.sup.2 /A=(maximum length).sup.2 ×π×100/(area×4)
In the case of a complete sphere, the average shape index ML 2 /A is 100. In practice, an average shape index can be obtained by inputting the image of a toner under an optical microscope into an image analyzer (LUZEX III manufactured by Nireco Corporation), measuring the circle-equivalent diameters, and calculating ML 2 /A for every particle from its maximum length and area.
The first aspect toner, which satisfies relationship (1), i.e., M 50 (b)>M 50 (c)>M 50 (c), and preferably has an average shape index of 105 to 145, provides a developer counterbalancing the disadvantages of shapeless particles and spherical particles while taking full advantage of both types of particles. As to fluidity, spherical particles act as a fluidity assistant, compensating for the poor fluidity of shapeless particles and for the change of the state of adhesion of an external additive to shapeless particles, and nearly spherical particles retain satisfactory fluidity over a prolonged period of time because they scarcely have depressions into which an external additive, such as a fluidity imparting agent, may fall or buried by mechanical impact. Additionally, nearly spherical particles undergo less change in chargeability and maintain stable chargeability for a long time.
As for transfer properties, large diameter particles and nearly spherical particles have weak adhesion to a photoreceptor and are transferred easily. In the first aspect toner, shapeless particles have a relatively large diameter and are transferred easily. Even small diameter particles can be transferred easily by making their shape near to spheres. Having a nearly spherical shape, small diameter particles hardly cause external additives, such as an agent for imparting chargeability, an agent for imparting fluidity, and an agent for imparting transfer properties, to fall into depressions thereof or be buried therein by mechanical shock in a developing unit and therefore maintain satisfactory transfer properties for a prolonged period of time.
Further, since small diameter and spherical toner particles have weak adhesion to a photoreceptor and hardly cause changes with time of external additives, cleanability in a developing unit is improved so that a non-recovered toner remaining on a photoreceptor, if any, does not deteriorate image quality.
With regard to chargeability, large diameter particles have a reduced probability of contact with a carrier or a sleeve so that they produce an extremely small charge quantity per unit weight, showing a broad charge distribution. As a result, they tend to cause selective development. Now by making the shape of small diameter particles near to a sphere, the probability of contact with a carrier can be increased over that of shapeless particles thereby narrowing the charge distribution. Further by making the shape spherical, the non-static adhesion to a carrier or a sleeve is diminished thereby achieving development even if the charge quantity is smaller than that of shapeless particles. Thus, occurrence of selective development can be suppressed by controlling the shape and size distribution according to the present invention.
With reference to image quality, fine line reproducibility and edge reproducibility are improved by reducing the particle diameter and making the particles spherical, but particle diameter reduction leads to reduction in transfer efficiency, and making the particles spherical results in increase in rate of change of the amount of a developer transported with the change of the distance between a magnetic roll and a transport control plate, which makes the amount of transport instable. The control on the shape and size distribution according to the present invention makes it possible to provide a developer which comprises small diameter and spherical toner particles and yet exhibits stable transportability and excellent performance in transfer and reproduction of fine lines and edges. That is, there is provided a developer which is excellent in image quality, fluidity, transfer properties and suitability to a cleanerless system.
The second aspect toner, which satisfies relationship (2), i.e., M 50 (b)<M 50 (c)<M 50 (c), and preferably has an average shape index of 110 to 145, provides a developer which counterbalances the disadvantages of shapeless particles and spherical particles while taking full advantage of both particles. As to fluidity, relatively large diameter particles, whose shape is nearly spherical, act as a spacer, compensating for the poor fluidity of shapeless particles and preventing the external additives from changing the state of adhesion to the shapeless particles. Nearly spherical particles retain satisfactory fluidity over a prolonged period of time because they scarcely have depressions into which external additives such as an agent for imparting fluidity may fall or be buried by mechanical impact. Additionally, nearly spherical particles undergo less change in chargeability and maintain stable chargeability for a long time.
As for transfer properties, relatively large diameter and nearly spherical particles have weak adhesion to a photoreceptor or a transfer belt and are transferred easily. It is a generally observed phenomenon that shapeless particles cause external additives, such as an agent for imparting chargeability, an agent for imparting fluidity, and an agent for imparting transfer properties, to migrate into depressions thereof or be buried therein by mechanical impact in a developing unit and therefore impair transfer properties. In the present invention, because the relatively large particles have a nearly spherical shape, they function as a spacer effective in preventing such a phenomenon thereby maintaining the transfer properties for a long period of time.
As for cleanability, large diameter particles and spherical particles, both having weak adhesion to a photoreceptor or a transfer belt, are transferred easily, and shapeless particles remaining on a photoreceptor or a transfer belt can easily be cleaned off with a rubber-made cleaning blade. If any particles having a relatively nearly spherical shape remain non-transferred and forwarded to the cleaning step, they are hardly deposited on the cleaning blade because toner particles which shape is relatively close to shapeless and a small diameter act like abrasive grains.
With regard to chargeability, since large diameter particles have a reduced probability of contact with a carrier or a sleeve, they produce an extremely small charge quantity per unit weight with a broad charge distribution. As a result, selective development tends to occur. By making the shape of large diameter particles near to a sphere, the probability of contact with a carrier can be increased over that of shapeless particles thereby narrowing the charge distribution. Further by making the shape spherical, the non-static adhesion to a carrier or a sleeve is diminished thereby achieving development even if the charge quantity is smaller than that of shapeless particles. Thus, occurrence of selective development can be suppressed by controlling the shape and size distribution according to the present invention.
With reference to image quality, to reduce the particle diameter and to make the particles spherical bring about improvement in fine line reproducibility and edge reproducibility but make it more difficult to satisfy both the requirements of cleanability and transfer properties. That is, large diameter particles tend to be transferred selectively, while small diameter toner particles, which are less cleanable, tend to remain on a photoreceptor. In the present invention, since the toner particles have such a shape distribution that those particles having a relatively small diameter are shapeless, such small particles can be cleaned off with ease even if large diameter particles are transferred selectively. Thus, there is provided a developer excellent in image quality, cleanability, and transfer properties.
The toner of the present invention comprises a binder resin and a colorant and has a number average particle diameter of from 3 to 10 μm. The first aspect toner which satisfies relationship (1) preferably has an average shape index (ML 2 /A) of 105 to 145. The second aspect toner which satisfies relationship (2) preferably has an average shape index of 110 to 145.
Where the average shape index is smaller than 110, the shape distribution is substantially very narrow, and there are scarcely any particles having a shape index of 130 or more, tending to fail to produce desired effects of the invention. On the other hand, it is practically difficult to produce toner particles having an average shape index greater than 145 by conventional processes. If produced by an emulsion polymerization and flocculation process, toner particles having an average shape index greater than 145 have very weak fusion bonding strength and are liable to destruction by mechanical stress in a developing unit or other units. They may be seen as effective in the initial stage of use but fail to continue manifesting their effects in the course of time.
The production process of the toner according to the present invention is not particularly limited as far as the above-described shape and size conditions are fulfilled. The toner can be made up of a single kind or two or more kinds which have different average particle diameters or average shape indices or are produced by different processes and combined so as to have the size and shape distribution satisfying relationship (1) or (2).
While not limiting, the toner satisfying relationship (1) can be obtained by, for example, mixing large diameter and shapeless particles and small diameter and spherical particles, and the toner satisfying relationship (2) can be obtained by, for example, mixing large diameter and spherical particles and small diameter and shapeless particles.
Processes for preparing the toner include: a kneading and grinding process which comprises kneading a binder, a colorant and, if necessary, additives, such as a release agent and a charge control agent, grinding the blend, followed by classification; a process comprising giving a mechanical impact or heat energy to the particles obtained by the kneading and grinding process to alter their shape; an emulsion polymerization and flocculation process consisting of emulsion polymerizing a monomer(s) to prepare a binder resin emulsion, mixing the emulsion with a dispersion of a colorant and necessary additives, causing the particles to flocculate and fuse thermally to obtain toner particles; a suspension polymerization process consisting of polymerizing a solution of a monomer(s) providing a binder resin, a colorant, and necessary additives as suspended in an aqueous medium; and a dissolution suspension process comprising suspending a solution of a binder resin, a colorant and necessary additives in an aqueous medium followed by granulation. The toner can have a core/shell structure, which is obtained by further adhering and fusion bonding flocculated particles to core particles prepared by any of the above-mentioned processes.
Examples of the binder resin for use in the present invention include homo- and copolymers of styrene, styrene derivatives, such as chlorostyrene, olefins, such as ethylene, propylene, butylene and isoprene, vinyl esters, such as vinyl acetate, vinyl propionate, vinyl benzoate, and vinyl butyrate, α-methylene aliphatic monocarboxylic acid esters, such as methyl acrylate, ethyl acrylate, butyl acrylate, dodecyl acrylate, octyl acrylate, phenyl acrylate, methyl methacrylate, ethyl methacrylate, butyl methacrylate, and dodecyl methacrylate, vinyl ethers, such as vinyl methyl ether, vinyl ethyl ether, and vinyl butyl ether, and vinyl ketones, such as vinyl methyl ketone, vinyl hexyl ketone, and vinyl isopropenyl ketone. Typical examples of these binder resins are polystyrene, a styrene-alkyl acrylate copolymer, a styrene-alkyl methacrylate copolymer, a styrene-acrylonitrile copolymer, a styrene-butadiene copolymer, a styrene-maleic anhydride copolymer, polyethylene, and polypropylene. Additional examples of useful binder resins include polyester, polyurethane, epoxy resins, silicone resins, polyamide, modified rosin, and paraffin wax.
Examples of the colorant for use in the present invention typically include magnetic powders, such as magnetite and ferrite, carbon black, Aniline Blue, Chalcoyl Blue, Chrome Yellow, Ultramarine Blue, Du Pont Oil Red, Quinoline Yellow, Methylene Blue chloride, Phthalocyanine Blue, Marachite Green oxalate, lamp black, Rose Bengale, C.I. Pigment Red 48:1, C.I. Pigment Red 122, C.I. Pigment Red 57:1, C.I. Pigment Yellow 97, C.I. Pigment Yellow 17, C.I. Pigment Blue 15:1, and C.I. Pigment Blue 15:3.
If desired, the toner can contain known charge control agents. Suitable charge control agents include azo type metal complex compounds, metal complex compounds of salicylic acid, and polar group-containing resin type charge control agents. In preparing the toner in a wet process, it is preferred to use sparingly water-soluble materials from the standpoint of ionic strength controllability and reduction of water pollution.
If desired, the toner can contain waxes, such as low-molecular polypropylene and low-molecular polyethylene, as an offset inhibitor. The toner may be either a magnetic toner containing a magnetic material or a nonmagnetic toner containing no magnetic material.
It is essential for the toner to have a number average particle diameter ranging from 3 to 10 μm, preferably 4 to 8 μm. If the number average particle diameter exceeds 10 μm, the toner fails to develop a dot and line latent image with fidelity only to have inferior reproducibility of a photographic image or fine lines. If the number average particle diameter is smaller than 3 μm, the surface area per unit weight is too large to form a stable image with difficulty in controlling chargeability and fluidity.
According to the end use, the toner particles can have inorganic fine particles as an external additive adhered thereto. Inorganic fine particles known as an external additive for a toner, such as silica, alumina, titania, calcium carbonate, magnesium carbonate, calcium phosphate, and cerium oxide, can be used. If necessary, the inorganic fine particles can be surface-treated in a usual manner.
The developer according to the present invention may be either a one-component developer mainly composed of the above-described toner or a two-component developer composed of the toner and a carrier. Known carriers can be used in the two-component developer with no particular limitation. For example, a resin-coated carrier comprising a carrier core and a resin coat is preferably used. A carrier comprising a matrix resin having electrically conductive powder dispersed therein is also useful.
The coating resin and the matrix resin used for carriers include polyethylene, polypropylene, polystyrene, polyacrylonitrile, polyvinyl acetate, polyvinyl alcohol, polyvinyl butyral, polyvinyl chloride, polyvinylcarbazole, polyvinyl ether, polyvinyl ketone, a vinyl chloride-vinyl acetate copolymer, a styrene-acrylic acid copolymer, a straight silicone resin comprising an organosiloxane bond or modified products thereof, fluororesins, polyester, polyurethane, polycarbonate, phenolic resins, amino resins, melamine resins, benzoguanamine resins, urea resins, polyamide, and epoxy resins.
Useful electrically conductive materials include metals, such as gold, silver and copper, titanium oxide, zinc oxide, barium sulfate, aluminum borate, potassium titanate, tin oxide, and carbon black.
Useful carrier cores include magnetic metals, such as iron, nickel, and cobalt, magnetic oxides, such as ferrite and magnetite, and glass beads. In order to adjust the volume resistivity in a magnetic brush development system, the carrier core is preferably made of a magnetic material. The carrier core generally has an average diameter of 10 to 500 μm, preferably 30 to 100 μm.
The resin-coated carrier is prepared by immersing core particles in a coating resin solution (immersion method), spraying core particles with a coating resin solution (spray method), spraying fluidized core particles with a coating resin solution (fluidized bed method), or mixing core particles and a coating resin solution in a kneader coater while evaporating the solvent (kneader coater method).
The developer of the present invention is useful in an image forming method consisting of developing an electrostatic latent image formed on a latent image holding member with a developer layer formed on a developer carrier. The image forming method according to the present invention comprises the steps of forming a latent image on a latent image holding member, developing the latent image with a developer, and transferring the formed toner image to a receiving material. The latent image holding member includes an electrophotographic photoreceptor, a dielectric recording material, and the like, on which an electrostatic latent image is formed through a conventional process. The developer carrier includes, for example, a rotatable nonmagnetic sleeve having in the inside thereof a magnetic role. The developer carrier is disposed to face the latent image holding member. The toner image formed on the latent image holding member by development is then transferred to a receiving material through a known process and fixed thereon by a heat roll.
Where the first aspect toner of the invention is used, the image forming method does not include a cleaning step after transfer, and the toner remaining on the latent image holding member is recovered simultaneously with development. Where the second aspect toner is used, the residual toner remaining on the latent image holding member after transfer step is removed by blade cleaning. Where a transfer belt is used, a residual toner on the transfer belt is similarly cleaned off with a cleaning blade after the second transfer step.
Where the second aspect toner is used, it is preferable that the transfer step be carried out by forming a toner image once on a transfer belt as a first receiving material and then transferring the toner image from the transfer belt to a second receiving material. The transfer belt is usually a film support having thereon coated a coating resin layer having dispersed therein a resistance adjusting material. The transfer belt may have a seam, but a seamless belt is preferred.
The present invention will now be illustrated in greater detail with reference to the following Examples, but should not be construed as being limited thereto. Unless otherwise noted, all the parts and percents are by weight. D 50 means 50 percent diameter on a number basis.
I. Preparation of Toner A
______________________________________Linear styrene-n-butyl acrylate polymer 100 parts(Tg: 58° C.; Mn: 4,000; Mw: 24,000)Carbon black 3 parts(Mogal L, produced by Cabot G.L. Inc.)______________________________________
The above components were kneaded in an extruder, ground in a jet mill, and classified with an air classifier to obtain black toner particles having D 50 of 5.0 μm, M 50 (a) of 139.8, M 50 (b) of 140.7, M 50 (c) of 141.0, and ML 2 /A of 140.5.
The toner particles were blended with 0.65% silica (R972, produced by Nippon Aerosil Co., Ltd.) in a Henschel mixer to obtain a black toner (designated toner A).
II. Preparation of Toner B
II-1. First Step
II-1-1. Preparation of Resin Dispersion (1):
______________________________________Styrene 370 gn-Butyl acrylate 30 gAcrylic acid 8 gDodecanethiol 24 gCarbon tetrabromide 4 g______________________________________
The above components were mixed and dissolved. The mixture was emulsified in a flask containing a solution of 6 g of a nonionic surface active agent (Nonipol 400, produced by Sanyo Chemical Industries, Ltd.) and 10 g of an anionic surface active agent (Neogen SC, produced by Dai-ich Kogyo Seiyaku Co., Ltd.) in 550 g of ion-exchanged water. While stirring the emulsion slowly for 10 minutes, ion-exchanged water weighing 50 g and having 4 g of ammonium persulfate dissolved therein was poured into the flask. After displacing the atmosphere with nitrogen, the contents of the flask were heated on an oil bath with stirring till the temperature reached 70° C. The emulsion polymerization was continued at that temperature for 5 hours to obtain resin dispersion (1) having dispersed therein resin particles having an average particle diameter of 155 nm, Tg of 59° C., and Mw of 12,000.
II-1-2. Preparation of Resin Dispersion (2):
______________________________________ Styrene 280 g n-Butyl acrylate 120 g Acrylic acid 8 g______________________________________
The above components were mixed and dissolved. The mixture was emulsified in a flask containing a solution of 6 g of a nonionic surface active agent (Nonipol 400) and 12 g of an anionic surface active agent (Neogen SC) in 550 g of ion-exchanged water. Ion-exchanged water weighing 50 g and having 3 g of ammonium persulfate dissolved therein was poured into the flask while slowly stirring for 10 minutes. After displacing the atmosphere with nitrogen, the contents of the flask were heated on an oil bath with stirring till the temperature reached 70° C. The emulsion polymerization was continued at that temperature for 5 hours to obtain resin dispersion (2) having dispersed therein resin particles having an average particle diameter of 105 nm, Tg of 53° C., and Mw of 550,000.
II-1-3. Preparation of Colorant Dispersion (1):
______________________________________Carbon black (Mogal L) 50 gn-Butyl acrylate (Nonipol 400) 5 gIon-exchanged water 200 g______________________________________
The above components were mixed and dissolved, and the mixture was dispersed in a homogenizer (Ultratarax T50, manufactured by IKA) for 10 minutes to prepare colorant dispersion (1) comprising carbon black particles having an average particle diameter of 250 nm dispersed therein.
II-1-4. Preparation of Release Agent Dispersion (1):
______________________________________Paraffin wax (HNP0190, produced by 50 gNippon Seiro Co., Ltd.; melting point: 85° C.)Cationic surface active agent (Sanizol B50, 5 gproduced by Kao Corp.)Ion-exchanged water 200 g______________________________________
The above components were heated to 95° C., and the mixture was dispersed in a homogenizer (Ultratarax T50, manufactured by IKA) and then in a pressure homogenizer to prepare release agent dispersion (1) having release agent particles having an average particle diameter of 550 nm dispersed therein.
II-2. Second Step
II-2-1. Preparation of Flocculated Particles:
______________________________________Resin dispersion (1) 120 gResin dispersion (2) 80 gColor dispersion (1) 200 gRelease agent dispersion (1) 40 gCationic surface active agent (Sanizol B50) 1.5 g______________________________________
The above components were put in a round flask made of stainless steel and mixed and dispersed by means of a homogenizer (Ultratarax T50, manufactured by IKA). The flask was heated to 50° C. on an oil bath while stirring. After keeping the dispersion at 45° C. for 20 minutes, microscopic observation of the dispersion revealed formation of flocculated particles having an average particle diameter of about 4.0 μm.
II-2-2. Adhesion of Resin to Particles:
Resin dispersion (1) weighing 60 g (total volume of the dispersed resin particles was 25 cm 3 ) was slowly added to the dispersion obtained in II-2-1 above, and the temperature of the oil bath was raised to 50° C., at which the mixture was maintained for 30 minutes. Adhesion of flocculated particles to the original flocculated particles to increase the average particle diameter to about 4.8 μm was confirmed under observation with an optical microscope.
II-3. Third Step
To the dispersion obtained in II-2-2 above was added 3 g of an anionic surface active agent (Neogen SC), and the stainless steel-made flask was closed. The contents were heated up to 105° C. while stirring by means of a magnetic seal, at which temperature the contents were kept for 4 hours. After cooling, the reaction product was collected by filtration, washed thoroughly with ion-exchanged water, and dried to obtain a black toner having D 50 of 5.0 μm, M 50 (a) of 140.6, M 50 (b) of 103.8, M 50 (c) of 102.7, and ML 2 /A of 103.5.
The toner particles were blended with 0.65% silica (R972, produced by Nippon Aerosil Co., Ltd.) in a Henschel mixer to obtain a black toner (designated toner B).
III. Preparation of Toner C
Toner C was prepared in the same manner as for toner B with the following exceptions. In the step of preparing flocculated particles, the mixture in the flask was kept at 45° C. for 20 minutes to obtain flocculated particles having an average particle diameter of 3.8 μm. In the step of adhering particles, the mixture was maintained at 50° C. for 30 minutes to obtain flocculated particles having an average particle diameter of about 4.9 μm. In the third step, the contents of the flask were maintained at 93° C. for 5 hours to obtain a black toner having D 50 of 5.1 μm, M 50 (a) of 123.2, M 50 (b) of 133.8, M 50 (c) of 119.8, and ML 2 /A of 125.8.
The toner particles were blended with 0.65% silica (R972, produced by Nippon Aerosil Co., Ltd.) in a Henschel mixer to obtain black toner C.
IV. Preparation of Toner D
Toner D was prepared in the same manner as for toner B with the following exceptions. In the step of preparing flocculated particles, the mixture in the flask was kept at 50° C. for 30 minutes to obtain flocculated particles having an average particle diameter of 6.5 μm. In the step of adhering particles, the mixture was maintained at 50° C. for 30 minutes to obtain adhering particles having an average particle diameter of about 7.3 μm. In the third step, the contents of the flask were maintained at 93° C. for 3 hours to obtain a black toner having D 50 of 7.5 μm, M 50 (a) of 135.4, M 50 (b) of 139.6, M 50 (c) of 125.8, and ML 2 /A of 133.0.
The toner particles were blended with 0.43% silica (R972, produced by Nippon Aerosil Co., Ltd.) in a Henschel mixer to obtain black toner D.
V. Preparation of Toner E
Toner E was prepared in the same manner as for toner B with the following exceptions. In the step of preparing flocculated particles, the mixture in the flask was kept at 45° C. for 30 minutes to obtain flocculated particles having an average particle diameter of 5.5 μm. In the step of adhering particles, the mixture was maintained at 50° C. for 30 minutes to obtain flocculated particles having an average particle diameter of about 6.4 μm. In the third step, the contents of the flask were maintained at 105° C. for 3.5 hours to obtain a black toner having D 50 of 6.5 μm, M 50 (a) of 118.2, M 50 (b) of 120.8, M50(c) of 116.3, and ML 2 /A of 118.5.
The toner particles were blended with 0.50% silica (R972, produced by Nippon Aerosil Co., Ltd.) in a Henschel mixer to obtain black toner E.
EXAMPLE 1
Toner A and toner B were blended at a weight ratio of 1:1. The toner blend was added to a ferrite carrier coated with 1% polymethyl methacrylate (produced by Soken Kagaku) and having an average particle diameter of 50 μm, so as to give a total toner concentration of 5%, and mixed in a twin-cylinder mixer to prepare a two-component developer.
EXAMPLE 2
A developer was prepared in the same manner as in Example 1, except for changing the ratio of toner A to toner B into 1:3.
EXAMPLE 3
A developer was prepared in the same manner as in Example 1, except for replacing toners A and B with toners C and D, respectively.
EXAMPLE 4
A developer was prepared in the same manner as in Example 1, except for replacing the blend of toners A and B with toner E.
COMPARATIVE EXAMPLE 1
Toner A was added to a ferrite carrier coated with 1% polymethyl methacrylate (produced by Soken Kagaku) and having an average particle diameter of 50 μm, so as to give a toner concentration of 5%, and mixed in a twin-cylinder mixer to prepare a two-component developer.
COMPARATIVE EXAMPLE 2
A developer was prepared in the same manner as in Comparative Example 1, except for using toner B.
The size and shape characteristics of the toner in the developers prepared in Examples 1 to 4 and Comparative Examples 1 and 2 are shown in Table 1 below.
TABLE 1______________________________________Color D.sub.50 M.sub.50 (a) M.sub.50 (b) M.sub.50 (c) ML.sup.2 /A______________________________________Example 1 B 6.3 124.9 145.8 105.8 125.3Example 2 B 6.0 119.8 142.4 104.3 123.2Example 3 B 6.3 127.8 137.8 118.6 126.3Example 4 B 6.5 118.2 120.8 116.3 118.5Compara. B 5.0 139.8 140.7 141.0 140.5Example 1Compara. B 5.0 104.6 103.8 102.7 103.5Example 2______________________________________
A copying test was carried out using the developers prepared on a copier (A-Color, produced by Fuji Xerox Co., Ltd., modified to omit the cleaning step) to obtain 50,000 copies in a black-and-white mode. The results of the test are shown in Table 2, in which SAD stands for an image density (hereinafter the same).
TABLE 2__________________________________________________________________________Initial After 50,000 Copies Transfer TransferSAD Efficiency SAD Efficiency(B) Image Quality (%) (B) Image Quality (%)__________________________________________________________________________Example 11.52 no problem 95.2 1.50 no problem 93.9Example 21.45 no problem 98.1 1.43 no problem 97.2Example 31.46 no problem 94.2 1.42 no problem 90.4Example 41.47 no problem 97.4 1.44 no problem 95.0Compara.1.56 streaks due to 85.6 1.20 external additive buried 72.2Example 1 insufficient in toner surface, removal of reduction in density due residual toner to shortage of charge quantity, and streaks due to residual tonerCompara.1.42 no problem 98.6 1.25 scattering of carrier 95.5Example 2 due to overfeed of developer, and reduction in density and dropping of toner due to shortage of charge quantity__________________________________________________________________________
As is apparent from the above results, the developers of Examples 1 to 4 showed satisfactory performance in terms of image density, image quality, and transfer efficiency and maintained the performance over the testing period. The developer of Comparative Example 1 had a low transfer efficiency and developed streaks due to insufficient removal of the residual toner from the photoreceptor from the initial stage. A noticeable reduction in density occurred due to shortage of the charge quantity after obtaining 50,000 copies, when the external additive particles were found buried in the surface of the toner particles in a micrograph. The developer of Comparative Example 2 exhibited satisfactory performance in density, image quality and transfer efficiency in the initial stage but encountered difficulty in adjusting the amount to be transferred by means of the transport control plate, showing liability to overfeed. After obtaining 50,000 copies, scatter of the carrier particles on the photoreceptor due to the overfeed was observed, which accompanied development of scratches on the photoreceptor, partial missing of the image, and reduction in charge quantity.
VI. Preparation of Toner F
VI-1. Preparation of Toner F(B):
______________________________________Linear styrene/n-butyl acrylate copolymer 100 parts(Tg: 58° C.; Mn: 4,000; Mw: 24,000)Carbon black (Mogal L) 3 parts______________________________________
The above components were kneaded in an extruder, ground in a jet mill, and classified through an air classifier to obtain black toner particles having D 50 of 5.0 μm, M 50 (a) of 139.6, M 50 (b) of 138.9, M 50 (c) of 139.4, and ML 2 /A of 139.0.
The toner particles were blended with 0.68% silica (R972, produced by Nippon Aerosil Co., Ltd.) in a Henschel mixer to obtain a black toner (designated toner F(B)).
VI-2. Preparation of Toner F(C):
In the same manner as for toner F(B), except for replacing carbon black (3 parts) with 5 parts of C.I. Pigment Blue 15:3, toner F(C) having D 50 of 5.1 μm, M 50 (a) of 139.7, M 50 (b) of 139.0, M 50 (c) of 139.5, and ML 2 /A of 139.6 was obtained.
VI-3. Preparation of Toner F(M):
In the same manner as for toner F(B), except for replacing carbon black (3 parts) with 6 parts of C.I. Pigment Red 112, toner F(M) having D 50 of 5.0 μm, M 50 (a) of 138.6, M 50 (b) of 139.1, M 50 (c) of 139.2, and ML 2 /A of 139.4 was obtained.
VI-4. Preparation of Toner F(Y):
In the same manner as for toner F(B), except for replacing carbon black (3 parts) with 7 parts of C.I. Pigment Yellow 74, toner F(Y) having D 50 of 4.8 μm, M 50 (a) of 139.5, M 50 (b) of 138.2, M 50 (c) of 139.5 and ML 2 /A of 139.0 was obtained.
VII. Preparation of Toner G
VII-1. Preparation of Toner G(B):
VII-1-1. First Step
Resin dispersions (1) and (2), colorant dispersion (1), and release agent dispersion (1) were prepared in the same manner as in the preparation of toner B.
VII-1-2. Second Step
VII-1-2-1. Preparation of Flocculated Particles
______________________________________Resin dispersion (1) 120 gResin dispersion (2) 80 gColor dispersion (1) 200 gRelease agent dispersion (1) 40 gCationic surface active agent (Sanizol B50) 1.5 g______________________________________
The above components were put in a round flask made of stainless steel and mixed and dispersed by means of a homogenizer (Ultratarax T50). The flask was heated to 50° C. on an oil bath while stirring. After keeping the dispersion at 50° C. for 40 minutes, microscopic observation of the dispersion revealed formation of flocculated particles having an average particle diameter of about 8 μm.
VII-1-2-2. Adhesion of Resin
Resin dispersion (1) weighing 60 g (total volume of the dispersed resin particles was 25 cm 3 ) was slowly added to the dispersion obtained in VII-1-2-1, and the temperature of the oil bath was raised to 50° C., at which the mixture was maintained for 1 hour. Adhesion of flocculated particles to the original flocculated particles to increase the average particle diameter to about 8.4 μm was confirmed under observation with an optical microscope.
VII-1-3. Third Step
To the dispersion obtained in VII-1-2 above was added 3 g of an anionic surface active agent (Neogen SC), and the stainless steel-made flask was closed. The contents were heated up to 105° C. while stirring by means of a magnetic seal, at which temperature the contents were kept for 3 hours. After cooling, the reaction product was collected by filtration, washed thoroughly with ion-exchanged water, and dried to obtain a black toner having D 50 of 8.5 μm, M 50 (a) of 118.8, M 50 (b) of 118.4, M 50 (c) of 117.5, and ML 2 /A of 118.5.
The toner particles were blended with 0.40% silica (R972, produced by Nippon Aerosil Co., Ltd.) in a Henschel mixer to obtain a black toner (designated toner G(B)).
VII-2. Preparation of Toner G(C), Toner G(M) and Toner G(Y):
Cyan, magenta and yellow toners were prepared in the same manner as for toner G(B) except for changing the pigment in the same manner as for toner F(C), toner F(M) and toner F(Y), respectively. The size and shape characteristics of the resulting toners are shown in Table 3 below, in which B, C, M, and Y stand for black, cyan, magenta, and yellow, respectively (hereinafter the same).
VIII. Preparation of Toner H
Toner H(B) was prepared in the same manner as for toner G(B) with the following exception. In the step of preparing flocculated particles, the mixture in the flask was kept at 45° C. for 20 minutes to obtain flocculated particles having an average particle diameter of 4 μm. In the step of adhering resin to flocculated particles, the mixture was maintained at 50° C. for 30 minutes to obtain flocculated particles having an average particle diameter of about 4.8 μm. In the third step, the contents of the flask were maintained at 93° C. for 3 hours. The resulting toner particles had D 50 of 5.1 μm, M 50 (a) of 140.2, M 50 (b) of 144.0, M 50 (c) of 137.8, and ML 2 /A of 139.0. The toner particles were blended with 0.67% silica (R972, produced by Nippon Aerosil Co., Ltd.) in a Henschel mixer.
Cyan, magenta and yellow toners (toner H(C), toner H(M), and toner H(Y)) were prepared in the same manner as for toner H(B) except for changing the pigment in the same manner as for toner F(C), toner F(M) and toner F(Y), respectively. The size and shape characteristics of the resulting toners are shown in Table 3.
IX. Preparation of Toner I
Toner I(B) was prepared in the same manner as for toner G(B) with the following exception. In the step of preparing flocculated particles, the mixture in the flask was kept at 50° C. for 30 minutes to obtain flocculated particles having an average particle diameter of 6.5 μm. In the step of adhering resin to flocculated particles, the mixture was maintained at 50° C. for 30 minutes to obtain flocculated particles having an average particle diameter of about 7.3 μm. In the third step, the contents of the flask were maintained at 93° C. for 6 hours. The resulting toner particles had D 50 of 7.5 μm, M 50 (a) of 120.0, M 50 (b) of 123.2, M 50 (c) of 118.7, and ML 2 /A of 121.0. The toner particles were blended with 0.45% silica (R972, produced by Nippon Aerosil Co., Ltd.) in a Henschel mixer.
Toner I(C), toner I(M), and toner I(Y) were prepared in the same manner as for toner I(B), except for changing the pigment in the same manner as for toner F(C), toner F(M) and toner F(Y), respectively. The size and shape characteristics of the resulting toners are shown in Table 3.
X. Preparation of Toner J
Toner J(B) was obtained in the same manner as for toner G(B). Further, toner J(C), toner J(M), and toner J(Y) were prepared in the same manner as for toner F. The size and shape characteristics of the resulting toners are shown in Table 3.
TABLE 3______________________________________Toner Color D.sub.50 M.sub.50 (a) M.sub.50 (b) M.sub.50 (c) ML.sup.2 /A______________________________________F Y 4.8 139.5 138.2 139.5 139.0 M 5.0 138.6 139.1 139.2 139.4 C 5.1 139.7 139.0 139.5 139.6 B 5.0 139.6 138.9 139.4 139.0G Y 8.5 119.1 118.0 117.3 118.1 M 8.6 119.2 118.1 117.1 118.1 C 8.5 119.2 118.8 116.9 118.9 B 8.5 118.8 118.4 117.5 118.5H Y 5.2 140.3 144.0 137.2 139.1 M 5.0 140.5 144.3 137.7 139.3 C 5.0 140.1 144.2 137.5 139.7 B 5.1 140.2 144.0 137.8 139.0I Y 7.6 120.0 123.5 118.9 121.2 M 7.4 119.8 125.4 118.8 120.7 C 7.5 119.5 127.0 118.5 120.5 B 7.5 120.0 123.2 118.7 121.0J Y 5.0 138.6 140.0 141.5 140.9 M 5.1 139.5 141.5 141.5 140.8 C 5.0 139.0 139.8 140.9 140.0 B 5.0 139.8 140.7 141.0 140.5______________________________________
EXAMPLE 5
Toner F(B) and toner G(B) were blended at a weight ratio of 1:1. The toner blend was added to a ferrite carrier coated with 1% polymethyl methacrylate (produced by Soken Kagaku) and having an average particle diameter of 50 μm, so as to give a total toner concentration of 5%, and mixed in a twin-cylinder mixer to prepare a developer (designated developer (B)).
Similarly developers (C), (M) and (Y) were prepared by using the other color toners F and G.
EXAMPLE 6
Color developers were prepared in the same manner as in Example 5, except for changing the ratio of toner F to toner G into 4:1.
EXAMPLE 7
Color developers were prepared in the same manner as in Example 5, except for replacing toners A and B with toners H and I, respectively.
EXAMPLE 8
Color developers were prepared in the same manner as in Example 7, except for changing the ratio of toner H to toner I into 1:4.
COMPARATIVE EXAMPLE 3
Toner G was added to a ferrite carrier coated with 1% polymethyl methacrylate (produced by Soken Kagaku) and having an average particle diameter of 50 μm, so as to give a toner concentration of 5%, and mixed in a twin-cylinder mixer to prepare three color developers.
COMPARATIVE EXAMPLE 4
Color developers were prepared in the same manner as in Comparative Example 3, except for using toner J.
The size and shape characteristics of the toner in the developers prepared in Examples 5 to 8 and Comparative Examples 3 and 4 are shown in Table 4 below.
TABLE 4______________________________________Color D.sub.50 M.sub.50 (a) M.sub.50 (b) M.sub.50 (c) ML.sup.2 /A______________________________________Example 5 Y 6.7 130.2 126.0 134.0 130.5 M 6.7 132.5 127.1 136.2 132.6 C 6.6 130.9 126.8 133.9 131.1 B 6.8 129.9 125.5 134.2 130.0Example 6 Y 5.9 125.0 120.2 137.3 126.2 M 5.8 126.4 119.7 137.8 126.4 C 5.8 125.8 120.4 133.9 126.0 B 5.9 126.9 120.9 136.4 127.0Example 7 Y 6.3 128.4 124.7 136.0 130.0 M 6.3 128.5 123.3 135.8 129.5 C 6.3 127.2 124.6 134.3 127.2 B 6.2 128.0 125.1 135.9 128.5Example 8 Y 7.0 124.6 123.1 137.2 125.7 M 7.1 124.5 122.9 137.6 125.9 C 7.2 123.7 121.9 136.5 124.3 B 6.9 123.4 120.8 138.0 124.6Compara. Y 8.5 118.0 119.1 117.3 118.1Example 3 M 8.6 118.1 119.2 117.1 118.1 C 8.5 118.8 119.2 116.9 118.9 B 8.5 118.4 118.8 117.5 118.5Compara. Y 5.0 138.6 140.0 141.5 140.9Example 4 M 5.1 139.5 141.5 141.5 140.8 C 5.0 139.0 139.8 140.9 140.0 B 5.0 139.8 140.7 141.0 140.5______________________________________
A color copying test was carried out using the four color developers prepared in Examples and Comparative Examples on a copier (A-Color 635, produced by Fuji Xerox Co., Ltd., modified in such a manner that a toner image was successively transferred to a transfer belt, the full color image thus formed on the transfer belt was transferred to paper all at once, the transfer belt was then cleaned with a urethane resin-made blade, and the processing speed was elevated to produce 50 copies of 4A size per minute) to obtain 50,000 copies in a full color (inclusive of black) mode. The results of the test are shown in Table 5.
TABLE 5__________________________________________________________________________Initial After 50,000 Copies Transfer Transfer Effi- Effi-SAD SAD Image Clean- ciency SAD SAD Clean- ciency(B) (C + M + Y) Quality ability (%) (B) (C + M + Y) Image Quality ability (%)__________________________________________________________________________Example1.50 1.62 no no 88.2 1.49 1.57 no problem no 85.35 problem problem problemExample1.48 1.59 no no 86.1 1.53 1.58 no problem no 80.96 problem problem problemExample1.45 1.53 no no 90.2 1.45 1.56 no problem no 86.47 problem problem problemExample1.42 1.54 no no 87.4 1.40 1.55 no problem no 82.08 problem problem problemCompara.1.52 1.59 no toner 97.3 1.25 1.27 streaks and white consid- 88.2Example problem slightly dots due to erable3 remained insufficient insuffi- unremoved cleaning, scattering ciency of carrier due to of developer overfeed, cleaning and dropping of tonerCompara.1.40 1.49 no no 85.0 1.25 1.25 external additive no 55.7Example problem problem buried in toner problem4 surface, and reduction in density due to shortage of charge quantity__________________________________________________________________________
As is apparent from the above results, the developers of Example 5 to 8 showed satisfactory performance in terms of image density, image quality, and transfer efficiency and maintained the performance over the testing period. The developer of Comparative Example 3 suffered from instability of transport in the developing unit from the initial stage. After obtaining 50,000 copies, scattering of the carrier on the photoreceptor was observed, which accompanied scratches on the photoreceptor, image missing, and reduction in charge quantity. Further, the toner adhered to the cleaning blade to impair the cleaning performance, which resulted in development of streaks on the image. The developer of Comparative Example 4 exhibited satisfactory performance in density, image quality and transfer efficiency in the initial stage. However, it suffered from reduction in image density due to shortage of charge quantity after obtaining 50,000 copies, when the toner particles were observed under FE-SEM to have the external additive particles buried on the surface thereof. Further, the developer of Comparative Example 4 had poor transfer efficiency over the whole testing period.
While the invention has been described in detail and with reference to specific examples thereof, it will be apparent to one skilled in the art that various changes and modifications can be made therein without departing from the spirit and scope thereof.
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A toner comprising toner particles comprising a binder resin and a colorant, wherein the toner particles have a number average particle diameter of from 3 to 10 μm and satisfy relationship (1) or (2):
M.sub.50 (b)>M.sub.50 (a)>M.sub.50 (c) (1)
M.sub.50 (b)<M.sub.50 (a)<M.sub.50 (c) (2)
wherein M 50 (a) is an average shape index at a number average particle diameter D 50 which is calculated from cumulative 50% particles counting from the larger diameter side, M 50 (b) is an average shape index at a number average particle diameter D 16 which is calculated from cumulative 16% particles counting from the larger diameter side, and M 50 (c) is an average shape index at a number average particle diameter D 84 which is calculated from cumulative 84% particles counting from the larger diameter side. The toner satisfying relationship (1) is suitable for use in an image forming apparatus adopting a cleanerless system, and the toner satisfying relationship (2) is suitable for use in an image forming apparatus adopting a blade cleaning system.
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BACKGROUND OF THE INVENTION
[0001] This invention relates to an integral type thrust bearing in which a bearing ring and a retainer for housing rollers are mounted inseparably.
[0002] Among thrust bearings, there is an integral type in which the bearing rings and the retainer for housing the rollers are mounted inseparably from each other so that the thrust bearing can be easily mounted in a housing or on a shaft.
[0003] [0003]FIGS. 10A and 10B show an example of such an integral type thrust bearing. It is a three-part type having a retainer 2 for radially housing a plurality of rollers 1 , an inner ring 3 having a flange 3 a on the inner-diameter side, and an outer ring 4 having a flange 4 a on the outer-diameter side. The inner and outer edges of the retainer 2 are engaged by outwardly protruding claws 5 and inwardly protruding claws 6 formed by staking at the tips of the flanges 3 a and 4 a, respectively, so that the inner and outer rings 3 , 4 and the retainer 2 are inseparable from each other. Among integral type thrust bearings, there are two-part type ones which include only one of the inner and outer rings and the retainer is inseparable from the inner or outer ring.
[0004] In these integral type thrust bearings, the bearing rings, retainer and rollers are individually heat-treated beforehand, and thereafter, they are assembled into an integral unit. Normally, the bearing rings and the retainer are subjected to carburizing, hardening and tempering after forming. The rollers are hardened and tempered after rough forming, and then subjected to finish grinding. The retainer is in some cases subjected to soft nitriding instead of carburizing, hardening and tempering.
[0005] With such a conventional integral type thrust bearing, since the bearing rings, retainer and rollers are individually heat-treated before assembling, heat treatment steps increase, so that the heat treatment cost increases. Also, the manufacturing period tends to be long for adjustment of heat treatment steps for the respective parts.
[0006] In order that even if radial gap in the bearing increases, the bearing rings and the retainer can be made inseparable to increase the eccentricity allowance of an integral type thrust bearing, the present applicant proposed in JP patent application 2001-272336 to form the flanges of the bearing rings by bending instead of staking, thereby increasing the protruding amounts of the claws. In order to form such markedly protruding claws by bending, such bending has to be carried out after the retainer has been mounted. Thus, during heat treatment of the bearings, it is necessary to prevent hardening of the portions to be bent, or add a step of annealing the bent portions after heat treatment.
[0007] An object of this invention is to reduce heat treatment steps in the manufacture of an integral type thrust bearing.
SUMMARY OF THE INVENTION
[0008] According to this invention, there is provided a thrust bearing comprising a retainer formed with pockets for radially housing a plurality of rollers, and at least one of an inner ring having a flange on its inner-diameter side and an outer ring having a flange on its outer-diameter side, the flange restricting a radial gap in the thrust bearing, so that the bearing ring and the retainer are made inseparable from each other, characterized in that after the bearing ring and the retainer have been assembled together with the rollers into a bearing with the bearing ring and the retainer not hardened, the thus assembled bearing is subjected to carburizing, hardening and tempering. With this arrangement, it is not necessary to heat treat the bearing ring and the retainer individually, so that the heat treatment steps of the bearing decreases. For the rollers, they may be ones that have been heat-treated before assembling the bearing or ones that have not been heat-treated.
[0009] According to this invention, claws are formed by staking or bending at tip of the flange of the inner or outer ring so as to protrude toward the retainer and engage the inner or outer peripheral edge of the retainer, and the bearing ring and the retainer are made inseparable from each other by the claws.
[0010] The retainer may be made of a thin steel plate, and the radial section of the pockets for housing the rollers may be formed in the shape of W or inverted V to make the retainer inexpensive.
[0011] If the retainer is formed with pockets having a radial section in the shape of inverted V, substantially the radial center of roller guide surfaces on both sides of the inverted V-shaped pockets is compressed to form by plastic flow roller stopping claws protruding inwardly of the pockets from the respective roller guide surfaces. The roller stopping claws serve to prevent the rollers from coming out during assembly of the bearing. In particular, in a two-part type thrust bearing in which the pockets are open on one side, they are also effective in preventing the rollers from coming out during carburizing, hardening and tempering after assembling the bearing.
[0012] By forming recesses for receiving excess retainer material that plastically flows by compression on both sides of the portion of the roller guide surface where the roller stopping claw is to be formed, it is possible to prevent local wear of the rollers by eliminating build-up of excess material by plastic flow on the roller guide surfaces.
BRIEF DESCRIPTION OF THE DRAWINGS
[0013] Other features and objects of the present invention will become apparent from the following description made with reference to the accompanying drawings, in which:
[0014] [0014]FIG. 1A is a plan view showing a thrust bearing of a first embodiment;
[0015] [0015]FIG. 1B is a longitudinal sectional view thereof;
[0016] [0016]FIG. 1C is a front view showing claws of the outer ring of the thrust bearing of FIG. 1A before bending;
[0017] [0017]FIG. 2A is a plan view of the retainer of the thrust bearing of FIG. 1;
[0018] [0018]FIG. 2B is a longitudinal sectional view of the retainer of FIG. 2A;
[0019] [0019]FIG. 3A is a partial enlarged bottom view of the retainer of FIG. 2A;
[0020] [0020]FIG. 3B is a sectional view along line IIIb-IIIb of FIG. 3A;
[0021] [0021]FIG. 3C is a sectional view along line IIIc-IIIc of FIG. 3A;
[0022] [0022]FIG. 4 is a longitudinal sectional view showing a modified example of the thrust bearing of FIG. 1;
[0023] [0023]FIG. 5A is a plan view showing the thrust bearing of a second embodiment;
[0024] [0024]FIG. 5B is a longitudinal sectional view thereof;
[0025] [0025]FIG. 6A is a plan view showing the thrust bearing of a third embodiment;
[0026] [0026]FIG. 6B is a longitudinal sectional view thereof;
[0027] [0027]FIG. 7 is a longitudinal sectional view showing a modified example of the thrust bearing of FIG. 6;
[0028] [0028]FIG. 8A is a plan view showing the thrust bearing of a fourth embodiment;
[0029] [0029]FIG. 8B is a longitudinal sectional view thereof;
[0030] [0030]FIG. 9A is a plan view showing the thrust bearing of a fifth embodiment;
[0031] [0031]FIG. 9B is a longitudinal sectional view thereof;
[0032] [0032]FIG. 10A is a plan view showing a conventional thrust bearing; and
[0033] [0033]FIG. 10B is a longitudinal sectional view thereof.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
[0034] Hereinbelow, with reference to FIGS. 1 - 9 , the embodiments of this invention will be described. FIGS. 1 - 3 show the first embodiment. This thrust bearing is, as shown in FIGS. 1A and 1B, of a three-part type having a retainer 2 for housing a plurality of rollers 1 , an inner ring 3 having a flange 3 a on its inner-diameter side, and an outer ring 4 having a flange 4 a on its outer-diameter side. A radial gap in the bearing is set at a large value so that the inner and outer peripheral surfaces of the retainer 2 will not contact the flanges 3 a or 4 a even if a marked eccentric rotation occurs.
[0035] The inner ring 3 and the outer ring 4 have their respective flanges 3 a and 4 a formed by pressing thin steel plates (SPC or SCM). At the tip of the flange 4 a of the outer ring 4 , a plurality of claws 6 are formed by bending so as to protrude inwardly by a longer distance than the bearing inner gap. These claws 6 engage the outer peripheral edge of the retainer 2 so that the retainer 2 and the outer ring 4 are inseparable from each other. Each claw 6 has its thickness reduced beforehand by forming a step to making bending easy. As shown in FIG. 1C, on both sides of the base of each claw 6 , cutouts are formed. The retainer 2 and the inner ring 3 are made inseparable by outward claws 5 formed by staking at the tip of the flange 3 a.
[0036] The retainer 2 is formed by pressing a thin steel plate (SPC). As shown in FIGS. 2A and 2B, pockets 7 of the retainer 2 for radially receiving the rollers 1 have an inverted V-shaped radial section, and the inner and outer peripheral edges of the retainer 2 which engage the respective claws 5 and 6 are formed flat.
[0037] As shown in FIGS. 3A, 3B and 3 C, at substantially radially central portions of roller guide surfaces 8 on both sides of each of the inverted V-shaped pockets 7 , roller stopping claws 9 that protrude inwardly from the roller guide surfaces 8 are formed by plastic flow by compressing these portions. On both sides thereof, recesses 10 are formed to receive excess material that plastically flows by compression. Thus, the rollers 1 , which are housed in the respective pockets 7 , are prevented from coming off by the roller stopping claws 9 on both sides, and are guided by the smooth roller guide surfaces 8 which are free of bulging formed by excess material. Thus, their life will not be shortened due to local wear.
[0038] After assembled into an integral unit as shown in FIGS. 1A and 1B, the thrust bearing is carburized in a carburizing atmosphere, hardened in oil, and subjected to tempering. The rollers 1 , which are formed of a bearing steel (SUJ2), are subjected to hardening and tempering before assembling the bearing.
[0039] The thrust bearings of the below-described embodiments and modified examples are, as with the first embodiment, carburized, hardened and tempered after assembling, and the materials of the parts are the same as in the first embodiment.
[0040] [0040]FIG. 4 shows a modification of the first embodiment. It differs therefrom in that the retainer is formed in the shape of W in radial section by pressing. The shapes of the rollers 1 , inner and outer rings 3 , 4 are the same as in the first embodiment.
[0041] [0041]FIGS. 5A and 5B show the second embodiment. It is also of a three-part type, and differs in that claws 5 and 6 provided at the tips of the flanges 3 a and 4 a of the inner and outer rings 3 , 4 are both formed by staking. Otherwise it is the same as the first embodiment.
[0042] [0042]FIGS. 6A and 6B show the third embodiment. It is of a two-part type having a retainer 2 for radially housing a plurality of rollers 1 , and an inner ring 3 having a flange 3 a on its inner-diameter end. At the tip of the flange 3 a of the inner ring 3 , an outwardly protruding claw 5 is formed over the entire circumference. The claw 5 engages the inner peripheral edge of the retainer 2 so that the retainer 2 and the inner ring 3 are inseparable from each other. The claws 5 have their thickness reduced beforehand by forming a step to make bending easy.
[0043] As with the first embodiment, the retainer 2 is formed with pockets 7 having their radial section formed in the shape of inverted v by pressing. While not shown, at substantially radially central portions of the roller guide surfaces 8 on both sides of each pocket 7 , inwardly protruding claws 9 are formed. On both sides thereof, recesses 10 for receiving excess material are formed. FIG. 7 shows a variant of the third embodiment. It differs in that the radial sectional shape of the retainer 2 is formed in the shape of W by pressing. The shapes of the rollers 1 , inner and outer rings 3 , 4 are the same as in the third embodiment.
[0044] [0044]FIGS. 8A and 8B show the fourth embodiment. It is of a two-part type having a retainer 2 for radially housing a plurality of rollers 1 , and an outer ring 4 having a flange 4 a on its outer-diameter side. Inwardly protruding claws 6 are partially formed at the tip of the flange 4 a. The claws 6 engage the outer peripheral edge of the retainer 2 so that the retainer 2 and the outer ring 4 are inseparable from each other. The retainer 2 is the same as in the first embodiment, and the radial section of each pocket 7 is formed in an inverted V shape by pressing.
[0045] [0045]FIGS. 9A and 9B show the fifth embodiment. It is also of a two-part type and differs from the third embodiment in that claws 5 at the tip of a flange 3 a provided on the inner-diameter side of the inner ring 3 are formed by staking. Otherwise it is the same as the third embodiment.
[0046] In the above-described thrust bearings of the embodiments, the bearing ring or rings and the retainer are both formed by pressing thin steel plates. But one or both of them may be formed by machining steel material.
[0047] The following is the Example and Comparative Example.
[EXAMPLE]
[0048] Thrust bearings were prepared which were of a three-part type shown in FIG. 1 and which were subjected to carburizing/hardening/tempering after assembling. As for the heat treatment conditions, they were carburized by keeping at 850° C. for 35 minutes in a carburizing atmosphere, oil-hardened and then subjected to tempering at 165° C. for 60 minutes. The rollers 1 were used which were oil-hardened at 840° C. for 30 minutes beforehand, and then subjected to tempering at 180° C. for 90 minutes. The bearing dimensions were as follows: inner diameter: 56 mm, outer diameter: 76 mm, and thickness: 4.8 mm.
[Comparative Example]
[0049] Thrust bearings were prepared which were of a three-part type shown in FIG. 10 and in which the respective parts were individually heat-treated before assembling. As for the heat treatment conditions, the rollers 1 were oil-hardened at 840° C. for 30 minutes, and then subjected to tempering at 180° C. for 90 minutes. The retainer 2 was subjected to soft nitriding at 580° C. for 35 minutes. The inner and outer rings 3 , 4 were carburizing by holding them at 850° C. for 60 minutes in a carburizing atmosphere, oil-hardened and then subjected to tempering at 165° C. for 60 minutes. The bearing dimensions and the number of rollers 1 were the same as in Example.
[0050] For the thrust bearings of Example and Comparative Example, a rolling life test was conducted. In the rolling life test, with the inner ring 3 mounted at the rotating side and the outer ring 4 at the fixed side, they were mounted on a thrust rotary tester and the test was conducted under the following conditions for two cases, one in which axis eccentricity existed and the other in which it did not exist. For both Example and Comparative Example, the number of samples was ten, and the rolling life was evaluated in terms of L10 life (in which 90% of the samples can be used without destroyed).
[0051] Axial load: 4300 N
[0052] Rotating speed: 3000 rpm
[0053] Axis eccentricity: 0.0 mm, 0.5 mm
[0054] Lubricating oil: ATF (Automatic transmission fluid)
TABLE 1 Compara. Example example Vickers roller surface 765 700˜800 hardness inside 790 700˜800 retainer surface 730 380˜500 inside 175 150˜220 outer & surface 710 650˜800 inner inside 380 350˜500 rings Life No axis 1.1 1.0 ratio eccentricity Axis eccentricity 1.0 0.5 existed
[0055] The results are shown in Table 1. The rolling lives of the Example and Comparative Example are shown in terms of life ratio in comparison with the L10 life of Comparative Example when no axis eccentricity of rotation existed. In Table 1, the Vickers hardness Hv on the surface of and inside the bearing parts are also shown. The hardnesses Hv of the respective parts of Example are not so different from those of Comparative Example in which the parts were individually heat-treated. The hardnesses Hv of the parts of Example are the values actually measured this time. The hardnesses Hv of the parts of Comparative Example, which is a conventional article, are the values obtained previously.
[0056] The test results show that the rolling lives of the thrust bearings of the Example are substantially equal to the rolling life of Comparative Example irrespective of whether or not axial eccentricity existed. Thus it was confirmed that the rolling life equivalent to those of conventional articles can be achieved even if heat treatment steps are reduced by carrying out carburizing, hardening and tempering after assembling. The reason why in Comparative Example, when axis eccentricity existed, the rolling life decreased to half is because, as described above, in conventional articles, the retainer was made inseparable by the claws formed by staking, so that radial gap in the bearing was small.
[0057] As described above, in the thrust bearing of this invention, after the bearing rings and the retainer have been assembled together with rollers into a bearing with the bearing rings and the retainer not hardened, the thus assembled bearing is subjected to carburizing, hardening and tempering. Thus, it is not necessary to individually heat-treat the bearing rings and the retainer, and it is possible to reduce the heat treatment steps of the bearing and thus to markedly reduce the manufacturing cost. Also, the manufacturing steps are simplified, so that it is possible to shorten the manufacturing period.
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An integral type thrust bearing is proposed which can be manufactured with fewer heat treatment steps. The retainer and the inner and outer rollers not hardened are assembled together with rollers into a bearing and thereafter the assembled bearing is carburized, hardened and tempered. This eliminates the need of individual heat treatment of the retainer and the inner and outer rings and decreases heat treatment steps for the production of thrust bearings.
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BACKGROUND OF THE INVENTION
This application is a continuation-in-part application of Ser. No. 564,074, filed Apr. 1, 1975, entitled "Toothbrush."
This invention relates to dental equipment for promoting oral hygiene and, in particular, relates to a unique and improved toothbrush for effecting more thorough cleansing of teeth and gum areas near the base of the teeth. With prior art toothbrushes it is very difficult to effectively clean the gingival margins and sulcus areas, particularly is difficult to reach portions of the mouth, because of the fixed relationship of the bristles to the handle, and also due to the large size of the bristles and handle. Further, the construction of prior art toothbrushes makes it necessary to tilt the handle both horizontally and vertically in order to reach certain areas of the teeth.
The importance of cleaning not only the tooth surfaces, but also of cleaning the gingival crevice and of massaging the gums is clearly evident when it is recognized that diseases of the gums, such as gingivitis, for example, afflict approximately 65% of the nation's school children, and in adults, at the age of 40 for example, nearly 100% have some form of tooth or gum disease. If the teeth were properly cleaned, the bacteria which cause tooth and gum diseases could be significantly reduced, if not eliminated, and the incidence of disease reduced accordingly.
One of the most common and widely used dental instruments for cleaning the teeth and gums is the toothbrush, but unfortunately, for the reasons suggested above, the toothbrush is not frequently used correctly, and according to one report ("Toothbrushing--the Hoax of American Dentistry," Robert F. Barkley, Arizona Dental Journal, 1967), the toothbrush and its use is probably responsible for only a 10% reduction in tooth and gum diseases.
In this connection, there are many widely recognized and proven methods of using a toothbrush, and such methods include the vertical, rolling, Fones, Stillman and Charters methods. Whichever method used, it is desirable to thoroughly clean the interproximal areas of the teeth, as well as the buccal and lingual surfaces, and the sulcus areas at the base of the teeth. Also the occlusal surfaces of the teeth should be thoroughly cleaned. However, due to the natural arc of the teeth, and the fact that the teeth have both concave and convex surfaces and the teeth are of different sizes, on both upper and lower jaws, and teeth are frequently malposed, all tooth surfaces are usually not effectively cleaned. Also, the buccal surfaces of the posterior teeth are particularly difficult to clean because of the inward pressure of the cheek against these teeth.
Many attempts have been made in the prior art to devise a toothbrush capable of performing satisfactorily all of the above functions. However, most efforts in this regard have been directed toward different bristle configurations, whereby the bristles are constructed such that they more readily enter the interproximal areas or the gingival margins at the base of the teeth. However, even with such prior art constructions, it is very difficult to reach the lingual surfaces of the lower anterior teeth, and the buccal surfaces of the posterior teeth, as well as the gingival crevice of the posterior teeth. For example, when attempting to brush the lingual surfaces of the lower anterior teeth, it is necessary with prior art toothbrush constructions to elevate the handle of the toothbrush in order that access of the bristles to the lingual surfaces of the anterior teeth can be gained. This, of course, is awkward for anyone to do, and is particularly difficult for persons suffering from arthritis or other ailments which renders it difficult for them to elevate their arms above certain positions, and it is also difficult for children to manipulate the handle in a proper manner to gain proper access to the various surfaces of the teeth. Consequently, such persons, including small children, frequently do not brush the difficult to reach surfaces of the teeth, and the incidence is thereby increased.
The toothbrush according to the present invention is relatively small in comparison with conventional prior art toothbrushes, and may be easily carried in the pocket or the like for use away from home. Further, the base of the handle of the present toothbrush enables the toothbrush to be free standing, thus avoiding the hygienic problems encountered due to laying a conventional toothbrush on an unclean surface, or supporting it from a holder or the like.
Additionally, the bristle head of the toothbrush of the invention is small in size, thus making it easier to use to reach relatively inaccessible areas of the mouth. Further, with the toothbrush of the invention, the small, replaceable bristle head can easily be replaced, and it is not necessary to replace the whole toothbrush, as with prior art toothbrushes.
OBJECTS OF THE INVENTION
Accordingly, it is an object of this invention to provide a toothbrush having a unique construction which provides for easy access of the bristles to all of the surface areas of the teeth in a person's mouth.
Another object of the invention is to provide a toothbrush having a pivotal head carried by the handle thereof, such that the head may be pivoted to a plurality of positions, and in said positions, access to the lingual surfaces of the teeth on opposite sides, respectively, of the mouth is greatly enhanced, and wherein the handle is small and is configured whereby is may be readily grasped and manipulated with the fingers.
A further object of the invention is to provide a toothbrush having a pivotal head thereon which is offset from the handle axis, whereby the handle and bristles in effect straddle the teeth, and access to all of the lingual and buccal surfaces of the teeth can be gained without requiring excessive elevation of the toothbrush handle and the like, thus rendering it much easier for all persons, and particularly infirm persons or small children, to gain access to those areas of the teeth.
A still further object of the invention is to provide a toothbrush having a removable head and bristles thereon, whereby heads having different bristle configurations can be quickly and easily attached to the handle for providing the best bristle configuration for particular cleaning operations to be performed on the teeth and gums, such as, for example, small bristle heads for reaching confined areas in the mouth.
Yet another object of the invention is to provide a toothbrush having a pivotally mounted head and bristle arrangement, wherein the handle of the toothbrush has a hollow storage compartment therein and is enlarged such as to be self-supporting in an upright, free standing position.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a top perspective view of the preferred form of toothbrush according to the invention, and shows the toothbrush supported in an upright, free standing position.
FIG. 2 is a vertical sectional view of the toothbrush in FIG. 1.
FIG. 3 is an enlarged, fragmentary, sectional view taken along line 3--3 in FIG. 2.
FIG. 4 is a fragmentary, perspective view of a portion of the toothbrush handle showing a pick attached thereto rather than the bristle head configuration.
FIG. 5 is a fragmentary view in section of a portion of the end of the handle showing a modified form of attachment means for the bristle head to the handle.
FIG. 6 is a plan view of a second modification of the invention showing a further structural arrangement for attaching the bristle head to the handle.
FIG. 7 is a fragmentary view in section taken along line 7--7 in FIG. 6.
FIG. 8 is a vertical sectional view with a portion thereof broken away of a third modification of the invention.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
In the drawings, wherein like reference numerals indicate like parts throughout the several views, a first form of brush in accordance with the invention is indicated generally at 10 in FIGS. 1-3, and comprises and upright, self-supporting handle 11 having an enlarged, hollow base end 12, and an elongate, tubular forward end 13 axially slidable relative to the base end 12. A bristle head configuration 14 is releasably connected to the upper or distal end of the forward end portion 13 of the handle 11.
The base portion 12 of the handle in one form of the invention is hexagonal in cross-sectional configuration, and includes a substantially constant diameter lower end portion 12a and a convergent upper end portion 12b terminating in a diametrically enlarged thumb-engaging portion 15. A removable end cap 16 is suitably removably secured in the lower open end of base portion 12, defining an enclosed, hollow storage chamber or compartment 17 in the base portion in which various items may be stored, as, for example, a bristle head 14 or pick implement or the like P. The upper end of the base portion 12 is internally threaded at 18. An elongate support shaft or rod 19 extends coaxially from the upper end of the base portion 12 and has a reduced diameter externally threaded lower end extension 20 threadably engaged in the threaded opening 18 in the upper end of base portion 12 for supporting the support shaft or rod 19 thereon. The upper end of the support shaft or rod has a diametrically enlarged portion or flange 21 thereon, defining a spring stop shoulder.
The slidable, upper tubular end 13 of the handle is telescopically engaged over the support shaft or rod 19 and has an open lower end 22, which normally abuts against the upwardly facing end surface of the thumb-engaging portion on the upper end of base portion 12. The upper end of the sleeve 13 has a diametrically enlarged inner bore portion 23 defining an upwardly, axially facing stop shoulder 24 is spaced, opposed, confronting relation to the spring stop shoulder defined by flange 21. A coil spring 25 is engaged between its ends on the respective stop shoulders for resiliently biasing the sleeve downwardly into engagement with the upper end of the base portion, as shown in FIG. 2.
The upper end of the sleeve 13 has a pair of diametrically opposite aligned openings or holes 26 and 27 formed therethrough adjacent the extreme upper end thereof and the bristle head 14 includes a cylindrical, elongate shaft 28 rotatably received in the openings 26 and 27.
As seen best in FIGS. 2 and 3, the shaft 28 has a plurality of short bores or recesses 29 formed therein in circumferentially spaced apart locations therearound for cooperation with a detent pin 30 on the upper end of the support shaft or rod 19 to retain the bristle head 14 in a selected one of a plurality of adjusted, rotated positions.
The support shaft or rod 19 has a bifurcated upper end structure at 31 defining a generally U-shaped recess 32 in which the shaft 28 is received, and at the bottom of which the pin 30 is formed.
The sleeve 13 additionally has a plurality of cleaning openings 33 formed through the side thereof in the vicinity of the internally enlarged upper end portion wherein the spring 25 is received, which, in conjunction with the open upper end of the handle, enables water or other cleaning liquid to be flushed through the openings and through the spring receiving chamber for cleansing the toothbrush.
The various components of the brush may be made of plastic or metal or other suitable material, as desired, and the cap 16 may be press-fitted into place or retained with a snap detent rather than the threaded engagement shown in the drawings. Additionally, the support shaft or rod 19 may be formed integrally with the base portion 12 rather than separately attached thereto, as illustrated and described, and the shaft 28 of the bristle head structure 14 may be snugly received in the openings 26 and 27 so as to enable its rotation therein, but prevent it from dropping out of the openings when the pin 30 is retracted from the openings 29.
In FIG. 5 a modified form of the the invention includes inwardly directed detent portions 34 on the confronting inner end surfaces of the bifurcated end 31 of support rod 19, whereby a positive forceful action is required in order to urge the sleeve 13 and bristle head 14 with shaft 28 thereof upwardly to free the pin 30 from the opening 29.
A further modification of the invention is shown in FIGS. 6 and 7, and this form of the invention is substantially the same as that previously described, except that the shaft 28 of the bristle head 14 has a pair of circumferential, spaced apart channels 35 and 36 formed therein, in which a plurality of parallel, spaced apart ribs 37 and 38 formed on the inner confronting surfaces of bifurcated end 31 are slidably engaged to prevent the shaft 28 of the bristle head 14 from falling or slipping out of the openings 26 and 27 when the pin 30 is disengaged. However, the ribs are disengaged from the channels upon the requisite amount of movement of the sleeve 13, to enable the bristle head to be removed.
A further modified toothbrush 10' is illustrated in FIG. 8, and in this form of the invention the handle 11' includes a base portion 12' having a lower end 12a' and coverging intermediate portion 12b', with an elongate, tubular, reduced diameter upper end portion 12c. A cap 16 is releasably engaged on the lower open end of base portion 12' and defines a hollow cavity or chamber 17 in the base portion, as in the previous form of the invention, and a substantially shorter support shaft or rod 19' has a lower threaded end 20 engaged in a threaded opening 18 in the upper end of base portion 12' .
In FIG. 4 the pick P is shown attached to the handle in place if the bristle head 14.
The toothbrush of the present invention may be completely disassembled for cleaning, repair or replacement of various parts, without requiring the use of any special tools or the like.
As this invention may be embodied in several forms without departing from the spirit or essential characteristics thereof, the present embodiment is, therefore, illustrative and not restrictive, since the scope of the invention is defined by the appended claims rather than by the description preceding them, and all changes that fall within the metes and bounds of the claims or that form their functional as well as conjointly cooperative equivalents are, therefore, intended to be embraced by those claims. 9n
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A toothbrush having a bristle supporting head pivotaly mounted to a handle for pivotal movement of the head and bristles about a pivot axis substantially perpendicular to the axis of the handle to a plurality of positions to gain easy access to tooth surfaces at opposite sides of the mouth, the bristles extending in a direction mutually perpendicular to the axis of the handle and pivot axis, and the handle having an enlarged hollow end for storage therein of a bristle supporting head or the like and for supporting the toothbrush in an upright, free standing position.
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BACKGROUND OF THE INVENTION
[0001] The subject matter disclosed herein relates to power outlet and in particular to a power outlet having a controller for regulating the operation of an appliance.
[0002] Air conditioning units, such as those mounted in windows, are a popular appliance that is broadly utilized during warm weather periods. These appliances are popular since they may be added to an existing space by a homeowner or apartment resident without need for contractors. This is especially advantageous where the space is rented and the lease prohibits modification of the structure. The appliances are also movable, allowing them to be installed when desired and removed when the tenant moves or during cooler weather conditions.
[0003] While air conditioning appliances are convenient for homeowners and tenants, these appliances consume a large amounts of electrical power. This may be especially problematic in large metropolitan areas having a high population density. While central or whole-building air conditioning system can be cycled (turning the compressor off while keeping the fan on to comfort) easily by building managers or utilities during peak demand periods, window or room air conditioners do not provide an easy way for utilities to control and offer an acceptable level of comfort to the users at the same time.
[0004] Accordingly, while existing appliance control systems are suitable for their intended purpose, there remains a need for improvements in coordinating control of a plurality of individual appliances during peak demand time periods and offer the adequate level of comfort to the users.
BRIEF DESCRIPTION OF THE INVENTION
[0005] According to one aspect of the invention, a power outlet device is provided. The power outlet device includes a power inlet and a switch electrically coupled to the power inlet. The switch has a first open position and a second closed position. A power outlet is electrically coupled to the switch. A controller is operably coupled to the switch to selectively move the switch between the first position and the second position. A temperature sensor is operably coupled to the controller. A communications circuit is operably coupled to the controller.
[0006] According to another aspect of the invention, a power outlet device is provided. A switch is movable between a first state and a second state. A controller is operably coupled to the switch. A temperature sensor is operably coupled to the controller. A communications device is operably coupled to the controller. Wherein the controller includes a processor that is responsive to executable computer instructions when executed on the processor for moving the switch between the first state and the second state in response to a signal from the communications device when the temperature sensor measures a temperature less than a predetermined set point.
[0007] According to yet another aspect of the invention, a method of operating an air conditioning unit is provided. The method includes electrically coupling the air conditioning unit to a power outlet device having a switch arranged to electrically couple and decouple the window mounted air conditioning unit from an electrical circuit. A set point temperature is selected with a user interface on the power outlet device. An ambient temperature is measured with a temperature sensor on the power outlet device. A wireless command signal is received at the power outlet device. The air conditioning unit is decoupled from the electrical circuit with the switch in response to the wireless command signal when the measured temperature is less than the set point temperature.
[0008] These and other advantages and features will become more apparent from the following description taken in conjunction with the drawings.
BRIEF DESCRIPTION OF THE DRAWING
[0009] The subject matter, which is regarded as the invention, is particularly pointed out and distinctly claimed in the claims at the conclusion of the specification. The foregoing and other features, and advantages of the invention are apparent from the following detailed description taken in conjunction with the accompanying drawings in which:
[0010] FIG. 1 is a block diagram illustrating power outlet device in accordance with an exemplary embodiment of the invention;
[0011] FIG. 2 is a block diagram of the power outlet device of FIG. 1 coupled for communication to a home area network;
[0012] FIG. 3 is a block diagram of the power outlet device of FIG. 1 coupled for communication with an electrical utility meter; and,
[0013] FIG. 4 is a flow diagram illustrating a method for operating an air conditioning appliance.
[0014] The detailed description explains embodiments of the invention, together with advantages and features, by way of example with reference to the drawings.
DETAILED DESCRIPTION OF THE INVENTION
[0015] Embodiments of the invention described herein provide advantages in controlling the operation of a plurality of air conditioning appliances using a power outlet device. Embodiments of the invention, when integrated with a Home Area Network (HAN), provide advantages in allowing an electrical utility or a building operator to implement demand response programs in residences using individually controlled window mounted air conditioning appliances. Embodiments of the disclosed power outlet device provide advantages in allowing a user to set a maximum temperature the conditioned space may achieve without the appliance operating. The disclosed power outlet device may provide further advantages in allowing the set point to be locally programmed or via a computer network. The disclosed power outlet device may provide yet further advantages in allowing a user to over-ride a demand response command.
[0016] An exemplary embodiment of the power outlet device 20 is illustrated in FIG. 1 . The power outlet device 20 includes a power inlet 22 that is configured to connect with a standard electrical wall outlet plug 28 . In the exemplary embodiment, the power inlet is configured to connect with a National Electric Manufacturers Association (NEMA) type 5-15 wall outlet. The power inlet 22 is connected with a power outlet 24 by a relay or switch 26 . The power outlet 24 is configured to receive the electrical power plug, such as a NEMA 5-15 plug for example, from an appliance 30 such as a window mounted air conditioning appliance for example.
[0017] The switch 26 may be any suitable device, such as a switch, a relay or a solid state device for example, capable of moving between a first state and a second state to electrically decouple and couple the appliance 30 from a source of electrical power. In the exemplary embodiment, the first state or open state is one where the appliance 30 is electrically decoupled from the wall outlet plug 28 . The second state or closed state is one where the appliance 30 is electrically coupled to the wall outlet plug 28 . It should be appreciated that when the switch 26 is in the first state, the appliance 30 will shut off and will not operate. In the exemplary embodiment, the switch 26 is configured to switch 120-240 Volts of electrical power.
[0018] The power outlet device 20 further includes a control device 32 . The control device is a suitable electronic device capable of accepting data and instructions, executing the instructions to process data and storing the results. The control device may accept instructions and data through a user interface 34 , or other means such as but not limited to electronic data card, voice activation means, manually operable selection and control means, radiated wavelength and electronic or electrical transfer. Therefore, the processor 38 can be a microprocessor, microcomputer, a minicomputer, an optical computer, a board computer, a complex instruction set computer, an ASIC (application specific integrated circuit), a reduced instruction set computer, an analog computer, a digital computer, a molecular computer, a quantum computer, a cellular computer, a superconducting computer, a supercomputer, a solid-state computer, a single-board computer, a buffered computer, a computer network, a desktop computer, a laptop computer, or a hybrid of any of the foregoing.
[0019] It should be appreciated that while the control device 32 is described herein as a digital processor, this is for exemplary purposes and embodiments of the control device 32 may also be embodied as an analog circuit.
[0020] In the exemplary embodiment, the control device 32 includes a controller 36 having a processor 38 and memory 40 . The controller 36 is coupled to transmit a signal to the switch 26 and cause the switch 26 to move between the first state and the second state. The memory 40 may include one or more types of memory, including random access memory (RAM), non-voltile memory (NVM) or read-only memory (ROM).
[0021] The controller 36 includes operation control methods embodied in application code, such as that illustrated in FIG. 4 for example. These methods are embodied in computer instructions written to be executed by the processor 38 , typically in the form of software. The software can be encoded in any language, including, but not limited to, assembly language, VHDL (Verilog Hardware Description Language), VHSIC HDL (Very High Speed IC Hardware Description Language), Fortran (formula translation), C, C++, Visual C++, Java, ALGOL (algorithmic language), BASIC (beginners all-purpose symbolic instruction code), visual BASIC, ActiveX, HTML (HyperText Markup Language), and any combination or derivative of at least one of the foregoing. Additionally, an operator can use an existing software application such as a spreadsheet or database and correlate various cells with the variables enumerated in the algorithms. In one embodiment, the controller 36 includes an imbedded web server that allows service personnel to communicate with the controller 36 from remote locations. Furthermore, the software can be independent of other software or dependent upon other software, such as in the form of integrated software.
[0022] As will be discussed in more detail below, the user may interact with the controller 36 via the user interface 34 . In the exemplary embodiment, the user interface 34 includes a digital display 42 that displays the current set point defined by the user. The user interface 34 may also include buttons or actuators, such as first actuator 44 and a second actuator 46 for example. The user depresses the actuators 44 , 46 to raise and low the desired set point. The user interface 34 may further have an override button or selector that allows the user to bypass the control functionality of the controller 36 and moves the switch 26 to the closed state.
[0023] Control device 32 further includes a temperature sensor 48 that measures the ambient temperature of the environment in which the power outlet device is located. The temperature sensor 48 transmits a signal to the controller 36 that indicates the ambient temperature. In one embodiment, the temperature sensor 48 may be a thermocouple or a thermistor for example. In another embodiment, the temperature sensor 48 may be bimetal strip coupled to a mercury switch.
[0024] The control device 32 further includes a communications device 50 that is coupled to send and receive signals from the controller 36 . In the exemplary embodiment, the communications device 50 provides a means for the controller 36 to communicate signals embodying information on communications carriers as will be described in more detail herein. The communications device 50 may incorporate any type of communications protocol capable of allowing the controller 36 to receive, transmit and exchange information with one or more external devices. Communications device 50 may use wireless communication systems, methodologies and protocols such as, but is not limited to, IEEE 802.11, IrDA, infrared, radio frequency, electromagnetic radiation, microwave, Bluetooth, and laser. Further, communications device 50 may include one or more wired communications systems, methodologies and protocols such as but not limited to: TCP/IP, RS-232, RS-485, Modbus, power-line, telephone, local area networks, wide area networks, Ethernet, cellular, and fiber-optics.
[0025] In the exemplary embodiment, the communications device 50 may include one or more communications circuits or devices, such as IEEE 802.11 device commonly referred to as Wifi, a satellite device, a CDMA compliant cellular device, a GSM compliant cellular device, a radio frequency device, a IEEE 802.15.4 device commonly referred to as Zigbee, and a Bluetooth compliant device. In the exemplary embodiment, the communications device 50 is an IEEE 802.15.4 device that communicates with a home area network. In another embodiment, the satellite device transmits data on a frequency range of 3 to 40 gigahertz. In another embodiment, the radio frequency device transmits on a frequency range of 30 kilohertz to 3000 megahertz. The controller 36 may further include an optional antenna to assist in the transmission to the communication medium or carrier.
[0026] In one embodiment, the control device 32 may also include a timer 52 . As will be discussed in more detail below, the timer 52 is activated when the switch 26 is move between the first state and the second state. The timer 52 measures a predetermined amount of time, such as ten (10) minutes for example, and is used to prevent the power outlet device 20 from repeatedly cycling the electrical power to the air conditioning appliance 30 at a shorter than desired interval. It is believed that repeated cycling of the air conditioning appliance 30 may result in unnecessary wear on the air conditioner compressor and other internal components. It should be appreciated that while the timer 52 is illustrated as separate from the controller 36 , the timer 52 may be embodied in software executed on the processor 38 , on a separate processor (not shown), or as an analog circuit.
[0027] In operation, the power outlet device 20 is plugged into a wall outlet 28 as illustrated in FIG. 2 . The power outlet device 20 communicates with communication device 50 with a home area network 53 using a communications protocol such as IEEE 802.15.4 for example. This provides two-way communications that allow the power outlet device 20 to transmit signals, such as the temperature set point or switch 26 state for example, and to receive signals. In one embodiment, the utility or electric power provider may have a program sometimes referred to as a “demand response program” for lowering energy consumption during peak periods to reduce the stresses on the electrical network. In this embodiment an external party, such as utility 54 for example, transmits a signal via the Internet 56 . The signal is addressed to the power outlet device 20 and is received via a computer or router 58 . The router 58 transmits the signal via the home area network 53 to the power outlet device 20 . As will be discussed in more detail below, when the power outlet device 20 receives the signal, the power outlet device 20 will selectively couple and decouple electrical power to the air conditioning appliance 30 . It should be appreciated that while embodiments herein describe the external party transmitting the signal as a utility, the claimed invention should not be so limited and the transmitting entity may be a public utility, an energy provider, a power aggregator, a building owner, or a building manager for example. In one embodiment, the signal may be transmitted or originate from a building management system.
[0028] Another embodiment where the power outlet device 20 receives a signal from an external party, such as utility 54 for example, is illustrated in FIG. 3 . In this embodiment, the utility 54 includes an infrastructure that allows for two-way communication with electrical meters 60 . In one embodiment, the electrical meter is an Advanced Metering Infrastructure (“AMI”). The AMI meter 60 has a processing and communication circuits that allow the meter 60 to communicate information and receive instructions from the utility 54 . The meter 60 further has communications circuitry to communicate with the home area network 53 . This may allow the customer to control or monitor their electrical consumption in real-time or near-real time such as with a person computer 64 or a mobile device (e.g. cell phone) for example. The communications between the meter 60 and the home area network 53 may be wireless, using a protocol such as IEEE 802.15.4 (e.g. Zigbee) for example, or using a wired connection such as Ethernet or powerline carrier systems for example.
[0029] When the utility desires to reduce demand on the electrical grid, a first signal is transmitted from the utility 52 through the communications infrastructure 62 to the meter 60 . The meter 60 receives the first signal from the utility and transmits a second signal to the power outlet device 20 via the home area network 53 . In one embodiment, the second signal may pass through an intermediary device 66 connected to the home area network 53 . The intermediary device 66 may be a home energy monitor 66 or base unit that allows the user to monitor and/or control appliances to reduce energy consumption. When the power outlet device 20 receives the signal, the power outlet device 20 will selectively couple and decouple electrical power to the air conditioning appliance 30 to reduce electrical consumption as will be discussed in more detail below.
[0030] Referring now to FIG. 4 , a method 68 of operating the power outlet device 20 will be described. The method 68 starts in block 70 and proceeds to query block 72 where it is determined if there is a demand response signal from the utility or energy provider. As discussed above, the demand response signal may come from any source that the user provides access, such as the electrical utility, a power aggregator or even the user themselves. In one embodiment, the signal may be transmitted by the user remotely via their cellular phone or other wireless device for example. If the query block 72 returns a negative, the method 68 proceeds to block 74 where the switch 26 is set to the closed or connected state and the method 68 loops back to start block 70 .
[0031] If query block 72 returns a positive, meaning that a signal has been received, the method 68 proceeds to query block 76 where it is determined if the temperature at the power outlet measured by sensor 48 is greater than the temperature T set defined by the user via user interface 34 . It should be appreciated that if the user defines T set to be a higher temperature than the normal operating temperature of the air conditioning appliance, then there will be a reduction in electrical usage by the air conditioning appliance. If the query block 72 returns a negative, meaning the measured temperature is less than T set , then the method 68 proceeds to block 78 where a where the switch 26 is moved to the open state and the power to the air conditioning appliance is halted. If the query block 72 returns a positive, meaning the measured temperature is greater than T set , then the method 68 proceeds to block 80 where the switch 26 is closed allowing electrical power to flow to the air conditioning appliance. It should be appreciated that if the switch 26 is already in the desired position or state when the method 68 reaches block 74 , block 78 or block 80 , then the switch 26 simply remains in the desired position.
[0032] After completing block 78 or block 80 , the method proceeds to block 82 where the timer 52 is initiated. It has been found that repeated cycling of the power to an air conditioning appliance may result in unnecessary wear on the appliances components, such as the compressor for example. Therefore, the timer 52 is initiated to allow a predetermined amount of time to elapse before the state of switch 26 may be changed. In the exemplary embodiment, the timer 52 is set for ten (10) minutes.
[0033] Once the timer 52 is initiated, the method 68 proceeds to query block 84 where it is determined if the timer 52 has expired. If the query block 84 returns a positive, meaning the timer 52 expired, then the method 68 loops back to query block 72 to determine if the demand response or demand curtailment is still desired. If the query block 84 returns a negative, then method 68 proceeds to query block 86 where it is determined if the customer has overridden the set temperature. In one embodiment, the power outlet device 20 has an override selector that allows the user to prevent the device 20 from turning the air conditioner appliance off. If the query block 86 returns a positive, the method 68 loops back to block 74 where the state of the switch 26 is set to the closed state or position. If the query block 86 returns a negative, the method 68 loops back to query block 84 until the timer 52 expires.
[0034] While the invention has been described in detail in connection with only a limited number of embodiments, it should be readily understood that the invention is not limited to such disclosed embodiments. Rather, the invention can be modified to incorporate any number of variations, alterations, substitutions or equivalent arrangements not heretofore described, but which are commensurate with the spirit and scope of the invention. Additionally, while various embodiments of the invention have been described, it is to be understood that aspects of the invention may include only some of the described embodiments. Accordingly, the invention is not to be seen as limited by the foregoing description, but is only limited by the scope of the appended claims.
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A power outlet device for regulating the operation of an appliance, such as a window mounted air conditioner is provided. The device includes a power inlet and a power outlet coupled to a switch. A controller having a communications device controls the state of the switch. The controller is connected to a temperature sensor that measures the ambient temperature of the room. A user interface allows the user to define a maximum temperature for the room. In response to the receipt of a signal via the communications device, the controller regulates the flow of electrical power to the appliance based on the defined maximum temperature. A timer is also provided that minimizes short time period cycling of the appliance.
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This application is the U.S. national phase of International Application No. PCT/EP00/09874, filed on Oct. 3, 2000, which claims priority to Application Nos. EP 99203264.9, filed on Oct. 4, 1999, and EP 99203429.8, filed on Oct. 18, 1999.
FIELD OF THE INVENTION
The present invention relates to a novel method for the rapid detection of the presence or absence of antimicrobial residues in products preferably food products. A one step test method is described in which residues of antimicrobial compounds such as antibiotics are detected while disturbing compounds, such as natural pigments (e.g. blood) and naturally inhibiting compounds (e.g. lysozyme) present in the samples, which may interfere with the test, are inactivated. These compounds are inactivated after combining the sample with the test.
DESCRIPTION OF THE PRIOR ART
The presence of antimicrobial residues in food and feed is a growing concern among the consumers due to health-related problems and the increase of drug resistant bacteria. Antibiotics are not only applied as medication, but also widely used as antimicrobial growth promoting substances.
Antimicrobial residues might be present in e.g. body liquids, organs, meat and eggs which are used for consumption. Antimicrobial residues might also be present in food products in which the said animal products are added as an ingredient. Examples of food products are milk; meat of cow, pig, poultry and fish; sea food such as shrimps; liver, processed meat products such as sausages; ready to eat meals and baby food. Antimicrobial residues might also be present in body liquids or animal tissues, which are suitable for examination by for example food-inspection authorities. Examples are blood, kidney tissue or pre-urine obtained from the kidney and urine. Urine and blood are suitable for examination prior to slaughtering of the animal.
It is well known that concentrations of antimicrobial residues in animal body liquids, animal tissues and food products may be too high. In most countries, such as the countries of the European Union, Canada and the United States, Maximum Residue Levels (MRL) are regulated by legislation.
Test methods to detect antimicrobial residues in milk products such as microbial inhibition tests (e.g. agar diffusion tests) or methods making use of selective binders (e.g. antibodies or tracers) are well known. Examples of microbiological test methods have been described in GB-A-1467439, EP 0005891, DE 3613794, CA 2056581, EP 0285792 and U.S. Pat. No. 5,494,805. These documents all deal with ready to use tests that make use of a test organism. The test organism is mostly imbedded in an agar medium, which may contain an indicator, a buffer solution, nutrients and substances to change the sensitivity for certain antimicrobial compounds in a positive or negative way.
Examples of suitable test organisms are strains of Bacillus, Streptococcus or E. coli . In general, the principle of these tests is that when antibacterial compounds are present in a sample at a concentration sufficient to inhibit the growth of the test organism the colour of an acid/base or redox indicator will remain the same. However, when no inhibition occurs, growth of the test organism is accompanied by the formation of acid or reduced metabolites leading to a change in the colour of the indicator.
These test methods are suitable for the detection of antimicrobial residues in many food products. However up to now detection of antimicrobial residues in samples (e.g. some types of milk such as individual cow milk, liver, urine, kidney, meat juice, eggs), which contain a high concentration of natural antimicrobial substances (e.g. lysozyme, lactoferrin, lactoperoxidase) or a high concentration of natural pigments (e.g. blood), has not been easy to perform.
The inhibiting substances referred to above show inhibitory activity against the test microorganism leading to false positive results (Okada et al., Journal of the Japan Veterinary Medical Association 46: (2) 103-107 (1993); Schiffmann, Methodische und rechtliche Probleme beim Nachweis von Hemmstoffen in Milch, Publisher Tierarztliche Hochschule, Hannover, Germany; Weisser, Tierarztliche Umschau 31: (6) 276-278 (1976); Heinert et. al., Archiv für Lebensmittelhygiene 27: (2) 55-60 (1976); Carlsson et. al., Milchwissenschaft 42: (5) 282-285 (1987); Carlsson et al., Journal of Dairy Science 72: (12) 3166-3175 (1989)).
Natural inhibiting substances present in samples can be inactivated by heating, e.g. at 80° C. for 10 minutes (Vermunt et. al., Netherlands Milk and Dairy Journal 47: (1) 31-40 (1993); Weisser, Tierarztliche Umschau 31: (6) 276-278 (1976)) or by using well known dialysis methods (Takahiro, Shokuhin Eiseigaku Zasshi 24: (4) 423-428 (1983); van Wall, Archiv fur Lebensmittelhygiene 29: (6) 235 (1978)). After this pretreatment the sample can be used for further testing by following the procedures of the test. In case of a microbial agar diffusion test (e.g. as described in EP 0005891) the liquid sample can be added directly to the test, after which the test is incubated.
Natural pigments (e.g. blood) present in the sample (e.g. meat juice or juice obtained from organs) will always interfere with the agar matrix. In the case of tests based on a colour shift using e.g. an acid/base or redox indicator, the presence of such natural pigments often leads to an unreadable test. A method to diminish the effect of the natural pigments is to carry out a pre-incubation. In case of an agar diffusion test according to the method described in EP 0005891, the sample (e.g. meat fluid) is added to the test, followed by a pre-incubation of, e.g. 10-30 minutes, at room temperature. This pre-incubation should be long enough to let the antimicrobial residues diffuse into the agar matrix. After the pre-incubation the sample is removed, the test is washed with water and incubated following the instructions of the manufacturer. However, the methods require extra time and handling and will not prevent diffusion of disturbing compounds such as natural pigments into the agar. Even worse in case where a heating step (inactivation of natural inhibitors) is included, a brown colour always appears, making the test results even more unreadable. Mistakes in reading the results of the test may lead to both false positive and false negative results.
Moreover laboratories executing studies concerning the presence or absence of antimicrobial residues in foods are limited by the time available to execute these studies. With the present time consuming methods only a very limited amount of samples can be examined. Further, these assays can only be executed in well-equipped laboratories and by well-educated persons, which is also a limiting factor.
It can be concluded that up to now no suitable test methods for detecting antimicrobial residues in samples containing high concentration of natural inhibiting compounds and/or natural pigments have been available. The present methods are time consuming and may lead to both false positive and false negative results, which leads to unacceptable amounts of antibiotics in the food chain and to economic losses.
DETAILED DESCRIPTION OF THE INVENTION
The present invention now seeks to provide a reliable and simple to carry out one-step test for the detection of antimicrobial residues in liquid samples which might contain natural inhibitors and/or disturbing compounds such as natural pigments.
It has been found that when such a sample is added to a test suitable for detecting antimicrobial residues and then incubated for a sufficient time at a sufficient temperature to inactivate the natural inhibiting compounds of the sample, the test can be incubated directly after heating to determine the presence or absence of antimicrobial residues.
According to another aspect of the invention it has also been found that a suitable thickening agent can be added to the liquid sample, and disturbing compounds present in the sample can be caught in the matrix. Said matrix is preferably formed during the heating step.
It is even more surprising that antimicrobial residues diffuse directly from the solid matrix into the test system. Thus, additional extraction methods to obtain the antimicrobial residues from the matrix are not required.
According to the invention there is thus provided a process for determining the presence or absence of an antimicrobial residue in a sample, which process comprises:
(i) contacting the sample with a test suitable for determining the presence or absence of an antimicrobial residue in the sample; (ii) treating the contacted sample and test for a sufficient time interval to inactivate a natural disturbing compounds present in the sample; and (iii) incubating the contacted sample and test.
By natural disturbing compounds are meant compounds which may disturb the test and which are naturally present in the sample such as naturally inhibiting compounds (e.g. lysozyme) or natural pigments (e.g. blood). Thus by disturbing or inhibiting is meant the behaviour of these compounds on part of the test, for example the test microorganism or the colour indicators.
The invention also provides a test kit for determining the presence or absence of an antimicrobial residue in a sample, which test kit comprises:
(i) a test suitable for determining the presence or absence of an antimicrobial residue in a sample; and
(ii) a sample, wherein a natural inhibiting substance present in the sample has been inactivated.
The invention also provides a test kit for determining the presence or absence of an antimicrobial residue in a sample, which test kit comprises:
(i) a test suitable for determining the presence or absence of an antimicrobial residue in a sample; and
(ii) a thickening agent.
Any test suitable for determining the presence or absence of antimicrobial residues may be in used in a process or test kit of the invention. Suitable tests are those in which selected sensitive microorganisms are used, e.g. microbial agar diffusion tests, or tests based on selective binding of the compound to be detected. Selective binding can be achieved using the well-known antibody technology or by using specific tracers. An example of a specific tracer is the penicillin binding protein, which is used in e.g. the Delvo-X-Press® for detecting beta-lactams.
Examples of suitable microbial agar diffusion tests are tests in which species of Bacillus, Streptococcus or E. coli are used. Preferably thermophilic species, e.g. Bacillus stearothermophilus and Streptococcus thermophilus are used. Examples of preferred strains are Bacillus stearothermophilus var. calidolactis C953 (deposited with the Laboratory of Microbiology of the Technical University of Delft under the accession number LMD 74.1 in 1974 and with the Centraal Bureau voor Schimmelcultures (CBS), Baam under the accession number CBS 760.83 in 1983 were the strain is available to the public) and Streptococcus thermophilus T101 (DSM 4022, deposited on Mar. 3, 1987). Both strains are very sensitive to antimicrobial compounds, especially chemotherapeutics such as sulfa compounds and antibiotics such as penicillins and tetracyclines. E. coli strains or other suitable gram-negative bacteria can be used for the detection of e.g. quinolones.
Bacillus stearothermophilus var. calidolactis C953 and Streptococcus thermophilus T101 are fast growing and have the advantage that they are thermophilic. For example the optimum growth temperature of said Bacillus strain is from 50° to 70° C. The test organism is therefore very suitable for a test according to the invention as it is not killed by heating to inactivate the natural inhibiting compounds which may be present in the sample.
When the test organism is a Bacillus strain, it is preferably incorporated into the agar medium in the form of a spore suspension which may be prepared and incorporated into the agar medium prior to solidification by known methods (see for example GB-A-1467439). When the test organism is a Streptococcus strain, the bacteria are preferably incorporated into the agar medium in the form of bacterial cells which may be prepared according to known methods (see for example EP 0285792). The concentration of the test organism in the agar medium is preferably from 10 5 to 10 10 colony forming units per ml of agar medium.
Suitable nutrients to enable multiplication of the test organism in the absence of antimicrobial residues are for example assimilable carbon sources (e.g. lactose, glucose or dextrose), assimilable nitrogen sources (e.g. peptone) and sources of growth factors, vitamins and minerals (e.g. yeast extract).
The growth of the test microorganism can be detected using well known methods, preferably by colour change of the agar medium of the test sample. Typically a colour indicator, preferably an acid-base or a redox indicator, is used. Examples of suitable acid-base indicators include bromocresol purple and phenol red. Examples of suitable redox indicators include brilliant black, methylene blue, toludine blue and nile blue. Also combinations of two or more indicators can be used.
Typically, a solid matrix is a matrix which retains disturbing compounds, for example pigments, but which also allows antimicrobial residues in the sample, to diffuse in the test.
Optionally the sensitivity of the test may be altered by adding certain substances, by changing the test conditions such as pH or concentration of buffering substances or agar or by varying the ratio of the volumes of agar and the sample. Examples of substances that may be added to the test system to change sensitivity are nucleosides such as adenosine, or antifolates such as trimethoprim, ormethoprim or tetroxoprim, which improve the sensitivity of the test organism to sulfa compounds. Salts of oxalic acid or hydrofluoric acid may be added to improve the sensitivity to tetracyclines. Cysteine may be added to diminish the sensitivity to penicillins.
Samples suitable for use in the invention include any substance for which the absence or presence of antimicrobial residues is to be determined. For example the sample may be an animal body fluid, an animal tissue or an extract, for example a liquid extract thereof. In addition, the sample may be a foodstuff. Examples of animal body fluids include blood, urine, pre-urine, milk and meat juice. Examples of animal tissues include muscle, heart, liver and kidney. The sample may be an extract of one of those tissues.
The amount of liquid sample to be added to the test depends on the test system. For microbial diffusion tests typically from 0.01 to 1.0 ml, preferably from 0.05 to 0.5 ml is added to the test using well-known methods.
According to one embodiment of the invention a suitable thickening agent can be added to the sample. Examples of suitable thickening agents for use in a process or test kit of the invention are, for example polysaccharides (e.g. cellulose such as methylcellulose, HMPC, locust bean gum, starch or xanthan) or proteins (e.g. egg albumin, whey proteins or bovine albumin). Preferably methylcellulose and bovine albumin are used. Also combinations of suitable thickening agents can be used. The concentration of the suitable thickening agent should be sufficient to form a solid matrix.
According to another embodiment of the invention, inhibiting compounds are inactivated by a temperature treatment. For example the sample/test is heated for about 10 minutes at about 80° C. e.g. to inactivate the natural inhibiting compounds. The concentration of the thickening agent should be sufficient to maintain the solid matrix during the incubation of the test. Alternatively the solid matrix can also (partly) be formed during the incubation of the test. The thickening agent can be added to the liquid sample using any method known in the art, e.g. as a powder or as a tablet. The thickening agent can be added to the sample prior to addition of the sample to the test or after the sample is added to the test. Alternatively the thickening agent may be part of the test, e.g. as an ingredient of the agar or added onto the agar, e.g. as a tablet or as a powder, before the liquid sample is added to the test. Also a combination of temperature treatment and addition of a thickener is comprised by the invention.
Typically, a solid matrix is a matrix which retains disturbing compounds, for example pigments, but which allows antimicrobial residues in the sample to diffuse out of it.
After addition of the sample the test can be heated to inactivate the natural antimicrobial compounds present in the sample, for example lysozyme. The heating step may also optionally to aid formation of a solid matrix. Preferably, the test is heated for from 2 to 20 minutes at from 70° C. to 100° C. More preferably, the test is heated for from 10 to 15 minutes at from 75° C. to 85° C. or for from 2 to 6 minutes at about 100° C. Any other time/temperature treatment, which is sufficient to inactivate the natural inhibiting compounds of the sample without inactivating the antimicrobial residues to be detected, may be used.
The exact time/temperature requirements depend on e.g. the type of sample (milk, meat or organ juice, urine, egg, blood, etc.); the condition of the sample (e.g. the starting temperature, the volume of the sample); the type of test (e.g. microbial inhibition tests or assays based on selective binders (e.g. antibodies or tracers)); or the microorganism used in the test (e.g. thermophilic or non-thermophilic Bacillus or Streptomyces species). Of course it should be taken care of that the heat treatment will not inactivate the antimicrobial residues to be detected. The heat treatment can be executed using any method known in the art, e.g. by using an incubator as described below or by heating in a water bath.
After the heat treatment the test is incubated following the instructions of the test manufacturer. The incubation time of the test is dependent on the circumstances. In case of an agar diffusion tests using Bacillus stearothermophilus the test is incubated in a water bath or block heater at, for example, from 60° C. to 70° C., preferably at from 62° C. to 65° C. Typically, results may be obtained after from 1.5 to 4 hours, preferably from 2.5 to 3.5 hours. In case of tests using, selective binders, such as antibodies or tracers, the results may be obtained within about 30 minutes.
Conventional microbial inhibition tests suitable for use in the invention, include the commercial products Delvotest®, Premi®Test, BR-Test® (DSM, Holland), the ADM Copan® tests (Copan, Italy) and the CHARM® AIM tests (Charm, USA)). Inactivation of the natural inhibiting compounds present in the liquid sample, and optional formation of a matrix by adding a suitable thickening agent and activation of the spores of the test organism, is preferably achieved by heating for example for from 5 to 15 minutes at for example from 75° C. to 85° C. Alternatively any other temperature/time treatment, which is sufficient to obtain said effects, can be used.
In a further aspect, the invention provides test kits for carrying out the method of the invention. These test kits contain the test and are suitable to execute the method of the invention: add the liquid sample, heat to inactivate the natural inhibiting compounds of the sample, optionally to form a matrix, incubate the test and read the results.
Examples of kits useful for the purpose of the invention are transparent tubes, single or in a set, or combined as a block of translucent material provided with a number of holes shaped therein (incubator). The test kit may contain solidified agar medium, which may be optionally buffered; a test organism (e.g. a strain of Bacillus or Streptococcus ) at sufficient colony forming units; nutrients for growth of said organism; an indicator (e.g. an acid-base or redox indicator); optionally substances to change the sensitivity for certain antimicrobial compounds in a positive or negative way. All ingredients may optionally be added to the test as a separate source, for example as a tablet or paper disc.
The test kits preferably have determined sizes. This is because of the reliability of the test. In case of a test based on agar diffusion technology, preferably tubes are used. The test unit will preferably be high enough to contain an amount of agar medium and a sample corresponding to a height of from 3 to 30 mm, more preferably from 5 to 15 mm. The internal cross-sectional dimension of the test units is preferably from 1 to 30 mm, more preferably from 5 to 15 mm. The test units are preferably closed air tight during storage in which conditions they may be stored for at least several months. Of course any other test unit suitable for executing the method of the invention is included in this invention.
The volume of the agar medium in the test unit is determined by the height of the test unit, the internal cross-sectional dimension of the test unit and the percentage of the volume of the test unit, which is filled with the agar medium. The volume of the agar medium is preferably from 10 μl to 5 ml, more preferably from 100 μl to 1 ml.
Incubators suitable to execute the heat treatments as described in this invention can be constructed in such a way that after placing the test units in the incubator, heat and incubation treatments as described above can be done. The first heat treatment to inactivate the inhibiting compounds and optionally to form solid matrix and/or to activate the spores is executed at a higher temperature, after which the incubation of the test continues at a lower temperature. Optionally after the incubation of the test the incubator can cool down to a temperature sufficient to stop the test.
An example of such an incubator is a block heater in which test units (e.g. ampoules) can be placed. For example in case of a conventional microbial agar diffusion test using a Bacillus stearothermophilus strain the incubator/block heater may contain a number of holes suitable for placing the test ampoules or test plates (e.g. Delvotest® or Premi®Test) therein. After placing the ampoules or plates the incubator heats the test to a temperature of e.g. from 75° C. to 85° C. for e.g. from 10 to 20 minutes after which the incubator turns to a lower temperature of from 62° C. to 65° C. for from 1.5 to 4 hours (incubation of the test). Of course the exact time/temperature intervals depend on many factors and will differ per type of test. This invention includes all incubators capable to execute a pre-incubation at a certain temperature for a certain period of time directly followed by an incubation at a lower temperature for a certain period of time. Optionally after the incubation of the test the incubator can cool down to a temperature sufficient to stop the test.
The process described in this invention is very simple to carry out, so that persons who perform the test do not have to be specially educated or trained.
All documents mentioned in this application are herein incorporated by reference to the same extent as if each individual application or patent was specifically and individually indicated to be incorporated by reference.
EXAMPLE 1
Inactivation of Natural Inhibiting Compounds Present in a Pre-Urine Sample
Fresh kidneys of 7 negative (negative in the sense of the presence of antibiotics) cows were obtained from a slaughterhouse. To obtain samples for testing for the presence or absence of antimicrobial drug residues, the rosettes of the kidneys were divided into pieces. The pieces were gently squeezed using a garlic press to obtain pre-urine.
The samples were then examined using microbial inhibition test ampoules produced according to the methods described in EP 0005891 with the nutrients present in the agar. The said test is also known as Premi®Test (commercially available from DSM N.V., Delft, The Netherlands).
100 μl of each of the 7 squeezed samples (pre-urine) was added to the test ampoules (in triplicate) and preincubated for 20 minutes at room temperature. It is known that this pre-incubation time is sufficient to let antimicrobial residues (if present in the sample) diffuse into the agar matrix of the test. After this pre-incubation the sample was removed. Finally, the test was incubated in a waterbath at 64° C. following the instructions of the manufacturer. After 185 minutes incubation at 64° C. all 3 samples of 4 animals were still positive (>50%), After 200 minutes all 3 samples of 2 animals were still positive (>30%). These false-positive results were caused by the inhibiting effect of natural inhibiting compounds present in the pre-urine.
100 μl of each of the 7 squeezed samples (pre-urine) was added to the test ampoules and heated for 10 minutes at 80° C. in a waterbath, the ampoules were immediately placed in a waterbath of 64° C. and incubated following the instructions of the manufacturer. After 175 minutes the colour of all tests turned from purple to yellow, indicating that no antimicrobial residues were present.
These results clearly demonstrate that natural inhibiting compounds of the pre-urine inhibit the test leading to false positive results. When the test is executed according to the method described in this invention, i.e. by adding the sample directly to the test, heating the test as described above and incubating the test following the instructions of the producer, the activity of the natural inhibiting compounds was eliminated and no false-positive results were observed.
EXAMPLE 2
Inactivation of Natural Inhibiting Compounds Present in Around-Kidney Sample
This experiment was executed according to the methods described in Example 1, except for the sampling procedure. In this experiment samples from the rosette of the kidney were ground. 100 μl of each of the 7 ground samples (in triplicate) were added to the test ampoules and pre-incubated for 20 minutes at room temperature, after which the samples were removed and the test was incubated as described in Example 1. After 220 minutes all 21 samples were still positive. Moreover, due to discoloration of the test caused by a combination of the presence of natural pigments (e.g. blood) and heating of those pigments, it was not possible to read the results of the test in a proper way.
The experiment was repeated. However now the ground samples were diluted 1:1 with water. After 185 minutes 3 samples were still positive.
Finally, the diluted samples were examined according to the method described in this invention. 100 μl of each of the 7 ground diluted samples was added to the test ampoules, heated for 10 minutes at 80° C. and directly incubated as described in Example 1. After 175 minutes, the colour of all tests turned from purple to yellow, indicating that no antimicrobial residues were present.
These results clearly demonstrate that natural inhibiting compounds of the ground kidney samples inhibit the test leading to false positive results. When the test is executed according to the method described in this invention, by adding the sample directly to the test, heating the test as described above and incubating the test following the instructions of the producer, the activity of the natural inhibiting compounds was eliminated and no false-positive results were observed.
EXAMPLE 3
Inactivation of Natural Inhibiting Compounds Present in an Egg Sample
Samples of 5 eggs (in duplicate), which did not contain antimicrobial residues, were obtained for examination for the presence or absence of antimicrobial residues. A hole of approximately 1-2 cm2 was made in the egg, the egg yolk was pricked and the egg was placed with the hole down on a bottle allowing the egg white and egg yolk to drip into the bottle. After the egg had emptied, the bottle was closed and the sample was homogenized by shaking.
To inactivate the natural inhibiting compounds present in the egg sample, 100 μl of each of the 5 samples was added on Delvotest® ampoules. The test was produced according to the methods described in EP 0005891 with the nutrients present in the agar. After heating for 10 minutes at 80° C. in a waterbath, the ampoules were immediately placed in a waterbath at 64° C. and incubated following the instructions of the producer. After 140 minutes the colour of all tests turned from purple to yellow, indicating that no antimicrobial residues were present.
Control samples were not heated at 80° C. for 10 minutes, but directly placed on the ampoule. These tests remained purple for at least 4 hours.
These results clearly demonstrate that natural inhibiting compounds in the egg sample inhibited the test leading to false-positive results. When the sample was heated as described above, the activity of the natural inhibiting compounds was eliminated and no false-positive results were observed anymore.
EXAMPLE 4
Determination of the Sensitivity of the Delvotest® According to the Method Described in this Invention Using Spiked Samples
Egg samples were obtained according to the method described in Example 3. The samples were spiked by adding Penicillin G (0 and 4 ppb) or Sulphadiazine (0 and 100 ppb). The egg samples were added to Delvotest® ampoules (see Example 3) according to the method described in this invention: heated for 10 minutes at 80° C., and then, immediately placed in a waterbath at 64° C. and incubated following the instructions of the manufacturer. The results were read as soon as the colour turned to yellow (after 140 minutes). The samples containing no Penicillin G or Sulphadiazine (o ppb) were negative, while the samples spiked with 4 ppb Penicillin G and 100 ppb sulphadiazine remained purple (positive).
These results clearly demonstrate that the method described in this invention is suitable for detecting antimicrobial residues in egg samples.
EXAMPLE 5
Use of a Thickening Agent in a Kidney Sample
Ground kidney samples were obtained following the methods described in Example 2. However, in this experiment the kidneys were first frozen. It is well known that after freezing of a ground kidney sample many inhibiting compounds are released so that up to now detecting antimicrobial residues using a microbial inhibition test was not possible.
A part of the sample was examined (five fold) using the methods described in Example 2. After 175 minutes all samples were positive, even after 190 minutes 3 samples were positive. Moreover, the results were very difficult to read caused by the presence of natural pigments (e.g. blood).
Another part of the sample was examined as described above. However, the thickening agent bovine albumin (Sigma) was added to the sample (6% and 8%, five fold), after which the sample was added to the tests and heated for 10 minutes at 80° C. After incubation of the tests for 175 minutes at 64° C. all 10 tests were negative, indicating that no antimicrobial residues were present. Moreover, the purple and yellow colours of the test were very bright. Due to the presence of the matrix formed by adding bovine albumin both inhibiting compounds and natural pigments were caught in the matrix.
These results clearly demonstrate that adding a thickening agent to the ground and frozen kidney sample makes it possible to execute the test in a proper way. Both natural inhibiting compounds and natural pigments are caught in the matrix.
EXAMPLE 6
Use of a Thickening Agent in a Chicken Meat Sample
Fresh chicken breast meat of a negative chicken was obtained from a slaughterhouse (negative in the sense of the presence of antibiotics). To obtain meat fluid for further testing pieces of meat were heated for 10 minutes at 64° C. and gently sqeezed using a garlic press. Spiked samples were prepared by adding Amoxicillin (0, 5 and 10 ppb), Oxytetracycline (0, 75 and 100 ppb) or Sulphadiazine (0, 75 and 100 ppb) to the meat juice.
To a part of said samples the thickening agent methylcellulose (4000 c.p.i., Sigma) was added to a final concentration of 1.5%.
100 μl of each sample was added to the Premi®Test ampoules (in duplicate) following the procedure described in Example 1. However, since a thickening agent was added, the pre-incubation step was not required anymore. Also the heating of the samples for 10 minutes at 80° C. was not required for this specific sample.
After 160 minutes the colour of all control tests turned from purple to yellow, indicating that no antimicrobial residues were present. Tests executed with samples containing 5 and 10 ppb of Amoxicillin; 75 and 100 ppb of. Oxytetracycline and 75 and 100 ppb of Sulphadiazine remained purple (positive).
In addition a similar experiment was executed. However, now samples containing 10 ppb of Amoxycillin or 200 ppb of Oxytetracycline were prepared and the thickening agent bovine albumine (Sigma) was added to a final concentration of 6%. After 165 minutes the colour of all control tests turned from purple to yellow, while the tests executed with samples containing the antibiotics remained purple.
Due to the presence of the matrix formed by adding methylcellulose or bovine albumine natural pigments present in the meat juice sample were catched in the matrix. As a result of this said tests demonstrated much brighter colours (purple and yellow) as tests executed with samples not containing a thickening agent.
These results clearly demonstrated that adding a thickening agent to the meat juice makes it possible to read the test 20 minutes earlier (no preincubation). Further the test is easier to read, because of brighter colours.
EXAMPLE 7
Use of a Thickening Agent in a Fish Sample
Fresh trouts were obtained from a fish farm. The fish was negative in the sense of the presence of antibiotics.
An experiment similar to the experiment described in Example 6 was executed. As thickening agent methylcellulose was used.
The results were similar as the results described in Example 6, indicating that the method described in this invention is also beneficial for the examination of fish samples.
EXAMPLE 8
Use of a Thickening Agent in a Pre-Urine Sample
The experiment was executed as described in Example 1. However now to a part of the pre-urine sample the thickening agent methylcellulose (4000 c.p.i., Sigma) was added to a final concentration of 1.5%. Also spiked samples were prepared following the method described in Example 6.
After 185 minutes the colour of the control tests, which prior to incubation were heated 10 minutes at 80° C. to inactivate natural inhibiting compounds present in the sample, turned from purple to yellow indicating that no antimicrobial residues were present. Controls which were not heated prior to incubation remained purple for more as 240 minutes (false-positive results).
All test executed with samples containing 5 and 10 ppb of Amoxicillin; 75 and 100 ppb of Oxytetracycline and 75 and 100 ppb of Sulphadiazine remained purple (positive).
Also in this experiment it was demonstrated that due to the presence of the matrix formed by adding methylcellulose natural pigments present in the pre-urine sample were catched in the matrix. As a result of this said tests demonstrated much brighter colours (purple and yellow) as tests executed with samples not containing the thickening agent.
These results clearly demonstrated that adding a thickening agent to the pre-urine makes it possible to read the test 20 minutes earlier (no pre-incubation). Further the test is easier to read, because of brighter colours.
EXAMPLE 9
Use of a Thickening Agent in a Urine Sample
Bovine urine of a negative animal was obtained from a slaughterhouse (negative in the sense of the presence of antibiotics).
Spiked samples were prepared by adding Amoxicillin (0 and 10 ppb) or Oxytetracycline (0 and 200 ppb).
To a part of said samples the thickening agent bovine albumine (Sigma) was added to a final concentration of 6%.
100 μl of each sample was added to the Premi®Test ampoules (in duplo) following the methods described in Example 6.
After 210 minutes the colour of the control tests executed with samples containing bovine albumine turned from purple to yellow. The control samples, to which no thickening agent was added, remained purple (false-positives). Tests executed with samples containing the antibiotics remained purple (positive).
These results clearly demonstrates that due to the presence of the matrix formed by adding bovine, albumine natural inhibitors present in the urine sample were catched in the matrix. Also said tests demonstrated much brighter colours (purple and yellow) as tests executed with samples not containing the thickening agent.
EXAMPLE 10
Use of a Thickening Agent in a Milk Sample
Raw milk samples of negative cows were obtained from a farmer (negative in the sense of the presence of antibiotics).
Spiked samples were prepared by adding Penicillin G to the milk (0, 4 and 6 ppb).
To a part of said samples the thickening agent bovine albumine (Sigma) was added to a final concentration of 6%.
The samples were then examined using microbial inhibition test ampoules produced according to the method described in EP 0005891 with the nutrients in the agar.
100 μl of milk was added to the test ampoules. A part of the test ampoules with the raw milk sample was heated for 10 minutes at 80° C. as described in Example 1. All experiments were executed in five fold. The tests were further incubated following the methods described in Example 1.
After 160 minutes the colour of all control tests, which were heated for 10 minutes at 80° C., turned from purple to yellow indicating that no antimicrobial residues were present. Also all control tests to which bovine albumine was added turned form purple to yellow after 160 minutes. The control tests to which no bovine albumine was added and which were not heated for 10 minutes at 80° C. turned yellow after 185 minutes.
All tests executed with samples containing 4 and 6 ppb of Penicillin G remained purple (positive).
Due to the presence of the matrix formed by adding bovine albumine natural inhibiting compounds present in the raw milk were catched in the matrix. As a result of this the duration of the incubation time of said tests was 25 minutes shorter.
It was also demonstrated that this effect is obtained by heating the test ampoule containing the raw milk sample for 10 minutes at 80° C.
Therefore it can be concluded that with both methods described in this invention natural inhibiting compounds present in the raw milk sample are inactivated: by catching these compounds in the matrix formed by a thickening agent or by inactivation by a heating step.
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The present invention relates to a novel method for the rapid detection of the presence or absence of antimicrobial residues in products preferably food products.
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CROSS-REFERENCE TO RELATED APPLICATIONS
This application claims priority from U.S. Provisional Patent Application No. 60/735,558, filed Nov. 9, 2005, which is incorporated herein by reference.
STATEMENT REGARDING FEDERALLY SPONSORED RESEARCH OR DEVELOPMENT
This invention was made in part with government support under grant number N00014-02-1-0807 from the Defense Advanced Research Projects Agency (DARPA), United States Navy, and 1U54CA119367-01 from the United States National Cancer Institute. The government has certain rights in this invention.
FIELD OF THE INVENTION
The present invention relates generally to sample preparation. More particularly, the present invention relates to a magnetic sifter. The magnetic sifter is especially suitable for preparation of biological samples.
BACKGROUND
Numerous biomedical applications require rapid and precise identification and quantitation of biomolecules present in relevant biological and environmental samples. The starting point in such experiments is an appropriate sample preparation procedure, which often determines if the experimental outcome is successful or not. For example, sample collection, pre-purification, and preparation procedures are crucial in molecular diagnostics such as genomic and proteomic analyses. These analyses usually depend on specific hybridization or affinity binding between DNA/RNA/protein targets (unknown) and probes (known). The specificity of hybridization or affinity binding can be negatively affected by the presence of abundant impurities. Furthermore, the concentration of target molecules may vary by many orders of magnitude and fall out of the dynamic range of the biosensors used to detect them.
Despite the importance of sample preparation methods, no universal or standard sample preparation protocols exist in the biomedical community. Variations in sample preparation may contribute to major discrepancies in the quantity and type of biomolecules identified by different laboratories, even though the same reagents and biosensors (or biochips) are employed. Therefore, better and more affordable sample preparation methods and tools are still in great demand.
There are a number of devices available for sorting or capturing biomolecules of interest using magnetic sorters. With these devices, a wall of the device contains a magnet, fluid is passed over the magnet in a planar configuration, and magnetic probes attached to a biomolecule of interest sticks to the magnet, allowing impurities to pass through. These devices have a number of shortcomings, including large size, low capture rates, low flow rates, and cumbersome methods of releasing captured biomolecules. Accordingly, there is a need in the art to develop a new magnetic device that is small in scale, enables three dimensional flow normal to the substrate, allows relatively higher flow rates and higher capture rates, and provides a relatively easy method of releasing captured biomolecules.
SUMMARY OF THE INVENTION
The present invention provides a magnetic sifter with all of the above properties. The magnetic sifter includes at least one substrate. Each substrate contains a plurality of slits, each of which extends through the substrate. The sifter also includes a plurality of magnets attached to the bottom surface of the substrate. These magnets are located proximal to the openings of the slits. An electromagnetic source controls the magnitude and direction of magnetic field gradient generated by the magnets. Either one device may be used, or multiple devices may be stacked on top of one another. In addition, the magnetic sifter may be used in connection with a detection chamber.
Preferably, the magnets are made of a soft magnetic material and the substrate is made of silicon, silicon oxide, or silicon nitride. In the latter two cases, the sifter also preferably includes a support layer. The support layer preferably has a plurality of openings, each of which connects to a plurality of slits in the substrate.
The present invention also provides a method of preparing a biological sample with the inventive magnetic sifter. With this method, a biological sample is mixed with capture probes. The capture probes are labeled with magnetic tags, such that at least one target biomolecule binds to the capture probes. A magnetic field is then generated in the magnetic sifter with an electromagnetic source. The biological sample/capture probe mixture is then passed through the magnetized magnetic sifter. In this way, capture probes, bound to the at least one biomolecule, are captured by the magnetic sifter, whereas impurities in the biological sample pass through. At this point, the capture probes may be kept bound to the magnetic sifter. Alternatively, the capture probes may be released by rotating the direction of the applied magnetic field by 90 degrees. This serves to reduce the magnitude of the magnetic field gradient. The magnetic sifter may also be flushed with a washing buffer during this process to aid in the removal of capture probe. The biomolecule of interest may be separated from the capture probe at this point, or prior to release of the capture probe.
BRIEF DESCRIPTION OF THE FIGURES
The present invention together with its objectives and advantages will be understood by reading the following description in conjunction with the drawings, in which:
FIG. 1 shows a cross-sectional view of a magnetic sifter according to the present invention.
FIG. 2 shows a bottom view of a magnetic sifter according to the present invention.
FIG. 3 shows a cross sectional view of stacked magnetic sifters according to the present invention.
FIG. 4 shows rotation of magnetization of the magnetic sifter according to the present invention.
FIG. 5 shows another example of a magnetic sifter according to the present invention.
FIG. 6-8 show methods of fabricating a magnetic sifter according to the present invention.
FIG. 9 shows a bottom view of a magnetic sifter in a honeycomb configuration according to the present invention.
FIG. 10 shows a detailed plan of the magnetic sifter shown in FIG. 9 .
FIG. 11 shows a micrograph of a magnetic sifter fabricated according to FIG. 9-10 .
FIG. 12 shows an example of a magnetic sifter in fluidic connection with a detection chamber according to the present invention.
DETAILED DESCRIPTION OF THE INVENTION
FIG. 1 shows a magnetic sifter 100 according to the present invention. Magnetic sifter 100 includes a substrate 110 , with top surface 112 and bottom surface 114 . A plurality of slits 120 extends through substrate 110 . These slits are preferably between about 0.5 μm and about 10 μm wide at bottom surface 114 . Also preferably, the distance between neighboring slits is between about 0.5 μm and about 10 μm. Substrate 110 includes magnets 130 on its bottom surface 114 . Magnets 130 are preferably soft magnets. As shown, magnets 130 are proximal to openings 122 of slits 120 . Magnetic sifter 100 also includes an electromagnetic source 140 for controlling the magnitude and direction of a magnetic field gradient generated by magnets 130 . Preferably, electromagnetic source 140 induces magnets 130 to generate a magnetic field gradient in the range of about 0.1 T/μm and about 1 T/μm at the openings 122 of the slits 120 . Magnetic sifter 100 is preferably micromachined.
Magnetic sifter 100 can be used in the following way. A raw sample containing target molecules 150 and impurities 160 are first mixed with specific capture probes 170 labeled with magnetic tags 172 . The magnetic tags 172 may be magnetic beads or any other magnetic tag known in the art. The magnetic tags are preferably magnetic nanotags, as described in U.S. patent application Ser. No. 10/829,505, by Wang et al, which is incorporated by reference herein. The size of slits 120 is scaled accordingly to accommodate the size of the utilized magnetic tags. In the embodiment of the invention shown, a sequence of the capture probes 170 is complementary to a sequence of the target molecules 150 so that they can readily hybridize under appropriate conditions. In this case, the target molecules 150 are nucleic acid, such as RNA or DNA. The impurities 160 are not complementary with the capture probes 170 so that they remain unchanged in the mixture. In another embodiment, the capture probes 170 are antibodies attached to a magnetic nanotag 172 , and the target molecule 150 is a protein or peptide. The mixture is then passed through magnetic sifter 100 , with the direction of flow indicated by dashed arrows 150 . It is also feasible to reverse the flow direction. The magnetic nanotags 172 in capture probes 170 , which have zero remanent magnetization in the absence of an applied magnetic field, become magnetized by magnets 130 and trapped at the edges of magnets 130 along with targets 150 , while the impurities 160 pass through the slits. (The direction of the magnetic field in this and subsequent figures is indicated by bold arrows).
FIG. 2 shows a bottom view of a magnetic sifter 200 . As shown in the blown up section on the right of FIG. 2 , in order to achieve a high throughput (or flow rate) of samples, slits 220 are preferably etched into substrate 210 in a rectangular shape so that at least one dimension is not a limiting factor to fluid flow. Furthermore, the rectangular shape is conducive to generating a strong horizontal magnetic field by magnets 230 , which ensures capture of most of the magnetic nanotags and thus the target molecules.
Depending on the gap between soft magnets, a horizontal field gradient ranging from ˜0.01 T/μm to ˜1 T/μm can be readily attained. As an example, consider iron oxide nanotags in aqueous solution. Presume that their radius is r=7 nm, their saturation magnetization is M=340 emu/cc, water viscosity is η=8.9×10 −4 kg/(m s), and the field gradient near a 0.5 μm wide gap of the soft magnets is ∇B˜1 T/μm at a distance of d=0.15 μm from the gap edge. Then, the drift velocity Δv of the nanotags is determined by the balance between the magnetic force and viscous force (Stoke's law):
Δ
v
=
m
·
∇
B
6
π
η
r
=
340
·
1000
(
A
/
m
)
·
(
4
/
3
)
·
(
7
·
10
-
9
m
)
3
·
10
6
(
T
/
m
)
6
·
(
8.9
·
10
-
4
kg
/
m
·
s
)
·
7
·
10
-
9
m
=
4170
im
/
s
This drift velocity is substantial if the fluid flow velocity is ˜1 mm/s perpendicular to the substrate, leading to a high capture probability. Furthermore, at sufficient field amplitudes magnetic nanoparticles (nanotags) may form chains along the applied field direction, which is along the short axis of the slits in FIG. 2 . If the chain length is equivalent to or greater than the slit width, the nanotags will not be able to pass through the slits. The present invention makes use of this benefit of chain formation to allow high capture yield.
The same sample can be recycled through the sifter several times to improve the capture yield if needed. Alternatively, multiple but identical substrates can be stacked in series to achieve nearly 100% capture yield ratio. For example, presume that the number of flow recycles (or the number of stacked substrates) is 3, the capture ratio in one cycle (or through one substrate in the case of stacked substrates) is 70%, then the overall capture ratio is 70%+(1-70%) 70%+(1-70%) (1-70%) 70%=97.3%. An example of stacked substrates is shown in FIG. 3 . FIG. 3 shows a first substrate 310 , with a first plurality of slits 320 and a first plurality of magnets 330 . Magnets 330 are stacked on top surface 316 of second substrate 312 , with second plurality of slits 322 and second plurality of magnets 332 . Magnets 330 may be stacked directly on top surface 316 , as shown, or a spacer may be used.
After the impurities are fully washed away, the trapped targets (attached to the capture probes) can be either harvested by denaturing the DNA duplex or antibody/peptide complex or kept with the nanotags without denaturing. In either case, the capture probes conjugated to the nanotags can be released from the magnetic sifter by rotating the applied field by 90°, as shown in FIG. 4 , while flushing with a washing buffer. FIG. 4 shows substrate 410 , slits 420 , and magnets 430 . The direction of the applied magnetic field is shown by bold arrows 440 . The applied magnetic field is then reduced (or even removed) to prevent possible chain formation of magnetic nanotags. The magnetization will be stable along the long axis of the soft magnets because of shape anisotropy and deposited uniaxial anisotropy along the long axis of soft magnets. The magnetic field between the magnets is greatly reduced when they are magnetized in parallel, so that the nanotags can be dislodged from the edges of the magnets. If the denaturing step is skipped, then a mixture of nanotags conjugated to target molecules and nanotags with capture probes only are released from the sifter (because excess capture probes are used in FIG. 1 ). This mixture could be directly applied to a magnetic biochip for detection according to one scheme of the present invention, to be discussed later.
In one aspect of the present invention, shown in FIG. 5 , the substrate is a thin membrane. FIG. 5 shows magnetic sifter 500 , having thin substrate 510 , slits 520 , and magnets 530 . Magnetic sifter 500 also includes a support layer 540 , with a plurality of openings 542 that extend through support layer 540 . Preferably, each opening 542 connects to a plurality of slits 520 , as shown. Support layer 540 may be any material but is preferably silicon, e.g. (100) silicon. Thin substrate 510 may also be made of any material, but is preferably made of silicon nitride or silicon oxide. Openings 542 are preferably between about 100 μm and about 500 μm in width. Openings 542 may be tapered, as shown, but need not be.
Magnetic sifters according to the present invention may be fabricated by a number of different methods. A first method is a self-aligned fabrication method. First, a (100) Si substrate 610 is acquired and polished to an appropriate thickness, as shown in FIG. 6 a . Then the substrate 610 is masked and anisotropically etched as shown in FIG. 6 b , e.g., by wet etching in an alkaline solution, to create slits 620 . If the aperture of the Si wafer is exposed to anisotropic etchants such as alkaline hydroxides, the (100) crystal planes (parallel to the substrate) etch much faster than the (111) crystal planes, resulting in a cavity whose side wall is parallel to the (111) planes, which will be at an angle of 54.7° with the substrate plane. Third, the bottom side 612 of the substrate 610 is coated with a layer of soft magnetic material 630 (such as NiFe, CoTaZr, CoFe alloy, CoFeHfO, or a combination of any of these materials) without a masking layer ( FIG. 6 c ). In this step, the soft magnets are self aligned to the etched slits. The soft magnetic layer can also be electroplated as practiced in the magnetic recording industry after adding a conductive seed layer. Finally, the soft magnetic layer is patterned into the stripes shown in FIGS. 2 and 4 . Note that the gaps of the soft magnets will have a slope, due to the non-ideal nature of film deposition processes, rather than be exactly vertical as shown in FIG. 6 , but the slope can be controlled and will not hamper the operation of the magnetic sifter. In addition, the soft magnets are properly passivated to withstand the washing buffer, hybridization (or affinity binding), and denaturing solutions necessary for the biochemical procedures set forth in FIG. 1 .
For the magnetic sifter shown in FIG. 6 , the sample flow rate will be limited by the width of the slits at the bottom of the substrate or the gaps of the soft magnets, whichever is smaller. Thus, this invention also provides a self-aligned fabrication method of a micromachined magnetic sifter with a high density of slits so that the sample flow rates can be greatly enhanced compared to the magnetic sifter shown in FIG. 6 . First, the bottom side of a (100) Si substrate 710 is thermally oxidized or coated with SiN x or other appropriate materials to form a membrane layer 720 ( FIG. 7 a ). Then the Si substrate 710 (but not the SiO 2 or SiN x membrane layer) is anisotropically wet etched ( FIG. 7 b ) to form openings 730 . In this case the Si opening widths are much greater than those in FIG. 6 . Third, the membrane layer 720 is etched (e.g., using reactive ion etching or RIE) into small rectangular slits, which are closely spaced while maintaining the mechanical strength of the membrane ( FIG. 7 c ). Fourth, a soft magnetic layer is coated on the bottom side of the wafer without using a masking layer ( FIG. 7 d ). Finally, the soft magnetic layer is etched into rectangular strips similar to those shown in FIG. 2 except that their widths and gaps are much smaller. The dimensions of the strips are limited only by the thickness of the membrane layer and the RIE process.
The sample flow rate is limited by the width of the membrane slits. Since the membrane slits in the sifter shown in FIG. 7 can effectively occupy a much greater fraction of the Si substrate than in the sifter shown in FIG. 6 , a much higher flow rate is achieved. Furthermore, the smaller gaps between the soft magnets lead to a higher field gradient, which is desirable for a higher capture ratio.
A third fabrication process is shown in FIG. 8 . With this method, approximately 1 μm of SiN x (low stress) is deposited on an about 375 μm thick double polished Si (100) wafer 810 to form a thin membrane 820 ( FIG. 8 a ). Next, a first mask is used to anisotropically dry etch the Si to give openings 830 with side walls of nearly 90° ( FIG. 8 b ). Third, the SiNx layer 820 is anisotropically dry etched using a second mask to give slits 840 ( FIG. 8 c ). Photoresist can then be coated around the active region with a third mask. Next, approximately 1 μm of NiFe 850 is sputter plated (or electroplated, if needed) ( FIG. 8 d ). Unwanted NiFe is then lifted off and the NiFe is passivated if needed. Finally, the wafers may be diced and bonded to syringes.
A key issue in the fabrication process shown in FIG. 8 is that the width of the etched cavities at the bottom may vary. If the thickness varies by ±15 μm, and the dry etch sidewall angle is 10 degrees, then the bottom width may be 66±3 μm narrower than the top width. The design of the second mask must tolerate this variation. Thus, the Si bottom openings are designed to be 200 μm wide, and each side may vary by ±3 μm, so the SiN x slits are chosen to be approximately 11 μm away. Each 200 μm width bottom translates into 200 μm+2×66 μm=332 μm. If the length of the cavities is also chosen to be 332 μm, one can fit about π×(2.5 mm) 2 /(0.332 mm) 2 =˜178 in one syringe. If 25% of 200 μm×200 μm SiN x is etched, and the flow speed at the bottom of the slits is 1 mm/s, then the flow rate is 25%×178×0.04 mm 2 ×1 mm/s=1.8 μl/s or 0.11 ml/min. This allows capture of a large number of capture probes.
FIG. 9 shows a preferred layout for a magnetic sifter 900 according to the present invention. The size of the slits in each honeycomb 910 is preferably around 2 μm×5 μm. The white areas surrounding and between honeycombs is unetched Si/SiNx 920 , which provides rigidity to the sifter. A diagram of the layout of individual honeycombs 910 , with slits 912 , is shown in FIG. 10 . The grid step size is 10 μm in this layout, and is preferably in the range of about 5 to 20 μm. FIG. 11 shows a micrograph of a fabricated magnetic sifter according to the present invention, with unetched Si/SiNx 920 , honeycombs 910 , and slits 912 indicated.
A key element of the present invention is that the released nanotags and capture probes can be optionally reused as detection probes to “stain” the same target molecules which are eventually immobilized on a magnetic biochip (see U.S. patent application Ser. No. 10/829505, filed Apr. 22, 2004 for details on using nanotags as detection probes). At that stage the nanotags generate a magnetic signal, which can be used to identify and quantify the target molecules on the biochip. Thus, the present invention also provides an integrated magnetic biosensor with a sample preparation chamber 1210 and detection chamber 1220 in one cartridge 1200 as illustrated in FIG. 12 . The two chambers are interconnected with a fluidic channel 1230 . After mixing the raw sample containing target DNA/RNA fragments (or proteins) with capture probes, the mixture is delivered to the sample preparation chamber 1210 of the cartridge 1200 via one of the inlets 1270 , and the impurities are washed away from one of the outlets 1280 while the targets are trapped by the magnetic sifter 1212 . In one embodiment of the present invention, the nanotag-labeled targets are first released as shown in FIG. 4 and subsequently delivered to a detection chamber 1220 containing a MagArray® chip 1222 (see U.S. application Ser. No. 10/829,505, filed Apr. 22, 2004, which is incorporated by reference herein). The nucleic acid or protein targets are then interrogated. The inlets, 1270 , outlets 1280 and interconnect fluidic channel 1230 are all equipped with valves (not shown). The compact cartridge 1200 is situated near three pairs of electromagnets: 1240 is for applying the longitudinal bias field (relatively small) to the magnetic sifter 1212 (when releasing the nanotags) and to the magnetic sensors on the MagArray® chip 1222 ; 1250 is for saturating the soft magnets when trapping the nanotags; 1260 is for applying modulation field to the MagArray® chip 1222 during the magnetic readout of nanotags bound on the MagArray® chip 1222 .
In another embodiment of the present invention, after washing away the impurities the captured targets in the sample preparation chamber 1210 are harvested with a denaturing step before releasing the nanotags. These targets are subsequently delivered to detection chamber 1220 to bind with immobilized probes on the MagArray® chip 1222 . Then the nanotag-labeled probes are released from the sample preparation chamber and delivered to the detection chamber 1220 to “stain” the specific targets bound on the chip. To speed up the staining process, one can optionally inject additional nanotag-labeled probes to the detection chamber 1220 in this step. Afterwards the MagArray® chip 1222 is read out to identify and quantify the targets present in the original sample.
The magnetic sifter in combination with magnetically tagged target molecules has many applications in the biological sciences. For example, DNA, RNA, proteins, and pathogens may be detected. In addition, targets that are part of a cell or organism may be identified. Finally, target molecules may be biomarkers of disease, including, but not limited to, cancer, heart disease, neurological disease and infectious disease. The examples of such applications provided below are for illustrative purposes only, and do not limit the scope of the present invention.
The nanotag-labeled probes shown in FIG. 1 can be used for pathogen extraction as well as pathogen detection. For example, important pathogens in sepsis include candida, staphylococcus, enterobacterium , and E. coli , among others. These pathogen targets can be fished out of a raw sample using the magnetic sifter with capture probes that hybridize with an oligomer of each target. The denatured pathogen targets can then be hybridized to a magnetic biochip. The immobilized probes at each site hybridize to another oligomer of each pathogen target. Afterwards the released nanotag-labeled capture probes can be used as detection probes to “stain” the magnetic biochip. Finally, the identity and quantity of each pathogen target can be read out magnetically by counting the number of nanotags at each specific site of the chip.
The above scheme can be adapted for human papillomavirus (HPV) detection and genotyping. For example, the capture probes can be oligomers that bind to the common ends of the E1 region of numerous HPV types. After releasing the various E1 regions from the magnetic sifter, their polymorphisms can be interrogated by a magnetic biochip in a similar manner. Of course, the immobilized probes in this case are specific probes complementary to the E1 regions of targeted HPV types.
Nanotag-labeled probes can also be used for human genomic DNA sample extraction and profiling. In short tandem repeat (STR) based DNA profiling and human identification using, e.g., the Combined DNA Index System (CODIS), a unique set of 13 loci in non-coding regions of human DNA are used to identify any person based on the STR alleles at each locus. Each locus is flanked by specific oligomers. Therefore, 13 capture probes can be designed that are complementary to the flanking oligomers of all 13 loci. The capture probes can then be labeled with magnetic nanotags. Using the magnetic sifter shown in FIG. 1 these probes can separate all the STR-containing DNA fragments out of a raw sample after lysis. The STR alleles can then be interrogated with microarrays with variable length probes either by enzymatic digestion, as described in U.S. patent application Ser. No. 11/125,558, filed May 10, 2005, or by branch migration assay, as described in U.S. patent application Ser. No. 11/231,657, filed Sep. 20, 2005, both of which are incorporated by reference herein. For example, as, nanotag-labeled capture probes hybridized with three-repeat STR targets may be further hybridized with variable length probes, ranging from one to three repeats, on a magnetic microarray. After enzymatic digestion with a single strand nuclease, or branch migration assay, the nanotags at the sites having variable length probes with one or two STR repeats will be removed while those at the site with three repeats remain. The step change in the signal strength from the first two sites to the third site will indicate the presence of the three-repeat STR allele. By spotting all the probes covering all the alleles of the 13 loci specified by CODIS in a single magnetic microarray, one can uniquely identify any person with magnetic nanotag-labeled capture/detection probes.
Nanotag-labeled probes can also be used for protein extraction and profiling such as in proteomics-based biomarker validation and cancer diagnostics. Nanotag-tethered antibody probes can capture specific protein targets. Then the protein targets can be delivered to a magnetic microarray with immobilized probes (such as aptamers or antibody probes) which specifically bind the protein targets that have already been labeled with magnetic nanotags. The protein targets can eventually be identified and quantified by magnetically detecting the nanotags at various sites on the microarray.
While it is advantageous to use the same probes for both capture and detection of target molecules as set forth, it is possible and sometimes preferable to use slightly or entirely different probes and labels in the capture and detection of target molecules. While magnetic labels must be used in conjunction with the magnetic sifter, other labels such as fluorescent dyes can be used in the detection of target molecules.
As one of ordinary skill in the art will appreciate, various changes, substitutions, and alterations could be made or otherwise implemented without departing from the principles of the present invention. Accordingly, the scope of the invention should be determined by the following claims and their legal equivalents.
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The present invention provides a magnetic sifter that is small in scale, enables three-dimensional flow in a direction normal to the substrate, allows relatively higher capture rates and higher flow rates, and provides a relatively easy method of releasing captured biomolecules. The magnetic sifter includes at least one substrate. Each substrate contains a plurality of slits, each of which extends through the substrate. The sifter also includes a plurality of magnets attached to the bottom surface of the substrate. These magnets are located proximal to the openings of the slits. An electromagnetic source controls the magnitude and direction of magnetic field gradient generated by the magnets. Either one device may be used, or multiple devices may be used in series. In addition, the magnetic sifter may be used in connection with a detection chamber.
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This application is a Continuation of application Ser. No. 09/421,930, filed Oct. 21, 1999, now abandoned.
BACKGROUND OF THE INVENTION
1. Field of the Invention
The invention relates to an explosion relief valve for confined spaces, volumes or vessels, and more particularly for the crankcase of internal combustion engines, which includes a valve seat which may be fitted into a boundary wall of the space to be protected, a spring-loaded closure plate co-operating with the valve seat and at least one flame barrier having low pressure resistance installed in a gas path leading through the valve, which flame barrier preferably consists of sheet-metal strips stacked one above another transversely to the throughflow direction of the gas, which sheet-metal strips are preferably provided at least over part of their width with irregular corrugations, and at least one other perforated wall in the gas path.
2. The Prior Art
A valve of this kind is described in DE 1 126 676 C and GB-A-2 017 269. Two flame barriers, one disposed behind the other, are provided in the relief valves described therein, the British publication disclosing the combination of a sheet-metal ring stack with expanded metal fabric layers disposed thereafter. However, there is no mention whatsoever in that publication of structures which increase the mechanical stability and/or of affecting the flow characteristic.
A valve of an even simpler design is described in AT 311 129 and has very low conductance, a heat absorption capacity sufficient to prevent flames from passing through the valve being achieved without the application of vaporizable substances by means of the sheet-metal strips acting like cooling ribs. On the other hand, however, because of the substantially parallel sheet-metal strips, the flow resistance is not inadmissibly increased and the gas is able to flow away in a linear manner, with the result that the overpressure in the space protected by the valve can easily be reduced.
Particularly important as fields of application for explosion relief valves of this kind are the protection of confined spaces such as, for example, the crankcases of two-and four-stroke diesel engines, gas containers, fairly large pipelines and other spaces in which explosive substances are stored or in which highly inflammable gases may form. Several of the relief valves described may also be provided in parallel or in series.
It is desirable to provide a valve of the type specified in the introduction, in which a flame front is in every case reliably prevented from passing through the explosion relief valve for all fields of application, the throughflow of the valve is optimized, and the valve is also protected against mechanical damage, even after repeated explosions.
SUMMARY OF THE INVENTION
According to the invention, the perforated wall is made of an expanded metal strip. This material offers the facility of controllably influencing the flow behavior, and the shape and location of the lozenge-shaped openings of the expanded metal and the alignment of the webs can be selected depending on the influence desired. The corresponding uniform turbulence enables the cooling capacity of the flame barrier to be optimally utilized without excessively increasing the flow resistance. As well as making the flow through the other expanded metal perforated wall more uniform, the characteristics of the frame front, if applicable, are changed in such a way that no sparks form in closely confined areas, but rather distribution takes place over a larger area with the result that the heat absorption capacity of the flame barrier is better utilized and no local overloads are able to occur. The time taken for the flame front to pass through the valve is also thereby increased. The passing of any flames through the valve can thus be reliably prevented. Diesel and gas engines protected with the valve according to the invention can therefore also be used in hazardous areas, and/or complicated above-roof pressure and flame outlets are no longer necessary, and the non-hazardous relief of pressure into the working space is possible. The expanded metal of the valve construction provides greater mechanical strength, on the other hand, enabling even repeated explosions to be withstood without deformations occurring which adversely affect operation, the valve remaining fully effective and operational. This is of great economic significance as the overriding majority of ships today are built without redundancy and the failure of the one and only engine may have dire consequences.
The effect of influencing the flow for improved utilization of the cooling capacity of the flame barrier is revealed particularly clearly if at least one expanded metal wall is positioned immediately in front of the first flame barrier.
According to another optional feature of the invention, on the other hand, at least one perforated wall may be positioned immediately after the last flame barrier.
According to another optional feature of the invention, at least one flame barrier and a perforated wall may be positioned behind the valve seat. As a result the first pressure peaks are caught by the closure plate of the valve before they impinge on the first flame barrier and/or perforated wall, which are thereby better protected from damage.
In order to achieve a directed gas flow after its exit from the explosion relief valve, the perforated wall is preferably made of expanded metal and its webs are set in such a way that the gas flow emerging from the valve is directed at the surface of the space to be protected. This means that even in the most confined conditions, danger to operating personnel may be prevented to the greatest possible extent and without great effort.
With the advantage of structural simplicity, the saving of weight and the low space requirement, the valve behind the last flame barrier can be free of any deflecting devices for the emerging gas flow. On the other hand, if there is available space provision, the valve may be larger in size and thus be more reliable in operation and/or suitable for higher explosion pressures.
Advantageously, according to another optional feature of the invention, at least one flame barrier may be annular and permit throughflow over substantially 360° and at least one additional perforated wall may be provided in an annular shape on the exterior or interior periphery of at least one flame barrier. This feature increases the effectiveness of the action to make flow more even and ensures the least possible load per unit area on the flame barrier and also on the other perforated wall.
To achieve advantageous weight and also size optimization and more economic production, at least one flame barrier may be made of aluminium or stainless strip steel.
A preferred embodiment of the present invention will be described in more detail with reference to the accompanying drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is an axial center section to an explosion relief valve according to the invention;
FIG. 2 is a corresponding section through a second relief valve according to the invention; and
FIG. 3 is a corresponding section through a third relief valve according to the invention, showing two different arrangements.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
The explosion relief valve represented in FIG. 1 is a version suitable above all for ships' engines and also diesel and gas engines for power plants, this version being installed in the crankcase or installation wall to avoid damage to the engine or installation when, specifically, gas or oil mist explosions occur. The valve consists of an annular valve seat 1 which is fixed externally by means of screws 2 or the like to an opening in the crankcase wall 3 . Cooperating with the valve seat 1 is a closure plate 4 loaded by means of a helical compression spring 5 wound preferably in an approximately conical shape. In addition, stay bolts 6 are screwed into the valve seat 1 concentrically around the closure plate 4 and hold an arresting device 7 which is designed as a cover plate and has a peripheral region bent towards the crankcase deflector 3 , at a distance from the valve seat 1 ; the bolts 6 are at the same time used for laterally guiding the closure plate 4 . The helical compression spring 5 is also supported on the valve cover or guard 7 . A sealing ring 8 fitted in a groove in the valve seat 1 ensures tight sealing in the closed position.
The relief valve is provided, preferably behind the valve seat 1 and the closure plate 4 viewed in the direction of flow, in a known manner with at least one flame barrier 9 positioned concentrically around the stay bolts 6 , for example, the flame barrier 9 thus being in the gas path leading through the opening in the valve seat 1 . The flame barrier 9 consists preferably of sheet-metal strips 10 stacked one above another, corrugated over part of their width, preferably that part nearer the centre of the valve, and loosely clamped between the valve seat 1 and the guard 7 . The corrugations extend preferably over about half the width of the strips 10 and their height decreases continuously from the inside edge of the strips 10 radially outwards. If necessary, non-corrugated, flat sheet-metal strips may also be inserted between the corrugated sheet-metal strips 10 .
In the embodiment of FIG. 1, there is at least one other perforated wall 11 immediately in front of the flame barrier 9 , preferably in front of the first flame barrier in the case of a consecutive series of flame barriers, in addition to the flame barrier 9 . This perforated wall 11 , like the flame barrier 9 also preferably behind the valve seat 1 and the closure plate 4 viewed in the direction of flow, is made of expanded metal, which is known per se. The webs and perforated openings thereof may be shaped as required so as to produce, when applied to the particular geometry of the valve, a more uniform pressure characteristic and flow characteristic of the explosion gases and to slow down the flame front so that the passing of the flame barrier 9 also takes longer and the gases are therefore better able to cool down. Moreover, the perforated wall 11 gives the valve construction greater mechanical stability, with the result that smaller sizes are possible with the same safety requirements and explosions do not directly lead to damage to the valve, i.e., it remains operational.
If an explosion occurs in the crankcase, the increase in pressure thereby produced causes the closure plate 4 to be lifted off the valve seat 1 against the force of the spring 5 and to move as far as the guard 7 . The valve opening of the valve is thereby freed, with the result that the explosion gases are able to flow away through the valve seat 1 , the perforated wall 11 and the flame barrier 9 towards the exterior, causing a rapid release of pressure to occur in the crankcase. The perforated wall 11 causes the gases to slow down and the pressure distribution and flow to become more uniform over the whole extent of the valve, so that no excessive local pressure peaks are able to occur. The flame barrier 9 then extinguishes the flames and, due to the cooling of the gases flowing—relatively slowly because of the effect of the perforated wall 11 —and the widening flow cross-section, prevents the flames from escaping to the exterior through the relief valve. The cooled gases are deflected towards the engine by the edge of the arresting device 7 which is bent towards the crankcase, so that danger to operating personnel is minimized.
The embodiment of FIG. 2 has, as well as the perforated wall 11 positioned immediately in front of the flame barrier 9 , another perforated wall 12 which is immediately behind the flame barrier 9 , if necessary immediately behind the last one of a series of flame barriers. While the inner expanded metal wall 11 is preferably clamped like the sheet-metal strips 10 of the flame barrier 9 between the valve seat 1 and the guard 7 , there are several attachment options for the outer perforated wall 12 .
As represented on the left-hand side of FIG. 2, the valve seat 1 may have a portion 3 a projecting radially outwards and the perforated wall 12 may be clamped between this portion 3 a and the guard. On the right-hand side of FIG. 2 another attachment option is shown, in which the flame barrier 9 and the two perforated walls 11 , 12 are joined together by means of metal rings 13 , 13 a flanged on the outer and inner edge to form a stack which can be handled all together, like a filter cartridge. This stack may be replaced as one piece and the stack is held in its entirety by being clamped between the valve seat 1 and the arresting device 7 .
In FIG. 3 —without going into the precise manner of its attachment—a single perforated wall 12 made of expanded metal behind the flame barrier 9 is shown, the webs 12 a of which are set in relation to the sheet-metal strips 10 of the flame barrier 9 , and thus also the emerging gas flow, in such a way that these gases are deflected towards the installation (ie. downwards as shown in FIG. 3 ). This means that there is no need for any other deflecting device, specifically the edge of the guard 7 bent towards the engine or the installation, which in this case should be flat on the outer edge and whose maximum diameter should be the size of the flame barrier 9 together with the perforated wall 12 . Thus, with the same dimensions of the valve seat 1 , and also of the flame barrier 9 , this valve requires less space or the valve seat 1 may have a larger diameter if there is available space.
The perforated walls 11 , 12 , like the flame barrier 9 also, are preferably manufactured from material which is a good heat conductor and advantageously is relatively light, for example aluminium or stainless strip steel. Because the valve construction is reinforced by the at least one perforated wall 11 , 12 , despite the light materials there is no fear of any loss of mechanical strength.
While the present invention has now been described in detail with respect to specific embodiments, changes can be made therein and still fall within the scope of the appended claims.
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An explosion relief valve for a confined space, more particularly for the crankcase of an internal combustion engine, includes a seat ( 1 ) which may be fitted into a boundary wall ( 3 ) of the space to be protected, a spring-loaded closure plate ( 4 ) cooperating with the valve seat, at least one flame barrier ( 9 ) having low pressure resistance in the gas path leading through the valve, preferably consisting of sheet-metal strips stacked one above another transversely to the throughflow direction of the gas, which sheet-metal strips are provided preferably at least over part of their width with irregular corrugations, and at least one other perforated wall ( 11, 12 ) in the gas path of expanded metal.
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CROSS REFERENCE TO RELATED APPLICATIONS
[0001] This application is a continuation of U.S. patent application Ser. No. 10/091,838 filed by Dean C. Alberson, et al., on Mar. 6, 2002, which is hereby incorporated by reference.
TECHNICAL FIELD OF THE INVENTION
[0002] The present invention relates generally to crash cushions and terminals used in highway applications to mitigate and preclude injuries to occupants of errant vehicles.
BACKGROUND OF THE INVENTION
[0003] Roadway crash cushions are widely used to absorb impacts and decelerate impacting vehicles in a controlled manner. Typically, crash cushions are positioned to shield fixed objects located within the roadway environment. Crash cushions are often positioned in front of obstacles such as concrete columns and abutments. Also, crash cushions are often located at the end of a guardrail installation to prevent the upraised end of the guardrail from spearing an impacting vehicle.
[0004] There are numerous crash cushion designs known that rely upon frangible members, or members that are intended to shatter or be destroyed upon impact, to absorb the energy associated with a vehicular impact. Examples are found in U.S. Pat. No. 3,768,781 issued to Walker et al. and U.S. Pat. No. 3,982,734 issued to Walker (both employing energy cells having internal frangible members of e.g., vermiculite). One problem with the use of frangible members is the crash cushion must be completely replaced after each collision. Thus, time and expense is incurred in replacing the frangible members.
[0005] A number of previous crash cushion designs rely upon the permanent deformation of plastics or steels to absorb the kinetic energy of errant impacting vehicles. A design of that nature suffers from the same drawbacks as those designs incorporating frangible members. The cost and time associated with replacing or repairing the deformed portions of the cushion is significant.
[0006] There have been a few attempts to provide reusable or restorable crash cushions. However, for the most part, these attempts have proven impractical or unworkable in practice. U.S. Pat. No. 4,452,431 issued to Stephens et al, for instance, describes a crash cushion wherein fluid filled buffer elements are compressed during a collision. It is intended that energy be absorbed as the fluid is released from the buffer elements under pressure. In practice, it is difficult to maintain the fluid filled cylinders as they are prone to loss of fluid through evaporation, vandalism and the like. Also, after a severe impact, holes or punctures may occur in the buffer elements rendering them incapable of holding fluid.
[0007] U.S. Pat. No. 4,674,911 issued to Gertz describes a pneumatic crash cushion that is intended to be reusable. This crash cushion employs a plurality of air chambers and valve members to absorb and dissipate impact energy. This arrangement is relatively complex and prone to failure. In addition, the numerous specialized components used in its construction make it expensive.
[0008] The Reusable Energy Absorbing Crash Terminal (“REACT”) 350 is a crash cushion wherein a plurality of polyethylene cylinders are used to absorb impact energy. The cylinders are retained within a framework of side cables and supporting frames. This system is effective and reusable to a great degree due to the ability of the cylinders to restore themselves after impact. The cylinders typically return to 85%-90% of their original shape after impact. Unfortunately, the REACT system is also expensive to construct. The number of manufacturers producing large diameter polyethylene cylinders is limited and, as a consequence, prices for the cylinders are elevated.
[0009] An improvement that addresses the problems of the prior art would be desirable.
SUMMARY OF THE INVENTION
[0010] The present invention provides devices and methods relating to roadway crash cushions. An energy absorbing terminal is described that is made up of a plurality of cells partially defined by cambered panels made of thermoplastic. The panels are supported upon steel diaphragms. The cambered portion of the thermoplastic panels provides a predetermined point of flexure for each panel and, thus, allows for energy dissipation during a collision. The stiffness of the crash cushion is variable by altering material thicknesses and diaphragm spacing.
[0011] In operation, a vehicle colliding in an end-on manner with the upstream end of the energy absorbing terminal will cause the cambered panels to bend angularly at their points of flexure and, thus, cause the cells to collapse axially. The use of thermoplastic, such as polyethylene, results in a reversible, self-restoring collapse of the terminal, meaning the terminal is reusable after most collisions.
[0012] The invention provides a number of advantages over conventional crash cushions, including cost, ease of construction, and maintenance.
BRIEF DESCRIPTION OF THE DRAWINGS
[0013] FIG. 1 is a plan view of an example crash cushion arrangement constructed in accordance with the present invention prior to impact from an errant vehicle.
[0014] FIG. 2 is a side view of the arrangement depicted in FIG. 1 .
[0015] FIG. 3 is a plan view of the crash cushion depicted in FIGS. 1 and 2 after being struck by an impacting vehicle.
[0016] FIG. 4 is a front view of a diaphragm used within the crash cushion shown in FIGS. 1, 2 , and 3 .
[0017] FIG. 5 is a side view of the diaphragm shown in FIG. 4 .
[0018] FIG. 6 is a plan view of the diaphragm shown in FIGS. 4 and 5 .
[0019] FIG. 7 is a schematic depiction of an exemplary crash cushion shown prior to an end on impact by a vehicle.
[0020] FIG. 8 is a schematic depiction of the crash cushion shown in FIG. 7 , at approximately 0.18 seconds following an end-on impact.
[0021] FIG. 9 is a schematic depiction of the crash cushion shown in FIG. 7 , at approximately 0.27 seconds following an end-on impact.
[0022] FIG. 10 is a schematic depiction of the crash cushion shown in FIG. 7 , at approximately 0.345 seconds following an end-on impact.
DETAILED DESCRIPTION OF THE INVENTION
[0023] FIGS. 1-3 illustrate an example hybrid energy absorbing reusable terminal (“HEART”) crash cushion 10 that is constructed in accordance with the present invention. The crash cushion 10 is shown installed on a concrete pad 12 (visible in FIG. 2 ) that has been placed within a section of ground 14 . Although not shown, it should be understood that the crash cushion 10 is typically installed adjacent a rigid obstacle, such as a bridge abutment, concrete post or other barrier. In addition, the crash cushion 10 may be located at the upstream end of a guardrail installation.
[0024] The crash cushion 10 includes a nose portion 16 , central body portion 18 and downstream end portion 20 . An approaching vehicle 22 is shown adjacent the nose portion 16 of the cushion 10 in FIGS. 1 and 2 . The nose portion 16 consists of a sheet of plastic, or other suitable material, that is curved or bent into a “u” shape. The nose portion 16 may be painted with a bright color, such as yellow, or have reflective tape applied so that the cushion 10 may be easily recognized by drivers. The downstream end portion 20 includes a pair of upstanding rigid posts 24 , 26 that are typically formed of concrete or steel and are securely anchored, either to the ground 32 or to an adjacent abutment, post or other barrier (not shown).
[0025] The central body portion 18 also includes a steel basetrack formed from a pair of parallel rail members 28 , 30 that are attached to the ground 32 . Anchor members 19 , such as bolts, are typically used to secure the rail members 28 , 30 to a concrete slab 21 . The central body portion 18 features a plurality of openings 34 that are arranged linearly along the length of the cushion 10 . In the described embodiment, the openings 34 are shown to be hexagonally shaped. While the hexagonal shape is presently preferred, it should be understood that other suitable shapes may be used, including, for example, octagonal, rectangular and square. The central body portion 18 incorporates two substantially parallel rows 36 , 38 of cambered panels that are arrayed in an end-to end manner along their lengths. The panel rows 36 , 38 may comprise a single integrally formed sheet of plastic. Alternatively, they may be formed of a number of individual cambered panel members placed in an end-to-end, adjoining manner at each rectangular frame 40 . It is presently preferred that the rows of panel members 36 , 38 be formed of polyethylene. A suitable polyethylene material for use in this application is PPI recommended designation PE 3408 high molecular weight, high density polyethylene. A currently preferred thickness for the panel members 36 , 38 is approximately 1¼″. It is noted that the panel members 36 , 38 are created so as to be substantially stiff and sturdy in practice and to possess substantial “shape memory” so that they tend to substantially return to their initial form and configuration following elastic deformation. Presently, panel members having a secured in place height of about 20 inches have provided suitable resistance to collapse and sufficiently return to original shape. It is noted that the thickness of a given panel member as well as its height may be adjusted as desired to increase or decrease resistance to expected end-on collision forces. For example, increasing the height of the panel members 36 , 38 will increase the amount of panel material that would be bent by a colliding vehicle and would, therefore, be stiffer than a cushion that incorporated panel members of lesser height.
[0026] The crushable cells include rectangular frames or diaphragms 40 that join the parallel panel rows 36 , 38 together. In the drawings, individual diaphragms are designated consecutively from the upstream end of the cushion 10 as diaphragms 40 a , 40 b , 40 c , etc. The diaphragms 40 are preferably formed of steel box beam members welded to one another. In a currently preferred construction, bolts or rivets 42 (visible in FIG. 2 ) are used to affix the panel rows 36 , 38 to the frames 40 . Referring now to FIGS. 4-6 , a single exemplary diaphragm, or frame, 40 is shown in greater detail. The diaphragm 40 includes a widened upper portion, generally shown at 50 , and a narrower lower portion 52 . The lower portion 52 includes a pair of generally vertically oriented support members 54 and a connecting cross-piece 56 . U-shaped engagement shoes 58 are secured to one side of each of the support members 54 and slidably engage the rail members 28 , 30 . The upper portion 50 includes a pair of vertically disposed side members 56 , 58 with upper and lower cross-members 60 , 62 that interconnect the side members 56 , 58 to form a rectangular frame. Additional vertical and horizontal cross-members 64 , 66 , respectively, are secured to one another within the rectangular frame for added support. Plate gussets 68 are welded into each comer of the rectangular upper portion 50 in order to help to maintain rigidity and stiffness for the diaphragm 40 .
[0027] Tension cables are used to provide the crash cushion additional strength and stability and, thereby, materially assist in the lateral redirection of side impacts into the cushion 10 . As shown in FIGS. 1 and 2 , a pair of forward, or upstream, tension cables 72 , 74 are disposed through a forward plate 76 , threaded through the upstream diaphragms 40 a , 40 b and are then secured to the third diaphragm 40 c . A currently preferred method of securing the tension cables to a diaphragm is to secure a threaded end cap (not shown) onto each end of each cable and then thread a nut onto the end cap after passing the end cap through an aperture in the diaphragm. In the exemplary construction shown, a pair of rearward tension cables 78 , 80 are secured to the third diaphragm 40 c and extend rearwardly through corresponding diaphragm apertures toward the downstream end of the central portion 18 .
[0028] Longitudinal tension in the cushion 10 is provided by the side panels 36 , 38 that tend to want to remain in a substantially flattened (unfolded) configuration due to shape memory. As noted, prebending of the panels is done to provide a point of planned bending for the panels 36 , 38 at the cambered portions 44 .
[0029] FIGS. 7-10 are schematic representations of a crash cushion constructed in accordance with the present invention and illustrate the mechanics of collapse over time. In FIG. 7 , the cushion 10 has not yet been collapsed by an end on impact. Thus, the cushion 10 is at rest, and in a fully extended position. In FIG. 8 , an end on collision has taken place. The cushion 10 has been impacted by a vehicle (small car), shown schematically as load 82 , traveling at approximately 62 mph. The cushion 10 is shown at approximately 1.8 seconds into the collision in FIG. 8 . As can be seen, the cushion 10 has begun to collapse at two primary locations along its length. One of the locations 84 is proximate the upstream end of the cushion 10 . The second location 86 is proximate the downstream end of the cushion 10 . In FIG. 9 , the cushion 10 is shown approximately 0.27 seconds after the impact. By this time, a third location 88 of axial collapse has begun to form. This third location 88 is proximate the central point along the length of the cushion 10 . In FIG. 10 , the cushion 10 is essentially completely crushed or collapsed.
[0030] There are significant advantages to a system that provides for separate collapsing portions spread out in terms of location upon the cushion as well as time. These advantages include efficient use of material and aid in self-restoring nature of cushion. A collapse concentrated in one point along the length could cause that portion of the cushion 10 to be inelastically damaged.
[0031] As noted, the cells 34 may be hexagonal, octagonal, rectangular or square in shape, being formed between two adjacent frames 40 and the two panel rows 36 , 38 . As shown in FIG. 1 , the cells 34 need not all be the same size. The different lengths of the cells provides for differing resistances to collapse. The frames 40 have rollers or shoes (not shown) that engage the rails 28 , 30 in a manner known in the art so that the frames 40 may move longitudinally along the rails 28 , 30 . During an end-on collision with the crash cushion 10 , there is a dynamic wave that propagates through the cushion 10 and may collapse sections other that the lead sections (defined between the upstream frame 40 a , 40 b , 40 c , and 40 d ). Additionally, some inertial properties can be used by collapsing the segments in varying order.
[0032] It is noted that each of the panel segments, such as segment 43 of each row 36 , 38 are cambered at a point 44 approximately midway between adjacent frames 40 . This cambered portion 44 forms a point of flexure and preplanned weakness for the panel segment 43 , thereby permitting the segment 43 to collapse upon the application of an end-on force. The bend also prevents large acceleration spikes from being needed for initial column buckling of the segments 43 . Currently, it is preferred that the amount of bend at the cambered point 44 be about 5-10 degrees, as this amount of bend has been found to provide enough eccentricity to assure proper buckling. The bend at the cambered point 44 may be formed by using a press device of a type known in the art.
[0033] In operation, the cells 34 are substantially, reversably compressed during an end-on impact by a vehicle 22 . The use of a resilient, thermoplastic material, such as polyethylene, ensures that the terminal 10 will be self-restoring after minor end-on impacts. The nose 16 may be crushed during the impact, but should be easily replaceable. The posts 24 , 26 serve as a reinforcement portion at the downstream end of the terminal 10 . The central portion 18 is compressed against the posts 24 , 26 .
[0034] The terminal 10 of the present invention provides a number of advantages over prior art terminals. The first is cost. As compared to systems that incorporate polyethylene cylinders, suitable sheets of polyethylene may be obtained readily and inexpensively from a number of suppliers. Secondly, if it becomes necessary to replace one or more of rows 36 or 38 , or individual panels 43 within those rows, this may be accomplished quickly and easily, requiring only removal and replacement of the fasteners 42 used to secure them to the frames 40 .
[0035] Those of skill in the art will recognize that many changes and modifications may be made to the devices and methods of the present invention without departing from the scope and spirit of the invention. Thus, the scope of the invention is limited only by the terms of the claims that follow and their equivalents.
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An energy absorbing terminal is described that is made up of a plurality of cells partially defined by cambered panels made of thermoplastic or another suitable material. The panels are supported upon rectangular frames. The cambered portion of the panels provides a predetermined point of flexure for each panel and, thus, allows for energy dissipation during a collision. The stiffness of the crash cushion may be varied by altering material thicknesses and diaphragm spacing. In operation, a vehicle colliding in an end-on manner with the upstream end of the energy absorbing terminal will cause each of the cambered panels to bend angularly at its point of flexure and, thus, cause the cells to collapse axially. The use of thermoplastic, such as polyethylene results in a reversible, self-restoring collapse for the terminal, meaning that the terminal is reusable after most collisions.
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FIELD OF THE INVENTION
[0001] This mechanical process involves propagating subsurface pressure (excitation) waves that strain elastic porous media or fractured geologic media such that the induced pressure wave energy increases pore space, voids, or aperture size. The pressure waves promote a dynamic porosity that also increases pore size and interconnectivity and simultaneously causes fluids to both dispense and disperse, and otherwise mobilize and flow. The process also causes residual fluids to flow and this is currently the only known method to have this effect on a range of geologic media. Collectively, the described flow effects are known as subsurface pulsing treatment (SPT). SPT is utilized to more accurately estimate the volume and/or mass of recoverable residual non-aqueous phase liquids (“NAPL”). One known means for propagating subsurface pressure waves is through the equipment and science disclosed in U.S. Pat. Nos. 6,241,019; 6,405,797; 6,851,473 and U.K. Patent Number 2324819. This technology is marketed under the trademarks DEEPWAVE, PRIMAWAVE and POWERWAVE.
BACKGROUND OF THE INVENTION
[0002] The remediation of soil and groundwater contaminated by light (lighter than water) non-aqueous phase liquids (LNAPL) and dense (heavier than water) non-aqueous phase liquids (DNAPL), collectively known as non-aqueous phase liquids (NAPL), remains a difficult problem where these contaminants exist as a residual (undissolved) or free product within a soil and/or rock matrix. LNAPLs (e.g., oily substances that float in water) and DNAPLs (e.g., chlorinated solvents, coal tar, creosote, that sink in water) are not readily removable in their entirety and continue to contaminate groundwater and soil and prevent or restrict use of the site in which these contaminants exist, or pose a threat of migration onto nearby properties. In the case of LNAPL, free product can adversely impact soil and groundwater and migrate onto other properties. Sometimes the LNAPL contains in solution other compounds that are even more toxic than the pure LNAPL (e.g., polychlorinated biphenyls [PCBs] or benzene), and in this case a less toxic LNAPL can serve as a transport medium for the more toxic compound(s).
[0003] One of the difficulties in remediation of LNAPLs and DNAPLs is that the mass or volume of contaminant is poorly understood or completely unknown. In the case of LNAPLs, invalid methods are most often employed to estimate the volume of contaminant, so the recoverable quantity of contaminant is overestimated or underestimated and the benchmarks for cleanup are uncertain or unknown; largely they are unattainable and unrealistic using conventional products and methods. The non-recoverable LNAPL, that portion sequestered within the soil or rock matrix, i.e. the residual, remains behind in pore spaces or voids and continues to adversely affect soils and groundwater. The residual is vastly more difficult to remove than the free product using conventional in situ methods and, in practice, removal is effectively infeasible.
[0004] In the case of DNAPLs, the contaminant volume and/or mass is also uncertain or unknown. Again, accurate, reliable estimates of the contaminant mass frequently do not exist. Removal of subsurface DNAPL is very difficult because these compounds dispense, forming fingers and pools making them very hard to locate and accurately quantify. Most of the DNAPL exists as a residual that occupies the pore spaces or voids and is exceedingly difficult to remove, treat, or otherwise access, depending on the site geological characteristics. As with LNAPL, DNAPL residual removal is effectively infeasible.
[0005] Removal of LNAPL and DNAPL meets with varying degrees of success depending on the recovery or treatment method, the understanding of the contaminant, geology, the mass or volume present and available for removal or treatment, and clear and attainable benchmarks for cleanup.
[0006] The reason why LNAPLs and DNAPLs are so difficult to remove is that the contaminants occupying the small voids, pore spaces, or apertures within the soil or rock matrix are strongly held and effectively immobilized by capillary forces. Depending on the size of the pores, voids, or apertures, the LNAPL or DNAPL is more strongly or weakly held; smaller openings hold contaminants more strongly No known conventional technology can effectively remove contaminants from the pores or voids while the geologic media remains in place (in situ).
[0007] Most often, contaminant levels are compared against numerical cleanup standards for soil or groundwater. However, the remedial process frequently, for practical purposes, ignores the mass or volume of contaminant. Effective remediation of the source mass or volume is paramount if remediation is to ultimately be effective and restore groundwater resources, soil, and real estate to productive use and protect the public and the environment. Removal and/or destruction of contaminant mass are of overriding importance.
[0008] One example of ground contamination remediation is discussed in U.S. Pat. No. 4,435,292. In this method, perforated pipes and wells are inserted into the ground of a contaminated site, wherein a number of the pipes and wells are pressurized and others are simultaneously evacuated to effect the transfer of flushing fluid through the soil to accelerate removal of contaminants, and to prevent migration of contaminants into other areas. The system is closed and pressurized at one end and evacuated at another end, for example, by evacuating ducts connected to a central pressure manifold. The flushing fluid may be either liquid or gaseous, e.g. an inert gas such as nitrogen, or a reactive system which would react with the contamination to form an inert or harmless chemical.
[0009] The process, however, suffers from the need to have a reliable benchmark as to the mass or volume of contaminant present so as to know how much treatment chemical is required and for how long treatment will take, and a reliable benchmark as to when the contaminant has been effectively neutralized or destroyed. The process relies on subsequent soil and groundwater contaminant measurements to determine when treatment is complete. These types of measurements are notoriously variable and a great many data points from a plurality of locations, over time and in several seasons are required to evaluate whether treatment is complete. Another important limitation of this approach is that the greatest contaminant concentrations do not necessarily coincide with the location of the greatest amount of contaminant mass or volume. Even with abundant measurements, rebound, i.e. the contamination from residual contaminant that continues to migrate back into groundwater, may appear well after the data suggest that remediation is complete. Without a reliable before and after estimation of volume or mass, effective treatment is uncertain and questionable. This issue is of great importance to environmental regulatory agencies, or other bodies charged with deeming remediation complete to protect the public and the environment.
[0010] The flushing process is also dependent on the geologic media that control fluid movement and how effectively the treatment method reaches the contaminants. Most commonly, treatment fluids follow preferential pathways, also known in the field as “fingering,” channels of easiest fluid movement and, as such, treatments and/or removal processes reach only a small percentage of the contaminant mass; most of the contaminant mass remains untreated, where it continues to adversely impact soil and groundwater. This method (Pat. No. 4,435,292) does not have the capacity to alleviate fingering as it relies on the inherent geologic properties and does not alter, i.e. increase, the conductivity of the geologic medium so as to promote or enhance remediation.
[0011] Another attempt at soil and groundwater decontamination is described in U.S. Pat. No. 5,279,740. This process represents an improvement over the aforementioned approach and consists of a mechanism of contaminant removal using at least two injection wells positioned in the contaminated zone and at least one extraction well to remove the mobilized contamination. Steam is then introduced into the ground and forced into the contaminated zone while simultaneously introducing treatment agents, if desired. A removal force is then applied to the extraction well for withdrawal of the contaminants. Enhanced removal and treatment are contemplated using this process. In an ideal setting, an array of steam injection wells and extraction wells covers the contaminated area. This process suffers from the same limitations noted in the first example. Without reliable estimates of contaminant mass or volume, the same deficiencies remain with regard to lack of meaningful benchmarks to gauge before and after treatment. The second example contemplates the use of an extraction well and an extraction force, but the approach is subject to the same limitation caused by preferential pathways, “fingering” that causes contaminant removal or treatment to contact only a fraction of the total contaminant mass, and typically the mass that is most easily treated and/or removed. Again, this process does not alter the conductivity of the geologic medium so as to promote or enhance remediation.
[0012] Other methods to alleviate soil and/or groundwater contamination employ the creation of a vacuum within a withdrawal well situated in the vadose zone. Air injected into the well at various points surrounding the withdrawal well urge the flow of contaminants towards the withdrawal well where they are vaporized and collected in the well by vacuum. Examples of this method are described in U.S. Pat. No. 4,593,760 and Re. 33,102.
[0013] A variation of the vacuum method mentioned above is discussed in U.S. Pat. No. 4,730,672, which presents a method for removing and collecting volatile liquid contaminants from a vadose zone of contaminated ground by an active closed-loop process, in which a vacuum source in a perforated conduit in a withdrawal well is situated in a contaminated vadose zone and creates a reduced pressure zone to cause contaminants contained therein to vaporize and be drawn in to the withdrawal conduit for collection and disposal. While effective for the removal of some easily volatilized liquid contaminants in the vadose layer, such methods have proved to be of limited value in the removal and disposal of many other common subsurface contaminants. Additionally, such methods are not useful for removal of contaminants situated below the water table in a saturated zone.
[0014] All the methods described above are employed either with or without any reliable measure of contaminant mass or volume, before and/or after, and work within the existing geologic framework. The effectiveness of these measures is dictated or limited by the existing porosity, voids, or aperture size, and permeability of the geologic media within which the contamination resides. One characteristic all the aforementioned methods have in common is that they treat the geologic conditions as though they are static and immutable. They focus exclusively on the concentration levels of contaminant and neglect soil, geologic and fluid physical properties.
[0015] Accordingly, there is a need for an integrated assessment-remediation process that accurately estimates the volume or mass of NAPL, rapidly removes the NAPL and/or treats the NAPL in situ, and then quantitatively evaluates whether the contaminant volume or mass has been remediated following treatment. There is a need for an evaluation process that factors both soil and fluid properties and/or changes in contaminant mass in estimating their mass and/or volume before, after and/or during treatment so as to monitor/adjust treatment effectiveness in real time. There is a need to more efficiently access the contamination so that it may be rapidly physically removed from the geologic media and/or treated with an agent that destroys and/or neutralizes the contaminant or otherwise renders it non-toxic. Restoration by means of rapidly altering the physical properties of the geologic media, e.g. porosity, conductivity and permeability, in the saturated zone below the water table and/or the capillary fringe above the water table, is fundamental to the process. By promoting more effective in situ remediation, the public will be protected because it will not be exposed to excavated contaminant that frequently results in noxious odors and toxic or nuisance particulates.
SUMMARY OF THE INVENTION
[0016] The present inventive process satisfies the above-stated need and provides for the improved removal and/or in situ treatment of contaminants from a contaminated subsurface area of the earth.
[0017] The combining of the capillary pressure method for yielding reliable before—and—after treatment estimates of LNAPL or hydrocarbon volume and mass flux method for providing reliable before and after treatment estimates of the mass of DNAPLs or chlorinated compounds with a remediation method that overcomes fingering and preferential pathways or other resistance in the geologic media by rapidly altering the physical properties of the geologic media (porosity, conductivity and permeability) in the saturated zone below the water table and in the capillary fringe above the water table to promote remediation, represents a unique and beneficial process for restoring groundwater and soil to protect the public and returning property to a useful purpose.
[0018] In accordance with this invention, there is provided a process for evaluation of mass and/or volume of contaminant in a saturated subsurface environment before removal and/or treatment, a means of promoting remediation by altering the physical properties of the geologic media such that fingering and paths of least resistance are overcome, resulting in vastly greater contact between the treatment agent and the contaminant, increasing the conductivity of the geologic medium, a means of treating and/or removing contaminant, a means of mobilizing residual NAPL, and a means of re-evaluating the effectiveness of treatment, if warranted, by means of reliably estimating the volume or mass of contaminant treated following the remediation process in the saturated zone and capillary fringe zone wherein the process comprises some or all of the following steps:
[0019] (a) Estimate the mass and/or volume of an LNAPL using a capillary pressure method such as that developed by Anne Farr et al. 1990 and Lenhard and Parker 1990 and modified by Adamski et al. 2005. This is to be accomplished using environmental site data collected for the specific purpose and/or using a priori data collected from earlier site investigation(s). Determine the area of retention of LNAPL using at least two soil borings and/or monitoring wells positioned such that they define the area of retention and characterize the free LNAPL in the Area of Retention. The borings and wells are positioned such that they extend from the vadose zone through the water table to some point below the seasonal water table fluctuation or LNAPL smear zone.
[0020] (a)(1) Estimate the amount of contaminant mass of residual LNAPL in soil or other geologic media using the soil sampling results for the contaminants of interest, using the method by Gallagher et al. 1995 or similar or equivalent method, and the sampling depth information to prepare contaminant mass estimates and/or prepare isocontours of the contaminant mass such that the amount and location of contaminant mass are reasonably approximated. The purpose of this step is to target to contaminant treatment areas most effectively and to determine the treatment dose of an amendment, if needed, so as to optimize treatment of the contamination, and as a basis for determining treatment effectiveness. This will shorten and improve the efficacy of remediation by accurately targeting the contaminant source mass.
[0021] (b) Collect water table measurements and product thickness measurements such that a reasonable estimate of water table fluctuation is known.
[0022] (c) Collect soil samples for analysis for the percent saturation of hydrocarbon and collect groundwater and LNAPL for fluid properties (density, surface tension, interfacial tension).
[0023] (d) Alternatively, if DNAPL is the contaminant, employ steps a, a(1), b, and c, but sample the wells for the dissolved DNAPL concentrations and estimate the DNAPL mass flux using the method presented by Einerson and Mackay. Use of the mass flux method is contemplated for both measuring the amount of contaminant and to serve as a means of monitoring treatment effectiveness by collecting serial groundwater measurements (before and after treatment) and as a means of adjusting treatment dosage to optimize the amount of treatment necessary. In this manner, additional treatments may be effected adding only the incremental amount of amendment needed, if necessary. This is a cost control measure and a means of keeping the amount of treatment chemical added to the environment to the minimum required for remediation.
[0024] (e) With the Area of Retention reasonably known and a reliable estimate of the recoverable contaminant volume and/or mass in hand or, in the case of DNAPL contamination, the mass flux and/or mass reasonably known through contaminant measurements, and the center of mass and location in physical space within the geologic media of the LNAPL or DNAPL reasonably known through testing and a workable site conceptual model, establish at least one SPT well within or near the contaminant mass, capable of allowing the means for inducing subsurface pressure waves that strain the geologic formation such that it results in a dynamic porosity that both dispenses and disperses fluids and at least one extraction well within the influence of the pulsing well.
[0025] (f) engage the pulsing well such that pressure waves develop in the subsurface so as to induce strain forces resulting in a dynamic porosity that both dispenses and disperses fluids in the subsurface. The pressure waves must be of the proper amplitude and frequency, consistent with the geologic properties, in order yield effective wave energy. Achieving the appropriate frequency and amplitude is an iterative process done in the field. Experience and knowledge of local conditions will have a far greater impact than any algorithm or process for determining frequency and amplitude values.
[0026] (g) applying a withdrawing force to the extraction well when removal of LNAPL or DNAPL is warranted, where the said LNAPL and/or DNAPL contamination is caused to be drawn through the contaminated subsurface area to cause at least a portion of said contaminants in said subsurface saturated and capillary fringe zone to be displaced toward the perforated lower portion of said extraction well, in liquid or vaporized form or in a combination thereof, and where said contaminants are withdrawn through the extraction well and removed from said contaminated subsurface area for further treatment and/or disposal. Use of technology simultaneously in conjunction with a withdrawal force constitutes a “push-pull” effect to enhance liquid contaminant extraction and treatment. Applying a withdrawal force has two purposes: (1) to actively promote and enhance removal of contaminant, and (2) to prevent any mobilized contaminant from reaching receptors such as river, streams, nearby properties, residences, etc.
[0027] In a preferred embodiment of the present invention, a process is provided for estimating the mass and/or volume of contaminants from a contaminated subsurface area of the earth having a subsurface water table, a subsurface saturated zone below the water table, and a capillary zone above the water table, and wherein contaminants are present in either or both the saturated zone and the capillary zone, and where the process comprises the steps of the following:
[0028] (a) establish at least one injection and excitation well extending downwardly from the surface of the ground, wherein the injection well(s) has a perforated lower portion allowing pressure wave and strain forces to emanate into the formation, and wherein said perforated lower portion of the injection well is disposed in or is proximate to the subsurface saturated zone and capillary fringe zone.
[0029] (b) establish at least one extraction and excitation well extending downwardly from the surface of the ground wherein the extraction well has a perforated lower portion allowing flow of material there into, and wherein the perforated lower portion of the extraction well is disposed in or is proximate to the subsurface saturated zone and the perforate lower portion of the other of the extraction wells is disposed in or is proximate to the capillary zone.
[0030] (c) induce pressure wave (SPT) excitation stimulus into at least one of said injection wells where the pressure waves induce strain causing a dynamic porosity in the geologic media from said perforated lower portion into the subsurface saturated zone and/or capillary zone.
[0031] (d) simultaneously or subsequently introducing nutrients, chemical oxidants, or other treatment agents into the injection well wherein the treatment agents are caused to flow from the lower perforated portion of the injection well into the pores, voids, or apertures in the saturated zone and capillary fringe zone to effect the enhanced degradation and/or transformation of at least a portion of the contaminants present.
[0032] The contemplated process may be used in conjunction with a ‘value fluid,’ such as petroleum, crude oil, or, refined petroleum product, etc., such as might be found in an oil field, refinery spill, bulk storage facility spill, or petroleum processing facility spill.
[0033] The present invention is more fully described in the following detailed description with reference to additional illustrative preferred embodiments.
BRIEF DESCRIPTION OF THE DRAWINGS
[0034] The foregoing summary, as well as the following detailed description of preferred embodiments, is better understood when read in conjunction with the appended drawings. For the purpose of illustrating the invention, there is shown in the drawings exemplary constructions of the invention; however, the invention is not limited to the specific methods and instrumentalities disclosed.
[0035] In the drawings:
[0036] FIG. 1 is a plan view showing the general layout of soil borings and monitoring wells to estimate the contaminant volume using the capillary pressure method;
[0037] FIG. 2 is a view of a geologic cross-section showing the general location of LNAPL and DNAPL;
[0038] FIG. 3 is a plan view showing a general layout of wells and transects for estimating the contaminant mass flux;
[0039] FIG. 4 is a sectional view showing a general placement of a SPT injection well, an extraction well, and a representation of the force used to promote a dynamic porosity to remove and/or treat subsurface contamination;
[0040] FIG. 5 is a plan view showing an embodiment of multiple SPT injection wells and extraction wells such that they encompass the contaminant mass; and
[0041] FIG. 6 is a fluid retention graph.
DETAILED DESCRIPTION OF THE INVENTION
[0042] The present invention is useful for the in situ removal and/or in situ treatment of contaminants from a contaminated subsurface area of the earth and is especially useful for removing and/or rendering innocuous non-naturally occurring hydrocarbon contaminants. By use of the phrase “non-naturally occurring hydrocarbon contaminants,” this invention contemplates, as a non-limiting example, the removal of such hydrocarbons that are commonly found in petroleum such as aromatics, alkanes, olefins and heterocyclic compounds, and various derivatives of these compounds, such as alcohols, esters, ketones, carbonates, acids, and other halogenated derivatives. Especially contemplated for removal are halogenated aliphatic compounds such as trichloroethylene and 1,1,1-trichloroethane, which are typically employed as dry cleaning and industrial degreasing solvents, although it will be understood that the subject matter described herein and claimed is in no way limited to the removal of any particular compound except in those instances (should there be any such instances) where stated clearly and unequivocally.
[0043] Contaminated subsurface areas contemplated for cleanup and decontamination in accordance with this invention are areas having a subsurface water table, a subsurface saturated zone below the water table, and a subsurface capillary zone. A capillary or capillary fringe zone in which contaminants exist in both liquid and vapor form lies directly above a subsurface water table. The capillary zone can be defined as a transition region from the subsurface water table to the vadose (unsaturated) zone. For purposes of the present invention, however, the capillary zone is contemplated as being an extension or portion of the water table.
[0044] To effect the removal and/or in situ destruction of hydrocarbon contaminants from a contaminated subsurface area in accordance with this invention, a system of wells is put in place which is disposed within, around, or otherwise in close proximity to an area suspected of contamination. Wells of unconventional, e.g. wells capable of conveying excitation pulses into the geologic medium, and conventional design, e.g. injection and extraction wells, or combinations thereof, are contemplated for use in this invention. The excitation well, e.g. wells containing SPT equipment sold under the trademarks DEEPWAVE, PRIMIWAVE or POWERWAVE, which is able to induce pressure waves and strain stimulus that dispenses treatment agents within a contaminated area of subsurface earth, is critical to the process. At least one excitation well is contemplated for introducing the pressure stimulus as well as injecting treatment or removal agents or, if desired, only for introducing chemical oxidants or other treatment agents to effect the destruction and/or removal of contaminants. The terms excitation and injection are sometimes used interchangeably in the context of the present invention. The excitation waves being ‘injected’ through a well that may also be capable of injecting steam, occident surfactant or other treatment fluid, this interchangeability is appropriate.
[0045] The excitation well is constructed of a fluid impermeable conduit material disposed in boreholes, and has a perforated lower portion disposed in a subsurface saturated zone, i.e., below the water table, and which allows for injected pressure stimulus and treatment/removal agents to be introduced below ground level and into the saturated zone and capillary zone. Preferably, there are a multiplicity of such pressure stimulus SPT excitation wells, each which may depend upon such factors as the size and subsurface geology of the specific contaminated area to be treated, and the specific nature of the contamination.
[0046] Disposed among the injection wells is preferably, at least, one return or extraction well, which is of conventional design, and constructed of impermeable conduit material disposed in a borehole and having a perforated lower portion disposed in a subsurface saturated zone and capillary zone, which allows for the withdrawal of contaminant-bearing groundwater and/or non-value liquid from the saturated zone and capillary zone to the surface for treatment and removal of the contaminants. There are preferably multiplicities of such extraction wells located among and spaced apart from the aforesaid excitation well(s), to form an array or pattern of injection/excitation and extraction wells.
[0047] By application of a withdrawing force, e.g., by the mechanical action of a pump or by sub-atmospheric pressure applied by a vacuum pump, or by heat of compression from treatment agents reacting with the contaminants, to the extraction wells, and in tandem with the simultaneous pressure stimulus and dynamic porosity increase and injection of treatment amendments via SPT, gases and fluids including contaminated material in various physical states are caused to be displaced from their location in the saturated and capillary zones toward the perforated lower sections of the extraction well(s) (or uncased bore hole in the event that the extraction well is in rock). Such gases and liquids are then withdrawn through the perforated portions and up the extraction wells to the surface for treatment and/or disposal, to effect decontamination of targeted substances in areas of the earth. The amount of vacuum necessary to effectuate removal of non-value or value liquid without killing the SPT excitation well by creating a preferential pathway (short circuiting) is to be determined in the field by the supervising scientist or engineer. At present there is no known means of calculating the proper vacuum; it must be determined on an empirical basis by a scientist or engineer experienced with the SPT process.
[0048] In accordance with this invention, the application of pressure stimulus via one or more excitation wells effects the movement and dissolution of subsurface non-volatilized contaminants to facilitate their removal by the applied withdrawing force at the extraction wells in areas near or contiguous to the injection (excitation) wells. Especially targeted are pools, fingers, blobs, ganglia, or other concentrations of non-dissolved, residual NAPL contamination. Depending on the particular subsurface geology subject to pressure stimulus application and extraction including such factors as mineral makeup, physical structure, and porosity, the applied pressure stimulus and mobilized compounds and non-value or value liquids e.g. non-volatilized contaminants, are caused to move in various directions through the subsurface toward the lower perforated portion of the extraction wells in the saturated zone and capillary zone for their eventual removal to the surface. Liquids and otherwise non-volatilized material are coalesced and are mobilized and driven by the excitation process toward the perforated portion of the extraction wells.
[0049] Also in accordance with this invention, the injection of pressure stimulus into the subsurface saturated zone and capillary fringe zone is accompanied by the simultaneous injection, also into the saturated and capillary zone, of treatment agents. It has been found that oftentimes contaminating solvents are present in the subsurface in an undissolved state, thus rendering their removal from a contaminated subsurface area, particularly from a saturated zone, difficult, or nigh impossible, using conventional approaches. By employing pressure stimulus in conjunction with treatment agents, the enhanced degradation and/or transformation, and/or destruction of some contaminating compounds or solvents is readily achieved, thereby greatly facilitating their removal via groundwater and/or extraction wells, or facilitating their in situ destruction to harmless by-products. For example, the transformation of tri-chlorinated solvents results in chloride, carbon dioxide and water, which are innocuous and non-toxic.
[0050] It will also be appreciated by those persons skilled in the relevant art that the simultaneous injection of pressure stimulus and treatment agents with resulting mobilization and/or destruction of organic compounds and their subsequent removal from a contaminated subsurface area also has the effect of lowering the concentration of such organic contaminants to levels that are less toxic.
[0051] A preferred embodiment of this invention is best presented and understood with reference to FIGS. 1-5 , and the following discussion thereof. It is to be understood, however, that such discussion is for illustrative purposes only and/or merely sets forth some preferred embodiments and variations thereof will be readily apparent to those persons skilled in the relevant art and are not intended to limit the claims or the spirit thereof in any way.
[0052] Referring now to FIG. 1 of the drawings, there is depicted an LNAPL contamination scenario showing the defined LNAPL area of retention ( 2 ), a plurality of monitoring wells ( 4 ) for the purpose of measuring free product and water table fluctuations and a plurality of soil borings ( 6 ) for the purpose of measuring the LNAPL content in soils to define the area of retention ( 2 ) and develop estimates of recoverable LNAPL volume using the capillary pressure method. Soil samples obtained during installation of these wells, or from earlier wells/borings can also be used to estimate the contaminant mass and to prepare isocontours identifying the location of the contaminant mass. As shown in this preferred embodiment, the soil borings ( 6 ) and monitoring wells ( 4 ) extend across the surface of the ground, below which substantially lies the subsurface contaminated area to be evaluated and subsequently treated. FIG. 1 also shows the preferred embodiment of soil borings ( 6 ) used to develop an estimate of the residual LNAPL volume using conventional methods. Together, use of the capillary pressure method plus the conventional method for estimating residual is used to develop an estimate of the total undissolved LNAPL volume before treatment using SPT technology, and as a basis for measuring remediation following the application of SPT technology.
[0053] The capillary pressure method assumes the NAPL is at static equilibrium and movement of the NAPL in the vertical direction. The capillary pressure method uses energy pulses, e.g. SPT, applied to the subsurface to stress the soil/rock matrix. Before and after the soil/rock properties change in response to pulsing, an estimate is made of the volume of recoverable residual NAPL. Differences between the before and after estimations provides information for determining a more accurate estimation. NAPL thickness is an important variable in estimating the thickness of NAPL and is measured in a monitoring well ( 4 ). The ultimate goal is that the “more accurate estimate” of contamination mass/volume is known before removal or abatement begins; thus providing a more reliable metric of success of the removal/abatement.
[0054] LNAPL and DNAPL are normally measured by gauging the thickness in monitoring wells. This is performed by inserting a measuring device (interface probe) that detects the interface between water or air and the NAPL. It can also be performed by using a tape measure with paste that is sensitive to water and another sensitive to NAPL, but the interface probe is the most commonly used. DNAPL is more difficult to accurately measure because the thickness can depend on the location of the well relative to the bottom of the DNAPL. LNAPL is lighter than water (by definition) so it is above the water level and is easier to measure.
[0055] Difficulty arises when estimating the volume of free-phase or readily recoverable NAPL because the thickness that appears in a given well typically does not reflect the volume available in the geologic formation for recovery. There are several reasons for this. The volume of recoverable NAPL depends on both the soil properties and the fluid properties, and the amount available for conventional recovery varies tremendously with these properties. Despite the thickness in wells, there may be very little recoverable NAPL in some soils even with large NAPL thickness because the thickness is exaggerated by fine-textured soils. The opposite is true as well, as even moderate NAPL thickness in very permeable soils can mean that there is a lot available for recovery.
[0056] The amount of NAPL occupying a given volume of soil is a function of soil pore size and fluid properties. However, even with a lot of oil (oil being a common example of NAPL) in a well most of the soil pore space is occupied by water, not NAPL. This is a counter-intuitive result that often results in confusion. The misunderstanding results in errors that result in misguided remediation that is inefficient, ineffective and costly. Residual NAPL, by definition, is very difficult to recover and constitutes a long-term source of contamination.
[0057] The capillary test method comprises the following steps:
[0058] 1. Estimate the total NAPL mass over the soil volume of interest from soil borings, soil physical data (bulk density and porosity), and TPH (“total petroleum hydrocarbons”), total VOC (“volatile organic compounds”)+SVOC (“semi-volatile organic compounds”) measurements on soil samples. Calculate residual NAPL saturation level (percent) from this data. These calculations are in accordance with known NAPL mass estimation methods. See, e.g., Wiedemeier, T. et al., Natural Attenuation of Fuels and Chlorinated Solvents in the Subsurface, pp. 104-106, (1991), John Wiley & Sons, Inc, incorporated by reference herein in its entirety.
[0059] Step 1 is a direct measure of the total NAPL mass in the soil volume. The purpose is to obtain an estimate of the percent NAPL saturation. This serves as a benchmark for comparison with the estimates from Steps 2 through 6. Having an estimate of the percent NAPL saturation provides another means of comparing what is removed to what was there originally. That is, it is used as a metric of completeness.
[0060] 2. Estimate the static (non-pulsed) volume of recoverable NAPL using the capillary pressure methods using LNAPL measurements in monitoring wells over the area of interest. Convert to the estimated volume to mass. This static estimation may be calculated using Farr, A. M., et al., Volume Estimation of Light Nonaqueous Phase Liquids in Porous Media, Ground Water (1990), Vol. 28, No. 1, pp. 48-56 and/or Lenhard, R. J. and Parker, J. C., Ground Water (1990), Vol. 28, No. 1, pp. 57-67, both of which are incorporated herein by reference in their entireties. Other methods exist, though these, it is believed, are the most appropriate, accurate, and field proven methods of estimating the amount of recoverable NAPL in monitoring wells because of the difficulties described in measuring NAPL, above. Other methods are prone to errors in estimating the volume of recoverable free-phase NAPL.
[0061] 3. Subtract the mass result in Step 2 from the mass result in Step 1. This difference is an estimation of residual LNAPL mass.
[0062] 4. Estimate the minimum LNAPL thickness from individual monitoring well(s) NAPL measurements using fluid entry pressure data from a fluid retention curve, see, e.g., FIG. 6 , fluid density information, calculation from fluid properties and grain-size information, and the equation (1):
[0000]
T
o
=
ρ
ow
Δ
ρ
g
[0063] T 0 yields the critical NAPL thickness below which all NAPL is residual.
Where:
[0000]
T 0 =Original minimum non-zero thickness below which all NAPL is at zero gauge (cm)
ρ ow =Entry pressure for the soil type (cm)
Δρ=Change in fluid density (g/cm 3 )
g=Gravity (dynes/gm)
ρ=Fluid density (g/cm 3 ), w=water, o=NAPL
[0069] 5. Estimate residual NAPL, i.e. NAPL not recoverable by standard techniques, that can be recovered by using SPT technology. This estimation is made by stressing the saturated soil/rock matrix using the SPT technology (“estimate pulsing”):
[0070] Case 1: Static LNAPL thickness, T, decreases in well after estimate pulsing for a given duration.
i. Measure the stabilized decrease in NAPL thickness in a monitoring well. ii. Subtract this thickness from the original entry pressure ρ ow value obtained from the laboratory (or literature value) for this parameter. iii. Insert this value into equation (1) and re-compute T new Calculate
[0000]
T
0
−T
new
=ΔT
ΔT corresponds to a new capillary pressure and NAPL retention function, which in turn corresponds to the amount of residual now available for recovery. Refer to FIG. 6 .
iv. Apply Step 2 to ΔT and re-calculate the new recoverable volume. The difference between the original volume and the new volume is the residual volume/mass available for removal.
[0076] The operating principal in Case 1 is that the SPT process stresses the soil/rock matrix and causes the pore bodies and pore throats to expand and increase their interconnectivity. The soil/rock matrix consists of pore bodies of varying sizes and the pores are connected to each other by pore throats, much like a balloon and the much thinner stem through which it fills. The ratio of the diameter of the pore body (e.g. balloon) and the pore throat (balloon stem) very strongly influences the degree to which NAPL is held to the soil/rock matrix. The larger the ratio of the pore throat to the pore body, the greater the NAPL will be held in the soil/rock matrix. As this ratio decreases NAPL is held less strongly and is more able to flow (when all other factors are met). At some point, in response to SPT pulsing, the pore throat-pore body ratio may lower to a threshold value where the resistance to NAPL flow is reduced. At, or before, this point the NAPL thickness in the well can now overcome the resistance to flow in the soil/rock matrix. That is, less mechanical energy is now required, because of relaxing the resistance by reducing the ratio, so the NAPL flows out of the well and the thickness is reduced.
[0077] SPT pulsing acts differentially on the pore body and pore throat because of the difference in size. The mechanism by which this works is that when a pulse (subsurface pressure wave) traverses the medium it exerts force (mechanical energy) on the geologic matrix that results in pressure changes in the pores. Since pressure is energy per unit area (e.g., dynes per square centimeter or pounds per square inch), the force acting on the pore body is less than the force acting on the pore throat because the pore throat has a much smaller radius and opening size. As a result of the difference in force on the pore throat compared to the pore body, the pore throat opens more (force is the same but area is reduced). This effect can be easily seen on a larger scale along a shoreline, where “blowholes” evidence waves forcing their way into small openings and resulting in a water geyser. The geyser is a result of the dramatic pressure increase. This is analogous to what occurs on the pore-scale level in the soil/rock matrix. The result is a smaller ratio, i.e. the capillary pressure P c , becoming greater than the entry (displacement) pressure ρ ow , enabling the NAPL to move. The effect is greatest when the pulsing frequency and amplitude are optimized for the specific soil/rock type. Achieving the appropriate frequency and amplitude is an iterative process done in the field. Experience and knowledge of local conditions will have a far greater impact than any algorithm or process for determining frequency and amplitude values.
[0078] Case 2: Static LNAPL thickness, T, increases in well after test pulsing for a given duration.
i. Measure the stabilized increase in LNAPL thickness. This increase above the static level is taken to be the new estimate of ρ ow . ii. Add this thickness to the original ρ ow value obtained from the laboratory (or literature value) for this parameter. iii. Insert this value into equation (1) and re-compute T new iv. Calculate
[0000]
T
new
−T
0
=ΔT
v. Apply Step 2 to ΔT and re-calculate the new recoverable volume. The difference is the amount of residual volume/mass removed.
[0084] The operating principal in Case 2 is identical to that in Case 1 except that the pore throat to pore body ratio is not increased significantly, or quickly enough, so that PC remains less than or equal to the entry (displacement) pressure ρ ow . In this instance, NAPL accumulates in the well from mobilized residual in response to pulsing and the thickness increases. The increase in NAPL thickness above static is then taken to equal or approximate the modified ρ ow , which is then treated as in Case 2 steps (ii) through (v).
[0085] In practice, both Case 1 and Case 2 will occur within an area of interest. All the wells will have to be treated and adjusted individually before re-computing the new recoverable volume for the entire set of wells, using Step 2 to estimate the total residual available for recovery.
[0086] Referring now to FIG. 2 of the drawings, there is depicted a cross-section of the contaminated area. As shown in this preferred embodiment, the monitoring well(s) ( 4 ) and soil boring(s) ( 6 ) extend vertically through the contaminant area to be treated ( 12 , 14 ). FIG. 2 shows the surface of ground (S), the capillary zone (CZ) extending from some distance above the surface of the water table (WT) and the saturated zone extending below the water table. The smear zone ( 12 , 14 ) is the area above and below the water table that contains residual LNAPL. As also shown in FIG. 2 , a non-aqueous phase non-value liquid contaminant in an undissolved state that occupies a portion of the contaminated area of the saturated zone ( 14 ) below the water table and a portion of the capillary zone ( 12 ) above the water table.
[0087] Referring now to FIG. 3 , there is depicted a DNAPL contamination scenario showing the defined DNAPL-impacted area ( 16 ) and a plurality of monitoring wells ( 18 , 20 , 22 , 24 , 26 , 28 , 30 , 32 , 34 , 36 , 38 , 40 , 42 , 44 , 46 , 48 , 50 , 52 , 54 , 56 , 58 , 60 ) along transects ( 62 , 64 , 66 , 68 , 70 ) used to estimate the DNAPL mass flux. As shown in this preferred embodiment, monitoring wells extend across the surface of the ground, below which substantially lies the subsurface contaminated area to be treated. FIG. 3 also shows the preferred embodiment of monitoring wells used to develop an estimate of the DNAPL mass flux. The local flow of groundwater (GW) is shown by the arrow. The mass flux method for estimating DNAPL is used to develop an estimate of the total undissolved DNAPL before treatment using SPT technology and as a basis for measuring remediation following the application of SPT technology. FIG. 2 shows the generalized distribution of NAPL, either LNAPL or DNAPL, applicable to this process.
[0088] Referring now to FIG. 4 , there is depicted the treatment process consisting of the pulsing apparatus ( 72 ) on the surface or inside the SPT injection/excitation well into which a fluid and/or treatment agent ( 74 ) is injected into the excitation well ( 76 ). The excitation well ( 76 ) is perforated or fitted with screens ( 78 ) (an open borehole may be used in the case of rock) to permit the injected fluid and/or treatment agent ( 74 ) to create pressure pulses ( 79 ) in the capillary zone ( 12 ) and the saturated zone ( 14 ) below the water table (WT) to be decontaminated. The injected fluid creates pulses ( 79 ) that emanate through the perforated or screened portion ( 78 ) of the excitation well ( 76 ), and in turn effect changes in the physical properties of the geologic medium ( 80 , 82 )(increasing conductivity and creating new openings for flow) that promote and enhance remediation.
[0089] The pulses open the pore spaces, voids, or apertures in the geologic medium and dispense and disperse fluids and contaminants toward the extraction well ( 84 ).
[0090] The extraction well ( 84 ) has a vacuum applied ( 86 ) that facilitates removal of the contaminants and/or prevents mobilized contaminants from reaching receptors. Removal is facilitated by the vacuum, the perforated or screened portion ( 90 ) of the extraction well ( 84 ). The extraction well ( 84 ) operates simultaneously or within one week following injection from the excitation well ( 76 ). Use of a vacuum applied to one or more extraction wells ( 84 ) results in a push-pull operation. The purpose of the vacuum on the extraction well(s) serves two purposes. One purpose is to enhance removal of the contaminant by creating a lower gradient towards which the contaminant will preferentially flow, also preventing the contaminant from reaching receptors. The second purpose of the vacuum is to generally create lower atmospheric pressure in the subsurface, i.e. without consideration for the existence of direction of a pressure gradient. Lowering the atmospheric pressure in the subsurface causes fluids to more readily flow through the pores, voids, or apertures in the geologic medium and thus further enhances the SPT process. LNAPL or DNAPL exits through the extraction well ( 84 ) via tubing or other means ( 92 ) and then to a container ( 94 ) for eventual treatment or removal off site.
[0091] In this preferred embodiment, the well screens or perforated portions ( 78 , 90 ) of the excitation/injectoin well(s) ( 76 ) and extraction well(s) ( 84 ) extend into an area of undissolved liquid contaminant, or a non-aqueous liquid phase (NAPL), which occupies a portion of the saturated zone ( 14 ) and/or capillary zone ( 12 ) to be decontaminated. Such a non-aqueous liquid phase is oftentimes contained in a substantially well defined area, for example, when the subsurface saturated or capillary zone borders a stratum of clay or densely packed gravel, or some other substantially impermeably fill material. The present invention, however, also contemplates the pulsing of fluid and/or treatment agent via perforated riser bottoms ( 78 ) into contaminated subsurface areas which lack a non-aqueous liquid phase or which, due to particular subsurface geology, lack a well defined non-aqueous liquid phase zone. In either case, undissolved contaminating liquid hydrocarbons, if any, are dispersed throughout a greater portion of the subsurface contaminated area and, for example, are trapped within pore spaces, voids, or between subsurface strata.
[0092] A further plurality of spaced apart vertical excitation wells ( 76 ) and extraction wells ( 84 ) extending downward into the capillary zone ( 12 ) and saturated zone ( 14 ) below the water table (WT) for the extraction of contaminant-bearing groundwater are shown also contemplated in the preferred embodiment. Further, the well and extraction wells can also extend downward into the ground in an angular fashion relative to the surface of the ground, up to and even beyond a horizontal fashion, as desired or necessary.
[0093] Extraction well(s) ( 84 ) for removal of contaminant or contaminant-bearing groundwater from the capillary zone (CZ) and saturated zone (SZ) are connected to a suitable device for maintaining an induction force (e.g. a pump ( 86 ) for maintaining a vacuum or sub-atmospheric pressure) for drawing the contaminant-bearing groundwater and contaminants to the perforated portions ( 90 ) of extraction well(s). In the case of rock, open boreholes may be used, either alone or in combination with perforated portions ( 90 ).) The contaminant proceeds thusly to the surface for treatment and/or disposal. It is also contemplated in this invention that, depending on the depth of return risers, an additional withdrawing force, e.g. sub-atmospheric pressure, may be applied to the saturated zone (SZ) and/or capillary zone (CZ) by one or more pumps ( 96 ) installed at a subsurface location.
[0094] Groundwater containing extracted contaminants is received from extraction well ( 84 ) via line ( 92 ) and is deposited in storage tank ( 94 ) via vacuum pumps ( 86 ). Alternatively, the extracted material can be pumped to any conventional disposal apparatus.
[0095] In FIG. 4 , there is shown a cross-sectional view of the preferred embodiments of excitation well(s) and extraction wells. At the upper ends of the excitation/injection well ( 76 ) and extraction well ( 84 ), breaching the surface of the ground (S), portions of the respective annular areas of ground, extending downward from S, are filled with a low permeability material, such as cement, grout, clay or compacted soil, to prevent wave pressure stimulus from short circuiting the excitation well ( 76 ). Similarly, the contemplated method includes treatment using SPT sources in a direct push mode in lieu of wells if deemed more appropriate give field conditions.
[0096] At the bottom end of each of the excitation and extraction risers ( 76 , 84 ) extending into their respective boreholes into a subsurface saturated area ( 14 ) or capillary zone ( 12 ) to be treated in accordance with this invention, are perforations or screens ( 78 , 90 ). In FIG. 4 , fluid and/or treatment agents introduced through riser ( 76 ) flow via SPT pressure pulses through screen ( 78 ) into the annulus area and thereafter into a target area of the subsurface earth to be treated. In this preferred embodiment, the aperture size of the perforated or screened portions of the well ( 78 ) are engineered to maximize the pulsing effectiveness.
[0097] The preferred embodiment of the push-pull injection-extraction design in FIG. 4 is intended for use in groundwater extraction and/or monitoring wells situated in a capillary fringe zone ( 12 ) above and saturated zone ( 14 ) below the water table (WT). Extracted material(s) enter the perforated or screened area ( 90 ) from contiguous or surrounding areas of the contaminated subsurface and are thereafter drawn into extraction riser ( 84 ) through perforated portions of the screen ( 90 ) situated at the bottom end of the riser under the influence of an applied withdrawing force, such as sub-atmospheric pressure applied via a vacuum pump, to the extraction well as discussed above.
[0098] Referring now to FIG. 5 , there is shown a typical array of spaced apart injection/excitation wells ( 96 , 98 , 100 ) interspersed with an array of spaced apart extraction wells ( 102 , 104 , 106 , 108 , 110 , 112 , 114 , 116 , 118 ). While not specifically indicated, the extraction wells are intended to illustrate both extraction wells situated in the capillary fringe zone, the saturated zone or both. The spacing of each excitation well ( 96 , 98 , 100 ) is determined by such factors as the nature and extent of the contamination and by the particular nature of the subsurface geology to be decontaminated.
[0099] It is noted that the foregoing examples have been provided merely for the purpose of explanation and are in no way to be construed as limiting of the present invention. While the invention has been described with reference to various embodiments, it is understood that the words which have been used herein are words of description and illustration, rather than words of limitations. Further, although the invention has been described herein with reference to particular means, materials and embodiments, the invention is not intended to be limited to the particulars disclosed herein; rather, the invention extends to all functionally equivalent structures, methods and uses, such as are within the scope of the appended claims. Those skilled in the art, having the benefit of the teachings of this specification, may achieve numerous modifications thereto and changes may be made without departing from the scope and spirit of the invention in its aspects.
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A remediation process that a employs improved quantitative method(s) of estimating of the volume and/or mass of contaminant in the subsurface, removal and or in situ degradation of the contamination using subsurface pulsing treatment (“SPT”) technology, and evaluation of the degree of remediation by re-applying the quantitative contaminant evaluation methods. The process uses SPT technology with the addition of a vacuum or sub-atmospheric pressure to an extraction well in order to create a push-pull effect to remove free contaminant or residual in conjunction with the pressure wave driving force created in the excitation or excitation well. The process can quantitatively measure the amount of residual contaminant, which up until now has not been possible or tractable using in situ methods, as well as measure the amount of residual that can be removed by SPT.
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This application is a divisional of application Ser. No. 07/721,944, filed Jun. 27, 1991 and now U.S. Pat. No. 5,328,491.
BACKGROUND OF THE INVENTION
The present invention relates to a dispersant having excellent properties of dispersing organic and inorganic substances and an effect of remarkably improving the stability of the dispersion system. In particular, the present invention relates to a dispersant for a coal/water slurry which dispersant exhibits excellent effects of increasing the concentration and improving stability of the slurry when it is left to stand.
It is known that polystyrenesulfonic acid produced by sulfonating polystyrene and salts thereof are usable as antistatic agents, dispersants and various other agents. They are used as, for example, antistatic agents for papers [Japanese Patent Publication for Opposition Purpose (hereinafter referred to as “J.P. KOKOKU” ) No. Sho 57-53953], antistatic agents for resins [Japanese Patent Unexamined Published Application (hereinafter referred to as “J.P. KOKAI”) No. Sho 59-8741], dispersants for coal/water slurry (J.P. KOKAI Nos. Sho 57-145187, Sho 62-590 and Sho 63-278997 and Japanese Patent Application No. Hei-1-338564), and dispersants for cements (J.P. KOKAI Nos. Sho 51-525, Sho 51-64527, Sho 56-41866, Sho 57-156355, Sho 60-46956 and Sho 63-25251). The polystyrenesulfonic acid and salts thereof are usually produced by polymerizing styrenesulfonic acid monomer or by sulfonating polystyrene. They have a structure shown the following general formula (II) or the like:
wherein l represents an integer and k represents 0 or an integer of at least 1. Although styrene of l recurring units in the above formula has one SO 3 X group, some of the recurring units may have 0 or two or more SO 3 X groups.
Although these known polymers exhibit an excellent effect for increasing the concentration of the dispersion system, their effect of improving the stability of the dispersion system is yet insufficient.
SUMMARY OF THE INVENTION
A primary object of the present invention is to provide a new dispersant, in particular, capable of improving the stability of a dispersion system.
This and other objects of the invention will be apparent from the following description and Examples.
The inventors have found that the stability of the dispersion system can be improved by using a sulfonated polystyrene having a specified amount of indane ring at a terminal of the styrene recurring unit.
Namely, the present invention provides a dispersant comprising a polystyrenesulfonic acid having a weight-average molecular weight in the range of 2,000 to 100,000 or a salt thereof, wherein at least 70% of the terminals of the polymer chains have an indane ring of the formula (I):
wherein X represents a cation selected from the group consisting of a hydrogen, alkali metals, alkaline earth metals, ammonium and organic amines, and n and m each represent 0 or an integer of at least 1.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is an NMR chart of polystyrene used as a starting material for the dispersant of the present invention. FIGS. 2 are a GC-MS gas chromatogram (A) of the dispersant of the present invention and an MS spectrum (B) thereof. FIG. 3 is an NMR chart of the dispersant of the present invention. FIG. 4 is an NMR chart of a lower molecular part of the dispersant of the present invention. FIG. 5 is an NMR chart of starting polystyrene for a comparative dispersant. FIG. 6 is an NMR chart of a comparative dispersant. FIG. 7 is an NMR chart of a methanol-soluble part of the starting polystyrene for the dispersant of the present invention.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
In the present invention, other terminals of the polymer than the indane ring of the above formula (I) have a structure shown by the following formula (III):
The part of the polymer other than its terminals comprises recurring units having a structure of the following general formula (IV):
wherein X and n are as defined above.
The polymers used in the present invention are preferably those having a molecular weight of 2,000 to 50,000 and a degree of sulfonation of at least 60%, preferably 80 to 95%, based on the styrene units.
In the formula (I), n and m are preferably not zero at the same time. X in the formula is preferably an alkali metal such as sodium or potassium, an alkaline earth metal such as calcium or magnesium or ammonium cation, more preferably sodium, calcium or ammonium.
The polystyrene having an indane ring at the terminal thereof used in the present invention can be produced by cationic polymerization of commercially available styrene monomer. It is preferred to use a metal halide, particularly a metal chloride, as the polymerization catalyst. Examples of them include tin dichloride, tin tetrachloride, aluminum chloride and titanium tetrachloride. other cationic polymerization catalysts are also usable. However, when, for example, BF 3 is used, the relative amount of the polystyrene having the indane ring at the terminal is reduced to about 50%. The amount of the catalyst used is preferably 0.01 to 1% by weight based on the styrene monomer.
Halogenated hydrocarbons are used as the reaction solvent. They include dichloromethane, chloroform, carbon tetrachloride, dichloroethane and tetrachloroethane.
Although the weight ratio of the solvent used for the polymerization reaction to the styrene monomer is not particularly limited, it is preferably 10/90 to 90/10, more preferably 20/80 to 80/20, from the viewpoints of the control of the reaction system and after-treatment.
The polymerization reaction is preferably conducted by previously heating the reaction solvent to a predetermined temperature and then adding styrene monomer dropwise to the reaction system to conduct the polymerization. After completion of the addition of the styrene monomer, the reaction is completed by aging. It is also possible to further add the catalyst after completion of the addition in order to accelerate the completion of the reaction.
The polymerization temperature usually ranges 30 to 150 ° C.
After completion of the reaction, the remaining catalyst is neutralized with ammonia or the like by an ordinary method and a precipitate thus formed can be removed by filtration or by washing with water. The remaining catalyst can be removed also by adsorbing it on an adsorbent and then filtering it.
The styrene polymer having the indane ring at the terminals in an amount of least 70%, preferably 80 to 95% obtained by the above-method, is sulfonated by an ordinary method to obtain the dispersant of the present invention.
Examples of the sulfonation reaction conditions are as follows: the sulfonation can be conducted with sulfuric anhydride, fuming sulfuric acid, chlorosulfonic acid or sulfuric acid as the sulfonating reagent. These sulfonating reagents can be directly added dropwise to the reaction system or, alternatively, they can be introduced into the reaction tank together with polystyrene to continuously conduct the sulfonation. Sulfuric acid anhydride can be introduced into the system after dilution with nitrogen or dry air or, alternatively, it is reacted with dioxane or the like to form a complex to be added dropwise.
The reaction solvents usable herein are those inert to the sulfonating reagent. The solvents inert to the sulfonating reagent include halogenated hydrocarbons such as dichloromethane, chloroform, carbon tetrachloride, dichloroethane and tetrachloroethane. When such a solvent is used as the polymerization solvent, the sulfonation can auto be conducted without changing the solvent.
After completion of the sulfonation, the solvent is removed and the product is neutralized to obtain the new dispersant usable in the present invention.
The dispersant thus produced is practically used directly in the form of the aqueous slurry having a concentration of about 5 to 50%, concentrate having a concentration of 50 to 60% or powder prepared by drying by an ordinary method.
The dispersant of the present invention is usable for any dispersion system for which an ordinary dispersant is usable. For example, it is usable as a dispersant for organic dispersions such as a coal dispersion, pigment dispersion, dye dispersion, paint dispersion, developer dispersion, microcapsule dispersion; as a dispersion stabilizer for suspension polymerization; as a levelling agent for a dye; or as a dispersant for inorganic dispersions such as silica or TiO 2 dispersion. The dispersant of the present invention is effective for stabilizing a dispersion such as a concrete admixture and particularly coal/water slurry. Thus it is effective for inhibiting coagulation of a slurry. The dispersant for the coal/water slurry is effective for preparing an aqueous slurry of anthracite, bituminous coal, sub-bituminous coal or brown coal. The amount of the dispersant is usually selected so that the amount of the polymer of the present invention will be in the range of 0.05 to 3.0% by weight based on the coal/water slurry.
When the coal/water slurry is to be produced by using the polymer of the present invention, the polymer can be added as it is to the fine coal powder or it can be used in the form of an aqueous solution thereof having a concentration of about 5 to 50% by weight. The mixture of the fine coal powder and water can be produced by, for example, a method wherein the coal is dry-pulverized to a desired particle size by means of a pulverizer such as a crusher or ball mill, water is added thereto in an amount determined so that the fine coal powder concentration in the final high-concentration coal/water slurry will be 55 to 75% in due consideration of water content of the fine coal powder and water content of the dispersant and they are homogeneously mixed with kneader, co-kneader or Bambury mixer; a method wherein the coal is pulverized to a desired particle size in the presence of water in an excess amount by means of a pulverizer such as a ball mill or rod mill and it is dehydrated so that the coal concentration in the final high-concentration coal/water slurry will be 55 to 75% in due consideration of water content of the dispersant; or a method wherein coal and water are mixed together to obtain a mixture of a predetermined concentration and the mixture is ground to a desired particle size by means of a pulverizer such as ball mill or rod mill to obtain a homogeneous mixture.
According to the present invention, a dispersant having a quite excellent dispersion stability is provided.
The following Examples will further illustrate the present invention.
EXAMPLE 1
200 g of ethylene dichloride as solvent was placed in a flask and 0.7 g of tin tetrachloride as catalyst was added thereto. The temperature was elevated to 70° C. while the reaction mixture was stirred and then 200 g of styrene was added dropwise thereto for 1 h. The stirring was continued at 84° C. for 5 h to complete the reaction. The weight-average molecular weight of the polymer (Polymer-1) determined by gel permeation chromatography was 7,500.
300 g of a solution of Polymer-1 in ethylene dichloride was diluted with 450 g of ethylene dichloride and sulfonation was conducted with sulfuric acid anhydride as the sulfonating reagent in molar ratio of 1.05:1 to synthesize a dispersant of the present invention (Polymer-2). The weight-average molecular weight of the polymer (Polymer-2) determined by gel permeation chromatography was 15,000.
The properties of the polymers were determined as follows:
(1) Weight-Average Molecular Weight of Polymer-1:
The weight-average molecular weight of Polymer-1 was determined by GPC method by using standard polystyrene as the standard substance, TSK G1000HXL (7.8 mm ID×30 cm) (a product of Toso Co., Ltd.) was used as the separation column and an ultraviolet ray detector (wave length: 266 nm) was also used. When styrene was detected in the sample, the weight-average molecular weight was determined by excluding styrene.
(2) Weight-average Molecular Weight of Polymer-2:
The weight-average molecular weight of Polymer-2 was determined by GPC method by using standard sodium polystyrenesulfonate as the standard substance, TSK G3000SW (7.5 mm ID×30 cm) and TSK G4000SW (7.5 mm ID×30 cm) (products of Toso Co., Ltd.) as the separation columns and an ultraviolet ray detector (wave length: 238 nm). When styrenesulfonic acid was detected in the sample, the weight-average molecular weight was determined by excluding styrenesulfonic acid.
(3) Recognization of Terminal Indane Ring of Polymer-1
Polymer-1 was examined with 400 M NMR (GSX-400; a product of JEOL., Ltd.) and CDCl 3 solvent under conditions comprising a determination temperature of 25° C., integrated circuit (16 times), pulse angle of 45° and pulse intervals of 5 sec. The presence of indane ring was confirmed by proton NMR. The NMR chart is shown in FIG. 1 .
In FIG. 1, the shift position of each proton was as follows:
Proton Shift Position (PPM)
A: 1.1, B: 1.4 to 2.8, C: 4.1 to 4.5 benzene ring 6.4 to 7.4.
The polymer having terminal indane ring was determined by enlarging a part (5 to 10 ppm) of the NMR chart of FIG. 1 and calculating the ratio of protons in the indane ring to protons in the terminal methyl group from the integration curve. As a result, it was found that 90% of the polymer produced by the synthesis process of the present invention had terminal indane ring.
(4) Characteristic Peak of Indane Ring
The characteristic peak showing the presence of the indane ring was determined by analyzing the low molecular components by the following GC-MS and NMR. At first, a low molecular fraction (about hexamer or below) was extracted from the styrene polymer produced by the process of the invention with methanol extractant and the analysis was conducted by GC-MS. The GC-MS determination conditions were as shown below:
GC: packing for the column: Ultra 2 (5% phenylmethyl silicone)
Column size: inner diameter of 0.2 mm and length of 12.5 m
Carrier gas: helium flow rate: 1.0 ml/min
Column temperature: 40° C.→300° C. (15° C./min)
Split ratio: 100:1
MS: Ionization mode: electron impact (E.I.)
Ionic voltate: 70 eV
Accelerating voltage: 3 kV
Molecular weight range: 35 to 500.
Scan speed: 1 sec.
The gas chromatogram of GC-MS and MS spectral chart are shown in FIG. 2 .
From the data file based on the parent peaks of MS spectrum and the fragment peaks, it was found that the two main components of the dimers were two optical isomers of 1-methyl-3-phenylindane and the balance was 2,4-diphenyl-1-butene. From the area ratio in the gas chronatogram, it was found that it comprised 93% of 1-methyl-3-phenylindane and 7% of 2,4-diphenyl-1-butene. To confirm the structure of this substance by NMR, the dimer fraction was taken from low molecular fraction by gel permeation chromatography [SC-8010 series (a product of Toso Co., Ltd.), Column G 4000 H and column G 1000 H, detector UV, wave length 238 nm, flow rate 0.5 ml/min, determination temperature: 40° C.]. The NMR chart of the dimer is shown in FIG. 3 .
The dimer was analyzed by proton MNR and proton proton COSY method to find that the main components of the dimer were two optical isomers of 1-phenyl-2-methylindane. These results supported the results of GC-MS. The shift positions of the respective protons in the NMR chart in FIG. 3 were assigned to as follows on the basis of the analytical results of the COSY chart.
Proton shift position (PPM)
a1: 1.4
b1: 1.3
a2: 3.2
b2: 3.4
a3: 2.7
b3: 2.2
a4: 1.6
b4: 2.3
a5: 4.2
b5: 4.4
benzene ring: 7.1 to 7.3
benzene ring 7.1 to 7.3
According to the NMR analysis, it was found that the proton on the α-position carbon of the benzene ring of 1-methyl-3-phenylindane has a specific peak at 4 to 4.5 ppm. The relative amount of the polymer having the indane ring was determined on the basis of the proton peak.
(5) Indane Ring of Polymer-2:
The presence of-indane ring of the sulfonated polymer (Polymer-2) was examined by NMR (under the same conditions as those of the above-described NMR determination except that heavy water was used as the solvent and that the number of integration was changed to 32). However, no peaks of indane ring could be recognized, since the peaks were widened because the relative amount of the indane ring in the polymer was very small in the polymer-2 and heavy water was used as the solvent. Therefore, a low molecular part which supposedly contained a larger relative amount of the indane ring was subjected to the NMR analysis. In this process, ethanol-soluble matter was extractd from the synthesized polymer and the resulting low-molecular sample (about hexamer or lower) was analyzed in the same manner as that described above. The results are shown in FIG. 4 . The presence of the indane ring could be recognized in FIG. 4 . From these results, it was found that 90% of the polymer in the dispersant of the present invention contained terminal indane ring. The sulfonation rate of Polymer-2 was 90%.
EXAMPLE 2
200 g of ethylene dichloride as solvent was placed in a flask and 1.0 g of tin tetrachloride as catalyst was added thereto. The temperature was elevated to 84° C. while the reaction mixture was stirred and then 200 g of styrene was added dropwise thereto for 1 h. The stirring was continued at 84° C. for 5 h to complete the reaction. The weight-average molecular weight of the polymer (Polymer 3) was 4,000.
300 g of a solution of Polymer 3 in ethylene dichloride was diluted with 450 g of ethylene dichloride and sulfonation was conducted with sulfuric acid anhydride as the sulfonating agent in molar ratio of 1.05:1 to synthesize a dispersant of the present invention (Polymer 4). The weight-average molecular weight of the polymer (Polymer-4) was 8,000. It was examined in the same manner as that of Example 1 to find that 90% thereof had terminal indane ring. The sulfonation rate of Polymer-4 was 86%.
EXAMPLE 3
200 g of ethylene dichloride as solvent was placed in a flask and 0.6 g of tin tetrachloride as catalyst was added thereto. The temperature was elevated to 30° C. while the reaction mixture was stirred and then 200 g of styrene was added dropwise thereto for 3 h. The stirring was continued at 30° C. for 72 h to complete the reaction. The weight-average molecular weight of the polymer (Polymer-5) was 15,000.
300 g of a solution of Polymer-5 in ethylene dichloride was diluted with 450 g of ethylene dichloride and sulfonation was conducted with sulfuric acid anhydride as the sulfonating reagent in molar ratio of 1.05:1 to synthesize a dispersant of the present invention (Polymer-6). The weight-average molecular weight of the polymer (Polymer-6) was 30,000. It was examined in the same manner as that of Example 1 to find that 91% thereof had terminal indane ring. The sulfonation rate of Polymer-6 was 93%.
EXAMPLE 4
Stainless steel balls were placed in a 6 liter stainless steel ball mill (inner diameter: 19 cm) to fill 50% of the mill. 465 g of water and 1,000 g of bituminous coal (Mt. Tholey coal) roughly pulverized to a particle size of 3 mm or below were placed in the ball mill and then the dispersant of the present invention (Polymer-2, 4 or 6, counter ion: Na) was added thereto in such an amount that it would be 0.4% by weight based on the slurry. The ball mill was rotated at 65 rpm to pulverize the coal. The particle size of the coal was determined with a laser diffraction-type size distribution measuring device and the pulverization was continued until 80% of the coal had a particle diameter of 74 μm or below. After completion of the pulverization with the ball mill, the coal/water slurry was taken out of the mill and it was further stirred in a homomixer at 4000 rpm for 10 min to obtain a coal/water slurry.
The properties of the coal used in the experiment are given in Table 1 and the results of the determination are given in Table 2.
TABLE 1
Item
Analytical value (wt. %)
Technical
Water content
4.4
analysis
Ash content
14.0
Volatile matter
32.4
Fixed carbon
49.2
Elementary
C
84.3
analysis
H
5.4
N
1.8
O
8.1
S
0.4
The resultant slurry was evaluated by the following methods:
(a) Viscosity of Slurry:
The viscosity of the slurry was determined with a Haake rotational viscometer at 25 ° C. and the viscosity at 100 sec −1 down was determined from the rheogram.
(b) Stability of Slurry Left to Stand:
The stablity was tested by pot test method, wherein a slurry produced as described above was placed in a 250 ml wide-mouth polymer bottle and left to stand at 25° C. for 10 days. Then it was poured on a 1 mm sieve, then the quantity of the slurry remaining on the sieve (% by weight based on the whole slurry) was determined, the slurry remaining in the polymer bottle was stirred with a spatula and the hardness of the precipitate layer was organoleptically classified as follows to determine the stability:
∘: The slurry was soft.
Δ: The slurry was hard.
x: The slurry was quite hard.
COMPARATIVE EXAMPLE 1
A polystyrene (weight-average molecular weight: 7,500) synthesized by radical polymerization was sulfonated in the same manner as that of Synthesis Example 1. The effects of the resulting polymer as the dispersant for coal/water slurry was examined in the same manner as that of Example 4. The results are shown in Table 2. The NMR chart of the polystyrene before the sulfonation and that of methanol-soluble matter (about hexamer or lower) are shown in FIGS. 5 and 6, respectively. Since no peak at 4.1 to 4.5 which indicates the presence of the indane ring was observed in the figure, it was found that the polystyrene had no indane ring and that the sulfonated product thereof was different from the dispersant of the present invention. (NMR determination conditions were the same as the polymer analysis conditions of the present invention).
For reference, NMR chart of methanol-soluble polymer of the present invention (Example 1) before the sulfonation is given in FIG. 7 .
TABLE 2
Results of determination of properties of coal/water slurry
Stability
Amount of
Hardness
slurry on
of the
Molecular
Viscosity
the sieve
precipi-
weight
(cP)
(%)
tate
Present
Polymer-4
8,000
850
3
∘
invention
Polymer-2
15,000
800
4
∘
Polymer-6
30,000
790
6
∘
Comparative Example
15,000
790
11
∘
When the polymer of the present invention was used as the dispersant, the amount of the aggregate of the slurry [amount of that remaining on the sieve (%)] was reduced to ⅓ as compared with that remaining when a known dispersant was used.
EXAMPLE 5
The fluidity of concrete and amount of air were determined by using Polymer-2 produced in Example 1 (molecular weight: 15,000, counter ion: Ca) and radical-polymerized polystyrenesulfonate (molecular weight: 15,000, counter ion: Ca) produced in Comparative Example 1 as the super plasticizer for flowing concrete according to Nippon-Kenchiku Gakkai JASS ST-402 (the standard estimation for flowing concrete) and, in addition, the separation of aggregates caused when the additive was added in an excess amount was also examined.
The materials used were as follows and the obtained composition is shown in Table 3.
Materials Used:
Cement: ordinary portland cement (specific gravity: 3.15)
Fine aggregate: sand produced in Kasima district (specific gravity: 2.62)
Coarse aggregate: crushed stone from Tsukui Lake (specific gravity: 2.66)
TABLE 3
Composition
Water/
Fine
Coarse
Cement
Water
cement
aggregate
aggregate
s/a
320
179
55.9%
794
991
45%
Note 1) 0.028 % of an air entraining agent was used so that the amount of air in the concrete would be 4.5%.
Note 2) s/a = fine aggregate / (fine aggregate + coarse aggregate) (%)
50 l of a concrete having a composition given in Table 3 was kneaded with an lancaster mixer (100 l) for 90 sec. The slump value of the base concrete was 8.0 cm and the quantity of air was 4.3%. After leaving to stand for 15 min, 0.1% (by weight), based on the cement, of the polymer of the present invention was added thereto as the dispersant and they were kneaded for 30 sec. Then the slump value of the concrete and the quantity of air were determined. To examine the influence of the excess amount of the dispersant added thereto, the similar test was also conducted except that the amount of the dispersant was increased to 0.25% by weight. The similar test was repeated by using the radical-polymerized product. The test results are given in Table 4. It will be apparent that the fluidizing agent of the present invention exerts an excellent effect of reducing the separation of the aggregate.
TABLE 4
Results of concrete property test
Present invention
Comparative Example
Amount of fluidizing
0.1
0.25
0.25
agent added
(% based on cement)
Base concrete
8.0
8.0
8.0
Slump (cm)
Quantity of air (%)
4.3
4.3
4.3
Flowing concrete
19.1
22.7
22.5
slump (cm)
Quantity of air (%)
4.3
4.5
4.6
Aggregate separation
none
none
separated
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A dispersant comprises a polystyrenesulfonic acid having a weight-average molecular weight in the range of 2,000 to 100,000 or a salt thereof, wherein at least 70% of the terminals of the polymer chain have an indane ring of the formula (I):
wherein X represents a cation selected from the group consisting of a hydrogen, alkali metals, alkaline earth metals, ammonium and organic amines, and n and m each represent 0 or an integer of at least 1. The dispersant has excellent properties of dispersing organic and inorganic substances and an effect of remarkably improving the stability of a dispersion system such as a coal/water slurry.
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FIELD OF INVENTION
This invention relates to the field of contraceptive and sterilization devices and more particularly to reversible contraceptive devices and the methods of using such devices.
BACKGROUND OF THE INVENTION
Conventional contraceptive strategies generally fall within three categories: physical barriers, drugs and surgery. While each have certain advantages, they also suffer from various drawbacks. Barriers such as condoms and diaphragms are subject to failure due to breakage and displacement. Drug strategies, such as the pill and Norplant™, which rely on artificially controlling hormone levels, suffer from known and unknown side-effects from prolonged use. Finally, surgical procedures, such as tubal ligation and vasectomy, involve the costs and attendant risks of surgery, and are frequently not reversible. Thus, there remains a need for a safe, effective method of contraception, particularly a non-surgical method which is reversible.
SUMMARY OF THE INVENTION
The present invention is directed to a contraceptive or sterilization system for occluding a reproductive tract or lumen to prevent the passage of reproductive cells through the tract or lumen. The invention includes an occluding member expandable within the body lumen from a first configuration suitable for introduction into the body lumen to a second larger configuration to facilitate securing the expanded occluding member to at least a portion of a wall which defines the reproductive body lumen. The invention also includes means to facilitate securing the expanded occluding member to the wall of the body lumen and means to contract the expanded occluding member and the wall portion secured to the occluding member to occlude the reproductive body lumen sufficiently to prevent the passage of reproductive cells therethrough.
One presently preferred embodiment of the invention comprises a reversible contraceptive system which can be used to occlude either the fallopian tubes of a female patient, the vas deferens of a male patient or other reproductive tract. A key feature of the contraceptive system is a occluding member which is first secured to the wall defining the reproductive tract in an expanded condition and then is collapsed to smaller transverse cross-sectional dimensions to cause the collapse of the secured portion of the wall and thereby block the vessel passageway to prevent the passage of reproductive cells. The occluding member may be reopened by any number of suitable means. For example, by collapsing the occluding member about a plug or mandrel which can be left in place to effectively blocking the passageway until the patient wishes to reverse the procedure. The plug can be removed by suitable means such as conventional laparoscopic or other instruments to reopen the passageway. A balloon dilatation catheter may be used to further expand the opening once the plug is removed Other ways of reopening the reproductive lumen include leaving the proximal portion of the occluding member open when the member is collapsed so that an expandable member such a balloon on a catheter can be inserted and expanded. By means of a series of expansions and stepped advancements, the entire passageway can be reopened.
Preferably, the occluding member comprises a tubular member formed from a shape-memory alloy material and has a primary configuration which is relatively small in transverse dimensions to facilitate the insertion of the member into the desired body lumen. Once in place, the occluding member is then expanded to a second configuration with transverse dimensions roughly corresponding to or slightly larger than the body lumen so that the occluding member can be secured to the wall defining the body lumen. With the open, lattice-like framework of the occluding member expanded within the body lumen, endotherlialization through the open structure secures the occluding member to the wall defining the body lumen. By heating the occluding member formed of shape-memory alloy material to a temperature at or above the transition temperature of the shape-memory material, it transforms to a remembered closed or collapsed configuration which causes the wall secured to the occluding member to close down so that the passageway therethrough is occluded. The occluding member may be delivered to the desired location within the body lumen by suitable means such as a conventional balloon catheter similar to those used for delivering stents, aortic grafts and various types of prosthesis.
In one presently preferred embodiment, the occluding member has an open or lattice-like framework so that the growth of endothelial tissue through the openings of lattice-like framework so as to interconnect the occluding member and the wall of the body lumen. The surface of the occluding member may be treated to promote the endothelialization.
Once the occluding member is implanted into the body lumen and it has been sufficiently endothelialized to secure it to the body wall (which may take a week or more), it may be activated by warming the occluding member to a temperature at or above the transition temperature of the shape-memory material so it may revert to its remember constricted shape. Since the endotheliaization has secured the occluding member to the wall of the body lumen, the contraction of the occluding member to its remembered collapsed shape, causes the wall defining the body lumen to collapse along with the occluding member, effectively blocking the passageway. Alternatively, a plug may be located within the interior of the occluding member prior to heat activation so that the occluding member collapses onto the plug to block the lumen.
The occluding member may be mounted onto the exterior of a balloon of a dilatation balloon catheter in the first configuration with small transverse dimensions, and then be introduced and positioned within the region of the reproductive lumen to be occluded. The balloon is inflated to expand the occluding member, preferably with the outer diameter slightly larger than the inner dimensions of the reproductive lumen to which it is secured. The occluding member will remain in the open configuration until heated to a temperature at or above its martensite to austenite transition temperature which causes it to revert to its collapsed state. If the occluding member is collapsed about a plug, the plug may be extracted to reopen the passageway when the patient wishes to become fertile again.
The present invention provides effective sterilization or contraception for both males and females and importantly it is easily reversed. Moreover, the implantation and activation of the occluding member as well as the subsequent restoration of vessel patency requires easily used minimally invasive devices such as catheters, guidewires, guiding catheters and the like. These and other advantages of the invention will become more apparent from the following detailed description of the invention when taken in conjunction with the accompanying exemplary drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 illustrates a catheter with an occluding member embodying features of the invention mounted on an expandable member on a distal section of the catheter.
FIGS. 2 and 3 show one embodiment of the occluding member in expanded and contracted or closed configurations respectively.
FIGS. 4 and 5 show another embodiment of the occluding member in expanded and closed configurations respectively.
FIGS. 6 and 7 show yet another embodiment of an occluding member in expanded and closed configurations respectively.
FIG. 8 depicts the occluding member on a delivery catheter as shown in FIG. 1 within a reproductive tract or lumen.
FIG. 9 illustrates the expansion of the occluding member within the reproductive tract or lumen.
FIG. 10 illustrates the female reproductive anatomy and shows the occluding member positioned within one of the patient's fallopian tubes.
FIG. 11 illustrates the male reproductive anatomy and depicts an expanded occluding member within a vas deferens of a male patient.
FIG. 12 illustrates the occluding member secured to the wall of the reproductive tract by epithelial tissue.
FIG. 13 is a transverse cross-sectional view of the expanded epithelized occluding member as shown in FIG. 12 taken along the lines 13 — 13 .
FIG. 14 shows the occluding member in a collapsed state after being activated by warmed saline.
FIG. 15 is a transverse cross-sectional view of the collapsed occluding member as shown in FIG. 14 taken along the lines 15 — 15 .
FIG. 16 is similar to FIG. 14 and illustrates the occluding member collapsed about an elongated removable plug or mandrel.
FIG. 17 illustrates a transverse cross section of the occluding member shown in FIG. 16 , taken along line 17 — 17 .
FIG. 18 shows the occluding member being activated in a location distal to the proximal extremity thereof in order to keep the proximal end partially open to facilitate reopening the passageway.
FIG. 19 shows an embodiment of the occluding member having hooks.
DETAILED DESCRIPTION OF THE INVENTION
FIG. 1 illustrates a catheter 10 useful in the practice of the invention, which comprises an elongated shaft 12 having an inflation lumen 14 which is in fluid communication with inflatable member 16 mounted on a distal section of the catheter shaft and adapter 18 . Occluding member 20 , a self-supporting metallic member of shape-memory material, closely conforms to the diameter of the uninflated inflatable member 16 to facilitate introduction into the desired body lumen. Occluding member 20 is formed so that it has a remembered collapsed configuration with relatively small transverse dimensions. The occluding member 20 may be deformed to facilitate mounting onto the inflatable member 16 and is expanded by the inflatable member to an open expanded configuration within a body lumen. Upon heating to a transition temperature it will revert to the remembered configuration. In this embodiment the occluding member 20 has an open, lattice-type structure facilitating endothelialization which secures the occluding member to the wall defining the body lumen. Preferably, occluding member 20 can be deformed to an expanded diameter, preferably equal to or slightly larger than the dimensions of the body lumen within which the occluding member is to be disposed. For disposition within a female patient's fallopian tubes the expanded transverse dimensions should be about 0.1 mm to about 5 mm.
The occluding member may have a number of suitable configurations as shown in schematically in FIGS. 2–7 . FIG. 2 illustrates occluding member 22 in an open configuration and FIG. 3 its relatively small dimensioned configuration for introduction and advancement into the patient's body lumen. Occluding member 22 may be constructed from a length of shape memory hypodermic tubing. Slots 24 cut into the wall of the tubing allow expansion of the occluding member into an open configuration as shown in FIG. 2 . Likewise, in FIGS. 4 and 5 , occluding member 26 is a coil 28 of shape-memory wire or ribbon. FIGS. 6 and 7 show occluding member 30 , which comprises a braided tube of shape-memory wire or ribbon 32 . Finally, in FIGS. 1 and 8 occluding member 20 comprises a number of closed sinusoidal rings of shape-memory wire or ribbon and is mounted onto an inflatable member 16 of catheter 10 .
Inflation of inflatable member 16 expands occluding member 20 in a reproductive tract 38 to an open, relatively large diameter configuration as shown in FIG. 9 .
In each of these embodiments, the shape memory material of the occluding member should have a transition temperature sufficiently above the normal variation of human body temperature to prevent accidental activation which might prematurely collapse the occluding member. On the other hand, the transition temperature should be high enough so that thermal activation of the occluding member does not cause undesirable thermal damage to the surrounding tissue. The shape memory-material is preferably a shape memory, nickel-titanium alloy such as NITINOL and preferably has a transition temperature of between about 43° C. to about 70° C.
In each of the embodiments described above, certain conventional refinements may be employed. For example, the surface of the occluding member's framework may be designed to facilitate endothelial growth. Such modifications generally comprise providing the occluding member with an open or lattice-like framework to promote endothelial growth into as well as around the member to ensure it secure attachment to the wall of the body lumen. Suitable surface techniques include EDM machining, laser drilling, photo etching, scintering and the like. Additionally, increasing the surface area of the occluding member can also provide greater adhesion for the endothelial tissue. Suitable surface treatments include plasma etching, sand blasting, machining and other treatments to roughen the surface. In other embodiments, the shape-memory material may be coated or seeded to spur endothelialization. For example, the occluding device can be coated with a polymer having impregnated therein a drug, enzyme or protein for inducing or promoting endothelial tissue growth. In yet another refinement, the occluding member could be plated with or otherwise incorporate copper to produce an inflammatory response in the tissue of the wall defining the body lumen, which further contributes to the obstruction of the lumen. Other inflammatory materials my be suitable as well. For example, the occluding member could be radioactive, emitting alpha, beta or gamma particles.
The practice of the invention comprises the following general steps. An occluding member 20 having relatively small transverse dimension is mounted onto the exterior of balloon 16 of catheter 10 as shown in FIG. 1 . The catheter 10 is advanced under fluoroscopic or endoscopic visualization until occluding member 20 is positioned within one of the female patient's fallopian tubes 34 , as shown in FIG. 10 . Inflation fluid is introduced through adapter 18 to inflate inflatable member 16 . As shown in FIGS. 9–10 , inflation of inflatable member 16 expands occluding member 20 to an open configuration and lodging it in body lumen 38 . Catheter 10 is removed, leaving the expanded occluding member 20 implanted in body lumen 38 as shown in FIG. 12 . Another expandable member is delivered to the patient's other fallopian tube and expanded therein in the same manner. Alternatively, the occluding member may be expanded into positioned within the vas deferens 36 of a male patient as shown in FIG. 11 to provide male contraception using the same procedures.
Over a period of a week or more epithelial cells lining the lumen will proliferate, growing around the open framework of occluding member 20 as shown in FIGS. 12 and 13 thereby securing the wall defining the body lumen 38 to the expanded occluding member 20 . After the expanded occluding member 20 is sufficiently epithelized within the patient's reproductive tract 38 , it is thermally activated to return it to its remembered collapsed configuration. The occluding member may be activated by several means, including warmed fluid, RF energy, laser energy, or other suitable energy sources. A suitable activation system is shown in FIG. 14 where the distal end of catheter 40 is positioned adjacent to the occluding member 20 , saline fluid somewhat above the transition temperature is introduced to bathe occluding member 20 , raising its temperature to the transition point or higher, causing occluding member 20 to collapse to its closed, reduced-diameter configuration. The layer of epithelial tissue that forms within the lattice-like structure of the occluding member helps block and seal the lumen so as to prevent the passage of reproductive cells, eggs or sperm cells.
In an alternative embodiment of the invention is shown in FIG. 16 where a plug 42 is positioned inside occluding member 20 in the expanded condition so that upon activation the occluding member 20 collapses onto plug 42 , blocking the lumen 38 . The plug is preferably formed from an inert material such as a fluoropolymer, e.g. PTFE. Other suitable materials include high density polyethylene and silicone rubber. A number of modifications to the plug may also be suitable. For example, the plug could be used as a drug delivery device, similar to the Norplant™ device. The plug could also be used to provoke an inflammatory response as described above to augment the occlusion of the lumen. In such embodiments, plug 42 preferably has an outer diameter from about 0.25 mm to about 4 mm. The plug 42 may also have holes, deep grooves or which help to preserve at least part of the natural lining of the reproductive tract.
The occlusion of the lumen may be reversed simply by removing the plug 42 . If a passageway larger than passageway left by the removed plug 42 is desired, a balloon catheter can be advanced within the body lumen until the balloon is within the lumen left by the removal of the plug and then the balloon on the catheter is inflated to expanded the occluding member 20 , deforming it into an open configuration. It may be desirable when activating the expanded occluding member to the collapsed configuration to leave the proximal end of the occluding member somewhat open or in an expanded condition to facilitate the introduction of dilatation balloon on a catheter to facilitate the opening of the body lumen. As shown in FIG. 15 , the catheter 40 used to activate the occluding member may be positioned within the proximal end of the occluding member, so that the proximal end is unable to completely revert to its closed configuration. The reproductive tract could be subsequently close should contraception again be desired by heating the occluding member 20 so as to activate the transformation thereof to the collapsed configuration.
In embodiments of the invention employing the plug 40 , various other strategies are suitable to reverse the occlusion. For example, the plug 40 can simply be removed, restoring the lumen 38 to patency. Alternatively, the plug 40 may be hollow with a removable core (not shown). This core may be formed from a softer material, such as silicone, or could be threaded, in order to facilitate its removal. Similarly, the plug itself may be threaded so that removal would comprise a twisting motion, minimizing the stress on the tissue in which the occluding member is located.
In still other embodiments, mechanical, adhesive or other means may be employed to secure the expanded occluding member 20 to the vessel wall defining the reproductive passageway 38 . For example, the means to secure a stent or prosthetic device to an aortic or arterial wall described in U.S. Pat. No. 4,140,126; U.S. Pat. No. 4,562,596; U.S. Pat. No. 4,577,631; U.S. Pat. No. 4,787,899; U.S. Pat. No. 5,104,399; U.S. Pat. No. 5,167,614; U.S. Pat. No. 5,275,622; U.S. Pat. No. 5,456,713; and U.S. Pat. No. 5,489,295 may be used with the present invention to interconnect the wall defining the reproductive tract and the expandable member. These patents are incorporated herein in their entireties by reference.
FIG. 19 illustrates one embodiment of invention having hook members 50 on the occluding member 20 . The hook members 50 spread radially outward from the longitudinal axis of the occluding member 20 , so that they contact the wall defining the reproductive tract as the occluding member expands therein. Thus, the hook members 50 become embedded in the wall defining the reproductive tract to anchor the occluding member 20 therein. In the embodiment illustrated in FIG. 19 , the hook members 50 are located on the distal and proximal ends of the occluding member 20 , although other suitable configurations exist including hook members 50 which are disposed along all or part of a length of the occluding member 20 . A variety of suitable means may be used to attach the hook members 50 to the occluding member 20 , such as welding or brazing. Alternatively, as shown, they are attached to a connecting member 51 which is attached to the occluding member 20 .
Various modifications and improvements may be made to the present invention without departing from the scope thereof. For example, a mechanical expandable member such as described in U.S. Pat. No. 4,585,000, which is incorporated herein by reference, may be used to expand the expandable member within the reproductive tract to engage the wall thereof. Moreover, although individual features of embodiments of the invention may be shown in some of the drawings and not in others, those skilled in the art will recognize that individual features of one embodiment of the invention can be combined with any or all the features of one or more of the other embodiments.
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A device and method of using the device for contraception or sterilization and particularly for reversible contraception by occluding a reproductive lumen to prevent the passage of reproductive cells through the lumen for a desired period of time until the patient wishes to become fertile again and then be reopened. The occluding member preferably comprises a tubular framework formed from a shape memory material configured to be implanted in a reproductive lumen. The occluding member is implanted within a body lumen, secured to the wall of the reproductive lumen and then collapsed to collapse the wall and occlude the lumen. Alternatively, the occluding member may be collapsed upon a solid plug. The closure of the reproductive lumen may be reversed by introducing a balloon catheter and by a series of inflations of the balloon reexpanding the collapsed occluding member or by removing the plug. The occluding member and the plug may be configured to facilitate endothelialization, to provoke an inflammatory responses or to deliver a drug.
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FIELD OF THE INVENTION
[0001] The field of the invention generally relates to interconnection technologies to transport data between data devices. In particular, the invention relates to transporting data between data devices, for example between private branch exchange elements, using symbol encoded physical layer.
BACKGROUND OF THE INVENTION
[0002] In many circumstances, proprietary interconnection technologies are utilized to exchange data between data devices. For example, RS-485 type technology is used to transport Time Division Multiplexed (TDM) data in many present commercial practices. TDM data are exchanged, for example, between private branch exchange (PBX) equipments. RS-485 transport data across four (4) pairs of wires (8 conductors) as CLK, SYNC, DATA_IN and DATA_OUT.
[0003] The proprietary interconnection technologies, such as the traditional TDM PBX elements (e.g. line cards, switching elements or expansion boxes), are typically costly to produce and to maintain. Also, due to the proprietary nature, interoperability with other communication equipments becomes limited. In addition, physical distances between data elements are limited when using communication technologies like the RS-485.
[0004] Standard interconnection technologies are also utilized to exchange data between data devices, and these technologies provide the benefit of defined, standardized layers. For example, the Ethernet network, based on carrier sense multiple access with collision detection (CSMA/CD) standard, is widely used. Also Token Ring is widely used.
[0005] Because of the standardization, the equipments are less costly to produce and to maintain. Also, the interoperability is high. In addition, these technologies allow the transport distances to be large.
[0006] However, these standards do not guarantee delivery of data within a fixed periodic interval of time. Thus, there is a risk in utilizing such standardized networks to transport time critical data.
SUMMARY OF THE INVENTION
[0007] The present invention is intended to address one or more of the disadvantages of the conventional systems to exchange communications data. Thus, according to an embodiment of the present invention, a TDM apparatus comprises a media access controller (MAC) layer device configured to generate a framed TDM data to be delivered to at least one destination TDM apparatus and a physical layer device configured to transmit the framed TDM data to a neighbor TDM apparatus over a transport medium. The framed TDM data is guaranteed to be delivered to the at least one destination TDM apparatus within a fixed periodic interval.
[0008] According to another embodiment of the present invention, a method to exchange TDM data for a TDM apparatus comprises generating a framed TDM data to be delivered to at least one destination TDM apparatus and transmitting to the framed TDM data to a neighbor TDM apparatus over a transport medium. The generated framed TDM data is guaranteed to be delivered to the at least one destination TDM apparatus within a fixed periodic interval.
[0009] According to yet another embodiment of the present invention, a system to exchange TDM data comprises a plurality of TDM apparatuses. Each of the plurality of TDM apparatuses includes a MAC device configured to generate a framed TDM data to be delivered to at least one destination TDM apparatus and a physical layer device configured to symbol encode and transmit the symbol encoded framed TDM data to a neighbor TDM apparatus over a transport medium. The system is such that the symbol encoded framed TDM data is guaranteed to be delivered to the at least one destination TDM apparatus within a fixed periodic interval.
BRIEF DESCRIPTION OF THE DRAWINGS
[0010] Features of the present invention will become more fully understood to those skilled in the art from the detailed description given herein below with reference to the drawings, which are given by way of illustrations only and thus are not limitative of the invention, wherein:
[0011] FIG. 1 illustrates communication apparatuses connected to each other over a transport medium according to an embodiment of the present invention;
[0012] FIG. 2 illustrates an exemplary media access control frame format according to an embodiment of the present invention;
[0013] FIG. 3 illustrates an example of a data stream framed by the media access control layer according to an embodiment of the present invention;
[0014] FIG. 4 illustrates an example communication apparatuses where retransmission of framed TDM data occurs according to an embodiment of the present invention;
[0015] FIG. 5 illustrates steps of a method for generating and transmitting communication data according to an embodiment of the present invention;
[0016] FIG. 6 illustrates exemplary details of the framed data generating step of FIG. 5 according to an embodiment of the present invention;
[0017] FIGS. 7A and 7B illustrate a method of receiving and processing framed data according to an embodiment of the present invention; and
[0018] FIGS. 8, 9 , and 10 illustrate various networking architectures of systems according to embodiments of the present invention.
DETAILED DESCRIPTION
[0019] For simplicity and illustrative purposes, the principles of the present invention are described by referring mainly to exemplary embodiments thereof. The same reference numbers and symbols in different drawings identify the same or similar elements. Also, the following detailed description does not limit the invention. The scope of the invention is defined by the claims and equivalents thereof.
[0020] The expression “connects” or “communicates” as used herein refers to any connection, coupling, link or the like by which signals carried by one element are imparted to the “connecting element.” Such “communicating” devices are not necessarily directly connected to one another and may be separated by intermediate components and/or devices. Likewise, the expressions “connection”, “operative connection”, and “placed” as used herein are relative terms and do not necessarily require a direct physical connection.
[0021] In an embodiment of the present invention, an apparatus may exchange time critical information - video, voice, stock market quotes, etc.—with another similar apparatus. Voice quality is measured using a scale known as the “Mean Opinion Score” (MOS), which ranges from 1 (very poor, unintelligible) to 5 (perfect quality). For example, for a good quality voice transmission (MOS>4), using the standard ITU G.711 A-law/Mu-law codec, it is generally accepted that data bytes should be delivered to the destination within 125 microsecond intervals.
[0022] For videos, a full frame of data should be delivered ranging from every 1/20 th second to every 1/30 th second and even faster. Another example of time critical data is the information of various stock markets. In this environment, prices of stocks change continually and having the up to the second information is very valuable. Trades that can be delivered to the brokers with a guaranteed delivery time ensures the trade can be made against a known stock price.
[0023] FIG. 1 is an embodiment of the present invention where communication apparatuses 102 and 104 communicate with each other over a transport medium 110 . The apparatuses 102 and 104 may be TDM apparatuses and one can be considered to be a neighbor of the other. For simplicity, only two TDM apparatuses are illustrated. However, it is entirely possible, and indeed contemplated, that there are many more communication apparatuses connected with one another.
[0024] Also, for simplicity, the TDM apparatuses 102 and 104 are shown as being directly connected to each other through the transport medium 110 . Such direct connection may be accomplished through a physical connection, such as a fiber optic line or a twisted pair line.
[0025] However, there may be one or more intervening devices between the TDM apparatuses 102 and 104 such as repeaters, amplifiers, and re-transmitters that allow the message traffic to flow between the TDM apparatuses 102 and 104 . Thus, the transport medium 110 is best viewed as a logical connection. As will be shown later, the transport medium 110 may carry standardized physical layer message traffic.
[0026] The arrows entering into both TDM apparatuses 102 and 104 indicates that the transport medium 110 is bi-directional. Indeed, the transport medium 110 may be such that the communication between the TDM apparatuses 102 and 104 is full-duplex.
[0027] Each TDM apparatus 102 , 104 may implement one or more layers of the ISO/IEC Model for Open Systems Interconnection (OSI). Again for simplicity, only two layers are shown—the Media Access Control (MAC) layer (which is a sublayer of OSI's data link layer) and the physical (PHY) layer. The MAC layer device 106 receives data from one or more MAC clients, frames the received data, and passes the framed data to the PHY layer device 108 .
[0028] An exemplary MAC frame format 200 according to an embodiment of the present invention is illustrated in FIG. 2 . Each frame may include a synchronization pattern, a plurality of time slots (time slots O to n), a control channel, and a frame check sequence.
[0029] The synchronization pattern may be a sequence that indicates a repetitive period of the MAC layer packet. It also provides a unique pattern to allow a bit synchronous receiver to locate and delineate a correct boundary in a sequence of bit stream. For example, the synchronization pattern may define the correct octet boundary.
[0030] Time slots may include time critical multiplexed payload data (for example, telephone speech samples, video data or stock prices). Each timeslot represents a unique telephone call, video stream or stock price.
[0031] Control channel may be a sequence used for conveying inter-equipment control messages, for example, assigning unique addresses to each apparatus, indicating error conditions, and indicating clock source reliability.
[0032] Frame Check Sequence may be a sequence calculated using common frame checksum techniques (For example: (Cyclic Redundancy Check) CRC- 32 (4 octets), CRC- 16 (2 octets) or (Byte Interleaved Parity) BIP- 8 (1 octet) over the entire packet. The Frame check sequence may be used to provide indication of possible packet corruption due to bit-errors, and also allows the receiver to correctly identify and delineate the packet boundaries.
[0033] It is possible to transport multiple channels of information a single transport medium through a multiplexing technique. An example of multiplexing technique is time division multiplexing (TDM). This is a technique in which different pieces of data occupy a particular time slot in a message data stream.
[0034] FIG. 3 illustrates an example of a data stream framed by the MAC layer device 106 according to an embodiment of the present invention. The framed data stream may include one or more channels. Data contained within each channel are destined for a particular destination apparatus, i.e. a particular TDM apparatus node in a network. Multiple channels may be destined for the same node. For example, channels 1 and 4 of FIGS. 3 may be destined to a particular TDM apparatus, which is different from a destination of channel 2 .
[0035] In FIG. 3 , n channels are transmitted within a fixed time interval—in this instance 125 microseconds (to transport voice data for example)—by the MAC layer device 106 . It should be noted that the fixed time interval may be any value deemed appropriate for the type of data. Indeed, different frames transmitted by the same MAC layer device 106 may have different time interval associated with each packet.
[0036] Each channel may include one or more time slices (TS) of data, and each time slice may represent data for a particular communication instance within the node of the network. For example, if the node is a PBX equipment, each TS may represent data for telephone conversations being processed by the PBX equipment. In FIG. 3 , channel 4 includes 32 time slices (TS 0 -TS 1 F). Thus, the PBX equipment may handling as many as 32 simultaneous telephone conversations. For the situation described in FIG. 3 , the MAC framed data of FIG. 3 may be considered to be a framed TDM data.
[0037] More than one time slice may be associated with the same communication instance. For example, again referring to FIG. 3 , time slices TS 0 and TS 1 may be associated with the same telephone conversation. Also, multiple time slices may be used to deliver higher data rate for those communication instances that require the higher rate. For example, video information for an application on a node may be delivered to the node using all or some of the time slices. In short, each time slice may represent a specific type of time critical data.
[0038] In FIG. 3 , the data width of the time slices is shown to be a byte or an octet (8 bits). However, the time slices are not limited to this data width. The widths of the time slices may be set to any arbitrary value depending on the physical transport medium and the needs of applications.
[0039] It should be noted that the MAC frame format 200 in FIG. 2 may include timing information and destination information which are used to ensure that the data channels arrive at the proper destination within the fixed periodic interval set by the MAC layer device 106 . Such timing and destination information may be included in the control channel.
[0040] The MAC layer device 106 may set the fixed periodic interval for each frame from a plurality of predetermined fixed periodic intervals. The MAC frame format 200 may include an interval code to indicate the particular fixed periodic interval set for the associated framed TDM data. As noted above, the framed TDM data such that the framed TDM data is guaranteed to be delivered to the designated destination within the fixed periodic interval of time. This significantly reduces the risk when transporting time critical data over the network.
[0041] The framed TDM data stream of FIG. 3 may be encoded by the PHY layer device 108 before being provided to the transport medium 110 . The PHY layer device 108 may utilize standardized physical layer protocols that are widely available today. Examples of standardized physical layer protocols include the standards listed in the IEEE Standard 802.3 documentation. These include, but not limited to, the IEEE 100BASE-X, 100BASE-TX, 1000BASE-T, 1000BASE-X, 10GBASE-X and all variants (copper, fiber, etc.) thereof. Of course, there are other standardized physical layer protocols such as Fiber Channel (FC- 1 , FC- 2 , 10 GFC, etc.), Serial Rapid-IO, PCI-Express, etc.
[0042] The PHY layer device 108 may symbol encode the framed TDM data. For example, every four bits of the MAC frame data may be translated to five bits (4B/5B transmission coding) by the PHY layer device 108 . This is a form of dc-balanced encoding mechanism used to prevent too many consecutive ones or zeros from being transmitted and thereby allow common phase-locked loop techniques to be used to recover the original bit clock used to send the data. Other examples of symbol encoding include 8B/10B transmission coding (which is another form of dc-balanced encoding), 4D-PAM5 (data encoding using 5 voltage levels), and MLT-3 (data encoding using 3 voltage levels)—as used by 100-BASETX.
[0043] The PHY layer device 108 may symbol encode the framed TDM data from the MAC layer device 106 and transmit the symbol encoded framed TDM data to a neighbor TDM apparatus. For example, the PHY layer device 108 of the TDM apparatus 102 may transmit the symbol encoded framed TDM data to the neighbor TDM apparatus 104 over the transport medium 110 .
[0044] The PHY layer device 108 of the TDM apparatus 104 may receive the symbol encoded framed TDM data from the TDM apparatus 102 , decode the received symbol encoded framed TDM data, and provide the decoded framed TDM data to its corresponding MAC layer device 106 . The decoded framed TDM data is the same framed TDM data from the MAC layer device 106 of the TDM apparatus 102 . In other words, the decoded framed TDM data may include the interval code, at least one channel including at least one time slice, and destination information associated with each channel.
[0045] The MAC layer device 106 may examine the decoded framed TDM data to determine if one or more channels are destined for the corresponding TDM apparatus. I.e., the MAC layer device 106 of the apparatus 104 determines whether any channels of the decoded framed TDM data are destined for the TDM apparatus 104 . If so, the MAC layer 106 proceeds to process the corresponding channel or channels.
[0046] As implied above, the TDM apparatus 104 may not be the ultimate destination for some channels of the framed TDM data from the TDM apparatus 102 . In this situation, the remaining channels should be delivered to their correct destinations. To accomplish this, the PHY layer device 108 may transmit the framed TDM data received from a first neighbor TDM apparatus to a second neighbor TDM apparatus. This is illustrated in FIG. 4 .
[0047] In FIG. 4 , the TDM apparatus 104 is illustrated to have TDM apparatus 102 as a first neighbor (connected through a first transport medium 110 ) and TDM apparatus 402 as a second neighbor (connect through a second transport medium 410 ). The PHY layer device 108 of the TDM apparatus 104 may retransmit to the framed TDM data from the first neighbor TDM apparatus 102 to the second neighbor TDM apparatus 402 as long as there are channels with destination other than itself—i.e. destinations other than TDM apparatus 104 . Likewise, the TDM apparatus 402 may also retransmit the framed TDM data to yet another neighbor if the there are channels with destinations other than itself.
[0048] If the TDM apparatus 104 receives framed TDM data from the TDM apparatus 402 , the retransmission, if necessary, would be to the TDM apparatus 102 . It should be noted that communications through one or both of the transport mediums 110 and 410 may be full duplex.
[0049] To ensure that the framed TDM data is not transmitted and retransmitted forever, upon determining that there are channels destined for the current TDM apparatus, the MAC layer device 106 may reframe the TDM data received from the first neighbor TDM apparatus to mark the corresponding channel or channels as “consumed”. The PHY layer device 108 may then symbol encode the reframed TDM data prior to transmitting to the second neighbor TDM apparatus. Eventually, when all channels are consumed, the framed and reframed TDM data need not be retransmitted again.
[0050] As another way to ensure that a particular framed TDM data is not transmitted and retransmitted unnecessarily, each framed TDM data may include a frame identification, for example in the control channel. The MAC layer device 106 may then be able to recognize that a particular framed TDM data has been previously been received by the current TDM apparatus. When this occurs, the MAC layer device 106 and/or the PHY layer 108 may simply prevent retransmitting the particular framed TDM data.
[0051] It may be that a particular framed TDM data may have no channels destined for the current TDM apparatus. For example, again referring to FIG. 4 , the framed TDM data from the TDM apparatus 102 may not have any channels with destination designated as the TDM apparatus 104 . In this instance, since there will be no consumed channels, there would be no need for reframing the data and therefore, no need to symbol encode the reframed TDM data. The TDM apparatus 104 , through the corresponding PHY layer 108 , may simply retransmit the received symbol encoded framed TDM data from the first neighbor TDM apparatus 102 to the second neighbor TDM apparatus 402 .
[0052] FIG. 5 illustrates steps of a method 500 for generating and transmitting communication data according to an embodiment of the present invention. The steps may be performed by the TDM apparatus 102 , 104 , 402 of FIG. 4 for example. As illustrated in FIG. 5 , framed data may be generated (step 502 ). The framed data may be framed TDM data as discussed above. The framed TDM data may be symbol encoded (step 506 ) and then transmitted through a transport medium (step 506 ).
[0053] FIG. 6 illustrates exemplary details of the framed data generating step 502 according to an embodiment of the present invention. To generated the framed data, data from MAC clients may be received (step 602 ). For each data from the clients, destinations may be determined (step 604 ). The client's data may be packaged in time slices and framed accordingly (step 606 ). An appropriate fixed periodic interval may be set and coded into the framed data (step 608 ).
[0054] Just as a TDM apparatus may generate and transmit framed data, the same TDM apparatus may also receive and process framed data from other TDM apparatuses. FIGS. 7A and 7B illustrate this aspect. As illustrated, symbol encoded framed TDM data may be received (step 702 ) and decoded (step 704 ).
[0055] The decoded framed TDM data may be examined to determine if processing may stop (step 706 ). For example, the decoded framed TDM data may have been examined previously by the current TDM apparatus. This would indicate that the decoded framed TDM data has been examined and processed other TDM apparatuses of the network as well. In other words, the decoded framed TDM data has been processed before and there is no need to continue. Another reason for stopping the process is if all the channels have been consumed—i.e., there is no data left to process.
[0056] If it is determined to stop the process, then the method may end (YES branch from step 706 ). If it is determined that process should continue (NO branch from step 706 ), this indicates that there are still information channels that have not been processed (not consumed).
[0057] If there are still unconsumed channels, the framed TDM data may be examined to determine if the current TDM apparatus is designated to be the destination of one or more channels of the framed data (step 708 ). If not, then the received symbol encoded framed data may simply be retransmitted to another neighbor since there is no change to the data (step 710 ). If there are channel or channels designating the current TDM apparatus as the destination, then the corresponding channels may be processed accordingly (step 712 ) and the processed channels may be marked as consumed (step 714 ).
[0058] After the processing and marking the channels, the method once again may determine if the processing may stop (step 716 ). For example, all channels of the framed TDM data may have been consumed at this point, which makes further processing by any TDM apparatus unnecessary.
[0059] As another example, the current TDM apparatus may be designated as being “end of the line” where the current node simply does not retransmit any received framed data. This may be appropriate where a TDM apparatus is connected to only one other TDM apparatus. The processing may be halted if appropriate (YES branch from step 716 ).
[0060] If the processing of the framed data is to be continued (NO branch from step 716 ), then the framed TDM data, including the channels marked as consumed, may be reframed (step 718 ), symbol encoded (step 720 ), and transmitted to another neighbor (step 722 ).
[0061] FIGS. 8, 9 , and 10 illustrate possible networking architectures of system made up of multiple TDM apparatuses. FIG. 8 illustrates a ring architecture, FIG. 9 illustrates a star architecture using a central bridge, and FIG. 10 illustrates a chain architecture.
[0062] In FIG. 8 , the system 800 includes six (6) TDM apparatuses, much like the TDM apparatuses 102 , 104 , and 402 of FIG. 4 . While six TDM apparatuses 802 - 1 to 802 - 6 are illustrated, it is to be noted that the architecture is not so limited and may include an arbitrary number of TDM apparatuses. The bidirectional arrows between the TDM apparatuses indicate that the direction of communication is bidirectional between each neighboring TDM apparatuses. Further, the communication may be full duplex.
[0063] Any TDM apparatus may transmit framed TDM data to any other TDM apparatus, even if the two apparatuses do not directly communicate with each other. For example, the TDM apparatus 802 - 1 may transmit framed TDM data with one or more channels that are destined for the TDM apparatus 802 - 4 . The framed data would first go to either the TDM apparatus 802 - 6 or to the TDM apparatus 802 - 2 . The receiving TDM apparatus 802 - 2 or 802 - 6 , after examining the framed TDM data, would forward the framed TDM data onward until the destination TDM apparatus 802 - 4 is reached.
[0064] Due to the structure of the MAC frame format and the functioning of the TDM apparatuses, the channels of the framed TDM data destined for the TDM apparatus 802 - 4 is guaranteed to reach the destination within the fixed interval period set by the originator TDM apparatus 802 - 1 .
[0065] As described above, a framed TDM data may be prevented from circling forever as described above. For example, all channels may be consumed making further retransmission and processing unnecessary. Also the framed TDM data may complete a loop in the network and then detected as having been processed previously by one of the TDM apparatuses.
[0066] It is to be noted that the ring illustrated in FIG. 8 is a logical ring. Between any two neighboring TDM apparatuses, there may physically exist intervening devices such as signal repeaters, amplifiers and re-transmitters. However, the communication between any two neighboring TDM apparatuses is not interfered with.
[0067] FIG. 9 illustrates a system 900 of a star architecture utilizing a central bridge 904 . The system 900 includes a plurality of TDM apparatuses 902 - 1 to 902 - 6 . Again, the number of TDM apparatuses is not so limited. In this architecture, each TDM apparatuses 900 -k, k=1 to n, is connected (again logically) to the central bridge 904 . The communication between the TDM apparatus 900 -k and the central bridge 904 may be bidirectional and also may be full duplex. Like the architecture of FIG. 8 , between the TDM apparatus 902 -k and the central bridge 904 , intervening devices such as signal repeaters, amplifiers and re-transmitters may be included.
[0068] In this architecture, the originating TDM apparatus may simply transmit the framed TDM data to the central bridge 904 , which then may examine the framed TDM data and route the data to the appropriate destination(s).
[0069] The central bridge 904 may be intelligent in its routing. For example, when an original framed TDM data from a TDM apparatus is received, the central bridge 904 may convert the original framed TDM data and transmit new framed TDM data to the appropriate destination(s).
[0070] As an illustration, assume that the TDM apparatus 902 - 1 transmits an original framed TDM data with channels destined for TDM apparatuses 902 - 2 and 902 - 5 . The central bridge 904 may generate a new framed TDM data particularized for each destination TDM apparatus 902 - 2 , 902 - 5 . The particularized framed TDM data for the TDM apparatus 902 - 2 would only include channels originally destined for the TDM apparatus 902 - 2 . Like wise, the TDM apparatus 902 - 5 would receive a particularized framed TDM data with channels only destined for itself.
[0071] The receiving TDM apparatuses would not retransmit the particularized framed TDM data since all channels would be consumed. Also, each TDM apparatus would be, by definition, is an end of the line TDM apparatus.
[0072] A less intelligent routing alternative is the following. The central bridge 904 may still examine the framed TDM data from the originator. However, instead of generating new framed TDM data particularized for each destination TDM apparatus, the central bridge 904 may simply retransmit exact copies of the original framed TDM data to the appropriate destination TDM apparatus. In other words, the central bridge 904 may multicast as necessary. Using the above-noted illustration, the central bridge 904 may multicast the original framed TDM data from the TDM apparatus 902 - 1 to both TDM apparatuses 902 - 2 and 902 - 5 .
[0073] In this less intelligent routing, the destination TDM apparatuses would not retransmit the multicasted framed TDM data since they are both end of the line TDM apparatuses.
[0074] At the other extreme, a brute force routing may be employed by the central bridge 904 . In this instance, any original framed TDM data received from each TDM apparatus may simply be broadcasted to all other TDM apparatuses. This ensures that the designated destination TDM apparatuses receive the framed TDM data. And again, the framed TDM data would not be retransmitted by the TDM apparatuses since all are end of the line apparatuses.
[0075] The choice of routing scheme employed in this star architecture may depend on particular circumstances. For example, the intelligent approach would be suitable in situations where the processing power of the central bridge is very high in relation to the bandwidth of the connections between the TDM apparatuses and the central bridge. In other words, intelligent routing is appropriate if the connections between the bridge and the TDM apparatuses is the bottleneck. Conversely, if the processing capability of the central bridge is the bottleneck, then it may be more efficient overall to utilize the multicast or broadcast routing.
[0076] FIG. 10 illustrates system 1000 of a chain architecture as noted above. As illustrated, the system 1000 includes a plurality of TDM apparatuses 1000 - 1 to 1000 -N. The TDM apparatuses 1000 - 1 and N are the end of the line TDM apparatuses. Similar to the architectures of FIGS. 8 and 9 , between adjacent TDM apparatuses, intervening devices such as signal repeaters, amplifiers and re-transmitters may be included. In this architecture, an originating TDM apparatus may simply send the framed TDM data in both directions with the exceptions of the apparatuses 1000 - 1 and 1000 -N.
[0077] As a more intelligent alternative, each TDM apparatus may generate framed TDM data segregating the destinations so that each framed TDM data need be sent to only one side. For example, the TDM apparatus 1002 - 3 may generate a framed TDM data for destinations TDM apparatuses 1002 - 1 and 1002 - 2 and generate another framed TDM data for destinations 1002 - 4 to 1002 -N.
[0078] It is to be noted that the architectures of the systems are not limited to the architectures of FIGS. 8, 9 , and 10 . It is fully contemplated that other types of network architectures are possible without departing from the scope of the invention. Also, while not shown, the particular architecture employed may be a combination of architectures.
[0079] While the invention has been described with reference to the exemplary embodiments thereof, it is to be understood that various modifications may be made to the described embodiments without departing from the spirit and scope of the invention thereof. The terms as descriptions used herein are set forth by way of illustration only and are not intended as limitations.
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Embodiments of methods, apparatuses, and systems to transport Time Division Multiplexed (TDM) utilizing symbol encoded physical layer are disclosed. The embodiments of the invention provide a low cost solution to exchange data between TDM data elements while retaining guaranteed performance. A media access control layer generates framed data and the system guarantees delivery of the framed data to the designated destination within a fixed interval period of time.
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BACKGROUND OF THE INVENTION
This invention is in the field of copper and through-silicon via (TSV) chemical mechanical polishing (CMP). More specifically, it is related to the CMP slurry compositions and method of using the slurry compositions.
The use of chemical mechanical planarization (CMP) in semiconductor manufacturing is well known to those of skill in the art. For example, CMP processing can be used to remove excess metal, such as copper, used to form interconnects, vias and lines. Work has been done in the field of the invention.
U.S. Pat. No. 6,436,811 discloses a process for forming a metal interconnect comprising the steps of forming a concave in an insulating film formed on a substrate, forming a copper containing metal film over the whole surface such that the concave is filled with the metal and then polishing the copper-containing metal film by chemical mechanical polishing, characterized in that the polishing step is conducted using a chemical mechanical polishing slurry comprising a polishing material, an oxidizing agent and an adhesion inhibitor preventing adhesion of a polishing product to a polishing pad, while contacting the polishing pad to a polished surface with a pressure of at least 27 kPa. This invention allows us to prevent adhesion of a polishing product to a polishing pad and to form a uniform interconnect layer with an improved throughput, even when polishing a large amount of copper-containing metal during a polishing step.
U.S. Pat. No. 5,770,095 provides a polishing method including the steps of forming a film made of material containing a metal as a main component over a substrate having depressed portions on a surface thereof so as to fill the depressed portions with the film, and polishing the film by a chemical mechanical polishing method using a polishing agent containing a chemical agent responsible for forming a protection film on a surface of the film by reacting with the material containing a metal as a main component, thereby forming a conductive film in the depressed portions. U.S. Pat. No. 5,770,095 also provides a polishing agent, which is used in forming a film made of material containing a metal as a main component in depressed portions of a substrate having depressed portions on a surface thereof by using a chemical mechanical polishing method, including a chemical agent responsible for forming a protection film on the surface of a substrate to be polished by reacting with the material containing a metal as a main component.
U.S. Pat. No. 6,585,568 provides a chemical mechanical polishing slurry for polishing a copper-based metal film formed on an insulating film comprising a concave on a substrate, comprising a polishing material, an oxidizing agent and water as well as a benzotriazole compound and a triazole compound. The polishing slurry may be used in CMP to form a reliable damascene electric connection with excellent electric properties at a higher polishing rate, i.e., a higher throughput while preventing dishing.
U.S. Pat. No. 6,679,929 teaches a polishing composition comprising the following components (a) to (g):
(a) at least one abrasive selected from the group consisting of silicon dioxide, aluminum oxide, cerium oxide, zirconium oxide and titanium oxide; (b) an aliphatic carboxylic acid; (c) at least one basic compound selected from the group consisting of an ammonium salt, an alkali metal salt, an alkaline earth metal salt, an organic amine compound and a quaternary ammonium salt; (d) at least one polishing accelerating compound selected from the group consisting of citric acid, oxalic acid, tartaric acid, glycine, a-alanine and histidine; (e) at least one anticorrosive selected from the group consisting of benzotriazole, benzimidazole, triazole, imidazole and tolyltriazole; (t) hydrogen peroxide, and (g) water.
U.S. Pat. No. 6,440,186 teaches a polishing composition comprising: (a) an abrasives; (b) a compound to form a chelate with copper ions; (c) a compound to provide a protective layer-forming function to a copper layer; (d) hydrogen peroxide; and (e) water, wherein the abrasive of component (a) has a primary particle size within a range of from 50 to 120 nm.
U.S. Pat. No. 6,838,016 discloses a polishing composition comprising the following components (a) to (g): (a) an abrasive which is at least one member selected from the group consisting of silicon dioxide, aluminum oxide, cerium oxide, zirconium oxide and titanium oxide, (b) a polyalkyleneimine, (c) at least one member selected from the group consisting of guinaldic acid and its derivatives, (d) at least one member selected from the group consisting of glycine, α-alanine, histidine and their derivatives, (e) at least one member selected from the group consisting of benzotriazole and its derivatives, (f) hydrogen peroxide, and (g) water.
US patent application No. 2007/0167017 A1 provides a metal-polishing liquid that comprises an oxidizing agent, an oxidized-metal etchant, a protective film-forming agent, a dissolution promoter for the protective film-forming agent, and water. The application also teaches a method for producing it; and a polishing method of using it. Also provided are materials for the metal-polishing liquid, which include an oxidized-metal etchant, a protective film-forming agent, and a dissolution promoter for the protective film-forming agent.
US 2009/0156006 discloses a chemical-mechanical polishing (CMP) composition suitable for polishing semi-conductor materials. The composition comprises an abrasive, an organic amino compound, an acidic metal complexing agent and an aqueous carrier. A CMP method for polishing a surface of a semiconductor material utilizing the composition is also disclosed.
US2010/0081279 teaches an effective method for forming through-base wafer vias in the fabrication of stacked devices is described. The base wafer can be a silicon wafer in which case the method relates to TSV (through-silicon via) technology. The method affords high removal rates of both silicon and metal (e.g., copper) under appropriate conditions and is tuneable with respect to base wafer material to metal selectivity.
As industry standards trend toward smaller device features, there is a continuous developing for copper and TSV CMP slurries.
Thus, there is still a significant need for CMP slurries that deliver superior planarization with high and tunable removal rates and low defects when polishing bulk copper layers of the nanostructures of IC chips.
The copper and TSV CMP slurry composition described herein satisfies the need for providing high, tunable, effective polishing at desired and high polishing rates for polishing copper films with low defects and high planarization efficiency.
BRIEF SUMMARY OF THE INVENTION
In one aspect, the invention provides a copper and TSV chemical mechanical polishing (CMP) slurry composition comprises:
a) an abrasive;
b) a chelating agent;
c) a corrosion inhibitor;
d) choline salt as copper removal rate booster and total defect reducer;
e) an organic amine;
f) an oxidizer;
g) biocide;
h) remaining is substantially liquid carrier;
wherein pH of the polishing slurry composition is between 5.0 to 8.0.
In another aspect, the invention provides a method of chemical mechanical polishing a removal material of copper or copper-containing material from a surface of a semiconductor substrate comprising steps of:
a) providing a polishing pad; b) providing a chemical mechanical polishing slurry composition comprising
1) an abrasive; 2) a chelating agent; 3) a corrosion inhibitor; 4) choline salt as copper removal rate booster and total defect reducer; 5) an organic amine; 6) an oxidizer; 7) biocide; 8) remaining is substantially liquid carrier; wherein pH of the polishing slurry composition is between 5.0 to 8.0;
c) contacting the surface of the semiconductor substrate with the polishing pad and the chemical mechanical polishing slurry composition; and d) polishing the surface of the semiconductor substrate; wherein at least a portion of the surface that containing the removal material is in contact with both the polishing pad and the chemical mechanical polishing slurry composition.
In yet another aspect, the invention provides a method of a selective chemical mechanical polishing comprising steps of:
a) providing a semiconductor substrate having a surface containing copper metal films; b) providing a polishing pad; c) providing a chemical mechanical polishing slurry composition comprising
1) an abrasive; 2) a chelating agent; 3) a corrosion inhibitor; 4) choline salt as copper removal rate booster and total defect reducer; 5) an organic amine; 6) an oxidizer; 7) biocide; 8) remaining is substantially liquid carrier; wherein pH of the polishing slurry composition is between 5.0 to 8.0;
d) contacting the surface of the semiconductor substrate with the polishing pad and the chemical mechanical polishing slurry composition; and e) polishing the surface of the semiconductor substrate to selectively remove the first material;
wherein at least a portion of the surface containing the first material is in contact with both the polishing pad and the chemical mechanical polishing slurry composition.
The CMP slurry compositions can further comprise a pH buffering agent; surfactant; and a biocide.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 shows Cu removal rates using CMP slurry compositions with or without choline bicarbonate added as the chemical additive.
FIG. 2 shows total defect counts using CMP slurry compositions with or without choline bicarbonate added as the chemical additive.
FIG. 3 shows Cu removal rates using CMP slurry compositions with choline bicarbonate added as the chemical additive at different concentrations.
DETAILED DESCRIPTION OF THE INVENTION
The copper and TSV CMP slurry compositions and methods described herein satisfies the need for tunable, high removal rates, low defects, and good planarization efficiency when used to polish copper films.
The CMP slurry composition disclosed herein comprises colloidal silica particles, high purity and nano-sized abrasives; chemical additives comprising choline salts used as copper film removal rate boosting and defect reducing agent; suitable chelating agents and surface wetting agents; corrosion inhibitors to protect copper film surface from further corrosion; organic amine compounds as copper removal rates boosters; oxidizing agents, and liquid carriers, such as water.
The CMP polishing slurry composition can further comprise pH adjusting agents, surfactants, and biocide.
The pH of the slurry composition is from about 5.0 to about 8; preferably from about 5.5 to 7.5; more preferably 6.5 to 7.
Abrasive particles used for the CMP polishing slurry compositions include, but are not limited to, colloidal silica particles doped by other metal oxide within lattice of the colloidal silica, such as alumina doped silica particles, colloidal aluminum oxide, which include alpha-, beta-, and gamma-, and other types of aluminum oxides, colloidal and photoactive titanium dioxide, cerium oxide, colloidal cerium oxide, nano-sized diamond particles, nano-sized silicon nitride particles, mono-modal, bi-modal, multi-modal colloidal abrasive particles, zirconium oxide, organic polymer-based soft abrasives, surface-coated or modified abrasives, and mixtures thereof. The colloidal silica particles can have narrow or broad particle size distributions, with various sizes and different shapes. The shapes of the abrasives include spherical shape, cocoon shape, aggregate shape and other shapes.
The CMP polishing slurry compositions contain from 0.0 wt % to 25 wt % abrasives; preferably from 0.001 wt % to 1 wt %, and more preferably from 0.0025 wt % to 0.1 wt %.
The suitable chemical additives comprising choline salts in the CMP polishing slurry compositions have a general molecular structure shown below:
Where, anion Y − can be bicarbonate, hydroxide, p-toluenesulfonate, bitartrate, and other suitable anionic counter ions.
The suitable chemical additives comprising choline salts in the CMP polishing slurry compositions include choline bicarbonate, and all other salts formed between choline and other anionic counter ions.
The CMP polishing slurry compositions contain from 0.0001 wt % to 0.50 wt % choline salts; preferably from 0.0010 wt % to 0.10 wt % and more preferably from 0.0025 wt % to 0.050 wt %
The selected and suitable chelating agents include glycine, other amino acids, and amino acid derivatives.
The CMP polishing slurry compositions contain from is from 0.01 wt % to 22 wt % chelating agent; preferably from 0.025 wt % to 20 wt %. The more preferred concentration range of the chelating agent is from 0.05 wt % to 16 wt %.
The selected and suitable corrosion inhibitors used for the CMP polishing slurry compositions include, but are not limited to, triazole and its derivatives, benzene triazole and its derivatives. The triazole derivatives include, but not limited to, amino-substituted triazole compounds, bi-amino-substituted triazole compounds.
The concentration range of the corrosion inhibitor is from 0.001 wt % to 0.15 wt %. The preferred concentration range of the corrosion inhibitor is from 0.0025 wt % to 0.1 wt %. The more preferred concentration range of the corrosion inhibitor is from 0.005 wt % to 0.05 wt %.
Organic amine compounds used to boost copper film removal rates include ethylene diamine, propylene diamine, other organic diamine compounds, and organic amine compounds containing multi amino groups in the same molecular framework.
The CMP polishing slurry compositions contain from 0.0001 wt % to 0.20 wt % amine compounds; preferably from 0.0010 wt % to 0.10 wt % and more preferably from 0.0025 wt % to 0.050 wt %.
Oxidizers used for the CMP polishing slurry compositions include, but are not limited to, periodic acid, hydrogen peroxide, potassium iodate, potassium permanganate, ammonium persulfate, ammonium molybdate, ferric nitrate, nitric acid, potassium nitrate, and mixtures thereof.
The preferred oxidizer is hydrogen peroxide.
The CMP polishing slurry compositions contain from 0.01 wt % to 10 wt % oxidizers; preferably from 0.25 wt % to 4 wt %, and more preferably from 0.5 wt % to 2 wt %.
pH adjusting agents used for the CMP polishing slurry compositions include, but are not limited to, nitric acid, hydrochloric acid, sulfuric acid, phosphoric acid, other inorganic or organic acids, and mixtures thereof.
The preferred pH adjusting agent is nitric acid.
The CMP polishing slurry compositions contain from 0.01 wt % to 0.5 wt % pH adjusting agent; preferably from 0.05 wt % to 0.15 wt %.
In certain embodiments, a surfactant is added to the polishing composition as surface wetting agent. The suitable surfactant compounds that may be added to the polishing composition as surface wetting agent include but are not limited to, for example, any of the numerous nonionic, anionic, cationic or amphoteric surfactants known to those skilled in the art.
The following four types of surfactants can be used as disclosed herein copper CMP slurry as surface wetting agents:
a). non-ionic surface wetting agents, these agents typically are oxygen- or nitrogen-containing compounds with various hydrophobic and hydrophilic moieties in the same molecules, the molecular weight ranges from several hundreds to over 1 million. The viscosities of these materials also possess a very broad distribution.
b). anionic surface wetting agents, these compounds possess the negative net charge on major part of molecular frame, these compound include, but not limited to the following salts with suitable hydrophobic tails, such as alkyl carboxylate, alkyl sulfate, alkyl phosphate, alkyl bicarboxylate, alkyl bisulfate, alkyl biphosphate, such as alkoxy carboxylate, alkoxy sulfate, alkoxy phosphate, alkoxy bicarboxylate, alkoxy bisulfate, alkoxy biphosphate, such as substituted aryl carboxylate, substituted aryl sulfate, substituted aryl phosphate, substituted aryl bicarboxylate, substituted aryl bisulfate, substituted aryl biphosphate etc. The counter ions for this type of surface wetting; agents include, but not limited to the following ions, such as potassium, ammonium and other positive ions. The molecular weights of these anionic surface wetting agents range from several hundred to several hundred-thousands.
c). cationic surface wetting agents, these compounds possess the positive net charge on major part of molecular frame, these compound include, but not limited to, the following salts with suitable hydrophobic tails, such as carboxylate, sulfate, phosphate, bicarboxylate, bisulfate, biphosphate, etc. The counter ions for this type of surface wetting agents include, but not limited to, the following ions, such as potassium, ammonium and other positive ions. The molecular weights of these anionic surface wetting agents range from several hundred to several hundred-thousands.
d). ampholytic surface wetting agents, these compounds possess both of positive and negative charges on the main molecular chains and with their relative counter ions. The examples of such bipolar surface wetting agents include, but not limited to, the salts of amino-carboxylic acids, amino-phosphoric acid, and amino-sulfonic acid.
The CMP polishing slurry compositions contain from 0.00 wt % to 1.0 wt % surfactants; preferably from 0.0001 wt % to 0.25 wt % and more preferably from 0.0005 wt % to 0.10 wt %.
In some embodiments, the surfactant(s) are nonionic, anionic, or mixtures thereof and are present in a concentration ranging about 1 ppm to about 1,000 ppm of the total weight of the slurry.
Biocide used in the CMP polishing slurry compositions is the commercial available Kathon type of biocides.
The CMP polishing slurry compositions contain from 0.0001 wt % to 0.05 wt % biocide; preferably from 0.0001 wt % to 0.025 wt % and more preferably from 0.0002 wt % to 0.01 wt %.
EXPERIMENTAL SECTION
General Experimental Procedure
The associated methods described herein entail use of the aforementioned copper or TSV CMP polishing slurry composition for chemical mechanical planarization of substrates comprised of copper. In the methods, a substrate (e.g., a wafer with copper surface) is placed face-down on a polishing pad which is fixedly attached to a rotatable platen of a CMP polisher. In this manner, the substrate to be polished and planarized is placed in direct contact with the polishing pad. A wafer carrier system or polishing head is used to hold the substrate in place and to apply a downward pressure against the backside of the substrate during CMP processing while the platen and the substrate are rotated. The polishing slurry composition is applied (usually continuously) on the pad during copper CMP processing to effect the removal of material to planarize the substrate.
All percentages are weight percentages unless otherwise indicated. In the examples presented below, CMP experiments were run using the procedures and experimental conditions given below. The CMP tool that was used in the examples is a Mirra®, manufactured by Applied Materials, 3050 Boweres Avenue, Santa Clara, Calif., 95054. An IC-1010 pad or other pad, supplied by Dow Chemicals or Fujibo, was used on the platen for the blanket copper wafer polishing studies. Other polishing pads, supplied by Dow Chemicals or Fujibo were also used on the platen for the blanket copper wafer polishing studies. Pads were broken-in by polishing twenty-five dummy oxide (deposited by plasma enhanced CVD from a TEOS precursor, PETEOS) wafers. In order to qualify the tool settings and the pad break-in, two PETEOS monitors were polished with Syton® OX-K colloidal silica, supplied by Planarization Platform of Air Products Chemicals Inc. at baseline conditions. Polishing experiments were conducted using blanket copper wafer with 15K Angstroms in thickness. These copper blanket wafers were purchased from Silicon Valley Microelectronics, 1150 Campbell Ave, CA, 95126.
Parameters
Å: angstrom(s)—a unit of length
BP: back pressure, in psi units
CMP: chemical mechanical planarization=chemical mechanical polishing
CS: carrier speed
DF: Down force: pressure applied during CMP, units psi
min: minute(s)
ml: milliliter(s)
mV: millivolt(s)
psi: pounds per square inch
PS: platen rotational speed of polishing tool, in rpm (revolution(s) per minute)
SF: polishing slurry composition flow, ml/min
Removal Rates, Defectivity, and Selectivity
Copper RR 2.0 psi Measured copper removal rate at 2.0 psi down pressure of the CMP tool
Copper RR 2.5 psi Measured copper removal rate at 2.0 psi down pressure of the CMP tool and total defects measured by SP2.
Copper RR 3.0 psi Measured copper removal rate at 3.0 psi down pressure of the CMP tool
Ta RR 3.0 psi Measured Ta removal rate at 3.0 psi down pressure of the CMP tool
TaN RR 3.0 psi Measured TaN removal rate at 3.0 psi down pressure of the CMP tool
Ti RR 3.0 psi Measured Ti removal rate at 3.0 psi down pressure of the CMP tool
TiN RR 3.0 psi Measured TiN removal rate at 3.0 psi down pressure of the CMP tool
Si RR 3.0 psi Measured Si removal rate at 3.0 psi down pressure of the CMP tool
Selectivity is calculated of Cu removal rates divided by other film removal rates at 3 psi down force.
Total Defect Counts: Collected on the copper blanket wafers polished by using disclosed herein copper and TSV CMP polishing slurry compositions at 2.5 psi down force.
Working Example
In the working examples, Polishing pad, IC1010 and other polishing pads were used during CMP, supplied by Dow Chemicals or Fujibo.
The high purity and nano-sized colloidal silica particles were prepared from TMOS or TEOS.
Amino acid, glycine, was used as the chelating agent, ethylenediamine was used as copper film removal rate boosting agent, kathon CG was used as biocide, 3-amino-1,2,4-triazole was used as corrosion inhibitor, hydrogen peroxide was used as oxidizing agent; and choline bicarbonate was used as removal rate boosting and defect reducing agent, pH was between 6.5-7.5.
Experiments were conducted using CMP slurry compositions with and without choline bicarbonate as the removal rate boosting and defect reducing agent. The polishing performances were compared.
The removal rates results of using choline bicarbonate in the CMP slurry composition on copper film at three different down forces were listed in Table 1.
As the results shown in Table 1, with the use of choline bicarbonate as the chemical additive in the copper CMP slurry composition, the copper film removal rates were increased by 11 wt % at 2.0 psi down force, 9 wt % at 2.5 psi down force, and about 10 wt % at 3.0 psi down force respectively. In overall, the copper film removal rates were increased by about 10 wt % at different applied down forces. The averaged about 10 wt % increase in copper film removal rate is significant while considering the copper CMP slurry composition being used as reference already afforded very high copper film removal rates.
TABLE 1
Copper CMP Slurries with/or without Choline Bicarbonate as
Additive on Cu Removal Rates
Cu Slurry
Removal Rate
Removal Rate
Removal Rate
composition
(A/min.)
(A/min.)
(A/min.) at
Samples
at 2.0psi
at 2.5psi
3.0psi
Reference Cu Slurry
16563
20676
24340
composition (no
Choline Bicarbonate)
Cu Slurry composition
18386
22540
26741
(with Choline
Bicarbonate as additive)
Removal Rate Change
+11%
+9%
About +10%
Furthermore, it is important to observe the reduction in total defects when choline bicarbonate was used as the chemical additive in the CMP polishing slurry compositions. The results of the impact of using choline bicarbonate as the chemical additive on the total defects were listed in Table 2.
TABLE 2
Total Defects of Copper CMP Slurries with/or without Choline
Bicarbonate as Additive
Cu Slurry composition
Total Defects
Total Defect
Samples
by SP2
Reduction
Reference Cu Slurry
429
—
composition (no Choline
Bicarbonate)
Cu Slurry composition
78
about 550%
(with Choline Bicarbonate
as additive)
As the results shown in Table 2, with the use of choline bicarbonate as the chemical additive in the copper CMP slurry composition, the total defects were reduced from 429 for the reference copper CMP slurry composition without using choline bicarbonate to 78 for the copper CMP slurry composition using choline bicarbonate as the chemical additive. This represents over 5 times more reduction in total defects. As a general matter, it is extremely important to reduce total defects when copper CMP slurry composition is selected and used for polishing copper films in copper CMP or TSV CMP processes.
The impacts of choline bicarbonate as copper film removal rate boosting agent and defect reducing agent were also depicted in FIG. 1 and FIG. 2 respectively.
The impacts of the concentrations of chemical additive, choline bicarbonate, in the copper CMP slurry composition on the copper film removal rates at different down forces were also studied. The results are listed in Table 3 and FIG. 3 respectively.
TABLE 3
Impacts of Choline Bicarbonate Concentrations in Copper CMP
Slurries on Cu Removal Rates.
Removal Rate
Removal Rate
Removal Rate
Cu Slurry composition
(A/min.) at
(A/min.)
(A/min.) at
Samples
2.0psi
at 2.5psi
3.0psi
Reference Cu Slurry
18184
21467
26677
composition (no Choline
Bicarbonate)
Cu Slurry composition
18025
22692
27320
(with 1X Choline
Bicarbonate as additive)
Cu Slurry composition
18823
23624
28549
(with 10X Choline
Bicarbonate as additive)
Cu Slurry composition
19071
21432
25988
(with 20X Choline
Bicarbonate as additive)
Removal Rate Change
Up to
Up to
About
+4.9%
+10%
+7%
As the results shown in Table 3, in general, copper film removal rates were increased more at 10× concentrated bicarbonate than the concentrations at 1× or 20×, respectively.
At 10× concentrated Choline Bicarbonate concentration, the copper film removal rate increased % seems higher than that at 20× concentrated Choline Bicarbonate concentration. This might be attributed to the fact 10× concentration of choline bicarbonate as additive in the disclosed Cu CMP slurry here afforded the optimized removal rate boosting effect than the 20× concentration of choline bicarbonate.
The polishing selectivity for copper and other materials such as Ta, TaN, Ti, TiN and Si have also been measured. The selectivity results were listed in Table 4, when 3 psi down force was used for polishing. The ratio of the removal rate of copper to the removal rate of dielectric base is called the “selectivity” for removal of copper in relation to dielectric during CMP processing of substrates comprised of titanium, titanium nitride, tantalum, tantalum nitride, and silicon.
TABLE 4
Selective of Cu vs. Other Films
Cu:Ta
Cu:TaN
Cu:Ti
Cu:TiN
Cu:Si
1250
5000
1389
397
253
As the data showed in Table 4, very high selectivity (>1000) was achieved for Cu:Ta, Cu:TaN, and Cu:Ti, and also reasonable high selectivity was achieved for Cu:TiN and Cu:Si (>250). This high selectivity for polishing copper relative to the other materials is highly desirable for many applications, such as, TSV applications, that demands high copper film removal rates.
While at least one exemplary embodiment has been presented in the foregoing detailed description of the invention, it should be appreciated that a vast number of variations exist. It should also be appreciated that the exemplary embodiment or exemplary embodiments are only examples, and are not intended to limit the scope, applicability, or configuration of the invention in any way. Rather, the foregoing detailed description will provide those skilled in the art with a convenient road map for implementing an exemplary embodiment of the invention, it being understood that various changes may be made in the function and arrangement of elements described in an exemplary embodiment without departing from the scope of the invention as set forth in the appended claims.
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Provided are novel chemical mechanical polishing (CMP) slurry compositions for polishing copper substrates and method of using the CMP compositions. The CMP slurry compositions deliver superior planarization with high and tunable removal rates and low defects when polishing bulk copper layers of the nanostructures of IC chips. The CMP slurry compositions also offer the high selectivity for polishing copper relative to the other materials (such as Ti, TiN, Ta, TaN, and Si), suitable for through-silicon via (TSV) CMP process which demands high copper film removal rates.
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BACKGROUND OF THE NEW VARIETY
The present invention relates to a new, novel and distinct variety of hop ‘Humulus lupulus L’ and which has been denominated varietally, hereinafter, as ‘Summit’.
ORIGIN
Hops are grown commercially and are principally used in the brewing industry to add bitterness and flavor to beverages such as beer. Lupulin glands found inside female hop cones provide the resins and essential oils which are the primary component of the hop flavor which is imparted to such beverages.
New hop varieties are typically evaluated for their growing characteristics, hop cone yields, disease resistance, and the chemical composition of the resins and essential oils contained within the hop cone glands. As should be understood, only female hop plants produce cones containing the lupulin glands, and thus only female hop plants have any significant commercial value.
The present hop plant was derived from a multitude of hop plants resulting from a controlled cross-pollination which was conducted during the summer of 2000. The aforementioned cross-pollination was performed between a non-patented, female hop plant owned by the inventor, and commonly referred to as ‘Lexus’; with a non-patented, male hop plant. The female parent ‘Lexus’ had previously been derived from a controlled cross-pollination which was conducted during the summer of 1999. In this regard, the female parent ‘Lexus’ was derived from a cross-pollination conducted between the female hop plant ‘Zeus’ which is commercially available, and non-patented; and a non-patented male hop plant designated as USDA 19058 m. The male parent had resulted from an earlier controlled cross-pollination conducted during the summer of 1999 between the female hop plant ‘Zeus’, first mentioned, above; and a non-patented male hop plant which is named ‘(Nugget X open) m ’ and which was owned by the inventor. This same male hop plant was earlier selected from a number of seedlings arising from the seeds which were collected from the Nugget hop cones. The Nugget hop cones had been pollinated and originated from a commercial hop field which is located near Harrah, Wash.
The controlled cross-pollination program resulting in the creation of the new hop variety of the present application was performed during the 2000 growing season by the inventor at his personal residence which is located in Yakima, Wash. The inventor discovered the new variety of hop during the 2001 growing season among the numerous hop plants then growing at his residence, and which had been germinated from seeds resulting from the above described controlled cross-pollination program. The seeds from the cross-pollination first referenced, above, were planted in the inventor's greenhouse during January, 2001. Thereafter, the most vigorous plants resulting from the aforementioned cross-pollination were selected and planted by the inventor in his experimental hop field which is located in Yakima, Wash. These plants were grown on twine attached to a 10 foot high trellis during the 2001 and 2002 growing seasons.
Subsequent chemical analysis and field observations made in 2002 and thereafter revealed the new hop plant ‘Summit’ had an unusually high percentage of alpha acids; short internode lengths which indicated a semi-dwarf characteristic; a lack of powdery mildew; and a reasonably projected per acre cone yield when grown on a low trellis. During the 2003 growing season, the ‘Summit’ hop plant was grown in two geographically different locations with no powdery mildew observed. Further, the production of alpha-acids were quite high as calculated at both locations. The plants growing at the two different geographical locations constituted the first asexual reproduction of the present variety. Based upon the field observations performed, and the chemical and analytical data collected during testing and evaluation of the variety during the 2002-2005 growing seasons, it appears that the second and third generation ‘Summit’ hop plants demonstrate genetic stability with respect to the new variety's novel characteristics of unusually high alpha-acids yields; very high alpha/beta ratios; excellent storage stability of alpha acids; and powdery mildew resistance.
In relative comparison to the unpatented commercially available ‘Zeus’ variety, the present variety ‘Summit’ is considered to be a semi-dwarf which makes it a better prospect for growth on low trellis arrangements. Further, the variety ‘Summit’ is resistant to the powdery mildew strains found in the Yakima Valley, and has much better storage stability of alpha acids and has a higher alpha/beta acid ratio in comparison to the variety ‘Zeus.’
BRIEF DESCRIPTION OF THE DRAWINGS
The accompanying drawings which are provided are color photographs of the present variety.
FIG. 1 shows several whole cones of the present variety.
FIG. 2 depicts a mature vine leaf of the present variety.
FIG. 3 depicts the growing characteristics of the present variety when grown on a low trellis (approximately 10 ft.).
The colors are as nearly true as is reasonably possible in color representations of this type. Due to chemical development and processing and printing, the leaves, and cones depicted in these photographs may or may not be accurate when compared to the actual specimen. For this reason, future color references should be made to the color plates (Royal Horticultural Society), and descriptions provided hereinafter.
DETAILED DESCRIPTION
Referring more specifically to the details of this new and distinct variety of hop plant, the following has been observed under the ecological conditions prevailing near Moxee, Wash. All major color code designations are by reference to the R.H.S. Colour Chart, 4 th Edition provided by The Royal Horticultural Society of Great Britain.
PLANT
Generally.— Considered semi-dwarf, and maintaining a height of approximately 14 to 16 feet. The present variety is a perennial producing annual climbing bines and a perennial crown. The present variety does not self-pollinate.
Bines.— Growth characteristic — Bines of the present variety climb in a clockwise direction with the aid of tricomes.
Bine.— Color — Green, (RHS 146C). The color of the bine is not distinctive of the present variety. Further, six light brownish purple stripes typically appear on the bine.
Bine.— Thickness — The bine of a mature hop plant may have a dimension of about ⅜ to about ½ of an inch in thickness when measured at a distance of approximately 6 feet above ground level.
Laterals.— Position — Considered caulous and substantially evenly spaced along the main bine. Laterals of the present variety grow from auxiliary buds at each node along the main bine.
Laterals.— Growth Habit — Generally speaking, Laterals grow from auxiliary buds at each node along the main bine. Inflorescences develop from axils of the Laterals. Each inflorescence becomes a hop cone at maturity.
Laterals.— Length — Considered shorter than most commercial varieties. The typical lateral length ranges from about 18 to about 30 inches.
Internodes.— Length — The present variety has internode lengths of approximately 1½ to about 4 inches. Typically, laterals will have approximately 6 to about 8 internodes each.
Stems. — Generally — The annual stems of the present variety grow from the crown and rhizomes of the plant in early Spring and twine around suitable supports.
Dormancy.— Generally — The present hop variety emerges from dormancy approximately one week later than the commercial variety ‘Zeus’ (unpatented); and approximately one week earlier than the variety ‘Galena’ (unpatented) at the same geographical location. In this regard, the commercial variety ‘Zeus’ (unpatented) emerges approximately the third or fourth week of March at the same geographical location in Washington, while ‘Galena’ does not emerge until the first week of April.
Shoot growth rate.— Generally — Considered average when compared against other common commercial varieties. The present variety, however, is slower than the hop variety ‘Nugget’ (unpatented) at the same geographical location.
Vine stems.— Shape — Generally considered to be hexagonal.
Vine stems.— Color — Green with the corners of the hexagonal shaped vine having a light purplish brown stripe similar to the commercial variety ‘Zeus’ (unpatented). This color, however, appears less pronounced. This purplish brown color is not particularly distinctive of the present variety.
Stems.— Growth — Average, as compared to other commercial varieties.
Stems.— Size — Typically about ⅜ inch in diameter when measured approximately 6 feet above ground level.
Cultural measures.— Generally — The present variety is considered to be a low trellis vine which self-trains, that is, the vines are allowed to grasp support strings to begin upward growth. The present variety, as a general matter, can reach the top of a low trellis in approximately 4 weeks after self-training which typically occurs in late May. In the event that the variety is grown on a conventional high trellis, early May training may be required. Low trellis heights stand typically at approximately 10 feet and normal trellis heights are typically about 18 feet.
Stipule growth direction.— Generally — Considered to be downward.
Plant shape.— Generally — Columnar on low trellis arrangements. Fusiform when grown on high trellis arrangements.
LEAVES
Leaves.— Generally — The leaves of the ‘Summit’ variety are borne in pairs at each node on the main bine.
Leaves.— Position — Considered opposite.
Stipules.— Location — Typically at the petiole base of each leaf.
Stipules.— Arrangement — Considered interpetiolar.
Leaves.— Size — Considered average as compared to other common varieties.
Leaf.— Width — Approximately 6-7 inches in width.
Leaf. — Shape — Cordate and having 3-5 palmate lobes and further having palmate venation.
Leaf margin. — Shape — Slightly serrated, and moderately dentate.
Sinus-Clefts.— Shape — Considered moderately cut.
Leaf color.— Upper surface — Dark Green (RHS 137A).
Leaf color.— Lower surface — Lighter Green (RHS 137C).
Leaf petiole. — Color — Green (RHS 146C).
Leaf petiole.— Color — Upper surface only — Green (RHS 146C). This green coloration is distinctly different from that of the ‘Zeus’ hop plant (unpatented) which displays a purple shading on the upper side of the petiole.
Leaf petiole.— Position — Extends from the main bine at approximately 90 degree angle and is slightly reflexed.
Petioles.— Shape — Slightly channeled and having a flat surface on the upper surface.
Leaves.— Upper surface texture — Rough. As a general matter, stiff fine hairs appear on the upper surface of the leaf. This creates a dull appearance and a rough texture.
Surface characteristics.— Lower surface of leaf — Many disc-shaped yellowish resin glands appear on the lower surface.
CONES
Generally. — Inflorescences of the present variety ‘Summit’ begin to appear on the bines in early July and mature during the second to third week of September under the ecological conditions prevailing in Central Washington. As the respective inflorescences mature, they form a cone-like structure or strobile and which is best seen in FIG. 1 .
Form.— the present variety develops inflorescence on a cranked axis and typically in even pairs, or clusters. The cones on the present variety develop on laterals from the top of the plant to a location approximately 24 inches above ground level.
Strig.— Generally — Considered compact with a model diameter.
Aroma.— Generally — Considered moderate, but pleasant.
Cone length.— Approximately 1.25 to about 1.40 inches when grown under the ecological conditions prevailing in Central Washington.
Cone tip.— Shape — Bluntly pointed.
Cone shape.— Ovoid in shape.
Compactness.— Considered tight and semi-dense for the present variety.
Bract tip.— Shape — Considered cuspidate.
Bracteole.— Shape — Considered acute to deltoid.
Central rachis.— Form — Compact, but not considered as thick as compared to the strig of the common commercial variety ‘Zeus’ (unpatented).
Lupulin glands.— Numbers — The cone of the present variety contains numerous lupulin glands. In this regard, it should be understood that average numbers of glands are usually impossible to quantify. The numbers of lupulin glands will vary from year to year based upon the weather and a multitude of other environmental and cultural factors. Further, it should be understood that there are a large number of individual glands in each cone, and significant variations between cones on the same plant. Generally speaking, it is clear that the present variety has numerous glands because it is characterized as a high alpha variety.
Date of maturity.— considered to be middle to late as compared to other common hop varieties grown in Central Washington.
Cone shape.— Uniformity — Considered uniform.
Harvestability.— Generally — The hop cones of the present variety ‘Summit’ are well adapted for mechanical harvesting because of their compactness and ovoid shape. The cones of the present variety are not shattered during harvest.
Lupulin glands. — Shape — Considered globular and having a golden yellow color (RHS 2A) which is not particularly distinctive of the present variety. This color is somewhat variable based upon environmental, and other cultural practices.
Bract tip position.— Considered appressed, however some bracts are slightly everted at full maturity.
Yield per acre.— Approximately 2,000 to about 2,300 pounds on average. However, this yield is contingent upon temperature, soil conditions and cultural practices and is therefore not distinctive of the present variety.
Cone bracteole.— Color — Green (RHS 145A).
Cone bract.— Color — Green (RHS 145C).
ANALYTICAL DATA OF THE CONES
Generally.— The analytical data as provided hereinafter of the cones have been gathered from cones having a cone moisture of approximately 8%.
Percentage of alpha-acids as calculated in a base.— About 18-19% as determined by the ASBC Spectrophotometric method.
Percentage of beta-acids as calculated in a bale.— Approximately 3.3-4.3% as calculated by the ASBC Spectrophotometric method.
Alpha/beta acid ratio.— About 5.0 to about 6.0.
Cohumulone (% of alpha - acids).—About 32.5%.
Colupulone (% of beta - acids).—Approximately 54%.
Storage characteristics.— The cones of the present variety experience a 12% transformation of alpha acids after about 6 months of storage at 22° C. In relative comparison to other common varieties, this rate of transformation is less than the best storing high alpha acid commercial varieties such as ‘Galena’ and ‘Nugget’ (both unpatented).
Total oil content.— About 1.5 milliliters per 100 grams.
Humulene (% of total oils ).—Approximately 15%.
Caryophyllene (% of total oils ).—Approximately 10%.
Humulene/caryophyllene ratio.— Approximately 1.5.
Farnesene (% of total oils ).—0.
Myrcene (% of total oils ).—Approximately 485.
Lupulin (% of total cone weight ).—Approximately 30%.
Ploidy. — The genetic make up of ‘Summit’ is diploid. In this regard, the mother is diploid and the father is diploid.
Disease resistance. — The variety ‘Summit’ appears to be moderately susceptible to hop downy mildew fungus. ‘Summit’ appears to be resistant to the strains of powdery mildew fungus typically found in the Yakima Valley of Central Washington. ‘Summit’ also appears tolerant to strains of Verticillium Wilt and other virus diseases found in U.S. growing areas. This variety also appears tolerant to the major soil borne pests that affect hops including Phytophthora root rot.
Regional adaptation. — The ‘Summit’ variety of hop appears to be adapted to the drier growing regions of Washington State, especially the Yakima Valley of Central Washington.
Life expectancy. — Unknown.
Although the new variety of hop possesses the desired characteristics when grown under the ecological conditions prevailing in the Yakima Valley of Central Washington, it should be understood that variations of the usual magnitude and characteristics incident to changing and growing conditions, fertilization, pruning, pest control and horticultural management are to be expected.
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A new variety of hop is described and which is characterized principally as to novelty by being semi-dwarf in stature; and which further produces cones having a high percentage of alpha-acids, high alpha/beta ratio and excellent storage stability of alpha-acids.
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FIELD OF THE INVENTION
[0001] The invention relates in general to image printing, and more specifically to a device for concentrating ink jet ink and removing excess fluid prior to imparting the ink onto a receiver member.
BACKGROUND OF THE INVENTION
[0002] Ink jet technology has become a technology of choice for printing documents and other digitally produced images on receiver members (e.g., paper and other media). In the ink jet process, described in more detail in Ink Jet Technology and Product Development Strategies by Stephen F. Ponds, and published by Torrey Pines Research in 2000, ink is jetted from an ink jet head that includes one or more ink jet nozzles onto a receiver member.
[0003] Contrasting with ink jet technology are other printing technologies, such as electrophotography and lithography. Lithography relies on the use of highly viscous inks in which pigment particles are dispersed with relatively small amounts of a fluid such as oil. Typically, the concentration of solids may exceed 90% by weight. The relatively small amount of solvent present in a lithographic print can be readily absorbed by the receiver member or treated using other suitable methods such as drying by heat, cross-linking, or overcoating with varnish.
[0004] Another advantage of the high viscosity inks used in lithography, is that the viscosity of the ink limits the ability of the ink to spread. Specifically, ink images often consist of sharp lines of demarcation, such as occur with alphanumeric symbols, halftone dots, edges of printed areas, etc. With high viscosity inks, the tendency of the ink to spread is minimized. This allows images on printed pages to have sharp edges and high resolution. It also reduces the tendency of ink to soak into relatively porous receiver members such as those that do not have a coating such as a clay overcoat. Examples of such receiver members include laser bond papers. If low viscosity ink soaks into the paper, paper fibers can show through. This limits the density of the printed image. Yet another advantage obtained with high viscosity inks is the minimization of halftone dot spread. This allows good gray scales to be produced and, for color images, allows images having a wide color gamut to be printed.
[0005] Yet another advantage of high viscosity inks such as those used in lithography is that such inks allow images to be printed on glossy papers such as those having a clay coating or polymer overcoat. Low viscosity inks tend to spread or run on these papers, adversely affecting various image quality parameters such as edge sharpness, resolution, and halftone dot integrity, and color balance.
[0006] U.S. Pat. No. 5,854,960 discloses a liquid electrophotographic engine having an inking roller, a squeegee to concentrate the liquid ink, and a photoreceptive member. In such apparatus, liquid electrophotographic ink is applied to an inking roller. The ink is then concentrated using the squeegee, preferably a squeegee in the form of a foam roller. This roller absorbs the clear solvent, leaving the marking particles in a concentrated ink. An electrostatic latent image is then formed on the photoreceptor and the latent image developed into a visible image by bringing the latent image bearing photoreceptor into contact with the concentrated ink bearing inking roller. The marking particles are then electrostatically attracted to the latent image sites on the photoreceptor. It should be noted that, during the ink concentration phase of this process, there is no image information in the ink so that image degradation during the concentration phase cannot occur.
[0007] U.S. Pat. No. 6,363,234 discloses a mechanism to concentrate liquid electrophotographic developer including a source of a gas that flows onto a surface containing a liquid developer image and a chamber adjacent to the source and the surface that receives the mixture.
[0008] Co-pending U.S. patent application Ser. No. ______ discloses a digital printing press capable of producing prints at a high speed and high volume that utilizes ink jet technology, rather than an electrophotographic process, for applying the ink. In this type of apparatus, there is no electrostatic latent image formed on a photoreceptive or primary imaging member. In fact, there is no photoreceptive element and there is no electrostatic charge to attract marking particles to specific sites on the primary imaging member. Rather, small ink droplets, often with volumes as little as a few picoliters, are jetted or otherwise deposited strictly where a portion of the image is to be constructed.
[0009] As discussed in co-pending U.S. patent application Ser. No. ______, the aforementioned problems associated with the dilute inks used in ink jet printing apparatus can be eliminated by first imaging by jetting the ink onto a primary imaging member, then concentrating the ink, and then transferring the concentrated ink to the receiver sheet such as paper. Alternatively, the concentrated ink can be transferred to a transfer intermediate member and then transferred from the transfer intermediate member to the receiver member.
SUMMARY OF THE INVENTION
[0010] In view of the above, this invention is directed to an apparatus for concentrating jetted ink including a fractionating device that fractionates the ink into a concentrated ink layer and a dilute, mainly clear, solvent layer. This invention also discloses an ink composition suitable for use with such a concentration apparatus. The present invention seeks to eliminate excess solvent from an image produced on a primary imaging or other suitable member such as a transfer intermediate member with an ink jet printer by fractionating the ink into a colorant-rich segment and a solvent-rich segment. The solvent-rich segment of the ink is then removed from the aforementioned member and the image then transferred from the aforementioned member to a secondary member, preferably a receiver member such as paper.
[0011] Fractionation into two phases is achieved by the application of an electrostatic force. The ink image, which is on an electrically conducting substrate, is passed through a nip formed by the substrate and a fractionating member, with a difference of potential established between the fractionating member and the substrate that drives the electrically charged marking particles to the substrate. The fractionated solvent is then skived from the substrate, leaving behind the image formed by the concentrated developer.
[0012] That is to say, according to this invention, in an apparatus for printing images on a moving primary imaging member by jetting ink, containing a fluid and marking particles, in an image-wise fashion onto the primary imaging member, a device for concentrating the ink prior to transferring a marking particle image to a receiver member. The ink concentrating device includes a fractionating unit for separating fluid of the ink from the marking particles. The fractionating unit is located a predetermined spaced distance from the primary image bearing member. An electrostatic field is established between the primary image bearing member and the fractionating unit for concentrating the marking particles in the liquid of the ink.
[0013] Another aspect of this invention is the use of a jetable ink having an electrical resistivity in excess of 10 10 Ω-cm and including marking particles.
[0014] The invention, and its objects and advantages, will become more apparent in the detailed description of the preferred embodiment presented below.
BRIEF DESCRIPTION OF THE DRAWINGS
[0015] In the detailed description of the preferred embodiment of the invention presented below, reference is made to the accompanying drawings, in which:
[0016] FIG. 1 is a side elevation view of the fractionating apparatus, according to this invention; and
[0017] FIG. 2 is a front elevation view of the fractionating apparatus, according to this invention.
DETAILED DESCRIPTION OF THE INVENTION
[0018] A printed image is formed using an ink having electrically charged marking particles. Although ink such as typical ink jet inks including pigment particles can be used (so long as the other physical requirements of the inks as described in this disclosure are met), it is preferable that the ink includes polymeric particles. Although clear polymeric particles can be used if desired, it is generally preferable to use polymeric particles having a dye, pigment, or other colorant. In this disclosure, the term “marking particles” shall include polymeric particles whether or not they include a colorant.
[0019] The ink is deposited in an image-wise fashion using appropriate ink jet deposition methods such as a continuous ink jet stream, or drop-on-demand technology onto an electrically conducting substrate. In the preferred mode of operations the substrate is electrically grounded, although it can be electrically biased if so desired. The image is then passed through a nip formed by the image-bearing substrate and a fractionating device. A potential difference is established between the fractionating device and the image bearing substrate. This is preferably done by electrically grounding the substrate and establishing a bias on the fractionating device that would drive the charged marking particles towards the substrate and the supernatant fluid comprising counter ions towards the fractionating device. Although the voltage is not critical, it is preferred that the difference of potential between the fractionating device and the substrate be between 100 and 1,000 volts, preferably between 100 and 500 volts and more preferably between 150 and 350 volts. Lower voltages may not be sufficiently strong to drive the marking particles towards the substrate within the nip residence times. Higher voltages are limited by arcing within the nip and possible by reversing the charge on the marking particles. Such charge reversal would preclude the ability to subsequently transfer the particles. After fractionating, the image is transferred from the primary imaging member to a secondary imaging member. The secondary imaging member could be an intermediate member, a receiver such as paper or transparency stock, etc. Although any appropriate means of transfer to the secondary imaging member could be employed, it is preferred that transfer be accomplished by applying an electrostatic bias of sufficient magnitude and polarity to urge the marking particles to the secondary imaging member. When the secondary imaging member is an intermediate imaging member, transfer to the receiver can, again, be accomplished using suitable transfer technology such as the application of pressure or heat and pressure or any other suitable means. However, it is preferable to transfer the image by applying an electrostatic field of such magnitude and polarity to urge the marking particles away from the secondary imaging member to the receiver. Methods of electrostatic transfer are known in the electrophotographic literature and comprise using a biased roller that presses the receiver against the imaging member, the use of a corona, etc. It should be noted that fractionation can be done, using this same technology, on an intermediate member rather than the primary imaging member. It is not, however, desirable to attempt to fractionate from the final receiver as the receiver may absorb the solvent or a sizable fraction thereof. Moreover, the presence of the relatively dilute, thereby low viscosity, ink can run on the receiver, thereby reducing image quality.
[0020] The nip formed between the fractionator and the imaging member should have a spacing of less than 250 μm, preferably less than 50 μm and more preferably less than 25 μm. In some embodiments of this invention, it is possible for the fractionator to be in physical contact with the image-bearing primary imaging member and form a nip with a finite nip width.
[0021] As an example, a fractionator can include a wedge-shaped metallic member in which the vertex of the wedge is held in close proximity to the primary imaging member. The fractionator is electrically biased as discussed above in this disclosure and the primary imaging member is grounded. The marking particles are driven towards the primary imaging member, leaving a layer of supernatant solvent that can then be skived off by the wedge.
[0022] Referring to the accompanying drawings, the preferred embodiment of the fractionator is shown in FIGS. 1 and 2 . In this embodiment, the fractionation roller 10 is physically and electrically separated from a metallic substrate by a pair of electrically insulating spacing wheels 20 . The spacing wheels are made of an insulating polymer such as delrin or nylon and are pressed onto wheel bearings 51 and 52 . The support bearings 50 and 53 are concentrically located on an axle shaft (not shown) with wheel bearings 51 and 52 and hold the roller 10 to front bracket 110 and rear bracket 111 . Wheel bearings 51 and 52 allow the spacing wheels 20 to rotate on the axle independently of the fractionation roller 10 . This allows the fractionation roller to rotate in a direction and at a speed that are different from the speed and direction of the imaging member upon which fractionation is occurring. The fractionation roller is belt driven by drive motor 100 through drive roller pulleys operating through drive roller pulleys 90 and 91 . In order to electrically bias the fractionation roller 10 , electrical contact is made to the axle shaft by means of a carbon brush 60 that is held in place by the carbon brush bracket 61 . The roller apparatus and motor drive mechanism is mounted via front bracket 110 , rear bracket 111 , and two bottom brackets 120 . The distance between the fractionation roller 10 and the imaging member is determined by pushing the fractionation roller towards the imaging member until the spacing wheels 20 contact the imaging member. This is done by allowing the front bracket 110 and rear bracket 111 to pivot on pivoting shaft 70 , with a force applied to the two brackets by a spring 130 . Travel of the brackets is limited by the travel limiter 140 . The space between the front and rear brackets and the bottom bracket is adjusted by spacers 80 in order to accommodate various fractionation roller lengths.
[0023] It is further preferred that the fractionator includes a squeegee blade to remove the supernatant liquid from the fractionating roller 10 . This blade is preferably made of an elastomeric polymer that is not plasticized by the solvent. The squeegee blade 30 is mounted so as to be in contact with the fractionating roller after fractionation has occurred. The supernatant fluid is then allowed to drain into a drip tray 40 , where it can be recycled or discarded.
[0024] In another embodiment of this invention, the imaging member on which fractionation occurs comprises a semiconducting polymer such as an elastomer such as polyurethane. Such materials are similar to those often used in transfer rollers in electrophotographic engines. However, in this instance, the polymer cannot be plasticizable or significantly swellable by the ink solvent. Materials such as these typically comprise a charge-conducting agent and typically have resistivities between 10 6 and 10 11 Ω-cm.
[0025] In yet another embodiment of this invention, the fractionator can have a compliant, electrically conducting blade or roller in contact with the imaging surface on which fractionation occurs. Suitable materials include elastomeric materials such as polyurethane or silicone rubber or foams made from such materials. Such fractionating members should also comprise sufficient charge conducting agent so as to result in the fractionating member having a resistivity less than 10 11 Ω-cm and preferably less than 10 6 Ω-cm.
[0026] For fractionation to occur, it is important that the ink possess certain physical properties. These properties are often significantly different from inks commonly used in ink jet printers that do not require electrostatic fractionation. The ink must be sufficiently electrically resistive so as to support an electric-field. The resistivity of the ink is determined by measuring the current generated by an alternating voltage (AC) having a frequency of 1 kHz. The resistance is the ratio of the root-mean-square (RMS) of the applied voltage (approximately 0.707 times the amplitude of the applied AC voltage for a voltage that is varying sinusoidally with time) to the current. The resistance is the product of the resistivity times the separation distance between the electrodes containing the ink divided by the area of the electrode. It is recognized that, for high resistance materials, it is often desirable to surround the biased or active part of the electrode with conductive material that is used to form a grounded or guard ring around the active part of the electrode in order to reduce noise. For the presently described fractionator to work, the AC electrical resistivity of the ink should be greater than 10 9 Ω-cm and preferably greater than 10 10 Ω-cm. This precludes the use of aqueous based ink jet inks and most alcohol based ink jet inks as their resistivities are typically less than 10 7 Ω-cm. Rather, the ink should comprise a dispersing liquid such as mineral oils such as Isopar L or Isopar G, both sold by Exxon Corporation, silicone oil, high molecular weight alcohols, etc. While certain alkanes and other aliphatic and aromatic hydrocarbons may be suitable, their associated flammabilities and the potential health risks make them less than fully desirable. For purposes of this disclosure, the AC resistivity was determined using an AC signal with an amplitude of 0.75 VAC, at a frequency of 1 kHz. 0.4 ml of the ink was placed into a cell using a pipette. The electrode spacing between electrodes was 10 μm and the active diameter of the electrodes was 1.3 cm. A guard ring surrounded one of the electrodes.
[0027] DC resistivity was determined using the same cell, but applying a DC voltage with a magnitude of 100 V. For fractionation and transfer to occur, the resistivity of the supernatant fluid should be sufficiently high so as not to short the field in either the fractionator or transfer station. This requires that the DC resistivity be in excess of 10 9 Ω-cm. This high resistivity precludes the use of aqueous and many alcohol based conventional ink jet inks in this process.
[0028] The ink should also comprise electrically charged marking particles. While the exact magnitude of the charge is not critical, it should be sufficiently large as to preclude flocculation of the marking particles and enable the particles to fractionate and transfer within the time allowed by the specific engine. Moreover, it is important that the vast majority of the particles have the same charge polarity to enable fractionation and transfer to occur and to prevent flocculation. The charge and charge sign can be determined using known techniques. The marking particles can comprise a colorant, which can be either a dye or a pigment. The marking particles can also comprise a polymeric binder such as polyester, polystyrene, polystyrene butyl acrylate, etc. Alternatively, the marking particles can comprise free pigment particles provided the pigment particles meet the size and charge criteria discussed in this disclosure. However, common ink jet inks that comprise dye would not be suitable as the dye is in solution and, accordingly, could be neither fractionated nor transferred in the manner disclosed herein. The particles need to be sufficiently small so as to be jetable from an ink jet head. This limits their average diameter to less than approximately 3 μm. Conversely, it would be difficult to control the motion of the particles, even in the presence of an electrostatic field, if the average particle diameter was less than approximately 0.1. Smaller particles would be subject to random motion such as that induced by Brownian motion. Particle diameters can be determined by known techniques including laser scattering, transmission electron microscopy, and scanning electron microscopy. In the preferred embodiment, the marking particles would comprise a polymeric binder. The marking particles can be colorless if desired.
[0029] The viscosity of the ink is also important, as it must be jetable. It is preferable that the viscosity be less than 20 centipoise, preferably less than 10 centipoise, and even more preferably less than 5 centipoise. The viscosity in the cited examples was measured using a Brookfield viscometer model number DV-E. The spindle model number was 00. The spindle rotated at 100 rpm. In general this viscometer model and spindle model could be used, however, depending on the viscosity the spindle would be rotated between 20 and 100 rpm. Alternatively, the viscosity could be measured with a Brookfield model LV viscometer with a UL adaptor at approximately 12 rpm.
EXAMPLES
Example 1
[0030] Commercially available ink sold as cyan colored Signature by Kodak, diluted with Isopar L, was used for this experiment. The marking particles in this ink are approximately 0.1 μm in diameter, as determined using transmission electron microscopy. The AC resistivity measured at 1 kHz with an applied voltage with an amplitude of 0.75 volts, was approximately 1.46×10 11 Ω-cm. The viscosity was 1.75 cPoise. The ink was jetted onto a primary imaging member comprising nickelized polyethylene terephthalate on an aluminum support. The primary imaging member was approximately 12.5 cm wide by 20 cm long. The nickel layer was electrically grounded. The roller fractionator that was described as the preferred embodiment of this invention was used in this experiment. As the Signature marking particles are charged, the roller was biased at +300 volts to drive the marking particles towards the primary imaging member. The spacer wheels used on the fractionator established a gap of approximately 40 μm. The fractionating roller was rotated at approximately 10.5 to 11 rpm counter to the direction of movement of the primary imaging member.
[0031] The ink was jetted onto the entire primary imaging member. It was then driven over the fractionator. After fractionation, the image was transferred to a clay-coated paper (Sappi Lustro Laser) that had been wrapped around a polyurethane transfer roller similar to those used in electrophotographic printing engines. The paper was chosen because it is nonporous and represents a very stressful receiver for conventional ink jet engines. Transfer was accomplished by biasing the roller at −1,000 volts to attract the marking particles to the receiver. It should be noted that it is well known that it is extremely difficult to electrostatically transfer dry toner particles having the same size as the marking particles used in this ink in electrophotographic engines.
[0032] During the fractionation process, clear supernatant liquid was observed to flow over the roller. Immediately after transfer, it was found that the image on the receiver was dry and virtually all of the marking particles transferred from the primary imaging member to the receiver. The image was also permanently fixed after transfer without having to use any external means of fixing the image such as fusing. These are surprising results.
[0033] In order to quantify how much solvent was present on the receiver after transfer, the image-bearing receiver was placed in a microbalance and its initial mass tared out. Upon evaporation of solvent, the receiver should become lighter. No solvent loss was found, to 0.1 mg, which was the limit of the balance, over a 24 hour period. This confirms that the marking particles were predominantly dry after fractionation.
Example 2
[0034] This example is similar to example 1 except that no bias was applied to the fractionator. In addition, no quantitative measurements of solvent evaporation were made. In this case there was a lot of solvent visible on the paper after transfer. Moreover, a large fraction of the marking particles were skived off the primary imaging member by the fractionator. This result shows the importance of the electrical bias applied to the fractionator.
Example 3
[0035] This example is similar to example 1 except that the polarity of the bias applied to the fractionator was reversed so as to attract the marking particles to, the fractionator. In this example, there were few marking particles transferred to the receiver, as most were removed from the primary imaging member by the fractionator. Solvent was visible on the receiver after transfer.
Example 4
[0036] This example is similar to example 1 except that the design of the fractionator was altered. In this case, the fractionator has an aluminum member, approximately semicircular in shape. This device was attached to the frame of the breadboard that also comprised the track on which the primary imaging member traveled. The trailing edge of this member, referenced to the direction of travel of the primary imaging member, was positioned so that there was a space between the fractionator and primary imaging member of approximately 40 μm at the leading edge of the primary imaging member. However, as the fractionator was fixed to the breadboard and its separation was not indexed to the primary imaging member, the space between the fractionator and primary imaging member varied between 40 μm and 75 μm. In this case, fractionation occurred, as was evidenced by the clear supernatant liquid on the fractionator after the fractionation process. However, the ink on the primary imaging member, although concentrated, was not concentrated to the point at which the transferred image was dry. Rather, some solvent was clearly visible on the transferred image. This example shows that, although the fractionator described in this example is within the specifications of this patent and does function, it is not the preferred mode.
[0037] The invention has been described in detail with particular reference to certain preferred embodiments thereof, but it will be understood that variations and modifications can be effected within the spirit and scope of the invention.
Parts List
[0000]
10 Fractionation Roller
20 Spacing Wheel
30 Squeegee Blade
40 Drip Tray
50 Support Bearings
51 Wheel Bearing
52 Wheel Bearing
53 Support Bearing
60 Carbon Brush
61 Carbon Brush Bracket
70 Pivot Shaft
80 Spacer
90 Roller Drive Pulley
91 Motor Drive Pulley
100 Drive Motor
110 Front Bracket
111 Rear Bracket
120 Bottom Bracket
130 Spring
140 Travel Limiter
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In an apparatus for printing images on a moving primary imaging member by jetting ink, containing a fluid and marking particles, in an image-wise fashion onto the primary imaging member, a device for concentrating the ink prior to transferring a marking particle image to a receiver member. The ink concentrating device includes a fractionating unit for separating fluid of the ink from the marking particles. The fractionating unit is located a predetermined spaced distance from the primary image bearing member. An electrostatic field is established between the primary image bearing member and the fractionating unit for concentrating the marking particles in the liquid of the ink.
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This is a continuation of application Ser. No. 136,889, filed Dec. 22, 1987, pending.
TECHNICAL FIELD
The subject invention generally pertains to airflow regulators that modulate a supply airflow to a comfort zone, and more specifically pertains to airflow regulators that are responsive to both temperature and upstream air pressure.
BACKGROUND OF THE INVENTION
The temperature of a comfort zone, such as a room within a building, can be controlled by regulating the amount of temperature conditioned air supplied to the zone. Airflow regulators used for this purpose are mounted to a supply air duct and are generally referred to as variable air volume valves, or simply VAV valves.
Airflow through VAV valves is often controlled by varying the valve opening in response to the temperature of the zone. Valves under such control are referred to as pressure dependent valves, because for a given valve opening, the amount of airflow depends on the air pressure upstream of the valve. In some systems, airflow regulation becomes inadequate as a result of widely varying upstream pressure due to varying supply air blower speed or the effects of the opening and closing of other VAV valves in the system.
An improvement in airflow regulation is provided by controlling VAV valves in response to upstream pressure in addition to zone temperature. Such valves are referred to as pressure independent valves. Should the upstream pressure vary for any reason, the pressure independent valve will compensate by opening or closing an appropriate amount to maintain the desired airflow.
Pressure independent valves are generally superior to pressure dependent valves, provided an airflow indicator associated with the pressure independent valve doesn't fail. Should failure occur, present VAV valves typically lock at a fixed position. Depending on the specific control, the valve may lock fully open, fully closed, or at some other intermediate position. Regardless of the position, the failure of a pressure transducer associated with the airflow indicator destroys the valves ability to modulate flow.
Therefore, it is an object of the invention to provide a VAV valve that modulates airflow in response to temperature and upstream pressure, and continues to modulate airflow even when a pressure transducer associated with the valve fails.
Another object of the invention is to provide a VAV valve with a control that avoids the flow regulating problems associated with pressure dependent valves.
A further object is to reduce a VAV valve's dependence on a flow indicator incorporating a pressure transducer.
A still further object is to provide a VAV valve that properly modulates airflow as it compensates for varying speeds of an upstream supply air blower and compensates for the opening and closing of other VAV valves.
Another object is to detect a faulty pressure transducer by determining the valve position and comparing a signal provided by the transducer to a predetermined normal range for the given valve position.
Yet another object is to determine an intermediate valve position between fully open and fully closed without actually sensing an intermediate position of the valve.
These and other objects of the invention will a apparent from the attached drawings and the description of the preferred embodiment that follows below.
SUMMARY OF THE INVENTION
A normally pressure independent VAV valve functions as a pressure dependent valve upon failure of a flow indicator associated with the valve.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 illustrates a VAV system incorporating a preferred embodiment of the invention.
FIG. 2 shows the control algorithm of the VAV valve controller.
DESCRIPTION OF THE PREFERRED EMBODIMENT
FIG. 1 shows a building 10 having three comfort zones 12 whose temperature is controlled by a VAV system incorporating the subject invention. Supply air 14 discharged by a variable speed blower 16 is temperature conditioned by a heat exchanger 18 before being distributed to zones 12. In the preferred embodiment, heat exchanger 18 is a refrigeration cooling coil (evaporator). However in a broader sense, heat exchanger 18 represents any device for heating or cooling air such as a steam coil, electric heater, combustion gas to air heat exchanger, and refrigeration coils, i.e., condensers and evaporators. A VAV valve 20 disposed in a supply air duct 22 leading to each zone 12 regulates the airflow to its respective zone 12 to meet each zone's temperature conditioning demand. Return air 23 is conveyed back to blower 16 via a return air duct 25.
The opening and closing of each valve 20 is controlled by separate valve controllers 24. Each valve controller 24 determines a desired supply airflow rate based on a control signal 26 provided by a thermostat 28. The deisred airflow rate is that which will meet the temperature conditioning demand of the zone. Thermostat 28 represents any temperature sensor that provides a control signal 26 that changes in response to a temperature associated with at least one zone 12.
Each valve controller 24 also determines the actual airflow rate based on a feedback signal 30 provided by a flow indicator 32. Flow indicator 32 represents any device which provides a feedback signal 30 that changes in response to a physical parameter of supply air 14. Examples of the physical parameter include, but are not limited to, the rate of airflow, total pressure, static pressure, and velocity pressure. The specific flow indicator 32 used in the preferred embodiment functions under the same operating principles as a Pitot tube; however, a wide variety of other flow indicators could also be used. For example, the rate of airflow could be determined as a function of valve position in conjunction with static or total pressure readings taken both upstream 34 and downstream 36 of valve 20. As another example, in certain installations, one could assume a predetermined downstream pressure and determine airflow as a function of valve position and upstream pressure alone. Airflow can also be measured using a variety of other flow indicators such as flow turbines, orifices, venturies, vortex sensors, and electric heat dissipators.
Based on the feedback signal 30 respresenting the actual airflow rate, and based on the thermostat's control signal 26 from which a desired airflow is derived, controller 24 determines the appropriate valve position and moves valve 20 accordingly. Should flow indicator 32 malfunction, valve controller 24 disregards erroneous feedback signals and varies the valve position in response to the temperature error. In effect, the normally pressure independent valve 20 functions as a pressure dependent valve in the event of a flow indicator failure. A means for detecting a flow indicator failure is incorporated in the valve controller's control algorithm shown in FIG. 2.
Referring to FIG. 2, control begins at blocks 37 and 38 by initially driving the valve to the closed position. In block 40, controller 24 determines the temperature error by comparing the actual temperature of the zone sensed by thermostat 28 to a setpoint temperature of the zone. If the error is within a deadband, e.g., 0.5° F., no control action is taken as indicated by decision block 42. Otherwise, block 44 determines a desired airflow rate as a function of the temperature error. Depending on the desired degree of control, the function can be proportional, integral, proportional plus integral, or any one of the many widely used control schemes.
Blocks 46 and 48 direct controller 24 to read the electrical feedback signal 30 provided by flow indicator 32, and compute the actual airflow as a predetermined function of signal 30.
Decision blocks 50, 52, and 54 provide means for detecting a flow indicator failure. A flow indicator failure is identified if the computed actual airflow rate is greater than a predetermined limit, e.g., 110% of a nominal value representing a maximum possible airflow rate. An indicator failure is also identified as a computed airflow rate of zero for a given valve position, e.g., 20% open. If an airflow indicator failure exists, block 58 computes a desired change in valve position as a predetermined function of desired airflow (block 44) and the valve position. If no failure exists, the change in valve position is computed by block 56 as a function of airflow (block 48) and desired airflow (block 44).
Decision block 60 determines whether valve 20 should be driven open or closed for the time increment "M" computed in blocks 56 and 58, and block 62 or 64 directs controller 24 to move valve 20 accordingly. The change in valve position "M" is in terms of time to eliminate the need for intermediate valve position sensors. Controller 24 is programmed to know the time it takes to move valve 20 between fully open and fully closed. The time period is 10 seconds in one embodiment of the invention. With this information, controller 24 controls and monitors the position of valve 20 based on the time increment that valve 20 is driven open or closed.For example, if the current position of valve 20 is 50% open and valve 20 is driven closed for 2 seconds, the new valve position will be 30% open. This new valve position is subsequently relied upon as the current valve position in blocks 54 and 58. The algorithm continually repeats as long as the VAV system is operating or an interrupt momentarily stops the algorithm to allow for valve position calibration.
In the preferred embodiment of the invention, the algorithm is carried out by means of an NEC 78C10 microcomputer. The microcomputer based control lends itself well to be externally controlled by a central controller 70. Controller 70 provides a convenient means for remotely monitoring and altering the acutal control of valves 20 and blower 16 to respond to accupancy, diurnal changes or varying temperature setpoints.
Although the invention is described with respect to a preferred embodiment, modifications thereto will be apparent to those skilled in the art. Therefore, the scope of the invention is to be determined by reference to the claims which follow.
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A pressure independent variable air volume valve (VAV valve) functions as a pressure dependent valve upon detecting a malfunctioning airflow indicator. Under normal operating conditions, the VAV valve modulates supply airflow to a comfort zone in response to the zone temperature and the rate of airflow through the valve. If the airflow indicator fails, the VAV valve modulates the supply airflow in response to the zone temperature, independent of the airflow indicator.
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CROSS-REFERENCE TO RELATED APPLICATIONS
This application is entitled to the benefit of Provisional Patent Application Serial No. 60/322,417 filed Sep. 15, 2001.
FIELD OF THE INVENTION
The present invention relates generally to a comfort management system for equine and, in particular, to a multi-purpose, multi-functional hoof-ware device, boot or shoe and inserts used in conjunction therewith, suitable for use on all equine hooves in all equine environments and in the treatment of different equine aliments.
BACKGROUND OF THE INVENTION
As is well known in the art, hoof-ware devices or steel shoes are designed to protect a horses hoof from the environment. Generally, equine steel shoe devices are attached to the bottom side of the horses hoof with “tangible” nails. Alternatively, other types of hoof-ware are available which are attached to the horses hoof by the use of a strap or multiple straps, molding the boot around the horses hoof, shrinking the material around the horses hoof, and/or clamping the boot to the horse hoof with metal brackets. It is also known to use “metal” or “plastic” inserts inside of the aforementioned boots to provide protection and to stabilize the hoof.
For example, to a limited degree, features encompassing equine hoof-ware devices are disclosed in the size-adjustable composition horse boot prior art invention U.S. Pat. No. 5,661,958 wherein a hard rubber device is used with a tensioning means including external brackets having a plurality of outwardly directed projections to provide an adjustable fit boot. The focus of this invention is to provide an adjustable mechanism to the boot to allow variation of the distance from the back of a serrated strap to the toe of the boot.
Prior art for invention U.S. Pat. No. 3,703,209, teaches a molded horseshoe which eliminates the need for frequent shoeing of the metal type and provides protection to the horses hoof.
U.S. Pat. No. 4,981,010 relates generally to a horseshoe, and in particular to a molded flexible horse boot focusing on the replacement of the metal horseshoe. The molded boot is designed to distribute the weight around the horse hoof and to also cover the hoof to keep it from direct contact with the ground.
Prior art for invention U.S. Pat. No. 4,174,754 relates to the adjustable boot-type composition horseshoe related to an improvement in composition horseshoes particularly of the type disclosed in U.S. Pat. No. 3,732,929 issued May 15, 1973 to Neel W. Glass and in U.S. Pat. No. 3,703,209 issued Nov. 21, 1972 to Neel W. Glass. These patents disclose 3 one piece molded horseboots or horseshoe type inventions to replace the horseshoe and having a sole and somewhat flexible envelope for surrounding the horse's hoof below the coronary band. The focus of these prior art patents is primarily on using side brackets, barbs, and brackets for tensioning. U.S. Pat. Nos. 3,703,209 and 3,732,929 disclose molded boots for horses secured in place by a cable and toggle arrangement.
Prior art for invention U.S. Pat. No. 5,174,382, issued Dec. 29, 1992, is a boot device and method for use in preventing laminitis in the foot of a horse. The boot is designed to fit over the horse's hoof. A bladder is positioned inside of the boot and beneath the frog of the horse's hoof. A pump is connected to the bladder to provide pulsating pressure to the frog of the horse's hoof to simulate the pressure applied to the frog while the horse is walking.
U.S. Pat. No. 5,588,288, issued Dec. 31, 1996, teaches a boot for horse's hooves designed for shod horses, that stays firmly anchored to the hoof and yet does not damage the structure of the hoof itself. This invention focuses on the equine hoof effects concerned with stabilizing, equalizing and comforting the loaded and/or unloaded shod hoof.
U.S. Pat. No. 3,967,683, issued Jul. 6, 1976, teaches a slipper-like footwear device in the form of a split ring having a configuration substantially corresponding to the peripheral configuration of a hoof with the split at the rear or heal portion of the slipper. This hoof-ware invention focuses on the equine hoof effects concerned with stabilizing, equalizing and comforting the loaded and/or unloaded hoof, shod or unshod.
U.S. Pat Nos. 2,988,828 and 3,486,561 disclose an animal boot of unitary molded construction with an annular wall of limited resiliency. U.S. Pat. Nos. 2,446,371, 2,064,566, and 3,209,726 disclose boots for dogs also of a flexible construction and generally shaped to fit the foot. U.S. Pat. No. 3,285,346 discloses a hoof covering molded in place to the hoof lower surfaces. U.S. Pat. Nos. 3,794,119 and 4,155,406 disclose boots held in place by straps or a strap. U.S. Pat. No. 3,236,310 discloses a boot of heat sensitive material thermally shrunk into place on the hoof. U.S. Pat. No. 3,967,683 discloses a bifurcated boot for clamping to the hoof. U.S. Pat. No. 3,386,226 discloses an elastomeric scalper-type covering disposable about the hoof to protect the hoof. U.S. Pat. No. 2,041,538 discloses a rubber horse boot having a continuous wall integral with the boot sole with the frontal wall portion being of greater height than the rear wall portion.
Prior art for invention U.S. Pat. No. 4,736,800, issued Apr. 12, 1988, is referred to as footware for hoofed animals comprising a cup-like, closed, resilient unit having a sole and hoof-covering part used as a substitute for a shoe and may be suitable for treatment of sick animals. This hoof-ware invention focuses on the equine hoof effects concerned with stabilizing, equalizing and comforting the loaded and/or unloaded hoof, shod or unshod.
Prior art for invention U.S. Pat. No. 5,715,661, issued Feb. 10, 1998, discloses a boot for horses designed for protecting a horse's hoof from damage, improved adjustability, is simple in structure, easy to put on the hoof, does not inadvertently pop open and is devoid of damaging internal metal protuberances. This hoof-ware invention focuses on the equine hoof effects concerned only with stabilizing equalizing and comforting the loaded and/or unloaded hoof, shod or unshod.
Prior art for invention U.S. Pat. No. 4,290,487, issued Sep. 22, 1981, teaches a protective boot of unitary construction shaped so as to lend itself to temporary radical distortion.
Prior art for invention U.S. Pat. No. 5,209,048, issued May 11, 1993, teaches a device with means for irrigation of medication and removal of fluids in the treatment of hoof injuries and disorders. This hoof-ware invention focuses on the equine hoof effects concerned with stabilizing, equalizing and comforting the loaded and/or unloaded hoof, shod or unshod.
Prior art for invention U.S. Pat. No. 5,363,632, issued Nov. 15, 1994, discloses an equine athletic boot which includes a panel of shock absorbing material that is wrapped around the lower leg of a horse for support and protection in the area of the pastern, fetlock, and canon bone, comprising shock absorbing material with a vertically oriented tubular bladder carried by the panel.
However, equine hoof steel one-dimensional shoes of known types, as well as the other types of hoof-ware discussed above, generally do not provide for optimized balanced cushioning, flexibility and comfort while also providing healing enhancements for different equine hoof ailments encountered in the overall normal wear of the horse's hoofs. Also of consideration is the prior art's silence regarding diagnostic, medical, corrective, rehabilitated and/or emergency environments related to horse hoof care. The known prior art does not provide for a “single” horse hoof-ware shoe and/or boot which addressees all of the foregoing needs, i.e., normal wear and tear to the horses hoof through the owners/caretakers use of the horse, and diagnostic, medical corrective, rehabilitated and/or emergency environments related to horse hoof care. Moreover, the prior art teaches horse style boots or hoof coverings primarily used for protective purposes. The boots/coverings have a problem of retention on the hoof because of forces, common and uncommon, to the hoof. The prior art addresses this retention problem by teaching the attachment of the boots with straps, molding the boot around the hoof, shrinking the materials around the hoof, and/or clamping the boot/covering with metal brackets, all causing the boot to be clumsily installed on the hoof and limited in their use. Also of concern is the problem that horse boots of the prior art have limited adjustability, insecure closures which tend to pop open during use, and metal protuberances inside and/or outside of the boot which can do further damage to a horse's hoof. These types of horse boots are also difficult to place on the hoof, with a somewhat complicated structure and are poor fitting which tends to have the horse walk on its toe, creating a stress on the leg. The prior art is also silent with respect to a horse hoof-ware that is adjustable in size such that it can fit any size horse hoof.
Hence, there is a need for solving the problem of providing an equine hoof shoe or boot that provides for optimized balanced cushioning, flexibility and comfort while also providing for healing enhancements for different equine hoof ailments and for a healthily hoof in the overall normal wear and use of the horses hooves. A need also exists for a horse shoe which provides not only either protection from the environment or addresses one specific medical need, but rather there is a need for a shoe which also provides for diagnostic, medical, corrective, rehabilitative, and/or emergency environments related to horse hoof care in a single shoe. A need also exists for horse boots/coverings which are not retained by being strapped with buckles, molded, clamped or retained with metal brackets and when subjected to forces, common and uncommon to the hoof, remains retained on the hoof. A horse shoe/boot is also needed which allows adjustability, and has secure closures that do not pop open during use. A need also exists for a boot which addresses all of the foregoing concerns and short comings in the prior art and further which fits the hoof in a manner that does not cause stress to the leg while in use. Evolving equine industry has established the fact that equine hoof care comprises more than the steel shoe now used in most equine environments. Enhanced flexibility within the healing process in solving multiple equine hoof diseases with the one-dimensional steel shoe is creating an environment wherein more thought is being made to alternative multi-dimensional solutions. Research has led the industry in the direction of a non-shod trend in the major equine environments, including, but not limited to, normal, medicated, corrective, rehabilitative and/or emergencies. This trend suggests there needs to be equine related hoof care shoes and management systems configured to be used in all of the foregoing environments.
SUMMARY OF THE INVENTION
The present invention is distinguished over the known prior art in a multiplicity of ways. For one thing, the present invention provides an equine hoof-ware system which establishes the general framework for equine hoof comfort variations using single and/or multiple inserts. The inserts are affixed to an internal interlocking mechanism uniquely designed inside the equine hoof shoe/boot/hugger to lock each insert while being used to reach the comfort level for the required healthy or unhealthy-to-healthy state of the horse. Individual horse owners/caretakers have available to them through the embodiments of this invention, a complete line of comfort products for their horses including variations, combinations, multiple fixed by using the multiple internal inserts designed for the general comfort, disease, external abnormalities, soft soles, or lost shoes.
Furthermore, the present invention provides an equine “lightweight” versatile hoof-ware specially configured to be used on a “non-shod” equine and for multiple hoof uses in all equine environments. Thus, one horse boot is provided that may be used for comfort, injury, emergency and all other situations arising in equine environments. The inserts are designed in multiple densities, thicknesses. and materials. When used in conjunction with the outer covering/hugger the hoof-ware system stabilizes equine hoof at normal use, enhances the medicinal healing processes as necessary, equalizes loading and unloading, provides corrective measures, optimizes rehabilitation processes, and comforts the hoof in all environments.
Moreover, the present invention, in one preferred form provides an equine hoof-ware device and specially designed insert devices to be used to comfort shod or non-shod horse hooves in either a healthy or unhealthy state, such as general comfort, cushioning, protection from sharp earthly objects, healing from surgery, recovering from diseases like founder, coffin bone, rotation, thrush, abscesses, general bruises, punctures, frog abnormalities, soft soles, or lost shoes. The insert devices of the present invention, preferably, in one embodiment, fit inside a hoof-ware device designed for multiple hoof mode environments, for example, diagnostics, normal use, performance, corrective, medicinal, emergencies, preventative measures against injury and the like and rehabilitation of the hoof. In addition, the hoof-ware system solves the problem of proper fit in that it is provided in multiple hoof sizes. The hoof-ware device of the present invention further provides a secure closure so that the device does not “pop open” when in use. Sucinctly, the aim of this invention is to create a hoof-ware device, including inserts, for hoofed animals and more particularly for shod or non-shod horses, which stabilizes and/or equalizes and/or comforts the equine hoof while in multiple environments, such as, normal work, pleasure, performance, preventative maintenance, medication, correction, rehabilitation, emergency and/or diagnostic situations.
In summary, the present invention provides an equine hoof-ware, comprising a sole having a base circumscribed by a peripheral wall having an upwardly and inwardly extending forward most end, an upwardly and outwardly extending rearward most end, and a pair of spaced apart upwardly extending sidewalls interposed between the forward most end and the rearward most end of the peripheral wall for defining a receiving area. A mid-sole received within the receiving area and circumscribed by the peripheral wall is also provided. The hoof-ware also includes a removable insert. An interlocking means is integrally formed with the mid-sole and with the removable insert and comprised of at least one complementary protrusion and indention pair mating of the removable insert and the mid-sole for receiving and interlocking the two together such that the removable insert can be inserted and then removed and replaced with a different removable insert for treating different equine hoof related aliments. The equine hoof-ware also include a front upper connected to the sole and circumscribing the forward most end and the pair of sidewalls of the sole for defining an opening for receiving an equine hoof into the front upper and onto the mid-sole and sole. The front upper extends upwardly from the sole and mid-sole at an angle and terminates into an upper edge which angles downwardly from the forward most end to the rearward most end of the sole such that the front upper tapers from the forward most end to the rearward most end of the sole for substantially covering a forward region and side regions of the equine hoof received therein. In addition, a contoured back upper comprised of a lower section operatively coupled to the rearward most end of the sole, an upwardly extending bulb section integrally formed with the lower section and shaped to receive an equine bulb of a heel, and a pair of extensions integrally formed with the upwardly extending bulb section for wrapping around the front uppers also provided. Means for coupling the pair of extensions to the front upper are included such that when the equine hoof is received into the front upper and onto the mid-sole and sole and when the pair of extensions are coupled to the front upper the equine hoof is essentially surrounded and secured within the equine hoof-ware.
The equine hoof-ware of the present invention is also distinguishable over the known prior art in that it is also comprised of a sole having a base extending from a forward most end to a rearward most end of the sole. A mid-sole connects to the base of the sole and includes a cross sectional area upwardly slopping from the rearward most end of the sole and then downwardly sloping for providing a relief area and then upwardly slopping to the forward most end of the sole such that when the mid-sole is compressed the cross sectional area absorbs equine impact. A front upper is connected to the mid-sole and circumscribes a forward most end and a pair of sidewalls of the mid-sole for defining an opening for receiving an equine hoof into the front upper and onto the mid-sole. The front upper also extends upwardly from the mid-sole at an angle and terminates into an upper edge which angles downwardly from the forward most end to the rearward most end of the sole such that the front upper tapers from the forward most end to the rearward most end of the sole for substantially covering a forward region and side regions of the equine hoof received therein. The equine hoof-ware also includes a contoured back upper comprised of a lower section operatively coupled to the rearward most end of the sole, an upwardly extending bulb section integrally formed with the lower section and shaped to receive an equine bulb of a heel, and a pair of extensions integrally formed with the upwardly extending bulb section for wrapping around the front upper. Means for coupling said pair of extensions to the front upper are provided such that when the equine hoof is received into the front upper and onto the mid-sole and sole and when the pair of extensions are coupled to the front upper the equine hoof is essentially surrounded and secured within the equine hoof-ware.
Moreover, having thus summarized the invention, it should be apparent that numerous modifications and adaptations may be resorted to without departing from the scope and fair meaning of the present invention as set forth as described hereinbelow by the claims.
OBJECTS OF THE INVENTION
Accordingly, a primary object of the present invention is to provide a new, novel and useful comfort management system for equine embodied in a single hoof-ware device.
A further object of the present invention is to provide a system as characterized above which is suitable for use on healthy equine.
Another further object of the present invention is to provide a system as characterized above which is suitable for use on unhealthy equine.
Another further object of the present invention is to provide a system as characterized above for use on shod or non-shod hooves.
Another further object of the present invention is to provide a system as characterized above which provides an outer shell, a sole and a mid sole, the mid-sole including integrally formed interlocking means, into which inserts, the inserts also including integrally formed interlocking means, of different geometric shapes and dimensions may be inserted, removed and/or replaced.
Another further object of the present invention is to provide a system as characterized above which protects equine from earthly objects.
Another further object of the present invention is to provide a system as characterized above for use on equine healing from surgery and/or recovering from any of the many equine diseases which may effect the hoof.
Another further object of the present invention is to provide a system as characterized above which, in one embodiment, provides a hoof-ware device that is designed to fit multiple hoof sizes.
Viewed from a first vantage point, it is an object of the present invention to provide an equine hoof-ware, comprising in combination: a sole having a base circumscribed by a peripheral wall having an upwardly and inwardly extending forward most end, an upwardly and outwardly extending rearward most end, and a pair of spaced apart upwardly extending sidewalls interposed between the forward most end and the rearward most end of the peripheral wall for defining a receiving area; a mid-sole received within the receiving area and circumscribed by the peripheral wall; a removable insert; an interlocking means integrally formed with the mid-sole and with the removable insert and comprised of at least one complementary protrusion and indention pair mating of the removable insert and the mid-sole for receiving and interlocking the two together such that the removable insert can be inserted and then removed and replaced with a different removable insert for treating different equine hoof related aliments; a front upper connected to the sole and circumscribing the forward most end and the pair of sidewalls of the sole for defining an opening for receiving an equine hoof into the front upper and onto the mid-sole and sole; the front upper extending upwardly from the sole and mid-sole at an angle and terminating into an upper edge which angles downwardly from the forward most end to the rearward most end of the sole such that the front upper tapers from the forward most end to the rearward most end of the sole for substantially covering a forward region and side regions of the equine hoof received therein; a contoured back upper comprised of a lower section operatively coupled to the rearward most end of the sole, an upwardly extending bulb section integrally formed with the lower section and shaped to receive an equine bulb of a heel, and a pair of extensions integrally formed with the upwardly extending bulb section for wrapping around the front upper; means for coupling the pair of extensions to the front upper such that when the equine hoof is received into the front upper and onto the mid-sole and sole and when the pair of extensions are coupled to the front upper the equine hoof is essentially surrounded and secured within the equine hoof-ware.
Viewed from a second vantage point, it is an object of the present invention to provide an equine hoof-ware, comprising in combination: a sole having a base extending from a forward most end to a rearward most end of the sole; a mid-sole connected to the base of the sole and including a cross sectional area upwardly slopping from the rearward most end of the sole and then downwardly sloping for providing a relief area and then upwardly slopping to the forward most end of the sole such that when the mid-sole is compressed the cross sectional area absorbs equine impact; a front upper connected to the mid-sole and circumscribing a forward most end and a pair of sidewalls of mid-sole for defining an opening for receiving an equine hoof into the front upper and onto the mid-sole; the front upper extending upwardly from the mid-sole at an angle and terminating into an upper edge which angles downwardly from the forward most end to the rearward most end of the sole such that the front upper tapers from the forward most end to the rearward most end of the sole for substantially covering a forward region and regions of the equine hoof received therein; a contoured back upper comprised of a lower section operatively coupled to the rearward most end of the sole, an upwardly extending bulb section integrally formed with the lower section and shaped to receive an equine bulb of a heel, and a pair of extensions integrally formed with the upwardly extending bulb section for wrapping around the front upper; means for coupling the pair of extensions to the front upper such that when the equine hoof is received into the front upper and onto the mid-sole and sole and when the pair of extensions are coupled to the front upper the equine hoof is essentially surrounded and secured within the equine hoof-ware.
These and other objects and advantages will be made manifest when considering the following detailed specification when taken in conjunction with the appended drawing figures.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a side view of a hoof-ware device shown with the hoof-ware attachments attached thereon.
FIG. 2 is a side view of a hoof-ware sole device.
FIG. 3 is a side view of a hoof-ware upper device.
FIG. 4 is a side view of a hoof-ware contoured rear device.
FIG. 5 is a downward perspective side view of the hoof-ware sole connected to the mid-sole, and contoured upper sole.
FIG. 6 is a side view of the hoof-ware sole cross-section profile front to back.
FIG. 7 is a side view of the hoof-ware sole cross-section profile side to side.
FIG. 8 is a side view of the hoof-ware sole section.
FIG. 9 is a side view of the hoof-ware side wall.
FIG. 10 is a top plan view of the hoof-ware sole.
FIG. 11 is a side view of the hoof-ware sole, attached to the mid-sole, sidewall and upper sleeve.
FIG. 12 is a sidewall diagram of the hoof-ware sole, side to side.
FIG. 13 is a sidewall diagram of the hoof-ware sole, front to back.
FIG. 14 is a sidewall diagram of the hoof-ware contour design.
FIG. 15 is a diagram of the hoof-ware interior sole dimensions.
FIG. 16 is a side view of the hoof-ware contoured back attached to the front upper, mid-sole and sole.
FIG. 17 is a top plan view of the insert and the tri-lock interlocking mechanism.
FIG. 18 is an exploded view of an insert shown with the tri-lock interlocking mechanism of FIG. 17 prior to its engagement into the mid-sole mechanism of the hoof-ware system.
FIG. 19 is a top and side plan view of a single density flat insert already engaged with the tri-lock interlocking mechanism of FIG. 17 .
FIG. 20 is a top and side plan view of a flat multi-density insert already engaged with the tri-lock interlocking mechanism of FIG. 17 .
FIG. 21 is a top and side plan view of a multi-compound flat insert already engaged with the tri-lock interlocking mechanism of FIG. 17 .
FIG. 22 is a top and side plan view of a wedge single density insert already engaged with the tri-lock interlocking mechanism of FIG. 17 .
FIG. 23 is a top and side plan view of a wedge multi-density insert already engaged with the tri-lock interlocking mechanism of FIG. 17 .
FIG. 24 is a top and side plan view of a multi-compound wedge insert already engaged with the tri-lock interlocking mechanism of FIG. 17 .
FIG. 25 is a top and side plan view of a flat cutout insert already engaged with the tri-lock interlocking mechanism of FIG. 17 .
FIG. 26 is a top and side plan view of a wedge cut-out insert already engaged with the tri-lock interlocking mechanism of FIG. 17 .
FIG. 27 is a top and side plan view of an add-on attachment for use with any wedge insert and already engaged with the tri-lock interlocking mechanism of FIG. 17 .
FIG. 28 is a top and side plan view of an add-on attachment for use with a flat insert already engaged with the tri-lock interlocking mechanism of FIG. 17 .
FIG. 29 is a top and side plan view of a perforated flat insert already engaged with the tri-lock interlocking mechanism FIG. 17 .
FIG. 30 is a top and side plan view of a concave contour flat insert already engaged with the tri-lock interlocking mechanism of FIG. 17 .
FIG. 31 is a top and side plan view of an angled convex contour insert already engaged with the tri-lock interlocking mechanism of FIG. 17 .
FIG. 32 is a top and side plan view of a rounded convex contour insert already engaged with the tri-lock interlocking mechanism of FIG. 17 .
FIG. 33 is a top and side plan view of a sizing insert already engaged with the tri-lock interlocking mechanism of FIG. 17 .
FIG. 34 is a top and side plan view of an impression form insert already engaged with the tri-lock interlocking mechanism of FIG. 17 .
FIG. 35 is a top and side plan view of a mechanical diagnostic insert already engaged with the tri-lock interlocking mechanism of FIG. 17 .
FIG. 36 is a top and side plan view of an x-ray/radiograph liner insert including adjustable wire markers already engaged with the tri-lock interlocking mechanism FIG. 17 .
FIG. 37 is a top and side plan view of an electronic diagnostic insert already engaged with the tri-lock interlocking mechanism of FIG. 17 .
FIG. 38 is a side and interior view of the sole with a slide-locking channel mechanism and an underside view of the hoof-ware device's mid-sole and upper sleeve.
FIG. 39 is a top and side plan view of an adjustable leveling positioning insert device already engaged with the slide-locking channel mechanism of FIG. 38 .
FIG. 40 is a side view of a liner sleeve sock.
FIG. 41 is a side view of an alternative embodiment of hoof-ware attachment already attached to the hoof-ware device.
FIG. 42 is a side view of an alternative embodiment of hoof-ware attachment already attached to the hoof-ware device.
DESCRIPTION OF PREFERRED EMBODIMENTS
Considering the drawings, wherein like reference numerals denote like parts throughout the various drawing figures, reference numeral 10 is directed to the comfort management system for equine according to the present invention.
In essence, and referring to the drawings, the present invention provides a comfort management system 10 for equine, comprising a sole 4 having a base circumscribed by a peripheral wall 5 having an upwardly and inwardly extending forward most end, an upwardly and outwardly extending rearward most end, and a pair of spaced apart upwardly extending sidewalls interposed between said forward most end and said rearward most end of said peripheral wall for defining a receiving area. The system 10 also includes a mid-sole 2 received within said receiving area and circumscribed by said peripheral wall 5 . A removable insert 14 is also provided. The system 10 also teaches an interlocking means 12 (FIG. 5) integrally formed with the mid-sole 2 and with said removable insert 14 and comprised of at least one complementary protrusion 16 d, 16 e, 16 f, and 16 g and indention pair 16 , 16 a, 16 b, and 16 c (FIG. 18) mating the removable insert 14 and the mid-sole 2 for receiving and interlocking said two together such that said removable insert 14 can be inserted and then removed and replaced with a different removable insert, for example 38 to be discussed hereinabelow, for treating different equine hoof related aliments. A front upper 6 connected to said sole 4 and circumscribing said forward most end W and said pair of sidewalls of said sole 4 for defining an opening 118 (FIG. 16) for receiving an equine hoof into said front upper 6 and onto said mid-sole 2 and sole 4 . The front upper extending upwardly from the sole 4 and mid-sole 2 at an angle and terminating into an upper edge 70 which angles downwardly from said forward most end to said rearward most end of said sole 4 such that said front upper 6 tapers from said forward most end to said rearward most end of said sole 4 for substantially covering a forward region and side regions of the equine hoof received therein. A contoured back upper 8 comprised of a lower section operatively coupled to said rearward most end of said sole 4 , an upwardly extending bulb section 128 integrally formed with said lower section and shaped to receive an equine bulb of a heel, and a pair of extensions 226 integrally formed with said upwardly extending bulb section for wrapping around said front upper 6 . Means are provided for coupling said pair of extensions to said front upper 6 such that when said equine hoof is received into said front upper 6 and onto said mid-sole 2 and sole 4 and when said pair of extensions 226 are coupled to said front upper 6 the equine hoof is essentially surrounded and secured within the equine hoof-ware.
Viewing FIGS. 1, 17 and 18 , it can be seen that the equine hoof-ware 10 includes an interlocking means 12 comprised of three triangularly spaced complementary protrusions 16 , e, 16 f, 16 g and indentions 16 a, b and c pairs disposed on the removable insert 14 and the mid-sole 2 for receiving and interlocking the two together such that the removable insert can be inserted and then removed and replaced with a different removable insert, for example 38 , for treating different equine hoof related aliments.
The equine hoof-ware interlocking means 12 is further comprised of a rectangularly shaped complementary protrusion 16 d and indention 16 pair disposed at a back end on the removable insert 14 and the mid-sole 2 for receiving and interlocking the two together such that the removable insert can be inserted and then removed and replaced with a different removable insert for treating different equine hoof related aliments.
The equine hoof-ware interlocking means 12 is further comprised of a triangularly shaped complementary protrusion and indention disposed proximate the back ends of the removable insert 14 and the mid-sole 2 at a location surmounting said rectangularly shaped complementary protrusion and indention pair for receiving and interlocking the two together such that the removable insert can be inserted and then removed and replaced with a different removable insert for treating different equine hoof related aliments.
The equine hoof-ware front upper 6 is further comprised of a front section and side sections which upwardly extend from said sole 4 and mid-sole 2 at an angle and terminates into the upper edge 70 which angles downwardly from said forward most end to said rearward most end of the sole 4 such that the side sections of upper 6 taper from the forward most end to the rearward most end of the sole 4 for substantially covering a forward region and side regions of the equine hoof received therein.
The equine hoof-ware further includes at least one stretch insert 72 integrally formed with at least one of the side sections of the front upper 6 for stretching and accommodating hoof size variations (FIG. 1 ).
The equine hoof-ware 10 is further comprised of, and viewing FIG. 1, a sole 4 having a base extending from a forward most end to a rearward most end of the sole 4 , a mid-sole 2 connects to the base of the sole 4 and including a cross sectional area upwardly slopping from the rearward most end of the sole 4 and then downwardly sloping for providing a relief area and then upwardly slopping to the forward most end of the sole 4 such that when the mid-sole 2 is compressed the cross sectional area absorbs equine impact. A front upper 6 is provided and is connected to the mid-sole 2 and circumscribing a forward most end and a pair of sidewalls of mid-sole 2 for defining an opening 118 for receiving an equine hoof into the front upper 6 and onto said mid-sole 2 . The front upper 6 extending upwardly from the mid-sole 2 at an angle and terminating into an upper edge 70 which angles downwardly from the forward most end to said rearward most end of said sole such that said front upper tapers from said forward most end to the rearward most end of the sole 4 for substantially covering a forward region and regions of the equine hoof received therein. A contoured back upper 8 is also disclosed and is comprised of a lower section operatively coupled to said rearward most end of the sole 4 , an upwardly extending bulb section 128 integrally formed with the lower section and shaped to receive an equine bulb of a heel, and a pair of extensions 226 integrally formed with the upwardly extending bulb section for wrapping around the front upper 6 . Means are also provided for coupling the pair of extensions 226 to the front upper 6 such that when the equine hoof is received into said front upper and onto said mid-sole and sole and when said pair of extensions are coupled to the front upper 6 , the equine hoof is essentially surrounded and secured within the equine hoof-ware.
The equine comfort management system of the present invention, and further when viewing FIG. 1, further provides a hoof-ware device including a bottom sole 4 which includes an upper periphery 5 and a mid-sole 2 surmounted to the upper periphery 5 . The mid-sole 2 is in turn attached to a front upper 6 via a trim line 122 by means of stitching or adhesive which is well known in the art, and as informed by the present disclosure. The trim line 122 traverses the mid-sole 2 from its forward most end to its rearward most end and attaches to a back 8 , which in turn is attached to a back contoured heel cover 128 via adhesive and/or stitching as is well known in the art and as disclosed in the present invention. An upper trim or edge 70 is also provided and is preferably formed from leather or a similar acceptable type material which in turn, connects via stitching or adhesive (as is well known in the art and disclosed by the present invention) with inwardly shown reinforced power frame 224 (shown in phantom) and pulling up over the front hoof wall, and connected by hook and loop attachment 116 , connected to the back 8 , which is preferably formed from stretchy neoprene material, protruding from the inside pulled outwardly and outside pulled inwardly and/or vice versa as a hook and loop stretch strap 226 wrapping around the hoof-ware front upper 6 from the outside and/or inside and/or vice versa. The strap 226 is held in place with a Velcro or similar type adhesive material to securely hold the straps in place, even when exposed to normal and abnormal stress and forces.
Viewing the individual details of the component parts of the present invention, FIG. 2 shows details of the bottom sole 4 attached to contoured mid-sole 2 with reinforced power frame 224 juxtaposed therebetween.
FIG. 3 discloses the front upper 6 which resides interior of the front Wall W and which is designed to form to horse hoof contours. i.e., the front upper 6 includes at least one stretch insert 72 integrally formed with at least one of the side sections of the front upper 6 such that the hoof-ware system 10 adjusts to all hoof shapes and sizes and attaches to the mid-sole 2 , and sole 4 via stitching or adhesive as is well known in the art and as is informed by the present invention.
FIG. 4 shows details of contoured back 8 which wraps around the bulb of the heel of a hoof and attaches forward around the front of hoof. adhering to mid-sole 2 and front upper 6 as is apparent throughout the various drawings. At least one hole 120 is provided on the back 8 for example, providing through air flow.
The details of the interior of the hoof-ware sole 4 connection to a shock absorbing mid-sole section or a contoured mid-sole section 14 , contoured to the upper sole and revealing the embodiments of the sole 4 connection to the base of mid-sole 2 with a height range of ½ an inch to 3½ inches are shown in FIG. 5 . The mid-sole 2 includes dual angled sole sidewalls 18 having a lower angle of 90 degrees to 160 degrees and an upper angle which varies from 90 degrees to 30 degrees. The shock absorbing mid-sole section or insert 14 has a varied derometer from 20 A to 90 D which provides a vented air flow base. Alternatively, both a single and dual density are provided at contoured mid-sole section or insert 14 with a hoof bracket 20 residing immediately thereabove and traversing laterally across section 14 thereby causing reinforced outer hoof stability. Back 8 , operatively connected to the sole 4 , mid-sole 2 , varies from 90 degrees to 30 degrees and includes a drainage system 11 for the through entry and departure of solutions of sorts. Residing abut against the mid interior portion of back 8 and bordered on each side by the shock absorbing mid-sole section 14 and dual angled side wall 18 of mid-sole 2 , is a tri-lock insole interlocking system/device 12 to be used for holding inserts in place, to be discussed hereinafter.
FIG. 6 is side view of the hoof-ware sole 4 taken in cross-section and profiling the dimensions of the device, front to back, sole 4 has a range of 1.0 to 15.0 millimeters thickness, front to back 52 , a range of 76.0 millimeters to 350 millimeters, front bend or corner 48 of sole 4 is 5.0 R millimeters to 30.0 millimeters, a front sole 4 rising up 50 has a range of 10.0 millimeters to 50.0 millimeters, thickness 46 has a range of 1.0 millimeters to 10.0 millimeters, a top thickness range of 1.0 to 10.0 millimeters 40 and length of angle range 0.0 millimeters to 50 millimeters, angle 42 embodying a range of 45 degrees to 65 degrees 42 , back bottom bend or corner 60 has a range of 0.0 millimeters to 30 millimeters, 28 to back device bend 58 has a range of 1.0 millimeters at 10.0 millimeters in length at top of sole back 58 , range degree 56 angle ranging from 45 degrees to 90 degrees, mid-sole inset 38 has a range of 1.0 millimeters of 10.0 millimeters.
FIG. 7 is a side view of hoof-ware sole 4 taken in cross-section profiling from side to side the dimensions of mid-sole insert 38 which has a range 1.0 millimeters to 10.0 millimeters thickness, sole 4 bottom thickness 29 has a range of 1.0 millimeters to 15.0 millimeters, corner or bend of sole and mid-sole thickness range of R 0.0 to R 30.0, side height 32 has a range of 10.0 millimeters to 50.0 millimeters, front sole thickness 26 has a range of 1.0 millimeters to 10.0 millimeters, top thickness 24 has a range of 1.0 millimeters to 10.0 millimeters, interior side to side length 34 has a range of 64.0 millimeters to 350.0 millimeters.
FIG. 8 is a side view of the hoof-ware sole section of sole 4 showing its range of thickness of 1.0 millimeters to 15.0 millimeters for an internal reinforcement strip 62 with a range of thickness of 1.0 millimeters to 10.0 millimeters for an alternative embodiment molded mid-sole 36 which embodies combinations of multiple materials as the construction composites, such as, EVA, rubber compounds, polyethylene, silicon, sorbothane, polymers, and other similar materials resulting in a hoof-ware device that has utilities of flex, cushion, shock absorption, medicinal applications, performance applications, use in diagnostic situations, for stimulation and/or corrective purposes, emergency situations, and/or rehabilitation of the hoof.
FIG. 9 is a side view profile of hoof-ware wall contour of mid-sole ( 2 ) when viewing the mid-sole 2 in a downward angle.
FIG. 10 is a top plan view of hoof-ware mid-sole 2 showing a range of 64.0 millimeters to 350.0 millimeters 74 when the dimensions is taken from side to side, and 76.0 millimeters to 350.0 millimeters 76 when the dimensions are taken from front to back.
FIG. 11 is a side view of an alternative embodiment of the hoof-ware sole 4 connected to a mid-sole 38 , connected to sidewall 18 (shown in section) and upper 6 . Sole 4 and mid-sole 38 are of a contoured shape for correct movement and break over with variable thickness for support and wear which are desirable for proper hoof maintenance. It is to be noted that multiple sole 4 designs for grip and wear have been established by horse breeders and are taught by the disclosure herein such that angled wall 40 is angled to conform to a hoof, and interior wall 62 is configured to bracket the hoof, and tapered side edge 64 , interposed between mid-sole 38 and upper 6 , is configured to blend with upper material 6 to contour with the hoof providing breathable materials that are angled upper from front to back as shown by 70 from 45 degrees to 90 degrees. A Velcro hook or connection 68 connects to back section. 8 padded trimmed upper 70 , stretch insert 72 and front upper 6 and is used for accommodating hoof size variations, including angled back 8 to contour with the hoof heel shape that is 45 degrees to 90 degrees.
FIG. 12 is a sidewall diagram of the hoof-ware sole 4 , without mid-sole 38 , shown in a side to side view, this embodiment of sole 4 at end of sole protruded rubber 84 there is shown a range of 1.0 millimeters to 15.0 millimeters, and a range of 1.0 millimeters to 12.0 millimeters at inside of protruded rubber 86 , corner or bend 94 has a range of 0.0 R to 30.0 R, upper wall width has a range of 1.0 millimeters to 10 millimeters 78 , front height has a range of 10.0 millimeters to 50.0 millimeters 100 , embodying and resulting in a thickness of 1.0 millimeters to 10.0 millimeters, and a length range from side to side of 76 . 0 millimeters to 350.0 millimeters 98 .
FIG. 13 is a sidewall diagram of the hoof-ware sole 4 front to back, with a range length of 76.0 millimeters to 350.0 millimeters 98 a, front range of 10.0 millimeters to 50.0 millimeters 80 , a top thickness range of 1.0 millimeters to 10,0 millimeters 78 , corner or bend in front range of 0.0 R to 30.0 R 82 , back height 92 range of 10.0 millimeters to 50 millimeters, back corner or bend 94 range 0.0 R to 30.0 R, and two grooves 96 for stitching.
FIG. 14 is a view of the sidewall 18 profile of the hoof-ware contour design, height range of 10.0 millimeters to 50.0 millimeters 102 , with a beginning angle height of contour 106 range 20.0 to 50.0, a mid-angle height range of 10 millimeters of contour 108 to 50 millimeters. end contour design range 110 extending 10 millimeters to 50 millimeters.
FIG. 15 is a top plan view of the hoof-ware interior sole 4 dimensions, with a range of 64 millimeters to 350.0 millimeters side to side 112 , and with a range of 76.0 millimeters to 350 millimeters front to back 114 .
FIG. 16 is a side view of the hoof-ware contoured back 8 , contoured to be shaped in a manner that is upward of the hoof to fit the shape of a hoof wherein the lower leg is held in place by the front upper sleeve 6 and, in this embodiment, mid-sole 38 and sole 4 . The contoured padded trim or collar 70 is operative coupled to the upper 6 and includes stretch material, bonded to the trim line 122 , and adhered with adjustable wrap-around strap 226 which embodies an attachment system using hook and loop and attachment 116 , for example, or other latching devices. The contoured upper front receiving section 118 is shaped to fit a hoof and vented to allow air flow at 124 , via hook and loop strip for back attachments 116 which ultimately are contoured to back heel cover 128 , which also provides for a vented back with breathable backing holes 120 .
FIG. 17 is a top plan view diagramming the dimensions of an insert and tri-lock interlocking mechanism shown in FIG. 18 with an interchangeable sole insert using multiple materials, shapes, densities. designs, colors, diagnostics, evaluation components, air flow venting, and providing an insert 130 a of multiple hoof sizes front to back having dimensions sizing range 3 inches to 12 inches, shown by line demarcation 130 b, side to side sizing range 2½ inches to 12 inches, shown by line demarcation 130 c, bottom right side circular interlock 16 f, shown by line demarcation 132 a and has a range ¼ inch to 1 inch diameter and looking downward toward the back, bottom left side circular interlock 16 d, shown by line demarcation 132 c and has a range ¼ inch to 1 inch diameter looking downward toward the back. circular interlock 16 g, shown by line demarcation 132 b range ¼ inch to 1 inch diameter, tri-lock locking system for pads 132 , tri-lock attachment to sole 134 , back of sole perpendicular lock 132 d, being ½ inch, back of sole to tip point of triangle 132 e, being 2.4 inches, bottom of triangle 132 f, being 1½ inches, perpendicular bottom of triangle is a ½ inch by 2 inches.
FIG. 18 a top and side plan view of alliterative embodiment insert into hoof-ware device with tri-lock interlocking mechanism of FIG. 17 into sole 4 and shock absorbing mid-sole section 14 mechanism of the hoof-ware device, downwardly view of the tri-lock 12 interlocking device embodied to the mid-sole 14 thereby being embodied to the sole 4 , tri-lock inset 16 of interlocking mechanism with complementing tri-lock device 16 d, tri-lock mechanism 16 a interlocking with tri-lock mechanism 16 f, tri-lock mechanism 16 b interlocking with tri-lock mechanism 16 e, tri-lock mechanism 16 c, interlocking with tri-lock mechanism 16 g.
FIG. 19 a top and side plan view of an alternative embodiment of an insert and particularly a single density flat insert 136 into hoof-ware device with tri-lock interlocking mechanism 12 , height ( 136 a ) range {fraction (1/10)} inch to 2 inches. comparable densities ( 138 a ) range 1 to 100 on the A derometer scale and/or 1 to 100 on the C derometer scale embodying combinations of multiple materials construction composites, EVA, rubber compounds, polyethylene, silicon, sorbothane, polymers, and other similar materials embodying utilities of flex, cushion, shock absorption, medicinal, performance, diagnostic, stimulation, correction, emergency, and/or rehabilitation environments.
FIG. 20 is a top and side plan view of an alternative embodiment of insert and particularly the flat single-density insert 136 into hoof-ware device with tri-lock interlocking mechanism 12 , and used in combination with a multi-density flat insert 140 , thereby resulting in a multi-density insert, which when viewed from side to side 140 c has a range of 2.5 inches to 12 inches. and front to back 140 b has a range of 3.0 inches to 12 inches, and multi-density compound 140 a and preferably with two or more combinations of parts of EVA, polyethylene, polyurethane, silicon, sorbothane, polymers, composites and/or similar materials consisting of C scale of 1 to 100 and/or A scale of 1 to 100 and/or 0 scale 1 to 100.
FIG. 21 is a top and side plan view of an alternative embodiment and particularly a multi-compound flat insert into hoof-ware device with tri-lock interlocking mechanism 12 , flat insert 136 is altered by a multi-compound insert into insert 142 composed, preferably of, single or multiple combinations EVA, polyethylene, polyurethane, silicon, sorbothane, polymers, composites and/or similar materials, front to back 142 a is ½ inch back from mid-point side to side, or to 0.0 inches, side to side 142 b has a range to ½ inch right side and/or left side, whereas the insert side to side 142 c has a range of 2.5 inches to 12 inches, a front of insert 136 to the front of multi-compound insert 142 has a range of 3.0 inches to 6.0 inches, back of multi-compound insert 142 e to back of insert 136 is ½ inch.
FIG. 22 is a top and side plan view of an alternative embodiment single density wedge insert 144 for placement into hoof-ware device with tri-lock interlocking mechanism 12 , single density wedge insert 144 includes combinations of compounds of EVA, polyethylene, polyurethane, silicon, sorbothane, polymers, composites and/or similar materials. Insert 144 has a dimensional range, front to back 144 a of 3 inches to 12 inches, from side to side 144 b of 2.5 inches to 12 inches, from the back of wedge insert height 144 c varying in range from 2 inches to {fraction (1/10)}th inch, and an angle range of 0 degrees to 35 degrees, wherein the front of wedge insert height 144 e is {fraction (1/10)} inch. It is to be noted that wedge insert 144 embodies multiple configurations at multiple points.
FIG. 23 is a top and side plan view of an alternative embodiment of a wedge multi-density insert 146 into hoof-ware device with tri-lock interlocking mechanism 12 , with dimensions from side to side, insert 146 a of 2½ inches to 12 inches, from front to back, insert 146 b ) of 3 inches to 12 inches, and a back height of multi-density wedge insert 146 c with a range of 0 to 2 inches. with the mid-point if multi-density wedge insert 146 of 0 to 2 inches. The multi-density wedge insert is comprised of one or more compound combinations 148 a of EVA, polyethylene, polyurethane, silicon. sorbothane, polymers, composites and/or similar materials, and having a constant insert thickness measurement of 0 to 2 inches, 148 b.
FIG. 24 a top and side plan view of an alternative multi-compound wedge insert 150 into hoof-ware device with tri-lock interlocking mechanism 12 , the multi-compound 148 a wedge insert, and wedge indentation insert 152 are combined with an insert front to top of wedge 150 a with a range of 3 inches to 6 inches, from back of wedge insert to back of insert 150 c of ½ inch to 0.0 inches, from side to side 150 b of 2.5 inches to 12 inches, from the top of wedge insert to back of wedge insert 150 e, mid-point side to side to 0.0 inches of back of insert, side to side of wedge insert 150 d, mid-point side to side of insert to maximum ½ inches on the right side and ½ inches on the left side.
FIG. 25 a top and side plan view of an alternative cut out 154 of flat insert 136 into hoof-ware device with tri-lock interlocking mechanism 12 , top of insert to top of cutout 136 a has a dimension of {fraction (1/10)}th inches to 2 inches, back of cutout to back of insert 136 b has as dimension of ½ inch to 6 inches, viewing downwardly left side mid-side of insert to mid-side of cutout 136 c has a dimension of ½ inches, downwardly right side mid-side of insert to mid-side of cutout 136 d ha a dimension of ½ inch, cutout height 154 a has a dimension of {fraction (1/10)}th inch to 2 inches, cutout front to back 154 b ½ inch to 0 inches, cutout side to side 154 c ha a dimension of ½ inch on front and side and side.
FIG. 26 is a top and side plan view of triangle cut out 156 of wedge insert 148 with tri-lock interlocking mechanism 12 , back of triangle cut out to back of Insert 148 a bottom of triangle cutout to a inches, side to side of Insert 148 b 2½ inches to 12 inches, front to tip of triangle 148 c {fraction (1/10)}th inches to 2 inches, height of triangle, cut out 156 a {fraction (1/10)}th inches to 2 inches, mid-point side to side triangle 156 b maximum of ½ inch from outer side or side, front to back triangle cut out 156 c ½ inches back from mid-point side to side 148 b to 0 inches.
FIG. 27 is a top and side plan view of add-on triangle attachment 158 to wedge insert 148 into hoof-ware device with tri-lock interlocking mechanism 12 , back height of wedge insert 148 a {fraction (1/10)}th inch to 2 inches, mid-point height of wedge insert 148 b {fraction (1/10)}th inch to 2 inches, front height of wedge Insert 148 c {fraction (1/10)}th inch to 2 inches, front of wedge insert to tip 148 d of triangle insert 158 , 1¾ inches to 7 inches, side to side mid-point of wedge insert 148 e 2½ inches to 12 inches, front tip to back of triangle attachment 158 a 1¼ inches to 5 inches, base side to side of triangle attachment range 1 inches to 6 inches, width of base from triangle to triangle base 156 c ¼ inch to 1 inch, top of triangle base to back of triangle base 158 d ½ inches to 1 inches height of triangle attachment 158 e.
FIG. 28 is a top and side plan view of triangle add-on attachment 160 to a flat Insert 136 into hoof-ware device with tri-lock interlocking mechanism 12 with a height of flat insert 136 a {fraction (1/10)}th inches to 2 inches, front of flat insert to tip of triangle attachment 136 c 1¾ inches to 7 inches, mid-point side to side of flat insert 136 b 2½ inches to 12 inches, tip of triangle insert to back of triangle insert 160 a 1¼ inches to 5 inches, mid-point side to side of triangle insert 160 b 1 inch to 6 inches, width of base from triangle to triangle base 160 c ¼ inch to 1 inch, height of triangle attachment 160 d {fraction (1/10)}th inches to 2 inches, front to back of triangle base from base of triangle to back of insert 160 c.
FIG. 29 is a top and side plan view of flat insert 136 with 15 perforated holes 162 into hoof-ware device with tri-lock interlocking mechanism 12 height of flat insert 136 a {fraction (1/10)}th inches to 2 inches, front to back of flat insert 136 b ½ inch to center point of side to side dimension, midpoint side to side of flat insert 136 c 2.5 inches to 12 inches, diameter of each 3-10 holes 162 a {fraction (1/44)} inches placed ¼ inches inside of edge of insert ranging ½ inch to 1½ inch hole centers, diameter of each 3-22 holes 162 b ¼ inches placed ¼ inch inside of edge of insert ranging ½ inch to 1½ inch hole centers, diameter of each 3-22 holes 162 c ¼ inches placed ¼ inch inside of edge of insert ranging ½ inch to 1½ inch hole centers, diameter of each 3-22 holes 162 d ¼ inches placed ¼ inch inside of edge of insert ranging ½ inch to 1 inch centers.
FIG. 30 is a top and side plan view of concave contour 164 flat insert 136 into hoof-ware device with tri-lock interlocking mechanism 12 with a height of flat insert 136 a {fraction (1/10)}th inches to 2 inches, mid-point side to side of flat insert 136 to outer wall of concave contour 136 b ½ inch to center point of side to side dimension, mid-point side to side of flat insert 136 to right side looking downward to outer wall of concave contour 136 d ½ inch to center point of side to side dimension. back of concave contour 164 to back of flat insert 136 c range to 0 inches, downwardly look at front of flat insert 136 to front of concave contour 164 is 136 e ½ inch to center point of side to side dimension, front to back of concave contour 164 a range of ½ inch to 0 inches, back of concave contour base to height of flat insert 136 ) is 164 b range of {fraction (1/16)}th inch from bottom of insert to top of insert. mid-point side to side 164 c of concave contour multiple ranges from {fraction (1/16)}th inch upward slope to top of insert 136 .
FIG. 31 is a top and side plan view of an angled convex contour insert 166 into hoof-ware device with tri-lock interlocking mechanism 12 height of convex contour at mid-point 168 a {fraction (1/10)} inches to 2.0 inches, mid-point side to side at convex point 168 b range {fraction (2.5)} inches to 12 inches, front to back of convex contour insert 168 c 3.0 inches to 12 inches, front point of base of convex contour 166 a {fraction (1/10)}th inch to 2 inches, mid-point front side to side of convex contour 166 b {fraction (1/10)}th inch to 2 inches, apex of convex side to side 166 c {fraction (1/10)}th inch to 2 inches, mid-point side to side of back half of convex contour 166 d {fraction (1/10)}th inch to 2 inches, back point of base of convex contour 166 e {fraction (1/10)}th inch to 2 inches.
FIG. 32 is a top and side plan view of a rounded convex contour insert 170 into hoof-ware device with tri-lock interlocking mechanism 12 with a height of rounded convex contour 170 a range {fraction (1/10)}th inch to 2 inches, side to side of rounded convex contour apex 170 b range 2.5 inches to 12 inches, front to back of rounded convex contour insert 170 c range 3.0 inches to 12 inches, height front base point of rounded convex contour 172 a range {fraction (1/10)}th inch to 2 inches, height of mid-point of rounded convex contour 172 b range {fraction (1/10)}th inch to 2 inches, height of apex of rounded convex contour 172 c range {fraction (1/10)}th inch to 2 inches, mid-point height back base point of rounded convex contour 172 d range {fraction (1/10)}th inch to 2 inches, height of base point of back of rounded convex contour 172 e range {fraction (1/10)}th inch to 2 inches.
FIG. 33 is a top and side plan view of a sizing insert 174 into hoof-ware device with tri-lock interlocking mechanism 12 with a height of insert 174 a range {fraction (1/10)}th inches to 2.0 inches, exterior side to side of sizing insert 174 b 2.5 inches to 12 inches, exterior front to back of sizing insert 174 c 3.0 inches to 12 inches, exterior to interior back wall of sizing insert 174 d range ¼ inches to 1 inches, exterior to interior right side wall looking downwardly 174 e range ¼ inches to 1 inches, interior to exterior left side wall looking downwardly 174 g range ¼ inches to 1 inches, interior to exterior front wall looking downwardly 174 f range ¼ inches to 1 inches.
FIG. 34 is a top and side plan view of impression form insert 176 into hoof-ware device with tri-lock interlocking mechanism 12 , height of impression form insert 176 a range {fraction (1/10)}th inch to 2 inches, interior side to side of impression form insert 176 b range exterior walls 2.5 inches to 12 inches, interior front to back of impression form insert 176 c range exterior 3.0 inches to 12 inches, right side interior to exterior side wall of impression form insert 176 e range {fraction (1/10)} inches to 1 inch, back side interior to exterior side wall of impression form insert 176 d range {fraction (1/10)} inches to 1 inch, front side interior to exterior side wall of impression form Insert 176 f range {fraction (1/10)} inch to 1 inch, left side wall of impression form Insert 176 g range {fraction (1/10)}inches to 1 inch.
FIG. 35 is a top and side plan view of mechanical diagnostic insert 180 with tri-lock interlocking mechanism 12 with a measurement device 180 a capturing hoof data in back one-half of hoof; capture hoof data in mid-point of hoof 180 b, capture hoof data in front one-half of hoof; captured front hoof data ( 180 d ). independent data gathering module 178 device, connecting insert of module device to diagnostic insert 178 c.
FIG. 36 is a top and side plan view of x-ray/radiograph liner insert 190 into hoof-ware device with adjustable wire markers with tri-lock interlocking mechanism 12 base object for x-ray/radiograph 184 b, side vertical measuring device 186 a, width 186 b configurations vary and may be exactly the same as front vertical measuring device 186 a and width 186 b same device attaches to the non-pictured side and back side. height 188 b from top base in front to top of upper device 188 a.
FIG. 37 is a top and side plan view of electronic hoof insert into hoof-ware device with tri-lock interlocking mechanism 12 comprised of multiple combinations transistors and microprocessors, systems software programmed, applications/analyses programmed and data base driven, hard wire and wireless communications, integrated to pcs to mainframes, collecting-analyzing-decision driven data based on multiple combinations of hoof modes—diagnostics, normal use, performance, corrective, medicinal emergencies, preventative, rehabilitation environments—embodying multiple material combinations construction composites, EVA, rubber compounds, polyethylene, silicon, sorbothane, polymers, and other similar materials and/or densities—embodying one or more C scale range 1 to 100 and/or A scale range 1 to 100 and/or 0 scale range 1 to 100, fitting multiple hoof sizes.
FIG. 38 is a side view of detachable hoof-ware sole 202 , hoof-ware device 210 , sliding-channels for slide-channel device 206 , a front panel 204 with replaceable t-channel slide-locking replaceable channel mechanism 206 with hoof-ware device slide of multiple sizes and shapes conforming to hoof-ware device, fitting multiple combinations hoof mode environments—diagnostics, normal use, performance, corrective, medicinal, emergencies, preventative, rehabilitation—embodying multiple combinations materials construction—composites, EVA. rubber compounds, polyethylene, silicon, sorbothane, polymers, and other similar materials and/or densities embodying one or more C scale ranges 1 to 100 and/or A scale range 1 to 100 and/or D scale range 1 to 100—fitting multiple hoof sizes.
FIG. 39 is a side view of adjustable level position insert 216 device into hoof-ware devices with tri-lock interlocking mechanism and/or self-locking devices 212 , with minimum of 18 upward-downward, side-to-side, slant-to-slant adjustment devices 214 designed to accommodate minimum of 18 combinations of hoof locations subject to changing and/or combinations of mode environments—diagnostics, normal use, performance, corrective, medicinal emergencies, preventative, rehabilitation—embodying multiple combinations of materials construction—composites, EVA, rubber compounds, polyethylene, silicon, sorbothane, polymers, and other similar materials and/or densities embodying—one or more C scale range 1 to 100 and/or A scale range 1 to 100 and/or 0 scale range 1 to 100, fitting multiple hoof sizes.
FIG. 40 is a side view of liner sleeve sock 220 fitted in and/or over hoof and/or into hoof-ware devices 218 , elasticized for snug fitting 222 , constructed from liquid shedding materials and/or liquid absorbing materials, changing combinations of mode environments—diagnostics, normal use, performance, corrective, medicinal emergencies, preventative, rehabilitation—size fitting all hooves.
FIG. 41 is a side view of an alternative embodiment hoof-ware device showing similar qualities as FIG. 1 and FIG. 42, and other previously descended hoof-ware art, and as taught by the present invention with attachment system 234 , sole 4 connected molded to mid-sole 2 , attached to upper neoprene 8 contoured back 128 , connected to upper leather trim 70 , power frame 224 with dotted lines showing non-open view attached to mid-sole 2 and sole 4 and protruding upwardly on front hoof wall with attached hook and loop 116 attached to outside of power frame 224 material, front hoof wall cover device 228 is attached to front mid-sole 2 opened widely in front of hoof-ware device and closed tightly over power frame attached to upper back with metal/plastic zipper 230 , further closed tightly with single and/or combination metal or plastic quick release bratchet/zipper type buckle attachment 232 that is easily releasable, adjustable and/or ratcheted, connects front hoof wall cover 228 to back strap device 234 .
FIG. 42 is a side view of the hoof-ware device showing sole 4 , connected to, the mid-sole 2 , attached to the upper 6 with a trim line 122 , attached to the back 8 , attached to the back contoured heel cover 128 , attached to the upper leather and like materials as upper trim 70 , inwardly showing reinforced power frame 224 pulling up over the front hoof wall, connected by hook and loop 116 attachment, connected to the back stretchy neoprene material 8 , pultruding from the inside pulled outwardly and outside pulled inwardly and/or vice versa as a hook and loop stretch strap ( 226 ) wrapping around hoof wall from the outside and/or inside and/or vice versa.
In addition, the equine lightweight versatile hoof-ware 10 comprising an upper 6 , a mid-sole 2 , a sole 4 , embodying multiple inserts is provided. The hoof-ware sole 4 embodying multiple rubber compounds and/or poly/urethane. The hoof-ware 10 is capable of multiple ground engaging equine compression surface configurations including multiple soft, tough, uniquely spaced and integrally formed designs calibrated to equine breeds pointed downwardly below bottom surface of sole 4 , wherein said designs. when compressed, will absorb and/or cushion all and/or partial equine impacts during all ground engagements in all healthy environments, said designs fit multiple equine breed's total environment.
Further the sole 4 is uniquely bonded to the mid-sole 2 , hoof-ware mid-sole 2 having multiple configurations of polyurethanes, EVA/foam composites, rubber compounds, polyethylenes, silicones, sorbothane, polymers, and other similar materials embodied to flex, cushion, absorb partial and/or all shocks and equine impacts in all ground engagements in all earthly environments.
The hoof-ware upper 6 is uniquely bonded and attached to mid-sole 2 and sole 4 , mid-sole 2 comprising multiple stretch and non-stretch fabrics, leathers, embodied wear and/or weather resistant materials designed for all equine environments. The upper embodiments further comprising multiple materials with multiple attachment devices designed for all equine earthly environments.
Moreover, the hoof-ware 10 is configured to embody multiple inserts including, but not limited to normal use, medicinal, correction, rehabilitation, emergencies, performance, and/or preventative. The inserts further embodying all equine hoof related diseases, symptoms and/or lameness designed for: partial and/or all configurations involved in all equine earthly environments. The hoof-ware 10 and/or inserts and/or used together size range is miniature (3 inches front to back. 2.5 inches side to side at mid-point). pony. 000. 00. 0, 1, 2,3,4,5,6,7,8,9,10, 11,12 (12 inches front to back, 12 inches side to side at mid-point), 13, 14.
The hoof-ware configuration, combination and integration of equine hoof-ware device embodying insert devices for purposes of diagnostics, performance, correction, medicinal, emergencies, preventative, rehabilitation and or normal use. Multiple configurations are provided of inserts embodying multiple compounds, densities, cut outs, convex and concave contours, perforations, sizes, add-ons. In addition, inserts are provided, such inserts embodying multiple mechanical devices to comprehensively measure, diagnose, analyze equine hoof configurations. Further, inserts embodying multiple x-ray devices to comprehensively measure, diagnose, analyze equine hoof configurations. In addition, inserts embodying multiple electronic devices to comprehensively measure, diagnose, analyze equine hoof configurations. Moreover, inserts embodying multiple movements of same insert, up and down, side to side. slant to slant. are also provided.
In use and operation, and referring to the drawings, a hoof is to be received within a boot, as shown in FIG. 1, and the hoof is fastened into the boot for ultimate comfort and fit by means of extensions. These extensions wrap and secure the hoof in place and are fastened to at least one fastener which may be located for example at the forward region of the boot. Inserts are also provided in a multitude of designs, shapes, thicknesses, dimensions and material of construction to provide interchangeable inserts such that the boot is not only comfortable and well fitting, but serves many different equine functions. Succinctly, the inserts are used to make the boot acceptable for use for medical purposes, comfort, balance, and protection. Moreover, the hoof-ware of the present invention can be used in many and all environments into an equine may be exposed. Finally, the interchangeable inserts are changed by the equine owner or caretaker such that one boot may be used for multiple sizes of hooves, and many purposes and functions of the equine.
Moreover, having thus described the invention, it should be apparent that numerous modifications and adaptations may be resorted to without departing from the scope and fair meaning of the present invention as set forth hereinabove and as described hereinbelow by the claims.
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The present invention relates generally to a comfort management system for equine and, in particular, to a multi-purpose, multi-functional hoof-ware device, boot or shoe and multiple, interchangeable inserts for all equine hooves that uses, attaches, wraps, and fits the hoof while the equine is stalled, walking, trotting, loping for the purposes of protection, healing, alignment. cushioning and/or any other medicinal purposes for any given period of time fitting all sizes of equine hooves in multiple hoof environments, such as, diagnostics, normal use, during and after performance, corrective, medicinal purposes, emergencies situations, for preventative purposes, and rehabilitation of the hoof.
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TECHNICAL FIELD
[0001] The present invention relates to reinforcing the wood roof structures of existing houses and similar low-rise buildings against wind uplift by means of a retrofitting method and apparatus for securing roof frames to walls without having to remove roofing/sheathing.
BACKGROUND OF THE INVENTION
[0002] While today's steel strap connectors excel for new construction of houses and like small buildings for securing wood roof structures to their supporting walls, they are not readily applicable to retrofitting existing structures. Such strap “ties” or “tie-downs” should have an upper portion extending over the top of a roof frame (rafter or truss) to ensure adequate tie-down strength by applying much of the restraining force onto the top of the roof frame as compression across the grain, which wood withstands quite well. If the tie-down connectors are simply nailed into the side of the roof frame—as commonly done until recent years—localized tensions are induced across the grain of the wood during nailing or especially under load, such that the rafter/truss member tends to split under hurricane-force uplifts, releasing the tie-downs' nails too easily—often much before the “design load” is reached.
[0003] The over-the-top or “wrap over” tie-down method is now widely recommended or required in the US Hurricane Belt for new construction, and even for retrofits of existing buildings. It's easily done in new construction: the roof frame and supporting wall is entirely accessible before the roof sheathing is applied. During retrofitting, however, accessing the top portion of the rafter/truss requires removal and re-installation of an area of roofing and sheathing; such a laborious and costly operation discourages such retrofit upgrading of existing housing and building stock altogether, leaving the stock needlessly vulnerable.
[0004] There have been recent efforts to devise methods for retrofit reinforcement of wood roof structures. Some steel tie-down examples simply provide more area aligned with the roof slope to allow insertion of more nails through the strap and into the side of the rafter/truss, but that can exacerbate splitting under load (and indeed the very act of crowding nails into the ultra-dry wood encountered in existing houses is seen to cause especially extensive splitting, even “shredding”).
[0005] Considerable older retrofit thinking does try to avoid such splitting. In U.S. Pat. No. 5,257,483 Netek discloses ways of installing anchor points in roof fascias and the wall surfaces below, allowing temporary placement of ties in the event of an impending storm. Winger, in U.S. Pat. No. 5,319,816, and several other inventors, disclose other temporary arrangements using multiple cables or nets over the roof which are anchored to the ground. Such temporary devices demand that the householder be at home and ready to react to storm warnings. In U.S. Pat. No. 5,311,708, Frye shows a retrofit roof tie-down method in which lag screws are installed upwardly through an angled steel plate into the bottom edge of the rafters/trusses, but costs and load transfer distortions are problematic.
[0006] Accordingly, I have devised and tested a “slant toggle” tie down (U.S. Pat. No. 7,562,494 Jul. 21, 2009), which involves drilling a hole slantingly upwards through the roof frame so that a tie can run through to emerge near the top, just under the sheathing, and be there secured to restrain the roof frame against upward movement. That, however, involves precisely angled drilling from below and awkward insertion of a clip just under the sheathing. Therefore I devised and tested a “claw” device, slope-adjustable, featuring a sharp-edged top flange hammered into the interface between frame and sheathing to apply its restraining force top-down on the roof frame (U.S. patent application Ser. No. 12/607,154, Oct. 28, 2009). That claw device proves difficult to insert in some cases, however, and is intrinsically somewhat costly. The need remained clear: devise a better retrofit over-the-top tie-down method and apparatus to upgrade existing buildings to the strength achieved by applying over-the-top strap ties in new construction.
[0007] The concept in this invention is to force the sheathing just a little off the roof frame, allowing over-the-top insertion of a tie-down strap much as practiced in new construction. It's neither an obvious nor readily practicable approach: Any kind of sledging or hammering the sheathing upward tends to puncture or smash it and/or lift it off too much, the latter itself leaving it unacceptably bulged upward and perhaps with a significantly large area poorly fastened to the roof framing. On the other hand, trying to pry or wedge the sheathing up by driving say a broad chisel between it and the top edge of the roof frame roof involves awkward and misaligned driving (the sheathing interfering with the chisel's proper stance—and sheathing and neighboring rafters/trusses interfering with a hammer's swing), and even if somehow doable can cut into the roof sheathing or roof frame or hit a roofing nail.
SUMMARY OF THE INVENTION
[0008] A method and apparatus is provided for reinforcing the connection of an existing roof frame to a wall or like structure below it, which comprises a) lifting just a small area of the roof sheathing off the roof frame just sufficiently to allow b) inserting a head end of a tie-down strap (the strap) into the gap on one side of the roof frame and completely inward over the frame's top edge, and with the lifting means and amount reliably set to avoid damage to sheathing or frame or the hold of one to the other; then c) pushing the head end of the strap further to protrude beyond the top far edge of the roof frame sufficiently to allow d) bending the protruding portion of the strap tightly down over the far edge and onto the far side of the roof frame far enough to accept sound fastening there; and finally e) driving fasteners such as nails or screws through that bent-down portion of the strap and into the far side of the roof frame, so that the strap itself (when its tail is fastened in prior-art manner on the near side of the roof frame too, and secured to the wall below) must apply much of its restraining force downward into the top of the roof frame, so that wood splitting forces are minimized and any such splitting during installation or under uplift load will have minimal weakening effect on the strap's restraining strength.
[0009] It will be clear that the strap itself should differ from prior art straps, in that its head end should be angled flatwise outward from the main axis of the rest of the strap so that when protruding beyond the top far edge of the roof frame and bent downward it is oriented outward, despite the usual slope of the top of the roof frame, and so remains outboard of any potentially interfering framing (such as common “blocking” between roof frames) and is accessible for fastening operations such as nailing or screwing into the far side of the roof frame.
[0010] It will be clear that the strap itself should differ from prior art straps, in that its head end should be angled flatwise outward from the main axis of the rest of the strap so that when protruding beyond the top far edge of the roof frame and bent downward it is oriented outward, despite the usual slope of the top of the roof frame, and so remains outboard of any potentially interfering framing (such as common “blocking” between roof frames) and is accessible for fastening operations such as nailing or screwing into the far side of the roof frame.
[0011] In accordance with one embodiment of the present invention, the lifting of the roof sheathing off the roof frame is accomplished by driving a sharp-pointed wedge squarely into the interface between the top of the roof frame and the underside of the roof sheathing and then across much of said top, preferably using a worm gear or ratchet type of drive, the wedge and drive being mounted in a horizontally oriented bar (hereinafter the device being named the “bar wedge”), which bar is adjustably fitted between that roof frame and the next with its opposing end restrained by the near side of the next roof frame; whereby the driving of the wedge of a certain thickness lifts the roof sheathing to provide just a sufficient gap off the roof frame's top alongside the wedge to allow full insertion and thence deployment of the over-the-top tie-down strap.
[0012] There being many sheathing nails and some roofing nails intruding through the roof sheathing into the top of the roof frame, with perhaps a 1 : 8 chance of one happening to intrude into the path of the advancing wedge across the top of the roof frame, a means of evading such an obstruction is provided according to the invention by having the point and head end portion of the wedge divided into at least two prongs, each prong being pointed so that even if one hits the nail the wedge need only sidestep slightly as it proceeds across the top of the roof frame, the nail being accommodated between prongs or alongside the wedge.
[0013] In a second embodiment of the present invention, called the U-wedge, the lifting of the roof sheathing off the roof frame is accomplished by positioning a first wedge squarely against the first side and a second wedge squarely against the opposite side of the roof frame, the two wedges being directed toward each other into the interface between the top of the roof frame and the underside of the roof sheathing, each wedge being equipped with a worm gear or ratchet type of drive and each such assembly being integrally mounted on a vertical arm of a U frame which fits up over the sides of the roof frame from below to provide exact positioning and restraint for the wedges; thence driving both wedges into that interface toward each other with each being capable of advancing across much of the top of the roof frame, so that if an obstructing sheathing or roofing nail brings one wedge to a premature stop the other wedge can continue being driven toward the stopped wedge across the remaining top of the roof frame until that other wedge is also stopped by the nail, the wedges then intruding across almost all of the top of the roof frame and just sufficiently lifting the roof sheathing therefrom.
[0014] In a further embodiment of the invention the lifting of the roof sheathing off the roof frame is accomplished by positioning a lever assembly near one side of the roof frame where it crosses the supporting wall, and preferably a second lever assembly near the other side of the roof frame, each such lever assembly having a fulcrum seated solidly on the supporting wall near its exterior surface or on the blocking often present atop that wall, a short load arm projecting inward from that fulcrum to a lifting end set against the underside of the roof sheathing, and a long effort arm extending outward, whereby pushing down on the lever's effort arm exerts a multiplied force upwards at the lifting end against the underside of the roof sheathing to force the roof sheathing off the roof frame just the amount needed for passage of the tie-down strap. Excessive lifting is prevented by the downswing arc of the lever's effort arm being limited by the wall's exterior surface below, the short length of the lever's load arm and the shape of the lever's load tip being such that said limited downswing can only lift the load tip a desired amount.
[0015] These and other features and advantages of the present invention, my “Strapeze™” invention, will be better understood with reference to preferred embodiments described hereinafter.
BRIEF DESCRIPTION OF THE DRAWINGS
[0016] Reference will now be made to the accompanying drawings showing by way of illustration preferred embodiments of the present invention, each being a method/device for lifting a small area of roof sheathing slightly off the top of a roof frame in a controlled, practicable manner.
[0017] FIG. 1 is a front elevational view of a bar wedge device placed horizontally between roof frames and with its top surface against the underside of the roof sheathing.
[0018] FIG. 2 is a partial front elevational view of the operative wedge portion of the bar wedge with cutouts showing the driving gear inside, the wedge itself being in its retracted position.
[0019] FIG. 3 is a partial front elevational view of the operative wedge portion of the bar wedge with cutouts showing the driving gear inside, the wedge extended.
[0020] FIG. 4 is a plan view of the wedge divided into two prongs to enable it to to sidestep an obstructive nail.
[0021] FIG. 5 is a partial side elevational section of a wedge driven under the roof sheathing, showing the gap made between the top of the roof frame and the sheathing with a tie-down strap using that gap.
[0022] FIG. 6 is a side elevational view of a lever assembly in place in the typical case where a blocking is present between roof frames.
[0023] FIG. 7 is a front elevational view of a fulcrum plate for the lever assembly.
[0024] FIG. 8 shows cross sections of a lever bar.
[0025] FIG. 9 is a perspective view of a pair of lever bars connected for convenient use together.
[0026] FIG. 10 is a side elevational view of a lever assembly in place in a common case where there's no blocking between roof frames.
[0027] FIG. 11 is a front elevational view of a U wedge device pushed up over a roof frame.
[0028] FIG. 12 is a perspective view of the operative wedge portion of the U wedge device mounted on one vertical arm of the U-bar.
[0029] FIG. 13 shows various views of a tie-down strap and the roof frame with the leading end of the tie-down strap formed at an angle to one side to avoid interference from blocking and roof sheathing when being fastened to the far side of the roof frame.
DETAILED DESCRIPTION OF PREFERRED EMBODIMENTS
[0030] First, FIGS. 1 to 5 illustrate the bar wedge device held up against the underside of the sheathing and directing the wedge tip straight into the interface between sheathing and the top of the roof frame.
[0031] In FIG. 1 , a side elevation of the bar wedge device is shown ready to work, with the wedge 1 poised with its tip at the interface between a left side roof frame 9 and the roof sheathing 10 . A driving device 2 is set in the backbone 4 of the wedge. The handle 4 a is useful for setting the device at ready, while a telescoping extension 5 is approximately adjusted by means of setting a pin in the group of holes 6 and more finely 7 , while a cam or gear adjuster 8 pushes teeth into the right side roof frame 9 .
[0032] FIG. 2 is a side elevation of just the front end of the bar wedge device, showing the wedge 1 (still retracted) connected to a worm gear drive 2 b and 2 by means of a traveler 3 , ready for operation by means of a crank (not shown) which drives the worm gear and traveler by turning the worm gear 2 through the receptacle 2 a.
[0033] In FIG. 3 , the wedge 1 is shown driven forward by the traveler 3 pushed by the worm gear 2 and 2 a, so that the wedge would now be fully extended over the top of the roof frame to force up the roof sheathing (not shown), while the other end of the bar wedge would push against the right side roof frame (not shown). Section AA shows the cross section of the bar 4 , shaped to guide the driving end of the sliding wedge 1 . (Once the strap has been inserted, as in FIG. 5 , the wedge can be withdrawn by the traveler 3 on the worm gear 2 and 2 a; this retraction also takes considerable force.)
[0034] FIG. 4 shows a preferred design of the wedge 1 , illustrating the two-prong forked wedge with each prong pointed. This forked and pointed design comes crucially into play whenever the advancing wedge hits a sheathing nail (which will happen often, such nails generally being driven into the roof frame only 10 or 15 cm. apart). A prong hitting a nail will force the advancing wedge to move slightly sideways (also the end of the bar 4 of course, FIGS. 2 and 3 —which bar end moves easily sideways since it's being pushed away from the roof frame being wedged). The wedge can thereby advance past the nail with the nail to one side or in the gap between the prongs; thus the wedge's sideways movement need never exceed half the width of one prong (typically being less than 1 cm. sideways). The sections A-A, B-B and C-C show how the wedge's edge shape facilitates sidewise sliding as the wedge moves forward; neither sheathing nor roof frame is cut by the motion and the forces are moderate. Section D-D shows how the wedge's pushed end is shaped to fit into and be securely guided by the bar's section A-A of FIG. 3 .
[0035] FIG. 5 is a sketch of the wedge 1 fully engaged, showing the wedged-open gap allowing insertion of a tie-down strap on either side of the wedge. The dashed lines 11 indicate where the strap might preferably be located. The driving worm gear 2 is engaged by a power driver or hand crank 2 c, all angled downward for easy operation. Once the strap is inserted—with no need to wait for it to be fastened—the drive train 2 c and 2 is operated in reverse to retract the wedge and move the bar wedge device to the next roof frame position. The sheathing's remaining “bulge” of about 3 mm or less is not visible on the generally shingled surface above, nor is there significant weakening of the sheathing's hold-down to the roof frame.
[0036] Next, FIGS. 6 to 9 illustrate a lever device with a fulcrum assembly resting on the top of the “blocking” generally affixed atop the wall between roof frames.
[0037] In FIG. 6 , TP is wall top plate on which a wood blocking member B is set, in general practice, fixed between roof frames R/T (rafter or truss) at each end, and sized to leave a certain vent gap between the top of blocking B and the underside of the roof sheathing S. A lever 12 has been inserted into the venting space to bear on the top of a fulcrum assembly 13 which has been seated on the blocking B, so that pushing downward (arrow) on the lever's effort arm 12 a causes the load tip 12 b to push upward against the underside of the roof sheathing S. That push is transferred by way of a bearing pad 12 d, which pad (affixed to the lever's load tip 12 b by a pin 12 c ) acts as a “load spreader” allowing great force upwards on the roof sheathing S without unduly stressing it in compression across the grain. The roof sheathing S is thereby forced off the frame R/T, with the resulting gap 14 allowing insertion and adjustment of a tie-down strap 11 (dashed line) over the top edge of the frame R/T.
[0038] Preferably two such lever setups are used for each such sheathing lift, with a fulcrum assembly 13 set alongside each side of an R/T and with a pair of lever bars lifting the sheathing at both points simultaneously, as noted below.
[0039] The lever device lifts the roof sheathing just enough to allow passage of a tie down strap over the top of the roof frame, as follows: The fulcrum assembly 13 is adjusted so that the actual fulcrum (the top of the plate 13 a ) is a certain distance below the underside of the roof sheathing S (a distance preferably set by “horns” 13 d, as shown below); the geometry is such that the lever's load tip 12 b can lift the pad 12 d just a certain amount, no more, as the lever's effort arm is pushed down through the available arc which is limited by the wall below; further, when the lever bar is tilted down past a certain angle it will simply slide downward across the fulcrum, friction being overcome. It can be shown that such controlled lifting is obtained, creating the correct gap 14 , with a range of roof slopes from flat to say 7:12 slope. Almost all roofs in “hurricane country” are sloped within this range. Moreover, where steeper slopes are encountered the typical side-nailed straps generally suffice even for retrofit purposes, the force on their nails or screws being more aligned with the grain of the wood and much less likely to cause splitting under load—so lifting for over-the-top tie straps is not needed.
[0040] FIG. 7 is a front elevational view of the fulcrum plate 13 a, showing one or perhaps two protruding “horns” 13 d which set its closeness to the roof sheathing, and the slot 13 f which allows such adjustment.
[0041] In FIG. 8 , cross sections are shown of the lever bar 12 a and its load tip 12 b, the latter having small pins 12 c ready to hold onto the pad 12 d (as seen in FIG. 6 ), which pad has one side 12 e attached by a screw as shown, in this embodiment, so that the side 12 e can be attached to secure the pad 12 d to the lever's load tip 12 b.
[0042] FIG. 9 shows a preferred paired arrangement wherein two lever setups are operated as one, joined as shown by a member 12 f. As noted above, one fulcrum 13 is seated close by one side of a roof frame, a second fulcrum close by the other side of same, so that the paired lever setups can simultaneously apply lifting force against the roof sheathing at each such side, to lift effectively with least strain on the roof sheathing. The sheathing's “plate action” helps form a smoothly arched lift (gap 14 in FIG. 6 ).
[0043] Testing has shown that both the wedge and lever devices work well to lift roof sheathing off a roof frame, whether the roof sheathing is formed of wood boards as in older houses or of modern plywood. The recent OSB forms (Oriented Strand Board) have not been tested but they're generally found in the “hurricane belt” only in newer houses already using “wrap over” tie down straps.
[0044] The two distinct “Strapeze™” devices, the wedge and the lever, should be discussed further at this point.
[0045] The wedge can be placed between two adjacent R/Ts close to the wall line, but also 1) farther outboard where appropriate for certain types of tie-down straps. Not so with the lever. Conversely, the wedge is usable where roof frames are normally spaced apart (from 16″ o.c. to 24″ o.c., generally) but not where close together (e.g. where three in a group offer no space of at least 16″ o.c. on either side of the middle one requiring retrofit tie-down). Many houses have at least one such condition. There, the lever would be needed. (Skipping retrofitting of just one of such close-together R/Ts would often be acceptable engineering-wise, real-world-wise . . . but not likely to the eyes of an inspector or the letter of a building code, where acceptability and simple physics may not be related.) Further, the wedge might be somewhat awkward to handle and use on a scaffold, and perhaps a little slow in operation.
[0046] FIG. 10 illustrates the lever apparatus adapted for the common case where there's no blocking between roof frames atop the wall. Here the fulcrum 13 a′ is formed of two plates adjustably fixed together to extend from the underside of the roof sheathing S to the wall top TP, regardless of the height of the (typical) roof frame. The bottom edge of the fulcrum plates 13 a ′ is set on and pulled forward on the base plate 13 b ′ atop the wall plate TP, but clearly the base plate 13 b ′ does not itself hold the fulcrum plate 13 a ′ upright. Therefore the uppermost plate in this case is formed with two horns 13 d ′(as better depicted in FIG. 7 , 13 d ), and their points are serrated so as to bite into the underside of the roof sheathing until lifting begins. In a further variation from the lever assembly of FIGS. 6 and 7 , the underside of the load tip 12 b ′ is here so shaped or fitted with a spring-like keeper that, once the roof sheathing is forced off the horns 13 d ′ the shape or keeper of the load tip 12 b ′ restrains the top of the fulcrum plates 13 a ′ from falling inward, the lever's load tip itself being set forcefully against the underside of the roof sheathing S during the lifting.
[0047] FIG. 11 is a side elevation of a “U Wedge” embodiment of the invention, complementary to or replacing the wedge of FIGS. 1-6 and the lever of FIGS. 7-9 . It enables retrofit-strapping of even close-together roof frames—whether or not they have blocking between them. (Being similar in its operating parts to the wedge, the U Wedge parts are here numbered similarly, differentiated only by the prime symbol.) Two wedges 1 ′ are forced by worm gear drives 2 ′ into the interface between a roof frame 9 ′ and a roof sheathing 10 ′, one wedge driven from one side of the frame 9 ′ and one from the other side, the driving gear 2 ′ being supported by a rigid clamp-like U-piece 4 ′ which is positioned to surround the roof frame 9 ′.
[0048] Where the wedge uses narrow prongs to allow it to move past a sheathing nail—requiring some sidewise movement—the U Wedge need not: An advancing wedge hitting a nail (the left one in this sketch) simply stops, the extra resistance being sensed by the installer, while the opposing wedge is driven further across until hitting the same nail from the other side or simply until completing the lifting of the roof sheathing. (Nails may be encountered often enough, as noted earlier, but never more than one in any one wedge path.)
[0049] FIG. 12 is an exploded perspective of one operative portion of the U Wedge, right hand side, where the U-piece 4 ′ is shown supporting the worm gear 2 ′ and the guide 15 for the wedge 1 ′, which is shown ready for insertion into the guide 15 . As in the wedge, the traveler 3 ′ is driven forward or retracted by the drive 2 b ′ (dashed line, not yet installed). The traveler 3 ′ in turn drives the wedge 1 ′ (attached to it by means of the screws 16 installed in the holes 16 ′, in this example).
[0050] Whereas the bar wedge can be placed to fit against any normal roof slope, the U Wedge must itself be positioned more or less vertically, so its wedges must rotate to fit into the interface between roof sheathing and sloping roof frames. Accordingly, the guide 15 is mounted on the U-piece 4 ′ by means of the drive 2 b ′ through the holes 17 , thus being freely hinged to rotate when pressed against the underside of the roof sheathing (not shown here). The rotation is here limited by the end protusion 18 and similar shelf 18 ′.
[0051] In FIG. 13 , final aspects of over-the-top (“wrap-over”) retrofitting are addressed. First, it can be seen in FIGS. 13A and B (looking straight down on the roof frame, in B, with the wall plane indicated below the strap), that the off-side portion of a conventional tie down strap becomes positioned inboard of the wall plane, which is fine in new construction because the roof sheathing is not yet in place and there's lots of room for bending the strap down and driving fasteners there. In our retrofitting operation, however, the roof sheathing is in the way, and there's often blocking interfering too. Accordingly, the tie down strap should feature a diverted end portion 19 , FIG. 13C , to ensure that the inserted wrap over offers its end outboard of the wall plane. (The faint lines beside the strap end 19 are intended only to show that such angled strap can still be punched out of flat metal, with very little waste.) In FIG. 13D (again looking straight down on the roof frame) it can be seen that the diverted “wrap-over” 19 of the tie-down strap is directed outward from the wall plane and the blocking B, thus being accessible for fastening.
[0052] Finally, in any such retrofitting, the strap's tail cannot readily be anchored to the wall's framing (as often so easily done in new construction, as seen in FIG. 12A ), but must lap down over and be fastened onto whatever forms the outer face of the top portion of the wall. Where that face is a plywood sheathing, say, fully adequate fastening can readily be done. Where there's no such strong sheathing present, a Top Band™ of plywood can first be installed around the house perimeter, itself nailed solidly into the wall framing underneath, and ready to hold the strap's nailing securely and transfer the uplift forces rather directly into the house framing. Such a Top Band could simply be ⅝ in. thick by 8-12 in. wide fir plywood, for example, and all of this work would be hidden when the soffit panels are replaced on the greatly strengthened house.
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It's now accepted that hurricane tie-down straps should be wrapped over the top of rafters/trusses, avoiding the crucial weakening effect of wood splitting around the nails of common side-nailed straps. That “wrap-over” is easy to do during construction but has been difficult and costly to do for existing houses, where the sheathing and roofing is in the way. But now such wrap-over can be an easy retrofit, according to this invention: Without damaging sheathing or roofing, force the sheathing off the rafter/truss just enough to allow a special strap to be pushed through the gap, then proceed much as in new construction. Unique wedge-blade and lever types of devices quickly create just the right gaps.
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CROSS-REFERENCE TO RELATED APPLICATIONS
[0001] This is a continuation application of pending U.S. patent application Ser. No. 11/855,822, filed on Sep. 14, 2007, which is a continuation application of U.S. patent application Ser. No. 11/680,658, filed on Mar. 1, 2007, now U.S. Pat. No. 7,292,688, issued Nov. 6, 2007, which is a continuation application of U.S. patent application Ser. No. 11/342,880, filed on Jan. 31, 2006, now U.S. Pat. No. 7,203,302, issued Apr. 10, 2007, which is a continuation application of U.S. patent application Ser. No. 10/789,977, filed on Mar. 2, 2004, now U.S. Pat. No. 7,054,432, issued May 30, 2006, which is a continuation application of U.S. patent application Ser. No. 10/388,635, filed on Mar. 17, 2003, now U.S. Pat. No. 6,724,882, issued Apr. 20, 2004, which is a continuation application of U.S. patent application Ser. No. 09/977,697, filed on Oct. 16, 2001, now U.S. Pat. No. 6,563,917, issued May 13, 2003; which is a continuation application of U.S. patent application Ser. No. 09/207,275, filed on Dec. 8, 1998, now U.S. Pat. No. 6,330,324, issued Dec. 11, 2001, which claims the benefit of U.S. Provisional Application No. 60/069,114, filed on Dec. 9, 1997, the contents of which are expressly incorporated by reference herein in their entireties.
1. FIELD OF THE INVENTION
[0002] The present invention generally relates to systems for routing telephone calls to appropriate numbers. More particularly, the present invention relates to an Advanced Intelligent Network (AIN) based system and methods for routing telephone calls based on the location of the calling party.
2. ACRONYMS
[0003] The written description provided herein contains acronyms which refer to various communication services and system components. Although known, use of several of these acronyms is not strictly standardized in the art. For purposes of the written description herein, acronyms will be defined as follows:
AIN—Advanced Intelligent Network AMA—Automatic Message Accounting CCIS—Common Channel Interoffice Signaling CO—Central Office CPN—Calling Party Number CPR—Call Processing Record DN—Dialed Number Trigger DRS—Data Reporting System EO—End Office (EO) ISCP—Integrated Service Control Point LSP—Local Service Provider NPA—Number Plan Area, i.e., area code NXX—Central Office Code RTN—Routing Telephone Number SCE—Service Creation Environment SCP—Service Control Point SCCP—Signaling Connection Control Part SMS—Service Management System SPC—Signaling Point Code SS7—Signaling System 7 SSP—Service Switching Point STP—Signaling Transfer Point TAT—Terminating Attempt Trigger TCAP—Transaction Capabilities Applications Protocol
3. DESCRIPTION OF THE RELATED ART
[0028] In recent years, a number of new telephone service features have been provided by advanced intelligent communications networks such as an Advanced Intelligent Network (AIN). The AIN evolved out of a need to increase the capabilities of the telephone network architecture to meet the growing needs of telephone service customers. The AIN architecture generally comprises two networks, a data messaging network and a trunked communications network. The trunked communications network handles voice and data communications between dispersed network locations, whereas the data messaging network is provided for controlling operations of the trunked communications network.
[0029] An illustration of the basic components of an AIN architecture is shown in FIG. 1 . As shown in FIG. 1 , Central Offices (CO) 10 - 16 are provided for sending and receiving data messages from an Integrated Service Control Point (ISCP) 20 via a Signaling Transfer Point (STP) 30 - 34 . The data messages are communicated to and from the COs 10 - 16 and the ISCP 20 along a Common Channel Inter-Office Signaling (CCIS) network 22 . Each CO 10 - 16 serves as a network Service Switching Point (SSP) to route telephone calls between a calling station (e.g., station 40 ) and a called station (e.g., station 48 ) through the trunked communications network 24 - 26 . For more information regarding AIN, see Berman, Roger K., and Brewster, John H., “Perspectives on the AIN Architecture,” IEEE Communications Magazine, February 1992, pp. 27-32, the disclosure of which is expressly incorporated herein by reference in its entirety.
[0030] While prior AIN or AIN-type intelligent network applications may have provided various features to subscribers and users, these prior applications do not allow users to dial one telephone number and reach a single point of contact for multiple services provided by a subscriber. Current systems and methods require users to identify one of many possible numbers to call depending on the specific information or service desired from the subscriber. This requires users to know the telephone number of all departments or service groups of the subscriber that they need information from.
[0031] Moreover, none of the current systems and methods allow a user to dial an abbreviated telephone number to access services from a subscriber. Currently, the user must lookup, write down, or memorize a full seven or more digit number for each department or service group that they may need information from.
[0032] Therefore, a system and method is needed that allows users to dial one telephone number and reach a single point of contact for Information and services provided by a subscriber, and that provides an abbreviated telephone number that is easy to remember for accessing the single point of contact for services from the subscriber.
SUMMARY OF THE INVENTION
[0033] Accordingly, the present invention is directed to a system and method for geographical call routing for a non-emergency calling service that substantially obviates one or more of the problems arising from the limitations and disadvantages of the related art.
[0034] It is an object of the present invention to provide an AIN system and method that routs calls to a non-emergency service based on the geographical location of the caller.
[0035] It is also an object of the present invention to provide an AIN system and method that allows users to dial one telephone number and reach a single point of contact for services provided by a subscriber.
[0036] It is a further object of the present invention to provide an AIN system and method that allows users to dial an abbreviated telephone number that is easy to remember for accessing a single point of contact for services from a subscriber.
[0037] Accordingly, one aspect of the present invention is directed to an advanced intelligent communications system for routing telephone calls based on the location of a calling party, The system includes: a plurality of call origination telephones; at least one switching device operatively connected to at least one of the plurality of call origination telephones, the at least one switching device servicing calls placed by at least one calling party using one of the plurality of call origination telephones; a processor operatively connected to the at least one switching device, the processor determining routing of the calls placed by the at least one calling party; a storage device operatively connected to the processor, the storage device containing location information related to the at least one calling party; and at least one destination telephone operatively connected to at least one of the at least one switching device, wherein the processor sends routing information to the at least one switching device for routing calls to one of the at least one destination telephone and a terminating announcement, based on the location of the at least one calling party.
[0038] According to another aspect of the present invention, each at least one switching device has an associated signaling point code that is used by the processor to determine the location of the at least one calling party relative to a defined service area.
[0039] According to yet another aspect of the present invention, the signaling point code indicates whether the at least one switching device services only calls within the defined service area.
[0040] According to a further aspect of the present invention, the signaling point code indicates whether the at least one switching device services calls both within the defined service area and outside of the defined area.
[0041] According to another aspect of the present invention, each signaling point code that indicates whether the at least one switching device services only calls within the defined service area, has an associated call routing telephone number.
[0042] According to yet another aspect of the present invention, the storage device contains information mapping the signaling point codes to the associated call routing telephone number for the at least one switching device that services only calls within the defined service area.
[0043] According to a further aspect of the present invention, for the signaling point codes that indicate the at least one switching device does not service any calls within the defined service area, the processor sends routing information to the at least one switching device to route the call to the terminating announcement.
[0044] According to another aspect of the present invention, the storage device contains information indicating whether the signaling point codes represent switching devices that service telephones within the service area.
[0045] According to yet another aspect of the present invention, the storage device contains information indicating whether the signaling point codes represent switching devices that service telephones both in the service area and outside the service area.
[0046] According to a further aspect of the present invention, the storage device contains information mapping telephone numbers of the at least one calling party to associated zip codes.
[0047] According to another aspect of the present invention, the storage device contains information mapping the associated zip codes to call routing telephone numbers.
[0048] According to yet another aspect of the present invention, information regarding the processing of the calls placed by the at least one calling party is recorded.
[0049] According to a further aspect of the present invention, a report generator generates reports based on the information recorded.
[0050] According to another aspect of the present invention, the calls placed by the at least one calling party are to an abbreviated telephone number comprising three digits.
[0051] According to yet another aspect of the present invention, the calls placed by the at least one calling party are to “1” plus an abbreviated telephone number comprising three digits.
[0052] According to a further aspect of the present invention, the calls placed by the at least one calling party are to “0” plus an abbreviated telephone number comprising three digits.
[0053] According to another aspect of the present invention, the defined service area comprises multiple service areas.
[0054] According to yet another aspect of the present invention, the at least one switch device comprises at least one of a 5ESS switch, a AXE10 switch, a 1AESS switch, and a DMS100 switch.
[0055] According to a further aspect of the present invention, the at least one switching device comprises an AIN switch.
[0056] According to another aspect of the present invention, the at least one switching device comprises a non-AIN switch.
[0057] According to yet another aspect of the present invention, the at least one switching device is a host switching device that services at least one remote terminal.
[0058] According to a further aspect of the present invention, the present invention includes a method for routing a call based on the location of the calling party number in an advanced intelligent communications system that includes: receiving a telephone call at a switching point, the telephone call being from a calling party number to an abbreviated dialed number, determining if the abbreviated dialed number is a triggering number; notifying a service control point of receipt of the telephone call by the switching point if the abbreviated dialed number is a triggering number; classifying the switching point; determining the location of the calling party number; determining the appropriate routing of the telephone call based on the location of the calling party number; sending call routing information regarding the telephone call to the switching point; and routing the telephone call to one of a destination number and a default announcement.
[0059] According to another aspect of the present invention, the abbreviated dialed number comprises three digits.
[0060] According to yet another aspect of the present invention, the abbreviated dialed number comprises ‘1’ plus three digits.
[0061] According to a further aspect of the present invention, the abbreviated dialed number comprises ‘0’ plus three digits.
[0062] According to another aspect of the present invention, the classifying includes determining whether the switching point receives telephone calls only from within a defined service area.
[0063] According to yet another aspect of the present invention, the classifying includes determining whether the switching point receives telephone calls from both within a defined service area and outside the defined service area.
[0064] According to a further aspect of the present invention, the notifying further comprises sending information related to the switching point to the service control point.
[0065] According to another aspect of the present invention, the determining if the abbreviated dialed number is a triggering number includes comparing the information related to the switching point to location information.
[0066] According to yet another aspect of the present invention, the notifying includes sending information related to the calling party number to the service control point.
[0067] According to a further aspect of the present invention, the determining of the location comprises comparing a zip code of the calling party number to location information.
[0068] According to another aspect of the present invention, the determining of the location comprises determining the location of the service switching point.
[0069] According to yet another aspect of the present invention, the determining of the appropriate routing comprises determining the zip code of the location of the calling party number.
[0070] According to a further aspect of the present invention, the routing comprises routing the telephone call to the destination number closest to the calling party number.
[0071] According to another aspect of the present invention, the default announcement recites a message and terminates the call.
[0072] According to yet another aspect of the present invention, the present invention includes an advanced intelligent communications system for routing telephone calls based on the location of a calling party that includes: calling means for originating a telephone call; switching means operatively connected to the calling means, the switching means servicing calls placed by a calling party using the calling means; processor means operatively connected to the switching means, the processor means determining routing of the calls placed by the calling party; storage means operatively connected to the processor means, the storage means containing location information related to the calling party; and at least one destination site operatively connected to at least one of the switching means, wherein the processor means sends routing information to the switching means for routing calls to one of the at least one destination site and a terminating announcement, based on the location of the calling party.
[0073] According to a further aspect of the present invention, the switching means has an associated signaling point code that is used by the processor means to determine the location of the calling party.
[0074] According to another aspect of the present invention, the signaling point code indicates whether the switching means services only calls from within a defined service area.
[0075] According to yet another aspect of the present invention, the signaling point code indicates whether the switching means services calls from both within the defined service area and from outside of the defined area.
[0076] According to a further aspect of the present invention, each signaling point code that indicates whether the switching means services only calls from within a defined service areas has an associated call routing telephone number.
[0077] According to another aspect of the present invention, the storage means contains information mapping the signaling point codes to the associated call routing telephone number for the switching means that services only calls from within the defined service area.
[0078] According to yet another aspect of the present invention, for the signaling point codes that indicate the switching means does not service any calls from within the defined service area, the processor means sends routing information to the switching means to route the call to the terminating announcement.
[0079] According to a further aspect of the present invention, the storage means contains information indicating whether the signaling point codes represent switching means that service calls from within the service area.
[0080] According to another aspect of the present invention, the storage means contains information indicating whether the signaling point codes represent switching means that service calls from both within the service area and outside the service area.
[0081] According to yet another aspect of the present invention, the storage means contains information mapping telephone numbers of the calling party to associated zip codes.
[0082] According to a further aspect of the present invention, the storage means contains information mapping the associated zip codes to call routing telephone numbers.
[0083] According to another aspect of the present invention, information regarding the processing of the calls placed by the at least one calling party is recorded.
[0084] According to yet another aspect of the present invention, the invention includes means for generating reports based on the information recorded.
[0085] According to a further aspect of the present invention, the calls placed by the calling party are to an abbreviated telephone number comprising three digits.
[0086] According to another aspect of the present invention, the calls placed by the calling party are to an abbreviated telephone number comprising “1” plus three additional digits.
[0087] According to yet another aspect of the present invention, the calls placed by the calling party are to an abbreviated telephone number comprising “0”, plus three additional digits.
[0088] According to a further aspect of the present invention, the present invention includes an advanced intelligent communications system for routing a call based on the location of the calling party number that includes: receiving means for receiving a telephone call at a switching point, the telephone call being from a calling party number to an abbreviated dialed number; determining means for determining if the abbreviated dialed number is a triggering number; notifying means for notifying a service control point of receipt of the telephone call by the switching point if the abbreviated dialed number is a triggering number; classifying means for classifying the switching point; second determining means for determining the location of the calling party number, third determining means for determining the appropriate routing of the telephone call based on the location of the calling party number; sending means for sending call routing information regarding the telephone call to the switching point; and routing means for routing the telephone call to one of a destination number and a default announcement.
[0089] According to another aspect of the present invention, the abbreviated dialed number includes a telephone number that comprises three digits.
[0090] According to yet another aspect of the present invention, the abbreviated dialed number comprises a telephone number that comprises ‘1’ plus three additional digits.
[0091] According to a further aspect of the present invention, the abbreviated dialed number includes a telephone number that comprises to plus three additional digits.
[0092] According to another aspect of the present invention, the classifying means determines whether the switching point receives telephone calls only from within a defined service area.
[0093] According to yet another aspect of the present invention, the classifying means determines whether the switching point receives telephone calls from both within a defined service area and outside the defined service area.
[0094] According to a further aspect of the present invention, the notifying means further sends information related to the switching point to the service control point.
[0095] According to another aspect of the present invention, the first determining means further compares the information related to the switching point to location information.
[0096] According to yet another aspect of the present invention, the notifying means further sends information related to the calling party number to the service control point.
[0097] According to a further aspect of the present invention, the second determining means compares a zip code of the calling party number to location information.
[0098] According to another aspect of the present invention, the second determining means determines the location of the service switching point.
[0099] According to yet another aspect of the present invention, the third determining means determines the zip code of the location of the calling party number.
[0100] According to a further aspect of the present invention, the routing means routes the telephone call to the destination number closest to the calling party number.
[0101] According to another aspect of the present invention, the default announcement recites a message and terminates the call.
[0102] Additional features and advantages of the present invention will be set forth in the description to follow, or may be learned by practice of the invention. The objectives and other advantages of the invention will be realized and attained by the methods particularly pointed out in the written description and claims hereof together with the appended drawings.
[0103] 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 examples and an explanation of the invention as claimed.
[0104] The accompanying drawings are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrating one embodiment of the invention. The drawings, together with the description, serve to explain the principles of the invention.
BRIEF DESCRIPTION OF THE DRAWINGS
[0105] The present invention is illustrated by way of example, and not by way of limitation, by the figures of the accompanying drawings in which like reference numerals refer to similar elements, and in which:
[0106] FIG. 1 shows a block diagram of an exemplary prior art AIN system;
[0107] FIG. 2 is a block diagram showing an AIN geographical call routing for a non-emergency calling service according to the present invention;
[0108] FIG. 3 is a block diagram of an Integrated Service Control Point according to the present invention;
[0109] FIG. 4 is a flow diagram of geographical call routing for a non-emergency calling service according to the present invention;
[0110] FIG. 5 is an exemplary Single Point Code Table according to the present invention;
[0111] FIG. 6 is an exemplary Zip Code to Routing Telephone Number table according to the present invention;
[0112] FIG. 7 is a block diagram of an AIN geographical call routing for a non-emergency calling service with multiple service areas according to the present invention;
[0113] FIG. 8 shows an exemplary multiple service area SPC table according to the present invention;
[0114] FIG. 9 is an exemplary table showing switch specific default announcement translations;
[0115] FIG. 10 is an exemplary table showing POTS and coin call disposition according to the present invention.
[0116] FIG. 11 shows an exemplary AMA record;
[0117] FIG. 12 is a flow diagram of the geographical call routing for a non-emergency calling service with DRS according to the present invention.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0118] The particulars shown herein are by way of example and for purposes of illustrative discussion of the embodiments of the present invention only and are presented in the cause of providing what is believed to be the most useful and readily understood description of the principles and conceptual aspects of the present invention. In this regard, no attempt is made to show structural details of the present invention in more detail than is necessary for the fundamental understanding of the present invention, the description taken with the drawings making apparent to those skilled in the art how the several forms of the present invention may be embodied in practice.
[0119] Many telephone services may be provided using an AIN or AIN-type network for centralized control of telephone services offered to subscribers, as opposed to localized control of services at the Central Office (CO). An AIN system is provided through interaction between switching points and other systems supporting AIN logic.
1. AIN Network
[0120] The geographical call routing for a non-emergency call service according to the present invention may be implemented using AIN Release 0.1 protocols and advanced intelligent network capabilities which are provided by a telephone company, i.e., programmable service control points (SCPs), central offices equipped with AIN service switching point (SSP) features, and existing Common Channel Interoffice Signaling (CCIS) networks. The Signaling System 7 (SS7) network is a widely used CCIS network that provides two-way communication of Transaction Capabilities Application Protocol (TCAP) formatted data messages between the SCP and the STP. The telephone network essentially employs an upper-level software network through the STPs and the SCP. The software resides over the hardware to check the call route and the availability of connection prior to hardware connection.
[0121] FIG. 2 illustrates a general block diagram of an Advanced Intelligent Network (AIN) in which a system and method for geographical call routing for a non-emergency calling service is embodied in accordance with the present invention. In FIG. 2 , local telephone lines 114 connect a plurality of individual locations 72 - 94 in each geographic area to the closest Central Office (CO), or End Office (EO) which contains Service Switching Points 60 - 70 . An End Office is a Central Office that is connected to the telephone equipment of a user. In FIG. 2 , each CO is shown as a Service Switching Point (SSP) 60 - 70 .
[0122] The SSPs may include, but are not limited to, 5ESS, AXE10, 1AESS, and DMS-100 switches. If 5ESS switches are utilized, then these switches should be equipped with generic 5E9 (or higher) and provided with the necessary trigger requirements (discussed below) in order to serve subscribers. Any 1AESS switches should be equipped with generic 1AE12.06 (or higher) and provided the necessary trigger requirements in order to serve subscribers. For DMS switches, DMS release (NA008), and the necessary trigger features should be provided. The corresponding software release for the ISCP is Release (5.0). For AXE10 switches, AXE 10 8.0 and the necessary trigger features should be provided. Future software releases on these network elements should not impact the service.
[0123] For purposes of illustration, only six SSPs are shown in FIG. 2 . However, more (or less) than six SSPs may be utilized. The SSPs 60 - 70 are programmable switches which: recognize AIN-type calls; launch queries to an Integrated Service Control Point (ISCP) 110 ; and, receive commands and data from the ISCP 110 to further process and route AIN-type calls. The SSPs 60 - 70 are connected by trunked communication lines 120 which are used to connect and carry telecommunication signals, e.g., voice and/or data, from a calling party to a called party. When one of the SSPs 60 - 70 is triggered by an AIN-type call, the SSP formulates an AIN service request and responds to call processing instructions from the network element in which the AIN service logic resides. A trigger event is the combination of the occurrence of receipt of a call, and the called telephone number satisfying the trigger criteria administered in the SSP, which invokes AIN or switch-based feature involvement in an originating or terminating call. A trigger occurs when the SSP determines that it must query the ISCP to continue processing a call. Triggers can occur from both the originating and terminating telephone numbers. The AIN service logic may reside in a database at ISCP 110 . A Call Processing Record (CPR) is a graphical representation of service logic. The CPR shows the flow of decisions and actions that are made as a call is processed.
[0124] In FIG. 2 , the SSPs 60 - 70 are equipped with Common Channel Inter-Office Signaling (CCIS) capabilities (or, alternatively, Common Channel Signaling (CCS)), e.g., Signaling System 7 (SS7), which provides for two-way communications of data messages between each SSP 60 - 70 and the ISCP 110 via SS7 links 116 . The data messages are formatted in accordance with the Transaction Capabilities Applications Protocol (TCAP). As shown in FIG. 2 , SSPs 60 - 70 are connected to Signaling Transfer Points (STPs) 100 - 104 by SS7 links 116 . The connections by links 116 to the STPs are for signaling purposes, and allow the SSPs to send and receive messages to and from the ISCP 110 . Each of the STPs can be connected to a number of other STPs. For purposes of illustration in FIG. 2 , SS7 links 116 are shown as connecting STPs 100 and 102 to a regional STP 104 and connecting the regional STP 104 to ISCP 110 .
[0125] FIG. 3 shows an ISCP 110 that may include a Service Management System (SMS) 118 , a Data and Reports System (DRS) 120 , a programmable Service Control Point (SCP) 122 , and a Service Creation Environment (SCE) 124 . The SCE 124 is a terminal that may be implemented to work with SMS 118 to create, modify, and load services into a database in the SCP 122 . The SCP 122 executes software-based service logic and returns call routing instructions to the SSPs. The SMS 118 and DRS 120 may be provided for compiling calling information to be used for billing and administrative purposes. By way of example, ISCP 110 may be implemented with the Bellcore Integrated Service Control Point (ISCP), loaded with ISCP software Version 3.4, available from Bell Telephone Laboratories, Inc., Murray Hill, N.J.
[0126] In a typical AIN-type system, when a non-AIN telephone call is initiated from, for example, party A at location 88 in FIG. 2 , the call is directed to the end office 68 serving the calling location 88 . While each of the end offices 60 - 70 may not be AIN-type SSPs, they are SS7 SSPs, and, therefore, part of the software data network. When the end office 68 receives the originating call, the call is suspended and the software network takes over the routing and connecting of the call. Normal call processing begins when an originating station 88 is off-hook and the end office 68 receives dialed digits (the telephone number of the party at station 88 ) from the originating station. End office 68 analyzes the digits and determines the call type, i.e., intraswitch or interswitch. An intraswitch call, i.e., a local call, directly connects calling station 88 with called station 90 without any querying outside of end office 68 , that serves both stations.
[0127] When the called station, for example, a party at station 82 , is not served by the same end office as originating station 88 , further processing may be necessary. In this situation, and assuming an entire SS7 network, the originating call from station 88 is suspended at the end office 68 , which further sends a query message through one or more of the STPs 100 and 102 , and/or regional STP 104 to ISCP 110 to offer termination of the call. The query message is routed to terminating end office 64 , the end office serving called station 82 . If station 82 is off-hook, i.e., busy, terminating end office 64 responds to the query from end office 68 that the call cannot be connected, and a busy signal is transmitted to calling station 88 . If station 82 is on-hook, end office 64 responds to the query of originating end office 68 by transmitting a ringback signal to calling station 88 , which is then serially connected through the trunked communication lines 120 to end office 64 and from end office 64 to called station 82 .
[0128] Advanced Intelligent Network (AIN) call processing differs from standard telephone call processing in that a query to a centralized database or service logic, e.g., ISCP 110 , is triggered by an AIN application. In AIN-type call processing, an SSP is responsible for identifying calls associated with AIN services, detecting when conditions for AIN service involvement are met, formulating service requests for call processing instructions, and responding to the instructions received. As with normal call processing, when the call is suspended at the calling party's end office, this end office may send a data message, via the SS7 links 116 , to the STPs to establish the call route. AIN services are created by assigning appropriate SSP call suspension points, known as AIN “triggers”, accessed via customer lines or telephone numbers, and accessing customer or service-specific logic in the ISCP 110 . A Dialed Number (DN) Trigger is an AIN 0, office-based, originating trigger which invokes AIN features when the trigger criteria are met. Trigger criteria are met when a call is placed to the designated NPA codes, NPA-NXX codes or NPA-NXX-XXXX codes. Ideally, AIN service should be triggered at the earliest possible point in the call, i.e., at the originating CO, however, service providers may only be able to provision the network with AIN triggers residing in the COs serving the subscribing customer or at an intermediate point on one of the connecting trunks. The SSPs launching the AIN queries are SSPs 60 - 66 , because SSPs 68 and 70 do not service any telephones within the service area, Thus, if an originating call through SSP 60 encounters an AIN trigger, i.e., a call requiring AIN service involvement, the SSP 60 suspends call processing, then queries the ISCP 110 through the STPs 100 and 104 over the SS7 links 116 .
[0129] The ISCP 110 executes software based service logic programs stored in the SCP 122 to perform subscriber functions, and returns a response to the originating end office with call routing instructions. The AIN service application may be stored in SCP 122 , or another element containing or consisting of an ISCP database. New services may be created by assigning appropriate SSP AIN triggers to customer lines or telephone numbers to access customer and/or service-specific logic in ISCP 110 . The SS7 message routing should be devised to minimize the need for data administration at the local and regional STPs.
[0130] When ISCP 110 receives a query, the intelligent network screening service logic will be executed. Call data may be collected and recorded in DRS 120 . For example, the ISCP 110 may contain resident service software that collects the calling (originating) telephone number, called (terminating) telephone number, the date, and the time of each query to the ISCP 110 A call processing record (CPR) that is stored within SCP 122 , may also be provided. The CPR may contain the service logic for network screening and call routing.
[0131] The ISCP service logic must have detailed knowledge of trunk group identifiers, route index numbers, and individual SSPs in order to service a customer. This information may be obtained during a service order process and may require that translation groups be consulted to complete such service order/provisioning information.
2. Geographical Call Routing For A Non-Emergency Calling Service System
[0132] An embodiment of the geographical call routing for a non-emergency calling service system according to the present invention that will be used for illustration is a geographical call routing for a non-emergency calling service system provided by a city to its residents. In the system, a caller may place a call to a nonemergency abbreviated telephone number to get information regarding city resources, activities, or services, etc. The abbreviated number may be three digits, such as 311, or “1” or “0” plus three digits; e.g. 1 311 or 0 311. The caller, or user, dials the 311 number to get answers to questions regarding information or services. Normally, the user would have to dial the number for the specific service, or the number for the office handling questions related to the information desired.
[0133] The non-emergency call routing system service is provided by a telephone service provider. The telephone service provider may or may not be the local telephone service provider of the subscriber to the service. In the above example, the city is a subscriber to the AIN-based geographical call routing system. A resident of the city is a user of the subscriber services provided by the system. If a user desired information regarding a city service, the user would normally call the telephone number associated with the department or agency that has information for that service. The present invention provides the user with the ability to dial only a single abbreviated telephone number to access information for all services provided by the subscriber.
[0134] Since only a single telephone number is used for information regarding all services, the frequency of calls to this number will be greater than if several telephone numbers, one for each department, is used. The present invention takes calls made to the abbreviated number and routes them to one of one or more destinations based on the location of the calling party. The location of the calling party is determined relative to a defined service area where the subscriber provides the abbreviated non-emergency call routing services. Only calls from users within this service area will be routed to one of the destinations that answer calls made to the non-emergency number. The location of the SSP that services the originating call from the calling party is used to determine routing of the call. The calling party number (CPN) is also used to determine how to route the call when the SSP location is not sufficient.
[0135] FIG. 4 is a flowchart of the geographical non-emergency call routing system according to the present invention. A telephone call to the 311 number is received at a SSP (S 2 ) that services calls for the CPN that placed the call. An AIN trigger is generated (S 4 ) for calls placed to telephone numbers having digits 311, 1+311, or 0+311. Information related to the call is sent to ISCP 110 from the SSP. The SSP will send information related to both the calling party, and the SSP. This information will include the CPN, as well as a Signaling Point Code (SPC). A SPC is associated with each SSP that services telephone numbers in the service area. The SPC relates to the location of the SSP. The SPC also identifies whether the SSP services only telephone numbers within the service area, or whether the SSP services telephone numbers both in the service area, and outside of the service area. ISCP 110 uses the SPC in determining the routing of the call.
[0136] ISCP 110 will determine if the SPC is contained in a SPC table contained in ISCP 110 (S 6 ). The SPC table maps each SPC to a Routing Telephone Number (RTN). The subscriber to the non-emergency call routing system may provide this mapping to the service provider. FIG. 5 is an exemplary SPC Table according to the present invention. The first column of FIG. 5 contains the SPC values identifying the SSPs. Column two of FIG. 5 shows a descriptive field designating what municipality, region, or area the SSP services based on the SPC. In the exemplary table in FIG. 5 , the region represents a city where the last character in the region field represents the state that the city is located in. The third column has a SPLIT variable that indicates whether the associated SSP services only telephone numbers that are within the service area, or services both telephone numbers within the service area and telephone numbers outside of the service area. If the SSP only services telephone numbers that are within the service area, the SPLIT variable will be “N”. If the SSP services both telephone numbers within the service area and telephone numbers outside of the service area, the SPLIT variable will be “Y”.
[0137] If the SPC, of the SSP that received the call, is not contained in the SPC table, the call is routed to a default announcement and terminated. Generally, the SPC of the SSP will not be in the SPC table if the SSP only services telephones located outside of the defined service area. SSP 68 and SSP 70 in FIG. 2 are examples of SSPs that do not service any telephone numbers within the defined service area. The service area is defined in FIG. 2 by thick solid lines forming a square. Therefore, a calling party from outside of the service area, for example outside of the city limits, would not have access to the services provided by the subscriber city or municipality.
[0138] If the SPC is in the SPC table, and indicates that the telephones serviced by the SSP are all within the service area, service logic in ISCP 110 will identify the routing telephone number (RTN) associated with the SPC of the SSP as shown in FIG. 5 . The service logic will send this routing information to the SSP, and the SSP will route the call accordingly. Column 5 of FIG. 5 shows an associated customer billing number for each RTN. The billing number is a telephone number related to the subscriber of the geographical non-emergency call routing service. This number is printed on billing information sent to the subscriber.
[0139] If the SPC indicates that the SSP is divided, or split (S 8 ), i.e. the SSP services telephones both in the service area, and telephones outside of the service area, the ISCP service logic performs additional processing to determine the appropriate routing of the call. The service logic verifies that a ten digit CPN has been received from the SSP (S 12 ). If a ten digit CPN has not been received, the ISCP will send routing information to the SSP to route the call to a default announcement and terminate the call (S 24 ).
[0140] However, if a ten digit CPN has been received, the service logic will attempt to identify a zip code associated with the CPN (S 14 ). This can be accomplished many ways. For example, a list of CPNs and associated zip codes may be contained in a database. The service logic would then send the CPN to the database to retrieve the associated zip code. The service logic may also, however, use a lookup table that contains a list of CPNs and their associated zip codes. Zip codes may vary in length from 5 digit zip codes to more than five digits.
[0141] If no zip code is found for the CPN (S 16 ), the service logic will cause the ISCP to send routing information to the SSP (S 27 ) directing the SSP to route the call to a default announcement and disconnect the call (S 24 ). If a zip code match is found for the CPN (S 16 ), the service logic then determines the associated RTN for the zip code (S 18 ). ISCP 110 will contain information such as that shown in FIG. 6 . FIG. 6 is an exemplary Zip Code Routing table that lists zip codes and their associated routing telephone numbers. If an associated routing telephone number is not found, the service logic will cause the ISCP to send routing information to the SSP (S 27 ) directing the SSP to route the call to a default announcement and disconnect the call (S 24 ). If an associated routing telephone number is found, ISCP 110 would send routing information to the SSP that contains the associated RTN (S 26 ).
[0142] Therefore, as shown in FIG. 4 , once the SSP receives the routing directions from ISCP 110 , the SSP will either route the call to the appropriate routing telephone number for the calling party number (S 28 ), or route the call to a default announcement and disconnect the call (S 24 ).
[0143] The geographical call routing for a non-emergency call service system according to the present invention may also be implemented for multiple service areas. For example, it is possible for several different areas to provide the non-emergency calling service for their residents.
[0144] FIG. 7 is a diagram showing an embodiment of the present invention where the non-emergency call routing system has multiple service areas (denoted by the thick black rectangles). In this embodiment, the geographical call routing for a non-emergency call service according to the present invention still determines the appropriate routing of the call based on the geographical location of the calling party. A 311 call from a calling party will be routed to the appropriate destination or routing telephone number based on which service area the calling party number is located in or serviced by, and by the location of the calling party relative to the service area. The SPC of each SSP defines the location of the SSP, and which service area the SSP services. If the SSP services telephones both within one service area, and telephones within another service area or no service area, then the associated zip code of the calling party number will be used to determine the routing of the call. If the zip code is not in the zip code routing table, then the call will be routed to a default announcement.
[0145] Four separate geographical areas, each one denoted by the thick box-shaped outlines, and the labels DALLAST, TULSAO, STLOUISM, and KANSASCM are shown in FIG. 7 . STPs 202 - 208 are connected to ISCP 220 through STP 210 . Connections between SSPs and STPs (e.g. SS7 links 116 ), and SSPs and calling party telephones (e.g. local telephone lines 114 ) are the same as shown in FIG. 2 discussed previously. In FIG. 7 , only one STP is shown in each geographical area, however, there may be multiple STPs in each area, and more SSPs and calling party telephones than shown, and still be within the spirit and scope of the present invention. ISCP 220 contains the SPC values for all 8SPs that service calls from all service areas that subscribe to the geographical non-emergency calling service system. The ISCP also contains all call routing telephone numbers associated with each service area.
[0146] For example, calls placed by a calling party at stations 260 , 262 , or 270 to the non-emergency number calling service would be routed to a default announcement and terminated because these stations are not within the STLOUISM service area, or any other service area. The SPC of SSP 242 will not have an associated call routing telephone number.
[0147] Calls placed by a calling party at stations 264 or 266 will cause a trigger in SSP 244 . Since SSP 244 services calls only from stations within the STLOUISM service area, the SPC of SSP 244 will likely have an associated routing telephone number for the STLOUISM service area. The routing telephone number for the SPC of SSP 244 will be sent to SSP 244 , and the calls routed accordingly.
[0148] Calls placed by stations 268 and 270 will cause a trigger in SSP 246 . The SPC of SSP 246 will be SPLIT since SSP 246 services stations both within the STLOUISM service area and stations outside of the STLOUISM service area. For calls to the non-emergency number placed at stations 268 and 270 , the calling party number will be sent to the ISCP to find an associated zip code. If the zip code is not found, the call will be routed to a default announcement and terminated. If a zip code is found, the associated routing telephone number will be sent to SSP 246 , and the call routed accordingly. Since station 268 is within the STLOUISM service area, the SPC of station 268 will likely have an associated zip code in ISCP 220 with an associated routing telephone number. Conversely, since station 270 is not within the STLOUISM service area, the SPC of station 270 will likely not have an associated routing telephone number.
[0149] An exemplary routing table with SPCs and associated routing telephone numbers for multiple service areas is shown in FIG. 8 . In this example, call routing numbers for the four different service areas, denoted by DALLAST, STLOUISM, TULSAO, and KANSASCM, are shown. This table is similar to that shown in FIG. 5 discussed previously, except FIG. 5 only related to a single service area. The SPC Table in FIG. 8 is for a system that services multiple service areas, as shown by the different regions that represent different cities. The last character in the region field represents the state that the city is located. As shown in FIG. 8 , there can be different SPCs for the same service area, and also different routing telephone numbers for calls from the same service area. The term “BLANK” means that there is no information for this entry.
3. Trigger Requirements
[0150] The present invention may be implemented with, for example: 5ESS, AXE10, 1AESS, and/or DMS-100 switches. A trigger will be set against the digits 311, 1+311, and 0+311 in the SSP switches. The 311 trigger should be activated only in those SSPs that serve telephone numbers located within the service area. If a trigger is generated, a query is launched to the ISCP 110 . The 311 digits will be translated into ten-digit numbers in each of these switches.
[0151] The non-emergency 311 service may be used by telephones that are serviced by non-AIN equipped switches. In these cases, in order to provide the 311 service, it will be necessary to route 311 calls to a nearby compatible 5ESS, AXE10, 1AESS, or DMS-100 SSP. Once the 311 number is received by one of these SSPs, a trigger will be generated, and the call processed accordingly.
[0152] For the terminating announcement, AIN Announcement ID # 99 is translated in each 311 participating SSP according to the switch specific features as shown in FIG. 9 . The announcement may be recorded and installed in any SSP that is part of the non-emergency calling service system. The terminating announcement is not limited to AIN Announcement ID # 99 , but may be any message desired, recorded, and installed for the terminating announcement.
[0153] a. 5ESS Switch Types
[0154] For a non-emergency 311 number served by a 5ESS switch, a N11 trigger is encountered and an Info_Analyzed query message is generated with a trigger criteria type of N11. The trigger on the 5ESS switch is a 10-digit trigger. The trigger may be based upon AIN Release 0.1 protocol and may preferably require that AIN Release 0.1 query call variables be converted into common call variables by a CPR (Calling Party Record) in the ISCP 110 . If the 5ESS switch is utilized, then these switches should be equipped with Generic 5E9.1 (or higher) and provided with the necessary trigger requirements in order to serve subscribers.
[0155] b. 1AESS Switch Types
[0156] For a non-emergency 311 number served by a 1AESS switch, a NPA (3/6/10) trigger is encountered and an Info_Analyzed query message is generated with a trigger criteria type of NPA. The trigger on the LAESS switch may be a dialed line number (DN) trigger based upon a 10 digit virtual number. The trigger may be based upon the AIN Release 0.1 protocol and may preferably require AIN Release 0.1 query call variables to be converted into common call variables by a CPR in the ISCP 110 . Further, if 1AESS switches are employed, they should preferably be equipped with Generic 1AE12.03 (or higher) and provided with the necessary trigger requirements in order to serve subscribers.
[0157] c. DMS-100 Switch Types
[0158] For a non-emergency 311 number served by a DMS switch, a NPA (3/6/10) trigger is encountered and an Info_Analyzed query message is generated with a trigger criteria type of NPA. The trigger of the DMS-100 switch may utilize a termination attempt trigger (TAT) based upon the AIN Release 0.1 protocol and may preferably require AIN Release 0.1 query call variables to be converted into common call variables by a CPR in the ISCP 110 . A TAT is a subscribed trigger that is assigned to a telephone number. AIN features are invoked because of an attempt to terminate a call on the dialed number which subscribes to this trigger. These were first available in AIN 0.1. If DMS-100 switches are used, DMS release NA008 (or higher) should preferably be provided.
[0159] d. AXE 10 Switch Types
[0160] For a non-emergency 311 number served by a AXE 10 switch, a N11 trigger is encountered and an Info_Analyzed query message is generated with a trigger criteria type of N11. If AXE 10 switches are used, AXE 10 8.0 (or higher) should preferably be provided.
4. Non-AIN Switches
[0161] In the non-emergency call routing system according to the present invention, switches that are not equipped for AIN can be used. The non-AIN switch is assigned an SSP (Hub SSP) that is AIN equipped, and part of the non-emergency call routing system. If a call to the non-emergency call routing service is received by the non-AIN switch, and the non-AIN switch services telephones that the non-emergency call routing system is providing service for, the call will be routed from the non-AIN switch to the Hub SSP. A trigger will then be generated, and the call processed the same as calls placed to AIN SSPs used in the non-emergency call routing system. The non-AIN switch should be assigned to an AIN Hub SSP with the same type non-emergency number routing table information in the ISCP.
[0162] The call processing of 311 calls to a non-AIN switch is determined based on the locations of both the non-AIN switch, and the Hub SSP. If both the non-AIN switch and the Hub SSP are entirely within the service area, the SPLIT variable will be “N”, and only the SPC Table will be accessed to determine the appropriate routing of the call. However, if either the non-AIN switch or the Hub SSP are outside of the service area, the SPLIT variable will be “Y”, and the ZIP Code Routing table will be used to determine the appropriate routing of the call.
5. Hosts/Remotes
[0163] The non-emergency call routing system according to the present invention can have host SSPs that service remote terminals. Remote terminals are line termination points that service one or more telephones. The remote terminals, however, are “dumb” terminals with no programming or processing means. Interoffice calls placed from telephones serviced by remote terminals are always routed to a host SSP. The host SSP then processes the call to determine the appropriate routing of the call. Remote terminals are not connected to trunk lines, and cannot route interoffice calls. Interoffice calls placed by a telephone number to another telephone number serviced by a remote terminal are always routed to the host SSP that services the remote terminal, and then from the host SSP to the destination end office.
[0164] Calls from telephones serviced by remote terminals to the 311 non-emergency number are processed similar to the way calls are processed for 311 calls to non-AIN SSPs. The call processing of 311 calls from a remote terminal is determined based-on the locations of both the remote terminal, and the host SSP. If both the remote terminal and the host SSP are entirely within the service area, the SPLIT variable will be “N”, and only the SPC Table will be accessed to determine the appropriate routing of the call. If, however, either the remote terminal or the host SSP are outside of the service area, the SPLIT variable will be “Y”, and the ZIP Code Routing table will be used to determine the appropriate routing of the call.
6. Local Service Providers
[0165] A subscriber who subscribes to the non-emergency call routing system, provided by a service provider, may desire to provide the non-emergency call routing service to users in an area that has telephone service provided by a telephone service provider (such as a local service provider) that is different from the provider that provides the non-emergency call routing system services. In this case, the local service provider (LSP) may provide service to some portion of the service area where the nonemergency call routing service is provided.
[0166] The local service provider may handle the non-emergency call by routing the call from a calling party to a routing telephone number, or the local service provider may route the non-emergency call to an SSP of the non-emergency call routing service provider where a trigger will be generated. If the LSP handles the non-emergency call, the LSP will have a database or some other means for mapping the calling party number to an associated telephone number for routing of the call, defined by the subscriber. If the calling party number does not have an associated call routing number, the LSP will route the call to a default announcement and terminate the call. If the LSP does not choose to handle calls placed to the non-emergency call routing service, all calls received by the LSP that have been placed to the non-emergency telephone number will be routed to an SSP that is part of the system of the service provider providing the non-emergency call routing services. In this case, a trigger will be generated and the call routed like other non-emergency calls received by the system.
7. POTS and Coin Call Dispositions
[0167] FIG. 10 shows the call disposition based oh the type of switch, the number dialed, and whether the call is placed from a Plain Old Telephone System (POTS), or from a coin telephone. The left most column lists the types of switches. The two columns to the right of this show whether a coin deposit is required, and whether the coin will be returned after it has been deposited. The next three columns represent the telephone number digits dialed that may initiate a trigger according to the non-emergency calling system of the present invention.
8. Usage Monitoring and Billing
[0168] The geographical call routing for a non-emergency calling service system according to the present invention monitors usage of the non-emergency calling service network. A distributed network function (in the SSPs) measures usage of the network and produces Automatic Message Accounting (AMA) records containing usage information. This information is used to obtain a count of completed calls to each 311 subscriber. This allows each subscriber to be billed on a number of completed calls basis. However, this information may be used for other purposes, and/or the subscriber billed based on different criteria related to the service, and still be within the spirit and scope of the present invention.
[0169] An AMA record is created in the SSP for each call made to the non-emergency number. The ISCP sends, to each SSP, information informing the SSP whether to create an AMA record for the call, and if so, the appropriate AMA parameters needed for the SSP to create the AMA record. This may include, among other items, a slip id (SLPID), as shown in Table 1 below, that tells the switch type, and the AMA originating number. The SLPID is then made part of the AMA record. An exemplary AMA record is shown in FIG. 11 . The first column in the AMA record shown in FIG. 11 is the title of the information collected. The second column is used to refer to tables that may reside in the ISCP if a table structure is used to collect this information. The third column is the information collected, and the fourth column contains any comments or additional information related to the information in column three. This information may be used for a variety of purposes, such as identifying high usage SSPs, or for billing the subscriber for the service.
[0000]
TABLE 1
AMA Originating Number
Switch Type
NPA
Number
1AESS & AXE
311
0000000
5ESS
000
3110000
DMS
000
0000311
[0170] In accordance with the present invention and as discussed previously, a billing telephone number may be associated with each routing telephone number. For each routing number associated with a SPC of an SSP, there may be an associated billing number. Also, when the SPC indicates SPLIT, for each zip code that has an associated call routing telephone number, an associated billing telephone number may exist. Therefore, when the ISCP receives the SPC and the CPN from the SSP to determine routing of the call, both the routing telephone number and the billing telephone number may be obtained simultaneously.
9. Data and Reports System
[0171] The ISCP in the geographical call routing for a non-emergency calling system according to the present invention passes call information to a Data and Reports System (DRS). The DRS stores call information related to calls to the non-emergency calling service system. For example, the DRS may store information related to: an occurrence of an event, the flow of decisions and actions that are made as a call is processed, the time of a call, the date of a call, and the calling party number. This information may be used to generate reports or billing information for the service provider. The information in these reports may also be useful, for example, if a call cannot be routed, or if an error condition arises.
[0172] FIG. 12 is a diagram of the AIN geographical call routing for a non-emergency calling service that includes the DRS for recording information related to the handling of the call. Reference step numbers in FIG. 12 that are the same as those in FIG. 4 represent the same activity as in FIG. 4 . FIG. 12 shows additional steps S 20 and S 22 representing the DRS function. As shown in FIG. 12 , whenever a call to the non-emergency number cannot be routed to a routing telephone number, i.e. the call is routed to a default announcement and terminated, information related to the call is gathered and recorded by the DRS in step S 22 . Also, when the call can be routed to a routing telephone number, call related information is recorded by the DRS in step S 20 .
[0173] A call disposition will be determined by the ISCP based on the handling of each call to the non-emergency number. The call disposition will be sent to the DRS. Some exemplary call dispositions are shown in Table 2.
[0000]
TABLE 2
NUM-
BER
DISPOSITION
1
Call routed to the 311 answer point without accessing Zip Code
Table
2
No CPN delivered
3
CPN delivered, but not in Zip Code Table
4
CPN delivered, CPN in Zip Code Table, but an associated Zip
code is not in Zip Code Table
5
Time-out condition
6
Return Error message
7
SCCP routing error
8
SPC not in SPC Table - Call originating from a subscriber that
is not in the customer's defined service area, or error in SPC
Table
9
No RTN in SPC Table
10
No RTN in Zip Code Table - Call originating from a subscriber
that is not in the customer's defined service area, or error
in Zip Code Table
11
Call routed to the RTN answer point after accessing Zip Code
Table
[0174] Call disposition 1 occurs after the “Yes” branch of step S 10 . Call disposition 2 occurs after the “No” branch of step S 12 . Call disposition 3 occurs after exiting step S 14 if the CPN is not found in the Zip Code Table. Call disposition 4 occurs after the “No” branch of step S 16 . Call dispositions 5, 6, or 7 may occur after exiting step S 14 . The SCCP is part of the SS7 protocol that provides communication between signaling nodes by adding circuit and routing information to the signaling message. Call disposition 8 occurs after the “No” branch of step S 6 . Call disposition 9 occurs after the “No” branch of step S 10 . Call disposition 10 occurs after the “No” branch of step S 19 . Call disposition 11 occurs after the “Yes” branch of step S 19 .
[0175] The disposition of each call will be sent to the DRS and recorded. The recorded dispositions will be monitored by the service provider to identify any problems with the system and for service assurance to subscribers.
[0000] 10. Interactions with Other AIN Type Services
[0176] The service provider may provide the geographical non-emergency call routing service system to a subscriber in area that is serviced by another AIN type service. This AIN type service may be provided by a LSP and consist of, for example, the LSP receiving operator, directory assistance, and local calls on their own network. The LSP may elect to receive some or all of these type calls on the network provided by the non-emergency call routing service system provided by the service provider.
[0177] If the LSP elects to receive not to receive local calls, i.e. these calls are processed by the non-emergency call routing service system, calls to the 311 number would generate a trigger, and the calls would be processed and routed by the non-emergency call routing service system as usual, If, however, the LSP elects to receive and process local calls itself, calls to the 311 number would be received by the non-emergency call routing service system and routed to the LSP via the LSP's own network. For this situation, no trigger would be generated, and R is the responsibility of the LSP to properly route the 311 call.
[0178] The non-emergency call routing service system according to the present invention also supports Disaster Routing Service. This is an intelligent call forwarding type of service. For example, if a police station had no one available to answer calls to its numbers because of some disaster or other situation, the police station could activate the Disaster Routing Service and then all calls made to the normal telephone number of the police station would be forwarded to another location. A service such as this can be supported for the 311 non-emergency number. If a call is placed to the 311 number, processing occurs as normal, and call routing information is sent back to the SSP. At the SSP, the received RTN would cause another trigger in the SSP, and cause the SSP to forward the call to another number accordingly.
[0179] The non-emergency call routing service system according to the present invention also supports Local Number Portability (LNP). This AIN based service, mandated by the FCC, provides the ability of users of telecommunications services to retain, at the same location, existing telephone numbers when switching from one service provider to another. If a call is placed to the 311 number, a trigger would be generated and the call processed normally. After the RTN is sent to the originating SSP, normal LNP service call processing would occur.
[0180] It is noted that the foregoing examples have been provided merely for the purpose of explanation and are in no way to be construed as limiting of the present invention. While the present invention has been described with reference to a preferred embodiment, it is understood that the words which have been used herein are words of description and illustration, rather than words of limitation. Changes may be made, within the purview of the appended claims, as presently stated and as amended, without departing from the spirit and scope of the present invention in its aspects. Although the present invention has been described herein with reference to particular means, materials and embodiments, the present invention is not intended to be limited to the particulars disclosed herein; rather, the present invention extends to all functionally equivalent structures, methods and uses, such as are within the scope of the appended claims.
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A method for location-based communicating includes identifying a service provider based on information received from a requesting party at a networked communications apparatus. The method also includes determining whether a plurality of predefined service areas have been defined for the identified service provider. When the plurality of the at least one predefined service areas have been defined for the service provider, determinations are made as whether the requesting party is in one of the predefined service areas. When the requesting party is in a predefined service areas, information specified for a service location for the predefined service area is forwarded to the requesting party.
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