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STATEMENT OF RELATED APPLICATIONS
This application is a continuation-in-part of U.S. Ser. No. 09/093,467, U.S. Pat. No. 6,106,662 filed Jun. 8, 1998; U.S. Ser. No.09/277,452 filed Mar. 26, 1999; and U.S. Ser. No. 09/307,995 filed May 10, 1999.
BACKGROUND OF THE INVENTION
1. Field of Invention
This invention relates to chemical mechanical polishing apparatus, and more particularly to the technique of optical polishing endpoint detection. The invention provides an apparatus for optical endpoint detection that avoids contamination of the detector's optical fiber tip and resultant endpoint errors.
2. Description of the Related Art
Chemical mechanical polishing (CMP) has emerged as a crucial semiconductor technology, particularly for devices with critical dimensions smaller than 0.5 micron. One important aspect of CMP is endpoint detection (EPD), i.e., determining during the polishing process when to terminate the polishing.
Many users prefer EDP systems that are “in situ EPD systems”, which provide EPD during the polishing process. Numerous in situ EPD methods have been proposed, but few have been successfully demonstrated in a manufacturing environment and even fewer have proved sufficiently robust for routine production use.
One group of prior art in situ EPD techniques involves the electrical measurement of changes in the capacitance, the impedance, or the conductivity of the wafer and calculating the endpoint based on an analysis of this data. To date, these particular electrically based approaches to EPD are not commercially available.
One other electrical approach that has proved production worthy is to sense changes in the friction between the wafer being polished and the polish pad. Such measurements are done by sensing changes in the motor current. These systems use a global approach, i.e., the measured signal assesses the entire wafer surface. Thus, these systems do not obtain specific data about localized regions. Further, this method works best for EPD for tungsten CMP because of the dissimilar coefficient of friction between the polish pad and the tungsten-titanium nitride-titanium film stack versus the polish pad and the dielectric underneath the metal. However, with advanced interconnection conductors, such as copper (Cu), the associated barrier metals, e.g., tantalum or tantalum nitride, may have a coefficient of friction that is similar to the underlying dielectric. The motor current approach relies on detecting the copper-tantalum nitride transition, then adding an overpolish time. Intrinsic process variations in the thickness and composition of the remaining film stack-layer mean that the final endpoint trigger time may be less precise than is desirable.
Another group of methods uses an acoustic approach. In a first acoustic approach, an acoustic transducer generates an acoustic signal that propagates through the surface layer(s) of the wafer being polished. Some reflection occurs at the interface between the layers, and a sensor positioned to detect the reflected signals can be used to determine the thickness of the topmost layer as it is polished. In a second acoustic approach, an acoustical sensor is used to detect the acoustical signals generated during CMP. Such signals have spectral and amplitude content that evolves during the course of the polish cycle. However, to date there has been no commercially available in situ endpoint detection system using acoustic methods to determine endpoint.
Finally, the present invention falls within the group of optical EPD systems. One approach for optical EPD systems is of the type disclosed in U.S. Pat. No. 5,433,651 to Lustig et al. in which a window is used to detect endpoint. However, the window complicates the CMP process because it presents to the wafer an inhomogeneity in the polish pad. Such a region can also accumulate slurry and polish debris.
Another approach is of the type disclosed in European application EP 0 824 995 A1, which uses a transparent window in the actual polish pad itself. A similar approach for rotational polishers is of the type disclosed in European application EP 0 738 561 A1, in which a pad with an optical window is used to transmit light used for EPD. In both of these approaches, various means for implementing a transparent window in a pad are discussed, but making measurements without a window were not considered. The methods and apparatuses disclosed in these patents require sensors to indicate the presence of a wafer in the field of view. Furthermore, integration times for data acquisition are constrained to the amount of time the window in the pad is under the wafer.
In another type of approach, the carrier is positioned on the edge of the platen so as to expose a portion of the wafer. A fiber optic based apparatus is used to direct light at the surface of the wafer, and spectral reflectance methods are used to analyze the signal. The drawback of this approach is that the process must be interrupted to position the wafer in such a way as to allow the optical signal to be gathered. In so doing, with the wafer positioned over the edge of the platen, the wafer is subjected to edge effects associated with the edge of the polish pad going across the wafer while the remaining portion of the wafer is completely exposed. An example of this type of approach is described in PCT application WO 98/05066.
In another approach, the wafer is lifted off of the pad a small amount, and a light beam is directed between the wafer and the slurry-coated pad. The light beam is incident at a small angle so that multiple reflections occur. The irregular topography on the wafer causes scattering, but if sufficient polishing is done prior to raising the carrier, then the wafer surface will be essentially flat and there will be very little scattering due to the topography on the wafer. An example of this type of approach is disclosed in U.S. Pat. No. 5,413,941. The difficulty with this type of approach is that the normal process cycle must be interrupted to make the measurement.
Yet another approach entails monitoring absorption of particular wavelengths in the infrared spectrum of a beam incident upon the backside of a wafer being polished so that the beam passes through the wafer from the nonpolished side of the wafer. Changes in the absorption within narrow, well-defined spectral windows correspond to changing thickness of specific types of films. This approach has the disadvantage that, as multiple metal layers are added to the wafer, the sensitivity of the signal decreases rapidly. One example of this type of approach is disclosed in U.S. Pat. No. 5,643,046.
One of the techniques for detecting when a silicon wafer surface has been polished to the extent required, is the use of optical endpoint detectors. Such detectors present several problems in practical application. In particular, optical endpoint detectors are subject to contamination of the sensor (optical fiber tip), resulting in errors or oversaturation as a result of receiving too much input light. The problems inherent in prior optical art endpoint detection systems may be better explained with reference to the attached FIGS. 1, 1 A, and 2 . FIG. 1 is a schematic representation, not to scale, of a common chemical mechanical polishing head, including a platen 10 ′ to which is mounted a central spindle 12 ′, for rotating the platen. The underface of the substantially circular platen 10 ′ is covered with a polishing pad 14 ′, that is attached by conventional means such as adhesives. As shown in FIG. 2, the polishing pad 14 ′ is often scored with grooves running in “x” and “y” directions to form a grid with parallel x-direction grooves 16 ′ and crossing perpendicular grooves 18 ′. These grooves are typically shallow and narrow and assist in the distribution of the chemical slurry during chemical mechanical polishing.
When an optical endpoint detector is used in the chemical mechanical polishing apparatus, an optical fiber 20 ′ is inserted through a bore in the platen 10 ′ and through a registering bore in pad 14 ′ so that the distal tip of the fiber is flush with the lower end of a groove 16 ′ and thus slightly spaced from the underside of pad 14 ′ by the groove depth, as schematically shown in FIG. 1 A. Ordinarily, two optical fibers 20 ′ are used—one to act as a “send fiber,” and the other a “receive fiber.”
It has been found that the above-described prior art optical endpoint detection system is subject to interference from contaminants resulting from workpiece polishing, and air bubbles that form in the chemical slurry and that intensify light received through the “receive fiber” 20 ′, sometimes resulting in oversaturation of its optical detector (not shown). As might be expected, during chemical mechanical polishing, especially of semiconductor wafers that include copper-based circuitry, copper particulates and reaction products of these particulates come into contact with optical fibers 20 ′, resulting in fouling and contamination of these fibers. As a result, precise optical endpoint detection is adversely affected.
There exists a need for an optical endpoint detection system that is simple, self-cleaning or easy to clean, and that may be retrofitted to existing chemical mechanical cleaning apparatus.
SUMMARY OF THE INVENTION
This summary of invention section is intended to introduce the reader to aspects of the invention and is not a complete description of the invention. Particular aspects of the invention are pointed out in other sections hereinbelow, and the invention is set forth in the appended claims which alone demarcate its scope.
The invention provides an apparatus for optical endpoint detection of a polishing process of a semiconductor wafer or other workpiece. The apparatus includes a hydrophobic light pipe in optical communication with the workpiece, and extending at least partially through the polishing pad of the apparatus. In certain embodiments, an optical fiber is in optical communication with an opposite end of the light pipe and is spaced from the polishing surface of the polishing pad, thereby preventing contamination of the optical fiber. In other embodiments, the light detector is in direct optical communication with the light pipe.
In a preferred embodiment, the light pipe is hydrophobic, i.e., the chemical slurry used in the chemical mechanical polishing process does not adhere to light pipe surfaces. Thus, the light pipe may be of any optically transparent substance, that is either hydrophobic or has a hydrophobic coating. The preferred hydrophobic light pipes are less subject to fouling with chemical mechanical polishing particulate debris and less susceptible to interaction with bubbles in chemical slurries that may cause light amplification with potential oversaturation of the light detector.
In another embodiment, a “window” is provided in a polishing pad, the window is substantially transparent to transmit sufficient light for optical endpoint detection, and is further also hydrophobic. As with the light pipes, the hydrophobic windows are less susceptible to fouling with polishing debris, preferably have a surface flush with the polishing pad's polishing surface, and are less susceptible to interaction with bubbles that make cause light amplification and oversaturation of the light detector.
BRIEF DESCRIPTION OF THE DRAWINGS
The following drawings are illustrative of embodiments of the invention and therefore do not limit the scope of the invention, but are presented to assist in providing a proper understanding of the invention. The drawings are not to scale, and are intended for use in conjunction with the explanations in the following detailed description section.
FIG. 1 is a schematic, illustrative depiction of a prior art chemical mechanical polishing pad, mounted to a rotatable platen;
FIG. 1A is a magnified view of the optical fiber insertion to the prior art apparatus of FIG. 1;
FIG. 2 is a schematic representation of the undersurface of a polishing pad (prior art), showing a grooved rectangular matrix;
FIGS. 3 and 3A are a schematic representations of an apparatus using an optical endpoint detection system, in accordance with the parent's application;
FIG. 4 is a schematic, not to scale, illustrative embodiment of the present invention;
FIG. 5 is an embodiment of the invention including a hydrophobic window in a polishing pad;
FIG. 6 is another embodiment of the invention showing a different version of a hydrophobic window in a polishing pad;
FIG. 7 is a graph of normalized light reflectance vs. time;
FIG. 8 is a graph of normalized light reflectance vs. time; and
FIG. 9 is a graph of normalized light reflectance vs. time.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
This section describes aspects of the invention, and points out certain preferred embodiments of these aspects. This section is not intended to be exhaustive, but rather to inform and teach the person of skill in the art who will come to appreciate more fully other aspects, equivalents, and possibilities presented by the invention, and hence the scope of the invention as set forth in the claims which alone limit its scope.
The invention provides a significant advancement in the art of endpoint detection in chemical mechanical polishing. More particularly, the invention provides an optical endpoint detection system that is less susceptible to fouling by contaminants and interference from bubbles formed in chemical slurry. The apparatus requires less maintenance, is readily retrofitted to existing CMP machines, is relatively inexpensive, and simple to maintain.
In our parent applications, hereby incorporated by reference, an apparatus is provided for use with a tool for polishing thin films on a semiconductor wafer surface that detects an endpoint of a polishing process. In one embodiment, the apparatus includes a polish pad having a through-hole, a light source, a fiber optic cable assembly, a light sensor, and a computer. The light source provides light within a predetermined bandwidth. The light passes through a fiber optic cable, through the through-hole to illuminate the wafer surface during the polishing process. The light sensor receives reflected light from the surface through the fiber optic cable and generates data corresponding to the spectrum of the reflected light. The computer receives the reflected spectral data and generates an endpoint signal as a function of the reflected spectral data. In a metal film polishing application, the endpoint signal is a function of the intensities of at least two individual wavelength bands selected from the predetermined bandwidth. In a dielectric film polishing application, the endpoint signal is based upon fitting of the reflected spectrum to an optical reflectance model to determine remaining film thickness. The computer compares the endpoint signal to predetermined criteria and stops the polishing process when the endpoint signal meets the predetermined criteria. Unlike prior art optical endpoint detection systems, an apparatus according to the parent's invention, together with the endpoint detection methodology, advantageously allows for accuracy and reliability in the presence of accumulated slurry and polishing debris. This robustness makes the apparatus suitable for in situ EPD in a production environment.
In another aspect, the light source, fiber optic cable assembly and light sensor are attached to a platen of a chemical mechanical polishing machine. The computer is located external to the platen, along with a detector. A wireless link is used to communicate the reflected spectral data to the computer. This aspect of the present invention can be advantageously used in rotary chemical mechanical polishing machine in which a fiber optic or wired link between the light sensor and the computer would be difficult to implement.
In yet another aspect of the parent's invention, a rotary union is included to allow the fiber optic cable assembly to be used in a rotary chemical mechanical polishing machine. A through-cylinder is used to provide a protected passage through the platen for the fiber optic cable as the fiber optic cable extends into the through-hole in the polishing pad. The through-cylinder also prevents cooling fluid within the platen from leaking out, thereby preventing loss of cooling fluid and contamination of the polishing pad and the surface being polished.
The parent applications provide an apparatus for use with a tool for polishing thin films on a semiconductor wafer surface that detects an endpoint of a polishing process. In one embodiment, the apparatus includes a polishing pad having a through-hole, a light source, a fiber optic cable assembly, a light source, a fiber optic cable assembly, a light sensor, and a computer. The light source provides light within a predetermined bandwidth. The fiber optic cable propagates the light through the through-hole to illuminate the wafer surface during the polishing process. The light sensor receives reflected light from the surface through the fiber optic cable and generates data corresponding to the spectrum of the reflected light. The computer receives the reflected spectral data and generates an endpoint signal as a function of the reflected spectral data. In a metal film polishing application, the endpoint signal is a function of the intensities of at least two individual wavelength bands selected from the predetermined bandwidth. In a dielectric film polishing application, the endpoint signal is based upon fitting of the reflected spectrum to an optical reflectance model to determine remaining film thickness. The computer compares the endpoint signal to predetermined criteria. Unlike prior art optical endpoint detection systems, an apparatus according to the parent's invention, together with the endpoint detection methodology, advantageously allows for accuracy and reliability in the presence of accumulated slurry and polishing debris. This robustness makes the apparatus suitable for in situ EPD in a production environment.
A schematic representation of the overall system of the invention of the parent application is shown in FIG. 3 . As seen, a wafer chuck 101 holds a wafer 103 that is to be polished. The wafer chuck 101 preferably rotates about its vertical axis 105 . A pad assembly 107 includes a polishing pad 109 mounted onto a pad backer 120 . The pad backer 120 is in turn mounted onto a pad backing plate 140 . In a preferred embodiment, the pad backer 120 is composed of urethane and the pad backing plate 140 is stainless steel. Other embodiments may use other suitable materials for the pad backer and pad backing. Further, the pad backing plate 140 is secured to a driver or motor means (not shown) that is operative to move the pad assembly 107 in the preferred orbital motion.
Polishing pad 109 includes a through-hole 112 that is coincident and communicates with a pinhole opening 111 in the pad backer 120 . Further, a canal 104 is formed in the side of the pad backer 120 adjacent the backing plate. The canal 104 leads from the exterior side 110 of the pad backer 120 to the pinhole opening 111 . In a preferred embodiment, a fiber optic cable assembly including a fiber optic cable 113 is inserted in the pad backer 120 of pad assembly 107 , with one end of fiber optic cable 113 extending through the top surface of pad backer 120 and partially into through-hole 112 . Fiber optic cable 113 can be embedded in pad backer 120 so as to form a watertight seal with the pad backer 120 , but a watertight seal is not necessary to practice the invention. Further, in contrast to conventional systems as exemplified by U.S. Pat. No. 5,433,651 to Lustig et al. that use a platen with a window of quartz or urethane, the parent invention does not include such a window. Rather, the pinhole opening 111 is merely an orifice in the pad backer in which fiber optic cable 113 may be placed. Thus, in the parent invention, the fiber optic cable 113 is not sealed to the pad backer 120 . Moreover, because of the use of a pinhole opening 111 , the fiber optic cable 113 may even be placed within one of the existing holes in the pad backer and polishing pad used for the delivery of slurry without adversely affecting the CMP process. As an additional difference, the polishing pad 109 has a simple through-hole 112 .
Fiber optic cable 113 leads to an optical coupler 115 that receives light from a light source 117 via a fiber optic cable 118 . The optical coupler 115 also outputs a reflected light signal to a light sensor 119 via fiber optic cable 122 . The reflected light signal is generated in accordance with the present invention, as described below.
A computer 121 provides a control signal 183 to light source 117 that directs the emission of light from the light source 117 . The light source 117 is a broadband light source, preferably with a spectrum of light between 200 and 1000 nm in wavelength, and more preferably with a spectrum of light between 400 and 900 nm in wavelength. A tungsten bulb is suitable for use as the light source 117 . Computer 121 also receives a start signal 123 that will activate the light source 117 and the EPD methodology. The computer also provides an endpoint trigger 125 when, through the analysis of the parent invention, it is determined that the endpoint of the polishing has been reached.
Orbital position sensor 143 provides the orbital position of the pad assembly while the wafer chuck's rotary position sensor 142 provides the angular position of the wafer chuck to the computer 121 , respectively. Computer 121 can synchronize the trigger of the data collection to the positional information from the sensors. The orbital sensor identifies which radius the data is coming from and the combination of the orbital sensor and the rotary sensor determine which point.
In operation, soon after the CMP process has begun, the start signal 123 is provided to the computer 121 to initiate the monitoring process. Computer 121 then directs light source 117 to transmit light from the light source 117 via fiber optic cable 118 to optical coupler 115 . This light in turn is routed through fiber optic cable 113 to be incident on the surface of the wafer 103 through pinhole opening 111 and the through-hole 112 in the polishing pad 109 .
Reflected light from the surface of the wafer 103 is captured by the fiber optic cable 113 and routed back to the optical coupler 115 Although in the preferred embodiment of the parent, the reflected light is relayed using the fiber optic cable 113 , it will be appreciated that a separate dedicated fiber optic cable (not shown) may be used to collect the reflected light. The return fiber optic cable would then preferably share the canal 104 with the fiber optic cable 113 in a single fiber optic cable assembly.
The optic coupler 115 relays this reflected light signal through fiber optic cable 122 to light sensor 119 . Light sensor 119 is operative to provide reflected spectral data 218 , referred to herein as the reflected spectral data 218 , of the reflected light to computer 121 .
One advantage provided by the optical coupler 115 is that rapid replacement of the pad assembly 107 is possible while retaining the capability of endpoint detection on subsequent wafers. In other words, the fiber optic cable 113 may simply be detached from the optical coupler 115 and a new pad assembly 107 may be installed (complete with new fiber optic cable 113 ). For example, this feature is advantageously utilized in replacing used polishing pads in the polisher. A spare pad backer assembly having a fresh polishing pad is used to replace the pad backer assembly in the polisher. The used polishing pad from the removed pad backer assembly is then replaced with a fresh polishing pad for subsequent use.
After a specified or predetermined integration time by the light sensor 119 , the reflected spectral data 218 is read out of the detector array and transmitted to the computer 121 , which analyzes the reflected spectral data 218 . The integration time typically ranges from 5 to 150 ms, with the integration time being 15 ms in a preferred embodiment. One result of the analysis by computer 121 is an endpoint signal 124 that is displayed on monitor 127 . Preferably, computer 121 automatically compares endpoint signal 124 to predetermined criteria and outputs an endpoint trigger 125 as a function of this comparison. Alternatively, an operator can monitor the endpoint signal 124 and select an endpoint based on the operator's interpretation of the endpoint signal 124 . The endpoint trigger 125 causes the CMP machine to advance to the next process step.
In a preferred embodiment of the present invention, illustrated in FIG. 4, a light pipe 22 is inserted into a hole or bore in the underside of polishing pad 14 . Preferably, the light pipe 22 is cylindrical and of sufficient height to extend throughout pad thickness up to the interface with platen 10 . However, the light pipe may be taller, extending at least partially into a bore in the platen, if desired. Preferably, the distal end of light pipe 22 is flush with the polishing surface 15 of the polishing pad 14 . In the preferred embodiment illustrated, the distal end of light pipe 22 would be in contact with the workpiece, such as a semiconductor wafer surface, being polished with polishing surface 15 . This location assists in avoiding the formation of any entrapped liquid under the light pipe that might incorporate a bubble of air that might in turn affect light transmittance through the system. Thus, unlike the prior art optical fibers that extend into the grooves of the polishing pad, with distal ends flush with the groove and spaced from the undersurface of the polishing pad so that bubbles in liquids trapped in the grooves may affect the readings, the preferred location of the light pipe eliminates this factor.
Also, as shown in FIG. 4, the opposite end of light pipe 22 is in optical communication with optical fiber 20 , that is in communication with a light detector (not shown).
As in the case of the prior art, at least two optical fibers should be used, one to receive and one to send light signals. In accordance with the invention, each of these optical fibers is spaced from direct physical contact with the workpiece, with a light pipe.
As indicated above, in a preferred embodiment, the light pipe is of a hydrophobic material, or coated with such a material. At present, the most preferred light pipe material is a clear silicone rubber plug of material sold under the trade name DEVCON, obtained from ITW Brands, of Wood Dale, Ill. Insertion of the plug into the pad is relatively simple: the plug is inserted into a hole in the pad of approximately the same diameter as the pipe, and any protruding end of the plug is trimmed flush with the pad polishing surface. The plug may be glued into the inside of the hole using a clear adhesive, such as a urethane ultraviolet light curable plastic; for example, Norland Optical Adhesive Type 65, obtainable from Norland Products, Inc., of New Brunswick, N.J. Clearly, other suitable materials may also be used as adhesives, or as plugs to form light pipes. The desired characteristics of the light pipe and adhesive materials are that they have requisite optical clarity and chemical resistance to the chemical slurry. It is also desirable, but not necessary, that the light pipe material have sufficient hardness or abrasion resistance to withstand the rigors of the polishing process, at is least to the same extent as the polishing pad, to minimize the frequency of light pipe replacement.
In a further alternative embodiment, the light pipe may be formed in situ. Thus, once a suitably sized throughbore has been formed in the pad, the bore may be filled with an optically transparent material that will cure and harden to form a light pipe. This method offers certain advantages, in that the light pipe so formed adheres to the pad material, as well as the distal tip of the optical fiber 20 , if the optical fiber is placed in position before the composition hardens to form the light pipe.
In accordance with another embodiment of the invention, a window 42 that is transmissive of light for optical endpoint detection, is formed or inserted into a polishing pad 14 . The window 42 is of a hydrophobic material (such as silicone), and thereby repels (aqueous) chemical slurry from its surface. Further, the window preferably has a polishing surface that is co-extensive or flush with the polishing surface of the polishing pad so that it does not cause a surface irregularity in the pad that may interfere with uniform polishing of the workpiece 50 . Preferably, the window 42 is of a material that has a similar wear pattern to the material of the polishing pad surface layer 15 . Alternatively, the window 42 may be located as shown in FIG. 5 with a back to an open space 52 , so that if the window 42 were to wear less than the pad surface layer 15 , and over time begin to protrude slightly beyond the surrounding pad surface, then pressing the pad against the workpiece will result in the window yielding and moving away from the workpiece (into space 52 ) until the polishing surface of the window is flush with surrounding surface of the polishing pad.
Similarly, FIG. 6 is a schematic illustration of a cross-section through a polishing pad 14 mounted to a platen 10 with a window 42 having, in cross-section, a stepped configuration. Thus, the smaller portion 42 a of the step configuration preferably has a surface 43 co-extensive or flush with the polishing surface of the polishing pad. A wall 45 of the step section abuts against a rear surface of the polishing pad, and the larger cross-sectional portion 42 b of the window overlaps and abuts against a back surface of the pad to hold the window 42 in place in the pad. The larger portion of the window 42 b is preferably spaced from the platen 16 by a small tolerance gap or space 54 . Thus, when the pad is subject to wear, and wears more readily or more quickly than the window material, the resultant protruding window 42 will be pushed through gap 54 until the window's rear surface contacts the platen, thereby permitting the polishing surface 43 of the window to become co-planar with the polishing surface of the polishing pad 14 . Clearly, when the pad wear relative to the window exceeds the amount of tolerance allowed, the window will no longer be able to align with its polishing surface flush with the polishing pad's surface. At this point, consideration should be given to pad replacement.
The following example illustrates the usefulness of aspects of the invention and does not limit the scope of the invention as set forth and claimed herein.
EXAMPLE
A workpiece (semiconductor wafer) with a copper plating on its surface was subjected to chemical mechanical polishing, and reflectance from its surface was measured to compare performance of an embodiment of the invention with the prior art. As a preliminary matter, as polishing proceeds on a copper surface, and as the copper layer is polished through, there is an expectation that the reflectance value will decrease to approximately one half of pure copper reflectance, with variations depending upon the amount of remaining metallization in wafer trenches and in lower layers of the workpiece. In the following example, the copper was intentionally not “cleared”, to show system stability while polishing only copper.
A prior art system, such as that illustrated in FIG. 1, with a recessed optical fiber connecting through a platen to view a workpiece, was used as a prior art control. During the polishing of the workpiece, the gap between the tip of the optical fiber and the polishing surface of the pad filled with chemical slurry. The slurry foamed or bubbled, causing a dramatic increase in the amount of light reaching the optical detector, causing normalized reflectance signals to increase from 1.0 to over 2.5, as shown in FIG. 7 .
Recognizing the effect of the gap in retaining slurry, the pad was cleaned and a light type of polyurethane was installed in the gap, with a polish surface surface flush with the surface of the polishing pad. Urethane and polyurethane light pipes are generally hydrophilic, especially when the surfaces have been conditioned with an abrasive, as is the usual practice in the chemical mechanical polishing industry. The inserted polyurethane light pipe eliminated the problems associated with bubbling or foaming of the slurry, but tended to pick up polish debris. As shown in FIG. 8, the reflectance signal tended to decrease with time, indicating the progressive fouling of the polyurethane material that tended to reduce light transmission. During a 60 second period, the signal strength decreased by about 40% of initial signal strength.
In accordance with the invention, a hydrophobic light pipe was substituted for the hydrophilic polyurethane light pipe. As shown in FIG. 9, the reflectance over the same period of 60 seconds remained substantially constant, decreasing by an estimated 5% only. This reduction is relatively insignificant and points out an advantage of the invention. The following table shows the change in reflectance signal amplitude for the prior art (no light pipe with gap between fiber optic and polish pad surface); hydrophilic light pipe and the preferred hydrophobic light pipes of the invention:
TABLE I
Hydrophilic
Hydrophobic
Seconds
No pipe
Pipe
Pipe
10
0.98
1.00
1.00
20
1.07
0.98
0.98
30
1.54
0.92
0.98
40
2.15
0.81
0.97
50
2.30
0.73
0.96
60
2.55
0.62
0.95
From the foregoing FIGURES and Table, it is apparent that the invention provides significant advantages over the prior art. The invention substantially eliminates any interference effects caused by air bubbles in chemical slurry, and reduction in normalized reflectance due to accumulation of polished debris on the sensing end of the light pipe or window.
The foregoing description provides an enabling disclosure of the invention, which is not limited by the description, but only by the scope of the appended claims. All those other aspects of the invention, and their equivalents, that will become apparent when a person of skill in the art has read the foregoing, are within the scope of the invention and of the claims hereinbelow. | An apparatus for optical endpoint detection of a chemical mechanical polishing process, that reduces or eliminates interference effects caused by air bubbles in chemical polishing slurries, and accumulation of polishing debris on components of the optical system. In particular, the invention provides hydrophobic light pipes and windows with polishing surfaces substantially coplanar with surrounding surfaces of polishing pads to thereby eliminate the effect of air bubbles trapped in recesses at the polishing pad surface. Moreover, hydrophobic surfaces have now been found to resist the accumulation of polished debris thereon, resulting in a reduction in loss of optical reflectance over polishing time. Accordingly, the invention provides an optical endpoint system that eliminates or reduces both the oversaturation and loss of reflectance problems of the prior art. | 1 |
BACKGROUND OF THE INVENTION
[0001] 1. Field of the Invention
[0002] Embodiments of the present invention relate to composition for use in drilling, completing and fracturing formations including an environmentally benign scale inhibitor.
[0003] More particularly, embodiments of the present invention relate to composition for use in drilling, completing and fracturing formations, where the composition includes an effective of an environmentally benign water scale inhibitor.
[0004] 2. Description of the Related Art
[0005] Historically, several scale inhibitors have been developed for water boilers, heat exchangers and similar systems. Generally, the choice of controlling scale is dependent on water chemistry and equipment. Thus, in some systems use of chemicals (antiscalants) might be combined with mechanical means to control scale formation. While mechanical control means include filtration, sedimentation filtration and clarification (coagulation and flocculation); scales can also be controlled chemically using dispersants such as polyphosphates, phosphonates, synthetic polymers and their blends. See, e.g., U.S. Pat. Nos. 7,087,189 and 5,024,783. Though polyphosphates have low toxicity to the environment (Zahid Amjhad, NACE-96-230), orthophosphates that are toxic to algae are easily formed at proper pH, temperature, polyphosphate concentration and water chemistry.
[0006] Although scale inhibitors, either alone or in combination with mechanical scale reduction means are known in the art, there is still a need in the art of scale inhibitors operable in aqueous environments that are environmentally benign and yet effective and do not suffer from the negative environmental problems associated with the use of polyphosphates and phosphonates based scale inhibitors or antiscalants.
SUMMARY OF THE INVENTION
[0007] Embodiments of the present invention provide an environmentally benign and economical scale inhibiting composition for boilers or other equipment in contact with water containing scale forming contaminants. The composition comprises a blend of one or a plurality chelating agents, one or a plurality dispersing agents, and one or a plurality of oxygen scavenging agents, pH adjusted to a pH greater than about 9. The blend can be diluted in water. Thus, the blend can be used neat or in an aqueous dilution down to about 20 wt. %. In certain embodiments, the blend is diluted in water at a concentration between about 60 wt. % to about 20 wt. %. In certain embodiments, the blend is diluted in water at a concentration between about 50 wt. % to about 20 wt. %. In certain embodiments, the blend is diluted in water at a concentration between about 40 wt. % to about 20 wt. %. In certain embodiments, the blend is diluted in water at a concentration between about 50 wt. % to about 30 wt. %. In certain embodiment, the blend is present in a solution to be treated in concentration less than or equal to 1500 ppm. In certain embodiment, the blend is present in a solution to be treated in concentration less than or equal to 1250 ppm. In certain embodiment, the blend is present in a solution to be treated in concentration less than or equal to 1000 ppm. In certain embodiment, the blend is present in a solution to be treated in concentration less than or equal to 750 ppm. In certain embodiment, the blend is present in a solution to be treated in concentration less than or equal to 500 ppm. In certain embodiment, the blend is present in a solution to be treated in concentration less than or equal to 250 ppm. In certain embodiment, the blend is present in a solution to be treated in concentration is between about 50 ppm and 5000 ppm. In certain embodiment, the blend is present in a solution to be treated in concentration is between about 100 ppm and 2500 ppm. In certain embodiment, the blend is present in a solution to be treated in concentration is between about 150 ppm and 2000 ppm. In certain embodiment, the blend is present in a solution to be treated in concentration is between about 200 ppm and 2000 ppm. In certain embodiment, the blend is present in a solution to be treated in concentration is between about 200 ppm and 1000 ppm. In certain embodiment, the blend is present in a solution to be treated in concentration is between about 100 ppm and 500 ppm.
[0008] Embodiments of the present invention provide methods for treating a fluid including scale forming contaminants in contact with a surface upon which a scale deposit can form including adding to the fluid an effective amount of a scale inhibiting composition of this invention, where the amount is sufficient to reduce or prevent scale deposits on the surfaces.
[0009] Embodiments of the present invention provide methods for treating a fluid including scale forming contaminants in contact with a surface upon which a scale deposit can form including continuously, semi-continuously, periodically and/or intermittently adding to the fluid an effective amount of a scale inhibiting composition of this invention, where the amount is sufficient to reduce or prevent scale deposits on the surfaces.
DETAILED DESCRIPTION OF THE INVENTION
[0010] The inventors have found that an environmental benign antiscalant or scale inhibiting composition can be formulated for use in aqueous environments contaminated with scale forming salts such as calcium sulfate, calcium carbonate, iron and magnesium oxides or hydroxides or the like. The scale inhibiting composition includes a chelating agent, a dispersant, an oxygen scavenger and a base, where the base is used to adjust the pH of the composition, but no additional base is required during the use of the composition. Each component of the composition is biodegradable and benign to the environment. Not only is the composition effective and efficient at low concentrations, like polyphosphate inhibitors, it is uniquely more economical than the phosphate or phosphonate inhibitors or other competitive products in the market. A water solution of this composition was found to be stable to temperature up to −15° F. without use of any pour point depressants. Unlike most known water scale inhibitors, this novel formulation precludes use of inorganic bases for pH adjustment during use, thereby eliminating handling of hazardous astringents and reducing chemical consumption and the need for additional equipment.
[0011] The inventors have found that a composition of this invention designated SI1 when added to a fluid including calcium and magnesium scale forming contaminants at 0.5 wt. % of a 35.1 wt. % solution of the composition corresponding to a 17.55 ppm treatment offered complete inhibition of calcium or magnesium scale deposit, where the calcium and magnesium concentrations were 250 ppm, which is higher than the concentration commonly found in boilers, which is generally <200 ppm. SI1 comprises sodium ethylenedimaine tetraacetate (EDTA), a metal chelating agent, FLOSPERSE™ 1000 A and sodium lignosulfonate, polyelectrolytes dispersing agents and d-sorbitol, an oxygen inhibiting agent. SI1 is essentially an environmentally benign product, eliminates the need and cost of chemicals for pH adjustment during use, and is recommended as scale inhibitor in boilers. However, this product inhibits higher than 250 ppm concentrations of multi-cations (see Example 2) and might find uses in other markets including water treatment.
Suitable Reagents of the Invention
[0012] Suitable chelating agents include, without limitation, alkaline earth salt of ethylene diamine tetraacetic acid (EDTA), such as sodium EDTA salt, potassium EDTA salt; ethylenediamine tetrakis(alkoxylate) tetrols, nitrilotriacetonitrile or its derivatives or mixtures or combinations thereof.
[0013] Suitable polyelectrolytes or dispersants include, without limitation, polycarboxylate dispersants such as the FLOSPERSE™ including FLOSPERSE™ 1000 A, sodium lignosulfonates, potassium lignosulfonates, cesium lignosulfonates, BELCLENE® 200 (BC), polymaleic acid (PMA), lignosulphonate sodium salt (LGS), 2-acrylamido-2-methylpropane sulfonic acid homopolymers such as AMPS® products (a registered trademark of Lubrizol Corporation, and mixtures or combinations thereof.
[0014] Suitable oxygen scavengers include, without limitation, sugar alcohols like D-Sorbitol, D-Mannitol, Xylitol; ascorbic acid or erythorbic acid and their salts or mixtures or combinations thereof.
[0015] Suitable base include, without limitation, such as sodium hydroxide, potassium hydroxide, cesium hydroxide, sodium carbonate, potassium carbonate, sodium oxide, cesium oxide, potassium oxide or mixtures or combinations thereof. This invention is illustrated by the following examples.
EXPERIMENTS OF THE INVENTION
Example 1
General Procedure
[0016] A formulation (Formula Y) with constituents presented in Table 1 was prepared by adding each component beginning with the addition of sodium hydroxide to measured amount of distilled water. To this solution was added the indicated amount of EDTA or other chelating agent. The resulting solution was then stirred for 30 minutes. To the resulting solution was added the indicated amount of lignosulfonate or similar polyelectrolyte, in four portions with a 30 minute stir time between each addition. After the last 30 minute stir time, the indicated amount of D-Sorbitol or other O 2 inhibitor was added and the resulting solution is stirred for 10 minutes. To this solution was added the indicated amount of FLOSPERSE™ 1000A, or other comparable polyelectrolyte, all at once and stirred for 10 minutes. The solution was then tested for pH, usually between pH 10 and pH 11.5. The specific gravity of the final product should be between 1.16 and 1.20.
[0000]
TABLE 1
Example 1 Formula Y Components and Amounts
Component
Amount (wt. %)
FLOSPERSE 1000A
12.00
EDTA
10.00
Sodium Lignosulfonate
12.00
D-Sorbitol
2.00
Sodium Hydroxide (50%)
15.00
Distilled Water
49.00
Total
100.000
Testing
[0017] Formula Y (FY) was used in two boilers at 250° F. on a drilling site. The results of the trial with the composition was quite impressive. Water analysis (see Table 2) showed that calcium carbonate and iron levels stayed below detectable levels indicating minimal scaling.
[0000]
TABLE 2
Water Analysis
Results
pH
10
Calcium
0.0
Hardness
100 ppm
Iron
0
Magnesium
0
Chloride
100 ppm
[0018] Once the pH was properly set, there was no need to add caustic to the composition during use, unlike many other scale inhibitors. For the field trials only 18 gallons of product in example 1 (FY) were used for 190 barrels of water compared to 35 gallons of phosphate based inhibitor without accounting for additional usual caustic consumption.
Example 2
[0019] Using NACE Standard™ 0197-2002, a sample of Formula Y (example 1) was tested against WFT commercial product Alpha 2867 at 208° F. Thus, to an untreated brine (Blank, 6) and 2 jars were added 350 ppm brine. The 2 jars (3, containing FY; and 5, WFT A2867) were treated with 0.5% of corresponding scale inhibitors, see Table 3. Similar treatments was carried out at 1.0% concentration with FY scale inhibitor (Table 3). Results show that FY inhibits satisfactorily at both 0.5 (or 17.6 ppm) and 1.0% whereas WFT A2867 failed. Essentially, complete inhibition is suggestive of overtreatment at 0.5% inhibitor (FY) concentration in 350 ppm brine containing 522 ppm Ca 2+ and 21 ppm Mg 2+ .
[0000]
TABLE 3
Jar Test Treatment of Brines with Scale Inhibitors
Brine Concentration
Scale Inhibitor
Scale Inhibitor
(ppm)
Bottle #
Scale Inhibitor
(wt. %)
(mL)
Observation
350
1
Brine A
NA
NA
NA
2
Brine B
NA
NA
NA
350
3
Formula Y
0.50
0.5
No Scale
4
Formula Y
1.00
1.0
No Scale
350
5
WFT A2867
0.50
0.5
Scaled
350
6
Blank (A + B)
NA
NA
Scaled
350
7
Control (A + C)
NA
NA
NA
Temperature Stability
[0020] In North America and some cold regions of the globe, pourability of the inhibitor in cold temperatures is critical. Therefore, pour point of FY was determined. FY remains fluid up to −10° C. (14° F.) or have a freezing point of 15° C. (5° F.). A formulation containing 10 wt. % ethylene glycol (EG) has a pour point below −45° C. (−49° F.) and therefore suitable for use when environmental temperature is expected to be below −10° C. while unmodified FY is desirable at or above 10° C.
[0021] All references cited herein are incorporated by reference. Although the invention has been disclosed with reference to its preferred embodiments, from reading this description those of skill in the art may appreciate changes and modification that may be made which do not depart from the scope and spirit of the invention as described above and claimed hereafter. | Scale inhibition compositions and methods for use are disclose, where the composition including one or a plurality chelating agents, one or a plurality dispersing agents, one or a plurality of oxygen scavenging agents including one sugar alcohol or a plurality of sugar alcohols, and pH adjusted to a pH greater than about 9. | 2 |
BACKGROUND OF THE INVENTION
1. Field of the Invention
The subject invention relates generally to computer work stations and, in particular, to mobile computer work stations suitable for integral use with a personal computer.
2. The Prior Art
The personal computer has found widespread application in the work place, homes and, increasingly, schools. It has become common in elementary and preschool classrooms to provide teachers with access to a personal computer for instructional purposes. In some schools one or more computers are dedicated to a classroom. In others, a computer is shared by more than one classroom and must be moved from one room to another. Mobility, therefore, is required.
In the classroom, students often share a computer on a rotational basis and use of the computer by students is often unsupervised. Security of the computer controls from tampering by students is often a problem for the teacher, particularly with younger students. Resetting altered computer controls is distracting to the teacher and interrupts other productive instruction.
An ancillary problem to sharing personal computers in a crowded classroom is that the noise from their use can be distracting to the other students. Physical isolation of the computer from the surrounding class is often not practical due to the crowded conditions in many schools.
Conventional desks sold for use with personal computers provide adequate surfaces for supporting the monitor, keyboard, and CPU housing of a personal computer but fail generally in meeting the needs of the market described above. Available work stations generally provide a work surface, a stand or shell to the rear of the work surface for supporting a video monitor, and a drawer for the keyboard at a forward of the work surface. A computer CPU housing is either stationed upon the work surface or is located on end on the floor beside the work station.
While functional, the available computer work stations do not prove the mobility required in many school applications. Nor do they provide security from unauthorized student manipulation of the controls of the computer CPU, monitor, speakers, or keyboard. Finally, conventional work stations are not acoustically isolated and the sound emanating therefrom can distract surrounding students.
SUMMARY OF THE INVENTION
The subject invention overcomes the aforementioned shortcomings in conventional computer work station. A wheel mounted cabinet is provided to enclose a computer central processing unit housing and render the work station mobile and the computer central processor unit safe from unauthorized access. The wheels of the cabinet allow its ready transportation to different locations. The top surface of the cabinet is dimensioned and shaped to support a computer video monitor. Mounted to a forward side of the cabinet is a vertical partition having a concave shape and defining a user station. A window is dimensioned and shaped to align with the screen of the video monitor. A first bezel plate surrounds the screen and affixes to the vertical partition. A lower portion of the first bezel plate is located so as to obscure the lower controls of the monitor and render them inaccessible absent removal of the bezel plate and covers a speaker cavity so that the controls of the speakers are likewise inaccessible.
S-shaped support bars are anchored at one end to the bottom of the CPU cabinet and project upward and forward therefrom through the vertical partition. Second end segments of the support bars support a keyboard platform. A central depression within the keyboard platform receives a keyboard support pad and a touch-sensitive keyboard. A second bezel plate is further provided that attaches to the keyboard platform to secure the keyboard to the keyboard platform.
A computer speaker cavity is defined behind the lower portion of the first bezel plate dimensioned to house and physically isolate one or more computer speakers. Slots through the first bezel plate lower portion direct the sound from the speakers into the concave user station. The shape of the partition and the orientation of the speakers relative thereto minimize the noise disturbance to surrounding areas. Moreover, the lower portion of the first bezel plate renders the speakers inaccessible to the computer user absent removal of the plate.
Accordingly, it is an objective of the present invention to provide a computer work station that is mobile and readily relocatable.
A further objective is to provide a computer work station providing enhanced acoustic isolation.
Still another objective is to provide a computer work station for a personal computer system having improved means for securing and rendering inaccessible to unauthorized parties the controls to the central processing unit, the computer monitor, the keyboard, and the speakers of the computer system.
Yet another objective is to provide a computer work station capable of accommodating standard dimensioned video monitors, keyboards, and central processing housings.
A further objective is to provide a computer work station having a user station visually and acoustically isolated from the surrounding environ.
Another objective is to provide a computer work station comprised of a minimal number of inexpensively produced components rendering the station cost effective and readily assembled.
These and other objectives, which will be apparent to one skilled in the art, are achieved by a preferred embodiment which is described in detail below and which is illustrated by the accompanying drawings.
DESCRIPTION OF THE DRAWINGS
FIG. 1 is an assembled front perspective view of the subject computer work station.
FIG. 2 is an assembled left rear perspective view thereof.
FIG. 3 is an assembled right rear perspective view thereof.
FIG. 4 a partially exploded perspective view thereof.
FIG. 5 is a front plan view of the partially assembled computer work station, shown without the vertical partition.
FIG. 6 is a transverse section view through the partially assembled computer work station of FIG. 5, taken along the line 6--6.
FIG. 7 is a rear plan view of the vertical partition.
FIG. 8 is a bottom plan view of the assembled computer work station.
FIG. 9 is an exploded perspective view of the cpu cabinet.
DESCRIPTION OF THE PREFERRED EMBODIMENT
Referring initially to FIGS. 1, 4 and 6, the subject computer work station 10 is shown to generally comprise a central processor unit (hereinafter "CPU") cabinet 12; a pair of S-shaped support bars or tubes 14, 16; a vertical partition 18; a keyboard support platform 20; a keyboard support insert 22; a keyboard bezel plate 24; and a monitor bezel plate 26. The work station 10 is intended to be used in conjunction with a personal computer system, generally comprising a video monitor 28, a rectangular, four sided CPU housing 30, a pair of speakers 32; a touch sensitive keyboard 34; and a mouse control (not shown).
FIGS. 6, 8 and 9 illustrate the CPU cabinet 12 of the subject work station intended to house and isolate from unauthorized access, the CPU of the computer system within an internal compartment 35. Cabinet 12 comprises a generally flat and rectangularly shaped lower panel 36 having a planar top surface 38. A rectangular central opening 40 extends through panel 36 and four, counter sunk screw bores 42 are provided extending into surface 38 at the corners of the opening 40.
A pair of spaced apart and parallel channels 44, 46 extend along an underside of the panel 36 as best seen if FIG. 8. Extending within the top surface 38 proximate a rearward edge is an elongate assembly channel 48 and an upwardly projecting flange 50. Multiple recessed pockets 52 are formed within the top surface 38 as a result of the preferred rotational molding manufacturing method of forming the panel from plastics material. Preferably the panel 36 is formed by the rotational molding manufacturing process out of commonly available plastic resin such as polyethylene.
A rectangular vibration dampening plate 54 formed of stamped metal is provided having a rectangular shaped through opening 56 and four assembly apertures 58 at the corners. Five upwardly extending brackets 60 are stamped during the fabrication of plate 54, and are located at the corners of the opening 56. The brackets, as will be further explained later, are spaced apart to accept a CPU housing therebetween and act as a locator to position the CPU.
A rear panel 62 is likewise provided as part of the CPU cabinet 12, manufactured of common plastic material such as polyethylene, preferably by a rotational molding process. The panel 62 has an array of rectangular recesses 64 extending therein. An edge flange 66 extends upward from an upper edge and a cable aperture 68 extends through a bottom portion of the panel. Upper and lower end portions 76 of the panel 62 are radiused inward and have hinge sockets (not shown) formed therein for a purpose explained below.
The side panels 70 and 72 comprise plastic molded doors, formed preferably by a blow molding process of polyethylene resin. A pivotal latch mechanism 71 of a type common in the industry is affixed to each door 70, 72 and latches to an edge of the panels 70, 72 surrounding the door openings in conventional manner. The doors 70, 72 are on opposite sides of the cabinet 12 and serve to provide access into compartment 35. The doors 70, 72 each have a hinge edge flange 74 along a side opposite the latch mechanism 71 which is received between portions 76 of the rear panel 62. The edge 74 is formed to provide upward and downward pivot pin segments 73 which are snapped into respective sockets in portions 76 and reside therein to pivotally connect each door 70, 72 to a respective side of the rear panel 62.
The top panel 78 component of the cabinet 12 is likewise manufactured preferably of polyethylene in a rotational molding process. The panel 78 has a planar top surface 80 of rectangular shape. A pair of L-shaped centering flanges 82, 84 project upward at respective rearward corners of panel 78 and center a video monitor upon surface 80. A cable aperture 86 proximate a rearward edge of the panel 78 extends downward from surface 80 through the panel 78, and an elongate shoulder 88 extends along from the forward edge of the panel 78. As best seen from FIG. 6, an elongate channel 90 is formed within the underside of panel 78 and extends generally along the rearward panel edge.
A power strip conventional in the computer industry is provided as part of the cabinet assembly, and is positioned upon the vibration dampening plate 54.
First and second S-shaped steel bars 14, 16, as best seen in FIGS. 4 and 6, are formed having a generally square cross section. The bars 14, 16 include a first elongate end segment 94, an upwardly projecting elongate mid-segment 96, and an elongate second end segment 98. Four casters 100 mount to undersides of bar first segments 94 in conventionally fashion. Two pairs of grommets 102 extend into end segments 98 and an aperture 104 extends into and through the mid-segment 96 of each bar. Appropriate hardware screws 106 and 108 are provided to project through apertures 104, 102, respectively.
Assembly of the cabinet proceeds as follows with reference to FIGS. 4, 6 and 9. The lower panel underside channels 46 receive the lower first segments 94 of the bars 14, 16 therein and casters 100 assemble to the underside of segments 94. The vibration dampening plate 54 sits on rubber bushings (not shown) and the bushings are mounted to surface 38 of the panel 36 and opening 56 of the plate 54 aligned with the opening 40 of panel 36. Appropriate screws (not shown) attach through apertures 58 of plate 54 and 42 of the panel 36 to fix plate 54 in place. A power strip is sized to position along a rearward length of the plate 54.
A lower edge of rearward panel 62 is received within the channel 48 of lower panel 36 and screws 107 (FIG. 3) are provided to secure the parts together. The doors 70, 72 are pivotally mounted between portions 76 of the rearward panel 62 as described previously. The top panel 78 mounts over the upper edge of the rearward panel 62 as flange 66 is received into channel 90. Screws 105 (FIG. 3) are provided to secure the parts together. The mid-segments 96 of the bars 14, 16 extend upward at the forward side of the cabinet 12 between forward ends of the lower and upper panels 36, 78 as will best be appreciated from FIG. 4. The forward edges of doors 70, 72 are recessed inward from the forward ends 101, 103 of the upper panels 36, 78 so as to allow a space to interfit with the vertical partition as described below.
It will also be noted from FIG. 4 that the computer monitor 28 is positioned upon the upper surface of the top panel 78 and extends forward upon the forward edge shoulder 88. As such, the monitor overhangs the cabinet 12. The computer CPU is housed within compartment 35, accessed through either door 70 or door 72. The CPU is vertically oriented to rest upon the vibration dampening plate 54 and is centered and registered by brackets 60. The openings 40, 56 in the panel 36 and plate 54 overlap to provide adequate ventilation into compartment 35. The apertures 64 in rearward panel 62 further aid in the ventilation of compartment 35.
Cable and power cord from the monitor are routed down through aperture 86 and into compartment 35 for connection to the CPU and the power strip 92 as appropriate. The power strip 95 cable emerges through panel aperture 68 of rearward panel 62 and can be plugged into an external outlet.
With reference to FIGS. 1, 4 and 7, the vertical partition 18 has a central planar portion 110 and first and second wing portions 112, 114 that flare outwardly from portion 110. The partition 18 is preferably formed as the panels previously described; that is, by a rotational molding process from plastic material such as polyethylene. The partition is supported by spaced apart feet 116, 118. Each wing has a rectangular slot 120 extending therethrough positioned substantially mid-way up the vertical dimension. Portals 124 are disposed in the panel as a consequence of the plastic rotational molding operation.
A rectangular window 126 is centered and extends through the partition portion 110. The window is sized and of a vertical height to admit the forward face of computer monitor 28 therein from a rearward direction and includes a lower window portion 122. From the rearward view of FIG. 7 it will be seen that the central panel portion 110 has a pair of vertical, spaced apart bar-receiving channels 184, 186. Two molded posts 188, 190 extend adjacent the channels 184, 186 respectively, and proximate the top of each post 188, 190 a molded in latch detent 192, 194, respectively, is provided.
Panel portions at opposite sides of the window 126 proximate a lower end include rectangular socket cavities 196, 198. Adjacent each cavity are detents 200, 202. Screws 204 are provided to attach the partition to the cabinet assembly as explained below. Along a lower edge of the partition and extending therein is a lower channel 206. Adjacent ends of the lower channel are detents 208, 210.
Assembly of the partition 18 to the cabinet assembly will be understood from FIGS. 3, 4 and 7. It will be appreciated that the forward segments 98 of the bars 14, 16 are inserted through the lower window portion 122 to a forward side of the partition 18, and mid-segments 96 of the bars enter into the channels 184, 186. As the cabinet 12 moves against the rearward side of the partition, the forward ends 101, 103 of the cabinet upper panel 78 enter into sockets 196, 198. The forward edge of the lower panel 36 enters into lower channel 206 of the partition. Thereafter, screws 204 are inserted into upper and lower detents 200, 202 and into the upper and lower panels 36, 78, to secure the panels to the partition. In the assembled condition, the lower portion of the partition encloses the cabinet compartment 35. The latch detents 192, 194 in the partition are situated adjacent the latch 71 of the side panel doors 70, 72. The latches 71 of each door engage in conventional manner into the detents 192, 194 of the partition to secure each door in the closed position.
It will further be noted that the flared wing portions 112, 114 form with central partition portion 110 a concave shape and define a user station that is substantially enclosed on three sides. Upon insertion of the bars 14, 16 through slot 122, the partition is assembled to the forward face of the cabinet 12 and encloses the forward side of the compartment 35.
With continued reference to FIGS. 4, 6, and 8, the keyboard support platform 20 is shown having an irregular elongate shape. The platform 20 is formed of plastic material by conventional means in the preferred embodiment. A planar top surface 128 is provided into which dual mouse pad receptacles 130 arc formed. The receptacles 130 are disposed toward respective ends of platform 20 adjacent a central, stepped keyboard receiving rectangular recess 132 having a lower central recess portion 133 therein. A rectangular through channel 134 is positioned at an upper corner of recess 132 and a cable channel 136 extends from the recess 132 toward a rearward side of the platform 20.
A pair of registration flange projections 138, 140 project outward and rearward from platform 20, located and dimensioned to enter into detent apertures 120 in the partition. First and second parallel channels 142, 144 are formed in the underside of the platform 20, dimensioned to closely receive the end segments 98 of the support bars 14, 16. Screws 146, 148 project upward through bar segments 98 and into the platform 20 to securely affix the platform to ends of bars 14, 16.
Extending downward into the platform at each corner of the recess 132 are sockets 150. Registration ribs 152, 154 extend along opposite longitudinal sides of the recess 132. The keyboard insert pad 22 is dimensioned to be closely received into the bottom of recess lower portion 133. Pad 22 is composed of soft plastic such as neoprene material and serves as a support base for the computer keyboard. The pad 22 has a through aperture 160 adjacent one corner that aligns with the opening 134 of the keyboard platform 20. A cable slot 156 extends through an edge flange 158 surrounding the pad 22 and aligns with the cable slot 136 of the platform 20. The edge flange 158 overlaps the registration ribs 152, 154 of the platform 20 to center the pad 22 on keyboard platform 20. The touch sensitive keyboard (not shown) of the computer system resides within the recess 132 upon the pad 22.
A rectangular keyboard bezel plate 24 is configured having a rectangular central opening 162 and narrow edge segments 164 define opening 162. Plate 24 is dimensioned to fit over the keyboard platform 20 and edge segments 164 overlap edges of the computer keyboard. Assembly apertures 166 are located at the corners of plate 24 and align with screw sockets 150 of the keyboard platform 20. Screws 178 attach through co-aligned apertures 166 and sockets 150 to affix the platform 20 and bezel plate 24 together and hold the keyboard in place upon the insert pad 22.
The video monitor bezel plate 26 is shown to comprise a central rectangular opening 170 defined by edge portions 172. Four screw apertures 174 extend through the plate 26 spaced to align with the apertures 127 proximate the partition window 126. Screws 176 extend through co-aligned apertures 174, 127 to detachably secure the plate 26 to the forward face of the partition 18.
The bezel plate 26 further includes a lower portion 178 that extends downward to the upper surface of the keyboard platform 20. The lower portion 178 has a series of through slots 180 therethrough. As best seen in FIG. 6, the lower portion 178 defines with the upper surface 128 of the keyboard platform a speaker cavity 182. With the speakers 32 of the computer system within the cavity 182, they are inaccessible from a forward side of the partition absent removal of the bezel plate 26.
The completely assembled computer work station is illustrated in FIGS. 1, 2, 3 and 6. It will be appreciated that the computer work station is mobile and can be readily transported from location to location. The casters 100 are affixed to first segments 94 of bars 14, 16 and support the cabinet assembly 12. To move the work station unitarily, the work station can be pushed upon castors 100 from a position in front of the keyboard support plate 20. Feet 116, 118 are radiussed to enable them to easily slide over a floor surface. Thereafter, the work station may be directed to a new location.
Moreover, the subject invention provides a work station having superior acoustic insulative properties relative to the surrounding environ. The concave user station defined by the partition walls 110, 112, 114 serve to substantially enclose the user on three sides. Placement of the speakers 32 within the cavity 182 and pointed forward, reduces the sound escaping to the sides of the work station. The sound is directed into the concave user station defined by the partition 18 at the user. Disruption to the surrounding area is accordingly minimized.
The concave configuration of the user station defined by partition 18 further serves to visually isolate the user from the surrounding area. This reduces the level of visual distraction from outside to inside the partition 18 and vice versa. Thus, the partition 18 functions to acoustically and visually isolate the work station occupant and is particularly well suited for busy environments such as the classroom.
A further advantage of the subject invention is that all components of the computer system are secured from unwanted unauthorized exposure to the user of the work station. The CPU is isolated behind the partition and within the compartment 35 of the cabinet 12. The doors 70, 72 are secured via latch 71 into the detents 192, 194 (FIG. 7) to prevent the doors from being opened. The latch 71 preferably can be a simple rotary finger actuated by a latch knob. Alternatively, if more security is desired, a lockable latch mechanism may be incorporated openable by a key of a type common in the industry.
The CPU is contained within the cabinet and cables from peripheral devices are routed into the cabinet 12. Cables from the keyboard positioned upon keyboard support plate 20 are routed through slots 156 and 136 of the insert 22 and plate 20, respectively, and thence through the lower window portion 122 and into the compartment 35. Likewise, speaker wires are routed rearwardly from speaker cavity 182 and into the cabinet compartment 35. The speakers 32 are isolated by the lower portion 178 of bezel plate 26 and the controls of the speakers and the wires connecting the speakers to the CPU are thereby rendered inaccessible to a user of the work station absent a removal of plate 26. Tampering with the speakers and their connection wires is, accordingly, thwarted.
The monitor 28 is positioned upon the top panel 78 and the screen thereof extends through window 120 of the partition 18 to a forward side. The bezel plate 26 attaches to the forward side of the partition 18 and lower bezel plate portion 178 obscures controls to the video monitor that are typically placed below the screen. Thus, access to such controls is not permitted unless the plate 26 is removed. Once set and plate 26 attached, the vulnerability of the controls to the monitor from unauthorized tampering is eliminated. Cables from the monitor are routed down through aperture 86 in the top panel 78 and into compartment 35 for connection to the CPU.
Similarly, the bezel plate 22 secures the keyboard to the keyboard support plate 20 and protects the keyboard from removal or tampering. The cable to the keyboard routes rearwardly through the lower window opening 122 and into the compartment 35.
It will further be appreciated that the S-shaped bars 14, 16 provide a structural linkage connecting the cabinet 12, keyboard plate 20, and partition 18 together. The segments 94 of the bars 14, 16 are anchored to the cabinet bottom panel 36; mid-segments 96 of the bars reside within the bar channels 184, 186 of the partition (FIG. 7), and segments 98 of the bars extend through the partition window portion 122 and fixedly connect to the keyboard support plate 20. A structural integrity results from the interconnection of the major work station components by the bars 14, 16.
While the above describes the preferred embodiment of the subject invention, the invention is not intended to be limited thereto. Other embodiments, which will be apparent to one skilled in the art, that utilize the teachings herein set forth are intended to be within the scope and spirit of the invention. | A mobile computer work station for a personal computer is disclosed comprising a wheel mounted cabinet (12) for enclosing the computer CPU therein and supporting a computer monitor thereon. A concave vertical partition (18) mounts to a forward side of the cabinet (12) and defines a three sided user station providing improved acoustic and visual isolation to the user. A window (120) extends through the partition (18) and receives the screen of the computer monitor therein. A bezel plate (26) affixes to a forward side of the partition (18) and surrounds the window (120). A lower portion (122) of the plate (26) protects the controls to the monitor there behind from unauthorized tampering. A speaker cavity is defined behind the lower plate portion (122) likewise isolated thereby from unauthorized contact. S-shaped support bars (14, 16) structurally connect cabinet (12) and partition (18) and support a keyboard support plate (20) upon bar segments (98) within the concave partition (18). A second bezel plate (24) attaches to a top surface of plate (20) to retain a touch sensitive keyboard component thereon. | 0 |
This application claims benefit of U.S. Provisional application Ser. No. 60/108,098, filed Nov. 12, 1998.
BACKGROUND OF THE INVENTION
The present invention relates to a furnace for producing dental prostheses with a muffle, whereby the furnace comprises a piston driven by a drive which can be introduced into the muffle for exerting pressure onto the dental material, whereby a pressure sensor for detecting the pressure exerted by the piston is provided.
Furnaces for producing dental prostheses or dental replacement parts comprised of dental materials, especially dental ceramics, have been known for a long period of time. A plunger-type piston applies pressure onto the dental material positioned in the muffle whereby the muffle together with at least the lower portion of the piston is heated in the furnace. The furnace heats the muffle and thus the dental material for such a length of time until the dental material, under pressure applied by the piston, has completely filled the voids present in the muffle for producing the dental prostheses.
From German Patent 664 133 it is known that the inclusion formation of bubbles can be avoided when pressure is applied for an extended period of time.
The drive of the piston can be provided either by weight application or pneumatically or electrically with corresponding drive devices. For providing a cycle time as short as possible, while preventing inclusion of bubbles, it is favorable when the advancing speed of the piston is controllable. In this respect, pneumatically or electrically driven drive devices have been successfully used.
Different types of such furnaces are known. It has also been suggested already to provide an electric pressure cylinder design for driving the piston. For detecting the working pressure of the piston, the current uptake of the drive motor for the corresponding drive spindle is employed whereby, in addition, a travel/time measurement is carried out.
It is an object of the present invention to improve a muffle furnace of the aforementioned kind such that, while preventing bubble inclusion, an improved product quality of the aforementioned dental prostheses is ensured.
SUMMARY OF THE INVENTION
This object is inventively solved in that the pressure sensing device comprises a deformation member that is loaded at one side, especially at the rear end of the piston with respect to the muffle, by a counter force of the piston and is supported with its other side at the muffle furnace.
The inventive measures, i.e., loading one side of the pressure sensing device with a counter force of the piston, take into account especially the elasticity of the piston, which, when employing travel measurement, remains unaccounted for, for the control function, respectively, the desired control parameters. Surprisingly, a very precise observation of the operating perimeters of the furnace and of the piston can be ensured. The inventive solution detects exactly the pressure forces acting within the piston whereby it is essential that the entire load of the piston is taken into consideration for computation.
In a preferred embodiment of the inventive furnace, a deformation member, which is especially made of metal, is positioned between the rear end of the drive and a support provided at the muffle furnace. This embodiment allows a realization of the pressure sensing device that is not prone to fatigue or aging.
In a further preferred embodiment of the invention, the pressure sensing device is arranged between the end of the piston, which is remote from the pressure-applying end of the piston, or the drive provided thereat and a counter plate. The drive is provided between the piston and the counter plate and is preferably a step motor. The entire force which is produced by the drive is then received by the counter plate and introduced into the pressure sensing device which is secured by pull elements that are connected to the bottom plate of the muffle.
Thus, a closed force circuit is provided. It is understood that the pressure force of the piston is distributed onto all employed pull elements. Inventively, it is especially favorable when the pressure sensing device is arranged coaxially so that angular deviations are compensated or arranged.
In another preferred embodiment, a homogenous rubber plate is provided as the deformation member. It supports one of the sensor elements while the other sensor element is supported at the sensor plate.
In this embodiment, a defined portion of the force produced by the drive can be detected by the pressure sensor whereby this portion corresponds to the surface area occupied by the pressure sensor at the surface area of the deformation element.
When, for example, a maximum force of 300 N is produced by the drive, a precision pressure sensor with a measuring range of 30 N can be employed which takes up a surface area of {fraction (1/10)} of the total surface area of the deformation member.
It is especially preferred to provide a drive comprising a step motor and to preassemble the drive as a complete drive unit. When needed, the preassembled unit is attached by an adapter to already existing furnaces for improving the manufacturing precision. The preassembled drive unit allows to adjust the initial pressure exerted on the deformation member to such a low level that it remains, for example, under half the measuring precision of the pressure sensor. When the measuring precision of the pressure sensor is, for example, 0.2%, and when the maximum force to be applied by the piston is 300 N, the initial securing force which acts on the deformation member can be adjusted such that it does not surpass 3 N. In this manner, on the one hand, a safe securing action is ensured and, on the other hand, it is ensured that no measurable false readings are produced by mounting the drive unit.
Even though, in principle, a controlled dc motor for providing the drive force can be used, it is preferred to employ a step motor. It comprises preferably a threaded spindle which is a unitary part of the drive axle and supports a threaded sleeve. The threaded sleeve transforms the rotational movement into a linear movement in accordance with the pitch of the thread. It is understood that a rotational stop is provided which prevents rotation of the threaded sleeve. Such a rotational stop can be, for example, positioned with minimal play at one of the pull elements and can be embodied as a stop that acts in both rotational directions. Such a stop, in a modified embodiment, can also serve as a base for providing a travel sensor. For this purpose, the stop can either be coupled to a potentiometer slide or can provide an optical means that indicates the exact position of the piston by a binary code.
Surprisingly, the inventive coaxially arranged drive exhibits a substantially improved driving precision, especially in comparison to a pneumatic drive or a drive with a motor that acts on a toothed piston rod. The axial force application direction eliminates angular errors and the resulting frictional losses, respectively, reduces frictional losses to a neglectable magnitude.
It is especially advantageous that for a complete pressing of the material into the muffle voids, no air buffers are present so that the drive system has a very minimal elasticity coefficient. When employing a step motor as the drive, each individual step of the motor provides a substantial increase of the drive force. The travel/force characteristic line of the inventive furnace is thus advantageously suddenly very steep so that an instant detection of the end of the pressing step can be realized.
In this context it is especially advantageous that, inventively, the end of firing within the furnace can be coupled to an exact point in time which is defined by the end of the pressing step. After completion of a programed, advantageously fixedly adjusted post-pressing period, in an advantageous embodiment the electrically driven pivot mechanism of the furnace cover can be pivoted so that the muffle can be automatically and quickly cooled by opening automatically the furnace chamber.
This embodiment of the furnace is especially advantageous for firing lithium disilicate glass ceramics which exhibit a very strong reaction with the embedding material in the hot state of the embedding material. The intensity of the reaction directly depends on the exposure time and is accordingly substantially reduced when the end of the firing process can be detected and a cooling process can be automatically started.
This solution provides an especially advantageous progress with respect to conventional solutions in which a time control was used and the end of the pressing step could not be detected within a time period of less than three minutes. The inventive solution thus allows to reduce the processing time by up to three minutes.
According to a further especially advantageous aspect of the invention, the inventive solution may eliminate a subsequent etching with acid such as HF so that the respective manufacturing time period is no longer needed and a more precise fitting of the dental prostheses can be achieved.
Inventively, it is further advantageous to adapt the advancing speed of the piston with respect to the speed as well as the force so that an optimized adaptation to the specified pressing and firing task can be performed. In a preferred embodiment a constant force, for example, 250 N is first applied and a constant speed results in an increase of the force whereby reaching of the maximum set-point driving force coincides with the end of the pressing step.
With a programable adaptation to different viscosities but also to different reactivity in regard to the embedding material, the different types of glass ceramic materials can be taken into account. It is also possible by providing free programing to adapt the inventive furnace to currently unknown materials of the future so that respective pressing steps can be provided and optimized for such materials.
It is especially advantageous that the preferred embodiment of embodying the drive as a step motor, in combination with the inventive pressure sensing device, prevents overloading of the step motor and thus the loss of steps. The pressure sensing device controls the step motor such that no overload can occur so that the advancing travel for the pressing step always corresponds to the preset values and the step motor operates within safe limits without requiring additional travel sensors.
It is especially advantageous that the inventive furnace allows to considerably shorten the exposure time of the ceramic to be pressed in the embedding mass. The switch off criteria can be precisely determined and it is also possible to employ ceramics with fine channels having inherently a higher flow resistance. By shortening the exposure time, the reaction between the ceramic to be pressed and the embedding material can be greatly reduced or prevented so that new high-quality materials which are comparatively reactive can be employed as a ceramic to be pressed. The invention can also be safely used for fine dental bridge parts due to the slow force build-up during pressing.
A further advantage of the inventively improved switch-off criteria is the shortening of the pressing step so that the productivity of the inventive furnace in comparison to those of the prior art is improved. Furthermore, the manufacturing precision is improved when etching of the dental prostheses is no longer needed and the surface of the dental prostheses is more smooth and more visually pleasing.
BRIEF DESCRIPTION OF THE DRAWINGS
The object and advantages of the present invention will appear more clearly from the following specification in conjunction with the accompanying drawings, in which:
FIG. 1 shows a view of a portion of the inventive furnace, showing partly in section the drive and the pressure sensing device;
FIG. 2 shows a bottom view in the direction of arrow II—II of FIG. 1 representing the unit receiving the drive and the pressure sensing device;
FIG. 3 shows an enlarged representation of the pressure sensing device of the embodiment according to FIG. 1;
FIG. 4 shows a representation of a further embodiment of a portion of the inventive furnace.
DESCRIPTION OF PREFERRED EMBODIMENTS
The present invention will now be described in detail with the aid of several specific embodiments utilizing FIGS. 1 though 4 .
The embodiment of the inventive furnace 10 represented in FIG. 1 has a muffle 12 which is covered in a well-known manner by a hood.
A piston 14 and, in the shown embodiment, pull elements 16 and 18 extend through the hood whereby, according to a modified embodiment, it is suggested that the pull elements 16 and 18 extend external to the hood to a non-represented bottom plate on which the muffle with the dental material can be placed.
The furnace hood can be heated by known means and melting of the dental material allows movement of the piston 14 in the downward direction so that the dental material can fill the hollow spaces or voids of the muffle for forming the dental prostheses.
The piston 14 is connected axially to a drive 20 which comprises a step motor 22 . The step motor 22 is supported at the side facing away from the piston 14 on a sensor plate 24 of a pressure sensing device PSD. The sensor plate 24 supports a pressure sensor 26 . The pressure sensor 26 rests together with a sensor plate 24 at a deformation member 28 which is preferably a rubber or silicone plate. The deformation member 28 is supported in the upward direction across its entire surface area at a support plate 30 which is connected fixedly to the pull elements 16 and 18 .
The step motor 22 comprises a shaft 31 which is an integral part of a drive spindle 32 . A nut 34 is connected to the drive spindle 32 which is fixedly connected to a sleeve 36 . The sleeve 36 thus functions as a threaded sleeve. According to another embodiment, it is suggested to provide the sleeve itself with a corresponding inner thread and to turn the sleeve downward of the inner thread to produce a blind bore.
Both embodiments have in common that independent of the position of the sleeve 36 relative to the drive spindle 32 the engagement area, i.e., the axial length along which the threaded engagement between drive spindle 32 and sleeve is realized, is identical. Accordingly, the frictional drive forces are also identical so that the step motor substantially can be actuated with the same drive currents and thus no additional non-linearity is introduced.
The sleeve 36 receives in the receiving opening 38 the piston 14 . The piston 14 is received without play whereby optionally for facilitating insertion an insertion slant (not represented in FIG. 1) may be provided. It is especially preferred that the end face 40 of the piston 14 which is opposite the acting end (pressure-applying end) of the piston is supported over a large surface area in order to avoid deformation of the sleeve 36 and the piston 14 .
The piston 14 is preferably comprised of a ceramic material while the sleeve 36 , for example, is comprised of stainless steel.
In order to prevent rotation of the sleeve 36 upon actuating the step motor 22 , a rotational stop 42 is provided which, as can be seen in FIG. 2, surrounds the pull element 18 in a substantially U-shaped manner so that a rotation of the sleeve 36 is prevented. The pull element 18 is comprised preferably of polished steel and the stop 42 can glide substantially without play and thus with minimal friction thereat, whereby the stop 42 is securely attached to the sleeve 36 .
The drive 20 is received together with the pressure sensing device PSD in the pre-assembled unit 44 . The unit 44 extends from the counter plate 30 to the support plate 46 whereby the two plates 30 and 46 are supported at one another by two support rods two of which, 50 and 52 , are shown in FIG. 1 .
Preferably, the support rods 50 and 52 are embodied as threaded rods secured by lock nuts so that the spacing between the counter plate 30 and the support plate 46 can be adjusted. The support plate 46 has a central cutout 60 in which the projection 62 of the step motor 22 is received. A flange 64 of the step motor 22 surrounds the projection 62 and is supported at the support plate 46 so that upon loading by the counter force of the piston 14 the step motor 22 is slightly removed from the support plate 46 but is securely guided in the cutout 60 while the deformation element 28 is compressed.
As can be seen in FIG. 1, the unit 44 is fastened with threaded bolts 70 , 72 to the pull elements 16 and 18 in the form of pull rods. This arrangement together with the embodiment of the sleeve 36 placed on the piston 14 allows a subsequent assembly of the inventive drive unit 44 which can be correspondingly pre-assembled and adjusted before it is mounted on the furnace. Preferably, the spacing between the support plate 46 and the counter plate 30 is such that the step motor 22 presses slightly onto the deformation member 28 without compressing it to a noticeable extent. This position corresponds to the zero loading of the pressure sensing device PSD which is electrically connected to a non-represented a control circuit for the step motor and the furnace.
FIG. 2 shows that instead of the two pull elements 16 and 18 shown in FIG. 1 a total of three such pull elements 16 , 18 , 74 arranged on the corners of a triangle can be realized. Identical reference numerals referred to same parts in the Figures so that no additional explanation is required for the parts. The support plate 46 in the shown embodiment is substantially triangular whereby it is understood that any other suitable guide can be employed without leaving the gist of the invention.
FIG. 2 shows also the arrangement of a travel sensor 76 which operates based on a potentiometer or by optical encoding and is fastened to the sleeve 36 .
FIG. 3 shows the design of the pressure sensing device PSD. The counter plate 30 is secured by the deformation member 28 at a spacing from the sensor plate 24 . The sensor plate 24 comprises a central cutout 80 having a surface area corresponding to {fraction (1/10)} of the surface area of the sensor plate 24 and corresponding in its dimensions to the actual pressure sensor 26 received therein. The pressure sensor 26 has two spaced apart plates as sensor elements 82 , 84 . The change in distance between the sensor elements is then transformed into electric signals as is known in the prior art. An example for such a pressure sensor 26 is a piezoelement or a capacitive pressure sensor.
Upon compression of the sensor plate 24 and of the counter plate 30 , the deformation member 28 is compressed. Due to the elastic properties of the deformation member 28 it thus substantially uniformly applies pressure across its entire surface area and thus also onto the pressure sensor 26 .
Since the greater portion of the surface area of the deformation member 28 rests at the sensor plate 24 and not at the pressure sensor 26 , the supporting action is thus distributed over substantially large portions directly between the sensor plate 24 and the deformation member 28 . A proportional smaller force is thus received by the pressure sensor 26 so that for an increasing pressure it will emit a correspondingly greater output signal.
It is understood that the pressure sensing device PSD comprised of sensor plate 24 , counter plate 30 , deformation member 28 , and pressure sensor 26 is already calibrated. For this purpose, it is possible to apply for a short period of time an increasing and known force, to plot this force as a function of the usually non-linear output signal of the piezoelement and save the results so that the corresponding measured values can be entered directly into the electronic control circuit for the step motor.
It is understood that instead of the piezoelement any other suitable force uptake, for example, strain gauge elements can be used. It should be noted that even for a strain gauge element a systematic non-linearity can be compensated by performing a calibration step and saving the calibration results.
While the inventive support of the sensor element 84 at the muffle furnace is preferably ensured by supporting the sensor element 84 at the counter plate 30 , which is connected fixedly by the pull elements to the bottom plate for the muffle, it is understood that an indirect support at the muffle furnace is also possible in which the pull elements are connected to the pivotable furnace hood which, during firing, is in a defined position relative to the muffle.
The embodiment according to FIG. 4 shows a modified design of the inventive furnace which is especially preferred. In this embodiment the pressure sensing device PSD comprises a deformation member 28 which is embodied as a bending bar having on one surface thereof a strain gauge 86 . The bending bar 28 is securely fastened to a support 88 which is itself fixedly connected to the muffle furnace.
The bending bar is comprised in the shown embodiment of aluminum and has a central cutout 90 which separates a pull leg 92 and a pressure leg 94 from one another. The cutout 90 and the corresponding legs 92 , 94 are shown in dashed lines in FIG. 4 because a cover 96 covers this sensitive area including the strain gauge 86 .
The drive 20 is connected to the deformation member 28 at the end adjacent to the pull leg 92 and supported on the support 88 . For centering, a mandrel 98 is provided at the deformation member 28 which is supported in the shown embodiment at the sensor plate 24 which is a pressure plate.
Despite this one-sided support action, the represented embodiment allows for an especially precise detection of the advancing force without being subject to fatigue. This embodiment is especially suitable for low viscosity ceramics to be pressed with short residence time of the ceramic in the embedding material.
The present invention is, of course, in no way restricted to the specific disclosure of the specification and drawings, but also encompasses any modifications within the scope of the appended claims. | A muffle furnace for producing dental prosthesis has a muffle into which dental material is placed and a drive to which a piston is connected. The piston is moveable by the drive into the muffle to apply pressure onto the dental material. A pressure sensing device for measuring pressure applied to the dental material is provided. The pressure sensing device has a pressure sensor and a deformation member having a first side and a second side. The first side of the deformation member is subjected to a counter force of the piston and the second side of the deformation member is fixedly attached to the muffle furnace. | 5 |
[0001] This is a continuation-in-part application of application Ser. No. 10/785174 filed Feb. 24, 2004, now pending.
BACKGROUND OF THE INVENTION
[0002] (1) Field of the Invention
[0003] This invention relates to a heat pipe, in particular, a microchannel flat-plate heat pipe used for heat dissipation for a central processing unit (CPU) or other electronic integrated circuit (IC) chips.
[0004] (2) Brief Description of Related Art
[0005] The latest generation of Pentium IV CPU generates power more than 100 watts (Joule/sec). In order to maintain its normal performance and avoid overheating of the unit, more effective heat dissipating mechanism is needed. U.S. Pat. No. 5,880,524 discloses a heat pipe for spreading the heat generated by a semiconductor device as shown in FIG. 1 . A cavity 105 is enclosed by a base metal 100 for a working liquid (not shown in the figure) to recycle. Heat sink fins 101 are arranged on the top of the base metal 100 for heat dissipation. Heat transfer medium 102 is under the base metal 100 to contact with a CPU.
[0006] A two-phase vaporizable liquid resides within the cavity 105 and serves as the working fluid (the coolant) for the heat pipe. A metal wick 103 is disposed on the inner walls to form a recycling loop within cavity 105 to facilitate the flow of the working fluid within the cavity. The working liquid in the cavity 105 flows in a direction as shown in arrows in FIG. 1 . Firstly the working liquid is absorbed in the bottom portion of the wick 103 . It evaporates when heat is transferred from the CPU and then condenses on the top portion of the wick 103 . Heat is further transferred upward to the heat sink fins 101 . The condensed liquid absorbed in the top portion of the wick 103 is then moved to the lower portion of the wick 103 due to capillary action of the wick 103 .
SUMMARY OF THE INVENTION
[0007] An objective of this invention is to devise a coolant recycle mechanism with space passages as part of the recycling passage to decrease the friction for the coolant flow in a heat pipe. Another objective of this invention is to devise a coolant recycle mechanism with parallel grooves as a part of the passage to decrease the friction for the flow of the working fluid. A further objective of this invention is to devise a more effective heat dissipation mechanism for a heat pipe. By using space passages, parallel grooves or a combination of both as part of the passage, the friction for the liquid flow is reduced and the capillary action effectively enhances the recycling of the coolant.
BRIEF DESCRIPTION OF THE DRAWINGS
[0008] FIG. 1 Prior art.
[0009] FIG. 2 First embodiment of this invention.
[0010] FIG. 3 Enlarged plane view of the recycle mechanism of FIG. 2 .
[0011] FIG. 4 Explosive perspective view of the recycle mechanism of FIG. 2 .
[0012] FIG. 5 Second embodiment of this invention.
[0013] FIG. 6 Third embodiment of this invention.
[0014] FIG. 7 Fourth embodiment of this invention.
[0015] FIG. 8 Fifth embodiment of this invention.
[0016] FIG. 9 Sixth embodiment of this invention.
[0017] FIG. 10 Seventh embodiment of this invention.
[0018] FIG. 11 Eighth embodiment of this invention.
[0019] FIG. 12 Vertical use of the invention.
[0020] FIG. 13 Ninth embodiment of this invention.
[0021] FIG. 14 Tenth embodiment of this invention.
[0022] FIG. 15 Eleventh embodiment of this invention.
[0023] FIG. 16 Twelfth embodiment of this invention.
[0024] FIG. 17 Thirteenth embodiment of this invention.
[0025] FIG. 18 Fourteenth embodiment of this invention.
[0026] FIG. 19 Fifteenth embodiment of this invention.
[0027] FIG. 20 Sixteenth embodiment of this invention.
[0028] FIG. 21 Seventeenth embodiment of this invention.
[0029] FIG. 22 Eighteenth embodiment of this invention
[0030] FIG. 23 Explosive perspective view of the embodiment FIG. 22 .
[0031] FIG. 24 Nineteenth embodiment of this invention.
[0032] FIG. 25 Twentieth embodiment of this invention.
[0033] FIG. 26 Twenty-first embodiment of this invention.
[0034] FIG. 27 Twenty-second embodiment of this invention.
[0035] FIG. 28 Twenty-third embodiment of this invention.
DETAILED DESCRIPTION OF THE INVENTION
[0036] The principle of this invention is to use space passages, parallel grooves or a combination of both as part of the passage for the flow of the working liquid within a flat-plate heat pipe. FIG. 2 shows the first embodiment of this invention. Cavity 105 is enclosed by a base metal 100 . Multiple sections are divided in the cavity 105 for the recycling of the working liquid. The working liquid moves in a direction following the arrows shown in the figure.
[0037] FIG. 3 shows an enlarged plane view of the recycle mechanism in the cavity 105 of FIG. 2 . There are four sets of parallel grooves shown in this design. A first set of left parallel grooves 201 and a second set of left parallel grooves 202 are arranged on the left of the wick 203 . A third set of right parallel grooves 201 and a fourth set of right parallel grooves 202 are arranged on the right side of the wick 203 . The two sets of grooves 201 and 202 are separated with an isolation plate 205 . The recycling principle for the left two sets of grooves 201 and 202 is exactly the same as that for the right-side two sets of grooves 201 and 202 , and therefore only two left-side grooves are described below.
[0038] Working liquid (not shown) is absorbed in the wick 203 . The wick 203 can be made of sintered copper (Cu) powder, sintered nickel (Ni) powder, or sintered stainless-steel powder. Alternatively, the wick 203 can be made of single-layer or multi-layer of metal wire mesh (not shown) or metal wire cloth (not shown). When the heat pipe is attached to a heat generating unit such as a central process unit (CPU), a certain amount of the working liquid in the wick 203 is heated and vaporized as shown by the arrows. Part of the vapor condenses on the inner top surface within the cavity 105 , which is enclosed by the base metal 100 . Part of the vapor enters a first set of parallel grooves 201 to condense. The condensed liquid is collected in the corners of the parallel grooves. The liquid is then driven by the vapor flow and the capillary action to a second set of parallel grooves 202 under the first set of parallel grooves 201 through a slot 204 . The conveying slot 204 is located at a common end of the two sets of grooves to connect the two sets of grooves 201 and 202 . The wick 203 is located on the other end of the grooves 202 and has a height no less than the height of the grooves 202 . The evaporation of the liquid in the wick 203 leads to a liquid-vapor interface within the wick 203 . This liquid-vapor interface results in a capillary pulling force on the working liquid in grooves 202 toward the wick 203 to make a full cycle: liquid→vapor→cooling→liquid, following the arrows as shown in FIG. 3 .
[0039] FIG. 4 shows the explosive perspective view of the recycle mechanism of FIG. 2 . The parallel grooves 201 and 202 can be made separately before being connected together. Alternatively, the parallel grooves 201 and 202 can also be made integrally as a single body by molding or extrusion, or by etching, cutting, or machining on a metal plate. The cross-sectional shape of the grooves is triangular as illustrated, or of other shapes, such as rectangular or trapezoidal, etc. The base material for grooves 201 and 202 can be metal or nonmetal such as silicon or plastics, etc. may also be used.
[0040] In this embodiment, the grooves 201 and 202 are essentially independent of each other except being communicated by the slot 204 so that the liquid flowing in grooves 202 is not dragged by the vapor flow in grooves 201 in the opposite direction.
[0041] In order for effective condensation of the vapor molecules in the first set of parallel grooves 201 , single-sided grooves in contact with the inner top surface of the cavity is desired for the first set of parallel grooves 201 . However, for the second set of parallel grooves 202 where condensed liquid flows, either a set of single-sided grooves or a set of double-sided grooves works equally well. Double-sided grooves can be made using a corrugated sheet (not shown). Single-sided grooves 202 are shown in FIG. 4 . They can be made by the way of molding, extrusion, or by etching, cutting, or machining on a metal plate.
[0042] FIG. 5 shows a second embodiment of this invention. This embodiment includes a vertical guiding plate 207 above the wick 203 to bridge the wick 203 and the inner top surface of the base metal 100 . The guiding plate 207 allows part of the condensed liquid on the inner top surface to flow downward back to the wick 203 directly. The guiding plate 207 also serves as a strengthener against the inward pressure when the cavity 105 is evacuated.
[0043] FIG. 6 shows a third embodiment of this invention. This embodiment uses an elongated grooves 201 B over the top of the wick 203 .
[0044] FIG. 7 shows a fourth embodiment of this invention. Shown herein is a half-cut piece, with the front surface representing the mid-plane cross-section of the whole unit. This embodiment shows that the first set of parallel grooves and the conveying slot 204 can be integrated with the top part of the base metal 100 to form a top metal base 201 C. The parallel grooves 2011 and the conveying slot 204 can be fabricated by molding, or by cutting, scribing, or etching the base metal 100 .
[0045] FIG. 8 shows a fifth embodiment of this invention. Shown herein is also a half-cut piece, with the front surface representing the mid-plane cross-section of the whole unit. Similar to the fourth embodiment of FIG. 7 , the second set of parallel grooves 202 and the conveying slot 204 can be integrated with the bottom part of the base metal 100 to form the bottom metal base 202 B. Parallel grooves 2021 and the conveying slot 204 can be fabricated by molding, or by cutting, scribing, or etching the base metal 100 .
[0046] FIG. 9 shows a sixth embodiment of this invention. This embodiment shows that the wick 203 in the previous embodiments can be replaced with a pin-array block 203 B. The space between the pins is used to absorb the working liquid by capillary attraction. The vertically open space allows for easy escape of bubbles once they are formed under high heat power conditions. This design is aimed at extending the dry-out limits of the working liquid in the wick 203 .
[0047] FIG. 10 shows a seventh embodiment of this invention. This embodiment uses a different shape of corrugated metal 207 B. The square corrugated metal 207 B used herein differs from the V-shaped corrugated metal 207 in FIG. 5 . Other forms of corrugation are also usable, such as spiral corrugation, S-shaped corrugation, etc., and are not exhaustive in this specification.
[0048] FIG. 11 shows an eighth embodiment of this invention. This embodiment uses a meshed metal 207 C as the guiding plate, rather than the non-meshed guiding plate 207 B in FIG. 10 .
[0049] FIG. 12 shows that the invention as shown in FIG. 3 can be used in a vertical direction. Part of the vapor from the wick 203 condenses directly on the inner wall opposite to the wick 203 or enters the first set of bottom parallel grooves 201 and condenses herein. The condensed liquid flows downward, driven by the vapor flow as well as the gravity, into the liquid pool at the bottom end (not shown). With the combined capillary action of the wick 203 and of the parallel grooves 202 , the working liquid is pulled up back to the wick 203 .
[0050] Part of the vapor from the wick 203 goes up to the first set of top parallel groves 201 and condensed herein. Some of the condensed liquid may drop into the first set of bottom parallel grooves 201 . Some of the condensed liquid is driven upward by the vapor flow to enter the top conveying slot 204 and then the second set of parallel grooves 202 , before it finally flows back to the wick 203 .
[0051] In order to enhance the capillary pulling force on the recycled liquid for those embodiments where two sets of parallel grooves are used, the hydraulic diameters (or the cross-sectional areas of the flow path) of the second set of parallel grooves 202 are made smaller than those of the first set of parallel grooves 201 .
[0052] FIG. 13 shows a ninth embodiment of this invention. This embodiment is a modified version of FIG. 12 . The first set of top parallel grooves 201 in FIG. 12 is replaced with a space A. As the vapor from the wick 203 enters space A, part of it condenses on the inner wall of the metal base 100 . The condensed liquid either drops to the first set of bottom parallel grooves 201 or is driven upward by the vapor flow across the conveying slot 204 into the second set of top parallel grooves 202 . The second set of parallel grooves 202 functions as a passage for the condensed liquid to flow back to the wick 203 by the capillary force provided by the micro grooves 202 and the wick 203 .
[0053] FIG. 14 shows a tenth embodiment of this invention. This embodiment is a modified version of FIG. 12 . The second set of top parallel grooves 202 in FIG. 12 is replaced with a space B. The space B functions as a passage for the condensed liquid to flow back to the wick 203 by gravity and the capillary force provided by the thin space B and the wick 203 .
[0054] FIG. 15 shows an eleventh embodiment of this invention. This embodiment is a modified version of FIG. 12 . The first set of top parallel grooves 201 in FIG. 12 is replaced with a space A; while the second set of top parallel grooves 202 is replaced with a space B. The space B functions as a passage for the condensed liquid to flow back to the wick 203 by gravity and the capillary force provided by the thin space B and the wick 203 .
[0055] FIG. 16 shows a twelfth embodiment of this invention. This embodiment is a simplified version of FIG. 3 or FIG. 4 . A single first set of parallel grooves 201 and a single second set of parallel grooves 202 are used. The recycle mechanism is exactly the same as described in FIG. 3 or FIG. 4 .
[0056] FIG. 17 shows a thirteenth embodiment of this invention. This embodiment is a modified version of FIG. 16 . The first set of parallel grooves 201 in FIG. 16 is replaced with a space A. As the vapor form the wick 203 enters space A, part of it condenses on the inner wall of the metal base 100 . The condensed liquid is driven by the vapor flow across the conveying slot 204 into the second set of parallel grooves 202 . The liquid in the grooves 202 then flows back to the wick 203 by gravity and the capillary force provided by the micro grooves 202 and the wick 203 .
[0057] FIG. 18 shows a fourteenth embodiment of this invention. This embodiment is a modified version of FIG. 16 . The second set of parallel grooves 202 in FIG. 16 is replaced with a space B. The space B functions as a passage for the condensed liquid to flow back to the wick 203 by the capillary force provided by the thin space B and the wick 203 .
[0058] FIG. 19 shows a fifteenth embodiment of this invention. This embodiment is a modified version of FIG. 16 . The first set of parallel grooves 201 in FIG. 16 is replaced with a space A; while the second set of parallel grooves 202 is replaced with a space B. As the vapor form the wick 203 enters space A, part of it condenses on the inner wall of the metal base 100 . The condensed liquid is driven by the vapor flow across the conveying slot 204 into the space B. The space B functions as a passage for the condensed liquid to flow back to the wick 203 by the capillary force provided by the thin space B and the wick 203 .
[0059] FIG. 20 shows a sixteenth embodiment of this invention. This embodiment is a modification to all the previous embodiments. FIG. 20 shows a second wick 204 B inserted into the slot 204 to smooth the liquid flow. The capillary action within 204 B grabs the condensed liquid stronger than a slot 204 as shown in the previous embodiments. This design prevents the vapor from entering the second set of parallel grooves 202 and, therefore, leads to a smoother liquid flow.
[0060] FIG. 21 shows a seventeenth embodiment of this invention. This embodiment is a modification to FIG. 3 by replacing the grooves 202 in the lower section with a space B. The space B functions as a passage for the condensed liquid to flow back to the wick 203 by the capillary force provided by the thin space B and the wick 203 .
[0061] FIG. 22 shows an eighteenth embodiment of this invention. This embodiment uses an elongated wick 203 C as wide as that of the lower section. The middle part of the elongated wick 203 C is used as an evaporator to absorb the heat from a heat-generating device attached below it (not shown). The other parts under the grooves 201 are used as a passage for the liquid to flow back to the middle part of the wick 203 C The wick 203 C can be sintered metal powder, metal wire mesh or metal wire cloth.
[0062] FIG. 23 is the explosive perspective view of the embodiment in FIG. 22 . Two sets of parallel grooves 201 are placed in the two sides of the upper section of the cavity 105 to help collect the condensed liquid.
[0063] FIG. 24 shows a nineteenth embodiment of this invention. A V-shaped corrugated metal 207 is placed on top of the wick 203 C and between the two sets of parallel grooves 201 . FIG. 25 shows a twentieth embodiment of this invention. This embodiment uses a set of elongated grooves 201 B over the top of the long wick 203 C. An isolation plate 205 made of a metal or nonmetal sheet is placed in between the elongated grooves 201 B and the long wick 203 C except for a space 300 arranged for the vapor to enter the grooves 201 B. In this embodiment, the isolation plate 205 can alternatively be made of wire mesh or wire cloth so that a part of the condensed liquid collected in the grooves 201 C can enter the wick 203 C directly without flowing through the conveying slot 204
[0064] FIG. 26 shows a twenty-first embodiment of this invention. This embodiment shows that a V-shaped corrugated wire mesh 302 is used to replace the elongated grooves 201 B in the previous embodiment. The isolation plate 205 can alternatively be made pf wire mesh or wire cloth in this embodiment.
[0065] FIG. 27 shows a twenty-second embodiment of this invention. This embodiment shows that the elongated wick 203 C as in FIG. 25 can be replaced with a corrugated metal wire mesh 302 .
[0066] FIG. 28 shows a twenty-third embodiment of this invention. This embodiment shows that a sheet of wire mesh 304 can be added above the corrugated metal mesh 302 to enhance capillary force, especially for the evaporator.
[0067] While the preferred embodiment of the invention have been described, it will be apparent to those skilled in the art that various modifications may be made without departing from the spirit of the present invention. Such modifications are all within the scope of this invention. | Heat from a heat generating device such as a CPU is dissipated by a heat sink device containing a recycled two-phase vaporizable coolant. The coolant recycles inside a closed metal chamber, which has an upper section and a lower section connected by a conveying conduit, and a wick evaporator placed in the lower section. The liquid coolant in the evaporator is vaporized by the heat from the heat generating device. The coolant vapor enters the upper section and condenses therein, with the liberated latent heat dissipated out through the inner top chamber wall. The condensed coolant is then collected and flows into the lower section, and further flows back to the wick evaporator by capillary action of the evaporator, thereby recycling the coolant. Space or a piece of element with parallel grooves is used to form at least one of the sections to reduce friction in the liquid flow path. | 7 |
CROSS-REFERENCES TO RELATED APPLICATIONS
The present application is a continuation of U.S. application Ser. No. 11/982,238, filed Oct. 31, 2007, now issued as U.S. Pat. No. 7,991,463 (the contents being incorporated herein by reference), which is a continuation of U.S. patent application Ser. No. 10/830,189, filed Apr. 21, 2004, now issued as U.S. Pat. No. 7,963,927 (the contents being incorporated herein by reference), which is a divisional of U.S. application Ser. No. 09/722,070, filed Nov. 24, 2000, now issued as U.S. Pat. No. 7,470,236 (the contents being incorporated herein by reference), which claims priority from U.S. Provisional Application Ser. No. 60/167,416 filed Nov. 24, 1999 (the contents being incorporated herein by reference).
TECHNICAL FIELD
The present invention relates to electromyography (EMG) and to systems for detecting the presence of nerves during surgical procedures.
BACKGROUND OF THE INVENTION
It is important to avoid unintentionally contacting a patient's nerves when performing surgical procedures, especially when using surgical tools and procedures that involve cutting or boring through tissue. Moreover, it is especially important to sense the presence of spinal nerves when performing spinal surgery, since these nerves are responsible for the control of major body functions. However, avoiding inadvertent contact with these nerves is especially difficult due to the high nerve density in the region of the spine and cauda equina.
The advent of minimally invasive surgery offers great benefits to patients through reduced tissue disruption and trauma during surgical procedures. Unfortunately, a downside of such minimally invasive surgical procedures is that they tend to offer a somewhat reduced visibility of the patient's tissues during the surgery. Accordingly, the danger of inadvertently contacting and/or severing a patient's nerves can be increased.
Systems exist that provide remote optical viewing of a surgical site during minimally invasive surgical procedures. However, such systems cannot be used when initially penetrating into the tissue. Moreover, such optical viewing systems cannot reliably be used to detect the location of small diameter peripheral nerves.
Consequently, a need exists for a system that alerts an operator that a particular surgical tool, which is being minimally invasively inserted into a patient's body, is in close proximity to a nerve. As such, the operator may then redirect the path of the tool to avoid inadvertent contact with the nerve. It is especially important that such a system alerts an operator that a nerve is being approached as the surgical tool is advanced into the patient's body prior to contact with the nerve, such that a safety distance margin between the surgical tool and the nerve can be maintained.
A variety of antiquated, existing electrical systems are adapted to sense whether a surgical tool is positioned adjacent to a patient's nerve. Such systems have proven to be particularly advantageous in positioning a hypodermic needle adjacent to a nerve such that the needle can be used to deliver anesthetic to the region of the body adjacent the nerve. Such systems rely on electrifying the needle itself such that as a nerve is approached, the electrical potential of the needle will depolarize the nerve causing the muscle fibers coupled to the nerve to contract and relax, resulting in a visible muscular reaction, seen as a “twitch”.
A disadvantage of such systems is that they rely on a visual indication, being seen as a “twitch” in the patient's body. During precision minimally invasive surgery, uncontrollable patient movement caused by patient twitching, is not at all desirable, since such movement may itself be injurious. In addition, such systems rely on the operator to visually detect the twitch. Accordingly, such systems are quite limited, and are not particularly well adapted for use in minimally invasive surgery.
SUMMARY OF THE INVENTION
The present invention provides methods and apparatus for informing an operator that a surgical tool or probe is approaching a nerve. In preferred aspects, the surgical tool or probe may be introduced into the patient in a minimally invasive cannulated approach. In alternate aspects, the surgical tool or probe comprises the minimally invasive cannula itself.
In a first aspect, the present invention provides a system for detecting the presence of a nerve near a surgical tool or probe, based upon the current intensity level of a stimulus pulse applied to the surgical tool or probe. When a measurable neuro-muscular (EMG) response is detected from a stimulus pulse having a current intensity level at or below a pre-determined onset level, the nerve is considered to be near the tool or probe and thus, detected.
In an optional second aspect of the invention, the onset level (i.e.: the stimulus current level at which a neuro-muscular response is detected for a particular nerve) may be based on EMG responses measured for a probe at a predetermined location relative to the nerve. Specifically, onset levels may first be measured for each of a plurality of spinal nerves, (yielding an initial “baseline” set of neuro-muscular response onset threshold levels), which are then used in the first (nerve detection) aspect of the invention. Therefore, in accordance with this optional second aspect of the invention, a system for determining relative neuro-muscular onset values (i.e.: EMG response thresholds), for a plurality of spinal nerves is also provided. Accordingly, the pre-determined onset level may be compared to the current level required to generate a measurable EMG response for a tool or probe being advanced toward one or more nerves of interest.
In alternate aspects, however, the neuro-muscular onset values that are used to accomplish the first (nerve detection) aspect of the invention are not measured for each of the patient's plurality of spinal nerves. Rather, pre-determined levels of current intensity (below which neuro-muscular responses are detected in accordance with the first aspect of the invention) can instead be directly pre-set into the system. Such levels preferably correspond to specific expected or desired onset threshold values, which may have been determined beforehand by experimentation on other patients.
In the aspect of the invention where initial “baseline” neuro-muscular onset values are determined prior to nerve detection, such onset values can optionally be used to calibrate the present nerve-detection system (which in turn operates to detect whether an minimally invasive surgical tool or probe is positioned adjacent to a spinal nerve).
It is to be understood, therefore, that the present invention is not limited to systems that first determine relative neuro-muscular onset values, and then use these neuro-muscular onset values to detect the presence of a nerve. Rather, the present invention includes an optional system to first determine relative neuro-muscular onset values and a system to detect the presence of a nerve (using the neuro-muscular onset values which have been previously determined). As such, the present invention encompasses systems that also use fixed neuro-muscular onset values (which may simply be input into the system hardware/software by the operator prior to use) when performing electromyographic monitoring of spinal nerves to detect the presence of a spinal nerve adjacent a tool or probe.
In optional aspects, the preferred method of sensing for the presence of a nerve may be continuously repeated as the probe/surgical tool is physically advanced further into the patient such that the operator is warned quickly when the probe/surgical tool is closely approaching the nerve.
In the first (nerve sensing) aspect of the invention, the present nerve-detection system comprises an electrode or electrodes positioned on the distal end of the surgical tool or probe, with an electromyographic system used to detect whether a spinal nerve is positioned adjacent to the surgical tool or probe. A conclusion is made that the surgical tool or probe is positioned adjacent to a spinal nerve when a neuro-muscular (e.g.: EMG) response to a stimulus pulse emitted by the electrode or electrodes on the surgical tool or probe is detected (at a distant myotome location, such as on the patient's legs) at or below certain neuro-muscular response onset values (i.e.: pre-determined current intensity levels) for each of the plurality of spinal nerves. The stimulus pulse itself may be emitted from a single probe, but in an optional aspect, the stimulus pulse may be emitted from separate left and right probes with the signals being multiplexed. As stated above, such pre-determined levels may be pre-input by the operator (or be pre-set into the system's hardware or software) and may thus optionally correspond to known or expected values. (For example, values as measured by experimentation on other patients).
In accordance with the optional second (neuro-muscular response onset value determination) aspect of the invention, the neuro-muscular response onset values used in nerve detection may instead be measured for the particular patient's various nerves, as follows.
Prior to attempting to detect the presence of a nerve, an EMG stimulus pulse is first used to depolarize a portion of the patient's cauda equina. This stimulus pulse may be carried out with a pulse passing between an epidural stimulating electrode and a corresponding skin surface return electrode, or alternatively, between a pair of electrodes disposed adjacent to the patient's spine, or alternatively, or alternatively, by a non-invasive magnetic stimulation means. It is to be understood that any suitable means for stimulating (and depolarizing a portion of) the patient's cauda equina can be used in this regard.
After the stimulus pulse depolarizes a portion of the patient's cauda equina, neuro-muscular (i.e., EMG) responses to the stimulus pulse are then detected at various myotome locations corresponding to a plurality of spinal nerves, with the current intensity level of the stimulus pulse at which each neuro-muscular response is first detected being the neuro-muscular response “onset values” for each of the plurality of spinal nerves.
It is to be understood that the term “onset” as used herein is not limited to a condition in which all of the muscle fibers in a bundle of muscle fibers associated with a particular nerve exhibit a neuro-muscular response. Rather, an “onset” condition may comprise any pre-defined majority of the muscle fibers associated with a particular nerve exhibit a neuro-muscular response.
In an additional aspect of the invention, the relative neuro-muscular response onset values can be repeatedly re-determined (at automatic intervals or at intervals determined by the operator) so as to account for any changes to the response onset values caused by the surgical procedure itself. Accordingly, a further advantage of the present invention is that it permits automatic re-assessment of the nerve status, with the relative neuro-muscular response onset values for each of the plurality of spinal nerves being re-determined before, during and after the surgical procedure, or repeatedly determined again and again during the surgical procedure. This optional aspect is advantageous during spinal surgery as the surgery itself may change the relative neuro-muscular response onset values for each of the plurality of nerves, such as would be caused by reducing the pressure on an exiting spinal nerve positioned between two adjacent vertebrae. This periodic re-determination of the onset values can be carried out concurrently with the nerve sensing function.
Accordingly, an advantageous feature of the present invention is that it can simultaneously indicate to an operator both: (1) nerve detection (i.e.: whether the surgical tool/probe is near a nerve); and (2) nerve status changes (i.e.: the change in each nerve's neuro-muscular response onset values over time). The surgeon is thus able to better interpret the accuracy of nerve detection warnings by simultaneously viewing changes in the various onset levels. For example, should the surgeon note that a particular onset value (i.e.: the current level of a stimulus pulse required to elicit an EMG response for a particular nerve) is increasing, this would tend to show that this nerve pathway is becoming less sensitive. Accordingly, a “low” warning may be interpreted to more accurately correspond to a “medium” likelihood of nerve contact; or a “medium” warning may be interpreted to more accurately correspond to a “high” likelihood of nerve contact.
Optionally, such re-assessment of the nerve status can be used to automatically re-calibrate the present nerve detection system. This can be accomplished by continually updating the onset values that are then used in the nerve detection function.
In preferred aspects, the neuro-muscular response onset values for each of the plurality of spinal nerves are measured at each of the spaced-apart myotome locations, and are visually indicated to an operator (for example, by way of an LED scale). Most preferably, the measuring of each of the various neuro-muscular response onset values is repeatedly carried out with the present and previously measured onset value levels being simultaneously visually indicated to an operator such as by way of the LED scale.
Accordingly, in one preferred aspect, for example, different LED lights can be used to indicate whether the value of each of the various neuro-muscular response onset values is remaining constant over time, increasing or decreasing. An advantage of this optional feature of the invention is that a surgeon operating the device can be quickly alerted to the fact that a neuro-muscular response onset value of one or more of the spinal nerves has changed. Should the onset value decrease for a particular nerve, this may indicate that the nerve was previously compressed or impaired, but become uncompressed or no longer impaired.
In a particular preferred embodiment, example, a blue LED can be emitted at a baseline value (i.e.: when the neuro-muscular response onset value remains the same as previously measured); and a yellow light can be emitted when the neuro-muscular response onset value has increased from that previously measured; and a green light being emitted when the neuro-muscular response onset value has decreased from that previously measured.
In an alternate design, different colors of lights may be simultaneously displayed to indicate currently measured onset values for each of the plurality of spinal nerve myotome locations, as compared to previously measured onset values. For example, the present measured onset value levels for each of the plurality of spinal nerve myotome locations can appear as yellow LED lights on the LED scale, with the immediately previously measured onset value levels simultaneously appearing as green LED lights on the LED scale. This also allows the operator to compare presently measured (i.e. just updated) neuro-muscular response onset values to the previously measured neuro-muscular response onset values.
In preferred aspects, the present system also audibly alerts the operator to the presence of a nerve. In addition, the volume or frequency of the alarm may change as the probe/tool moves closer to the nerve.
In a preferred aspect of the present invention, the neuro-muscular onset values, (which may be detected both when initially determining the relative neuro-muscular response onset values in accordance with the second aspect of the invention, and also when detecting a neuro-muscular onset response to the emitted stimulus pulse from the probe/tool in accordance with the first aspect of the invention), are detected by monitoring a plurality of distally spaced-apart myotome locations which anatomically correspond to each of the spinal nerves. Most preferably, these myotome locations are selected to correspond to the associated spinal nerves that are near the surgical site. Therefore, these myotome locations preferably correspond with distally spaced-apart on the patient's legs (when the operating site is in the lower vertebral range), but may also include myotome locations on the patient's arms (when the operating site is in the upper vertebral range). It is to be understood, however, that the present system therefore encompasses monitoring of any relevant myotome locations that are innervated by nerves in the area of surgery. Therefore, the present invention can be adapted for use in cervical, thoracic or lumbar spine applications.
During both the optional initial determination of the relative neuro-muscular response onset values for each of the plurality of spinal nerves (i.e.: the second aspect of the invention) and also during the detection of neuro-muscular onset responses to the stimulus pulse from the surgical probe/tool (i.e.: the first aspect of the invention), the emission of the stimulus pulse is preferably of a varying current intensity. Most preferably, the stimulus pulse is incrementally increased step-by-step in a “staircase” fashion over time, at least until a neuro-muscular response signal is detected. The stimulus pulse itself may be delivered either between a midline epidural electrode and a return electrode, or between two electrodes disposed adjacent the patient's spine, or from an electrode disposed directly on the probe/tool, or by other means.
An important advantage of the present system of increasing the level of stimulus pulse to a level at which a response is first detected is that it avoids overstimulating a nerve (which may cause a patient to “twitch”), or cause other potential nerve damage.
In optional preferred aspects, the “steps” of the staircase of increasing current intensity of the stimulus pulse are carried out in rapid succession, most preferably within the refractory period of the spinal nerves. An advantage of rapidly delivering the stimulus pulses within the refractory period of the spinal nerves is that, at most, only a single “twitch” will be exhibited by the patient, as opposed to a muscular “twitching” response to each level of the stimulation pulse as would be the case if the increasing levels of stimulus pulse were instead delivered at intervals of time greater than the refractory period of the nerves.
In another optional preferred aspect, a second probe is added to the present system, functioning as a “confirmation electrode”. In this optional aspect, an electrode or electroded surface on the second probe is also used to detect the presence of a nerve, (using the same system as was used for the first probe to detect a nerve). Such a second “confirmation electrode” probe is especially useful when the first probe is an electrified cannula itself, and the second “confirmation electrode” probe is a separate probe that can be advanced through the electrified cannula. For example, as the operating (electrified) cannula is advanced into the patient, this operating cannula itself functions as a nerve detection probe. As such, the operating cannula can be advanced to the operating site without causing any nerve damage. After this cannula has been positioned at the surgical site, it may then be used as the operating cannula through which various surgical tools are then advanced. At this stage, its nerve-sensing feature may be optionally disabled, should this feature interfere with other surgical tools or procedures. Thereafter, (and at periodic intervals, if desired) the second “confirmation electrode” probe can be re-advanced through the operating cannula to confirm that a nerve has not slipped into the operating space during the surgical procedure. In the intervals of time during which this second “confirmation electrode” probe is removed from the operating cannula, access is permitted for other surgical tools and procedures. The second “confirmation electrode” probe of the present invention preferably comprises a probe having an electrode on its distal end. This confirmation electrode may either be mono-polar or bi-polar.
In an optional preferred aspect, the second “confirmation electrode” probe may also be used as a “screw test” probe. Specifically, the electrode on the secondary “confirmation” probe may be placed in contact with a pedicle screw, thereby electrifying the pedicle screw. Should the present invention detect a nerve adjacent such an electrified pedicle screw, this would indicate that pedicle wall is cracked (since the electrical stimulus pulse has passed out through the crack in the pedicle wall and stimulated a nerve adjacent the pedicle).
An advantage of the present system is that it may provide both nerve “detection” (i.e.: sensing for the presence of nerves as the probe/tool is being advanced) and nerve “surveillance” (i.e.: sensing for the presence of nerves when the probe/tool had been positioned).
A further important advantage of the present invention is that it simultaneously monitors neuro-muscular responses in a plurality of different nerves. This is especially advantageous when operating in the region of the spinal cord due to the high concentration of different nerves in this region of the body. Moreover, by simultaneously monitoring a plurality of different nerves, the present system can be used to indicate when relative nerve response onset values have changed among the various nerves. This information can be especially important when the surgical procedure being performed can alter the relative nerve response onset value of one or more nerves with respect to one another.
A further advantage of the present system is that a weaker current intensity can be applied at the nerve detecting electrodes (on the probe) than at the stimulus (i.e.: nerve status) electrodes.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is an illustration of various components of the present invention in operation.
FIG. 2 shows a current intensity staircase for an electromyographic stimulation (nerve status) electrode.
FIG. 3 shows a current intensity staircase for an electromyographic stimulation pulse for a nerve detection electrode disposed on a probe.
FIG. 4 corresponds to FIG. 1 , but also shows exemplary “high”, “medium” and “low” warning levels corresponding to exemplary neuro-muscular response onset levels.
FIG. 5 shows a patient's spinal nerves, and corresponding myotome monitoring locations.
FIG. 6 is an illustration of the waveform characteristics of a stimulus pulse and a corresponding neuro-muscular (EMG) response as detected at a myotome location.
FIG. 7 is a schematic diagram of a nerve detection system.
FIG. 8A is an illustration of the front panel of one design of the present nerve status and detection system.
FIG. 8B is an illustration of the front panel of another design of the present nerve status and detection system.
DESCRIPTION OF THE PREFERRED EMBODIMENT
The present invention sets forth systems for detecting when a nerve is near or adjacent to an electrified surgical tool, probe, cannula, or other surgical instrument. The present invention also involves optional systems for simultaneously determining the “status” (e.g.: sensitivity) of a plurality of nerves.
As will be explained, the present system involves applying a signal with a current level to a probe near a nerve and determining whether an electromyographic “EMG” (i.e.: neuro-muscular) response for a muscle coupled to the nerve is present.
In preferred aspects, the present system applies a signal with a known current level (mA) to a “probe” (which could be midline probe, a cannula, a needle, etc.) Depending on the current level, distance to the nerve, and health of the nerve, an EMG may be detected in a muscle coupled to the nerve. In accordance with preferred aspects, an EMG response is determined to have been detected when the peak-to-peak response of the EMG signal is greater than some level (mVolts). In other words, an EMG response is determined to have been detected when the stimulus current level generates an EMG having a peak-to-peak value greater than a pre-determined level (for example, 60 mV or 80 mV in spinal nerve applications.) Such stimulus current level at which an EMG response is detected is termed the “onset” current level for the nerve.
In optional aspects, the present invention also sets forth systems for determining these onset current values (i.e.: determining the stimulus current level at which an EMG response is detected with a maximum peak-to-peak value greater than a predetermined level). Such onset values may be determined for a plurality of nerves either in absolute terms, or in relation to one another.
The first aspect of the present invention involves nerve detection. In the optional second aspect of the invention, nerve status information may be used to aid nerve detection. The nerve status aspect determines the minimum current level of a signal applied to a probe near a nerve needed to generate onset EMG response for a muscle coupled to a nerve of interest. The present invention may use this determined minimum current level when determining whether a probe is near the same nerve.
In optional aspects, the present invention may involve determining an initial set of “baseline” neuro-muscular response onset values for a plurality of different spinal nerve pathways. This optional second (nerve status) aspect of the present invention is preferably carried out prior to the first (nerve detection) aspect of the invention, with the initial set of “baseline” neuro-muscular onset values then optionally being used in the nerve detection function, as will be explained below. As the optional second aspect of the invention is carried out prior to carrying out the first aspect of the invention, it will be described first.
In the nerve status determination, the minimum current level of a signal applied to a probe needed to generate an onset neuro-muscular response (i.e.: EMG response) is first determined for each of a plurality of nerves, as follows. Referring to FIG. 1 , a patient's vertebrae L1, L2, L3, L4, L5, and S1 are shown. In a preferred aspect of the present invention, a portion of the patient's cauda equina is stimulated (i.e. depolarized). This depolarization of a portion of the patient's cauda equina may be achieved by conducting a stimulus pulse having a known current level between an epidural stimulating electrode 11 and a patient return electrode 13 . Electrodes 11 and 13 are referred to herein as “status” electrodes, as they assist in determining the initial status of the various nerve pathways). The epidural electrode is placed in the epidural space of the spine. Alternatively, the depolarization of a portion of the patient's cauda equina may be achieved by conducting a stimulus pulse having a known current level between a pair of status (baseline) electrodes 12 and 14 , which may be positioned adjacent the (thoracic/lumbar) T/L junction (above vertebra L1), as shown. Status electrodes 12 and 14 may be positioned in-line at the T/L junction, (as shown in FIG. 1 ). Status electrodes 12 and 14 could also be positioned on opposite lateral sides of the T/L junction.
In a preferred aspect, neuro-muscular (i.e., EMG), responses to the stimulus pulse by muscles coupled to nerves near the stimulating electrode are detected by electrodes positioned at each of a plurality of myotome locations MR 1 , MR 2 , and MR 3 on the patient's right leg, and myotome locations ML 1 , ML 2 , and ML 3 on the patient's left leg. The sensing of neuro-muscular responses at these locations may be performed with needle electrodes, or electrodes placed on the surface of the patient's skin, as desired. An EMG response at each location MR 1 to MR 6 is detected when the maximum peak-to-peak height of the EMG response to the stimulus pulse is greater than a predetermined mV value (called “onset”). Accordingly, the current level required to elicit an onset EMG response is called the “onset” current level. As described below, the current level of the stimulus pulse or signal applied to the electrode 11 or electrodes 12 , 14 may be incremented from a low level until an onset EMG response is detected for one or more of the myotome locations MR 1 to ML 3 .
It is to be understood that myotome sensing may be carried out at more than the three distal locations illustrated on each of the patient's legs in FIG. 1 . Generally, as greater numbers of distal myotome locations are monitored, a greater number of spinal nerves corresponding to each of these myotome locations can be individually monitored, thereby enhancing the present system's nerve detection ability over a larger section of the patient's spinal column.
It is also to be understood that the present invention can be easily adapted to cervical or thoracic spinal applications (in addition to the illustrated lumbar application of FIG. 1 ). In this case an appropriate portion of the spinal column is depolarized and myotome-sensing locations are selected according to the physiology of the associated nerves for portion of the spinal column of interest. In exemplary aspects, therefore, preferred myotome-sensing locations may therefore include locations on the patient's arms, anal sphincter, bladder, and other areas, depending upon the vertebrae level where the spinal surgery is to be performed.
In a preferred aspect, the current level of the stimulus signal conducted between status electrodes 11 and 13 (or 12 and 14 ) is incrementally increased in a staircase fashion as shown in the current staircase of FIG. 2 from a low value until an onset EMG response is detected at one or more myotome locations. In a preferred embodiment, onset EMG response peak-to-peak value is between 60 mV and 80 mV. (It is noted, however, that depending on the location the stimulating electrode relative to the nerve corresponding to a myotome and the nerve health/status, an onset EMG response may not be detected as the current level is incremented from the lowest level to the highest level shown in FIG. 2 .) In the illustrated exemplary aspect, the current level is shown as increasing from 4 mA to 32 mA, in eight 4 mA increments where the current level is incremented until an onset EMG response is detected. The present invention is not limited to these values and other current ranges (and other numbers “steps” in the staircase) may also be used, as is desired.
At lower current levels, an onset neuro-muscular (i.e., EMG) responses to the stimulus pulse may not be detected at each myotome ML 1 to MR 3 location. However, as the current level of the stimulus signal is incrementally increased (i.e.: moving up the staircase, step-by-step), an onset neuro-muscular (i.e., EMG) response may eventually be detected at each of the various myotome locations ML 1 through MR 3 for each of the six associated spinal nerves. As noted whether an onset EMG response is detected for myotome depends on the location of the electrode relative to the corresponding nerve and the nerve status/health. For example, when a nerve is compressed or impaired, the current level required to generate an onset EMG response may be greater than the similar, non-compressed nerve at a similar distance from the stimulating electrode. Accordingly, the onset neuro-muscular response for each of the various myotome ML 1 to MR 3 locations may be elicited at different stimulus current levels due at least in part to the various individual spinal nerves being compressed, impaired, etc., and also due simply to differences in the individual nerve pathway sensitivities.
For example, referring to the example illustrated in FIG. 1 , a stimulus signal having an initial current level is conducted between electrodes 11 and 13 (or between electrodes 12 and 14 ). The current level of the stimulus pulse is increased step-by-step according to the intensity staircase shown in FIG. 2 until an onset EMG response is detected at one or more selected myotomes. In particular, a response to the increasing current level stimulus pulse is detected at each of the various myotome locations ML 1 through MR 3 . Because each of the spinal nerve paths corresponding to the various myotome locations ML 1 through MR 3 may have different sensitivities (as noted), different onset EMG responses may be detected at the different onset current levels for different myotome locations.
For example, Table 1 illustrates the current level required to elicit an onset EMG response for myotome location. As seen in Table 1, myotome location ML 1 detected an onset EMG response to the stimulus pulse for a current level of 4 mA. Similarly, myotome MR 2 detected an onset neuro-muscular/EMG response to the stimulus pulse for a current level of 24 mA, etc. Summarizing in tabular form:
TABLE 1
Stimulus Current Level at Which Onset EMG Response is Detected:
ML1 - 4 mA
MR1 - 16 mA
ML2 - 16 mA
MR2 - 24 mA
ML3 - 20 mA
MR3 - 12 mA
The above detected stimulus current levels may then be optionally scaled to correspond to stimulus staircase levels 1 through 8, with the maximum signal strength of 32 mA corresponding to “8”, as follows, and as illustrated for each of Myotome locations ML 1 to MR 3 , as shown in Table 2 based on the levels shown in Table 1.
TABLE 2
Scaled Neuro-muscular Response Onset Values:
ML1 - 1
MR1 - 4
ML2 - 4
MR2 - 6
ML3 - 5
MR3 - 3
Accordingly, by depolarizing a portion of the patient's cauda equina and by then measuring the current amplitude at which an onset neuro-muscular (i.e., EMG) response to the depolarization of the cauda equina is detected in each of a plurality of spinal nerves, (i.e.: at each of the myotome locations corresponding to each of the individual spinal nerves), a method for determining the relative neuro-muscular response for each of the plurality of spinal nerves is provided. As such, the relative sensitivities of the various spinal nerve pathways with respect to one another can initially be determined. This information may represent the relative health or status of the nerves coupled to each myotome location where the stimulating electrode is approximately the same distance from each of the corresponding nerves. For example, the nerve corresponding to myotome location MR 2 required 24 mA to elicit an onset EMG response in the corresponding muscle. Accordingly, this nerve may be compressed or otherwise physiologically inhibited.
These respective stimulus pulse current levels at which an onset neuro-muscular response is detected for each of myotome locations ML 1 through MR 3 are detected may then be electronically stored (as an initial “baseline” set of onset EMG response current levels). In a preferred aspect, these stored levels may then be used to perform nerve detection for a probe at a location other than the midline as will be explained. As noted, once an onset neuro-muscular or EMG-response has been detected for each of the myotome locations, it is not necessary to apply further increased current level signals. As such, it may not be necessary for the current level of the signal to reach the top of the current level staircase (as shown in FIG. 2 ) (provided a response has been detected at each of the myotome locations).
By either reaching the end of the increasing current amplitude staircase, (or by simply proceeding as far up the staircase as is necessary to detect a response at each myotome location), the present system obtains and stores an initial “baseline” set of current level onset values for each myotome location. These onset values may be stored either as absolute (i.e.: mA) or scaled (i.e.: 1 to 8) values. As noted these values represent the baseline or initial nerve status for each nerve corresponding to one of the myotome locations. This baseline onset current level may be displayed as a fixed value on a bar graft of LEDs such as shown in FIG. 8A or 8 B. At a later point, the nerve status of the nerves corresponding to the myotomes may be determined again by applying a varying current level signal to the midline electrodes. If a procedure is being performed on the patient, the onset current level for one or more of the corresponding nerves may change.
When the onset current level increases for a nerve this may indicate that a nerve has been impacted by the procedure. The increased onset current level may also be displayed on the bar graft for the respective myotome (FIG. 8 A/ 8 B). In one embodiment, the baseline onset current level is shown as a particular color LED in the bar graph for each myotome location and the increased onset current level value is shown as a different color LED on the bar graph. When the onset current level decreases for a nerve this may indicate that a nerve has been aided by the procedure. The decreased onset current level may also be displayed on the bar graft for the respective myotome. In a preferred embodiment, the decreased onset current level value is shown as a third color LED on the bar graph. When the onset current level remains constant, only the first color for the baseline onset current level is shown on the bar graph. In one embodiment, a blue LED is depicted for the baseline onset current level, an orange LED is depicted for an increased (over the baseline) onset current level, and a green LED is depicted for a decreased onset current level. In one embodiment when the maximum current level in the staircase does not elicit an onset EMG response for a myotome, the baseline LED may be set to flash to indicate this condition. Accordingly, a clinician may periodically request nerve status (midline stimulation) readings to determine what impact, positive, negative, or neutral, a procedure has had on a patient. The clinician can make this assessment by viewing the bar graphs on the display shown in FIG. 8 for each of the myotome locations.
The above determined initial set baseline neuro-muscular response onset current levels for each nerve pathway (myotome location) may then be used in the first (i.e.: nerve sensing) aspect of the present invention, in which a system is provided for detecting the presence of a spinal nerve adjacent to the distal end of a single probe 20 , or either of probes 20 or 22 . (It is to be understood, however, that the forgoing nerve status system (which may experimentally determine neuro-muscular response onset values) is an optional aspect of the present nerve detection system. As such, it is not necessary to determine such relative or absolute neuro-muscular response baseline onset current levels as set forth above prior to nerve detection. Rather, generally expected or previously known current onset levels may instead be used instead. Such generally expected or previously known current onset levels may have been determined by experiments performed previously on other patients.
In accordance with the first aspect of the present invention, nerve detection (performed as the surgical tool or probe is advancing toward the operative site), or nerve surveillance (performed in an ongoing fashion when the surgical tool or probe is stationary has already reached the operative site) may be carried out, as follows.
The first (nerve detection/surveillance) aspect of the invention will now be set forth.
Returning to FIG. 1 , a system is provided to determine whether a nerve is positioned closely adjacent to either of two probes 20 and 22 . In accordance with the present invention, probes 20 and 22 can be any manner of surgical tool, including (electrified) cannulae through which other surgical tools are introduced into the patient. In one aspect of the invention only one probe (e.g.: probe 20 ) is used. In another aspect, as illustrated, two probes (e.g.: 20 and 22 ) are used. Keeping within the scope of the present invention, more than two probes may also be used. In one preferred aspect, probe 20 is an electrified cannula and probe 22 is a “confirmation electrode” which can be inserted through cannula/probe 20 , as will be explained. Probes 20 and 22 may have electrified distal ends, with electrodes 21 and 23 positioned thereon, respectively. (In the case of probe 20 being a cannula, electrode 21 may be positioned on an electrified distal end of the cannula, or alternatively, the entire surface of the electrified cannula may function as the electrode).
Nerve detection is accomplished as follows. A stimulus pulse is passed between electrode 21 (disposed on the distal end of a probe 20 ) and patient return electrode 30 . In instances where a second probe ( 22 ) is also used, a stimulus pulse is passed between electrode 23 (disposed on the distal end of a probe 22 ) and patient return electrode 30 . In one aspect, electrodes 21 or 23 operate as cathodes and patient return electrode 30 is an anode. In this case, probes 20 and 22 are monopolar. Preferably, when simultaneously using two probes ( 20 and 22 ) the stimulus pulse emitted by each of electrodes 21 and 23 is multiplexed, so as to distinguish between their signals.
It should be understood that electrodes 21 and 23 could be replaced by any combination of multiple electrodes, operating either in monopolar or bipolar mode. In the case where a single probe has multiple electrodes (replacing a single electrode such as electrode 21 ) probe 20 could instead be bi-polar with patient return electrode 30 no longer being required.
Subsequent to the emission of a stimulus pulse from either of electrodes 21 or 23 , each of myotome locations ML 1 through MR 3 are monitored to determine if they exhibit an EMG response.
In a preferred aspect, as shown in FIG. 3 , the intensity of the stimulus pulse passing between electrodes 21 and 30 or between 22 and 30 is preferably varied over time. Most preferably, the current intensity level of the stimulus pulse is incrementally increased step-by-step in a “staircase” fashion. As can be seen, the current may be increased in ten 0.5 mA steps from 0.5 mA to 5.0 mA. This stimulus pulse is preferably increased one step at a time until a neuro-muscular (i.e., EMG) response to the stimulus pulse is detected in each of myotome locations ML 1 through MR 3 .
For myotome locations that exhibit an EMG response as a result of the stimulus pulse, the present invention then records the lowest amplitude of current required to elicit such a response. Subsequently, this stimulus level is interpreted so as to produce an appropriate warning indication to the user that the surgical tool/probe is in close proximity to the nerve.
For example, in a simplified preferred aspect, the staircase of stimulus pulses may comprise only three levels, (rather than the 8 levels which are illustrated in FIG. 3 ). If an EMG response is recorded at a particular myotome location for only the highest level of stimulation (i.e.: the third step on a 3-step staircase), then the system could indicate a “low” alarm condition (since it took a relatively high level of stimulation to produce an EMG response, it is therefore unlikely that the tool/probe distal tip(s) are in close proximity to a nerve). If an EMG response is instead first recorded when the middle level of stimulation (i.e.: the second step on the 3-step staircase) is reached, then the system could indicate a “medium” alarm condition. Similarly, if an EMG response is recorded when the lowest level of stimulation (i.e.: the first step on the 3-step staircase) is reached, then it is likely that the probe tips(s) are positioned very close to a nerve, and the system, could indicate a “high” alarm condition.
As can be appreciated, an important advantage of increasing the stimulus current intensity in a “staircase” function, increasing from lower to higher levels of current intensity is that a “high” alarm condition would be reached prior to a “low” alarm condition being reached, providing an early warning to the surgeon. Moreover, as soon as a “high” alarm condition is reached, the present invention need not continue through to the end (third step) of the staircase function. In preferred aspects, when the current level of the applied signal to the probe ( 20 or 22 ) elicits an EMG response greater than the pre-determined onset EMG response, the current level is not increased.
In the above-described simplified (only three levels of stimulation) illustration of the invention, it was assumed that all nerves respond similarly to similar levels of stimulation, and the proximity (nerve detection) warning was based upon this assumption. Specifically, in the above-described simplified (three levels of stimulation) illustration, there was an assumed one-to-one (i.e. linear) mapping of the EMG onset value data onto the response data when determining what level of proximity warning indication should be elicited, if any. However, in the case of actual spinal nerve roots, there is not only a natural variability in response onset value threshold, but there is often a substantial variation in neuro-muscular response onset values between the nerve pathways caused as a result of certain disease states, such as nerve root compression resulting from a herniated intervertebral disc.
Accordingly, in a preferred aspect of the present invention, the initial “baseline” neuro-muscular EMG response onset value data set which characterizes the relative EMG onset values of the various nerve roots of interest, (as described above), is used to guide the interpretation of EMG response data and any subsequent proximity warning indication, as follows.
Referring back to FIG. 1 and Table 1, the stimulation staircase transmitted between electrodes 11 and 13 (or 12 and 14 ) resulted in measures neuro-muscular (i.e.: EMG) response onset values of 4, 16, 20, 16, 24 and 12 mA at myotome locations ML 1 , ML 2 , ML 3 , MR 1 , MR 2 and MR 3 , respectively. As can be seen, twice the intensity of current was required to produce a neuro-muscular response at MR 2 as was required to produce a neuro-muscular response at MR 3 (since “24” mA is twice as big as “12” mA). Thus, the nerve pathway to MR 3 is more “sensitive” than to MR 2 (since MR 3 is able to exhibit a neuro-muscular response at ½ of the current intensity required to exhibit a neuro-muscular response at MR 2 ). Consequently, during nerve detection, when electrode 21 or 23 (positioned on the distal end of tool/probe 20 or 22 ) is positioned adjacent the nerve root affiliated with MR 3 , twice the current stimulation intensity was required to produce an EMG response. In contrast, when electrode 21 or 23 (on the distal end of tool/probe 20 or 22 ) was positioned adjacent to the nerve root affiliated with MR 2 , the same level of stimulation that produced a response at MR 3 would not produce a response at MR 2 .
In accordance with preferred aspects of the present invention, the sensitivities of the various spinal nerve pathways (to their associated myotomes) are incorporated into the nerve detection function of the invention by incorporating the various neuro-muscular response onset values, as follows.
A decision is made that either of electrodes 21 or 23 are positioned adjacent to a spinal nerve when a neuro-muscular response is detected at a particular myotome location at a current intensity level that is less than, (or optionally equal to), the previously measured or input EMG response onset value for the particular spinal nerve corresponding to that myotome. For example, referring to myotome location ML 1 , the previously determined neuro-muscular response onset level was 4 mA, as shown in Table 1. Should a neuro-muscular response to the stimulus pulse be detected at a current intensity level at or below 4 mA, this would signal the operator that the respective probe electrode 21 (or 23 ) emitting the stimulus pulse is in close proximity to the spinal nerve. Similarly, the neuro-muscular response onset value for myotome location ML 2 was determined to be 16 mA, as shown in Table 1. Accordingly, should a neuro-muscular response be detected at a current intensity level of less than or equal to 16 mA, this would indicate that respective probe electrode 21 (or 23 ) emitting the stimulus pulse is in close proximity to the spinal nerve.
In addition, as illustrated in FIG. 4 , “high”, “medium” and “low” warning levels may preferably be mapped onto each stimulation staircase level for each myotome location. For example, the neuro-muscular onset level for ML 1 was 4 mA, corresponding to the first level of the 8-level status electrode current staircase of FIG. 2 . Thus, the first (4 mA) step on the staircase is assigned a “high” warning level. Level two (8 mA) is assigned a “medium” warning level and level three (12 mA) is assigned a “low” warning level. Thus, if an EMG response is recorded at ML 1 at the first stimulation level, (4 mA), a “high” proximity warning is given. If a response is detected at the second level (8 mA), then a “medium” proximity warning is given. If a response is detected at the third level (12 mA), then a “low” proximity warning is given. If responses are detected only above the third level, or if no responses are detected, than no warning indication is given.
Similarly, for ML 2 , with a onset value of 16 mA, (i.e.: the fourth level in the status electrode current staircase sequence), the “high”, “medium” and “low” warning levels are assigned starting at the fourth step on the status electrode current staircase, with the fourth step being “high”, the fifth level being “medium” and the sixth level being “low”, respectively, as shown. Accordingly, if an EMG response is detected for ML 2 at (or above) the first, second, third, or fourth surveillance levels, (i.e.: 4, 18, 12 or 16 mA), then a “high” warning indication will be given. For a response initially detected at the fifth level (i.e.: 20 mA), then a “medium” warning indication is given. If a response is not detected until the sixth level (i.e.: 24 mA), then a “low” warning indication is given. If responses are detected only above the sixth level, or not at all, then no indication is given. Preferably, each of myotome locations ML 1 through MR 3 are monitored at conditions indicating “high”, “medium” and “low” likelihood of a nerve being disposed adjacent the surgical tool/probe.
As can be seen in FIG. 4 , ten levels are shown for each of the myotome locations, whereas the illustrated status electrode current staircase has only eight levels. These optional levels “9” and “10” are useful as follows. Should scaled level 8 be the minimum onset level at which a neuro-muscular response is detected, levels “9” and “10” can be used to indicate “medium” and “low” warning levels, respectively.
As explained above, the various neuro-muscular response current onset levels used in detection of spinal nerves may either have been either determined in accordance with the second aspect of the present invention, or may simply correspond to a set of known or expected values input by the user, or pre-set into the system's hardware/software. In either case, an advantage of the present system is that different neuro-muscular response onset value levels may be used when simultaneously sensing for different nerves. An advantage of this is that the present invention is able to compensate for different sensitivities among the various spinal nerves.
As can be seen comparing the current intensities of stimulus electrodes 11 and 13 (or 12 and 14 ) as shown in FIG. 2 (i.e.: up to 32 mA) to the current intensities of probe electrodes 21 and 23 as shown in FIG. 3 (i.e.: up to 5.0 mA), the current intensities emitted by probe electrodes 21 and 23 are less than that of electrodes 12 and 14 . This feature of the present invention is very advantageous in that electrodes 21 and 23 are positioned much closer to the spinal nerves. As such, electrodes 21 and 23 do not depolarize a large portion of the cauda equina, as do electrodes 12 and 14 . In addition, the placement of electrode 11 in the epidural space ensures that the electrode is at a relatively known distance from the spinal nerves.
In an optional preferred aspect of the invention, if a neuro-muscular response (greater than the onset EMG response) is detected for all six myotome sensing locations ML 1 through MR 3 before all of the steps on the staircase is completed, the remaining steps need not be executed.
Moreover, if it has been determined that a maximal level of stimulation is required to elicit an EMG response at a particular myotome sensing location, then only the top three stimulation levels need to be monitored during the neuro-muscular response detection sequence. In this case, the top three monitored levels will correspond to “high”, “medium”, and “low” probabilities of the surgical tool/probe being disposed adjacent the a nerve. In another optional aspect, if any of the myotome locations do not respond to the maximum stimulation level (i.e.: top step on the staircase), they are assigned the maximum scale value (i.e.: a “low” warning indication).
Preferably, each of the spinal nerves monitored at myotome locations ML 1 through MR 3 will correspond to nerves exiting from successive vertebrae along the spine. For example, as shown in FIG. 5 , a main spinal nerve 50 will continuously branch out downwardly along the spinal column with spinal nerve 51 exiting between vertebrae L2 and L3 while nerve 52 passes downwardly. Spinal nerve 53 exits between vertebrae L3 and L4 while spinal nerve 54 passes downwardly to L4. Lastly, spinal nerve 55 will exit between vertebrae L4 and L5 while spinal nerve 56 passes downwardly. As can be seen, neuro-muscular (i.e., EMG) response measurements taken at myotome location MR 1 will correspond to EMG signals in spinal nerve 51 , response measurements taken at myotome location MR 2 correspond to EMG signals in spinal nerve 53 , and response measurements taken at myotome location MR 3 correspond to EMG signals in spinal nerve 55 .
In accordance with the present invention, the detection of a neuro-muscular (EMG) response, whether in accordance with the first (i.e.: nerve detection), or second (i.e.: establishing initial “baseline” neuro-muscular response onset values) aspect of the invention, may be accomplished as follows.
Referring to FIG. 6 , an illustration of the waveform characteristics of a stimulus pulse and a corresponding neuro-muscular (EMG) response as detected at a myotome location is shown. An “EMG sampling window” 200 may be defined at a fixed internal of time after the stimulus pulse 202 is emitted. The boundaries of window 200 may be determined by the earliest and latest times that an EMG response may occur relative to stimulus pulse 202 . In the case of stimulation near the lumbar spine, these times are, for example, about 10 milliseconds and 50 milliseconds, respectively.
During EMG sampling window 101 , the EMG signal may optionally be amplified and filtered in accordance with guidelines known to those skilled in the art. The signal may then be rectified and passed through a threshold detector to produce a train of pulses representing the number of “humps” of certain amplitudes contained in the EMG waveform. A re-settable counting circuit may then count the number of humps and a comparator may determine whether the number of pulses is within an acceptable range. By way of example only, the number of acceptable pulses for EMG responses elicited by stimulation in the lumbar spine region may range from about two to about five. If only one pulse is counted, then it is unlikely that a true EMG response has occurred, since true EMG waveforms are typically biphasic (having at least one positive curved pulse response and one negative curved pulse response) resulting in at least two pulses. This pulse-counting scheme helps to discriminate between true EMG waveforms and noise, since noise signals are typically either sporadic and monophasic (and therefore produce only one pulse) or repetitive (producing a high number of pulses during the EMG sampling window).
In a further optional refinement, a separate noise-sampling window may be established to remove noise present in the EMG responses to increase the ability of the system to discriminate between true EMG responses and false responses caused by noise. The boundaries of noise sampling window are chosen such that there is no significant change of a true EMG signal occurring during the window. For example, it may be deemed acceptable that one curved pulse of an EMG response may be comprised primarily of noise, but if more than one curved pulse of an EMG response is primarily comprised of noise, an alarm would be triggered indicating that excess noise is present on that particular channel.
In preferred aspects of the present invention, both the optional second aspect of determining the neuro-muscular response onset values for each of the plurality of spinal nerves and the first aspect of sensing to detect if a nerve is positioned adjacent to a surgical tool/probe are repeated over time. Preferably, the sensing of whether a nerve is positioned adjacent to a surgical tool/probe is continuously repeated in very short intervals of time, such that the operator can be warned in real time as the surgical tool/probe is advanced toward the nerve. The present system of determining the neuro-muscular response onset values for each of the plurality of spinal nerves is also preferably repeated, and may be repeated automatically, or under operator control.
Typically, the above two aspects of the present invention will not be carried out simultaneously. Rather, when the neuro-muscular response onset values are being determined (using electrodes 11 and 13 or 12 and 14 ), the operation of probe electrodes 21 and 23 will be suspended. Conversely, when sensing to determine whether a nerve is positioned adjacent either of probes 20 or 22 , the operation of stimulation electrodes 11 and 13 or 12 and 14 will be suspended. A standard reference electrode 32 may be used for grounding the recording electrodes at the myotomes.
FIG. 6 depicts a particular exemplary embodiment of the present invention. Other embodiments are also possible, and are encompassed by the present invention. Pulse generator 100 creates pulse trains of an appropriate frequency and duration when instructed to do so by controller 118 . By way of example, the pulse frequency may be between 1 pulse-per-second and 10 pulses-per-second, and the pulse duration may be between 20 μsec and 300 μsec. Pulse generator 100 may be implemented using an integrated circuit (IC), such as an ICL75556 (Intensity) or generated by a software module. Amplitude modulator 102 produces a pulse of appropriate amplitude as instructed by controller 118 , and may comprise a digital-to-analog converter such as a DAC08 (National Semiconductor). The output of amplitude modulator 102 drives output stage 103 , which puts out a pulse of the desired amplitude. Output stage 103 may comprise a transformer coupled, constant-current output circuit. The output of output stage 103 is directed through output multiplexer 106 by controller 118 to the appropriate electrodes, either to status (baseline) electrodes 11 and 13 , or to a combination of screw test probe 109 , probe electrode 21 , 23 and patient return electrode 13 . Impedance monitor 104 senses the voltage and current characteristics of the output pulses and controller 118 elicits an error indication on error display 127 if the impedance falls above or below certain pre-set limits. Input keys 116 may be present on a front panel of a control unit of the present invention, as depicted in FIG. 8 , to allow the user to shift between modes of operation.
EMG inputs 128 to 138 comprise the six pairs of electrodes used to detect EMG activity at six different myotome locations. It will be appreciated that the number of channels may vary depending upon the number of nerve roots and affiliated myotomes that need to be monitored. A reference electrode 140 may also be attached to the patient at a location roughly central to the groupings of EMG electrodes 128 to 138 to serve as a ground reference for the EMG input signals. Electrodes 128 to 140 may either be of the needle-type or of the gelled foam type, or of any type appropriate for detecting low-level physiological signals. EMG input stage 142 may contain input protection circuit comprising, for example, gas discharge elements (to suppress high voltage transients) and/or clamping diodes. Such clamping diodes are preferably of the low-leakage types, such as SST-pads (Siliconix). The signal is then passed through amplifier/filter 144 , which may amplify the signal differentially using an instrumentation amplifier such as an AD620 (Analog Devices). The overall gain may be on the order of about 10,000:1 to about 1,000,000:1, and the low and high filter bands may be in the range of about 1-100 Hz and 500 to 5,000 Hz, respectively. Such filtering may be accomplished digitally, in software, or with discrete components using techniques well known to those skilled in the art. The amplified and filtered signal then passes through rectifier 141 , which may be either a software rectifier or a hardware rectifier. The output of rectifier 146 goes to threshold detector 147 which may be implemented either in electronic hardware or in software. The output of threshold detector 147 then goes to counter 148 which may also be implemented by either software or hardware.
Controller 118 may be a microcomputer or microcontroller, or it may be a programmable gate array, or other hardware logic device. Display elements 120 to 127 may be of any appropriate type, either individually implemented (such as with multicolor LEDs) or as an integrated display (such as an LCD). | Methods for determining structural integrity of a bone within the spine of a patient, the bone having a first aspect and a second aspect, wherein the second aspect separated from the first aspect by a width and located adjacent to a spinal nerve. The methods involve (a) applying an electrical stimulus to the first aspect of the bone; (b) electrically monitoring a muscle myotome associated with the spinal nerve to detect if an onset neuro-muscular response occurs in response to the application of the electrical stimulus to the first aspect of the bone; (c) automatically increasing the magnitude of the electrical stimulus to until the onset neuro-muscular response is detected; and (d) communicating to a user via at least one of visual and audible means information representing the magnitude of the electrical stimulus which caused the onset neuro-muscular response. | 0 |
CLAIM OF PRIORITY
The present patent application claims the priority benefit of the filing date of European Application (EPO) No. 04 025 504.4 filed Oct. 27, 2004, which is incorporated herein by reference.
TECHNICAL FIELD
This application relates generally to servicing of a software system landscape by means of transport requests, and more particularly to a method for tracking transport requests and a computer system with a software system landscape and trackable transport requests.
BACKGROUND
Complex software like applicant's SAP R/3 Release 4.5 (SAP) requires customization, e.g. selection of predefined functionality, and adaptation, e.g. addition of or amendment to functionality, as well as other servicing like program and data updates, cf. “SAP System Landscape Optimization” by A. Schneider-Neureither (Ed.), SAP Press, 2004, ISBN 1-59229-026-4, and “SAP R/3 Änderungs-und Transportmanagement” by Metzger and R6 hrs, Galileo Press GmbH, Bonn, Germany, 4 th reprint 2004, ISBN 3-934358-42-X.
Before such servicing may be performed, however, it has to be assured that the customizations, adaptations, program and data updates etc. are free of errors and integrate flawlessly into the software and data environment. In a factory for instance servicing errors are bound to result in costly workflow disruptions due to software malfunction or data corruption. Apart from the servicing side, other use of the software like training of new or inexperienced users may also result in a disruption of the productive system.
Such complex software may therefore be implemented in form of separate logical systems that together form a system landscape. A typical implementation of the aforementioned SAP software for instance may, cf. FIG. 1 , comprise a development system 101 for customizing and development work, a quality assurance system 102 for testing functionality using representative test data, a training system 103 for training new users, and several productive systems 104 , e.g. each for a different factory, for actual productive use. Other or additional users and systems may be defined according to the particular requirements.
The logical systems are identical in large parts, function autonomously and may be run on a single computer. The quality assurance system 102 for example resembles the productive system 104 in that it provides all the functionality, its present data and additionally special test data. New customization settings or adaptations may thus be thoroughly tested in the quality assurance system 102 without jeopardizing the productive system 104 . Likewise, the training system 103 resembles the productive system 104 in that it provides some of the functionality and special test data. A new user using the training system 103 may thus become accustomed to the functionality and observe the effect of his actions, albeit without disturbing the productive system 104 .
A transport management system connects the logical systems and serves to forward approved services to the next stage of the system landscape via logical transport paths 105 . A service may for example be approved in the development system 101 for export. It will then be forwarded to an input buffer of the quality assurance system 102 . Import into the quality assurance system 102 is approved manually by an operator. Once the service has been imported into the quality assurance system 102 , it will automatically be forwarded to an import buffer of the training system 103 and the productive systems 104 where it will be imported following manual approval by an operator.
The operator is in charge of manually assuring that no untested service is imported. For that purpose, he needs to manually compare a service identifier with approved service identifiers. This process is time consuming and bears the risk of errors.
The operator is also in charge of manually assuring that services are imported into their target systems only. A project like adaptation of the software to new legislation may require servicing of particular systems of the system landscape only. Presently, all systems simply forward the imported services to all other systems connected thereto. During the project, a considerable number of services may be required over a considerable period of time, and access to systems that are not affected by the project has to be denied manually by the operator for each and every service. This process is time consuming and bears the risk of errors. An automated way presently is to change system changeability parameters of each system on a project basis, e.g. to specify in each system whether it accepts services corresponding to a particular project. This, too, is time consuming and bears the risk of errors and requires authorized access to each system.
The operator is finally in charge of manually assuring that the services are imported in the correct order. The importance of the correct order is illustrated in FIG. 2 a and FIG. 2 b . An original version 201 of the software and data is first modified by a first service 202 , resulting in modified version 203 , and subsequently by a second service 204 , resulting in modified version 205 , cf. FIG. 2 a . However, if the second service 204 is imported before the first service 202 , the original version 201 is changed into modified version 206 by the second service 204 and subsequently into modified version 207 by the first service 202 , cf. FIG. 2 b . The modified versions 205 and 207 differ and the version 207 will not perform as intended.
In view of the fact that an SAP R/3 implementation may comprise dozens of systems and require thousands of services per month during phases of change, the operator time required becomes considerable as does the risk for errors to occur.
SUMMARY
In one aspect of the invention, a method is provided for tracking transport requests in a system landscape comprising a central control system and a plurality of logical systems interconnected by logical transport paths, a transport request defining a software service for a system in the landscape, the method including feeding a transport request into a logical system of the plurality of logical systems; providing a data supplier in the logical system for supplying, to the central system, data supplier information containing information about the transport request; providing a data collector in the central system for obtaining the data supplier information and accordingly updating status data; and providing a tracking service in the central system, the tracking service allowing to analyze the status data.
In a further aspect of the invention, a computer system is provided comprising: a central control system; a plurality of logical systems; logical transport paths that interconnect the logical systems to form a software system landscape, the logical transport paths allowing a transport request to be fed into a first system of the plurality of logical systems, a transport request defining a software service for a system in the landscape; a data supplier in the system for supplying, to the central system, data supplier information containing information about the transport request; a data collector in the central control system for obtaining the data supplier information and accordingly updating status data; and a tracking service in the central system, the tracking service allowing to analyze the status data.
In a still further aspect of the invention, a computer program product is provided, the computer program product comprising on a storage medium a computer code that upon execution on a computer system performs the method according to the invention.
BRIEF DESCRIPTION OF THE DRAWINGS
Further embodiments of the invention are inferable from the following description and the claims.
FIG. 1 shows a system landscape of the prior art.
FIGS. 2 a and 2 b illustrate services performed in different orders according to the prior art.
FIG. 3 illustrates a system landscape according to an example embodiment of the invention.
FIG. 4 shows an example embodiment of the hardware of a computer system according to the invention.
FIG. 5 shows a flow diagram of a method according to an example embodiment of the invention.
DETAILED DESCRIPTION
The embodiment shown in FIG. 3 shows an SAP R/3 Release 4.5 system landscape 300 with separate logical systems 301 that are here divided into a global part 302 , e.g. at a main development and production facility, and local parts 303 a , 303 b , 303 c , e.g. at other production facilities.
The global part 302 comprising at least a development system 301 a for customizing and development work, a quality assurance system 301 b for testing functionality using representative test data, and a productive system 301 c for actual productive use.
The local part 303 a comprises a development system 301 d for customizing and development work of local adaptations to SAP, e.g. to meet different legal requirements if part 303 a is localized in a different country than the global part 302 . The local part 303 a further comprises a quality assurance system 301 e for testing functionality using representative test data, a training system 301 f for training new users, and a productive system 301 g for actual productive use.
The local part 303 b comprises a development system 301 h , a quality assurance system 301 j and a productive system 301 k , but no training system. The local part 303 c is a two system landscape comprising a development system 301 l and a productive system 301 m only.
The system landscape may be different according to the actual requirements. Fewer or more, different or differently connected or grouped systems 301 may be defined as needed.
The logical systems 301 are identical in large parts and function autonomously. The quality assurance system 301 j for example resembles the productive system 301 k in that it provides all the functionality, its present data and additionally special test data. New customization settings or adaptations may thus be thoroughly tested in the quality assurance system 301 j without jeopardizing the productive system 301 k.
Each system 301 comprises an import buffer 304 and a data supplier 305 . A transport management system connects the logical systems 301 and serves to effect software services across the system landscape via logical directional transport paths 306 . A service may for example relate to customization of a system 301 , e.g. a selection of predefined functionality in the system 301 , or an adaptation of a system 301 , e.g. an addition of or amendment to functionality, or to program and data updates or the like. A system path (not shown) is provided between each system 301 and a central system 307 having a data collector 308 .
The systems 301 of each part 302 , 303 a , 303 b , 303 c and the central system 307 may be located and simultaneously executed in a single computer, or may be distributed across separate hardware. The global part 302 and the local parts 303 a , 303 b , 303 c each run on physically separate computer systems, which themselves may comprise different computers.
An example implementation of the local part 303 a may comprise, cf. FIG. 4 , a data base layer 401 for storing and retrieving business data like a factory inventory, employee data, sales figures etc. The data base layer 401 comprises one or more data base servers 402 and four data bases 403 , one for each of the systems 301 d , 301 e , 301 f and 301 g.
Connected to the data base layer 401 by a suitable network 404 , e.g. a LAN, is an application layer 405 for execution of the software of the systems 301 d , 301 e , 301 f and 301 g . The application layer 405 comprises one or more application servers 406 .
Finally, connected to the application layer 405 by a suitable network 407 , e.g. a LAN, is a presentation layer 408 for the graphical user interface (GUI). The presentation layer 408 comprises dumb terminals 409 , Personal Computers 410 and/or wireless access devices 411 like PDAs.
The method according to an example embodiment of the invention is now described with reference to FIG. 5 and FIG. 3 .
A software service is provided 501 using a transport request 309 . The transport request 309 is structured data comprising an identifier 310 , e.g. DEVK900251, general information 311 regarding the service, e.g. indicating that the service is a program patch, and service data 312 , e.g. a piece of program code for a patch.
The transport request 309 is fed 502 into the import buffer 304 of one of the systems 301 , e.g. the quality assurance system 301 b of the global part 302 . This initial feeding may occur from the development system 301 a through a transport path 306 , but may also be effected manually as shown by path 313 . At operation 503 , the data supplier 305 of system 301 b detects the transport request 309 , accesses at least a part of its data, in particular the identifier 310 and the general information 311 , and provides, at operation 504 , the accessed data together with further information in a predefined format as system supplier data 315 to the data collector 308 . The further information may comprise a system identifier and system status information, e.g. a list of the support packages and services installed on the system 301 b , project data, project status indicators etc.
The data collector 308 updates, e.g. generates, deletes or changes, status data in a data file 314 that in this example is located within the central system 307 , operation 505 . The data file 314 may also be held in a different place or be a data base entry. The status data may contain a copy of the system supplier data 315 , or data based on an analysis of the system supplier data 315 . Likewise stored in the data file 314 or other data files is system supplier data 315 provided by the data suppliers 305 of the other systems 301 .
The data collector 308 maintains an up to date record of the state of all systems 301 of the system landscape 300 . For this purpose, the data collector 308 calls each data supplier 305 periodically for an update. Alternatively or additionally, the data suppliers 305 may contact the data collector 308 if relevant data has changed.
The central system 307 provides tracking services based on the data in data file 314 , operation 506 . These tracking services may comprise a request analysis, a status analysis, a sequence analysis, a project analysis, generation of reports, checking services etc. as explained in detail in the following.
A request analysis allows the search through all transport requests pending in the system landscape 300 according to certain criteria. For example, all transport requests belonging to a particular project, originating from a particular developer, being older than a predeterminable period of time may be determined and provided in a results list using this tracking service.
A status analysis allows the status of certain requests, e.g. the requests of the results list of the request analysis, to be analyzed. The analysis may state in which systems the requests have been approved, when they have been approved, in which systems they are pending to be approved, whether errors or system messages have been recorded during importation into a system etc.
A sequence analysis allows to determine the import sequence of the transport requests into each system, the sequence of transport requests in the import buffers, and the automated centralized assessment whether the sequences are correct.
A project analysis allows to determine the transport requests belonging to a particular project and its state.
Reports may be generated and automatically analyzed. Such analysis may comprise comparing a report with a reference report to check for completeness, comparing the imports of transport requests in two different systems, comparing and analyzing import sequences in order to identify sequence errors, comparison of a request list with the contents of the import buffer of a system, determining the overall status of an object list, e.g. a list of objects belonging to a project, etc.
Based on the tracking service results, and with consideration of further information like project association and project status data, one or more transport requests may be imported automatically, operation 507 . A manual approval of the automated import by an operator may be required.
Although the foregoing has been a description of an example embodiment of the invention, it will be apparent to those skilled in the art upon review of this disclosure that numerous variations and modifications may be made in the invention. For example, instead of using SAP R/3 Release 4.5, other SAP and non-SAP systems may benefit from the invention. | A method for tracking transport requests in a system landscape comprising a central control system and a plurality of logical systems interconnected by logical transport paths, a transport request defining a software service for a system in the landscape, is described. The method includes feeding a transport request into a logical system of the plurality of logical systems; providing a data supplier in the logical system for supplying, to the central system, data supplier information containing information about the transport request; providing a data collector in the central system for obtaining the data supplier information and accordingly updating status data; and providing a tracking service in the central system, the tracking service allowing to analyze the status data. | 6 |
BACKGROUND AND SUMMARY OF THE INVENTION
The present invention relates to methods of treatment of cellulosic fibers and particularly to methods for producing low fines content pulp for use in tissue, fluff and towel products.
Known methods of mechanical defibration of wood chips, impregnated or not, such as disc or grindstone defibration, produce substantial quantities of fines. High levels of fines, however, are detrimental to many products, such as tissue, fluff and towel products, because they cause dusting, drainage problems on the paper making machinery, poor fiber retention and decreased softness in the resulting product. Short fibers in the pulp for use in these products are also not desired.
Cellulosic fibers are sometimes treated in an apparatus comprising a pair of intermeshing screws in a treatment housing in communication at one end with an inlet for receiving the cellulosic fibers and at its opposite end with an outlet for the treated fibers. The screws counter-rotate in the area where the flights of the screws intermesh and that area constitutes a treatment zone. Treatment is conducted under compression and shear. This generally provides pulps having certain beneficial advantages. Such apparatus is commercially available under the trademark Frotapulper®.
Methods of treating pulp using that apparatus have been effective in modifying pulp fibers by the application of compressive and shear forces on the pulp at high consistencies and high temperature. For example, with respect to kraft and sulfite pulps, this treatment results in a reduction in tensile strength, water retention value and swollen volume. Porosity, stretch and tear strength are increased. Rejects from chemical pulps may also be defibered using the foregoing described apparatus. Additionally, such apparatus has been used to disperse waste paper contaminants and modify the physical properties of such waste paper. In that connection, the apparatus defibers waste without producing substantial fines. Other uses of the foregoing apparatus have included removal of resin from pulps, the mixing of chemicals in pulp, defibration of flax, and defibration and development of properties of semi-chemical and chemimechanical pulps.
According to the present invention, there is provided a method for producing low fines content pulp for use in producing tissue, fluff and towel products. For purposes of this application, low fines content pulp may be defined as a pulp containing about 10% fines or less. To accomplish the foregoing, cellulosic fibrous chips are conventionally washed and squeezed to reduce their moisture content. The fiber material is then sequentially subjected to compressive and shearing forces while being impregnated with chemicals. For example, to form high freeness fluff, the washed and squeezed cellulosic fibers are refined by subjecting them to compressive and shearing forces at the same time a chemical, for example a mixture of sodium sulfite and DTPA, is added to the fiber. This compressive and shearing action may be characterized by low frequency high amplitude compression-relaxation cycles affording high energy transfer into the pulp at a low rate. After a certain residence time in a reaction chamber, the fibers are once again subjected to compressive and shearing forces of the same character and additional chemical, for example caustic, is added whereby the fibers are further softened. The fibers are subsequently subjected to additional compressive and shearing forces of like character in further similar stages of treatment while chemicals, such as bleaching agents, may be added until this controlled defibration produces a high freeness fluff with very few fines. Also, the treatment with the bleaching agent brightens the fibers. Thus, by sequentially subjecting the fibers in different treatment stages to compressive and shearing forces of this type while adding the appropriate chemicals, the fibers are gradually broken down without producing substantial fines. Rejects from the sequential treatment stages can be recycled back to previous treatment stages for further defibration and treatment.
Accordingly, it is a primary object of the present invention to provide a novel and improved method for producing low fines content pulp for use in tissue, fluff and towel products.
These and further objects and advantages of the present invention will become more apparent upon reference to the following specification, appended claims and drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a schematic illustration of a process for producing low fines content pulp according to the present invention; and
FIG. 1A is a schematic illustration of additional apparatus useful for providing pulp with particularly low freeness grades, such additional apparatus being located in the apparatus of FIG. 1 as indicated by the FIG. 1A in FIG. 1.
DETAILED DESCRIPTION OF THE INVENTION
Referring now to the drawing, cellulosic chips are initially stored in a chamber 10 where they are prepared for further processing by washing. The washed chips are transferred through a chip sump 12 and said separator 13 for disposition in a steaming vessel 14. From the steaming vessel 14, the chips flow to a first treatment stage, generally designated TS1. At this first treatment stage, the washed and steamed chips flow through a plug screw feeder 16 which reduces the moisture content and removes or reduces the concentration of other soluble material from the chips. The chips are then fed to a defibrating apparatus 18 wherein compressive and shear forces are applied to the chips, while simultaneously a chemical or combination of chemicals is added to the chips. The apparatus preferably comprises the commercially available processing apparatus sold under the trademark Frotapulper®. Such apparatus includes counter-rotating screws, the intersection of the flights of which defines a treatment zone in which compressive and shearing forces are applied to the chips or fiber disposed therebetween. At this stage, the chips are impregnated with one or more chemicals, such as sodium sulfite, DTPA, or other chemicals such as caustic and/or bleaching agents, and which chemicals are added directly to the material in the defibrating apparatus through one or more inlets 19. In addition to the chemical impregnation, there is also provided in the defibrating apparatus a breakdown of the chips wherein the chips are converted to fibers with reduced production of fines.
From this treatment stage TS1, the fibers are disposed in a reaction chamber 20 for a predetermined time interval. The time and temperature in reaction chamber 20 helps to determine and control the fiber length distribution. Fiber length is also determined and controlled by the action of the compressive and shearing forces in the first treatment stage TS1.
From reaction chamber 20, the fibers are subjected to a second stage of treatment indicated TS2. The fibers from reaction chamber 20 are first fed through a plug screw feeder 22 which, similarly as described above, reduces the moisture content of the fiber and removes soluble material. From the feeder, the fibers are fed to a second defibrating apparatus 24, that is, apparatus sold under the trademark Frotapulper®. In this apparatus 24, compressive and shearing forces are applied to the fibers at the same time the fibers are impregnated, for example, with caustic, supplied through an inlet 26.
The fibers from the second stage treatment are fed to a third treatment stage TS3, where the fibers are first washed, pressed and squeezed in a wash press 30 to once again reduce their moisture content and to remove or reduce soluble material content. In this stage, the washed and pressed fibers are fed to a third defibrating apparatus 32, i.e., a Frotapulper® processing apparatus, where compressive and shearing forces are applied to the fibers simultaneously with the addition of bleach, preferably peroxide bleach, supplied to the fibers through an inlet 34. The bleached fibers are then disposed in a reaction chamber 36 for a predetermined time and temperature.
The bleached fibers are then fed to a fourth treatment stage TS4, where the fibers are again squeezed in a plug screw feeder 38 to reduce their moisture content and reduce or remove soluble material content. The fibers are then once again subjected to compressive and shearing forces in a fourth defibrating apparatus 40, i.e., a Frotapulper® processing apparatus, in which the fibers are simultaneously impregnated with a bleach, preferably peroxide bleach, supplied through inlet 42. The bleached fibers from the fourth treatment stage TS4 constitute pulp, which has very low fines content. Thus, there is provided a multi-stage, gentle, continuing separation of fibers. This results in low fines content pulp, 10% or less, with good paper making properties. This pulp is then transmitted to a bleach tower 44. It will be appreciated that rejects from the various treatment stages, as well as the chemicals removed from the fibers in those stages, are recycled back for further use in prior treatment stages. Additional similar treatment stages may be provided as desired depending upon the requirements for the final pulp product.
The process may be continued further to produce pulp having lower freeness grades, for example down to 300 CSF, for tissue and towel products. To accomplish this, additional similar treatment stages are provided intermediate treatment stage TS4 and the bleach tower 44 as indicated in FIG. 1A. These additional treatment stages use additional processing apparatus, preferably a Frotapulper® processing apparatus, for sequentially compressing and shearing the fibers in conjunction with chemical additives. For example, the pulp produced from the fourth treatment stage TS4 may be washed and pressed and subsequently, in a fifth treatment stage TS5, provided with a fifth processing apparatus 46 for further compressive and shearing action. Suitable chemicals may be added or not at this processing stage. The fibers resulting from that action are transported to a reaction chamber 48 for retention over a suitable time interval. The fibers are then transported to a sixth treatment stage TS6, wherein the fibers are again squeezed and pressed to reduce their moisture content and disposed in a defibrator 48, i.e., a Frotapulper® processing apparatus, for further compression and shearing action. The resulting fibers may then be screened to recycle the shives and this low freeness grade fiber may then be disposed in the bleach tower 44 for subsequent processing as indicated previously.
Soluble hemicelluloses may be removed during this process. Thus, the normal leaching out of these hemicelluloses from the pulp over periods of time which cause adhesion problems in the manufacture of tissue is reduced in the formation of the tissue pulp.
It will be appreciated that the defibrating apparatus used in the present invention affords a different kind of action in comparison with the action in more conventional refiners, such as disc or conical refiners. Particularly, the frequency and amplitude of the compression-relaxation cycles are different, resulting in a different type of breakdown of the wood fibers. For example, in disc refiners, there are a very large number of compression-relaxation cycles per minute, on the order of about 200 million for a standard fifty-four inch disc refiner. On the other hand, the defibrating apparatus used in the present invention has a much lower number of compression-relaxation cycles per minute, on the order of about ninty-seven thousand. The relative frequency of compression cycles per minute in comparing a standard 54-inch disc refiner with a Frotapulper® refiner is therefore about 2000/1. Thus, the conventional disc refiners may be characterized as having high frequency, low amplitude compression-relaxation cycles affording low energy transfer into the pulp at a high rate. The refining apparatus used in the present invention provides low frequency, high amplitude compression-relaxation cycles affording high energy transfer into the pulp at a low rate. The duration of the compression-relaxation cycle in the refining apparatus hereof is also longer in comparison with the standard disc refiner. Consequently, it will be appreciated that the combination of (1) thorough impregnation of chemical additions caused by Frotapulper® treatment of wood (the compression-relaxation cycles cause the chemical addition to move into the wood substance); (2) the difference in rate of energy transfer associated with lower frequency, longer duration compression-relaxation cycles in comparison with standard disc refiners; and (3) the reduction in internal bonding of the wood (a softening effect) as a result of the presence of a chemical produces a long fiber, low fines content pulp.
While the invention has been described in connection with what is presently considered to be the most practical and preferred embodiment, it is to be understood that the invention is not to be limited to the disclosed embodiment, but on the contrary, is intended to cover various modifications and equivalent arrangements included within the spirit and scope of the appended claims. | A method for producing low fines content pulp having successive treatment stages in each of which compressive and shearing forces are applied to the cellulosic fiber while simultaneously one or more chemicals are added. Gradual breakdown of the fibers is achieved with resulting low fines production whereby the pulp may be used for tissue, fluff and towel products. | 3 |
This application is a Divisional Application of U.S. application Ser. No. 09/077,662, filed May 29, 1998, now U.S. Pat. No. 6,051,017 which application is incorporated herein by reference, and which application was filed in the U.S. under 35 U.S.C. §371 based on international application number PCT/US97/02576, filed Feb. 19, 1997; which international PCT application claimed priority to U.S. Provisional Applications Ser. Nos. 60/011,870; 60/012,019; 60/011,868; and 60/011,869; all filed Feb. 20, 1996.
BACKGROUND OF THE INVENTION
Muscles serve a number of functions, most of which are dependent upon their regular contraction, which is in turn dependent upon their strength and health. For example, in addition to the well known functions of supporting the skeleton and permitting movement, muscles serve to pad the force of bone protuberances against the skin, and they promote blood flow, particularly through deep blood vessels. In response to repeated contractions against a load, muscle fibers grow in cross-sectional area and develop more force, and in response to repeated contraction over a long period of time, the oxidative capacity and blood supply of the fibers is enhanced.
In normal individuals, muscles are activated to contract by electrical signals that are communicated from the brain and spinal cord by way of muscle nerves. Many medical diseases, physical disabilities and cosmetic disfigurements arise from abnormal or absent electrical signals to the muscles. Such abnormal or absent electrical signals may be pathological or may simply be due to prolonged immobility or confinement that restricts or prevents the voluntary movement of one or more muscles. Without normal, routine electrical stimulation, muscles atrophy, that is lose their normal size and strength. Also contributing to muscle atrophy may be a wide range of other pathophysiological mechanisms, including absence of sustaining hormones and other endogenous trophic substances.
Many situations exist in which voluntary muscle contraction cannot be used effectively to operate, condition or strehgthen muscles. The most extreme loss of voluntary muscle function occurs when the brain or spinal cord is injured by trauma, the growth of tumors or cerebrovascular accidents. In patients suffering from these conditions, muscles become wholly or partially paralyzed because the electrical commands that are normally generated in the nervous system are no longer available to stimulate muscle contractions. Less extreme degrees of muscle weakness and atrophy can come about when some of the nerve fibers supplying a muscle are damaged by disease or injury or when the muscle is immobilized or voluntarily rested, for example by casting or bedrest, in order to recover from an injury or surgical intervention involving a nearby body part, or other prolonged confinement or immobilization.
With respect to prolonged physical confinement or immobilization, the affect of muscle non-use and atrophy frequently leads to two disorders that are particularly difficult to avoid and expensive to treat, pressure ulcers of the skin and subcutaneous tissues and retardation of the normal circulation of blood through deep vessels. Continual, unrelieved pressure on localized regions of skin can result in the development of pressure ulcers of the skin and subcutaneous tissues, also known as bed sores or decubitus ulcers. Pressure ulcers are thought to occur when tissues underlying a site of pressure are deprived of oxygen and nutrients because blood flow is impeded, and when the area is subjected to frictional and shearing forces associated with continuous rubbing and movement. Pressure ulcers vary in size and degree of damage from small regions of redness to deep craters of tissue erosion passing through skin, connective tissues, muscle and even bone that can threaten the life of a patient by providing portals of entry for pathogenic organisms. They are often exacerbated in chronically paralyzed or bedridden patients because of atrophy of the unused muscles that normally provide a degree of padding between the skin and underlying bony protuberances. The treatment of pressure ulcers often requires prolonged, intensive medical care and occasionally extensive surgery, usually entailing further restrictions in the posture of the patient, which may further complicate medical and nursing care and cause other complications.
As mentioned above, prolonged immobilization or physical confinement of a body part often also results in retardation of circulation of blood through deep vessels, particularly the veins in an around muscles. For example, the failure to contract muscles in the limbs at regular intervals, as occurs normally when walking or standing, is known to cause stasis of blood in some veins. Venous stasis is a predisposing factor in the formation of clots in the veins. Such deep venous thrombosis further compromises blood flow to the immobilized body part and can be the source of dangerous emboli to the heart and lungs. Thrombosed veins may also become chronically infected, posing a danger of septicemia. Examples of particular populations of patients that are especially at risk for development of pressure ulcers and venous emboli include comatose and obtunded patients, patients who are confined by paralysis to bed or wheelchairs, bedridden patients who have medical or surgical conditions that limit their activity, and elderly patients with limited mobility. To reduce complications in these patients, it is necessary to reestablish movement of the vulnerable body parts; however, these patients are either incapable of voluntary movement or severely restricted in their ability to voluntarily move. Therefore, therapists often spend considerable time manipulating the passive limbs of these patients, but this is expensive and relatively ineffectual because it is the active contraction of muscle that tends to pump blood through the veins and to maintain the bulk of the muscle.
It has long been known that muscle contractions can be elicited involuntarily by stimulating muscles and their associated motor nerves by means of electrical currents generated from electronic devices called stimulators. This has given rise to various therapies that seek to prevent or reverse muscle atrophy and its associated disorders by the application of electrical stimulation to the muscles and their nerves via these stimulators. For example, the field of research known as functional neuromuscular stimulation (FNS) or functional electrical stimulation (FES) has begun, which seeds to design and implement devices capable of applying electrical currentsin order to restore functional movement to paralyzed limbs. Similarly, therapies employing stimulators to regularly apply specific patterns of electrical stimulation to muscles in order to prevent or reverse atrophy are known.
Many of the earliest stimulators were bulky and relied upon the delivery c)f large current pulses through electrodes affixed to the skin, a procedure that requires careful Positioning and fixation of the electrodes to the skin and frequently produces disagreeable cutaneous sensations and irritation ofthe skin. Additionally, such transcutaneous stimulation produces relatively poor control over specific muscles, particularly those that lie deep in the body. Thus, this procedure can be time-consuming, uncomfortable, and is generally useful only for muscles located immediately beneath the skin.
It is also possible to stimulate muscles more directly by passing electrodes through the skin into the muscles or by surgically implanting self-contained stimulators and their associated leads and electrodes in the body. These devices have many configurations, but most are large and have numerous leads that must be implanted and routed through the body to the desired muscles using complex surgical methods. Further, they are expensive to produce and the invasive procedures required for their implantation are impractical for most patients because they increase rather than decrease the required care and the danger of infection and other sources of morbidity in patients who are already seriously ill. Thus, such devices have been used˜primarily in patients with severe paralysis in order to demonstrate the feasibility of producing purposeful movements such as those required for locomotion, hand-grasp or respiration.
More recently a new technology has been described whereby electrical signals can be generated within specific tissues by means of a miniature implanted capsule, referred to as a “microstimulator”, that receives power and control signals by inductive coupling of magnetic fields generated by an extracorporeal antenna rather than requiring any electrical leads. See, U.S. Pat. Nos. 5,193,539; 5,193,540; 5,324,316; and 5,405,367, each of which is incorporated in its entirety by reference herein. These microstimulators are particularly advantageous because they can be manufactured inexpensively and can be implanted non-surgically by injection. Additionally, each implanted microstimulator can be commanded, at will, to produce a well-localized electrical current pulse of a prescribed magnitude, duration and/or repetition rate sufficient to cause a smoothly graded contraction of the muscle in which the microstimulator is implanted. Further, operation of more than one microstimulator can be coordinated to provide simultaneous or successive stimulation of large numbers of muscles, even over long periods of time.
While originally designed to reanimate muscles so that they could carry out purposeful movements, such as locomotion, the low cost, simplicity, safety and ease of implantation of these microstimulators suggests that they may additionally be used to conduct a broader range of therapies in which increased muscle strength, increased muscle fatigue resistance and/or increased muscle physical bulk are desirable; such as therapies directed to those muscle disorders described above. For example, electrical stimulation of an immobilized muscle in a casted limb may be used to elicit isometric muscle contractions that would prevent the atrophy of the muscle for the duration of the casting period and facilitate the subsequent rehabilitative process after the cast is removed. Similarly, repeated activation of microstimulators injected into the shoulder muscles of patients suffering from stroke would enable the paretic muscles to retain or develop bulk and tone, thus helping to offset the tendency for such patients to develop subluxation at the shoulder joint. Use of microstimulators to condition perineal muscles as set forth in applicant's copending patent application, Ser. No. 60/007,521, filed Nov. 24, 1995, entitled “Method for Conditioning Pelvic Musculature Using an RF-Controlled Implanted Microstimulator”, incorporated herein by reference, increases the bulk and strength of the musculature in order to maximize its ability to prevent urinary or fecal incontinence.
In addition to the therapeutic use of microstimulators to promote contraction of specific, isolated muscles in order to prevent or remedy the disorders caused or contributed to by inactive muscles, the administration of hormones, trophic factors and similar physiologically active compounds may also be useful. It is known that the extent to which a muscle will grow in response to any stimulation regime is affected by the hormonal and chemical environment around the muscle. Muscle fibers have receptors for many physiologically active compounds that circulate normally in the blood stream or are released from nerve endings. These trophic factors have significant effects on the nature, rate, and amount of growth and adaptation that can be expected of the muscle in response to stimulation, whether such is produced voluntarily or by electrical stimulation. Perhaps the best known of these hormones are the androgenic steroids often used by athletes to increase muscle bulk and strength; but other hormones such as estrogens and growth hormones are also known to affect muscle properties. For example, the dramatic reductions in circulating estrogens and androgens that occur in women following menopause appear to account for decreases in the mass of muscles and bones, which can be slowed or even reversed by administering the deficient hormones systemically.
Thus, the beneficial strengthening effects of electrical stimulation can be maximized by providing the affected muscles with a supportive hormonal environment for growth. These compounds can be provided systemically by administering them orally or by injection. However, many such compounds are rapidly metabolized by the liver, so that high doses must be administered to achieve a desirable therapeutic effect. This can expose all tissues of the body, including the liver, to high and perhaps poorly controlled levels of the compound, resulting in undesirable side-effects that may outweigh the desired actions of the agent. In one aspect, the present invention recognizes that this problem could be circumvented by using a more selective method of drug delivery directed specifically to the electrically exercised muscles. Even if the introduced compound were ultimately to be cleared by absorption into the bloodstream, high concentrations would be produced only in the tissue around the target. A steep dilutional gradient would ensure that other regions of the body were exposed to much lower levels of the administered compound. By providing a more conducive chemical environment in the early stages of electrical therapy, it is expected that muscle atrophy could be reversed more rapidly and effectively. After muscle function has been reestablished, longer-term performance of the muscle could be more easily maintained at the desired level by electrical stimulation alone or in combination with low-dose systemic replacement therapy.
The microstimulators described and claimed herein are elongated devices with metallic electrodes at each end that deliver electrical current to the immediately surrounding biological tissues. The microelectronic circuitry and inductive coils that control the electrical current applied to the electrodes are protected from the body fluids by a hermetically sealed capsule. This capsule is typically made of a rigid dielectric material, such as glass or ceramic, that transmits magnetic fields but is impermeable to water vapor.
Encapsulation in glass is an effective and inexpensive way to ensure a hermetic seal between the electronic components and the biological tissues. Methods for forming similar hermetic seals within the confined dimensions of the overall device are well-known in the fabrication of industrial magnetic reed relays and diodes and have been described specifically for implantable microstimulators. See, e.g., U.S. Pat. Nos. 4,991,582; 5,312,439; and 5,405,367, each of which is incorporated in its entirety by reference herein. Such a hermetic barrier is important both to ensure good biocompatibility with the body and to protect the sensitive electronics from the body fluids that might destroy their function.
Unfortunately, however, glass and similarly brittle materials such as ceramic may crack or shatter as a result of externally applied forces or even residual stress in the crystalline structure of the material itself. If such an event occurs within the body or during a surgical procedure, it is desirable to retain or capture the sharp fragments of the capsule and any internal components so that they do not irritate or migrate into the surrounding tissues. In a testing or surgical environment in which devices are handled repeatedly, the hard, slippery surface of the glass capsule makes the device difficult to handle, and could increase the likelihood that the device will be dropped or pinched with a force sufficient to break the glass. Therefore, in one aspect, the present invention provides a well-chosen biocompatible coating for the glass which would decrease the lubricity of the device and ensure that glass pieces resulting from device fracture would be contained/captured in a protective sleeve.
The reaction of a living body to an intact foreign body such as an implanted microstimulator depends at least in part on the shape and texture of the surface of the foreign body, as described, e.g., by Woodward and Saithouse (1986). The surfaces left by the manufacturing processes used for the implanted microstimulator are constrained by the nature of the materials and processes required to achieve the desired electronic and mechanical characteristics of the device. Therefore, modification of the microstimulators' chemical nature and/or superficial physical contours to avoid, prevent and/or discourage an immunological response by the body, would be advantageous. Additionally, in selecting an appropriate coating material the opportunity arises for the introduction of various chemical compounds, such as trophic factors and/or hormones, as discussed above, into or onto the coating. Such compounds could then diffuse from the surface of the coating into the surrounding tissues for various therapeutic and diagnostic purposes, as previously mentioned.
SUMMARY OF THE INVENTION
The present invention provides for the prevention and treatment of various disorders caused or exacerbated by abnormal or absent electrical signals to the muscles and apparatus useful therefore. In one aspect, the invention provides an improved microstimulator having a biocompatible polymeric coating on portions of its exterior, thereby reinforcing the mechanical strength of the microstimulator such that it may optionally be implanted deeply into the muscle, while also providing a means for capturing the fragments of the microstimulator should mechanical disruption occur. In preferred embodiments, the coatings provided herein are selected to improve the nature of the foreign body reaction to the implanted microstimulator by modifying its chemical surface, texture and/or shape.
The implantable microstimulators disclosed and claimed herein are preferably of a size and shape that allows them to be implanted by expulsion through a hypodermic needle or similar injectable cannula. The microstimulator includes a hermetically˜sealed housing, at least two exposed electrodes, and electronic means within the housing for generating an electrical current and applying the electrical current to the exposed electrodes. The coating, as described in detail herein, is formed on at least a portion of the exterior of the microstimulator in contact with the hermetic seal.
In another aspect of the present invention, the improved microstimulator, in addition to providing electrical stimulation to the muscle within which it is implanted, is modified to provide a locally high level of one or more desired chemical agents or drugs. In a preferred embodiment, the polymeric coating covering a portion of the microstimulator's surface contains a chemical agent that is released gradually from the coating. Thus, when the microstimulator is implanted within or adjacent to a muscle it produces an electrical current that activates the motor nerves and/or muscle fibers of the muscle while simultaneously dispensing the chemical agent(s) in the vicinity of the active muscle fibers.
Further, in preferred embodiments, the improved microstimulator is designed to provide electrical stimulation over a period of many years and to provide elution of the chemical agent(s) over a period of many days, weeks or longer without any percutaneous connections to the external world. Release of the chemical agent from the coating of the microstimulator may be by diffusion or, alternatively, may be at a predetermined rate controlled by electrical signals produced by the implantable device.
In yet another aspect of the present invention, systems providing involuntary movement to muscles for the purpose of preventing, treating and/or slowing the progress of various complications associated with muscle inactivity, especially inactivity due to prolonged physical confinement or immobilization, are provided. These systems employ one or more microstimulators non-surgically implanted in or near one or more inactive muscles. Once implanted, the prescribing physician uses an external controller to command each of the implanted microstimulators to produce various output stimulation pulses in order to determine a pattern of stimulation that produces the desired muscle contraction pattern. The external controller retains the programmed stimulation routine and, thereafter, administers the therapy on a regularly scheduled basis and/or whenever commanded to do so by the patient or any caregiver.
The systems provided herein are particularly useful for maintaining or improving the functional capacity of paralyzed, weak, immobilized or under-exercised muscle without requiring voluntary exercise and for preventing various complications of prolonged physical confinement, including but not limited to pressure ulcers, deep venous thrombosis, autonomic dysreflexia and sensorimortor spasticity. For example, the implantable microstimulators are employed to stimulate specific muscles in order to reduce the incidence and accelerate the healing of pressure ulcers on the sacrum heels and other bony protuberances of bedridden or immobilized patients. Alternatively or additionally, the systems are employed to reduce the possibility of venous stasis and embolus formation by eliciting regular muscle contractions in the legs of the bedridden or otherwise immobilized patient. Advantageously, these systems may be employed to produce the desired pattern of regular contractions in one or more muscles for periods of days or weeks without the need for ongoing, continuous patient or caregiver supervision.
BRIEF DESCRIPTION OF THE DRAWINGS
The above and other aspects, features and advantages of the present invention will be more apparent from the following more particular description thereof, presented in conjunction with the following drawings wherein:
FIG. 1 diagrammatically illustrates one embodiment of a microstimulator coated with a polymeric coating in accordance with the present invention;
FIG. 2 shows another embodiment of a microstimulator coated with a polymeric coating wherein the coating extends over a portion of the electrodes;
FIG. 3 illustrates another embodiment ofthe implantable device ofthe present invention that provides both electrical stimulation and release of a chemical agent;
FIG. 4 shows another embodiment of an implantable device in accordance with the present invention;
FIG. 5 diagrammatically illustrates an 5 implanted microstimulator in muscle tissue and its control using an external controller;
FIG. 6 shows a variation of the invention wherein a battery is included within the implantable device to allow it to operate independently of the external controller;
FIG. 7 illustrates a preferred manner used to implant a microstimulator in accordance with the present invention;
FIG. 8 illustrates the general circumstances that give rise to pressure ulcers, and illustrates one preferred manner in which an implanted microstimulator, in accordance with the present invention, may be used to reduce pressure ulcer formation; and
FIG. 9 illustrates the general circumstances that give rise to venous stasis, and further shows a preferred manner in which an implanted microstimulator may be used and controlled, in accordance with the present invention, to prevent and treat such a condition.
Corresponding reference characters indicate corresponding components throughout the views of the drawings.
DETAILED DESCRIPTION OF THE INVENTION
The following description is of the best mode presently contemplated for carrying out the invention. This description is not to be taken in a limiting sense, but is made merely for the purpose of describing the general principles of the invention. The scope of the invention should be determined with reference to the claims.
An implantable device 9 made in accordance with the present invention is illustrated in FIG. 1 . The device 9 includes a narrow, elongated capsule 2 containing electronic circuitry 4 connected to electrodes 6 and 8 , which pass through the walls of the capsule at either end1 together forming a microstimulator of the type disclosed and fully described in U.S. Pat. Nos. 5,193,539; 5,193,540; 5,324,316 and 5,405,367, each of which is incorporated herein, in its entirety, by reference. A coating 10 is applied over the longitudinal extent of the surface of the capsule 2 . In the particular embodiment of FIG. 1, the ends of the coating 11 do not extend over the surface of electrodes 6 , 8 , so that the coating does not change the overall profile of the microstimulator. The device 9 is shaped to per˜˜it its insertion through a tubular insertion cannula, such as a syringe, that can be passed transcutaneously into a target muscle with or without fluoroscopic guidance, as described further below.
The capsule 2 may be made of glass or a similar dielectric material, such as ceramic, that can provide a hermetic barrier to the permeation of body fluids and water vapor into circuitry 4 . The basic design of the current-generating circuitry 4 is the same or similar to that described in the above-referenced patents, in which electrodes 6 and 8 may be continuously charged (through inductive coupling) by a programmable magnitude of direct current and may be occasionally discharged so as to produce a large, brief stimulation pulse with a programmable magnitude and duration, which stimulation pulse is used for the activation of nearby motor nerve and/or muscle fibers.
The coating 10 of the improved microstimulator is selected to both be biocompatible and to be elastic enough to provide some reinforcement to the capsule 2 . Additionally, it is advantageous and preferred that the material chosen to form the coating 10 serve to reduce the risk of injury from and to provide means for the capture of capsule fragments in the event the capsule is broken. Finally, it is desirable that the coating 10 chosen reduces the lubricity of the device, as glass and ceramic materials, of which the capsule 2 is most often constructed, are slippery. It will be appreciated by those of skill in the art that several different coatings are available having these characteristics. By way of example only and in no way to be limiting, the polymeric coating 10 may be formed of a silicone elastomer or a thermoplastic material, such as polyethylene, polyester, polyurethane or a fluorinated carbon chain from the TEFLON family.
The preferred method of application of coating 10 or depends on its chemical composition and physical properties. For example, in one embodiment, the coating 10 is formed from a thin-walled extrusion of silicone elastomer whose inside diameter is slightly smaller than the outside diameter of capsule 2 . The extruded tubing is cut to the desired length and its diameter temporarily expanded by absorption of an appropriate solvent such as heptane, toluene or xylene. The expanded silicone tubing is then slipped over the microstimulator, subsequently shrinking tightly onto the surface of the microstimulator as the solvent is evaporated from the silicone elastomer, thereby forming the desired coating 10 .
In another embodiment, the coating 10 is made from a thermoplastic material such as a polyethylene, polyester, polyurethane or a fluorinated carbon chain from the Teflon family. A thin-walled extrusion of such thermoplastic material whose inside diameter is smaller than the outside diameter of capsule 2 is mechanically expanded so as to temporarily increase its inside diameter. The expanded extrusion is then cut to the desired length, slipped over the microstimulator, and caused to shrink onto the surface of the microstimulator by briefly heating it to the temperature at which it contracts toward its unexpanded dimensions, thereby forming the desired coating 10 .
In another embodiment1 coating 10 is made from˜.B liquid solution containing melted, dissolved or unpolymerized material which is applied to the surf ace of the microstimulator by dip-coating, injection molding, or other suitable methods known to those of skill in the coating art. After covering the desired portions of the microstimulator, the coating 10 is allowed or caused to harden by appropriate means.
FIG. 2 shows an alternative embodiment of a microstimulator 16 in accordance with the present invention. The microstimulator 16 of FIG. 2 is similar to the microstimulator 9 of FIG. 1 except that in FIG. 2 the ends 12 of coating 10 extend over electrodes 6 , 8 , thereby preventing concavities 14 from coming into direct contact with tissues surrounding the implanted microstimulator. Advantageously, concavities 14 may be filled with a solid material, such as silicone or other material, to eliminate the presence of pockets of fluid that may act as a nidus of chronic infection.
FIG. 3 shows another embodiment of an improved microstimulator 18 in accordance with the present invention. The microstimulator 18 of FIG. 3 is similar to the microstimulator 9 of FIG. 1 except that the coating 10 in FIG. 3 contains a chemical agent 20 which diffuses from the surface of the coating 10 into the surrounding tissues. The chemical agent 20 may be any of a large number of pharmacologic and diagnostic agents whose presence in the tissue surrounding the implantable microstimulator is desired as part of the treatment received by the patient. Examples of suitable chemical agents 20 include anti-inflammatory or antibiotic compounds intended to reduce the foreign body reaction, hormones, neuromodulators and neurotransmitters intended to potentiate the effects of the electrical currents, or dyes intended to mark the original location of the implanted microstimulator. This list of agents provides only examples and is not intended to limit the scope of the invention set forth in the claims.
The method of introduction of the chemical agent 20 into or onto the coating 10 depends upon the chemical nature of the agent and the selection of an appropriate coating material. In general, the types of agents and compatible coatings that may be used therewith are known to those of skill in the arts of chemical binding and diffusion and the design of sustained release pharmaceuticals.
In a preferred embodiment, the chemical agent 20 comprises a long-acting compound of testosterone, such as testosterone propionate, cypionate or enanthate. This agent 20 is mixed with or adsorbed onto a silicone elastomer that is injection-molded or dip-coated and subsequently polymerized to provide a thin coating 10 , which coating 10 is spread over a substantial portion of the surface area of the capsule 2 . It should be appreciated that silicone is a highly biocompatible compound that has been used previously to administer steroids to experimental animals without exposing the animals to the trauma of repeated injections. However, it should also be appreciated that coating 10 could be formed from a variety of other materials, or by using a variety of other processes, as described above.
It is thus seen that in this preferred embodiment, agent 20 comprises a trophic compound used to enhance muscle development, specifically a testosterone derivative. It should be appreciated that such compounds have been used for many years in humans to treat endocrine disorders or to retard the development of estrogen-sensitive mammary tumors, and that a single intramuscular bolus of the compound will exert its actions for 2 to 4 weeks. The chemical agent 20 associated with the external coating 10 of the present invention, however, could be selected from a variety of trophic chemicals with actions on muscle or connective tissues, and could be bound to the coating in any manner that advantageously affects its rate of release. The rate of release may be designed to be anywhere from a few hours to a few days or weeks. Furthermore, agent 20 might actually consist of a multiplicity of active compounds1 various of which affect or influence muscle fibers, nerve fibers, connective tissue, or inflammatory cells so as to modify many aspects of the response of the tissues to the presence and activation of the device.
Certain composite materials, such as the drug-filled polymeric matrix that may be used for coating 10 the device, have the property that electrical voltage influences a change in the rate at which the fillers diffuse form the matrix. Where it is desirable to use such compositions, the microstimulator illustrated in FIG. 2 is particularly useful, as the electrical output signals generated by circuit 4 are applied, at least in part, to the coating 10 by its contact with the electrodes 6 , 8 of the device. Such electrical output signals are systematically varied so as to produce the desired rate of elution of the chemical agent 20 into the tissues surrounding the implanted device. Thus, it is seen that the electrical currents produced by electrodes 6 and 8 in the process of stimulating the muscle could also advantageously have the effect of increasing the elution rate of agent 20 simultaneously with the electrically-induced muscle contraction.
As illustrated in FIG. 4, rate control of the elution of the chemical agent 20 from the coating 10 may alternatively be managed using additional electrodes 26 which are affixed to the capsule 2 and connected to the circuitry 4 of the device. Such additional electrodes provide for separate control of the electrical currents and voltages applied to stijiulate the muscle electrically and to control the rate of elution of chemical agent 20 from the polymeric coating 10 . Advantageously, such multiple electrodes facilitate the use of electrophoretic current through coating 10 to effect the release of agent 20 , independent of the currents required to charge and discharge those electrodes associated with muscle or nerve stimulation. As illustrated in FIG. 4, electrode 26 is entirely covered by the polymeric coating 10 , whereas electrodes 6 and 8 are exposed to the body fluids. Electrical current applied between electrodes 26 and 8 would pass through coating 10 to effect electrophoretic release of chemical agent 20 . Electrical current applied between electrodes 6 and 8 , on the other hand, would pass unobstructed through the body fluids and tissues to effect electrical stimulation of nearby nerve or muscle fibers.
Referring now to FIG. 5, an improved microstimulator 28 is shown implanted into muscle 30 . In this embodiment, as well as in those of FIGS. 1-3, the improved microstimulator receives power form an external control device 40 . The external control device 40 generates an alternating magnetic field, illustrated symbolically by the lines 36 , through an external coil 38 , which coil may advantageously be located underneath the patient in a seat or mattress pad or in a garment or item of bedclothes. The magnetic field 36 is coupled with an implanted coil 33 , which forms part of the microstimulator device 28 , and induces a voltage and current within the coil 33 . The induced voltage/current in the coil 33 is used to power the electronic circuitry 4 , and fluctuations (e.g., modulation) of the varying magnetic field 36 are used to control operation of the electronic circuitry 4 . That is, the device 28 delivers current to its electrodes 6 , 8 according to instructions encoded in fluctuations of the magnetic field 36 . In this preferred embodiment, electrical current emitted from electrodes 6 and 8 stimulates motor nerve fibers 32 . Muscle fibers themselves are relatively difficult to activate via such electrical currents, but the motor nerve fibers are more readily stimulated, particularly if the microstimulator is located near them in the muscle. Each time a motor nerve fiber is excited, it conveys an electrical impulse through its highly branched structure to synaptic endings on a large number of muscle fibers, which results in the activation of essentially all of those muscle fibers. Electronic circuit 4 , then, controls the amplitude and duration of the electrical current pulse emitted by the microstimulator 28 , thereby determining the number of such motor nerve fibers that are excited by each pulse.
As an example of a preferred use of the improved microstimulator, the prescribing physician uses a programming station 44 to command external controller 40 to produce various stimulation pulses, during the initial treatment session after implantation of the improved microstimulator 28 . This is done in order to determine an exercise program that will provide the desired therapeutic muscle contraction program for the individual patient. The exercise program is down-loaded into a memory element 42 of the external controller 40 , where it can be reinitiated at will by, for example, manually activating control 46 . This manual control may be performed, e.g., by the patient or an attending caregiver. In the preferred embodiment, programming station 44 is a personal computer, external controller 40 contains a microprocessor, and memory element 42 is a nonvolatile memory bank such as an electrically programmable read-only memory (EEPROM). However, it will be appreciated by those of skill in the art that many different systems, architectures and components can achieve a similar function.
In accordance with a variation of the invention, shown in FIG. 6, a battery 46 is included within the implanted device (microstimulator), and is employed as a continuous source of power for the electronic circuit 4 . Such battery also provides storage and production means for a program of output currents and stimulation pulses that may then be produced autonomously by the implanted device without requiring the continuous presence of extracorporeal electronic components, i.e., without the need for an external control device 40 . In such instance, means would be provided for transmitting the desired program to each microstimulator and for commanding each microstimulator to begin or to cease operating autonomously. Advantageously, such an embodiment as shown in FIG. 6 may provide for continuous biasing current or voltage applied to coating 10 (when at least one of the electrodes is positioned to contact the coating 10 , as shown in FIG. 2 above, or when a separate electrode is embedded in the coating 10 as illustrated in FIG. 4, above) so that the rate of elution of agent 20 would always be well-controlled.
In a preferred implantation method, the microstimulator is injected into the muscle of interest through an insertion device whose preferred embodiment is shown in FIG. 7 . The external cannula 110 of the insertion tool is comprised of a rigid, dielectric material with sufficient lubricity to permit the easy passage of the microstimulator without scratching its external surface. The central trochar 120 of the insertion tool is an electrically conductive rod whose sharpened point extends beyond the insertion cannula, where it can be used to deliver current pulses to the biological tissue near its point. The initial insertion of the tool is directed either by a knowledge of musculoskeletal landmarks or radiographic imaging methods to approach the region of muscle 30 in which motor nerve fibers 32 enter. Optimally, the insertion device is advanced into the muscle in parallel with the long axis of muscle fiber fascicles. Electrical stimuli may be delivered through the metallic trochar by connecting a conventional electrical stimulator (not shown) to connector 122 on the trochar. By observing the contractions of the muscle 30 , these test stimuli can be used to ensure that the tip of the insertion device is situated sufficiently close to motor nerve fibers 32 to permit activation of a substantial portion of the muscle 30 without undesirable activation of other muscles or nerves. Failure to elicit the desired muscle contractions would suggest a poor site of placement for the microstimulator and a need to reposition the insertion tool closer to the site of motor nerve entry.
When the desired position is reached, the trochar 120 is removed from cannula 110 , taking care to keep the cannula 110 in position within muscle 30 , and a microstimulator is pushed through cannula 110 and into muscle 30 using a blunt-ended push-rod 130 .
As stated above, the microstimulators provided herein are particularly useful in the prevention and treatment of various disorders associated with prolonged immobilization or confinement; such as muscle atrophy, pressure ulcers and venous emboli. Referring to FIG. 8, there is illustrated, in diagrammatic form, the general circumstances that give rise to pressure ulcers and a preferred embodiment whereby one or more microstimulators may be employed to reduce the incidence of and/or contribute to the healing of such pressure ulcers. As depicted in FIG. 8, force 52 applied between bone 50 and firm support surface 56 is transmitted through intervening soft tissues of the skin 34 and muscle 30 , resulting in compression of skin region 54 . Skin region 54 is thus in danger of developing a pressure ulcer. Active contraction of muscle 30 is induced by electrical stimulation applied by microstimulator 48 and its associated electrodes 6 and 8 . Such active contraction makes muscle 30 stiffer, causing force 52 to be dissipated over a larger region of the skin 34 . Further, active contraction of muscle 30 tends to shift the position of the body with respect to surface 56 , causing force 52 to be directed to a fresh region of skin 34 . Regular active contraction of muscle 30 induces various trophic mechanisms in the muscle that maintain or even enhance the bulk and tone of muscle 30 in its passive state, thereby reducing the concentration of force 52 on skin region 54 .
To further aid in the prevention and/or treatment of the pressure ulcer, the microstimulator as described above and illustrated in FIGS. 3-6 employing a coating 10 having a chemical agent 20 associated therewith, may be used. In this alternative, the chemical agent 20 may be a trophic factor employed to improve the bulk and tone of the muscle 30 or may be an antibiotic or similar therapeutic drug useful for preventing infection of the pressure ulcer, or the chemical agent may be a combination of the two different agents. Increasing the bulk and tone of the muscle 30 , can provide additional padding between the bone 50 and support surface 56 , thereby lessening the force 52 against the skin region 54 .
In the embodiment illustrated in FIG. 8, a microstimulator 48 has been injected into muscle 30 at (or very near) the skin region site 54 where a potential pressure ulcer may develop. However, it may be satisfactory (or even preferred in some instances) to inject one or more microstimulators into adjacent muscles or near various nerves that control muscle 30 and/or other muscles that can affect the magnitude and direction of force 52 upon various regions of skin 34 .
It should be appreciated that contraction of many different muscles and groups of muscles tends to lift the prominence of bone 50 so as to distribute the load of the body more evenly across the skin 34 , thereby reducing the amount of force 52 applied at a particular skin region 54 . Optimally, a particular temporal pattern of stimulation applied by one or more microstimulators generates a sustained contraction of the respective muscles that is maintained for several seconds to permit blood flow into vulnerable tissues. Such is accomplished by the extracorporeal components illustrated in FIG. 5 and described above. Thus, upon an external command, or at predetermined intervals, power and command signals sent from controller 40 cause the various microstimulators to emit a series of electrical current pulses (i.e., a pulse train) at the desired frequency and amplitude sufficient to cause the muscles to lift the body for the duration of the pulse train.
Further movement of the body part typically occurs after cessation of such pulse-train stimulation because of various nervous reflexes or voluntary movements that are triggered by the concomitant activation of various sensory nerve fibers resulting either from direct electrical stimulation of the sensory fibers or the mechanical consequences of the directly stimulated muscle activity. Such triggered movements are generally just as important, and may even be more important, than the directly stimulated muscle activity caused by the microstimulator˜generated pulse train for shifting body posture.
FIG. 9 illustrates the general circumstances that give rise to venous stasis and a particular embodiment for the use of microstimulators to reduce such stasis. Blood flow 64 in veins 66 running through and between muscles 30 , 62 depends in part on compressive forces 52 and general metabolic stimulation resulting from the occasional active contraction of muscles 30 and 64 . In the absence of such contractions, flow is reduced, resulting in stasis and an increased likelihood of the formation of clots or thrombi in the veins. One common site for this problem is in the calf muscles of the lower leg, which extend the ankle. In accordance with one aspect of the present invention, therefore, one or more microstimulators are injected into the extensor muscles of the ankle, and one or more microstimulators are injected into the flexor muscles of the ankle. The programmed sequence of stimulation stored in memory bank 42 is used by controller 40 to create the necessary transmission of power and command signals from coil 38 to cause the microstimulators injected into the ankle muscles to generate a prescribed stimulation sequence. Ideally˜this prescribed sequence elicits muscle contractions sufficient to shift the position of the foot alternately into extension and flexion for several seconds. The interval between the various muscle contractions and the strength and duration of the contraction in each muscle is set by an attending physician or physiotherapist using a programming station 44 that downloads the desired program into memory bank 42 . The rhythmic intermittent muscle contractions produced each time the program is activated causes compressive forces to act on deep veins 66 , augmenting venous flow 64 out of the muscle by a pumping action that reduces venous stasis.
It should also be noted that a particular pattern of stimulation applied through a particular microstimulator, or combination of microstimulators, may also be effective at reducing the incidence of both pressure sores and venous stasis simultaneously, as well as generating other useful trophic effects on the muscles themselves, metabolic stimulation of the cardiorespiratory system, and improvements in the functioning of nervous pathways responsible for various reflexive and autonomic functions commonly affected adversely by prolonged immobilization. Other specific dysfunctions that have been reported to be reduced by regular electrical stimulation of nerves and muscles include autonomic dysreflexia and sensorimotor spasticity, particularly in patients suffering from spinal cord injury.
It should also be noted that the particular complications of pressure sores and venous stasis illustrated respectively in FIGS. 8 and 9 are intended only to provide specific examples of the beneficial effects of regular, active muscle exercise that can be induced by microstimulators, and are not intended to limit the scope of the invention set forth in the claims regarding the utility of stimulation applied in this manner. The present invention pertains generally to all beneficial effects that a caregiver might achieve by the appropriate implantation and programming of one or more microstimulators in any patient immobilized for a period of more than a few days.
While the invention herein disclosed has been described by means of specific embodiments and applications thereof, numerous modifications and variations could be made thereto by those skilled in the art without departing from the scope of the invention as set forth in the claims. | Improved implantable microstimulators are covered with a biocompatible polymeric coating in order to provide increased strength to the capsule and to capture fragments of the microstimulator should it become mechanically disrupted. Such coating also makes the microstimulator safer and easier to handle. The coating may include one or more diffusible chemical agents that are released in a controlled manner into the surrounding tissue. The chemical agents, such as trophic factors, antibiotics, hormones, neurotransmitters and other pharmaceutical substances, are selected to produce desired physiological effects, to aid, support or to supplement the effects of the electrical stimulation. Further, microstimulators in accordance with the invention provide systems that prevent and/or treat various disorders associated with prolonged inactivity, confinement or immobilization of one or more muscles. Such disorders include pressure ulcers, venous emboli, autonomic dysreflexia, sensorimotor spasticity and muscle atrophy. The microstimulator systems include external control for controlling the operation of the microstimulators. The control includes memory for programming preferred stimulation patterns for later activation by the patient or caregiver. | 0 |
RELATED APPLICATIONS
There are no applications related hereto heretofore filed in this or any foreign country.
BACKGROUND OF INVENTION
1. Field of Invention
This invention relates generally to a skimmer cover for the neck of a secondary drainage system in a catch basin to prevent entry of floatable material including fluidic material into the neck.
2. Background and Description of Prior Art
Catch basins have long been used to aid the disposal of accumulations of runoff water from areas where the soil surface has been sealed by buildings, roadways, parking lots and the like that prevent direct earth absorption of the water. Such catch basins in their early developmental state were simplistic structures, generally defined by a peripheral berm which created a storage basin from which water directly permeated into the earth therebeneath over a period of time as conditions permitted. As land use became more concentrated and sophisticated, the size of catch basins decreased because of the economics involved and as this trend continued, the removal of water from catch basins came to be aided by the use of secondary drainage systems such as dry wells and storm sewers. With the increased use of such drainage facilities for areas that serviced substantial numbers of hydrocarbon fueled vehicles, such as parking lots, parking garages, roadways and the like, and the increase in societal concerns for environmental protection and pollution, new problems have arisen concerning such drainage facilities.
Generally in areas used for hydrocarbon fueled vehicles, there is a sufficient accumulation of hydrocarbons and their residues of various sorts to be of concern under present day environmental standards. These hydrocarbon materials often are carried into drainage systems, especially during storms or runoff periods that generate unusually high volumes of water, which in the traditional catch basin systems generally has been dispersed into the earth or into some type of a storm sewer system to ultimately be deposited in the earth environment.
This problem has been recognized in the past and a popular solution that has been developed to resolve it has been to create catch basins defined by berms to receive and retain the waste water. The water contacting surfaces of such catch basins are provided with a blanket of vegetation, commonly some type of ornamental grass, that is intended to catch and entrap fluidic hydrocarbon pollutants which supposedly are subsequently modified or changed in nature to alleviate the deleterious effects of such materials on the environment wherein they ultimately come to reside. This type of waste water disposal has become sufficiently popular and standardized that its use is required by various land use and planning statutes and ordinances, as well as by various administrative codes and engineering standards.
In such a system that is serviced by a secondary water disposal system such as a dry well or sewer input orifice to accommodate large volumes of runoff water, however, problems still exist that often allow passage of fluidic hydrocarbon materials or their residues into the secondary water disposal system of a catch basin. Normally if such secondary water disposal systems are provided their entry orifices are medially positioned in a catch basin that may have some substantial depth of water during high runoff periods, but such entry orifices generally by necessity project above the lower surface of the catch basin wherein they are located while. The catch basin, however, may allow storage of water at a substantially greater depth than the entry orifices so when a runoff occurs that results in a waste water level above the level of the entry orifice various floatable materials such as fluidic hydrocarbons and their residues may enter the secondary disposal system rather than remaining in the catch basin for natural degradation. My invention seeks to provide a skimmer cover for such entry orifices that prevents such happening and maintains fluidic and other floatable materials outside the entry orifices and within the associated catch basin.
Gravity separation of contaminant material in runoff water, whether that material be more or less dense than water, has heretofore been known and practiced. Most such separation has developed for sinkable materials such as silt, sand, pebbles and the like which, if they pass into a water disposal system and especially one of the dry well type, tend to plug that system and render it non-usable. Most systems that have removed floatables have been concerned with larger particulate debris such as various vegetative material. Some such systems have separated fluidic floatable material such as hydrocarbons, fats and greases, but generally those systems have captured that material in some type of a container that must be periodically emptied to maintain the operability of the system. Such systems generally have not been designed or adapted to deal with such material left in them. The instant apparatus differs from this prior art by providing a skimming cover that prevents entry of floatable material of either a fluidic or particulate nature into the orifice of a secondary disposal system, but yet maintains that material within the catch basin wherein it was entrapped for subsequent removal of solid material or transformation of floatable material according to normal management activity of the catch basin.
The instant skimmer cover to be practically usable on the orifice of a secondary water disposal system of a catch basin must be fastenably engageable within that orifice and positionally maintainable thereon for operation, while at the same time being removable to allow access to the system through the orifice. Covers heretofore known for such orifices have not provided simply operable positive fastening mechanism, but generally have relied upon the substantial mass of a cover to allow positional maintenance by means of gravity and have established proper positioning by use of particular joint structure, if at all. Covers that have provided positive fastening means generally have been complex and have provided fastening mechanism that may be easily tampered with by unauthorized users. The instant cover in contradistinction provides a simple but effective pivotally expandable arm structure that is operated by a medial threaded rod to cause fastening with proper concentric positioning in an orifice while not requiring interfitting joint structure or reconfiguration of the neck. The threaded rod may have a particularly shaped head to require use of a particular tool to cause its rotation to tend to avoid operation by unauthorized users.
My invention resides not in any one of these features individually, but rather in the synergistic combination of all of the structures of my skimmer cover that necessarily give rise to the functions flowing therefrom, as herein specified and claimed.
SUMMARY OF INVENTION
My invention provides a skimmer cover for a secondary water orifice defined by a neck that projects spacedly above the bottom of a catch basin to prevent floatable materials, either particulate or fluidic, from entering the orifice. The cover provides a top interconnecting a peripheral depending skirt similar in configuration and larger in size than the neck to be serviced so as to fit over that neck. Horizontal supports are carried in a vertically medial position within the skirt to support the cover on the neck, with the lower portion of the skirt spacedly below the orifice of the neck and spacedly above the surface defining the bottom of the catch basin serviced by the orifice. A depending cylinder similar in shape but smaller than the skirt extends from the cross supports to the cover top and defines a plurality of spaced orifices to allow water to pass therethrough to enter the orifice of the neck.
A fastening structure provides an elongate threaded rod rotatably supported by its head in a hole defined in the medial portion of the top to depend therefrom. The rod threadedly carries a first lower bracket pivotally supporting two diametrically opposed, upwardly angulated lower lever arms, each of greater length than half the diameter of the outlet orifice. A second upper bracket threadedly carried in a medial position on the rod, pivotally mounts two downwardly angulated diametrically opposed upper lever arms, each pivotally interconnected in its outer end with the medial portion of each of the lower pivot arms so that as the threaded rod is turned the lower arms responsively move toward or away from each other to contact the neck or to allow removal of the cover from the neck.
In providing such a device, it is:
A principal object to provide a skimmer cover for the upstanding neck of a secondary water disposal system in a catch basin to prevent entry of floatable materials, either fluidic or particulate, into the orifice of the neck and maintains such floatable materials within the catch basin notwithstanding the depth of water therein relative to the cover.
A further object is to provide such a skimmer cover that has mechanism to releasably fasten the cover in the neck for initial positioning and positional maintenance in an operative relationship with the neck while yet allowing simple and easy removal and fastening by manipulation of a threaded rod having a head that may be configured to aid in preventing unauthorized use.
A still further object is to provide such a skimmer cover that is of new and novel design, of rugged and durable nature, of simple and economic manufacture and otherwise well adapted to the uses and purposes for which it is intended.
Other and further objects of my invention will appear from the following specification and accompanying drawings which form a part hereof. In carrying out the objects of my invention, however, it is to be remembered that its accidental features are susceptible of change in design and structural arrangement, with only one preferred and practical embodiment of its best known mode being illustrated in the drawings and described in the specification as is required.
BRIEF DESCRIPTION OF DRAWINGS
In the accompanying drawings which form a part hereof and wherein like numbers of reference refer to similar parts throughout:
FIG. 1 is a vertical medially cross-sectional view of my skimmer cover in place on a dry well servicing a catch basin showing the various parts of my cover, their configuration and relationship.
FIG. 2 is a horizontal cross-sectional view through the cover of FIG. 1, taken on the line 2--2 thereon in the direction indicated by the arrows.
FIG. 3 is a partially cut-away elevational view of the fastening mechanism of my cover.
FIG. 4 is a top view of the fastening mechanism of FIG. 3 further showing its construction and details.
DESCRIPTION OF PREFERRED EMBODIMENT
My invention generally provides skimmer cover 12 having fastening structure 13 for use on the neck of dry well 11 servicing catch basin 10.
The practices of modern land improvement often provide a catch basin 10 formed on the surface of the earth 14 by a peripheral berm 15. Surplus runoff water is introduced into the catch basin by one or more inlets 16 defined in the berm, and the level of water in the system is generally limited by the level of inlets 16, depending upon the local typography. The earth surface defining the bottom 17 of the catch basin normally slopes downwardly to the medially positioned orifice of a dry well 11 or other secondary water disposal system to collect water in that area.
In modern engineering practice, the depth of water in the catch basin may possibly range to several feet above bottom 17, depending upon physical parameters associated with the system, the area serviced by it and the severity of storms that may cause runoff from its serviced area. The primary purpose of the catch basin is to serve as a temporary containment basin or reservoir to receive water and aid dispersement of that water from the catch basin over a period of time. Modern catch basins normally are provided with a cover of vegetative matter on their inner water containing surfaces to aid in entrapping and modifying various environmentally deleterious materials that may be carried into the basin in the normal course of its functioning. In the case of automotive associated hydrocarbons and their residues, modern theory indicates that that material will be contained and absorbed in this vegetative layer where it will be modified to make it less deleterious to the environment, either by subsequent natural deterioration, modification or change, or at least by subsequent dilution.
Some secondary water disposal system such as dry well 11 or a storm sewer drainage system (not shown) is commonly associated with catch basin 10 to aid and make more efficient the dispersement of water therefrom during and after periods of high water input. Dry well 11 traditionally provides tank 18 having truncated conic upper transition portion 19 communicating to diametrically smaller uppermost cylindrical neck 20. A plurality of outflow orifices 21 for dispersement of fluid from the tank into the surrounding environment are defined in the tank sides. Commonly tank 18 is buried in the earth and if so it commonly will be surrounded by permeable material 22 such as crushed rock or similar particulated solids that form passageways between particles to allow relatively free fluid passage therethrough. This secondary drainage system receives water from catch basin 10 for subsequent dispersement into the earth underlying and surrounding the catch basin in a fashion somewhat more efficient than direct dispersement from the catch basin itself, but in general also allows dispersement of any contained floatable materials that are environmentally deleterious directly into the earth's environment.
The uppermost portion of dry well 11 generally provides a cylindrical neck 23, as do most input orifices for storm sewer systems. In the instance illustrated, neck 23 is formed of metal with a lowermost radially outwardly flaring flange 24 structurally attached on the upper surface of transition structure 19 of the dry well, though in other instances this neck may be formed of concrete, plastic or other rigid material and it may be formed as an integral part of the dry well structure rather than as a separate structure mechanically attached thereto. Normally the dry well will be buried in the earth with the top of its transition structure spacedly below the bottom surface 17 of a catch basin being serviced and with the neck 23 projecting spacedly upwardly above that surface 17 in an orientation such as to present a substantially horizontal upper orifice 25.
The reason for this neck positioning is to allow smaller volumes of water carried in the catch basin to remain in that basin and simply permeate into the earth when the water level is not above the upper surface of neck 23, and only allow such waters to enter the dry well 11 through the neck orifice 25 when the volume of water in the catch basin is sufficient to bring its level above the neck orifice. Modern day building and land use regulations and practices often specify a required distance of projection of a neck structure of a dry well or storm sewer drain above the bottom of a catch basin, and this distance when specified is normally in a range of from four to eight inches with an average of about six inches. It is with such a secondary drainage system neck structure or similar storm sewer inlet neck that my skimming cover is used.
Skimmer cover 12 provides solid peripherally defined, preferably dome-shaped, top 26 structurally interconnecting at its periphery depending skirt 27. The peripheral shape of top 26 is preferably similar to the shape of the neck 23 of a dry well to be serviced, and in any event somewhat larger than the external periphery of the neck, so that the skimmer cover may be carried over the neck to extend thereabout. Normally both the neck 20 and skirt 27 will be of circular cylindrical shape, but other cross-sectional configurations are within the ambit and scope of my invention.
The skimmer cover 12 carries in a vertically medial position cross supports 28, in the instance illustrated comprising two elongate metal bars extending in perpendicular diametrical array with coplanar lower surfaces. These supports are carried by and structurally joined to the internal surface of skirt 27 by welding or other similar mechanical fastening. The purpose of the cross supports 28 is to support the skimmer cover on the upper surface of the neck 23 of a serviced secondary water disposal system, and various other supports and support configurations that accomplish this purpose, such as at least two supports extending parallel to each other, three supports extending in a symmetrical radial fashion or other arrays, are within the ambit and scope of my invention.
The vertical positioning of the supports 28 within the skimmer cover is essential to the operation of my invention. The lower edge 29 of skirt 27 must be positioned so that it extends spacedly below the upper edge of neck 23 defining orifice 25, but terminates spacedly above surface 17 defining the bottom of catch basin 10 to allow water in the catch basin to enter the neck orifice from beneath the skirt. Normally the extension of the lower edge 29 of the skirt below the top of neck 23 will be approximately one-half of the extension of the neck above catch basin bottom 17, but this dimensioning is not essential and may be varied according to individual parameters of particular systems.
Cylindrical input baffle 30 is an annular structure of similar cross-sectional shape to skirt 27 that is structurally carried between the lower surface of top 26 and upper surface of cross supports 28. The radial dimension of the baffle is somewhat less than the similar radial dimension of the depending skirt 27 so as to define an annular channel between the two elements. The input baffle defines a plurality of spaced slot-like holes 31 to allow flow of water therethrough and into the orifice 25 of neck 23.
Preferably the various elements of my skimmer cover are formed of sheet metal, normally aluminum or a mild rolled steel, and if so they are preferably structurally joined by welding. It is possible that the cover structure may be formed from resinous or polymeric plastic materials joined by methods known in the plastic manufacturing arts, but such materials may not provide sufficient strength, rigidity and durability for extended use in an exposed environment.
Fastening structure 13 is carried by the skimmer cover 12 to releasably fasten and positionally maintain the cover on the neck 23 of an associated secondary water disposal system. The fastening structure provides threaded fastening rod 32 rotatably carried in medial hole 33 defined in top 26, with rod head 34 above the hole and threaded rod body depending therethrough to a point spacedly below lower edge 29 of skirt 27. The fastening rod 32 carries lower pivot plate 34 and upper pivot plate 35, each defining a medial orifice to receive the rod 32. The orifice 36 in the lower pivot plate is threaded to engage the fastening rod and the orifice 37 in the upper plate is unthreaded and of sufficient size to allow rotatable motion of the fastening rod therein. The upper pivot plate 35 is maintained in a medial position below the cross supports 28 on the fastening rod 32 by lock nuts 38 positioned on each side of the plate in a spaced relationship to allow rotary motion of the rod relative to the plate.
The opposed end portions of lower pivot plate 34 each carry spaced paired fastening brackets 39 defining a channel therebetween to receive the inner end portions of lower fastening arms 40 and mount those arms in a substantially coplanar array. The lower fastening arms 40 each are of a length somewhat greater than the radius of the inside of dry well neck 23 to be serviced by the skimmer cover and are pivotally joined between fastening brackets 39 in their inner end portions by nut-bolt combinations 41 extending between the elements. The medial portions of each lower fastening arm 40 carry similar spaced upper arm fastening brackets 42 extending upwardly therefrom in spaced relationship to pivotally mount upper fastening arms therebetween.
The upper pivot plate 35 at each end carries spaced paired fastening brackets 43 defining a channel therebetween to pivotally receive the radially inner end portions of upper fastening arms 44, which are pivotally mounted between the brackets by nut-bolt combinations 45 extending therethrough. The length of the upper fastening arms 44 is such that they extend to upper arm fastening brackets 42 where they are pivotally mounted by nut-bolt combinations 46. With this fastening structure, as threaded rod 32 is rotated, lower pivot plate 34 will be moved toward or away from upper pivot plate 35 to cause resultant motion of the outer end portions of lower fastening arms 40 away from or toward each other to allow fastening and release of the fastening structure within neck 20.
Having described the structure of my invention, its use may be understood.
A skimmer cover 12 and associated fastening structure 13 are constructed according to the foregoing specification, with parameters determined by known engineering methods for use with a particular catch basin 10 and dry well structure 11 of the type described. The threaded rod 32 of the fastening structure is rotated to move the outer ends of the lower fastening arms 40 radially inwardly toward each other until the distance between them is less than the internal diameter of the neck 23 of a dry well to be serviced. The skimmer cover then is manipulated to position it over the neck 23 of that dry well, with the fastening structure extending downwardly through the orifice 25 defined by the neck and the cover structure resting with its cross supports 28 on the top of the neck. With the cover in this position, the threaded rod 32 is rotated by manipulating its head to cause the outer ends of the lower fastening rods 40 to move radially outwardly away from each other and come into fastenable engagement with the interior surface of the neck 23. As this occurs, the cover will be centered on the neck structure 23, at least along a line passing through the lower fastening arms, and if both the cover and neck are of circular cylindrical configuration the cover will be centered along any diameter. The cover then will be releasably and fastenably maintained in operative position for use.
As water is presented within catch basin 10, it will not pass into dry well 11 so long as its level remains below the level of the orifice 25 defined at the top of neck 23. With such a situation, the water will percolate into the soil underlying the catch basin primarily through the surface 17 defining the bottom of the catch basin or if not, it will in the course of time evaporate into the surrounding atmosphere.
As the water level in the catch basin rises above the lower edge 29 of skirt 27, floatable materials on the surface of water will be maintained outside the cover structure, except possibly for a small amount of such material that may be on the surface of the water between the skirt and dry well neck at the time water rises above the lower edge of the skirt. As the water level in the catch basin rises to the level of the top of the neck 20, the water will begin to flow into the orifice 25 defined by the neck. A flow pattern will be established wherein the water moves from beneath the periphery of the skirt 27 upwardly into the channel defined between the skirt and the dry well neck to pass over the top of the dry well neck and into the dry well.
During this course of flow, so long as the level of water in the catch basin remains above the lower edge of the cover skirt, floatable material of either a fluidic or solid nature will remain above that level and cannot ascend through the channel between the cover and the skirt to be carried into the dry well. When the water level in the catch basin ultimately lowers to and below the lower edge of the cover skirt, no floatable material will pass into the dry well or other secondary disposal system as the water level will be below the upper surface of the neck, and there will be no water flow through the orifice defined by the neck and into the dry well.
The foregoing description of my invention is necessarily of a detailed nature so that a specific embodiment of it might be set forth as required, but it is to be understood that various modifications of detail, rearrangement and multiplication of parts might be resorted to without departing from its spirit, essence or scope.
Having thusly described my invention, what I desire to protect by Letters Patent, and | A skimmer cover for a secondary dispersement system orifice in a storm water catch basin prevents inflow of floatable materials, and especially hydrocarbons from motor vehicles, from entering the orifice. The orifice is defined in a neck extending spacedly above the bottom of the catch basin surface to carry the skimmer cover. The skimmer cover provides a top with a peripheral skirt diametrically larger than the neck and supported on the neck to depend therebelow to a point spacedly above the catch basin bottom surrounding the neck. An internal cylinder depends from the cover top within the skimmer cover skirt and defines plural spaced orifices to allow fluid passage therethrough and into the orifice defined by the neck. A depending fastening structure having opposed pivotal lever arms moved by a medial screw therebetween is carried by the skimmer cover top to allow releasable fastening of the skimmer cover within the neck orifice for positional establishment and maintenance of the skimmer cover thereon. | 4 |
CROSS-REFERENCE TO RELATED APPLICATIONS
[0001] This application claims priority to U.S. provisional patent application Ser. No. 61/682,770, filed Aug. 14, 2012, the contents of which is incorporated herein by reference in its entirety.
BACKGROUND
[0002] The recent introduction of small gauge vitrectomy instrumentation in vitreoretinal surgery provides a great opportunity for more efficient, less traumatic and safer surgery. A trocar system is used through which instruments are introduced and exchanged throughout the procedure.
[0003] Introduction and removal of the trocars require several instruments and maneuvers that are typically implemented in multiple steps. These include: (a) stabilization of the eye; (b) location of the correct trocar position in pars plana in such a way that the natural lens is not traumatized by the introduction of the trocar or instruments and in such a way as not to introduce the instruments through the retina resulting in tears that can lead to retinal detachment; (c) dragging of the conjunctiva to cause a misalignment of entry points in conjunctiva and sclera; (d) removal of the sharp blade introducing the trocar; (e) positioning of the irrigation cannula; (e) repeating the key steps above three times in the most common three port pars plana vitrectomy surgery.
[0004] Completion of these steps is crucial to the initiation of the procedure in a safe and efficient manner. Presently these are performed using multiple instruments that are repeatedly exchanged for the performance of the individual steps and for the performance of each of the three sclerotomies.
SUMMARY
[0005] The present invention is for an eye fixation and stabilization system and accurate instrument positioning system which can be utilized for the fixating and stabilizing the eye and locating the accurate position for instruments to be positioned, introduced and manipulated during eye surgery, eye procedures and eye exams. It can be used in anterior segment surgery as exemplified but not limited to cataract surgery and refractive surgery as well as for vitreoretinal procedures and posterior segment surgeries as exemplified by but not limited to vitrectomy and intravitreal injections, providing a universal tool for stabilization, fixation and accurate positioning and manipulation of other instruments.
[0006] In one aspect, the invention provides an instrument having a handle, one end of which a swiveling, extended ring is attached. The extended ring includes (a) an internal edge with an internal circumference that approximately coincides with the limbus; (b) an external edge with an external circumference that is about 4 millimeters from the internal edge; (c) four windows at the external edge; and (d) a mark at each windows indicating a position that is about 3.5 millimeters from the internal edge. The extended ring has an inside surface that contacts the eye when the instrument is placed on the eye, the inside surface being roughened for improved contact with the eye thereby allowing the eye to be manipulated.
[0007] In some embodiments, the handle of the instrument is attached to the extended ring through two prongs on one end of the handle, each prong being secured to a tab on the internal edge of the extended ring using a pin inserted through the prong and tab.
[0008] In another aspect, the invention provides an extended ring that includes (a) an internal edge with an internal circumference that approximately coincides with the limbus; (b) an external edge with an external circumference that is about 4 millimeters from the internal edge; (c) four windows at the external edge; (d) a mark at each window indicating a position that is about 3.5 millimeters from the internal edge; and (e) two tabs on the upper edge of the extended ring to facilitate handling. The extended ring has an inside surface that contacts the eye when the instrument is placed on the eye, the inside surface being roughened for improved contact with the eye thereby allowing the eye to be manipulated.
[0009] Thus, in some embodiments, the positioning device is used for eye fixation and stabilization, as well as to assist in accurate instrument positioning, introduction and/or manipulation during eye examinations, surgeries or procedures. In some embodiments, the positioning device can be used in anterior segment surgery such as, for example, cataract surgery and refractive surgery, as well as for vitreoretinal procedures and posterior segment surgeries such as, for example, virectomy and intravitreal injections.
[0010] Any feature or combination of features described herein are included within the scope of the present invention provided that the features included in any such combination are not mutually inconsistent as will be apparent from the context, this specification and the knowledge of one of ordinary skill in the art.
[0011] 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. In case of conflict, the present specification, including definitions, will control. In addition, the materials, methods, and examples are illustrative only and not intended to be limiting. Although methods and materials similar or equivalent to those described herein can be used to practice the invention, suitable methods and materials are described below.
[0012] All patents and publications referenced or mentioned herein are indicative of the levels of skill of those skilled in the art to which the invention pertains, and each such referenced patent or publication is hereby incorporated by reference to the same extent as if it had been incorporated by reference in its entirety individually or set forth herein in its entirety. Applicants reserve the right to physically incorporate into this specification any and all materials and information from any such cited patents or publications.
[0013] Other features and advantages of the invention will be apparent from the following detailed description and from the claims.
BRIEF DESCRIPTION OF THE DRAWINGS
[0014] FIG. 1 is a view of instrument 1 from the underside of the swiveling extended ring 20 showing swiveling extended ring 20 attached to one end of handle 10 through two-prong ring 14 .
[0015] FIG. 2 is an enlarged view of underside 22 b of the swiveling extended ring 20 shown in FIG. 1 .
[0016] FIG. 3 is an enlaraged top view of the swiveling extended ring 20 attached to one end of the handle 10 shown in FIG. 1 .
[0017] FIG. 4 is a top view of the device placed on a model of an eye.
[0018] FIG. 5 is a top view of an embodiment of an extended ring of the invention without a handle, in particular, extended ring 20 without attached handle 10 .
DETAILED DESCRIPTION
[0019] The general purpose of the present invention is to position and stabilize the eye during various procedure, surgeries and examinations performed on the eye and allow the accurate positioning and manipulation of various instruments while reducing the number of instruments exchanges to a bare minimum.
[0020] The instrument can be used for a variety of procedures such as stabilization for cataract, LASIK and other refractive eye surgeries. A novel application of this specific instrument is described in further detail for the case of small gauge vitreoretinal surgery (trans pars plana vitrectomy (TPPV)).
[0021] The device of the invention is handheld instrument 1 that has a handle 10 at the end of which there is a swiveling extended “ring” 20 (or portion of a ring or arc). Handle 10 has elongated shaft 12 and two-prong end portion 14 . The handle is attached to the extended ring 20 through two-prong end portion 14 . The central portion of the ring (or portion of a ring or arc) has dimensions commensurate with the diameter of the cornea and is intended to approximately coincide with the limbus. Thus, the central portion has an internal edge 24 ( FIG. 1 , 2 ) with an internal circumference approximately coincides with the limbus when the instrument is placed on the eye as shown in FIG. 4 . The extended ring has external edge 26 with an external circumference that is larger than internal circumference of internal edge 24 as shown in FIGS. 1 and 2 . The external edge is positioned at a distance commensurate with the placement of a trocar in a phakic eye. This distance is often taken to be 4 mm from the limbus. There are four of small window 28 at external edge 26 of the extended ring. The windows angular and radial position allow for the accurate and safe positioning of the trocars. Mark 32 near the window allows for the sometime preferred positioning for a pseudophakic eye. Mark 32 can be placed next to each window as shown in FIG. 3 . Often that measurement is taken to be 3.5 mm from the limbus. The size of the windows is also such as to allow the safe introduction of the trocars and removal of the blades and other instruments (e.g. trocar cannula 48 and trocar system 50 , FIG. 4 ), as well as the stabilization of the trocar during the introduction of the infusion cannula without necessitating the use of another instrument. The extended ring inside surface 22 b (the one facing the eye) has a roughened surface in order to improve on the grasping ability of the eye and prevents slipping. It also allows full control and manipulation of the globe including rotation around a vertical axis (visual axis) to expose the areas of the eye needed for positioning before and after introduction of the trocars and this even in smaller eyes.
[0022] FIG. 1 illustrates instrument 1 of the invention. Handle 10 includes shaft 12 and two-prong member 14 . Swivel extended ring 20 includes internal edge 24 , external edge 26 , inside surface 22 b and four of windows 28 . FIG. 2 is an enlarged bottom view of one end of instrument 1 showing extended ring 20 with inside surface 22 b, internal edge 24 , external edge 26 , four of windows 28 attached to two-prong end of handle 10 . FIG. 3 is an enlarged top view of one end of instrument 1 showing extended ring 20 with outside surface 22 a, internal edge 24 , external edge 26 , four of windows 28 attached to two-prong end 14 of handle 10 . FIG. 4 illustrates instrument 1 on an eye showing window 28 is of a size sufficient to accomodate instrument 48 and 50 . Another embodiment of the invention is shown in FIG. 5 , which illustrates an embodiment of the invention in which extended ring 20 is without handle 10 .
[0023] In the current methods of small gauge vitreoretinal surgery, the introduction of the trocars involve several instruments which are exchanged multiple times each in three cycles, one for each port, for the completion of the safe and effective introduction of the trocar systems. The current instrument is positioned once and plays the role of stabilization, accurate measurement, removal of blade, introduction of the irrigation cannula, without the need for exchange of other instruments as the instrument is placed only once on the eye for the completion of the all cycles of trocar placement.
[0024] Procedures for which an instrument of the invention can be used include cataract surgery, refractive surgery including LASIK, anterior segment taps, vitreoretinal surgery and intravitreal injections including anti-VEGF, steroids, antibiotics and any pharmaceutical to be injected intravitreally.
[0025] The device of the invention can be made of material consistent with the materials used for similar surgical instruments. It can be made for repeated multiple uses and should be made in such a fashion as to allow for sterilization in the same fashion and along other surgical instruments. It can also be made in a disposable form for single usage to eliminate the need for repeat sterilization and allow for all the advantages typically associated with the use of disposable instruments.
[0026] The specific embodiments of the invention described above do not limit the scope of the invention described in the claims.
OTHER EMBODIMENTS OF THE INVENTION
[0027] While the invention has been described in conjunction with the detailed description, the foregoing description is intended to illustrate and not limit the scope of the invention, which is defined by the scope of the appended claims. Other aspects, advantages, and modifications are within the scope of the following claims.
[0028] The specific methods and devices described herein are representative of preferred embodiments and are exemplary and not intended as limitations on the scope of the invention. Other objects, aspects, and embodiments will occur to those skilled in the art upon consideration of this specification, and are encompassed within the spirit of the invention as defined by the scope of the claims. It will be readily apparent to one skilled in the art that varying substitutions and modifications may be made to the invention disclosed herein without departing from the scope and spirit of the invention. The invention illustratively described herein suitably may be practiced in the absence of any element or elements, or limitation or limitations, which is not specifically disclosed herein as essential. The methods and processes illustratively described herein suitably may be practiced in differing orders of steps, and that they are not necessarily restricted to the orders of steps indicated herein or in the claims.
[0029] As used herein and in the appended claims, the singular forms “a,” “an,” and “the” include plural reference unless the context clearly dictates otherwise. Under no circumstances may the patent application be interpreted to be limited to the specific examples or embodiments or methods specifically disclosed herein.
[0030] The terms and expressions that have been employed are used as terms of description and not of limitation, and there is no intent in the use of such terms and expressions to exclude any equivalent of the features shown and described or portions thereof, but it is recognized that various modifications are possible within the scope of the invention as described in the statements of the invention and as claimed. Thus, it will be understood that although the present invention has been specifically disclosed by preferred embodiments and optional features, modification and variation of the concepts herein disclosed may be resorted to by those skilled in the art, and that such modifications and variations are considered to be within the scope of this invention as defined by the appended claims. In addition, the invention has been described broadly and generically herein. Each of the narrower species and subgeneric groupings falling within the generic disclosure also form part of the invention. | The invention provides an eye fixation system that allows accurate positioning, stabilization and safe and efficient manipulation of the eye and surgical instrumentation used during procedures and surgeries of the anterior and posterior segments of the eye. | 0 |
BACKGROUND OF THE INVENTION
The present invention relates to appliance drawer constructions, and particularly to constructions of additive dispenser drawers used in washing appliances, such as automated laundry washing machines.
Automated washing machines (such as laundry washing machines) often include mechanisms for dispensing additives into a washing chamber (e.g., a drum of a laundry washing machine). Such dispenser drawers typically contain receptacles for holding and dispensing different additives, which can include detergents, whiteners, fabric softeners, scents, rinse aids, etc. Typically, a user fills a dispenser chamber with one or more additives. At selected times during a wash cycle, water is then automatically introduced into the dispenser chamber and mixes with the additive. The water/additive mixture then flows out of the dispenser drawer and into a separate washing chamber, e.g., drum.
An example of a drawer-style additive dispenser is illustrated and described in commonly-owned U.S. Patent Application Publication No. 2004/0011089 (titled “Washing Aid Dispenser and Washing Machine Comprising Said Dispenser”). Access to the drawer by the user is obtained by withdrawing the drawer from an associated dispenser housing provided within the appliance cabinet. Typically, the drawer slides in and out of the dispenser housing along guideways provided on opposite sides of drawer, and on corresponding sides of the cavity that receives the drawer. The drawer is retracted manually, and no separate latching mechanism is generally provided, since the friction between the mating surfaces of the drawer and the dispenser housing, along with the generally horizontal orientation of the guideways (in the typical level appliance installation), are sufficient to retain the drawer in the desired extended or retracted position.
PGP US 2006/0162392 discloses a dispenser additives drawer with frictional slide glides, and also having a stopper and elastic slot that serve to releasably hold the drawer in its fully inserted position.
U.S. Pat. No. 6,865,911 discloses a childproof lock/latch mechanism in a washer additives dispenser drawer.
Apart from laundry additive dispenser drawers, other mechanisms are known which cause release of a drawer, or opening of a door. See, e.g., U.S. Pat. No. 7,188,871 (push-button of glove box releases a latch, which allows a spring to bias the closure lid open); U.S. Pat. No. 5,002,074 (push-push ashtray drawer with spring to bias drawer to extended position); and U.S. Pat. No. 4,875,721 (push-button released door of microwave range).
In a modern trend, laundry appliances are taking on a more prominent stylistic role in the home. Along with this, greater emphasis is being placed on convenience, user friendliness and the “look and feel” of laundry appliances. An additive dispenser drawer that operates more smoothly and easily than the existing dispenser drawers would be a significant improvement in this regard.
SUMMARY OF THE INVENTION
Aspects of the present invention provide an appliance drawer construction of improved operability, allowing, upon the press of a button, the extension of the drawer. At the same time, inadvertent unintended opening caused, e.g., by a person's body brushing past or up against the appliance, may be avoided. In another aspect, the invention provides a simple and effective latch release linkage which is particularly well suited to a drawer, like a laundry washer additives dispenser drawer, that requires an offset of the latch from the operation push-button, due to the placement of an additive storage compartment portion of the drawer directly behind the front console of the drawer, and the space constraints within the housing that receives the drawer.
The above and other objects, features and advantages of the present invention will be readily apparent and fully understood from the following detailed description of preferred embodiments, taken in connection with the appended drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a front perspective view of a front load automatic laundry washer, including a push-button actuated additives dispenser drawer in accordance with an aspect of the invention.
FIG. 2 is a right front side perspective view of the exemplary additives dispenser drawer shown installed in FIG. 1 .
FIG. 3 is a right rear side partial perspective view of the exemplary additives dispenser drawer.
FIG. 4 is an exploded perspective view showing an assembly of parts of the exemplary additives dispenser drawer.
FIG. 5 is a partial bottom plan view, partially in section, of the exemplary additives dispenser drawer.
FIG. 6 is a partial bottom plan view of the additives dispenser drawer, with a portion cut-away to reveal components of the latch assembly thereof.
FIG. 7 is a longitudinal cross-sectional view of the additive dispenser drawer (front console omitted) received within the mating cavity of a housing of the additives dispenser.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
Referring to FIG. 1 , illustrated is an exemplary laundry washing appliance (machine) of the front-load, rotating drum variety. The washing machine includes an assembly of a drawer 1 and a housing 3 having a cavity that receives the drawer alongside a control panel 4 of the appliance. The drawer is extensible out of the housing to permit a user access to additive retention compartments of the drawer. Glides 6 (see FIG. 2 ) may extend along the sides of drawer 1 for making mating contact with corresponding bearing surfaces of the housing. This contact may comprise a sliding contact and/or a rolling contact, e.g., as may be provided by roller bearings. Incorporated into the housing, above the cavity, is an overhead water distribution tray 2 (see FIG. 7 ) for selectively delivering water into the drawer, in a generally known fashion. The assembly further includes a latch mechanism that serves to retain the drawer in the illustrated position, fully advanced into the housing. The latch mechanism includes a user operable latch release actuator, which may be a push-button 5 as shown. Referring to FIGS. 3-6 , the latch mechanism further includes a first hook-like catch 7 carried by the drawer 1 . Catch 7 is biased into engagement with a mating second catch 9 (see FIG. 6 ) provided on the housing, when the drawer is advanced into the housing (e.g., to the position shown in FIG. 1 ). Catch 9 may be provided in the form of an under-cut surface or the like, with a tapered guide surface adjacent thereto, for slidably guiding the first catch 7 into engagement with second catch 9 as drawer 1 is advanced fully into housing 3 .
Push-button 5 is operably connected with first catch 7 so as to effect a disengagement of first catch 7 from second catch 9 upon being pressed. In particular, as shown in FIG. 5 , the rear surface of push-button 5 engages with a laterally offset portion of a pivotably mounted linkage member 11 . As button 5 is pressed, linkage member 11 rotates (counterclockwise in FIGS. 5 and 6 ). Referring to FIG. 4 , linkage member 11 comprises a generally vertically extending, rib-reinforced, arcuate plate portion 13 . An arm 15 extends rearwardly from vertically extending portion 13 . Plate portion 13 has, on top and bottom flanges thereof, stub axles 14 (see FIG. 4 —only one visible) received in corresponding slots 16 (only one visible) to provide the pivotal mount. First catch 7 is provided at a rearward end of arm 15 such that upon pivotable movement of linkage member 11 , caused by a press of push-button 5 , first catch 7 swings through a generally horizontal arc away from (and out of engagement with) the second catch 9 .
A coil tension spring 17 is attached between the linkage member 11 and a side portion 19 (see FIGS. 4 and 5 ) of the drawer 1 , to bias linkage member 11 for pivotal movement that moves first catch 7 into engagement with the second catch 9 . Spring 17 also preferably preloads push-button 5 by pressing linkage member 11 against the rear side of push-button 5 , thereby avoiding undesirable looseness or play between these components. A press of push-button 5 acts to pivot linkage member 11 against the spring bias to thereby cause the first catch 7 to disengage from the second catch 9 during the time that the button is pressed. Upon release of button 5 , first catch 7 is returned to its original angular orientation, which may or may not be in engagement with second catch 9 , as will be explained.
The assembly further comprises a bias mechanism 20 (See FIG. 7 ) for biasing drawer 1 to move at least partially out of housing 3 upon a press of push-button 5 , under a condition that the drawer is not blocked from moving outwardly. As seen in FIG. 7 , bias mechanism 20 may comprise a compression spring 21 mounted upon a cylindrical guide rod 23 positioned in housing 3 behind inserted drawer 1 . Guide rod 23 is mounted so as to allow limited axial movement of the rod forwardly and rearwardly. A rearward end of spring 21 abuts against an oppositely facing seat 24 provided at an upper rearward part of housing 3 . The forward end of spring 21 is seated on a forward enlarged diameter portion of rod 23 , such that spring 21 biases rod 23 axially outwardly to a position that places a forward end of guide rod 23 in contact with a rear push-surface 25 of drawer 1 , when the drawer is fully advanced within the housing. This contact, upon full advancement of the drawer into the housing, also displaces rod 23 rearwardly against the bias of compression spring 21 , so as to preload the spring to bias rod 23 , and hence drawer 1 , outwardly. As a result, upon disengagement of first catch 7 from second catch 9 , the drawer will extend at least partially from the housing—so long as nothing is blocking it from doing so.
Under the aforesaid condition that the drawer is not blocked from moving outwardly, a spring-biased return of first catch 7 to its original angular orientation (upon a release of push-button 5 ) will not cause a reengagement of first catch 7 with second catch 9 . Thus, drawer 1 will remain free to be manually extended further out of the housing to allow a user full access to the additive storage compartments of the drawer. On the other hand, in a condition that drawer 1 is blocked from moving outward at a time that push-button 5 is pressed, first catch 7 remains in a position to be biased back into engagement with second catch 9 upon a release of push-button 5 , whereby the drawer remains secured within housing 3 .
The foregoing arrangement is of highly significant functional consequence. Namely, it can serve to avoid a situation where a person brushing by or up against the appliance inadvertently cause the drawer to open (move outwardly). With an occurrence of “brush-by,” it is possible that push-button 5 will be depressed, i.e., pushed inwardly causing a disengagement of the mating catches 7 , 9 . However, during this time, the person's hip or other body portion that inadvertently pressed button 5 will also typically be positioned so as to block drawer 1 from moving outwardly. Thus, in this condition, first catch 7 will remain in a position to be reengaged with second catch 9 upon a release of button 5 , and thus drawer 1 will advantageously be retained in its latched, retracted position. The principal operative forces are diagrammatically depicted by arrows A-C in FIG. 2 . Arrow A represents the pressing force on button 5 . Arrow B represents the reaction force of a body portion resisting the outward bias force C generated by bias mechanism 20 . Reaction force B is equal and opposite to bias force C, and thus the drawer is maintained stationary in its retracted position, despite a release of first catch 7 from second catch 9 by virtue of button-pressing force A.
The latch mechanism is preferably configured to permit the drawer to move sufficiently outwardly relative to push-button 5 , upon disengagement of first catch 7 from second catch 9 , to prevent a reengagement of the first catch with the second catch upon a user's release of push-button 5 . In the illustrated arrangement, a press of button 5 causes an initial pivot of linkage member 11 sufficient to release first catch 7 from second catch 9 . Thereafter, further rearward displacement of push-button 5 relative to drawer 1 is permitted to at least partially absorb the outward movement of drawer 1 caused by bias mechanism 20 upon a release of first catch 7 from second catch 9 . In this manner, a press of push-button 5 by a user does not, by itself, inhibit a release of the drawer allowing it to be thereafter fully extended from the housing.
In the illustrated laundry washing machine additive dispenser drawer embodiment, the push-button actuator 5 is positioned on a front face or panel of a front console 26 of drawer 1 . As seen in FIG. 2 , elevation-wise, button 5 is positioned generally centrally at least partially above a bottom of the drawer compartment structure 28 attached at the rear side of console 26 , through an intermediate joining member 30 of generally rectangular tubular shape. The first and second catches 7 , 9 are vertically offset below the push-buttons so as to be positioned, elevation-wise, at least partially below the bottom of the drawer compartment. This offset is accomplished simply and effectively by way of the described arrangement of push-button actuator 5 and linkage member 11 , including vertically extending portion 13 and arm 15 . Such an arrangement advantageously permits the push-button to be positioned centrally on console 26 directly in front of the drawer compartment structure 28 , while allowing the catches of the latch to be positioned where they can best be accommodated within the tight confines of the housing 3 . As best seen in FIGS. 4 and 5 , in the illustrated embodiment, arm 15 extends through an aperture 32 provided in a vertical step portion of joining member 30 , to position catch 7 at a backside thereof, below a floor portion 34 of joining member 30 . Mating second catch 9 may be provided within a depth-wise extending channel of a front console of housing, which aligns with aperture 32 upon insertion of drawer 1 . In addition to lending additional structural rigidity to the console, such a channel can serve to provide a protective enclosure around the mating catches. So positioned, the mating catches may be protected and further concealed from view of the user. In addition, such an arrangement can serve to avoid fouling of the catch mechanism by spillage of additives poured into the drawer compartments.
In the illustrated embodiment, the housing is a housing that receives the drawer of an automated laundry washing machine, and the drawer is an additive dispenser drawer thereof. It will be understood, however, that aspects of the invention may be applied to other automatic washing appliances, e.g., dishwashing machines, and to appliance and other storage drawers in general.
The present invention has been described in terms of preferred and exemplary embodiments thereof. Numerous other embodiments, modifications and variations within the scope and spirit of the appended claims will occur to persons of ordinary skill in the art from a review of this disclosure. | An appliance drawer construction allows, upon the press of a button, the extension of the drawer from a housing. At the same time, inadvertent unintended opening caused, e.g., by a person's body brushing past or up against the appliance, may be avoided. In another aspect, the invention provides a simple and effective latch release linkage which is particularly well suited to a drawer, like a laundry washer additives dispenser drawer, that requires an offset of the latch from the operation push-button, due to the placement of an additive storage compartment portion of the drawer directly behind the front console of the drawer, and the space constraints within the housing that receives the drawer. | 3 |
[0001] The application relates to processes for preparing valganciclovir and pharmaceutically acceptable salts thereof, as well as intermediates for the processes.
[0002] Valganciclovir (I) has a chemical name L-valine, 2-[(2-amino-1,6-dihydro-6-oxo-9H-purin-9-yl)methoxy]-3-hydroxypropyl ester. Valganciclovir hydrochloride is represented by Formula II. Valganciclovir is a mono-L-valyl ester (prodrug) of the antiviral compound ganciclovir (III). Valganciclovir hydrochloride is a cytomegalovirus (CMV) nucleoside analogue DNA polymerase inhibitor, prescribed for the treatment of CMV retinitis in patients with acquired immunodeficiency syndrome (AIDS) in adults and prevention of CMV disease in kidney, heart, and kidney-pancreas transplant patients at high risk in adults, and prevention of CMV disease in kidney and heart transplant patients at high risk in pediatric patients. The structure of valganciclovir (I) is shown below.
[0000]
[0003] The structure of valganciclovir hydrochloride (II) is shown below.
[0000]
[0004] The structure of ganciclovir (III) is shown below.
[0000]
[0005] European Patent Application 0 694 547 discloses a process for partial hydrolysis of the bis-ester 2-(2-amino-1,6-dihydro-6-oxo-purin-9-yl)methoxy-1,3-propanediyl bis(L-valinate) or a salt thereof, to afford the monoester 2-(2-amino-1,6-dihydro-6-oxo-purin-9-yl)methoxy-3-hydroxy-1-propanyl-L-valinate or a pharmaceutically acceptable salt thereof. The process disclosed in Example 6 of the application involves use of preparative reverse phase HPLC column, which makes the process unsuitable for commercial scale manufacturing.
[0006] U.S. Pat. No. 5,700,936 describes processes for preparing the compound 2-(2-amino-1,6-dihydro-6-oxo-purin-9-yl)methoxy-3-hydroxy-1-propanyl-L-valinate or a pharmaceutically acceptable salt or diastereomer thereof, comprising: hydrolyzing a compound of Formula IV:
[0000]
[0000] wherein P 1 is hydrogen or an amine-protecting group, and P 2 is an amine-protecting group; to form a compound of Formula V:
[0000]
[0000] in the presence of an amine, in a nonpolar aprotic solvent; and deprotecting the compound of Formula V to 2-(2-amino-1,6-dihydro-6-oxo-purin-9-yl)methoxy-3-hydroxy-1-propanyl-L-valinate or a pharmaceutically acceptable salt thereof; optionally followed by converting 2-(2-amino-1,6-dihydro-6-oxo-purin-9-yl)methoxy-3-hydroxy-1-propanyl-L-valinate into a pharmaceutically acceptable salt thereof; or separating 2-(2-amino-1,6-dihydro-6-oxo-purin-9-yl)methoxy-3-hydroxy-propanyl-L-valinate into its (R) and (S) diastereomers.
[0007] There remains a need to provide improved processes for preparing valganciclovir and pharmaceutically acceptable salts thereof, which are simple, cost-effective, commercially viable, sustainable, environmentally friendly, and avoid multiple protection-deprotection steps.
SUMMARY
[0008] In one aspect, the application provides methods for preparing valganciclovir and pharmaceutically acceptable salts thereof, embodiments comprising one or more of the following steps, individually or in the sequence recited:
[0009] a) reacting the compound of Formula III with a compound of Formula VI, to obtain a compound of Formula VII:
[0000]
[0000] wherein P 1 is hydrogen or an amine-protecting group;
[0010] b) partially hydrolyzing a compound of Formula VII, to obtain a compound of Formula VIII:
[0000]
[0000] wherein P 1 is as defined above; and
[0011] c) converting a compound of Formula VIII to valganciclovir of Formula I or a salt thereof.
DETAILED DESCRIPTION
[0012] In one aspect, the application provides methods for preparing valganciclovir and pharmaceutically acceptable salts thereof, embodiments comprising one or more of the following steps, individually or in the sequence recited:
[0013] a) reacting the compound of Formula III with a compound of Formula VI, to obtain a compound of Formula VII:
[0000]
[0000] wherein P 1 is hydrogen or an amine-protecting group;
[0014] b) partially hydrolyzing a compound of Formula VII, to obtain a compound of Formula VIII:
[0000]
[0000] wherein P 1 is as defined above; and
[0015] c) converting a compound of Formula VIII to valganciclovir of Formula I or a salt thereof.
[0016] Step a) involves reacting the compound of Formula III with a compound of Formula VI, to obtain a compound of Formula VII. Step a) may be carried out in presence of one or more suitable base. Suitable bases, which may be used in step a) include, but are not limited to, organic bases, inorganic bases, or resins, such as, for example: aliphatic amines, e.g., triethylamine, tributylamine, N-methylmorpholine, N,N-diisopropylethylamine, N-methylpyrrolidine, or the like; aromatic amines, e.g., pyridine, N,N-dimethylaminopyridine, or the like; alkali metal carbonates, e.g., sodium carbonate, potassium carbonate, or the like; alkali metal bicarbonates, e.g., sodium bicarbonate, potassium bicarbonate, or the like; alkali metal hydroxides, e.g., sodium hydroxide, potassium hydroxide, or the like; ammonia; resins bound to ions such as sodium, potassium, lithium, calcium, magnesium, or the like; any mixtures thereof; or any other suitable bases; either alone or as their aqueous solutions.
[0017] Step a) may be carried out in the presence of one or more suitable catalyst. Suitable catalysts, which may be used in step b) include, but are not limited to, triethylamine, pyridine, diisopropylethylamine, 1,8-diazabicyclo[5.4.0]undec-7-ene (DBU), 1,4-diazabicyclo[2.2.2]octane (DABCO), 1-methylmorpholine, 1-methyl piperidine, 1,5-diazabicyclo[4.3.0]non-5-ene, N,N-dimethylpiperazine, N,N-dimethyl aniline, 4-(dimethylamino)-pyridine (DMAP), hexamethylenetetramine (HMTA), tetra methylethylenediamine (TMEDA), collidine, 2,3,5,6-tetramethylpyridine (TEMP), or the like. Step a) may be carried out in presence of one or more suitable coupling agents. Suitable coupling agents, which may be used include, but are not limited to, N-hydroxy benzotriazole (HOBT), 4,5-dicyanoimidazole, dicyclohexylcarbodiimide (DCC), dicyclopentylcarbodiimide, diisopropylcarbodiimide, 1-ethyl-3-(3-dimethylamino propyl)carbodiimide hydrochloride, 1,1′-carbonyldiimidazole, cyclohexylisopropyl carbodiimide (CIC), bis[[4-(2,2-dimethyl-1,3-dioxolyl)]-methyl]carbodiimide, N,N′-bis(2-oxo-3-oxazolidinyl)-phosphinic chloride (BOP-CI), an acid chloride, ethyl chloroformate, or the like.
[0018] Step a) may be carried out in one or more suitable solvents. Suitable solvents, which may be used include, but are not limited to, an alcohol, e.g., methanol, ethanol, isopropyl alcohol, 1-propanol, 1-butanol, 2-butanol, or the like; a ketone, e.g., acetone, ethyl methyl ketone, methyl isobutyl ketone, or the like; a hydrocarbon, e.g., toluene, xylene, hexanes, heptanes, cyclohexane, or the like; a halogenated hydrocarbon, e.g., dichloromethane, ethylene dichloride, chloroform, or the like; an ester, e.g., ethyl acetate, n-propyl acetate, n-butyl acetate, t-butyl acetate, or the like; an ether, e.g., diethyl ether, diisopropyl ether, methyl t-butyl ether, tetrahydrofuran, dioxane, or the like; a polar aprotic solvent, e.g., N,N-dimethylformamide, N,N-dimethylacetamide, dimethylsulfoxide, sulfolane, N-methylpyrrolidone, or the like; a nitrile, e.g., acetonitrile, propionitrile, or the like; water; or any mixtures thereof.
[0019] Suitable temperatures for the reaction of step a) are less than about 100° C., less than about 80° C., less than about 60° C., less than about 40° C., less than about 20° C., less than about 0° C., or any other suitable temperatures.
[0020] Suitable times for completing the reaction in step a) depend on the temperature and other conditions, and may be generally less than about 30 hours, less than about 20 hours, less than about 10 hours, less than about 5 hours, less than about 2 hours, less than about 1 hour, or any other suitable times. Longer times also are suitable.
[0021] The product formed in step a) may be optionally recovered as a solid by conventional methods, including decantation, centrifugation, gravity filtration, suction filtration, or other techniques known in the art for the recovery of solids. The resulting solid may be optionally further dried. Drying may be suitably carried out using a tray dryer, vacuum oven, air oven, fluidized bed dryer, spin flash dryer, flash dryer, or the like, at atmospheric pressure or under reduced pressure. Drying may be carried out at temperatures less than about 100° C., less than about 60° C., less than about 40° C., or any other suitable temperatures, at atmospheric pressure or under reduced pressure, and in the presence or absence of an inert atmosphere such as nitrogen, argon, neon, or helium. The drying may be carried out for any desired time periods to achieve the desired quality of the product, such as, for example, about 1 to about 15 hours, or longer. Optionally, the product of step a) may be directly used in step b) without further isolation or after conventional work-up, such as, for example, quenching the reaction mixture with a quenching agent and extracting the product into a solvent.
[0022] Step b) involves partially hydrolyzing a compound of Formula VII to obtain a compound of Formula VIII. Step b) may be carried out in the presence of one or more suitable reagent such as a base, resin or any other suitable reagent. Suitable bases that may be used in step b) include but are not limited to: inorganic bases, such as, for example, ammonia, sodium hydroxide, potassium hydroxide, sodium methoxide, potassium t-butoxide, sodium t-butoxide, sodium carbonate, potassium carbonate, sodium bicarbonate, potassium bicarbonate, or the like; organic bases, such as, for example, triethylamine, n-propylamine, pyridine, N-methylmorpholine, diisopropylamine or diisopropylethylamine, or the like; resins including, but not limited to, ion exchange resins, such as resins bound to metal ions, including lithium, sodium, potassium, or the like; any mixtures thereof; or any other suitable reagents; either alone or as their aqueous solutions.
[0023] Optionally, step b) may be carried out in one or more suitable solvents. Suitable solvents include, but are not limited to: hydrocarbon solvents, including toluene, xylene, hexanes, heptanes, cyclohexane, or the like; halogenated hydrocarbon solvents, including dichloromethane, ethylene dichloride, chloroform, or the like; alcohol solvents, including methanol, ethanol, isopropyl alcohol, 1-propanol, 1-butanol, 2-butanol, or the like; ketone solvents, including acetone, ethyl methyl ketone, methyl isobutyl ketone, or the like; ester solvents, including ethyl acetate, n-propyl acetate, n-butyl acetate, t-butyl acetate, or the like; ether solvents, including diethyl ether, diisopropyl ether, methyl t-butyl ether, tetrahydrofuran, dioxane, or the like; polar aprotic solvents, including N,N-dimethylformamide, N,N-dimethylacetamide, dimethylsulfoxide, sulfolane, N-methylpyrrolidone, or the like; nitrile solvents, including acetonitrile, propionitrile, or the like; water; any mixtures thereof; or any other suitable solvents.
[0024] Suitable temperatures for the reaction of step b) may be less than about 150° C., less than about 120° C., less than about 100° C., less than about 80° C., less than about 60° C., less than about 40° C., or any other suitable temperatures. Suitable times for completion of hydrolysis in step b) depend on the temperature and other conditions and may be generally less than about 30 hours, less than about 24 hours, less than about 20 hours, less than about 10 hours, less than about 5 hours, less than about 1 hour, less than about 30 minutes, or any other suitable times.
[0025] Optionally, step b) may afford valganciclovir and pharmaceutically acceptable salts thereof by employing a suitable combination of reagent and solvent, including, for example, employing a base which performs partial hydrolysis of compound of Formula VII, as well as removal of protecting group P 1 .
[0026] The product obtained in step b) may be recovered by conventional methods including decantation, centrifugation, gravity filtration, suction filtration, or other techniques known in the art. The resulting compound may be in the form of a residue or a solid. When it is a solid, it may be crystalline or amorphous in nature. When it is in the form of a solid, it may be optionally further dried. Drying may be suitably carried out using a tray dryer, vacuum oven, air oven, fluidized bed dryer, spin flash dryer, flash dryer, or the like, at atmospheric pressure or under reduced pressure. Drying may be carried out at temperatures less than about 150° C., less than about 120° C., less than about 100° C., less than about 60° C., less than about 40° C., or any other suitable temperatures, at atmospheric pressure or under reduced pressure, and in the presence or absence of an inert atmosphere, such as nitrogen, argon, neon, or helium. The drying may be carried out for any desired time periods to achieve the desired quality of the product, such as, for example, about 1 to about 15 hours, or longer. The resulting solid may be crystalline or amorphous in nature.
[0027] Optionally, the product of step b) may be further purified one or more times by any suitable techniques known in the art. For example the product of step b) may be purified by precipitation, slurrying in a suitable solvent, or any other suitable techniques. The precipitation may be achieved by crystallization, such as by cooling a solution or by adding an anti-solvent to a solution of the product, or any other suitable methods known in the art. Anti-solvents are liquids in which valganciclovir or its salt is poorly soluble. Suitable anti-solvents include, but are not limited to: hydrocarbon solvents (e.g., hexanes, heptanes, cyclohexane, toluene, xylenes or the like); ether solvents (e.g., diethyl ether, diisopropyl ether, methyl t-butyl ether, or the like); or any other suitable anti-solvents.
[0028] Suitable solvents for purification include, but are not limited to: halogenated hydrocarbon solvents, including dichloromethane, ethylene dichloride, chloroform, or the like; alcohol solvents, including methanol, ethanol, 1-propanol, 2-propanol, 1-butanol, 2-butanol, or the like; ketone solvents, including acetone, ethyl methyl ketone, methyl isobutyl ketone, or the like; ester solvents, including ethyl acetate, n-propyl acetate, n-butyl acetate, t-butyl acetate, or the like; ether solvents, including diethyl ether, diisopropyl ether, methyl t-butyl ether, tetrahydrofuran, dioxane, or the like; polar aprotic solvents, including N,N-dimethylformamide, N,N-dimethylacetamide, dimethylsulfoxide, sulfolane, N-methylpyrrolidone, or the like; nitrile solvents, including acetonitrile, propionitrile, or the like; water; any mixtures thereof; or any other suitable solvents. Purification may be carried out at suitable temperatures less than about 150° C., less than about 120° C., less than about 100° C., less than about 80° C., less than about 60° C., less than about 40° C., or any other suitable temperatures. Suitable times for purification depend on the temperature and other conditions and may be generally less than about 30 hours, less than about 24 hours, less than about 20 hours, less than about 10 hours, less than about 5 hours, less than about 1 hour, less than about 30 minutes, or any other suitable times.
[0029] The product thus obtained may be recovered by conventional methods including decantation, centrifugation, gravity filtration, suction filtration, or other techniques known in the art. The resulting compound may be in the form of a residue or a solid. When it is in the form of a solid, it may be optionally further dried. Drying may be suitably carried out using a tray dryer, vacuum oven, air oven, fluidized bed dryer, spin flash dryer, flash dryer, or the like, at atmospheric pressure or under reduced pressure. Drying may be carried out at temperatures less than about 150° C., less than about 120° C., less than about 100° C., less than about 60° C., less than about 40° C., or any other suitable temperatures, at atmospheric pressure or under reduced pressure, and in the presence or absence of an inert atmosphere, such as nitrogen, argon, neon, or helium. The drying may be carried out for any desired time periods to achieve the desired quality of the product, such as, for example, about 1 to about 15 hours, or longer.
[0030] Step c) involves converting a compound of Formula VIII to valganciclovir or a salt thereof. Step c) may be carried out using any suitable deprotection technique, including, for example, catalytic hydrogenation using hydrogen gas in the presence of a metal, including Raney nickel, palladium on carbon, or the like; or hydrolysis using an acid or base; or any other suitable deprotection agents known in the art. Optionally, catalytic hydrogenation may be carried out in the presence of one or more suitable reagent. Suitable reagents that may be used include, but are not limited to, acids, bases, resins, or mixtures thereof, either alone or as their solutions in water, organic solvents or their mixtures. Suitable acids that may be used in step c) include but are not limited to: organic acids, including acetic acid, formic acid, propionic acid, butyric acid, isobutyric acid, fumaric acid, oxalic acid, tartaric acid, citric acid, or the like; and inorganic acids, including hydrochloric acid, hydrobromic acid, hydroiodic acid, nitric acid, sulfuric acid, phosphoric acid, methanesulfonic acid, p-toluenesulfonic acid, or the like. Suitable bases that may be used in step c) include but are not limited to: inorganic bases, including ammonia, sodium hydroxide, potassium hydroxide, sodium methoxide, potassium t-butoxide, sodium t-butoxide, sodium carbonate, potassium carbonate, sodium bicarbonate, potassium bicarbonate, or the like; and organic bases, such as triethylamine, pyridine, N-methylmorpholine, diisopropylamine, diisopropylethylamine, or the like. Suitable resins that may be used in step c) include, but are not limited to, ion exchange resins, such as: resins bound to metal ions, including lithium, sodium, potassium, or the like; and resins bound to acids, including phosphoric, sulfonic, methanesulfonic, p-toluenesulfonic, or the like.
[0031] Optionally, the deprotection in step c) may be carried out in the presence of one or more suitable solvents. Suitable solvents that may be used in step c) include, for example: alcohol solvents, e.g., methanol, ethanol, isopropyl alcohol, 1-propanol, 1-butanol, 2-butanol, or the like; ketone solvents, e.g., acetone, ethyl methyl ketone, methyl isobutyl ketone, or the like; hydrocarbon solvents, e.g., toluene, xylene, hexanes, heptanes, cyclohexane, or the like; halogenated hydrocarbon solvents, e.g., dichloromethane, ethylene dichloride, chloroform, or the like; ester solvents, e.g., ethyl acetate, n-propyl acetate, n-butyl acetate, t-butyl acetate, or the like; ether solvents, e.g., diethyl ether, diisopropyl ether, methyl t-butyl ether, tetrahydrofuran, dioxane, or the like; polar aprotic solvents, e.g., N,N-dimethylformamide, N,N-dimethylacetamide, dimethylsulfoxide, sulfolane, N-methylpyrrolidone, or the like; nitrile solvents, e.g., acetonitrile, propionitrile, or the like; water; or any mixtures thereof.
[0032] Step c) may be carried out at suitable temperatures less than about 150° C., less than about 100° C., less than about 60° C., less than about 40° C., or any other suitable temperatures. Optionally, step c) may be carried out at atmospheric pressure or under pressure. Suitable pressures that may be used are less than about 10 kg/cm 2 , less than about 5 kg/cm 2 , less than about 3 kg/cm 2 , less than about 1 kg/cm 2 , or any other suitable pressures. Suitable times for completing step c) depend on temperature and other conditions and may be generally less than about 15 hours, less than about 10 hours, less than about 5 hours, less than about 2 hours, less than about 30 minutes, or any other suitable times.
[0033] Optionally, the product formed in step c) after deprotection, which comprises valganciclovir or a salt thereof, may be further treated with suitable reagents before or after conventional work-up process or after isolation of the compound as described in International Application No. PCT/US2009/058397. Suitable reagents that may be used for the treatment include, but are not limited to, phosphines, resins, or mixtures thereof, or any other suitable reagents. Suitable phosphines that may be used include, but are not limited to, triphenylphosphine, tri-n-butylphosphine, or the like. Suitable resins that may be used include, but are not limited to, ion exchange resins, including resins bound to metal ions, such as lithium, sodium, potassium, or the like, and resins bound to acids, such as phosphoric, sulfonic, methanesulfonic, p-toluenesulfonic, or the like.
[0034] Optionally, one or more suitable solvents may be used in the treatment. Suitable solvents that may be used include, for example: alcohol solvents, e.g., methanol, ethanol, isopropyl alcohol, 1-propanol, 1-butanol, 2-butanol, or the like; ketone solvents, e.g., acetone, ethyl methyl ketone, methyl isobutyl ketone, or the like; hydrocarbon solvents, e.g., toluene, xylene, hexanes, heptanes, cyclohexane, or the like; halogenated hydrocarbon solvents, e.g., dichloromethane, ethylene dichloride, chloroform, or the like; ester solvents, e.g., ethyl acetate, n-propyl acetate, n-butyl acetate, t-butyl acetate, or the like; ether solvents, e.g., diethyl ether, diisopropyl ether, methyl t-butyl ether, tetrahydrofuran, dioxane, or the like; polar aprotic solvents, e.g., N,N-dimethylformamide, N,N-dimethylacetamide, dimethylsulfoxide, sulfolane, N-methylpyrrolidone, or the like; nitrile solvents, e.g., acetonitrile, propionitrile, or the like; water; or any mixtures thereof.
[0035] The treatment may be carried out at suitable temperatures less than about 150° C., less than about 100° C., less than about 60° C., less than about 40° C., or any other suitable temperatures, at atmospheric pressure or elevated pressures. Suitable pressures are less than about 10 kg/cm 2 , less than about 5 kg/cm 2 , less than about 3 kg/cm 2 , less than about 1 kg/cm 2 , or any other suitable pressures. Suitable times for completing the treatment depend on temperature and other conditions and may be generally less than about 15 hours, less than about 10 hours, less than about 5 hours, less than about 2 hours, less than about 30 minutes, or any other suitable times.
[0036] The product obtained after said treatment may be recovered using conventional methods including decantation, centrifugation, gravity filtration, suction filtration, or other techniques known in the art. The resulting compound may be in the form of a residue or a solid. When it is in the form of a solid, it may be optionally further dried. Drying may be suitably carried out using a tray dryer, vacuum oven, air oven, fluidized bed dryer, spin flash dryer, flash dryer, or the like, at atmospheric pressure or under reduced pressure. Drying may be carried out at temperatures less than about 150° C., less than about 120° C., less than about 100° C., less than about 60° C., less than about 40° C., or any other suitable temperatures, at atmospheric pressure or under reduced pressure, and in the presence or absence of an inert atmosphere, such as nitrogen, argon, neon, or helium. The drying may be carried out for any desired time periods to achieve the desired quality of the product, such as, for example, about 1 to about 15 hours, or longer.
[0037] Optionally, the product obtained after the treatment, which comprises valganciclovir or a salt thereof, may be further purified using purification techniques known in the art, for example using column chromatography or various types of isolation methods including precipitation, adding an anti-solvent to a solution, or the like, in order to achieve a diastereomeric ratio of valganciclovir or its salt in the range of (45:55) to (55:45). Suitable solvents that may be used for purification include, but are not limited to: alcohol solvents, e.g., methanol, ethanol, isopropyl alcohol, 1-propanol, 1-butanol, 2-butanol, or the like; ketone solvents, e.g., acetone, ethyl methyl ketone, methyl isobutyl ketone, or the like; ester solvents, e.g., ethyl acetate, n-propyl acetate, n-butyl acetate, t-butyl acetate, or the like; polar aprotic solvents, e.g., N,N-dimethylformamide, N,N-dimethylacetamide, dimethylsulfoxide, sulfolane, N-methylpyrrolidone, or the like; water; any mixtures thereof in varying proportions; or any other suitable solvents.
[0038] The purification may be carried out at suitable temperatures less than about 150° C., less than about 100° C., less than about 60° C., less than about 40° C., or any other suitable temperatures. Suitable times for completing the purification depend on temperature and other conditions and may be generally less than about 15 hours, less than about 10 hours, less than about 5 hours, less than about 2 hours, less than about 30 minutes, or any other suitable times.
[0039] The product thus obtained may be recovered using conventional methods including decantation, centrifugation, gravity filtration, suction filtration, or other techniques known in the art. The resulting compound may be in the form of a residue or a solid. When it is in the form of a solid, it may be in the form of a crystalline compound, a solvate, an amorphous compound, or a mixture thereof. The solid may be optionally further dried. Drying may be suitably carried out using a tray dryer, vacuum oven, air oven, fluidized bed dryer, spin flash dryer, flash dryer, or the like, at atmospheric pressure or under reduced pressure. Drying may be carried out at temperatures less than about 150° C., less than about 120° C., less than about 100° C., less than about 60° C., less than about 40° C., or any other suitable temperatures, at atmospheric pressure or under reduced pressure, and in the presence or absence of an inert atmosphere, such as nitrogen, argon, neon, or helium. The drying may be carried out for desired time periods to achieve the desired quality of the product, such as, for example, about 1 to about 15 hours, or longer.
[0040] Valganciclovir or a salt thereof thus obtained may be optionally milled or micronized before or after drying of the product to get desired particle size. Milling or micronization may be performed by using techniques including; without limitation; milling using mills such as ball mill, roller mill, hammer mill, jet mill, air jet mill, co mill, multi mill or any other conventional technique. The pressures that may be used for milling or micronization are less than about 20 kg/cm 2 , less than about 10 kg/cm 2 , less than about 8 kg/cm 2 , less than about 6 kg/cm 2 , less than about 4 kg/cm 2 , or less than about 3 kg/cm 2 .
[0041] Valganciclovir or its salt of the present application is substantially free of metal contaminants. The metal contaminants can include, but are not limited to, palladium, nickel, cobalt, or any other metals. “Substantially free of metal contaminants” as used herein unless otherwise defined refers to a metal content less than about 50 ppm (parts per million), less than about 40 ppm, less than about 30 ppm, less than about 20 ppm, less than about 10 ppm, less than about 5 ppm, less than about 2 ppm, or less than about 1 ppm. All tautomeric forms of the compounds within the present application are within the scope of the present invention. Additionally, structures depicted here are also meant to include compounds that differ only in the presence of one or more isotopically enriched atoms. For example, compounds having the present structure except for the replacement of hydrogen by deuterium or tritium, or the replacement of a carbon by a 13 C— or 14 C-enriched carbon are within the scope of this invention.
DEFINITIONS
[0042] The following definitions are used in connection with the present application unless the context indicates otherwise. DMSO is dimethylsulfoxide and HPLC is high-pressure liquid chromatography. The term “reacting” is intended to represent bringing the chemical reactants together under conditions such to cause the chemical reaction indicated to take place.
[0043] An “alcohol solvent” is an organic solvent containing a carbon bound to a hydroxyl group. “Alcohol solvents” include but are not limited to methanol, ethanol, 2-nitroethanol, 2-fluoroethanol, 2,2,2-trifluoroethanol, hexafluoroisopropyl alcohol, ethylene glycol, 1-propanol, 2-propanol (isopropyl alcohol), 2-methoxyethanol, 1-butanol, 2-butanol, i-butyl alcohol, t-butyl alcohol, 2-ethoxyethanol, diethylene glycol, 1-, 2-, or 3-pentanol, neo-pentyl alcohol, t-pentyl alcohol, diethylene glycol monomethyl ether, diethylene glycol monoethyl ether, cyclohexanol, benzyl alcohol, phenol, glycerol, C 1-6 alcohols, or the like.
[0044] “Amine-protecting group” refers to a radical when attached to a nitrogen atom in a target molecule is capable of surviving subsequent chemical reactions applied to the target molecule i.e. hydrogenation, reaction with acylating agents, alkylation etc. The amine-protecting group can later be removed. Amine protecting groups include, but are not limited to, fluorenylmethoxycarbonyl (FMOC), tert-butoxycarbonyl (t-BOC), benzyloxycarbonyl (Z), those of the acyl type (e.g., formyl, benzoyl, trifluoroacetyl, p-tosyl, aryl- and alkylphosphoryl, phenyl- and benzylsulfonyl, o-nitrophenylsulfenyl, o-nitrophenoxyacetyl), and of the urethane type (e.g. tosyloxyalkyloxy-, cyclopentyloxy-, cyclohexyloxy-, 1,1-dimethylpropyloxy, 2-(p-biphenyl)-2-propyloxy- and benzylthiocarbonyl). Amine-protecting groups are made using a reactive agent capable of transferring an amine-protecting group to a nitrogen atom in the target molecule. Examples of an amine-protecting agent include, but are not limited to, C 1 -C 6 aliphatic acid chlorides or anhydrides, C 6 -C 14 arylcarboxylic acid chlorides or anhydrides, t-butyl chloroformate, di-tert-butyl dicarbonate, butoxycarbonyloxyimino-2-phenylacetonitrile, t-butoxycarbonyl azide, t-butyl fluoroformate, fluorenylmethoxycarbonyl chloride, fluorenylmethoxycarbonyl azide, fluorenylmethoxycarbonyl benzotriazol-1-yl, (9-fluorenylmethoxycarbonyl)succinimidyl carbonate, fluorenylmethoxycarbonyl pentafluorophexoxide, trichloroacetyl chloride, methyl-, ethyl-, trichloromethyl-chloroformate, and other amine protecting agents known in the art. Examples of such known amine-protecting agents are found in pages 385-397 of T. W. Green, P. G. M. Wuts, “Protective Groups in Organic Synthesis, Second Edition”, Wiley-Interscience, New York, 1991.
[0045] An “anti-solvent” as used herein refers to a liquid in which valganciclovir or a salt thereof is less soluble or poorly soluble. Suitable anti-solvents include: hydrocarbon solvents, e.g., hexanes, heptanes, cyclohexane, toluene, xylenes, or the like; ether solvents, e.g., diethyl ether, diisopropyl ether, methyl t-butyl ether, or the like; or any other suitable anti-solvents.
[0046] An “ester solvent” is an organic solvent containing a carboxyl group —(C═O)—O-bonded to two other carbon atoms. “Ester solvents” include, but are not limited to, ethyl acetate, n-propyl acetate, n-butyl acetate, isobutyl acetate, t-butyl acetate, ethyl formate, methyl acetate, methyl propanoate, ethyl propanoate, methyl butanoate, ethyl butanoate, C 3-6 esters, or the like.
[0047] An “ether solvent” is an organic solvent containing an oxygen atom —O— bonded to two other carbon atoms. “Ether solvents” include but are not limited to diethyl ether, diisopropyl ether, methyl t-butyl ether, glyme, diglyme, tetrahydrofuran, 1,4-dioxane, dibutyl ether, dimethylfuran, 2-methoxyethanol, 2-ethoxyethanol, anisole, C 2-6 ethers, or the like.
[0048] A “halogenated hydrocarbon solvent” is an organic solvent containing a carbon bound to a halogen. “Halogenated hydrocarbon solvents” include, but are not limited to, dichloromethane, 1,2-dichloroethane, trichloroethylene, perchloroethylene, 1,1,1-trichloroethane, 1,1,2-trichloroethane, chloroform, carbon tetrachloride, or the like.
[0049] “Hydrocarbon solvent” refers to a liquid hydrocarbon, which may be linear, branched, or cyclic. It may be saturated, unsaturated, or aromatic. It is capable of dissolving a solute to form a uniformly dispersed solution. Examples of a hydrocarbon solvent include, but are not limited to, n-pentane, isopentane, neopentane, n-hexane, isohexane, 3-methylpentane, 2,3-dimethylbutane, neohexane, n-heptane, isoheptane, 3-methylhexane, neoheptane, 2,3-dimethylpentane, 2,4-dimethylpentane, 3,3-dimethylpentane, 3-ethylpentane, 2,2,3-trimethylbutane, n-octane, isooctane, 3-methylheptane, neooctane, C 5 -C 8 aliphatic hydrocarbons, cyclohexane, methylcyclohexane, ligroin, petroleum ethers, benzene, toluene, ethylbenzene, m-xylene, o-xylene, p-xylene, indane, naphthalene, tetralin, trimethylbenzene, C 6 -C 10 aromatic hydrocarbons, or mixtures thereof.
[0050] A “ketone solvent” is an organic solvent containing a carbonyl group —(C═O)— bonded to two other carbon atoms. “Ketone solvents” include, but are not limited to, acetone, ethyl methyl ketone, diethyl ketone, methyl isobutyl ketone, C 3-6 ketones, or the like.
[0051] A “nitrile solvent” is an organic solvent containing a cyano —(C≡N) bonded to another carbon atom. “Nitrile solvents” include, but are not limited to, acetonitrile, propionitrile, C 2-6 nitriles, or the like.
[0052] A “polar aprotic solvent” has a dielectric constant greater than 15 and is at least one selected from the group consisting of amide-based organic solvents, such as hexamethyl phosphoramide (HMPA), and hexamethyl phosphorus triamide (HMPT); nitro-based organic solvents, such as nitromethane, nitroethane, nitropropane, and nitrobenzene; ester-based organic solvents, such as γ-butyrolactone, ethylene carbonate, propylene carbonate, butylene carbonate, dimethyl carbonate, and propiolactone; pyridine-based organic solvents, such as pyridine and picoline; sulfone-based solvents, such as dimethyl sulfone, diethyl sulfone, diisopropylsulfone, 2-methylsulfolane, 3-methylsulfolane, 2,4-dimethyl-sulfolane, 3,4-dimethyl sulfolane, 3-sulfolene, and sulfolane; and nitrile-based organic solvents, such as acetonitrile, propionitrile, and benzonitrile. These organic solvents may be used alone or two or more of these may be combined appropriately.
[0053] “Protecting group” means a chemical group that (a) preserves a reactive group from participating in an undesirable chemical reaction, and (b) can be removed after protection of the reactive group is no longer required. For example, a benzyl group is a protecting group for a primary hydroxyl function. “Amine-protecting group” means a protecting group that preserves a reactive amine group that otherwise would be modified by certain chemical reactions. Useful amine protecting groups include, but are not limited to: benzyloxycarbonyl (Cbz), tert-butyloxycarbonyl (BOC), 9-fluorenylmethoxycarbonyl (FMOC), trifluoroacetyl, benzyl, trityl, formyl, or the like.
[0054] “Suitable coupling agent” refers to a compound, molecule, or substance, capable of activating carboxylic acids with respect to nucleophilic attack. In some embodiments, the suitable coupling agents are capable of activating carboxylic acids where the attacking nucleophile is an amine or alcohol, resulting in amide or ester formation. Non-limiting examples of such suitable coupling agents include carbodiimide compounds (e.g. N,N′-dicyclohexylcarbodiimide (DCC), N,N′-diisopropylcarbodiimide (DIC), 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride (EDC.HCl), or the like). Carbodiimide compounds may be either used alone or in combination with HOAt, HOBt, or HODhbt. Further examples of suitable coupling agents include alkyl chloroformate compounds (e.g. ethyl chloroformate, isobutyl chloroformate, or the like) that are generally used with a tertiary amine like triethyl amine, diethyl azodicarboxylate (DEAD) with triphenylphosphine (the Mitsunobu reaction), various chlorosilanes, chlorosulfonyl isocyanate, N,N′-carbonyldiimidazole (CDI), phosphonium reagents (e.g. BOP, AOP, PyBOP, PyAOP, BroP, PyBroP, CF 3 —NO 2 -PyBOP or the like), in situ acid fluoride generators (e.g. TFFH, BTFFH, DAST, cyanuric fluoride, or the like), aminium reagents (e.g. HBTU, HATU, HBPyU, HAPyU, or the like) phosphinyls (e.g. DPPA, DEPC, or the like), pentafluorophenyl active ester generators (e.g. PfTU, PfPyU, FDPP, PFP-trifluoroacetate, FPFOH plus DCC, or the like), mixed carbon anhydrides (e.g. EEDQ, IIDQ, or the like), CIP, and BOP-CI.
[0055] All percentages and ratios used herein are by weight of the total composition and all measurements made are at about 25° C. and about atmospheric pressure, unless otherwise designated. All temperatures are in degrees Celsius unless specified otherwise. As used herein, “comprising” (open ended) means the elements recited, or their equivalent in structure or function, plus any other element or elements that are not recited. The terms “having” and “including” are also to be construed as open ended. All ranges recited herein include the endpoints, including those that recite a range “between” two values. Terms such as “about,” “generally,” “substantially,” or the like are to be construed as modifying a term or value such that it is not an absolute. Such terms will be defined by the circumstances and the terms that they modify as those terms are understood by those of skill in the art. This includes the degree of expected experimental error, technique error, and instrument error for a given technique used to measure a value.
[0056] Certain specific aspects and embodiments of the present disclosure will be explained in more detail with reference to the following examples, which are provided only for purposes of illustration and should not be construed as limiting the scope of the disclosure in any manner. Reasonable variations of the described procedures are intended to be within the scope of the present disclosure.
EXAMPLES
[0057]
Example 1
[0058] PREPARATION OF BIS-(Cbz-L-VALYL)-ESTER OF GANCICLOVIR (FORMULA IX). To a solution of ganciclovir (10.0 g) in DMSO (80 mL) is added Cbz-L-valine (29.5 g), 4-(dimethylamino)-pyridine (DMAP) (400 mg), and dicyclohexylcarbodiimide (DCC) (24.2 g) at 25-30° C. The mass is maintained at 25-30° C. for 5-6 hours. The mass is filtered and washed with DMSO (20 mL). The filtrate is added to 10% sodium chloride solution (200 mL) and ethyl acetate (70 mL). The organic layer is separated and aqueous layer is washed with ethyl acetate (30 mL). The combined organic layer is washed with 20% sodium chloride solution (100 mL). Cyclohexane (300 mL) is added to the organic layer and the mixture is maintained for 12-14 hours at 25-30° C. The formed solid is collected by filtration, washed with cyclohexane (50 mL), and dried to afford the title compound. Yield: 26.5 g. Purity by HPLC: 98.87%; mono-(Cbz-L-valyl)-ester of Formula X: 0.58%.
Example 2
[0059] PREPARATION OF BIS-(Cbz-L-VALYL)-ESTER OF GANCICLOVIR (FORMULA IX). To a solution of ganciclovir (10.0 g) in DMSO (175 mL) is added Cbz-L-valine (39.3 g), 4-(dimethylamino)-pyridine (DMAP) (100 mg) and dicyclohexylcarbodiimide (DCC, 36.3 g) at 25-30° C. The mass is maintained at 25-30° C. for 5-6 hours. The mass is filtered and washed with DMSO (20 mL). The filtrate is added to water (1200 mL) and ethyl acetate (100 mL) is added to produce a clear solution at 25-30° C. n-Hexane (500 mL) is added and the mass is maintained at 25-30° C. for 15-20 hours. The solid is collected by filtration, washed with n-hexane (50 mL), and dried to afford the title compound. Yield: 27.0 g. Purity by HPLC: 95.27%; mono-(Cbz-L-valyl)-ester of Formula X: 3.11%.
[0000]
Example 3
[0060] PREPARATION OF MONO-(Cbz-L-VALYL)-ESTER OF GANCICLOVIR (FORMULA X). To a solution of the bis-(Cbz-L-valyl)-ester of ganciclovir of Formula IX (25 g) in methanol (375 mL) is added diisopropylethylamine (33.3 g) at 25-30° C. The mixture is maintained for 15-20 hours at 25-30° C. Acetic acid (10.2 mL) is added and the mass is maintained for another 1-2 hours at 25-30° C. The solvent is evaporated and water (500 mL) and ethyl acetate (400 mL) are added, followed by refluxing for 30-60 minutes. The mass is maintained at 30-35° C. for 1-2 hours. The solid is collected by filtration, washed with ethyl acetate (70 mL), and is dried to afford the title compound. Yield: 7.5 g. Purity by HPLC: 96.5%; ganciclovir: 2.0%; bis-(Cbz-L-valyl)-ester of ganciclovir of Formula IX: 0.40%.
Example 4
[0061] PREPARATION OF MONO-(Cbz-L-VALYL)-ESTER OF GANCICLOVIR (FORMULA X). To a solution of bis-(Cbz-L-valyl)-ester of ganciclovir of Formula IX (100 g) in methanol (200 mL) is added n-propylamine (12.28 g) at 25-30° C. The mixture is maintained for 24 hours at 25-30° C. Acetic acid (12.42 mL) is added, followed by addition of water (1.0 L) at 5° C. The solid is collected by filtration, washed with water (500 mL) and ethyl acetate (2×100 mL), and then dried to afford the crude title compound. The crude mono-(Cbz-L-valyl)-ester of ganciclovir of Formula X is further purified by repeated precipitation, involving dissolving in acetic acid followed by adding water and collecting the solid by filtration. The resulting compound is further purified by repeated crystallization from a mixture of ethyl acetate and water, to finally afford pure mono-(Cbz-L-valyl)-ester of ganciclovir of Formula X. Purity by HPLC: 97.65%; ganciclovir: 1.56%; bis-(Cbz-L-valyl)-ester of ganciclovir of Formula IX: 0.43%.
Example 5
[0062] PREPARATION OF MONO-(Cbz-L-VALYL)-ESTER OF GANCICLOVIR (FORMULA X). To a solution of bis-(Cbz-L-valyl)-ester of ganciclovir of Formula IX (15 g) in methanol (225 mL) is added diisopropylamine (10.5 g) at 25-30° C. The mixture is maintained for 15-20 hours at 25-30° C. Acetic acid (8.24 mL) is added and the mass is maintained for another 1-2 hours at 25-30° C. The solvent is evaporated, and water (225 mL) and ethyl acetate (150 mL) are added, followed by refluxing for 30-60 minutes. The mass is maintained at 30-35° C. for 2-3 hours. The solid is collected by filtration, washed with water (100 mL), and dried to afford the crude title compound. The crude mono-(Cbz-L-valyl)-ester of ganciclovir of Formula X is further purified by repeated crystallization from a mixture of ethyl acetate and water to finally afford pure mono-(Cbz-L-valyl)-ester of ganciclovir of Formula X. Yield: 4.5 g. Purity by HPLC: 97.2%; ganciclovir: 0.97%; bis-(Cbz-L-valyl)-ester of ganciclovir of Formula IX: 1.25%.
Example 6
[0063] PREPARATION OF VALGANCICLOVIR HYDROCHLORIDE SALT. To a solution of mono-(Cbz-L-valyl)-ester of ganciclovir of Formula X (6.5 g) in ethanol (208 mL) in an autoclave vessel is added aqueous HCl (1.62 mL) and 10% palladium on carbon (50% wet, 0.78 g), and a hydrogen pressure of 0.8-1 kg/cm 2 is maintained for 6-7 hours at 25-30° C. The mass is filtered and the collected solid is washed with ethanol (30 mL). The filtrate is evaporated below 40° C. to remove ethanol and the volume is adjusted to 10 mL with water. The filtrate is washed with toluene (3×13 mL) and 1-butanol (2×13 mL) at 25-30° C. Isopropyl alcohol (39 mL) is added to the mixture and stirred for 15 hours for solid formation at 25-30° C. Isopropyl alcohol (32.5 mL) is added and the mixture is stirred for 2-3 hours at 25-30° C. The mass is cooled and formed solid is collected by filtration at −10 to −15° C., washed with chilled isopropyl alcohol (13 mL), and dried under reduced pressure at 40-50° C. to afford the title compound. Yield: 3.6 g. Purity by HPLC: 96.25%; ganciclovir: 2.31%; bis-(Cbz-L-valyl)-ester of ganciclovir of Formula IX: 0.20%.
Example 7
[0064] PREPARATION OF VALGANCICLOVIR HYDROCHLORIDE SALT. To a solution of mono-(Cbz-L-valyl)-ester of ganciclovir of Formula X (10 g) in methanol (320 mL) in an autoclave vessel is added aqueous HCl (2.33 mL) and 10% palladium on carbon (50% wet, 1.0 g), and a hydrogen pressure of 0.7-1 kg/cm 2 is maintained for 17-18 hours at 25-30° C. The mass is filtered and the collected solid is washed with methanol (46 mL). To the filtrate is added triphenylphosphine (25 mg) and charcoal. The reaction mass is maintained for 1-2 hours at 25-30° C. The mass is filtered and the collected solid is washed with methanol (30 mL). To the filtrate is added water (10 mL), the mixture is evaporated below 40° C. to remove methanol, and the volume is adjusted to 13.5 mL with water. The aqueous layer is washed with toluene (3×18 mL) and 1-butanol (2×18 mL) at 25-30° C. Isopropyl alcohol (100 mL) is added to the mixture and maintained for 15-18 hours for solid formation at 25-30° C. Cyclohexane (45 mL) is added to the reaction mass. Reaction mass is cooled and maintained for 1-2 hours at 0 to −15° C. The formed solid is collected by filtration at −10 to −15° C., washed with chilled isopropyl alcohol (18 mL), and dried under reduced pressure at 40-50° C. to afford the title compound. Yield: 5.0 g. Purity by HPLC: 98.24%; ganciclovir: 0.67%; methoxymethyl guanine: 0.09%; bis-(Cbz-L-valyl)-ester of ganciclovir of Formula IX: 0.33%; Pd content: 42 ppm.
Example 8
[0065] PREPARATION OF BIS-(Cbz-L-VALYL)-ESTER OF GANCICLOVIR (FORMULA IX). Dicyclohexylcarbodiimide (DCC) (64.6 g) solution (DCC (64.6 kg) in DMSO (40 mL) is slowly added to a reaction mixture containing 9-((2-hydroxy-1-(hydroxymethyl)ethoxy)methyl) guanine (20 g), Cbz-L-valine (69 g), 4-(dimethylamino)-pyridine (DMAP) (0.8 g), and DMSO (140 mL) at 18-25° C. and the reaction mixture maintained at 18-25° C. for 30 minutes. The reaction mixture temperature is increased to 28° C. and stirred for 6 hours. The mass is filtered and the collected solid washed with DMSO (40 mL). The filtrate is added to a mixture of 5% sodium bicarbonate solution (500 mL) and ethyl acetate (140 mL) at 25-30° C. and stirred for 15 minutes. The organic layer is separated and the aqueous layer is extracted with ethyl acetate (60 mL). The combined organic layer is washed with 20% sodium chloride solution (2×200 mL). Cyclohexane (460 mL) is added to the organic layer at 25-35° C. and the mixture is maintained for 17 hours at 25-35° C. Reaction mixture is further cooled to 10-15° C. and maintained at 16° C. for 15 minutes. The separated solid is collected by filtration, washed with a pre-cooled (10-15° C.) cyclohexane (100 mL) and ethyl acetate (30 mL) mixture, and dried at 48° C. for 4 hours, under reduced pressure. Charged the dried compound and water (400 mL) into round bottom flask and stirred at 28° C. for 1 hour 30 minutes. Reaction mixture is filtered, the collected solid is washed with water (80 mL), and dried at 48° C. for 22 hours under reduced pressure to afford 47.8 g of the title compound. Purity by HPLC: 99.8%.
Example 9
[0066] PREPARATION OF MONO-(Cbz-L-VALYL)-ESTER OF GANCICLOVIR (FORMULA X). Bis-(Cbz-L-valyl)-ester of ganciclovir of Formula IX (100 g) and methanol (200 mL) are charged into round bottom flask and stirred for 5 minutes. n-Propylamine (13.6 mL) is added to the reaction mass at 27° C. and maintained at 27° for 30 hours. Acetic acid (9.5 mL) is slowly added and the mass and cooled to 16° C. Acetic acid (390.5 mL) is added to the reaction mass at 15-20° C. and maintained reaction mass at 12° C. for 1 hour. The resultant reaction mass is slowly added to water (2000 mL) at 12° C. and maintained at 12° C. for 1 hour. The separated solid is collected by filtration, washed with pre-cooled (10-15° C.) water (1000 mL), and dried at 45° C. for 12 hours under reduced pressure. The obtained dry compound (80 g) and acetic acid (320 mL) is charged into round bottom flask and stirred for 1 hour. The resultant reaction mass is slowly added to water (1600 mL) at 12° C. and stirred for 1 hour. The separated solid is collected by filtration and washed with pre-cooled (10-15° C.) water (1600 mL). The obtained wet compound and ethyl acetate (600 mL) are charged into round bottom flask and stirred at 62° C. for 8 minutes. Reaction mass is cooled to 26° C. and stirred for 1 hour. The separated solid is collected by filtration and washed with ethyl acetate (60 mL). The obtained wet compound, ethyl acetate (750 mL), and water (22.5 mL) are charged into round bottom flask and stirred at 62° C. for 75 minutes. The reaction mass is cooled to 26° C. and stirred for 80 minutes. The separated solid is collected by filtration and washed with ethyl acetate (45 mL). The obtained wet compound, ethyl acetate (270 mL), and water (18 mL) are charged into round bottom flask and stirred at 62° C. for 1 hour. Reaction mass is cooled to 6° C. and stirred for 1 hour 30 minutes. The separated solid is collected by filtration and washed with ethyl acetate (36 mL). The obtained wet compound, ethyl acetate (216 mL), and water (14.4 mL) are charged into round bottom flask and stirred at 62° C. for 1 hour 30 minutes. Reaction mass is cooled to 26° C. and stirred for 70 minutes. The separated solid is collected by filtration, washed with ethyl acetate (28.8 mL), and dried at 45-50° C. for 10 hours under reduced pressure. Dry compound is milled and further dried at 45-50° C. for 24 hours to afford 28.0 g of the title compound. Purity by HPLC: 99.59%; ganciclovir: 0.37%; bis-(Cbz-L-valyl)-ester of ganciclovir of Formula IX: 0.22%.
Example 10
[0067] PREPARATION OF VALGANCICLOVIR HYDROCHLORIDE SALT. To a solution of mono-(Cbz-L-valyl)-ester of ganciclovir of Formula X (10 g) in methanol (200 mL) in an autoclave vessel is added aqueous HCl (2.2 mL) and 10% palladium on carbon (50% wet, 1.0 g). A hydrogen pressure of 3.0-3.5 kg/cm 2 is maintained for 2 hours 30 minutes at 29° C. The mass is filtered and the collected solid is washed with methanol (20 mL). To the filtrate is added triphenylphosphine (20 mg) and charcoal. The reaction mass is maintained for 75 minutes at 28° C. The mass is filtered and the collected solid is washed with methanol (30 mL). The filtrate is evaporated below 40° C. to remove methanol and the water (10 mL) is added and stirred for 15 minutes. Isopropyl alcohol (200 mL) is added to the mixture at 3° C. and stirred for 3 hours. The separated solid is filtered and washed with isopropyl alcohol (20 mL). The obtained wet compound, water (15 mL) and n-propyl alcohol (30 mL) are charged into round bottom flask and stirred for 15 minutes. The resultant reaction mass is filtered and washed with mixture of water (5 mL) and n-propyl alcohol (10 mL). To the obtained filtrate n-propyl alcohol (160 mL) is added at 5° C. and stirred for 2 hours 10 minutes. The separated solid is filtered, washed with n-propyl alcohol (10 mL), and dried at 45° C. for 17 hours under reduced pressure to afford 5.7 g of the title compound.
[0068] Throughout this application, various publications are referenced. The disclosures of these publications in their entireties are hereby incorporated by reference into this application in order to more fully describe the state of the art as known to those skilled therein as of the date of the application described and claimed herein.
[0069] While particular embodiments of the present invention have been illustrated and described, it would be obvious to those skilled in the art that various other changes and modifications can be made without departing from the spirit and scope of the invention. It is therefore intended to cover in the appended claims all such changes and modifications that are within the scope of this invention. | The application relates to processes for preparing valganciclovir and pharmaceutically acceptable salts thereof, as well as intermediates for the processes. valganciclovir hydrochloride is represented by Formula II. | 2 |
This non-provisional application claims priority from provisional application U.S. Ser. No. 60/081,250 filed on Apr. 9, 1998 (now abandoned).
BACKGROUND OF THE INVENTION
The present invention relates to the cyclization of a key intermediate in the synthesis of an endothelin antagonist.
The endothelin antagonist compound possessing a high affinity for at least one of two receptor subtypes, are responsible for the dilation of smooth muscle, such as blood vessels or in the trachea. The endothelin antagonist compounds provide a potentially new therapeutic target, particularly for the treatment of hypertension, pulmonary hypertension, Raynaud's disease, acute renal failure, myocardial infarction, angina pectoris, cerebral infarction, cerebral vasospasm, arteriosclerosis, asthma, gastric ulcer, diabetes, restenosis, prostatauxe endotoxin shock, endotoxin-induced multiple organ failure or disseminated intravascular coagulation, and/or cyclosporin-induced renal failure or hypertension.
Endothelin is a polypeptide composed of amino acids, and it is produced by vascular endothelial cells of human or pig. Endothelin has a potent vasoconstrictor effect and a sustained and potent pressor action (Nature, 332,411-415 (1988)).
Three endothelin isopeptides (endothelin-1, endothelin-2 and endothelin-3), which resemble one another in structure, exist in the bodies of animals including human, and these peptides have vasoconstriction and pressor effects (Proc. Natl. Acad, Sci, USA, 86, 2863-2867 (1989)).
As reported, the endothelin levels are clearly elevated in the blood of patients with essential hypertension, acute myocardial infarction, pulmonary hypertension, Raynaud's disease, diabetes or atherosclerosis, or in the washing fluids of the respiratory tract or the blood of patients with asthmaticus as compared with normal levels (Japan, J. Hypertension, 12, 79, (1989), J. Vascular medicine Biology, 2, 207 (1990), Diabetologia, 33, 306-310 (1990), J. Am. Med. Association, 264, 2868 (1990), and The Lancet, ii, 747-748 (1989) and ii, 1144-1147 (1990)).
Further, an increased sensitivity of the cerebral blood vessel to endothelin in an experimental model of cerebral vasospasm (Japan. Soc. Cereb. Blood Flow & Metabol., 1, 73 (1989)), an improved renal function by the endothelin antibody in an acute renal failure model (J. Clin, invest., 83, 1762-1767 (1989), and inhibition of gastric ulcer development with an endothelin antibody in a gastric ulcer model (Extract of Japanese Society of Experimental Gastric Ulcer, 50 (1991)) have been reported. Therefore, endothelin is assumed to be one of the mediators causing acute renal failure or cerebral vasospasm following subarachnoid hemorrhage.
Further, endothelin is secreted not only by endothelial cells but also by tracheal epithelial cells or by kidney cells (FEBS Letters, 255, 129-132 (1989), and FEBS Letters, 249, 42-46 (1989)).
Endothelin was also found to control the release of physiologically active endogenous substances such as renin, atrial natriuretic peptide, endothelium-derived relaxing factor (EDRF), thromboxane A 2 , prostacyclin, noradrenaline, angiotensin II and substance P (Biochem. Biophys, Res. Commun., 157,1164-1168 (1988); Biochem. Biophys, Res. Commun., 155, 20 167-172 (1989); Proc. Natl. Acad. Sci. USA, 85 1 9797-9800 (1989); J. Cardiovasc. Pharmacol., 13, S89-S92 (1989); Japan. J. Hypertension, 12, 76 (1989) and Neuroscience Letters, 102, 179-184 (1989)). Further, endothelin causes contraction of the smooth muscle of gastrointestinal tract and the uterine smooth muscle (FEBS Letters, 247, 337-340 (1989); Eur. J. Pharmacol., 154, 227-228 (1988); and Biochem. Biophys Res. Commun., 159,317-323 (1989)). Further, endothelin was found to promote proliferation of rat vascular smooth muscle cells, suggesting a possible relevance to the arterial hypertrophy (Atherosclerosis, 78, 225-228 (1989)). Furthermore, since the endothelin receptors are present in a high density not only in the peripheral tissues but also in the central nervous system, and the cerebral administration of endothelin induces a behavioral change in animals, endothelin is likely to play an important role for controlling nervous functions (Neuroscience Letters, 97, 276-279 (1989)). Particularly, endothelin is suggested to be one of mediators for pain (Life Sciences, 49, PL61-PL65 (1991)).
Internal hyperplastic response was induced by rat carotid artery balloon endothelial denudation. Endothelin causes a significant worsening of the internal hyperplasia (J. Cardiovasc. Pharmacol., 22, 355-359 & 371-373(1993)). These data support a role of endothelin in the phathogenesis of vascular restenosis. Recently, it has been reported that both ET A and ET B receptors exist in the human prostate and endothelin produces a potent contraction of it. These results suggest the possibility that endothelin is involved in the pathophysiology of benign prostatic hyperplasia (J. Urology, 151, 763-766(1994), Molecular Pharmocol., 45, 306-311(1994)).
On the other hand, endotoxin is one of potential candidates to promote the release of endothelin. Remarkable elevation of the endothelin levels in the blood or in the culture supernatant of endothelial cells was observed when endotoxin was exogenously administered to animals or added to the culture endothelial cells, respectively. These findings suggest that endothelin is an important mediator for endotoxin-induced diseases (Biochem. Biophys. Commun., 161, 1220-1227 (1989); and Acta Physiol. Scand., 137, 317-318 (1989)).
Further, it was reported that cyclosporin remarkably increased endothelin secretion in the renal cell culture (LLC-PKL cells) (Eur. J. Pharmacol., 180, 191-192 (1990)). Further, dosing of cyclosporin to rats reduced the glomerular filtration rate and increased the blood pressure in association with a remarkable increase in the circulating endothelin level. This cyclosporin-inducea renal failure can be suppressed by the administration of endothelin antibody (Kidney Int., 37, 1487-1491 (1990)). Thus, it is assumed that endothelin is significantly involved in the pathogenesis of the cyclosporin-induced diseases.
Such various effects of endothelin are caused by the binding of endothelin to endothelin receptors widely distributed in many tissues (Am. J. Physiol., 256, R856-R866 (1989)).
It is known that vasoconstriction by the endothelins is caused via at least two subtypes of endothelin receptors (J. Cardiovasc. Pharmacol., 17(Suppl.7), S119-SI21 (1991)). One of the endothelin receptors is ET A receptor Selective to ET-1 rather than ET-3, and the other is ET B receptor equally active to ET-1 and ET-3. These receptor proteins are reported to be different from each other (Nature, 348, 730-735 (1990)).
These two subtypes of endothelin receptors are differently distributed in tissues. It is known that the ET A receptor is present mainly in cardiovascular tissues, whereas the ET B receptor is widely distributed in various tissues such as brain, kidney, lung, heart and vascular tissues.
Substances which specifically inhibit the binding of endothelin to the endothelin receptors are believed to antagonize various pharmacological activities of endothelin and to be useful as a drug in a wide field. Since the action of the endothelins is caused via not only the ET A receptor but also the ET B receptor, novel non-peptidic substances with ET receptor antagonistic activity to either receptor subtype are desired to block activities of the endothelins effectively in various diseases.
Endothelin is an endogenous substance which directly or indirectly (by controlling liberation of various endogenous substances) induces sustained contraction or relaxation of vascular or non-vascular smooth muscles, and its excess production or excess secretion is believed to be one of pathogeneses for hypertension, pulmonary hypertension, Raynaud's disease, bronchial asthma, gastric ulcer, diabetes, arteriosclerosis, restenosis, acute renal failure, myocardial infarction, angina pectoris, cerebral vasospasm and cerebral infarction. Further, it is suggested that endothelin serves as an important mediator involved in diseases such as restenosis, prostatauxe, endotoxin shock, endotoxin-induced multiple organ failure or disseminated intravascular coagulation, and cyclosporin-induced renal failure or hypertension.
Two endothelin receptors ET A and ET B are known so far and antagonists of these receptors have been shown to be potential drug targets. EP 0526708 A1 and WO 93/08799 A1 are representative examples of patent applications disclosing non-peptidic compounds with alleged activity as endothelin receptor antagonists.
The present invention discloses a method for preparing a compound of Formula I, ##STR2## comprising reacting a solution of a compound of Formula II, ##STR3## with a chlorodi(C 1 -C 4 )-alkylphosphate and a base to cyclize to the compound of Formula I.
SUMMARY OF THE INVENTION
The present invention discloses a method for preparing the compound of Formula I, ##STR4## wherein: ##STR5## represents: a) 5- or 6-membered heterocyclyl containing one, two or three double bonds, but at least one double bond and 1, 2 or 3 heteroatoms selected from O, N and S, the heterocyclyl is unsubstituted or substituted with one, two or three substituents selected from the group consisting of: OH, CO 2 R 4 , Br, Cl, F, I, CF 3 , N(R 5 ) 2 , C 1 -C 8 alkoxy, C 1 -C 8 alkyl, C 2 -C 8 alkenyl, C 2 -C 8 alkynyl, C 3 -C 8 cycloalkyl, CO(CH 2 ) n CH 3 , and CO(CH 2 ) n CH 2 N(R 5 ) 2 ,
b) 5- or 6-membered carbocyclyl containing one or two double bonds, but at least one double bond, the carbocyclyl is unsubstituted or substituted with one, two or three substituents selected from the group consisting of: OH, CO 2 R 4 , Br, Cl, F, I, CF 3 , N(R 5 ) 2 , C 1 -C 8 alkoxy, C 1 -C 8 alkyl, C 2 -C 8 alkenyl, C 2 -C 8 alkynyl, C 3 -C 8 cycloalkyl, CO(CH 2 ) n CH 3 , and CO(CH 2 ) n CH 2 N(R 5 ) 2 ,
c) aryl, wherein aryl is as defined below,
C 1 -C 8 alkoxy, C 1 -C 8 alkyl, C 2 -C 8 alkenyl, C 2 -C 8 alkynyl, or C 3 -C 8 cycloalkyl, are unsubstituted or substituted with one, two or three substituents selected from the group consisting of: OH, CO 2 R 4 , Br, Cl, F, I, CF 3 , N(R 5 ) 2 , C 1 -C 8 alkoxy, C 3 -C 8 cycloalkyl, CO(CH 2 ) n CH 3 , and CO(CH 2 ) n CH 2 N(R 5 ) 2 ,
aryl is defined as phenyl or naphthyl , which is unsubstituted or substituted with one, two or three substituents selected from the group consisting of: OH, CO 2 R 4 , Br, Cl, F, I, CF 3 , N(R 5 ) 2 , C 1 -C 8 alkoxy, C 1 -C 8 alkyl, C 2 -C 8 alkenyl, C 2 -C 8 alkynyl, C 3 -C 8 cycloalkyl, CO(CH 2 ) n CH 3 , CO(CH 2 ) n CH 2 N(R 5 ) 2 , or when aryl is substituted on adjacent carbons they can form a 5- or 6-membered fused ring having one, two or three heteroatoms selected from O, N, and S, this ring is unsubstituted or substituted on carbon or nitrogen with one, two or three substituents selected from the group consisting of: H, OH, CO 2 R 6 , Br, Cl, F, I, CF 3 , N(R 7 ) 2 , C 1 -C 8 alkoxy, C 1 -C 8 alkyl, C 2 -C 8 alkenyl, C 2 -C 8 alkynyl, or C 3 -C 8 cycloalkyl, CO(CH 2 ) n CH 3 , and CO(CH 2 ) n CH 2 N(R 5 ) 2 ;
R 1 is:
a) C 1 -C 8 alkyl, C 2 -C 8 alkenyl, C 2 -C 8 alkynyl, C 3 -C 8 cycloalkyl,
b) aryl, or
c) heteroaryl;
heteroaryl is defined as a 5- or 6-membered aromatic ring containing one, two or three heteroatoms selected from O, N and S, which is unsubstituted or substituted with one, two or three substituents selected from the group consisting of: OH, CO 2 R 4 , Br, Cl, F, I, CF 3 , N(R 5 ) 2 , C 1 -C 8 alkoxy, C 1 -C 8 alkyl, C 2 -C 8 alkenyl, C 2 -C 8 alkynyl, C 3 -C 8 cycloalkyl, CO(CH 2 ) n CH 3 , and CO(CH 2 ) n CH 2 N(R 5 ) 2 ,
R 2 is: OR 4 or N(R 5 ) 2 ;
R is:
a) H,
b) C 1 -C 8 alkyl,
c) C 2 -C 8 alkenyl,
d) C 2 -C 8 alkynyl,
e) C 1 -C 8 alkoxyl,
f) C 3 -C 7 cycloalkyl,
g) S(O) t R 5 ,
h) Br, Cl, F, I,
i) aryl,
j) heteroaryl,
k) N(R 5 ) 2 ,
l) NH 2 ,
m) --CHO,
n) --CO--C 1 -C 8 alkyl,
o) --CO--aryl,
p) --CO--heteroaryl, or
q) --CO 2 R 4 ;
n is: 0 to 5;
t is: 0, 1 or 2;
R 4 is: C 1 -C 8 alkyl;
R 5 is: C 1 -C 8 alkyl, or aryl;
R 6 , is: H, C 1 -C 8 alkyl, or aryl; and
R 7 is: H, C 1 -C 8 alkyl, aryl, alkyl and aryl are unsubstituted or substituted with one, two or three substituents selected from the group consisting of: OH, CO 2 R 4 , Br, Cl, F, I, CF 3 , N(R 5 ) 2 , C 1 -C 8 alkoxy, C 1 -C 8 alkyl, C 2 -C 8 alkenyl, C 2 -C 8 alkynyl, C 3 -C 8 cycloalkyl, CO(CH 2 ) n CH 3 , CO(CH 2 ) n CH 2 N(R 5 ) 2 ; or when two R 7 substutients are on the same nitrogen they can join to form a ring of 3 to 6 atom;
comprising the following steps:
1) adding chlorodi(C 1 -C 4 )-alkylphosphate to a mixture of a compound of formula II and a first solvent at a temperature of about -30° C. to about 0° C., ##STR6## and 2) adding a base in a second solvent to the phosphate containing solution while maintaining the temperature of the reaction mixture between about -78° C. to about 25° C. to produce the compound of Formula I.
DETAILED DESCRIPTION OF THE INVENTION
The present invention discloses a method for preparing the compound of Formula I, ##STR7## wherein: ##STR8## represents: a) 5- or 6-membered heterocyclyl containing one, two or three double bonds, but at least one double bond and 1, 2 or 3 heteroatoms selected from O, N and S, the heterocyclyl is unsubstituted or substituted with one, two or three substituents selected from the group consisting of: OH, CO 2 R 4 , Br, Cl, F, I, CF 3 , N(R 5 ) 2 , C 1 -C 8 alkoxy, C 1 -C 8 alkyl, C 2 -C 8 alkenyl, C 2 -C 8 alkynyl, C 3 -C 8 cycloalkyl, CO(CH 2 ) n CH 3 , and CO(CH 2 ) n CH 2 N(R 5 ) 2 ,
b) 5- or 6-membered carbocyclyl containing one or two double bonds, but at least one double bond, the carbocyclyl is unsubstituted or substituted with one, two or three substituents selected from the group consisting of: OH, CO 2 R 4 , Br, Cl, F, I, CF 3 , N(R 5 ) 2 , C 1 -C 8 alkoxy, C 1 -C 8 alkyl, C 2 -C 8 alkenyl, C 2 -C 8 alkynyl, C 3 -C 8 cycloalkyl, CO(CH 2 ) n CH 3 , and CO(CH 2 ) n CH 2 N(R 5 ) 2 ,
c) aryl, wherein aryl is as defined below,
C 1 -C 8 alkoxy, C 1 -C 8 alkyl, C 2 -C 8 alkenyl, C 2 -C 8 alkynyl, or C 3 -C 8 cycloalkyl, are unsubstituted or substituted with one, two or three substituents selected from the group consisting of: OH, CO 2 R 4 , Br, Cl, F, I, CF 3 , N(R 5 ) 2 , C 1 -C 8 alkoxy, C 3 -C 8 cycloalkyl, CO(CH 2 ) n CH 3 , and CO(CH 2 ) n CH 2 N(R 5 ) 2 ,
aryl is defined as phenyl or naphthyl, which is unsubstituted or substituted with one, two or three substituents selected from the group consisting of: OH, CO 2 R 4 , Br, Cl, F, I, CF 3 , N(R 5 ) 2 , C 1 -C 8 alkoxy, C 1 -C 8 alkyl, C 2 -C 8 alkenyl, C 2 -C 8 alkynyl, C 3 -C 8 cycloakyl, CO(CH 2 ) n CH 3 , CO(CH 2 ) n CH 2 N(R 5 ) 2 , or when aryl is substituted on adjacent carbons they can form a 5- or 6-membered fused ring having one, two or three heteroatoms slected from O, N, and S, this ring is unsubstituted or substituted on carbon or nitrogen with one, two or three substituents selected from the group consisting of: H, OH, CO 2 R 6 , Br, Cl, F, I, CF 3 , N(R 7 ) 2 , C 1 -C 8 alkoxy, C 1 -C 8 alkyl, C 2 -C 8 alkenyl, C 2 -C 8 alkynyl, C 3 -C 8 cycloalkyl, CO(CH 2 ) n CH 3 , and CO(CH 2 ) n CH 2 N(R 5 ) 2 ;
R 1 is:
a) C 1 -C 8 alkyl, C 2 -C 8 alkenyl, C 2 -C 8 alkynyl, C 3 -C 8 cycloalkyl,
b) aryl, or
c) heteroaryl;
heteroaryl is defined as a 5- or 6-membered aromatic ring containing one, two or three heteroatoms selected from O, N and S, which is unsubstituted or substituted with one, two or three substituents selected from the group consisting of: OH, CO 2 R 4 , Br, Cl, F, I, CF 3 , N(R 5 ) 2 , C 1 -C 8 alkoxy, C 1 -C 8 alkyl, C 2 -C 8 alkenyl, C 2 -C 8 alkynyl, C 3 -C 8 cycloalkyl, CO(CH 2 ) n CH 3 , and CO(CH 2 ) n CH 2 N(R 5 ) 2 ,
R 2 is: OR 4 or N(R 5 ) 2 ;
R 3 is:
a) H,
b) C 1 -C 8 alkyl,
c) C 2 -C 8 alkenyl,
d) C 2 -C 8 alkynyl,
e) C 1 -C 8 alkoxyl,
f) C 3 -C 7 cycloalkyl,
g) S(O) t R 5 ,
h) Br, Cl, F, I,
i) aryl,
j) heteroaryl,
k) N(R 5 ) 2 ,
l) NH 2 ,
m) --CHO,
n) --CO--C 1 -C 8 alkyl,
o) --CO--aryl,
p) --CO--heteroaryl,
q) --CO 2 R 4 ,
n is: 0 to 5;
t is: 0, 1 or 2;
R 4 is: C 1 -C 8 alkyl;
R 5 is: C 1 -C 8 alkyl, or aryl;
R 6 , is: H, C 1 -C 8 alkyl, or aryl; and
R 7 is: H, C 1 -C 8 alkyl, aryl, alkyl and aryl are unsubstituted or substituted with one, two or three substituents selected from the group consisting of: OH, CO 2 R 4 , Br, Cl, F, I, CF 3 , N(R 5 ) 2 , C 1 -C 8 alkoxy, C 1 -C 8 alkyl, C 2 -C 8 alkenyl, C 2 -C 8 alkynyl, C 3 -C 8 cycloalkyl, CO(CH 2 ) n CH 3 , CO(CH 2 ) n CH 2 N(R 5 ) 2 ; or when two R 7 substutients are on the same nitrogen they can join to form a ring of 3 to 6 atom;
comprising the following steps:
1) adding chlorodi(C 1 -C 4 )-alkylphosphate to a mixture of a compound of formula II and a first solvent at a temperature of about -30° C. to about 0° C., ##STR9## and 2) adding a base in a second solvent to the phosphate containing solution while maintaining the temperature of the reaction mixture between about -78° C. to about 25° C. to produce the compound of Formula I.
The process as recited above, wherein the first solvent is selected from the group consisting of tetrahydrofuran, diethyl ether, MTBE (methyl t-butyl ether), toluene, benzene, hexane, pentane, and dioxane, or a mixture of said solvents. The process as recited above, wherein the preferred the first non-acidic, aprotic solvent is toluene.
The process as recited above wherein the chlorodi(C 1 -C 4 )-alkylphosphate is utilized in about 1.0 to about 2.0 equivalents, preferably about 1.5 equivalents.
The process as recited above, wherein the second solvent is selected from the group consisting of tetrahydrofuran, diethyl ether, MTBE (methyl t-butyl ether), toluene, benzene, hexane, pentane, and dioxane, or a mixture of said solvents. The process as recited above, wherein the preferred the second solvent is tetrahydrofuran.
The process as recited above, wherein the base is selected from sodium hydride, lithium diisopropylamide, lithium diethylamide, lithium dimethylamide and lithium hexamethyldisilazide.
The process as recited above wherein base is utilized in a ratio of about 2.0 to about 4.0 equivalents of base per equivalent of the the chlorodi(C 1 -C 4 )-alkylphosphate, preferably about 3.0 equivalents of base per equivalent of the chlorodi(C 1 -C 4 )-alkylphosphate.
The process as recited above, wherein the temperature range is about -78° C. to about 25° C. in Steps 2 and 3, and preferably about -15° C. to about 10° C.
The process as recited above, which includes the following additional steps:
3) aging the reaction mixture for about 2 to about 12 hours at a temperature of about -78° C. to about 25° C. to produce the compound of Formula I;
4) quenching the reaction mixture by addition of water and an acid, while maintaining the temperature of the reaction mixture at less than 30° C. producing a biphasic solution composed of an aqueous layer and an organic layer containing the compound of Formula I;
5) separating the biphasic solution to isolate the organic layer containing the compound of Formula I in organic solvent(s) from the aqueous layer; and
6) evaporating the organic solvent from the orgainc layer to isolate the compound of Formula I.
It is further understood that the substituents recited above would include the definitions recited below.
The alkyl substituents recited above denote straight and branched chain hydrocarbons of the length specified such as methyl, ethyl, isopropyl, isobutyl, tert-butyl, neopentyl, isopentyl, etc.
The alkenyl-substituents denote alkyl groups as described above which are modified so that each contains a carbon to carbon double bond such as vinyl, allyl and 2-butenyl.
Cycloalkyl denotes rings composed of 3 to 8 methylene groups, each of which may be substituted or unsubstituted with other hydrocarbon substituents, and includes for example cyclopropyl, cyclobutyl, cyclopentyl, cyclohexyl and 4-methylcyclohexyl.
The alkoxy substituent represents an alkyl group as described above attached through an oxygen bridge.
The aryl substituent represents phenyl and 1-naphthyl or 2-naphthyl, including aryl substituted with a 5- or 6-membered fused ring, such as an unsubstituted and substituted methylenedioxy, oxazolyl, imidazolyl, or thiazolyl ring.
The heteroaryl substituent represents a carbazolyl, furanyl, thienyl, pyrrolyl, isothiazolyl, imidazolyl, isoxazolyl, thiazolyl, oxazolyl, pyrazolyl, pyrazinyl, pyridyl, pyrimidyl, or purinyl.
The heterocyclyl substituent represents, oxazolidinyl, thiazolidinyl, imidazolidinyl, thiazolidinyl, oxadiazolyl, thiadiazolyl, morpholinyl, piperidinyl, piperazinyl, or pyrrolidinyl.
Each of the above substituents (alkyl, alkenyl, alkynyl, alkoxy, aryl, heteroaryl, or heterocyclyl) can be either unsubstituted or substituted as defined within the description.
The α,β,-unsaturated ester or amide ##STR10## can generally be prepared in two steps: 1) a coupling reaction at the one position of Ring A ##STR11## wherein R 3 is CHO, Z is a leaving group, such as Br, Cl, I, OTriflyl, OTosyl or OMesyl and R 2 is OR 4 or N(R 5 ) 2 ; and
2) the conversion of the aldehyde (R 3 ═CHO) to the desired chiral auxiliary (R 3 ), wherein R 3 represents ##STR12## X and Y are independently: O, S, or NR 5 ; R 4 is C 1 -C 8 alkyl; R 5 is: C 1 -C 8 alkyl, or aryl; RC, Rd, Re and Rf are independently: H, C 1 -C 8 alkyl, and aryl, such that either R c and R d are not the same and/or R e and R f are not the same, or R c and R e or R d and R f can join to form a 5- or 6-membered ring, which is unsubstituted or substituted with one, two or three substituents selected from the group consisting of: OH, CO 2 R 4 , Br, Cl, F, I, CF 3 , N(R 5 ) 2 , C 1 -C 8 alkoxy, C 1 -C 8 alkyl, C 2 -C 8 alkenyl, C 2 -C 8 alkynyl, or C 3 -C 8 cycloalkyl, CO(CH 2 ) n CH 3 , CO(CH 2 ) n CH 2 N(R 5 ) 2 ; and n is o to 5.
Commercially available pyridone 1 is alkylated via its dianion with propyl bromide, and the product is then converted into the bromopyridine 3a using a brominating agent such as PBr 3 . The nitrile 3a is then reduced to the aldehyde 3 using diisobutyl aluminum hydride (DIBAL). The aldehyde then undergoes a Heck reaction with t-butyl acrylate using NaOAc, (allyl) 2 PdCl 2 , tri-o-tolylphosphine, toluene, reflux to provide the unsaturated ester 4a in high yield. The unsaturated ester 4a is then heated with pseudoephedrine, or alternatively, N-methyl-cis-aminoindanol (not shown in the schemes), and acetic acid in toluene to give the protected aldehyde 5. ##STR13##
Commericially available acid 10 is reduced with in situ borane (NaBH 4 /BF 3 •Et 2 O) to the alcohol 11, which is then converted into the chloride 13, by treatment with SOCl 2 in dimethylformamide (DMF). ##STR14##
Commercial available 1,2-aminoindanol 7 is acylated (propionyl choride, K 2 CO 3 ) to give amide 8, which is then converted into the acetonide 9 (2-methoxypropene, pyridinium p-toluene-sulfonate (PPTS)). Acetonide 9 is then alkylated with the benzylchloride 13, (LiHMDS) to give 14, which is then hydrolyzed (6N HCl, dioxane) to give the carboxylic acid 15. Reduction (NaBH 4 /BF 3 •Et 2 O) of the acid provided the alcohol 16 in high yield and optical purity. Protection of the alcohol 16 (TBSCl, imidazole) provided bromide 17, the precursor to organolithium 17a. ##STR15##
Compound 17a is added to the α,β-unsaturated ester bearing a pseudoephedrine 5 (or the N-methyl-cis-aminoindanol chiral auxiliary, not shown) at -78° to -50° C. Work up with acid, THF and water (to remove the auxiliary) affords compound 6 in high yield and good selectivity. Please note other chiral axillary groups can be utilized in this asymmetric addition. See WO 98/06698, published by the World Intellectual Property Organization on Feb. 19, 1998. ##STR16##
Addition of the Grignard reagent (prepared from the aryl bromide and magnesium) to compound 6 at -78° C. to about -60° C. in THF affords compound 7 in quantitative yield and good stereoselectivity. ##STR17##
Cyclization of compound 7 by treatment with diethylchlorophosphate and lithium bis(trimethylsilyl)amide (LHMDS) at about -15° C. to about 10° C. give compound 8. Deprotection by treatment with HCl in acetonitrile followed by work up and purification by crystallization of its benzylamine salt affords the penultimate key intermediate 9. ##STR18##
Salt breaking followed by oxidation of the primary lacohol 9 according to the present invention gives the dicarboxylic acid 10 in high yield. ##STR19##
The instant invention can be understood further by the following examples, which do not constitute a limitation of the invention.
EXAMPLE 1
Preparation of 2-bromo-5-methoxybenzyl alcohol ##STR20##
Sodium borohydride (8.6 g) is slurried in THF (150 mL KF=150 μg/mL) in a round bottom flask equipped with a thermocouple, an addition funnel, a nitrogen inlet a mechanical stirrer and a cooling bath. 2-Bromo-5-methoxybenzoic acid (50 g) is dissolved in THF (100 mL KF=150 μg/mL) is added to the sodium borohydride slurry over 45 min while maintaining the temperature at 20-25° C. The reaction must be controlled with intermittent cooling and by careful monitoring of the addition rate. The mixture is aged for 30 min at 20-25° C. Boron trifluoride etherate (36.9 g) is added over a period of 30 min at 30-35° C.
The addition of boron trifluoride etherate produces a delayed exotherm and should be added slowly in order to control the reaction temperature. The resulting white slurry is aged for 1 h at 30-35° C. and then sampled for HPLC assay. A peak at RT=8.7 min is an impurity related to the starting material. The acid is at RT=9.1 min.
The reaction mixture is cooled to 15° C. and carefully quenched into a cold (10° C.) saturated ammonium chloride solution (150 mL) while maintaining the temperature <25° C.
Ethyl acetate (500 mL) is added and the layers are separated. The organic layer is washed with water (100 mL) and then transfered to a 1 L round bottom flask equipped for distillation. The solution was concentrated and charged with fresh ethyl acetate. This is repeated until a solution with a volume of 200 mL has KF<200 μg/mL. The solvent is then switched to DMF to give the final volume of 200 mL with a KF<200 μg/mL.
EXAMPLE 2
Preparation of 2-bromo-5-methoxybenzyl chloride ##STR21##
The DMF solution of the benzyl alcohol (91.3 g in 400 mL KF=300 μg/mL) is charged to a 2 L flask equipped with a mechanical stirrer, thermocouple, N 2 inlet, and cooling bath. The solution is cooled to 0-5° C. and the addition funnel is charged with thionyl chloride (55.0 g). The thionyl chloride is added over a period of 45 min while maintaining the temperture 5-10° C. The mixture is aged for 1 h at 5C. and assayed by HPLC.
The addition funnel is charged with water (400 mL) which is added dropwise to the reaction mixture over a period of 30 min. while maintaining the temperture <15° C. The temperature is controlled by cooling and monitoring the rate of addition. The initial addition of water is highly exothermic. Using large excess of thionyl chloride results in a more exothermic quench. If the quench temperture is not controlled, hydrolysis of the benzyl chloride back to the alcohol may result.
The resulting thick white slurry is aged for 1 h at 0-5° C. The benzyl chloride is isolated by filtration. The cake is washed with (1:1) DMF:H 2 O (100 mL) and then water (200 mL). The solid is dried in vacuo to give 93 g of the benzyl chloride(94% yield, 96 A %). HPLC assay: Column: Waters Symmetry C8, 4.6×250 mm; UV Detection: 220 nm; Column Temp: 25° C.; Flow rate: 1 mL/min.; Eluent: CH 3 CN:H 2 O:0.1% H 3 PO 4 (70:30); RT (benzyl alcohol)=3.9 min; RT (benzyl chloride)=7.3 min.; and RT (DMF)=2.6 min.
EXAMPLE 3
Preparation of the Acetonide of N-propanoyl (1R,2S)-cis-aminoindanol ##STR22##
A 5 L 3-neck round bottom flask equipped with a mechanical stirrer, N 2 inlet, thermocouple probe, heating mantle, and addition funnel is charged with (1R,2S)-cis-aminoindanol (100 g), tetrahydrofuran (1.2 L, KF 120 μg/mL), and triethylamine (96 mL, KF 500 μg/mL). The resulting slurry is heated under a N 2 atmosphere to 40-45° C. giving a yellow solution. Propionyl chloride (59 mL) is charged to an addition funnel and added to the solution while maintaining the temperature at 45-50° C.
The temperature is controlled by rate of propionyl chloride addition and a cooling bath. HPLC assay shows >99% amide formed. Methanesulfonic acid (3 mL) is added to the reaction slurry. 2-Methoxypropene (140 mL) is charged to an addition funnel and added over 30 minutes at a temperature of 50° C.
The addition of 2-methoxypropene is mildly exothermic. The temperature is maintained by the rate of addition and a heating mantle. The reaction remains a slurry but does become less thick.
The reaction slurry is aged for 1-2 hours at 50° C. HPLC assay at this point shows <0.5A % of the amide remaining. The amide is not removed in the isolation so it is important to push the reaction to completion. The reaction slurry is cooled to 0-5° C. and quenched by addition of 5% aqueous sodium carbonate solution (1 L) and heptane (1 L). The layers are stirred and separated and the organic is washed with water (300 mL).
HPLC assay at this point shows the acetonide in >98A % and >90% yield. The acetonide/THF/heptane solution is filtered into a 2 L round bottom flask and the solution is distilled to a final volume of 700 mL. Heptane (1 L) is added and the solution is distilled to a final volume of 700 mL. The distillation is done under partial vacuum at ˜50° C. NMR assay at this point shows <2 mol % THF. The solution is allowed to cool and is seeded with acetonide at 35-40° C. The thick slurry is aged for 1 hour at ambient temperature then cooled to 0-5° C. and aged for 1 hour. The slurry is filtered and the cake is washed with cold heptane (200 mL) and air dried to yield acetonide as a crystalline white solid (141.1 g, 85% yield, 99.6 A %).
EXAMPLE 4
Alkylation of the Acetonide with 2-bromo-5-methoxybenzyl chloride. ##STR23##
A THF solution (2 L, KF<200 μg/mL) of the acetonide (252 g) and the benzyl chloride (255 g) is cooled to -10° C. Lithium bis(trimethylsilyl)amide (1.45 L) is added dropwise over 5 h at 0-2° C. The mixture is then aged for 1.5 h and assayed by HPLC.
The reaction is quenched by adding aqueous saturated ammonium chloride solution (1 L). The initial addition of the ammonium chloride should be slow in order to control the foaming. The rate can be increased when the foaming subsides.
The quenched reaction is then transfered into a mixture of aqueous ammonium chloride (1.5 L), water (0.5 L), and ethyl acetate (3 L). The mixture is then agitated for 15 min and the layers are separated. The organic layer is washed with water (1 L) and brine (0.5 L). The ethyl acetate solution is concentrated to a low volume and solvent switched to 1,4-dioxane. The dioxane solution is adjusted to a final volume of 1.8 L.
The dioxane solution of the coupled product is charged to a 12 L round bottom flask and 6 M HCl (1.5 L) is charged. The mixture is heated to reflux and monitored by HPLC.
The mixture is cooled to 20° C. and MTBE (3 L) is added. The mixture is agitated for 15 min and the layers are separated. The organic layer is washed with water (1 L). The MTBE solution of the crude acid is extracted with 0.6 M sodium hydroxide (2 L). The aqueous solution of the sodium salt of the acid is combined with MTBE (2.5 L) and cooled to 10° C.
The two phase mixture is acidified with 5.4 M sulfuric acid (250 mL), agitated for 15 min, settled and the layers separated. The MTBE solution of the acid is washed with water (0.5 L). The MTBE solution of the acid is dried by distilation and then solvent switched to THF. The final volume of the THF is 2 L with a KF<250 μg/mL. HPLC assay: column: Waters Symmetry; Eluent: acetontrile: water: phosphoric acid (70:30:0.1); Flow rate: 1 mL/min.; RT (acetonide)=4.5 min.; RT (benzyl chloride)=7.5 min.; RT (coupled product)=11.5 min.; RT (aminondanol)=1.7 min.; RT (hydroxyamide)=1.7 min.; and RT (acid)=4.5 min.
EXAMPLE 5
Preparation of 3-(2-bromo-5-methoxyphenyl)-2-methylpropanol ##STR24##
Sodium borohydride (33 g) is slurried in THF (0.5 L KF=200 mg/mL) in a round bottom flask. The THF solution (2 L) of the acid is added to the sodium borohydride slurry over 1 h while maintaining the temperature at 20-25° C.
The reaction is controlled with a cooling bath and by carefully monitoring the addition rate. A nitrogen sweep and proper venting of the hydrogen is also important.
The mixture is aged for 30 min at 20-25° C. Boron trifluoride etherate (152 g) is added over 1 h at 30-35° C. The addition produces a delayed exotherm and should be carefully monitored in order to control the reaction temperature. The resulting milky white slurry is aged for 1 h at 30° C. and sampled for HPLC assay.
The reaction mixture is cooled to 15° C. and carefully quenched in a cold (10° C.) ammonium chloride solution (1.5 L) while maintaing the temperature at 25° C. The rate of hydrogen evolution is controlled by the rate of the addition of the mixture into the ammonium chloride. The quenched mixture is distilled in vacuo to remove the THF. The aqueous layer is extracted with MTBE (1.5 L) and the organic layer is dried by flushing with additional MTBE. The MTBE solution is then solvent switched to hexanes and adjusted to a volume of 350 mL and seeded. The slurry is aged for 2 h at 20° C. and then cooled to 0-5° C. aged for 1 h and filtered. The cake is washed with cold hexanes (200 mL). The solid is dried under a nitrogen sweep. The isolated solid (164 g) is >99A % by HPLC and >99% ee.
HPLC: Column: Waters Symmetry C8; Solvent: acetonitrile:water:phosphoric acid (50:50:0.1); Flow rate: 1 mL /min.; Detection: 220 nm; RT (acid)=10.2 min.; RT (alcohol)=10.7min.
Chiral HPLC: Column: Chiracel OD-H; Hexane:2-propanol (97:3); Flow rate: 1 mL/min.; Detection: 220 nm; RT minor isomer=21 min.; and RT major isomer=23 min.
EXAMPLE 6
Preparation of 3-(2-bromo-5-methoxyphenyl)-2-methylpropyl t-butyldimethylsilyl ether ##STR25##
Imidazole (1.6 g, 0.023 mol) is added to a solution of the alcohol (5.0 g, 0.019 mol) in DMF (15 mL) at 20° C. The addition of imidazole is endothermic and results in a 4-5° C. drop in temperature. TBSCl (3.0 g, 0.020 mol) is dissolved in DMF (5 mL) and is added slowly to the above solution while maintaining the temperature 20-25° C. using a cooling bath. The reaction is monitored by HPLC.
MTBE (50 mL) is added to the reaction mixture along with water (50 mL) and the phases are separated. The organic is washed with water (50 mL) and then concentrated to 10 mL total volume and solvent switched into THF in preparation for the next step. NMR assay of the organic layer after the second water wash indicates no residual DMF.
1 H NMR (CDCl 3 ) ε: 7.41 (d, J=8.74, 1H), 6.77 (d, J=3.04, 1H), 6.63 (dd, J=8.73, 3.06, 1H), 3.78 (s, 3H), 3.50 (d, J=5.75, 2H), 2.89 (dd, J=13.31, 6.15, 1H), 2.45 (dd, J=13.30, 8.26, 1H), 2.03 (m, 1H), 0.94 (s, 9H), 0.92 (d, J=5.01, 3H), 0.07 (s, 6H).
13 C NMR (CDCl 3 ) δ: 159.1, 141.6, 133.2, 117.0, 115.4, 113.2, 67.4, 55.4, 39.7, 36.3, 26.0 (3C), 18.4, 16.5, -5.3 (2C).
HPLC assay: column, Zorbax Rx C8 (4.6×250 mm); solvent: acetonitrile: water: phosphoric acid 90:10:0.1; flow rate: 1 mL /min; WV Detection: 220 nm; Retention times: RT (alcohol)=3.08 min; RT (DMF)=3.17 min; and RT (product)=7.7 min.
EXAMPLE 7
Pseudoephedrine Acetal Formation of t-butyl 3-(6-n-butyl-3-formylpyridyl)-2-prop-2-enoate ##STR26##
To a solution of Heck product 4a (2.907 kg) in toluene (7.049 kg) is added solid (1S,2S )-(+)-pseudoephedrine (1.74 kg) followed by acetic acid (2.87 ml). The reaction mixture is then heated to reflux. The toluene/water azeotrope begins to reflux at a pot temperature of 87° C. Over the course of 40 minutes, the pot temperature increases to 110° C. At this time, approximately 160 ml of water has been collected in the Dean-Stark trap.
A HPLC assay of an aliquot indicates that all starting Heck product has been consumed.
The reaction is then cooled to 40° C. and pumped into a 50 L extractor and diluted with MTBE (10.67 kg). The organic layer is washed with saturated NaHCO 3 (12.10 kg ) and then with water (23.64 kg). The organic layer is concentrated to a volume <10 L and a KF<120 μg/mL. The MTBE is removed prior to flushing with toluene. Typically 8-10 L of toluene is required as flush to obtain the desired KF. The dry toluene solution was stored under nitrogen until needed.
HPLC Assay: Column: Zorbax Rx-C8 4.6×250 mm; Solvent: Acetonitrile:water 95:5; Flow: 1.0 mL /min; UV Detection: 220 nm; RT (toluene)=3.2 min.; RT (Heck Product)=3.9 min.; and RT (N,O, acetal)=5.3 min.
EXAMPLE 8
Conjugate Addition-Hydrolysis ##STR27##
To a solution of arylbromide (4.08 kg) in THF (7.34 kg, KF<150 μg/mL) at -82° C. is added a 2.25 M solution of n-BuLi in hexanes (4.87 L). The addition takes 2 h and the internal temperature is maintained below -72° C.
Assay by HPLC indicates that the lithiation is complete after addition of the n-BuLi. The lithiation reaction is instantaneous at the reaction temperature. The purpose of checking an aliquot is to insure that the proper amount of n-BuLi is charged. To the above solution (re-cooled to approximately -80° C.) is added the pre-cooled (approximately -65° C.) toluene solution (KF<150 μg/mL) of the enoate. The addition is done very rapidly with the aid of a pump (addition time<5min.) and the reaction typically exotherms to -32° C.
In order to insure efficient pumping, the enoate solution was diluted with an additional 3-4 L of toluene.
The reaction is re-cooled to -60° C. and quenched carefully with 2.9 L of acetic acid. (Warning: exothermic reaction.) The reaction exotherms to approximately -20° C. The quenched reaction mixture is then pumped into a 100 L extractor. A citric acid solution (4.82 kg of citric acid in 8 kg of water) is then added and the two-phase mixture is rapidly stirred for 16 h at room temperature. HPLC assay indicates that the N, O acetal hydrolysis is complete.
The phases are cut and the aqueous layer is extracted with MTBE (14.23 kg). The combined organic layers are washed twice with 5% NaHCO 3 (2×23 kg). The organic layer is then washed with water (20.55 kg). The pH of the water wash should be neutral to slightly basic. The oganic layer is dried under reduced pressure to a volume <7 L and a KF<100 μg/mL. The MTBE is removed prior to flushing with toluene. Approximately 30 kg of toluene is needed as flush to obtain the desired KF value. The dry toluene solution is then pumped into a plastic carboy. The 100 L extractor and pump are then flushed with 2.5 kg of THF. HPLC assay indicates a yield of 4.2 kg (72% from the Heck Product, 3 steps). The ee of the product is determined to be 92%.
HPLC Assay: Column: Zorbax Rx-C8 4.6×250mm; Solvent: acetonitrile:water 95:5; flow rate: 1.0 mL /min.; UV Detection: 220 nm; RT (toluene)=3.2 min.; RT (ArH)=5.5 min.; RT (ArBr)=6.5 min.; RT (ArBu )=8.2 min.; RT (Aldehyde Product)=9.5 min.; and RT (N,O acetal Product)=18.2 min.
Chiral HPLC Assay: Column: Whelk-O; Solvent: 97:3 Hexane/IPA; flow rate=1.0 mL/min.; RT(toluene)=3.1 min.; RT(minor)=6.8 min.; and RT(major)=7.5 min.
EXAMPLE 9
Grignard Addition ##STR28## Step A: Preparation of the Grignard Reagent
To a 22 L reaction flask equipped with an efficient condenser is charged Mg (240 g, 9.87 mol) and dry THF (8.2 L, KF<100 μg/mL). The mixture is heated to 50° C. after degassing by two vacuum/N 2 cycles. The aryl bromide (1.89 kg, 9.40 mol) is then added carefully!
Due to the induction period and very exothermic reaction, the ArBr should be added very carefully! No more than 10% of the ArBr should be added before the reaction is initiated as indicated by the exotherm (the batch temperature will be higher than that of the bath) and color change from colorless to pale yellow. Cooling maybe required to control the reaction temperature. Once the reaction is initiated, the heating is stopped and the remaining ArBr is added slowly maintaining a gentle reflux. The reaction mixture is then aged at 50° C. for 2 hours to give a solution of ArMgBr (˜9.4 L, 1.0 M). The reaction is monitored by HPLC. Zorbax SB-C8 4.6×250 mm, 30° C.; 1.50 mL/min; linear gradient: MeCN 40-70% in 15 min, 0.1% H 3 PO 4 ; 220 nm; Retention time (min.): ArBr, 6.2; ArH, 9.2 min.
Step B: Addition of the Grignard Reagent to the Aldehyde
A dry solution of the crude Michael addition product (4.22 kg in ˜4.7 L toluene and 2.5 L THF, KF<200 ug/mL) is charged into a 72 L flask. Dry THF (20 L, KF<100 ug/mL) is added and the mixture is degassed by a vacuum/N 2 cycle. After the batch is cooled to -75° C. with a dry ice-methanol bath, the ArMgBr prepared above is added slowly maintaining the batch below -65° C. The mixture is aged at -70° C. for 1 hour and the completion of the reaction is confirmed by HPLC (<1A % aldehyde ). The reaction mixture is aged for two more hours then pumped into aqueous NH 4 Cl (14 L 20w %) to quench the reaction.
Toluene (14 L) is added and the mixture is warmed to 20° C. The organic layer is separated and washed with brine (14 L) to give a solution of the crude Grignard addition product (50.11 Kg).
Assay by HPLC indicates the presence of 4.67 Kg (91% yield) of the product in solution. It is dried with ˜2 kg of anhydrous Na 2 SO 4 overnight to remove the bulk of the water then filtered and concentrated to 15 L under vacuum.
HPLC conditions: Column: Zorbax SB-C8 4.6×250 mm; temperature: 30° C.; Solvent: CH 3 CN:H 2 O:0.1 H 3 PO 4 80:20:0.1 gradient to 100:0:0.1 over 15 min.; Flowrate: 1.5 mL /min.; RT (aldehyde)=12.15min.; RT (major stereoisomer)=9.93 min.; RT (minor stereoisomer)=10.65 min. The diastereomeric ratio was about 93:7 major to minor stereoisomer.
EXAMPLE 10
Cyclization-Deprotection ##STR29##
The Grignard addition product in toluene (˜15 L, KF=130 μg/ml) is cooled to -15° C. and the diethylchorophosphate (1.65 kg, 9.6 mol, 1.45 eq) is added. Then LiN(TMS) 2 in THF (1.0 M, 28.75 L, 4.35 eq) is added while keeping the temparature <5° C. The slurry is aged at 0-10° C. for 4 hrs. More diethyl chlorophosphate and LiN(TMS) 2 may be added as required to complete the reaction. The reaction is monitored by HPLC. After 3 h the reaction is typically complete. After the reaction is completed (SM<1%), water (17 L) and acetic acid (4.5 kg, exothermic!) is added while keeping the reaction temperature <30° C.
The temperature is contolled by controlling the rate of addition and by using a cooling bath. After the two layers are separated, the organic layer is washed with 14 L brine. The organic layer is concentrated under vacuum to minimum volume of 10-12 L and mixed with 20 L acetonitrile and then cooled to 0C. Concentrated HCl (13.2 kg) is added slowly while keeping the reaction temperature <25° C. The mixture is aged at 20-25° C. overnight.
The product is a mixture of the acid alcohol and the lactone. HPLC (same column and eluents) Time 0 A/B 50/50, 10 min A/B 90/10, 15 min 90/10. Retention time t-butyl ester alcohol 6.4 min, lactone 4.7 min, acid alcohol 2.9 min.
When the t-butyl ester alcohol is consumed (19 hrs), the reaction mixture is cooled to 0° C. and 40% w/w NaOH (˜12.4 kg until pH=3-5) is added while keeping the temperature <25° C. Water (6 L) is also added. When the pH of the aqueous layer reaches 3, the two layers are separated. The top organic layer is then mixed with 3.3 kg 40% NaOH (5 eq) and 12 L water. The mixture is vigorously stirred for 3 hrs until all the lactone is consumed (organic layer sample). The two layers are then separated and to the organic layer is added 20 L MTBE and 20 L water and 200 g 40% NaOH. The two layers are separated again after mixing. The organic layer is mixed with 100 g 40% NaOH, 10 L water and 20 L heptane. The layers are separated and the organic layer discarded.
To the combined aqueous layer is added H 3 PO 4 (85%, 4.6 kg, 6 eq) until pH=3-4 (exothermic, keep the temperature <25° C.) and MTBE (12 L). After the two layers are separated, the aqueous layer is extracted with 20 L toluene. The combined organic layer is dried with 1.5 kg Na 2 SO 4 and then concentrated under vacuum to a volume of ˜10 L. It was flushed with 5 L toluene to reach KF=450 μg/ml. The residue is then mixed with 50 L MTBE. Benzylamine (0.85 kg, 1.2 eq) is added as a solution in 3 L MTBE. Only 1.5 L of this solution is added initially and the batch is seeded with 0.5 g L-321,865 benzylamine salt. The batch is aged for one hour for the salt to precipitate. The rest of the benzylamine solution is added over 30 min. Additional 7 L MTBE is used for rinse. The batch is aged at ambient temperature overnight. The solid is collected by filtration and washed with 3×4 L MTBE until the wash is nearly colorless. The batch is dried with nitrogen flow and suction, wt. 2.96 kg (72% yield). HPLC showed ˜95 wt % pure and 98.5 area %. HPLC: Column: Zorbax SB C-8 column 4.6×250 mm size; Solvent: Eluent: A: MeCN and B: 0.1% H 3 PO 4 ; Gradient: Time 0 A/B 80/20, 10 min 95/5; 20 min A/B 98/2; 25 min 98/2; Flow rate: 1.5 ml/min; UV detection: 220 nm; RT (Grignard product)=10.9 min.; RT (intermediate)=11.7 min.; RT (intermediate)=13.2 min.; RT (product)=12.2 min
EXAMPLE 11
Oxidation of Primary Alcohol
Alternative A--Periodic Acid and Chromium Trioxide ##STR30##
A solution of H 5 IO 6 /CrO 3 is prepared by adding water (1.1 mL) and MeCN to 15.95 g of H 5 IO 6 to a volume of 160 mL. An aqueous solution of CrO 8 (0.16 mL 200 mg/mL) is then added and the mixture is stirred until all the solid dissolved.
A mixture of the benzylamine salt of the hydroxy acid (12.50 g, 20.0 mmol) in MTBE (100 mL) and water (50 mL) is treated with 2.0 N HCl (˜10 mL) until pH=3-4. The organic layer is washed with water (3×50 mL), brine (50 mL) then concentrated to ˜30 mL. It is flushed with acetonitrile (100 mL) then diluted with MeCN (to 100 mL). Water (0.75 mL) is then added and the mixture is cooled to ˜5° C. A portion of the H 5 IO 6 /CrO 3 solution (50 mL, 1.1 molar equiv.) is added in ˜5-10 minutes. The remaining portion (110 mL) is added in 30-60 minutes maintaining the batch temperature at -3 to 0° C.
The mixture is aged for 0.5 hour at 0° C. and the completion of the reaction is confirmed by HPLC (<2A % of the SM). The reaction is quenched with Na 2 HPO 4 solution (8.52 g in 150 mL H 2 0), then brine (50 mL). Some inorganic solid remains and is filtered off.
The pH of the aqueous layer should be 3-4.
Toluene (150 mL) is added and organic layer is separated and washed with 1:1 brine-water mixture (2×100 mL), then aqueous NaHSO 3 (2.15 g uin 50 mL H 2 O. The organic layer is concentrated to 160 mL to remove most of the acetonitrile (40 mmHg, 30° C. bath).
The mixture is treated with 0.30 N NaOH (150 mL) for 0.5 hour and the organic layer is separated and discarded. MTBE is added (100 mL) to the aqueous layer and the mixture is acidified with 2.0 N HCl (˜22.5 mL) to pH=3.5. The organic layer is separated and washed with water (2×50 mL), brine (50 mL) then concentrated to give the crude product as a brown foam.
HPLC conditions: Column: YMC-ODS AM 4.6×250 mm; Solvent: CH 3 CN:H 2 O:0.1 H 3 PO 4 80:20:0.1 gradient to 100:0:0.1 over 15 min.; Flow rate: 1.0 mL/min.; Temperature: 30° C.; UV detection: 220 nm; RT (hydroxy acid)=5.8 min.; and RT (diacid)=7.8 min.
Alternative B--TEMPO Oxidation ##STR31##
A mixture of the benzylamine salt of the hydroxy acid (25.0 g, 40.0 mmol) in MTBE (300 mL) and water (100 mL) is treated with 2.0 N HCl (˜20 mL) until pH=3-4. The organic layer is washed with water (2×100 mL) then extracted with NaOH (140 mL 0.63 N NaOH). To the NaOH extract are added MeCN (200 mL) and NaH 2 PO 4 (13.80 g, 100 mmol) and the mixture is heated to 35° C. The pH of the mixture should be 6.7. TEMPO (436 mg, 2.8 mmol) is added followed by a simultaneous addition (over 2 h) of a solution of sodium chlorite (9.14 g 80%, 80.0 mmol in 40 mL water) and dilute bleach (1.06 mL 5.25% bleach diluted into 20 mL, 2.0 mol %).
The sodium chlorite solution and bleach should not be mixed prior to the addition since the mixture appears to be unstable. The addition should be carried out as follows: approximately 20% of the sodium chlorite solution is added followed by 20% of the dilute bleach. Then the rest of the NaClO 2 solution and dilute bleach are added simultaneously over 2 h.
The mixture is aged at 35° C. until the reaction is complete (<2A % SM, 2-4 h). The batch is cooled to rt, water (300 mL) is added and the pH is adjusted to 8.0 with 2.0 N NaOH (˜48 mL). The reaction is quenched by pouring into cold (0° C.) Na 2 SO 3 solution (12.2 g in 200 mL water) maintained <20° C.
The pH of the aqueous layer should be 8.5-9.0. After aging for 0.5 hour at room temperature, MTBE (200 mL) is added with stirring. The organic layer is discarded and aqueous layer is acidified with 2.0 N HCl (˜100 mL) to pH=3-4 after more MTBE (300 mL) is added. The organic layer is washed with water (2×100 mL), brine (150 mL) to give a solution of the crude dicarboxylic acid in 90-95% yield (19.1-20.2 g). HPLC conditions: Column: YMC-ODS AM 4.6×250 mm; Flow rate: 1.00 mL/min; Solvent: MeCN 50-80% in 15 min, 0.1% H 3 PO 4 ; Temperature: 30° C.; UV detection: 220nm; RT (hydroxy acid)=5.8 min.; RT (dicarboxylic acid)=7.8 min. | This invention relates to a cyclization process useful in the preparation of a key intermediate in the preparation of an endothelin antagonist of the general formula shown below: ##STR1## | 2 |
This is a continuation of prior application Ser. No. 08/170,459 (aban.) filed Dec. 20, 1993, which is a cont. of Ser. No. 07/911,253 (aban.) filed on Jul. 7, 1992 which is a cont. of Ser. No. 07/497,195 (aban.) filed on Mar. 22, 1990.
BACKGROUND OF THE INVENTION
1. Field of the Invention
This invention relates to still video cameras using a solid-state memory device as the image recording medium.
2. Description of the Related Art
Electronic still video cameras using a magnetic floppy disc as the image recording medium are known ID view of recent advances in the high storage and low cost unit production technique of semiconductor memories, a new type of still video camera which makes use of a semiconductor memory device as the image recording medium is regarded as promising.
The image sensor of the still video camera, for example, the CCD type image sensor, even in the present state of art, has some five hundred thousand picture elements In the near future, it is likely to realize an increase of the number of picture elements to one million or more. To store data of the great number of picture elements in the memory without deterioration, as one picture element takes 8 bits, for one frame of five hundred thousand picture elements, four megabits have to be used. To provide an image storage capacity of 25 frames equivalent to that of a magnetic floppy disc, the number must be increase by a factor of twenty-five to one hundred megabits However far the high storage capacity technique of semiconductor memories may advance, there can be demerits in cost, size and consumption of electric power.
In addition, the prior known camera of the above-described new type is made to include a compressing means. This compressing means is of the fixed form. So, it has been impossible either to selectively use a plurality of compressing methods, or to alter the compressing method.
SUMMARY OF THE INVENTION
A first object of the invention is to provide a still video camera capable of recording a large amount of image information in a limited memory capacity.
The still video camera of an embodiment according to the invention is a still video camera using a solid-state memory device as the image recording medium, characterized in that a plurality of data compressing means including non-compression are provided, and that one of the plurality of compressing means is selected according to image data.
According to the above-described embodiment, by the above-described means, for the given image data; a proper one of the compression processes can be selected and the data amount necessary to record can be lessened. Therefore, it becomes possible to efficiently utilize the image recording medium.
Also, the present invention has been made under such situations as described above, and its second object is to provide a still video camera which can arbitrarily alter the compressing method.
In another embodiment of the invention, to achieve the above-described object, the still video camera is constructed in the following way (1) or (2):
(1) A still video camera in which the video signal output from the image sensor is analog-to-digital-converted and further compressed, before it is written in a memory element attachable to and detachable from the camera body, is provided with memory means capable of writing and erasing by an electrical signal supplied from the outside of the camera and usable for writing programs for the above-described compression.
(2) In the aforesaid way (1), a still video camera is provided with a memory element attachable to and detachable from the camera body, the memory element having programs for compression written therein, wherein by this memory element, the electrical signal from the outside of the camera is supplied.
According to the arrangement of the aforesaid way (1), the program for compression can be altered by supplying the electrical signal from the outside of the camera. According to the arrangement of the way (2), the program for compression can be altered by attaching the memory element with the program for compression written therein to the camera body.
Other objects and features of the invention will become apparent from the following written specification and drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a block diagram of the construction of an embodiment of the invention.
FIG. 2 is a block diagram illustrating the construction of the compression circuit.
FIG. 3 is a block diagram illustrating the construction of the expansion circuit.
FIG. 4 is a block diagram of another embodiment of the invention.
FIG. 5 is a flowchart for the operation of the embodiment of FIG. 4.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
The present invention is next described in connection with embodiments thereof by reference to the drawings.
FIG. 1 in schematic diagram shows an embodiment of the invention in which two compression processes can be selected to operate. A camera body 10 has a solid-state memory device 12 detachably attached thereto in which photographed images are recorded (stored). Light from an object to be photographed enters, through a photographic lens 14, an image sensor 16 where it is photoelectrically converted. The output of the image sensor 16 is converted to digital form by an A/D converter 18. A compression selecting circuit 20 determines selection of one of compression processes performed by compression circuits 22 and 24 to be applied to the data output from the A/D converter 18. Depending on the selection result, the compression selecting circuit 20 changes a switch 26 over between two positions, so that the output data of the A/D converter 18 is supplied to the selected one of the compression circuits 22 and 24. The compressed data by the compression circuit 22 or 24 is transferred to the solid-state memory device 12 where it is stored in a predetermined format.
If the camera body 10 has only a recording function, the solid-state memory device 12 is then detached from the camera body 10 and attached to a reproduction apparatus (not shown) where the recorded images are reproduced. In FIG. 1, however, the reproducing function too is illustrated. When the images are reproduced from the solid-state memory device 12, data stored in the solid-state memory device 12 is read out and supplied to one of two expansion circuits 28 and 30 selected by a switch 26. The expansion circuit 28 or 30 performs the expansion process corresponding to the compression process used in the recordings. In more detail, the expansion circuit 28 expands the data compressed by the compression circuit 22, while the expansion circuit 30 expands the data compressed by the compression circuit 24.
The image data restored by the expansion circuit 28 or 30 is converted to analog form by a D/A converter 32, and then to a video signal by a video circuit 34.
It is to be noted that FIG. 1 is depicted with regard to the flow of image signals. Therefore, various kinds of switches for operation commands, a display device and further a control circuit for controlling the entirety, an electric power source circuit, etc., are omitted.
Next, the compression process in the compression circuit 22 or 24 is explained in detail. The natural image has a very strong correlation between any adjacent two of the picture elements. So, taking the differences between the adjacent picture elements gives, in most cases, small values. In other words, compared with the use of the absolute values (of, for example, 8 bits) in storing (recording) the image, the use of their differences in the storage can largely compress the data amount. This compressing method is called the "DPCM". Besides this, there are another compressing methods as improved over the DPCM, one of which is to adaptively vary the non-linearity of the non-linear quantization circuit according to the image, namely, the ADPCM. Yet another method is by transforming the image into a frequency domain, with a larger weight on the coefficient of the low-frequency component and a smaller weight on the coefficient of the high-frequency component, (namely, for example, the discrete cosine transformation).
FIG. 2 in block diagram shows the construction of a compression circuit employing the DPCM, and FIG. 3 in block diagram shows the construction of an expansion circuit for expanding the compressed data. Incidentally, their details are described on pp. 146-159 of "Digital Signal Processing of Image" by Keihiko Suibatsu published by Nikkan Kogyo Shinbun Co. Ltd. The circuit of FIG. 2 comprises a subtractor 40, a non-linear quantization circuit 42, a representative value setting circuit 44, an adder 46, a delay circuit 48 and a coefficient multiplier 50. The subtractor 40 subtracts the output of the coefficient multiplier 50 from the input of 8-bit image data. The non-linear quantization circuit 42 non-linearly quantizes the output of the subtractor 40. Thereby the image data of the input is compressed from the 8 bits to, for example, 3 bits. The 3-bit output of the non-linear quantization circuit 42 is the compressed data which is aimed at.
The representative value setting circuit 44 reverts the 3-bit output of the non-linear quantization circuit 42 to a representative value of 8 bits. The adder 46 adds the output of the coefficient multiplier 50 to the output of the representative value setting circuit 44, i.e., the data (8 bits) of the representative value. The output of the adder 46 is delayed by one picture element by the delay circuit 48, concretely speaking, a data latch circuit, before it is supplied to) the coefficient multiplier 50. The coefficient multiplier 50 multiplies the input by a constant coefficient, for example, 0.95, and supplies the multiplication result to the subtractor 40 and the adder 46 at the time of the inputting of the next data.
By repeating such a procedure, the 8-bit data is compressed to the 3-bit data.
The non-linear quantization circuit 42, the representative value setting circuit 44 and the coefficient multiplier 50 can be realized in the form of table transformation of ROM. So, high speed processing is possible.
Next, the expansion circuit of FIG. 3 comprises a representative value setting circuit 52, an adder 54, a delay circuit 56 for delaying the input by one picture element and a coefficient multiplier 58. The representative value setting circuit 52 is similar to the representative value setting circuit 44 of FIG. 2, transforming the input data (3 bits) to a representative value of 8 bits, The adder 54 adds the output of the coefficient multiplier 58 to the output of the representative value setting circuit 52. The output of the adder 54 becomes the restored data which is aimed at. The delay circuit 56 is a data latch circuit similar to the delay circuit 48, delaying the output of the adder 54 by one picture element before it is supplied to the coefficient multiplier 58. The coefficient multiplier 58 multiplies the input by a constant coefficient, for example, 0.95. Its output is supplied to the adder 54. By such a loop process, the compressed data (3 bits) of the input is expanded to the original data of 8 bits.
The discrete cosine transformation method as its details are described in pp. 179-195 of "Digital Signal Processing of Image" by Keihiko Suibatsu published by Nikkan Kogyo Shinbun Co. Ltd., is briefly explained as follows. At first, by the discrete cosine transformation, the image data is orthogonally transformed and the frequency components are taken out. These frequency components are multiplied by such a coefficient that the low-frequency component is left, while the high-frequency component is removed. By this, the image information can be compressed. When the frequency components of the image are sided to the lower one, good compression with less deterioration can be carried out.
Next, the selection criterion by the compression selecting circuit 20 is explained. For simplicity, the compression circuits 22 and 24 themselves, or similar circuits, perform compression processing by each of the plurality of compressing methods, and whichever gives a less amount of data may be selected. If it is desired to speed up the selecting operation, a portion of the image, for example, the central one, only is subjected to the plurality of compression treatments. Based on the comparison of the data amounts, selection of one of the compression treatments may be made. Also, one of the compression circuits, say 22, employs a compression method which gives always a constant amount of compressed data, while the other compression circuit 24 employs another compression method which varies the amount of compressed data as a function of the image. So, from only the amount of data output from the compression circuit 24, which compression circuit 22 or 24 is to be selected may be determined.
The compression circuits 22 and 24 may employ different compressing methods from each other. But the compressing methods may be the same, or quantitatively different in the compression characteristic. In the case of DPCM, for example, the quantizing characteristic of the non-linear quantization circuit 42 is changed.
Though, in the above-described embodiment, the two compressing processes are selectively used, the invention is not confined to this and so includes a mode of non-compression and another mode of compression. Also, the image data is not only for black and white but also likewise for colors. Further, the selection of the compressing methods may otherwise be made not automatically but manually.
As is easily understandable from the foregoing description, according to the invention, the amount of data of an image to be recorded can be compressed by the method suitable to the respective individual image, thereby giving an advantage of more efficiently utilizing the image recording medium.
The invention is next described in connection with another embodiment thereof.
FIG. 4 in block diagram shows another embodiment of the still video camera according to the invention, and FIG. 5 is a flowchart for the operation of this embodiment In FIG. 4, the camera comprises a lens 61, a CCD 62 (solid-state image sensor) for converting an image formed thereon by the lens 61 to an electrical signal; a signal processing portion 63 for processing the signal output from the CCD 62, an A/D converter 64 for converting the signal output from the signal processing portion 63 to digital form, a data compressing portion 65 for compressing the digitized image signal, a connector 66; a memory cartridge 67 (memory element) detachably attached to the camera body, and a block 68 for controlling the entirety including a timing control circuit and a system control portion (hereinafter called the "system controller").
In the interior of the data compressing portion 65, a program ROM for determining the compressing method is incorporated. As this ROM, use is made of a rewritable EEPROM (Electrically Erasable Programmable Read-Only Memory). The memory cartridge 67 is available in types for photography and for a compression program. When the latter type is in use, the content of the EEPROM in the data compressing portion 65 is rewritten by the system controller 68 into the content of the compression program cartridge.
FIG. 5 shows a flowchart for the operation of this embodiment.
After initialization (step S101) has been done, when a memory cartridge is inserted (step S102), whether it is for photography or for compression programs is discriminated (step S103). If for compression programs; a compression code number representing the compression program is written (step S104) and the compression program is transferred to the EEPROM (step S105). When this has ended, the "end"display is presented (step S106). If it is for photography, an initiation of a shutter operation (step S110) is followed by writing the compression code number (step S111) and the photographed image data (step S112).
In such a manner, the program for use in the compression of the video signal can be written and rewritten in the form of electrical signals by the cartridges from the outside of the camera.
It should be noted that the camera may be provided with an input terminal for program, from which a program for compression is supplied in the form of an electrical signal by an adequate device, thus rewriting the program of the EEPROM of the data compressing portion 65.
As has been described above, according to the present embodiment, the program for compression of the data in the camera is alterable by the electrical signal supplied from the outside of the camera. Therefore, a wide variety of compressing methods become selectively usable. Hence, the camera is made convertible to the newest data compression type. Further, when the object to be photographed is a flower, the camera can be made to operate with selection of one of the compressing methods which is most suited to the flower. | A still video camera using a solid-state memory device as an image recording medium and wherein outset image data exists for processing comprises a plurality of data compression circuits, wherein one of the plurality of data compression circuits is selected according to the amount of image data following processing of the outset image data. The plurality of data compression circuits may effect compression of data by a data compression method selected from the compression method group consisting of DCPM, ADPCM and discrete cosine transformation. The plurality of data compression circuits may effect data compression by the same data compression method with respective different compressing characteristics. | 7 |
BACKGROUND OF THE INVENTION
The present invention relates to a weft reservoir for fluid jet looms, and more particularly relates to an improvement in the construction and operation of a weft reservoir for fluid jet looms wherein the weft is wound about a reservoir drum including conical and cylindrical sections through relative rotation between a yarn guide and the reservoir drum, reserved thereon and delivered therefrom for weft insertion under pin control.
In the following description, the side of the arrangement closer to the supply source of the weft is referred to in general as "the upstream side" whereas the side of the arrangement closer to the main jet nozzle for insertion of the weft is referred to in general as "the downstream side".
Weft reservation under pin control on a weft reservoir is roughly classified into two major types. In the first type of weft reservation, coils of weft for different cycles of weft insertion are separately reserved by cooperation of two or more control pins and, as a result of inter-pin assignment, are moved downstream on the reservoir drum. At the moment of weft insertion, coils of weft for that cycle of weft insertion are released by hold of the most downstream side control pin for delivery from the reservoir drum. In the case of this type, coils of weft for different cycles of weft insertion can be reserved in a fairly separated state and delivered quite independently of each other. But this type of weft reservation requires use of a relatively complicated mechanism to assure exactly phased movements of the control pins for proper inter-pin assignment of the weft and opportune release of weft for delivery.
In the second type of weft reservation, a sufficiently large number of coils of weft are reserved on the reservoir drum without any clear separation with use of a single control pin in engagement with the most downstream coil of weft. At the moment of weft insertion, the control pin is retained out of engagement with the weft, which is then subjected to delivery from the reservoir drum. When coils of weft for one cycle of weft insertion have been delivered from the reservoir drum, the control pin is brought into engagement with the most downstream coil of weft remaining on the reservoir drum. This type of weft reservation avoids the necessity for separate reservation of weft by two or more control pins. In addition, this type of weft reservation is very advantageous from the viewpoint of stable reservation of weft on the reservoir drum. The larger the number of coils of weft wound on the reservoir drum, the smaller the possibility of undesirable, accidental, slip-out of weft from the reservoir drum during the delivery of weft for weft insertion. Apparently such slip-out of weft lends to superfluous delivery of weft at that cycle of weft insertion and, further, to insufficient delivery of weft for the next cycle of weft insertion. Such slip-out of weft also tends to cause undesirable slippage of the weft on the reservoir drum in particular at the starting period of winding, which disables the reservation of the correct number of coils of weft for the next cycle of weft insertion. Despite such advantages, it is prerequisite to this type of weft reservation to provide a special expedient such as a photo-electric system to detect the number of coils of weft to be unwound from the reservoir drum during the delivery for weft insertion. In addition, the result of such detection has to be properly processed in order to incite a corresponding mechanical movement of the control pin. This also requires use of another complicated mechanism.
It is therefore strongly desirable to practice the above-described second type of weft reservation without complicating the mechanism of the weft reservoir involved.
Even when this requirement is satisfied and a control pin is very timely registered at its operative position for engagement with weft on the cylindrical section of a weft reservoir, the conventional construction of the weft reservoir, i.e. the uniform diameter of the cylindrical section for reservation of weft, cannot assure perfect prevention of the above-described accidental slip-out of weft at delivery.
It is then also required to provide a reliable expedient to prevent accidental slip-out of weft at delivery.
Aside from these requirements for a simple mechanism and stable the weft delivery without accidental slip-out of weft at delivery, care should be directed to the fact that operation of the control pin, more specifically maintaining control pin at its stand-by position, is closely related to the associated running of the loom, and that, as long as the main jet nozzle is in operation, coils of weft are freely delivered from the reservoir drum when the control pin is maintained at its stand-by position out of engagement with the weft under delivery. As explained already, the control pin is brought back to its operative position in engagement with the weft at a moment when coils of weft for one cycle of weft insertion have been delivered from the reservoir coil as long as normal loom operation continues.
Trouble starts when the loom stops running due to some accident such as yarn breakage in particular at the very moment of weft insertion. Coils of weft on the reservoir drum are delivered therefrom due to traction of the main jet loom in operation since the control pin has already been moved to the stand-by position out of engagement with the weft under delivery. Delivery of weft goes on but the control pin isn't brought back to the operative position since its operation is closely related to the running of the loom which has already stopped. As a consequence, more coils of weft are delivered than necessary for one cycle of weft insertion, which apparently causes insufficient weft delivery for the next cycle of weft insertion.
It is therefore strongly required that excessive delivery of weft should be prevented even when the loom stops its normal running even at the very moment of weft insertion.
SUMMARY OF THE INVENTION
It is the basic object of the present invention to provide a weft reservoir of a simple construction which allows reservation of sufficient number of coils of weft and delivery of weft exactly necessary for one cycle of weft insertion through use of a single control pin only.
It is another object of the present invention to provide a weft reservoir which further reliably prevents accidental slip-out of weft at delivery.
It is the other object of the present invention to provide a weft reservoir which restricts delivery of weft in excess of amount necessary for one cycle of weft insertion regardless of loom running condition.
In accordance with the basic aspect of the present invention, the weft reservoir includes a reservoir drum which includes an upstream side conical section converging downstream and a downstream side cylindrical section, a control pin is annexed to the reservoir drum with its point being directed to an operative position taken on the outer periphery of the reservoir drum on the downstream side of the cylindrical section, and the control pin is kept at a standby position away from the operative position over a period necessary for delivery of weft for one cycle of weft insertion.
In accordance with another aspect of the present invention, the weft reservoir is additionally provided with means for bar-ring accidental slip-out of weft at delivery from the reservoir drum which is arranged on the downstream side of the operative position for the control pin. In a typical embodiment of this aspect, the barring means includes a second conical section diverging downstream which is formed on the downstream side of the cylindrical section of the reservoir drum.
In accordance with the other aspect of the present invention, the weft reservoir is further provided with means for restricting delivery of weft in excess of the amount necessary for one cycle of weft insertion regardless of loom running condition. In a typical embodiment of this aspect, the restricting means includes an auxiliary control pin accompanying the control pin.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a side view of one embodiment of the weft reservoir in accordance with the present invention,
FIG. 2 is a side view of one embodiment of the pin drive unit used for the weft reservoir shown in FIG. 1,
FIG. 3 is a side view of another embodiment of the pin drive unit used for the weft reservoir shown in FIG. 1, and
FIG. 4 is a side view of the other embodiment of the pin drive unit provided with an auxiliary control pin for restricting excessive delivery of weft.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
One embodiment of the weft reservoir in accordance with the present invention is shown in FIG. 1, in which a stationary reservoir drum is used in combination with a rotary yarn guide. Needless to say, the present invention is well applicable to other types of weft reservoirs as long as weft taken from a given source of supply is supplied onto a reservoir drum through relative rotation between the reservoir drum and an annexed yarn guide. In one example, a stationary yarn guide may be combined with a rotary reservoir drum. In another example, a yarn guide and a reservoir drum may be both driven for rotation at different speeds. In the other example, an additional rotary guide may be used for reservation of weft on a reservoir drum.
The weft reservoir includes a stationary reservoir drum 1, a yarn guide 2 concentrically rotatable about the reservoir drum 1, a control pin P with its point being directed to the outer periphery of the reservoir drum 1 and a pin drive unit 100 arranged in a fixed relationship with respect to the reservoir drum 1. In this case, the pin drive unit 100 is arranged outside the reservoir drum 1 so that the control pin P is driven for movement between the operative position on the outer periphery of the reservoir drum 1 and a stand-by position radially outward of the operative position. As a substitute, however, the pin drive unit 100 may be arranged inside the reservoir drum 1 so that the control pin P is driven for movement between the operative position and a standby position radially inward of the operative position.
The yarn guide 2 is secured to a main drive shaft 3 which extends through a tubular housing 4 in order to support the reservoir drum 1 via suitable bearings (not shown). The reservoir drum 1 is blocked against free rotation by means of a suitable latching mechanism such as a magnet system (not shown). The main drive shaft 3 is supported for rotation by a bracket 5 by means of suitable bearings (not shown). The main drive shaft 3 is provided with a driven pulley 6b secured thereon and connected to a drive pulley 6a secured on an intermediate shaft 7 by means of a transmission belt 6c. The intermediate shaft 7 is operationally connected to the drive shaft of the associated loom for synchronized rotation. The yarn guide 2 is provided with an axial bore 21 which communicates with an axial bore 31 in the main drive shaft 3, both for passage of weft W.
The reservoir drum 1 in this embodiment includes the first conical section 11, converging in the downstream direction, a cylindrical section 12 formed on the downstream side of the first conical section 11 and the second conical section 13 diverging in the downstream direction and formed on the downstream side of the cylindrical section 12.
The weft W taken from a given source of supply (not shown) is brought to the outlet of the yarn guide 2 via the axial bores 31 and 21 and issued therefrom for reservation on the cylindrical section 12 of the reservoir drum 1. Presence of the second conical section 13 effectively prevents the of coils of weft from accidentally slipping out at delivery from the cylindrical section 12.
Any expedients may be substituted for the second conical section 13 diverging downstream as long as same effectively bars accidental slip-out of coils of weft at delivery. In one example, an annular brush may be arranged facing the outer periphery of the downstream end of the cylindrical section 12. In another example, the downstream end of the cylindrical section 12 may be encompassed by a circumferential covering to define an annular chamber in which an air flow is generated in order to press the weft under delivery onto the outer periphery of the cylindrical section 12.
A circumferential groove 14 is formed on the downstream side of the second conical section 13 in order to provide the operative position for the control pin P. More specifically, the point of the control pin P intrudes into the circumferential groove 14 when the control pin P is registered at the operative position being driven by the pin drive unit 100. In case of a weft reservoir employing a reservoir drum blocked against rotation, the circumferential groove may be replaced by a spot recess formed at a proper position in the outer periphery of the reservoir drum 1 corresponding to the operative position for the control pin P. In general, however, use of the above-described circumferential groove is rather advantageous since it allows slight rotation of the reservoir drum which may be conditionally caused by insufficient operation of the latching mechanism.
The weft reservoir further preferably includes a balloon breaker 8 arranged on its downstream end. This balloon breaker 8 effectively restricts radial expansion of the balloon of weft under delivery so that the weft W does not come into engagement with the control pin P kept at the stand-by position when the latter is moved radially outward from side of the operative zone on the outer periphery of the reservoir drum 1. The clearance between the inner wall of the balloon breaker 8 and the outer periphery of the reservoir drum 1 should preferably be as narrow as possible in order to minimize the path of travel of the control pin P. It is also preferable that the diameter of the balloon breaker 8 is freely adjustable in accordance with change in diameter of the reservoir drum 1.
In operation, the weft issued from the outlet of the yarn guide 2 winds about the first conical section 11 of the reservoir drum 1 and coils of weft automatically slide towards the cylindrical section 12 due to the converging construction of the first conical section 11. A sufficient number of coils of weft are thus reserved on the cylindrical section 12 with the most downstream coil of weft being in engagement with the control pin P now registered at the operative position. Delivery of weft is initiated when the control pin P is out of engagement with the weft, and continues as long as the control pin P is kept at the stand-by position out of engagement with the weft under delivery.
Obviously, the amount of weft to be delivered from the reservoir drum is proportional to the length of the period in which the control pin P is kept at the stand-by position away from the operative position. In accordance with the basic concept of the present invention, removal of the control pin P from the operative position and advance of the control pin P from the stand-by position are both timed so that the control pin P should stay out of any engagement with the weft under delivery over a period of a length necessary for delivery of weft for one cycle of weft insertion.
For example, if four coils of weft on the reservoir drum correspond to one cycle of weft insertion, the weft insertion starts at 90° crank cycle and terminates at 250° crank cycle, the fourth coil of weft will be fully unwound from the reservoir drum roughly at a moment between 220° and 230° crank angle. In this case, the operation of the control pin P should be timed to advance to the operative position in the circumferential groove 14 at a moment between 220° and 230° crank angle in order to initiate reservation of weft for the next cycle of weft insertion. In practice, a stroboscope is used to measure the moment at which the fourth coil of weft is unwound from the reservoir drum, and the pin drive unit 100 is set to drive the control pin P for advancement at a crank angle corresponding to the measured moment of unwind. In summary, the amount of weft necessary for one cycle of weft insertion is reserved by properly setting the length of period in which the control pin P is kept at the standby position out of engagement with the weft under delivery.
Assuming that weft insertion starts at TS° crank angle, terminates at TE° crank angle, and the number of coils of weft for one cycle of weft insertion is equal to N, unwinding of the fourth coil of the weft starts at {TS+(TE-TS)(N-1)/N}° crank angle and terminates at TE° crank angle. As a consequence, the control pin P should be returned to the operative position at a moment between {TS+(TE-TS)(N-1)/N} and TE° crank angles.
The control pin P is driven for such a timed movement by operation of the pin drive unit 100 annexed to the reservoir drum 1 as shown in FIG. 1, and one embodiment of the pin drive unit 100 is shown in FIG. 2, in which a pulse motor is used for driving of the control pin P. More specifically, the pin drive unit 100 includes a housing 101 having a slot 101a formed in its wall facing the outer periphery of the reservoir drum 1 for free passage of the control pin P. A cam shaft 103 is rotatably mounted to the inner framework 102 of the pin drive unit 100 and operationally coupled to an output shaft of a pulse motor (not shown). The pulse motor is set to rotate over 180° each time the control pin should move from the stand-by to the operative position and vice versa. An eccentric cam 104 is secured to the cam shaft 103 while bearing a follower ring 105. A support shaft 106 is secured to the framework 102 and idly carries a swing lever 107. The swing lever 107 holds, at one end, the control pin P and is operationally coupled, at the other end, to the cam follower ring 105 by means of a connecting link 108. At every 180° rotation of the eccentric cam 104, the lever 107 swings about the support shaft 106 clockwise or counterclockwise in order to move the control pin P between the operative and stand-by positions. As the lever 107 swings clockwise as reviewed in FIG. 2, the control pin P advances from the stand-by to operative position for engagement with weft on the reservoir drum 1. Whereas, as the lever 107 swings counterclockwise, the control pin P recedes from the operative to the stand-by position out of engagement with the weft on the reservoir drum 1.
Another embodiment of the pin drive unit 100 is shown in FIG. 3 in which a mechanical arrangement is used for causing the timed movement of the control pin P. Like the forgoing embodiment, the housing 101 is provided with the slot 101a on the side facing the outer periphery of the reservoir drum 1 for free passage of the control pin P. A cam shaft 121 is rotatably mounted to the inside framework 102 and operationally coupled to a proper drive motor (not shown) in order to perform one complete rotation per one complete rotation of the main drive shaft of the associated loom. A drive cam 122 is secured to the cam shaft 121. A support shaft 123 is secured to the framework 102 and pivotally carried one end of a swing lever 124. A cam follower 126 is rotatably mounted to the body of the swing lever 124 in resilient pressure contact with the drive cam 122 by assistance of a tension spring 127 interposed between the swing lever 124 and a spring seat 128 arranged on the framework 102. The other end of the swing lever 124 is pivoted to the top end of a hook lever 129 having a hook 129a at its lower end. The control pin P of this embodiment slidably extends through a guide 131 secured to the framework 102 and is provided, at a level corresponding to the hook 129a of the hook lever 129, with a fixed collar 132. A compression spring 133 is interposed between the guide 131 and the collar 132 surrounding the control pin P in order to resiliently press the control pin P towards its operative position on the outer periphery of the reservoir drum 1. A tension spring 134 is interposed between the body of the hook lever 129 and a spring seat 136 secured to the framework 102 in order to urge the hook 129a to move away from the collar 132 on the control pin P.
A pair of pulleys 137a and 137b are arranged for rotation in synchronism with the running loom and carry a selector 138 which is provided in the form of an endless belt having, at equal intervals, a number of surface bulges 139. A pusher rod 141 is slidably supported by a guide 142 secured to the framework 102 with one end in rolling contract with the back of the hook lever 129 and the other end facing the selector 138. The surface bulges 139 are arranged on the selector 138 so that one of them will come in contact with the end of the pusher rod 141 when the control pin P should be removed away from the operative position.
When the control pin P should be kept at the operative position, the bulges 139 on the selector 138 are out of contact with the end of the pusher rod 141 and the hook lever 129 swings about its top pivot by tension of the spring 134 so that its hook 129a should be kept out of engagement with the collar 132 on the control pin P which is now operationally disconnected from the cam drive system. As a consequence, the control pin P is kept at the operative position for engagement with weft on the reservoir drum 1 regardless of rotation of the drive cam 122.
At the very moment of weft delivery from the reservoir drum 1, one of the surface bulges 139 on the selector 138 comes in contact with the end of the pusher rod 141 which then pushes the hook lever 129 against tension of the spring 134 so that the hook 129a will come in engagement with the collar 132 on the control pin P. Now the control pin P is operationally connected to the cam drive system. As the drive cam 122 rotates, the lever 124 swings clockwise in the illustration about the support shaft 123 and, accordingly, the hook lever 129 lifts the control pin P via the collar-hook engagement so that the control pin P will be registered at the stand-by position out of engagement with weft to be delivered. After an amount of weft necessary for one cycle of weft insertion has been delivered, continued rotation of the drive cam 122 allows the control pin P to return to the operative position in engagement with the weft on the reservoir drum 1 and the control pin P is again operationally disconnected from the cam drive system by operation of the selector 138.
In accordance with the present invention, the amount of weft for one cycle of weft insertion is determined by the length of time in which the control pin P is kept at the stand-by position out of engagement with the weft under delivery. Weft on the continues to be delivered to the reservoir drum 1 during the above-described period. As long as the loom is operated normally, the operation of the control pin P is correctly timed to allow controlled delivery of the weft. When the loom ceases running for some unexpected reasons at the very moment of weft insertion, the control pin P is brought to the stand-by position and kept there even after the moment at which it should be returned to the operative position. In other words, delivery of weft continues even after the amount of weft necessary for one cycle of weft insertion has already been delivered, and this delivery continues until all coils of weft on the reservoir drum have been delivered, since the operation of the pin drive unit 100 is synchronized with the running of the loom which has already stopped.
In order to avoid this inconvenience, another embodiment of the present invention employs an auxiliary control pin P' accompanying the main control pin P. When the loom has ceased its normal operation, the auxiliary control pin P' is brought into contact with the outer periphery of the reservoir drum 1 in order to block the weft against delivery from the reservoir drum 1. During normal operation of the loom, the auxiliary control pin P' is kept out of contact with the reservoir drum 1 in order to pass the weft over to the sole control by the main control pin P. Operation of such an auxiliary control pin P' can be either manually or automatically controlled.
On embodiment of the manual control to this end is shown in FIG. 4, in which a swing lever 151 is pivoted at one end to a support shaft 152 and securedly holds at the other end the auxiliary control pin P' in the vicinity of the main control pin P. A pair of stoppers 153 and 154 are arranged on both vertical sides of the swing lever 151 while being properly spaced from each other. A fixed spring seat 156 is arranged near the support shaft 152 for the lever 151 and a tension spring 157 is interposed between the spring seat 156 and a pin 158 fixed to the body of the lever 151. The position of the fixed spring seat 156 is chosen so that, when the swing lever 151 is in contact with the lower stopper 154 and the auxiliary control pin P' is placed in contact with the reservoir drum 1, the axial line of the tension spring 157 should be located slightly below a straight line connecting the centers of the pin 158 and the support shaft 152 whereas, when the swing lever 151 is in contact with the upper stopper 153 and the auxiliary control pin P' is kept out of contact with the reservoir drum 1, the axial line of the tension spring 157 should be located above the above-described straight line.
When the loom has stopped its normal operation, the lever 151 is manually pushed towards the reservoir drum 1 via a knob 159. Then, the spring 157 acts to urge the lever 151 to swing counterclockwise in the illustration about the support shaft 152 so that the auxiliary control pin P' is kept in contact with the outer periphery of the reservoir drum 1 even after the manual action on the knob 159 has been removed. When normal operation of the loom reinstated, the lever 151 is manually pulled away from the reservoir drum 1 via the knob 159. Then, the axial line of the spring 157 comes above the straight line between the pin 158 and the support shaft 152 and the spring 157 acts to urge the lever 151 to swing clockwise about the shaft 152 so that the auxiliary control spring P' is kept out of contact with the outer periphery of the reservoir drum 1 even after the manual action on the knob 159 has been removed.
Alternatively, it is also possible to provide the main control pin P with the above-described function of the auxiliary control pin P' without using such a separate auxiliary control pin P'. In this case, a servo-motor is used for control of the operation of the control pin P. More specifically, such a servomotor is accompanied with an electric circuit including a manual switch which, when the loom has stopped its normal running, actuates the motor to bring the control pin into contact with the outer periphery of the reservoir drum. | On a drum-type weft reservoir for fluid jet looms, a single control pin used for control of reservation and delivery of weft is kept, without any detection of unwind of weft under delivery, away from engagement with weft on a reservoir drum over a period of a length necessary for delivery of weft for one cycle of weft insertion, preferably in combinating with an expedient for barring accidental slip-out of weft under delivery. | 3 |
PRIOR APPLICATION DATA
[0001] This application is a continuation of, claims priority to and the benefit of PCT Application No. PCT/IB2015/000927 which was published as WO 2015/189686 on Dec. 17, 2015 and claims priority to and the benefit of U.S. Provisional Patent Application No. 62/011,722 filed Jun. 13, 2014.
FIELD OF THE INVENTION
[0002] The present invention relates to gaming devices such as gaming tables.
BACKGROUND OF THE INVENTION
[0003] Gaming tables are utilized to implement a variety of games, including wagering games. These games may include, but are not limited to poker, baccarat and other games.
[0004] Originally, gaming tables were purely mechanical. The tables included a playing surface upon which cards, chips or the like could be placed. Cards were dealt manually and chips wagered and collected manually.
[0005] Recently, electronic gaming tables have been developed. These gaming tables incorporate one or more electronic features. The electronic features might comprise, for example, LED or LCD displays, lights or other electrically powered elements. The displays, lights or other features are built into the structure of the gaming machine, so as to be supported and/or protected by the structure of the table. These tables, however, are very expensive to manufacture and operate owing to the complexity of integrating the different electronic components into the table.
SUMMARY OF THE INVENTION
[0006] Aspects of the invention comprise gaming devices and methods of creating/manufacturing gaming devices, and methods of using such devices.
[0007] In one embodiment, a gaming table includes graphene ink enabled electronic features such as conductors, light or sound emitters, light detectors, touch or object detectors or displays. Conductive graphene ink may be printed on a gaming table fabric or felt which forms a playing surface of the gaming table. The graphene ink enabled electronic features may be coupled to or controlled by one or more controllers and be integrated into associated gaming systems. The graphene ink enabled features may replace larger, more expensive individual electronic components which must be assembled to implement functionality at a gaming table or other gaming device.
[0008] Further objects, features, and advantages of the present invention over the prior art will become apparent from the detailed description of the drawings which follows, when considered with the attached figures.
DESCRIPTION OF THE DRAWINGS
[0009] FIG. 1 illustrates a gaming system in accordance with an embodiment of the invention, the gaming system including at least one gaming table in accordance with the present invention; and
[0010] FIG. 2 illustrates the application of graphene ink via a printing device to a fabric or felt covering for a gaming table.
DETAILED DESCRIPTION OF THE INVENTION
[0011] In the following description, numerous specific details are set forth in order to provide a more thorough description of the present invention. It will be apparent, however, to one skilled in the art, that the present invention may be practiced without these specific details. In other instances, well-known features have not been described in detail so as not to obscure the invention.
[0012] One embodiment of the invention comprises gaming devices having grapheme ink enabled electronic features. In one embodiment, a gaming table includes a playing surface having electronic features which are enabled via grapheme ink.
[0013] One embodiment of the invention will be described with reference to FIG. 1 . FIG. 1 illustrates one embodiment of a gaming device in accordance with an embodiment of the present invention. In this embodiment, the gaming device comprises a gaming table 20 . The gaming table 20 may have a variety of configurations, including a variety of shapes, sizes and constructions. In one embodiment, the gaming table 20 defines at least one elevated playing surface 22 . The playing surface 22 may be supported, for example, by a support structure which includes one or more legs or other supports.
[0014] In one embodiment, the playing surface 22 is generally planar. However, the playing surface 22 could have raised and/or depressed areas. The playing surface 22 may be defined or covered by a fabric, such as felt or similar material.
[0015] The gaming table 20 may define or include one or more player areas and one or more dealer areas. For example, the gaming table 20 might have a first side 24 corresponding to a dealer area and a second side 26 corresponding to one or more player areas. Various information and/or features may be associated with the dealer and player areas.
[0016] In accordance with an embodiment of the invention, one or more of the features of the gaming table 20 are enabled or implemented by conductive ink or similar material, and most preferably conductive graphene ink. In a preferred embodiment, conductive graphene ink is used to create or define electrically conductive pathways or electronic components.
[0017] For example, graphene ink may be used to:
[0018] (1) define an electrically conductive pathway, such as to transmit electricity or electronic signals from one location to another, including between devices;
[0019] (2) detect light;
[0020] (3) emit light;
[0021] (4) emit sound;
[0022] (5) detect one or more objects;
[0023] (6) detect touch by a user;
[0024] (7) change the appearance of the playing surface (including via color, markings, 3-D texture, shape, etc.);
[0025] (8) be used as a display to display static or moving picture (video) information; and/or
[0026] (9) implement other features.
[0027] In one embodiment, graphene ink may be applied to or associated with the playing surface 22 . For example, referring to FIG. 2 , in one embodiment, graphene ink 201 may be applied to a felt 100 (or other fabric or material) which is associated with the gaming table 20 and forms the playing surface 22 . As one example, the graphene ink 102 may be applied via a printer 104 or by other devices or methods, to the felt 100 . In a preferred embodiment, the graphene ink is applied in a thin film or layer. The felt 100 , or at least the graphene ink areas, may be covered (such as by a protective film) in order to protect them from damage and wear. Because these electronic features are created by printing or deposition, they are referred to herein as “printed” electronic features (of course, graphene ink may be applied in other manners, so the term “printed” electronic features is not intended to be limiting, but is only used for convenience). Of course, the ink (and thus the features created thereby) could be applied to other materials comprising the playing surface 22 (such as glass, polymer films, or other coating which may be applied on or over a supporting substrate, such as a wood supporting surface, or even directly to the supporting substrate or surface itself).
[0028] The gaming table 20 may include various printed electronic features or components. For example, as illustrated in FIG. 1 , graphene ink might be applied to the playing surface 22 to define a progressive wager area 28 , an ante wager area 30 , a bet wager area 32 , and a game display 34 relative to each player location, among other features. In one embodiment, the graphene ink may be used to provide an illuminated border which defines each of the progressive wager area 28 , ante wager area 30 and bet wager area 32 . The border might be illuminated in one or more colors (including white) and the color may change, such as depending upon whether a player has placed a wager relative to that area (which may be detected by touch input or object detection, including by a graphene ink enabled detector relative to that area).
[0029] The game display 34 may comprise a graphene ink enabled display, such as for displaying changeable game information such as information about the size of a wager, game status and/or a variety of other information (including game-related information and other information such as advertisements, etc.). This information might comprise alpha, numeric, icon, image and/or other visible information.
[0030] As indicated above, the graphene ink may be used to implement one or more features such as a light detector, light emitter, sound emitter, display, touch input detector, object detector or other devices.
[0031] In one embodiment, the gaming table's printed electronic features may be associated with one or more controllers 36 . The controller 36 may be configured to receive input from the printed electronic features and/or to send information to those features. The controller 36 may comprise a computing-type device which comprises at least one controller or processor, one or more data storage devices such as hard drives, flash drives, RAM, ROM, EPROM, or other types of data storage devices now known or later developed, and one or more communication interfaces. The controller 36 may be configured to execute various instructions either embodied as hardware or embodied as computer readable code or “software” which is executed by a controller. The software may be stored on the associated memory or data storage devices, for example.
[0032] In one embodiment, the graphene ink enabled or printed electronic features may be hard-wired to the controller 36 . In other embodiments, the features might be configured as computing device peripherals, such as comprising USB type devices (in which event, the features might include a USB controller). In other embodiments, the features might include wired or wireless communication interfaces, such as to permit the features to communicate with the controller 36 (or other devices) via Bluetooth, Wi-Fi, TCP-IP or other communication protocols.
[0033] In one embodiment, the gaming table 20 may be part of a larger gaming network 50 . The gaming network 50 may include other features or components, such as other gaming tables, gaming machines such as video or slot machines, and one or more gaming systems, such as a player tracking system 52 , an accounting system 54 , and a jackpot systems 56 , among others. The player tracking system 52 , accounting system 54 and jackpot system 56 (and/or other systems) may be enabled by one or more computing devices, such as one or more servers. These systems may enable player tracking, accounting and jackpot functionality, as is well known in the casino arts. This connectivity allows integration of the printed electronic features with other gaming and non-gaming related devices and systems.
[0034] As one example, in the event a jackpot system 56 determines that a jackpot is active, the jackpot system 56 might send a jackpot instruction to the controller 36 . The controller 36 might then cause graphene ink on the table surface 22 which is applied to spell the word JACKPOT to illuminate, thus providing an indication to players that this game feature is active. Likewise, bet information and other player inputs to graphene ink enabled features may be transmitted to the controller 36 and thereon to the appropriate gaming systems, such as for tracking monies wagered and lost, game play parameters in association with identified players, etc.
[0035] Of course, the gaming table 20 illustrated in FIG. 1 is simply one embodiment of an implementation of the invention. For example, graphene ink might be used to implement other gaming device features. As indicated above, the graphene ink might be used to implement a variety of gaming-related functionality. This functionality might include, but is not limited to:
[0036] (1) Displaying game indicia, such as images of playing cards or the like, including based upon certain events or in mystery format;
[0037] (2) Highlighting a player's actions, such as placing of a bet or receiving other input, such as by changing a color or quantity of light emitted in one or more areas or via emitting sound;
[0038] (3) Detecting a player's presence at the gaming table;
[0039] (4) Highlighting the location or identify of a winner of a gaming event, such as the winner of a game or a jackpot;
[0040] (5) Changing a game table layout, such as to change the number of player locations (including adding or removing locations) or to configure the layout for use in presenting different types of games (such as different poker games, baccarat games or the like);
[0041] (6) Modify the appearance of the gaming table layout, such as based upon a random event;
[0042] (7) Make certain portions of the playing surface transparent or opaque;
[0043] (8) Cause sounds to be emitted from certain portions of the playing surface; and/or
[0044] (9) Receive player input, such as by detecting player touch of certain areas of the playing surface and/or detecting objects (such as chips, player tokens or the like).
[0045] In one embodiment, the gaming table 20 or other gaming device may have other electronic features (i.e. features which are not created via graphene ink). The one or more graphene ink implemented or “printed” features may be configured to integrate with or connect to those features. For example, graphene ink might be used to define a conductive pathway for electricity/power or electronic signals between the controller and an electronic device or two electronic devices. This may avoid the need for standard wiring, including wiring harnesses, connectors and the like.
[0046] The printed electronic features might also integrate with other electronic devices. As but one example, a gaming table might include a card reader which is capable of obtaining an image of a physical playing card (or at least information which identifies the card, such as rank and suit information). The card information which is obtained by the card reader might be used to cause a printed display to display a graphical image of the one or more scanned cards. As one example, a card reader might read a bonus card which is dealt from a deck of cards. An image of that card might be displayed on the printed displays 34 (see FIG. 1 ) at each player location. Of course, the printed electronic features of the invention might associate or integrate with a variety of other devices such as card shufflers, LED/LCD/plasma or other video displays, signs, lights, media readers (such as magnetic stripe, bar code, RFID or other readers), printers, etc.
[0047] It will also be appreciated that the invention may be applied to other gaming devices. For example, graphene ink might be applied to a surface of an electronic gaming machine in order to implement certain electronic features.
[0048] In the preferred embodiment of the invention, graphene ink is utilized to implement the electronic features because of its ease of application (such as via printing), low cost, flexibility (conforming to the substrate it is applied to and being flexible/bendable therewith), and its low profile/space requirements. Unlike wires, very thin layers of conductive graphene ink can be applied which do not interfere with the feel of the gaming able. For example, unlike a wire placed on the surface of a gaming table, a layer of graphene ink does not create a ridge or bump on that surface. One advantage to the invention is that electronic features can be enabled simply by printing the conductive graphene ink on a table surface or a covering for that surface, rather than by associating individual electronic components with a table, connecting those components, etc. The entire configuration of a gaming table can be changed by either simply replacing the gaming table felt or by activating or deactivating certain ones of the graphene ink enabled electronic feature. While conducive graphene ink is the preferred material which is used to implement the invention, other similar types of materials which are now known or later developed which have similar characteristics, could be utilized.
[0049] It will be appreciated that aspects of the invention comprise: (1) electronic features at a gaming device which are created by conductive ink; (2) the combination of such printed electronic features with other devices, (3) entire systems incorporating those printed electronic features, such as gaming systems which include gaming devices (including tables) which include a printed electronic feature; and (4) methods of creating and using such features, devices and systems.
[0050] It will be understood that the above described arrangements of apparatus and the method there from are merely illustrative of applications of the principles of this invention and many other embodiments and modifications may be made without departing from the spirit and scope of the invention as defined in the claims. | A gaming table includes graphene ink enabled electronic features such as conductors, light or sound emitters, light detectors, touch or object detectors or displays. Conductive graphene ink may be printed on a gaming table fabric or felt which forms a playing surface of the gaming table. The graphene ink enabled electronic features may be coupled to or controlled by one or more controllers and be integrated into associated gaming systems. The graphene ink enabled features may replace large, expensive individual electronic components which must be assembled to implement functionality at a gaming table or other gaming device. | 6 |
BACKGROUND OF THE INVENTION
This invention relates to improvements in hydraulic positioning apparatus for precisely and rapidly positioning objects of the type likely to exert high impact or shock loads on the positioning apparatus. In particular, the invention relates to improvements in hydraulic positioning apparatus of the automatic type in which a controller responsive to the position of the apparatus automatically controls its movements so as to obtain precise positioning. The invention is especially applicable, although not limited, to sawmill setworks for precisely positioning logs preparatory to sawing thereof, and to the use of linear hydraulic piston and cylinder positioning assemblies in such setworks.
Precise automatic hydraulic positioning devices of both the rotary and linear (i.e. piston and cylinder) types have been known for many years. An example of an exceptionally precise automatic linear positioning assembly, of a type capable of positioning objects to within several thousandths of an inch, is described in U.S. Pat. No. 4,121,504 issued Oct. 24, 1978, the text of which is incorporated herein in its entirety by this reference. The rapid, yet precise positioning function performed by devices of this type is made possible by the fine modulation of a servo valve which is controlled automatically by a controller responsive to the position of the movable element of the hydraulic positioning device. The actual position of the movable element is compared to a predetermined or desired position and the valve is modulated to achieve and retain such position. Moreover the automatic controller also controls acceleration, velocity and deceleration of the positioning device which is necessary for rapid as well as precise positioning. To accomplish all of this, the hydraulic components of the system, particularly the seals, servo valve modulating surfaces and internal moving surfaces of the hydraulic motor itself, must be in good condition so that undue leakage, friction or other obstacles do not hinder the precise control function.
Because of the foregoing requirements of such a hydraulic positioning system, difficulty has been encountered when attempting to apply such a system to the positioning of objects of the type expected to impose substantial impact loads on the system. Such impact loads can instantly increase hydraulic pressure to many times that for which the system was designed, leading to rapid deterioration or destruction of seals, valves and other components such that the system either becomes rapidly unreliable or requires an unreasonably high degree of continuous maintenance.
Previous methods of reducing the effect of impact loads on hydraulic systems have included interposing cushioning pneumatic bags or cylinders between the hydraulic motor and either its mount or the impact load. However these permit a nonrigid connection between the hydraulic device and the object to be positioned, and therefore are not compatible with the precision and quickness required of automatic positioning systems.
One commonly attempted method of attempting to overcome the problem of impact loading in automatic positioning systems is depicted in FIG. 7 of the aforementioned U.S. Pat. No. 4,121,504. This is the provision of a spring-operated pressure-relief valve which is intended to relieve overpressures which may occur on either side of the piston and cylinder assembly by exhausting overpressurized fluid to the sump. The problem with this arrangement is that the spring-operated pressure-relief valve is too slow to relieve instantaneously-applied impact pressure, especially when interposed between the servo control valve and the piston and cylinder assembly. The springs of such valves are heavy and operate over a substantial pressure range between full closure and full opening of the valve. In the time that it takes for the valve to open sufficiently to relieve impact pressure the damage from particularly high impact loads will already have occurred. What is needed is a system that is so fast-acting that the impact pressure is prevented from building up despite the instantaneous nature of the impact load.
A particularly appropriate potential application of automatic hydraulic positioning system exists with respect to sawmill setworks wherein carriages with transversely-movable setting knees receive and position logs preparatory to sawing. The log is moved onto the carriage with substantial momentum and impacts with great force against the setting knees, which then position the log precisely for sawing so as to obtain optimum yield from the particular log. A plurality of setting knees are spaced along the carriage and, pursuant to modern requirements, the knees are movable independently of one another so as to achieve infinite angular adjustment of the log with respect to the saws (known as achieving "infinite taper"). It has been known to use linear hydraulic piston and cylinder assemblies to position the setting knees of such setworks, but these are of the much less efficient, nonautomatic manually-controlled type where the absence of automatic controls makes deterioration and imprecision of the hydraulic system more tolerable. Because of the extremely high impact loads imposed by the logs on such a system, however, no automatic linear hydraulic positioning systems having precise, rapid automatic positioning have previously been employed to position the setting knees. Instead, ballscrew drives have been employed where automatic positioning is desired. However, a great disadvantage of using ballscrews has been the low setting speed of the knees. Also, to achieve infinite taper, each knee must have an individual ballscrew drive, which results in an extremely expensive system.
SUMMARY OF THE PRESENT INVENTION
The present invention provides a hydraulic positioning system which has novel shock-absorbing features which are compatible with the precision and quickness required of automatic hydraulic positioning systems and yet are sufficiently fast-acting to prevent damage to seals, valves and other hydraulic components under extremely high impact loads, thereby maintaining the precision of the system over extended operating periods despite such impact loading. The system makes it possible, for the first time, to reliably use automatic rotary and linear hydraulic positioning motors in extremely high impact applications, and particularly to use automatic linear hydraulic positioning motors, i.e. automatically-controlled piston and cylinder assemblies, on sawmill setworks carriages to reliably position setting knees to within a few thousandths of an inch despite the huge impact loads exerted on the knees by the placement of each log on the carriage.
Rather than relying on the presence of cushioning pneumatic devices, which would cause imprecise and slow positioning, or on spring-operated relief valves which are too slow acting to relieve high impact pressures adequately, the present invention provides a system whereby pressure in the hydraulic positioning motor is constantly balanced against system pressure at the source of pressurized hydraulic fluid through a simple one-way check valve which opens fully instantaneously and allows immediate relief of over-pressurized fluid when the pressure of fluid in the motor exceeds system supply pressure by a small predetermined amount (usually the amount needed to overcome a weak biasing spring which is merely strong enough to urge the one-way valve toward closure when the pressures on both sides thereof are equal). This type of system, wherein impact pressure must merely overcome system pressure to accomplish full relief thereof, is significantly faster acting than previous relief systems and is thus able to prevent high impact pressures from shock loads.
The principle of operation of the system involves relieving the fluid not merely to a sump, as in conventional relief valve arrangements, but rather to the system's source of pressurized fluid. This requires a certain volumetric elasticity of the pressurized fluid source so that it can immediately accept overpressurized fluid from the hydraulic motor through the one-way valve upon impact. Preferably this elasticity is provided by an accumulator. It is conceivable, however, that in some applications the elasticity provided by long hydraulic conduits between the hydraulic motor and the fluid source, combined with the limited compressibility of hydraulic oil and the eventual relief provided by a slow acting relief valve located at the source of pressurized fluid (i.e. remote from the hydraulic motor and separated therefrom by a servo valve) might provide sufficient volumetric elasticity.
The system can protect one or both sides of a double-acting positioning motor, depending on the application, and although well-suited for nonregenerative systems is especially adaptable for use in regenerative systems which transfer fluid from one side of a motor to the other side thereof. In the regenerative application, only a single one-way valve is required to protect both sides of the motor, and the system can completely prevent cavitation in the direction of highest expected impact.
It is therefore a principal objective of the present invention to provide an automatic hydraulic rotary or linear positioning system which has shock-absorbing features compatible with the required precision and quickness of such an automatic system and yet is sufficiently fast acting to protect the system from adverse effects of extremely high impact loads.
It is a further principal objective of the present invention to provide a sawmill setworks having an automatic hydraulic linear positioning system of high precision and quickness for independently positioning the individual setting knees thereof.
The foregoing and other objectives, features and advantages of the present invention will be more readily understood upon consideration of the following detailed description of the invention taken in conjunction with the accompanying drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a schematic diagram of a nonregenerative embodiment of the present invention as applied to a sawmill setworks.
FIG. 2 is a schematic diagram of a regenerative embodiment of the invention as applied to a sawmill setworks.
FIG. 3 is a schematic, simplified top view of an exemplary sawmill setworks utilizing the present invention.
DETAILED DESCRIPTION OF THE INVENTION
As shown in the figures, a linear hydraulic motor such as a selectively extensible piston and cylinder assembly 10 is shown connected to a setting knee 12 or equivalent log-positioning member. Both the piston and cylinder assembly 10 and setting knee 12 are mounted upon a carriage 14, the setting knee being linearly reciprocable on the carriage in response to the extension or retraction of the piston and cylinder assembly 10. A controller 16 is responsive, through any suitable connection depicted by the dotted line 18, to the reciprocating position of the setting knee 12 (in this case by sensing the extensible position of the piston of the piston and cylinder assembly 10), and automatically controls a servo valve 20 through a control connection 22 so as to position the setting knee 12 precisely in accordance with predetermined position data which has been preset in the controller 16. The controller 16 also preferably controls acceleration, velocity and deceleration of the setting knee through modulation of the servo valve 20. Preferably the automatic position sensing and controlling functions of the system are carried out in accordance with the structures shown in the aforementioned U.S. Pat. No. 4,121,504. However functionally equivalent arrangements satisfactory for the purpose are available on the market. Moreover, although a single three-position servo valve 20 is shown for controlling the extension and retraction of the piston and cylinder assembly, multiple separate valves controlling extension and retraction respectively could alternatively be used. Also the system is useful in many applications other than sawmill setworks. If the motion of the member to be positioned is linear, then a linear hydraulic motor such as that depicted in the figures is probably the most precise motor to use, since intermediate linkage is minimized. However if the member to be positioned has a rotary motion, it may well be that a rotary hydraulic motor would be preferable. All of these alternative possibilities are within the scope of the present invention.
In the figures the servo valve 20 receives hydraulic fluid from a source of pressurized hydraulic fluid indicated collectively by the elements contained within the phantom outline 24. These elements may include a prime mover such as an electric motor 26 which drives a suitable pump, such as a variable displacement, pressure-compensated hydraulic pump 28, which supplies hydraulic fluid under pressure to the servo valve through a fluid conduit 30. The source of pressurized hydraulic fluid also preferably includes an accumulator 32 and conventional spring-operated pressure-relief valve 34. The system draws fluid from, and returns fluid to, a reservoir 36.
In the nonregenerative embodiment of the system depicted in FIG. 1, extension of the piston and cylinder assembly 10 is accomplished by the actuation of the servo valve 20 by the controller 16 to move the valve toward the right as shown in FIG. 1. This introduces fluid under pressure to chamber 10a through conduit 38 while simultaneously exhausting fluid from chamber 10b through conduit 40. Retraction of the piston and cylinder assembly 10 is accomplished by movement of valve 20 to the left which introduces pressurized fluid to chamber 10b through conduit 40 while exhausting fluid from chamber 10a through conduit 38. When valve 20 is centered, fluid under pressure is prevented from entering either chamber 10a or 10b through parallel conduits 42, 42a and 42b respectively, which bypass valve 20, by virtue of one-way valves 44 and 46 respectively. Likewise, these one-way valves prevent the exhaust of pressurized fluid from the source 24 through the servo valve 20 when the valve 20 is in its right or left-hand positions.
The exertion of high instantaneous impact loading upon the piston and cylinder assembly 10 is exemplified in the figures by the movement of a log 48 into abutment with the setting knee 12. In the exemplary sawmill setworks illustrated in the figures, this impact-producing motion occurs each time a log is loaded onto the carriage 14 and thus occurs repeatedly in normal operation. Since the log has a high mass, a substantially instantaneous rise in the pressure of hydraulic fluid in chamber 10a occurs, which can be to a level many times the pressure produced by the source 24 unless the pressure in chamber 10a is instantaneously relieved. Without such instantaneous relief, the seals of the piston and cylinder assembly 10 and of the servo valve 20, the various hydraulic couplings and conduits and the high-tolerance modulating surfaces of the servo valve 20 can all become quickly deteriorated with the result that precise and rapid automatic control are no longer reliably obtained, thereby defeating the system.
In the present invention, relief of the pressure in the chamber 10a is obtained so instantaneously that there is little increase in pressure in the system as a result of the impact. This is because, immediately upon impact, fluid in chamber 10a is exhausted through one-way valve 44 and conduits 42a and 42 into the source of pressurized fluid 24. In this regard it is significant that one-way valve 44 is of a type whose opening and closure is responsive substantially entirely to the difference between pressure in chamber 10a and pressure at source 24 exerted through conduits 42 and 42a. Only a weak biasing spring (not shown) is incorporated into valve 44 to bias the valve toward closure when the pressures on both sides thereof are equal. Such weak biasing spring is overcome by a small differential pressure, for example on the order of 3 psi so that if system pressure at the source 24 is 2000 psi valve 44 will fully open as soon as the pressure in chamber 10a reaches as little as 2003 psi. This full relief action occurs instantaneously, and is to be sharply contrasted with the action of a conventional spring-operated relief valve which, rather than opening primarily in response to a pressure differential across the valve, opens gradually in response to upstream pressure overcoming the compression of a heavy spring. The fact that such a relief valve opens only gradually in response to overpressure, requiring a substantial overpressure to open the valve fully, makes such a valve too slow-acting to prevent the harmful instantaneous increase in pressure caused by the impact load.
Because of the pressure differential principle upon which the relief function of the present invention operates (as opposed to relieving to the reservoir 36 as would be the case with a conventional spring-operated relief valve), the source 24 must have a certain degree of volumetric elasticity in order to accept the overpressurized fluid. This volumetric elasticity is preferably provided by an accumulator such as 32. However in some applications it may be sufficient, if the source 24 is located sufficiently remote from the chamber 10a, that the elasticity of the conduits 30, 42 and 42a, coupled with the limited compressibility of hydraulic oil and the slow relief afforded for example by the relief valve 34 at the remote source 24, might provide sufficient cushioning to prevent severe impact overpressure if the impact load is sufficiently small.
In the particular embodiment shown, impact loads applied in a direction opposite to the movement of the log 48 would be relatively smaller, resulting possibly from too rapid stopping of the setting knee 12 during extension of the piston and cylinder assembly. However in other applications impact relief in both directions may be of equal importance. In any case, impact relief for chamber 10b is provided through one-way valve 46 and conduits 42b and 42 in the same manner previously described with respect to one-way valve 44.
Relieving overpressurized fluid through the above-described one-way valve directly to the source of pressurized fluid 24 which supplies the motor 10 is the simplest and preferred way of practicing the present invention since it utilizes the source 24 also as a shock-absorbing circuit. However it would of course be satisfactory, although more complicated, to relieve the overpressurized fluid through such a one-way valve to a shock-absorbing pressurized fluid circuit or accumulator other than the source 24, so long as the separate circuit or accumulator maintains fluid at a pressure at least equal to that of the source 24 and can accept overpressurized fluid through the one-way valve upon impact.
In FIG. 2, a more advantageous arrangement for obtaining instantaneous bidirectional relief of impact loads utilizing the principles of the present invention in a regenerative circuit is shown. The system is similar to that previously described with respect to FIG. 1, with like components having the same reference numerals. The only difference occurs in the interconnection of the fluid source 24 and servo valve 20 with the piston and cylinder assembly 10. It will be noted, for example, that servo valve 20 is interconnected controllably through a fluid conduit 52 only with chamber 10a of the piston and cylinder assembly. To extend the piston and cylinder assembly, valve 20 is moved toward the right in FIG. 1 introducing pressurized fluid from the source 24 through conduit 52 to chamber 10a. Hydraulic fluid is exhausted simultaneously from chamber 10b against system pressure through conduit 54 which, by virtue of its junction with pressurized fluid supply conduit 30, recirculates the exhausted fluid into chamber 10a, thereby requiring pump 28 to supply only a sufficient volume of fluid to equal the volume of that portion of the piston rod 10c being extended. In view of the fact that the fluid pressures on both sides of the piston are equal in a regenerative circuit, extension of the piston is caused by the fact that the working area of the piston exposed to chamber 10a is greater than its working area exposed to chamber 10b by a difference which is equal to the cross-sectional area of the piston rod 10c.
Retraction of the piston and cylinder assembly 10 is accomplished by movement of valve 20 toward the left as shown in FIG. 2, whereby fluid under pressure is introduced through conduit 54 into chamber 10b and fluid is simultaneously exhausted from chamber 10a to the reservoir 36 through conduit 52. The exhaust of fluid is under the modulating control of valve 20 which thereby controls the rate and degree of retraction of the piston even though the valve 20 has no direct control over the flow of pressurized fluid in conduit 54.
Upon the exertion of an impact load tending to retract the piston and cylinder assembly 10, such as that produced by the movement of the log 48 against the setting knee 12, the overpressurized fluid in chamber 10a is instantaneously relieved through conduit 56, one-way valve 50 and conduit 54 into the pressurized source 24 in the same manner as previously described with respect to one-way valve 44. The opening and closure of valve 50 is likewise responsive to the difference between the pressure of fluid in chamber 10a and the pressure of fluid at the source 24. A benefit of the regenerative circuit of FIG. 2 during this pressure-relief function, which is not present in the nonregenerative circuit of FIG. 1, is the fact that a portion of the relieved fluid flowing through one-way valve 50 is recirculated through conduit 58 into chamber 10b under pressure, thereby preventing cavitation in chamber 10b. This cavitation prevention feature can be important if impact loading is exceptionally high, although under most circumstances a small degree of cavitation would not be harmful.
Impact loading in the opposite direction, i.e. in the direction of extension of the piston and cylinder assembly 10, is relieved by permitting the exhaust of fluid from chamber 10b directly through conduits 58 and 54 into the source 24. It will be noted that, in a regenerative circuit, no second one-way valve is required in conduit 58 for the relief of chamber 10b, as was the case with respect to the nonregenerative system of FIG. 1. The relief of chamber 10b still operates on the same pressure differential principle, but reverse flow through conduit 58 is permitted.
FIG. 3 is a simplified schematic top view showing the system as installed on a sawmill setworks carriage having three individually-controllable setting knees. The assemblies which include a servo valve 20 and the associated one-way valves and relief circuitry enclosed by the phantom outline 60 in FIG. 1 are shown as single compact units 60 in FIG. 3. For regenerative applications, these may alternatively constitute the assembly enclosed by the outline 62 in FIG. 2. The carriage 14 is of elongate shape having a series of upwardly-facing spaced surfaces 14a for supporting a log 48 longitudinally with respect to the carriage 14. The log-positioning setting knees 12 are spaced longitudinally along the carriage 14 and are movably mounted on the carriage for reciprocation in a direction transverse to the longitudinal dimension of the carriage, each setting knee being reciprocable in response to the extension or retraction of a respective piston and cylinder assembly 10. The source of pressurized hydraulic fluid 24 supplies all of the piston and cylinder assemblies through the conduit 30, and the controller 16 likewise senses the positions of the various pistons through connection 18 and controls the extension or retraction of each piston and cylinder assembly separately through connection 22 in response to the position of each piston in comparison with predetermined criteria. With the log properly positioned by the setting knees, the carriage moves longitudinally so as to feed the log longitudinally with respect to the sawblades.
The terms and expressions which have been employed in the foregoing specification are used therein as terms of description and not of limitation, and there is no intention, in the use of such terms and expressions, of excluding equivalents of the features shown and described or portions thereof, it being recognized that the scope of the invention is defined and limited only by the claims which follow. | A hydraulic positioning system for precisely and rapidly positioning objects of the type likely to impose impact loadings on the system. The system is particularly adaptable for use in sawmill setworks for precisely positioning logs preparatory to sawing thereof. High impact loads are compensated for by special rapid-acting shock-absorbing hydraulic relief circuitry responsive to differences between impact overpressure and system pressure. | 1 |
This application is a continuation-in-part of our prior co-pending application for a "Micropipette Adaptor for Spectrophotometers" Ser. No. 377,476 filed July 10, 1989 now U.S. Pat. No. 4,991,958.
FIELD OF THE INVENTION
The present invention pertains to devices which hold sample materials while the composition of the material is being measured and analyzed. Specifically, the present invention pertains to sample holders which may be used with spectrophotometers and colorimeters. The present invention is particularly, but not exclusively, useful for obtaining spectroscopic measurements of very small samples of material while being heated.
BACKGROUND OF THE INVENTION
The use of spectrophotometers to measure the light absorption characteristics of sample materials is well known. Indeed, the basic principles involved are relatively simple. A beam of light, whose characteristics are known, is directed through the sample material and the light that emerges is analyzed to determine which wavelengths of the original beam were absorbed, or otherwise affected, by the sample material. Based on differences between the incident light and the transmitted light, certain characteristics of the sample material can be determined. Many variables are involved, however, that can make a spectrophotometric measurement quite complex. In sum, these complexities arise from the fact that the sensitivity and accuracy of a measurement rely on the ability of the spectrophotometer to measure the light which is absorbed by the samples.
Analytically, a spectrophotometric analysis relies on a known relationship of the variables involved. Specifically, in a standard spectrophotometric measurement, the amount of light transmitted through a test cuvette is measured and the percent of transmitted light is related to the material in the cuvette by the following relationship:
I.sub.t (λ)=I.sub.o (λ)10.sup.-OD
where I o (λ) and I t (λ) are respectively the input and transmitted intensities, and the optical density, OD, is given by:
OD=α(λ)L C
where α(λ) is the absorptivity of the material as a function of λ, L is the optical path length, and C is the concentration. From the above, it will be easily appreciated that the output intensity I t (λ) is directly proportional to the input intensity I o (λ). Therefore, it is clearly necessary to have an input intensity that is sufficient to give an output intensity which can be effectively used for analysis and measurement of the sample material. Further, the efficacy of the measurement will also be enhanced if the concentration of the sample material is increased. Thus, for spectrophotometric analysis it is desirable to have a light input of high intensity, and have a highly concentrated sample in solution. There is a problem, however, when low concentration solutions of sample material are available in only very small quantities (e.g. 0.5 to 50 micrograms/microliter).
To be effective for spectroscopic measurements, test cuvettes for holding the sample material must be completely filled. This typically requires a substantial amount of sample material. Consequently, when only a small amount of the sample material is effectively available for testing, presently available test cuvettes (e.g. 12.5 mm×12.5 mm cuvette) are inadequate because of their relatively large size. Merely reducing the size of the cuvette is not the answer. This is so because, with a size reduction of the cuvette there is also a reduction in the amount of sample material through which light can pass. Consequently, the intensity of the light passing through the sample material is reduced and the sensitivity and accuracy of the measurement is compromised.
The present invention recognizes that it is possible to take spectrophotometric measurements of very small quantities of a sample material, even where there is a relatively low concentration of the material in solution. The present invention recognizes that this can be done by properly focusing collimated light onto the sample material to obtain sufficiently high input light intensities for the desired measurements. Further, the present invention recognizes that this focusing can be accomplished by a device which is engageable, and operatively compatible, with presently available spectrophometers such as a UVIKON Model 820 spectrophotometer by Kontron.
The present invention further recognizes that occasionally it is important to make spectroscopic observations of small samples at various controlled elevated temperatures. For example, for DNA material, it is known that the double strands of DNA break into two single strands (denatures) at temperatures above 70° C. This denaturing of the DNA is also known to result in a significant increase in the light absorption of the sample. It is desirable to spectroscopically monitor denaturization. It is also desirable to spectroscopically monitor enzymatic and other thermally-induced reactions in small biological, as well as nonbiological, samples. For example, the progress of the polymerase chain reaction of assembling DNA segments can be studied if the sample is properly heated. Indeed, part of this study requires heating the DNA sample to raise the temperature above the denaturing temperature and then reducing the temperature to allow the single strands to find their complementary sites to form new double strands.
The present invention further recognizes that it is possible to monitor spectrophotometric changes at biologically significant temperatures. Study of bacteria or virus growth at human body temperatures of 37° C. could also be possible. In addition, nonbiological chemical reactions at temperatures elevated above room temperature can also be studied. The present invention accomplishes this by providing an apparatus which allows heating of the very small quantities of sample material in a controlled and efficient manner.
In light of the above, it is an object of the present invention to provide a micropipette adaptor for spectrophotometers which allows for spectrophotometric measurements of very small quantities of sample material in solution. Another object of the present invention is to provide a micropipette adaptor for spectrophotometers which permits recovery of the sample material after spectrophotometric measurements have been made. Yet another object of the present invention is to provide a micropipette adaptor for spectrophotometers which allows spectroscopic measurements of samples while the sample is in the process of being transferred through a micropipette. Still another object of the present invention is to provide a micropipette adaptor for spectrophotometers which provides for a high light collection efficiency to increase the sensitivity of the measurements which are made. Another object of the present invention is to provide a micropipette adaptor for spectrophotometers which allows a micropipette or other capillary sample holder to be easily installed and removed from the adaptor. Yet another object of the present invention is to provide a micropipette adaptor for spectrophotometers which provides approximately the same intensity light path length product for small samples as is provided for larger samples. Another object of the present invention is to provide a micropipette adaptor for spectrophotometers which is relatively easy to manufacture and comparatively cost-effective to operate.
Further, an object of the present invention is to provide a micropipette adaptor in which the temperature of the sample may be controlled. Another object of the present invention is to provide such a temperature-controlled micropipette adaptor which may be used in commercially available spectrophometers. Yet another object of the present invention is to provide a temperature-controlled micropipette adaptor capable of easily attaining higher sample temperatures, and capable of maintaining predetermined temperatures for desired lengths of time. Another object of the present invention is to provide a temperature-controlled micropipette adaptor which is relatively simple and convenient to manufacture and use.
SUMMARY OF THE INVENTION
The micropipette adaptor for spectrophotometers according to the present invention comprises a base member which is adapted to hold a capillary tube, such as a micropipette, which is filled with a solution of the sample material to be analyzed. More specifically, the base member is formed with an opening, and is formed with a hole which is distanced across the opening from a conical well. As formed on the base member, both the hole and the conical well are aligned with each other to respectively receive a portion of the micropipette and hold it on the base member. When so held, the micropipette extends across the opening of the base member to permit light to pass through the micropipette.
An optical system is provided for the adaptor and is attached to the base member to both focus a beam of collimated light onto the micropipette, and to recollimate the light that has passed through the micropipette. For focusing the beam of collimated light, a cylindrical quartz lens (i.e. a directing lens) is positioned between the base member and the source of collimated visual or ultraviolet light. Specifically, this directing lens is used to focus collimated light from the light source into a line. In accordance with the present invention, this linearly focused light is aligned along the longitudinal axis of the micropipette to provide a very high intensity light input for the sample material which fills the lumen of the micropipette. Another cylindrical quartz lens (i.e. a receiving lens) is positioned behind the base member to receive the light which has passed through the sample material in the pipette and to recollimate it for analysis and measurement by a detector.
As contemplated by the present invention, both the directing lens and the receiving lens are respectively held by holders which are positioned on opposite sides of the base member. Importantly, each of these holders is independently adjustable in its position relative to the base member. Thus, the directing lens may be independently moved relative to the micropipette to achieve alignment of its linearly focused light with the axis of the micropipette. Similarly, the receiving lens may be moved relative to the micropipette to achieve effective recollimation of the light that has passed through the micropipette. This recollimated light is then received by a detector in the spectrophotometer for further spectroanalysis. It will be appreciated by the skilled artisan that, depending on the wavelength of the light, the receiving lens and the directing lens may be made of quartz, glass, sapphire, fused silicon or any other appropriate light transmitting material.
The temperature control feature of the micropipette adaptor includes a metal base member sandwiched between two plastic material layers. The metal base member has an orifice adapted to hold a micropipette containing a sample material solution for analysis. The plastic material layers each have a lens mounted on either side of a passageway in the center of the base member, which forms the optical system to focus the collimated light through the sample in the micropipette. A resistive heater wire is held between the metal base and one of plastic layers, in position against the surface of the metal base, to transfer heat from the heater wire to the metal base. The metal base includes a thermocouple which provides a signal representative of the temperature of the metal base, which allows the temperature of the sample material to be monitored. The micropipette of sample material is inserted into the orifice of the metal base and heated to a desired temperature. The metal base acts as a thermal reservoir for heating the sample, in addition to maintaining the alignment between the micropipette sample and the focusing lens. By choosing a base material of high thermal conductivity, such as copper, brass, or aluminum, the temperature of the sample in the micropipette can be increased quickly and maintained at a desired level.
The micropipette adaptor further includes a temperature feedback control system to maintain the sample at any desired temperature. The control system comprises an analog thermocouple gauge display driver, a digital panel meter, a comparator, a set point programmer, and a transistor heater driver. Also provided is an external input to allow programming of desired temperature variations over time.
As contemplated by the present invention, the adaptor is intended for use with very small micropipettes. For example, it is within the contemplation of the present invention that a micropipette having a capillary tube with a lumen which is approximately half a millimeter (0.5 mm) in diameter can be effectively used with the adaptor disclosed herein. Even so, it will be appreciated by the skilled artisan that pipettes of various sizes may be used. Furthermore, it is to be appreciated that the light wavelengths which are useful with the adaptor of the present invention need not necessarily be limited to the visual and ultraviolet ranges.
The novel features of this invention, as well as the invention itself, both as to its structure and its operation, will be best understood from the accompanying drawings, taken in conjunction with the accompanying description, in which similar reference characters refer to similar parts, and in which:
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a schematic diagram showing the micropipette adaptor in its operative relationship with elements of a spectrophotometer;
FIG. 2 is a perspective view of the micropipette adaptor with selected elements shown in phantom and portions broken away for clarity;
FIG. 3 is a cross-sectional view of the micropipette adaptor as seen along the line 3--3 in FIG. 2;
FIG. 4 is a cross-sectional view of the micropipette adaptor as seen along the line 4--4 in FIG. 2;
FIG. 5 is a perspective view of a micropipette adaptor having temperature control in accordance with the present invention;
FIG. 6 is a top view of the adaptor with temperature control of FIG. 5;
FIG. 7 is a cross-sectional view of the adaptor with temperature control as seen along line 7--7 of FIG. 6;
FIG. 8 is a cross-sectional view of the adaptor with temperature control as seen along the line 8--8 of FIG. 6; and
FIG. 9 is a schematic diagram of a feedback control system used in conjunction with the adaptor of FIG. 5 in accordance with the present invention.
DESCRIPTION OF THE PREFERRED EMBODIMENT
Referring initially to FIG. 1, the micropipette adaptor for spectrophotometers in accordance with the present invention is schematically shown in its operative environment and is designated 10. As shown, adaptor 10 is positioned for operative engagement with a spectrophotometer 12 and, specifically, is positioned between a light source 14 and a detector 16. As so positioned, an input beam of collimated light 18, having an intensity I o (λ), is directed from the light source 14 toward the adaptor 10. In a manner to be subsequently disclosed, adaptor 10 focuses the beam 18 of collimated light onto a micropipette 20 which is held by the adaptor 10. Adaptor 10 then recollimates this light into an output light beam 22 which has an intensity of I t (λ). As will be appreciated by the skilled artisan, the difference between I o (λ) and I t (λ) is indicative of the light absorption characteristics of the sample material held in micropipette 22 and, hence, is an indication of the composition of the sample material.
The construction of adaptor 10 will, perhaps, be best seen by reference to FIG. 2 wherein it is shown that adaptor 10 comprises a base member 24 which is sandwiched between a resilient member 26 and a resilient member 28. Respectively positioned against resilient members 26 and 28 and opposite base member 24 are holders 30 and 32. Preferably, base member 24 and the holders 30 and 32 are made of a rigid material, such as black delrin plastic, while the resilient members 26 and 28 are made of an elastomeric material such as rubber or foam plastic. For purposes of the present invention, holder 30 is formed with an opening 34 as shown in FIG. 2, and base member 24, resilient members 26, 28 and holder 32 are each formed with openings (not shown in FIG. 2) which are aligned with opening 34 to establish a pathway 44 which allows light to pass through adaptor 10.
Referring now to FIG. 3, it will be seen that base member 24 is formed with an opening 36 which, as indicated above, is positioned in alignment with opening 34 of holder 30. Further, base member 24 is shown formed with a hole 38 and a conical-shaped well 40 which are positioned across the opening 36 from each other. Specifically, hole 38 and conical well 40 respectively receive portion of micropipette 20 to hold the micropipette 20 in place within and across the opening 36. A bushing 42, which is appropriately sized to receive micropipette 20, may be positioned in hole 38 to securely hold the micropipette on adaptor 10.
As best seen in FIG. 4, the base member 24, together with its adjacent resilient members 26, 28 and the holders 30, 32 are all positioned with their respective openings aligned to create a pathway 44 through adaptor 10 along which light can shine. FIG. 4 also shows that a lens 46 is positioned in pathway 44. Specifically, lens 46 is attached or mounted on holder 30 by any means well known in the pertinent art, such as by gluing or solvent bonding. Further, lens 46 may be mounted on holder 30 by a frictional snap-in configuration or held thereon by set screws (not shown). Similarly, a lens 48 is attached or mounted on holder 32 and is positioned in the pathway 44 substantially as shown. For purposes of the present invention, it is preferable that the lenses 46, 48 be cylindrical. This is so in order for the lens 46 (the directing lens) to linearly focus input light beam 18 onto a line which can be positioned along the longitudinal axis of micropipette 20. Further, a cylindrical shape for lens 48 (the receiving lens) is also preferable in order for the linearly focused input light beam 18 to be recollimated as output light beam 22. Preferably, both cylindrical lens 46 and cylindrical lens 48 are made of a quartz material which permits use of either visible or ultraviolet light.
As will be appreciated by the skilled artisan, input light beam 18 can be precisely focused along the longitudinal axis of micropipette 20 by appropriately moving lens 46 in a direction along the pathway 44. In order to linearly focus input light beam 18 and obtain the highest intensity I o (λ) for the light which is incident on the sample material being held in micropipette 20, the holder 30 on which lens 46 is mounted, can be moved relative to the base member 24 on which micropipette 20 is mounted. As seen in FIG. 4, when lens 46 is properly positioned, input beam 18 will be focused into a line which is coincident with the center of lumen 50 of micropipette 20. Following well known optical principles, light will emerge from micropipette 20 in a predictable fashion. Consequently, cylindrical lens 48 (the receiving lens) can receive this emerging light and recollimate the light into the output light beam 22. To accomplish this, lens 48 is mounted on holder 32 and is movable therewith relative to base member 24. As will be readily appreciated, the resilient members 26, 28 permit selective relative movement between base member 24 and the respective holders 30, 32. At the same time, resilient members 26, 28 provide a support for maintaining the relative positions of these components when they are not being moved. It is possible, however, to completely eliminate the resilient members 26, 28. Manufacturing tolerances may suffice to properly position lens 46 on holder 30 without any further adjustment necessary to predictably focus light from the lens 46 along the interior lumen of micropipette 20. Similarly, lens 48 may be mounted on holder 32 and positioned relative to base member 24 without the need for subsequent adjustments.
The mechanism for moving holders 30, 32 relative to base member 24 will be best seen by referring to FIG. 2 wherein a screw 52 is shown extending through holder 30 and resilient member 26 for threadable connection with base member 24. The screws 54 and 56 likewise connect holder 30 with base member 24. Similarly, screws (of which the screw 58 shown in phantom is exemplary) connect holder 32 with base member 24. In each case, the screws 52, 54, 56, 58 (and others not shown) can be individually rotated to independently move the holders 30, 32 relative to the base member 24. Consequently, this moves lenses 46, 48 relative to micropipette 20.
As intended for the present invention, movement of cylindrical lens 46 relative to micropipette 20 is accomplished to linearly focus input light beam 18 along the axis of micropipette 20. This increases the intensity I o (λ) of the light which is incident on the sample material held in solution in lumen 50 of micropipette 20. Similarly, movement of the cylindrical lens 48 relative to micropipette 20 is accomplished in order to recollimate the light which emerges from micropipette 20 for easier analysis of its intensity I t (λ) by the detector 16.
Referring now to the embodiment of a micropipette adaptor as shown in FIGS. 5-9, there is shown an adaptor with temperature control which is generally designated 100. The adaptor 100 can generally be thought of as being used in place of adaptor 10 earlier described. In particular, adaptor 100 comprises a base member 110 sandwiched between a layer 112 and a layer 114. Base member 110 is made of a metal material which has high thermal conductivity and is easy to machine, such as copper, brass or aluminum. Layers 112, 114 are made of a different material, preferably nonmetal, such as delrin plastic, which are attached, such as by bonding, to each side of base member 110. The overall dimensions of the adaptor are such that it easily fits into a conventional sample holder slot of a commercially available spectrophotometer. In the embodiment shown, the dimensions of layers 112 and 114 are approximately 12.5 millimeters in width, and approximately 38 millimeters in height. Base member 110 is slightly smaller in these dimensions, i.e. width and height, to prevent heat loss by contact of the base member 110 with the spectrophotometer. Lenses 116 and 118 are mounted in layers 112, 114 respectively, similar to mounting of lenses 46, 48 as earlier shown in FIG. 4.
Base member 110 has an orifice 120 in the top thereof. Orifice 120 is generally cylindrical and vertically oriented in base member 110 for receiving a micropipette containing sample material. Orifice 120 has a top 122 and walls 124 adapted to the shape of the micropipette. Base member 110 has a passageway 126, into which orifice 120 opens at orifice bottom 128. A micropipette which is inserted into orifice 120 then may extend through orifice 120 down into passageway 126. Then a collimated light beam, such as light beam 18 of FIG. 4, can be passed through the sample. Base member 110 further includes a thermocouple 130 for measuring the temperature of base member 110. Thermocouple 130 is preferably a chromel-alumel thermocouple having wires 132, 134, which provide a temperature signal.
Quartz lenses 118, 116 may be held in place with teflon tipped set screws inserted into set screw slots 136. A heater wire 138 is positioned and held between layer 112 and base member 110. It is routed around the perimeter of passageway 126 and is positioned against base member 110 being held firmly in place by layer 112. Heater wire 138 is preferably made of manganin, five thousandths (0.005) inches in diameter. It will be appreciated, however, that tungsten or other resistive type wires are also appropriate for use as heater wire 138. Wire 138 is connected to a direct current power supply (not shown) for heating the wire, with typical values for the output of the supply being from five tenths to one (0.5-1.0) amperes at two to four (2-4) volts.
Thus, the adaptor 100 serves at least two functions, namely maintaining the alignment between the sample and the focusing lenses, and further acting as a thermal reservoir. By applying the proper amount of voltage and power levels to heater wire 138, the base member 110 can be heated. This results in heating of the sample which is contained in a micropipette inserted in orifice 120 to the desired temperature. It has been found, for example, that use of four (4) watts of power may be used to obtain temperatures of a micropipette sample of eighty to one hundred degrees (80°-100° C).
There is further shown in FIG. 9 a feedback control system generally indicated as 140 for operably controlling the temperature of adaptor 100. In particular, system 140 comprises a thermocouple circuit 142 connected to thermocouple outputs 132, 134 from base member 110. The temperature output of thermocouple circuit 142 may be displayed by digital panel meter 144. In addition, output 146 of thermocouple circuit 142 is connected to a comparator 148. Also connected as an input to comparator 148 is a set point input signal line 150. The actual measured thermocouple output signal 146 is compared to the set point 150 at comparator 148. Set point signal information 150 can be alternately provided via switch 152 between a signal generated by a temperature set point potentiometer 154, or a signal generated by an analog temperature programming input device 156. Potentiometer 154 can be set by selecting a desired voltage which corresponds to the desired temperature at which the base member is to be maintained. On the other hand, the temperature programming input 156 provides an external input to provide a varying time/temperature wave form using an analog signal. Thus, the set point signal 150 can be programmed to maintain a constant temperature based on the potentiometer 154 setting, or specific temperatures for predetermined periods of time based on the programming input 156. Based upon the comparison between the set point signal 150 and the actual measured temperature signal 146, the comparator generates an "on" or "off" signal 158. This activates or deactivates a transistor heater driver 160. Driver 160 sends a current through heater wire 138 to heat up base member 110 when it is activated, or cuts off the current to allow base member 110 to cool down when it is deactivated.
In one experiment utilizing adaptor 100, the absorption of light at 260 nanometers of DNA was observed and measured as it was being denatured at a temperature of between seventy and eighty degrees centigrade (70°-80° C.). Since double-stranded DNA denatures at these temperatures, it was found that the absorption at 260 nanometers increased by approximately thirty-seven percent (37%). The melting temperature, or denaturing temperature, is approximately eighty-three degrees (83°). Thus, by ramping the temperature rapidly by applying one ampere to the adaptor 100, the temperature was allowed to ramp upward after reaching seventy degrees centigrade (70° C.), which is the temperature at which DNA should begin to denature. Using the adaptor 100 of the present invention took approximately ten minutes to reach eighty degrees centigrade (80° C.) from twenty-three degrees centigrade (23° C.). The absorbance of the sample used, namely Lambda DNA markers, at a concentration of 675 micrograms per milliter, changed from 0.589 before denaturing to 0.737 after denaturing, or changed approximately twenty-five percent (25%). Thus, the usefulness of the present invention can readily be appreciated by those skilled in the art.
While the particular micropipette adaptor for spectrophotometers with temperature control as herein shown and disclosed in detail is fully capable of obtaining the objects and providing the advantages herein before stated, it is to be understood that it is merely illustrative of the presently preferred embodiments of the invention and that no limitations are intended to the details of construction or design herein shown other than as defined in the appended claims. | A temperature-controlled micropipette adaptor includes a metal base sandwiched between two plastic layers. The metal base has an orifice to hold a micropipette. The plastic layers hold lenses in alignment for spectrophometric measurements of a sample contained in a micropipette inserted into the orifice. A resistive heater wire is held between the metal base and the plastic layer to transfer heat from the heater wire to the metal base and thus to the micropipette sample. A thermocouple is attached to the metal layer to monitor temperature changes. A feedback control system is coupled to the device for monitoring and programmably controlling changes in temperature of the heated sample over time. | 1 |
CROSS REFERENCE TO RELATED APPLICATIONS
Not applicable.
STATEMENT REGARDING FEDERALLY SPONSORED RESEARCH OR DEVELOPMENT
Not applicable.
REFERENCE TO SEQUENCE LISTING, A TABLE, OR COMPUTER PROGRAM LISTING
Not applicable.
BACKGROUND OF THE INVENTION
(1) Field of the Invention
This invention is directed to vertical stack (2,4,6 high) rolling mill stands used to roll out flat rolled metal products, particularly metals such as steel and aluminum, to a reduced gauge using a pair of work rolls that are between intermediate rolls, which in turn are between backup rolls. Vertical stack rolling mill stands include work rolls, and optionally, intermediate rolls and backup rolls. It is also directed to mills where the rolls are used for controlling the shape of the metal during rolling by applying significant bending forces on the roll ends.
(2) Description of Related Art
Currently, in the art, there is a need for improvement in roll bending design so that the bearing and hydraulic cylinder maintenance is lowered for a vertical stack rolling mill. Process needs for roll bending have caused higher bending forces with subsequent higher roll end deflections. Also, operating practices have changed which have caused the work rolls and intermediate rolls to be shifted perpendicular to the rolling direction for improved shape and edge performance, and these practices have raised important issues with regard to the placement of end bending forces. Current designs for work roll and intermediate roll chocks generally constrain them to vertical movement which causes the bearing raceways to pinch, gouge, or otherwise behave in ways that reduce the bearing life since the resultant force is not at the bearing center when the roll is shifted. There is also higher roll end maintenance when the ends have to be re-machined. Also, some current designs apply hydraulic forces in the positive bending direction only, which is less desirable.
Additionally, there is the need to provide for a rapid method of inserting rolls into the mill, which will also accommodate the need for a roll to be driven, but allow the use of a shifting mechanism to be the means by which the rolls are kept in the mill. In a typical, non-shifting mill arrangement, keeper plates are used to ‘lock in’ rolls into the mill window. In a shifting roll arrangement, it is important that the rolls maintain their engagement in the drive system at all times, and that the shifted position of the rolls is highly positive and precise.
Improved designs for inserting rolls into the mill without the need for electrically actuated clamping or lock in plates are of benefit if the rolls utilize a mechanical system rigid enough to hold the rolls in place during the rolling operation. There are production benefits to locking in rolls mechanically, rather than by a sequence of hydraulic/electronic actuators, due to the need to verify actual lock in and motion to ensure successful operation.
Others have worked on rolling mill designs. U.S. Pat. No. 4,537,057, for example, describes a six high rolling mill and certain features to reduce edge cracks in the sheet during rolling. FIGS. 4 and 5 in particular show improved mill window equipment and methods to apply rolling force to the metal strip work piece. The disclosed method, however, requires a large number of hydraulic cylinders to create the roll bending effect in the work roll and intermediate rolls, which causes maintenance issues and complicated control/operational problems. The bending effect ends up being applied to the work roll chocks less effectively, by use of a machined area in the chocks in a way that creates un-needed high stress points. The end result is that the work roll and intermediate roll chocks require a lot of machining, and therefore a high expense due to the complicated geometry required. Finally, the roll changing method is not described as to efficiency. Another patent, U.S. Pat. No. 7,004,002 has similar issues.
U.S. Pat. No. 4,744,235 incorporates push/pull hydraulic cylinders to provide backup roll and work roll bending forces. It also includes compact designs for the work roll and intermediate roll chocks. It includes complicated horizontal hydraulic cylinders to steady and clamp the work rolls into position which adds to maintenance and complicates the operation of the overall system. The roll bending design causes significant moments in the roll chocks as well as end rotations. There is no allowance for this in the design causing the hydraulic cylinders to carry the resultant stresses and therefore incur significant maintenance.
U.S. Pat. No. 7,086,264 describes a six high mill stand with rolls that are inserted into the mill with a release able connection using a clutch type arrangement. This type of arrangement is suitable for a rotating connection, but not adequate for a rapid connection where the rolls shift perpendicular to the rolling direction.
U.S. Pat. No. 4,369,646 describes a hydraulic keeper system where shiftable rolls are kept in a mill stand. However, the hydraulic means of actuation to keep the rolls connected to the shifting mechanism is a less desirable method due to the need for portable hydraulics, hoses, maintenance, etc.
These designs and attempts by others are lacking in important technical aspects, especially in light of current trends in the industry, and improvements in mill design to address these issues is greatly desirable.
BRIEF SUMMARY OF THE INVENTION
The present invention incorporates an integrated hydraulic cylinder design that improves bearing life by allowing the roll chock to rotate along with the end shaft of the roll. Also, the design includes improvements in bending cylinder design by utilizing multiple cylinders on the end, so that the center of force application on the end is neutral and applied to the roll end with a torque that allows the bearing to naturally rotate. The design further includes an improved cylinder design which allows use of a standardized double acting cylinder which is bolted into the project block on the window housing, and therefore allows for rapid and easy maintenance in the event of a problem.
BRIEF DESCRIPTION OF THE SEVERAL VIEWS OF THE DRAWING(S)
FIG. 1A-1B show an elevated view of the mill window design for a six high and a four high rolling mill stand.
FIGS. 2A-2E illustrate roll shifting and the advantage of the invention by the use of dual inline bending cylinders, including chock rocking to reduce stress concentration.
FIGS. 3A-3B illustrate how the bending block incorporates design features which allow for small rotations.
FIG. 3C shows a free body diagram of a Bending Block illustrating how the Guide Pins counter balance the applied bending force.
FIG. 4-5 illustrate how the hydraulic circuit is designed to provide good bearing life by balancing the placement of the bending force on the ends of the shifted roll.
FIG. 6A-6B illustrate a latching in mechanism which allow for the work roll or intermediate rolls to be readily inserted into the mill.
FIGS. 6C-6E illustrate how the latching mechanism is designed to release the work roll or and intermediate rolls from the mill.
DETAILED DESCRIPTION OF THE INVENTION
FIG. 1 is one embodiment of the mill window as conceived in the present invention. For convenience, Table 1 lists the features in the mill window as particularly directed to the roll bending. Other features of the mill are not shown.
TABLE 1
FIG. 1
101a, b
Back Up Roll (Lower and Upper)
102a, b
Intermediate Roll (Lower and Upper)
103a, b
Work Roll (Lower and Upper)
104a, b
Left Intermediate Roll Bending Block (Lower and Upper)
105a, b
Left Work Roll Bending Block (Lower and Upper)
107a, b
Right Intermediate Roll Bending Block (Lower and Upper)
106a, b
Right Work Roll Bending Block (Lower and Upper)
110a, b
Left Lower Intermediate Roll Bending Block Cylinders
111a, b
Left Lower Work Roll Bending Block cylinders
112a, b
Left Upper Work Roll Bending Block Cylinders
113a, b
Left Upper Intermediate Roll Bending Block Cylinders
114a, b
Right Lower Intermediate Roll Bending Block Cylinders
115a, b
Right Lower Work Roll Bending Block Cylinders
116a, b
Right Upper Work Roll Bending Block Cylinders
117a, b
Right Upper Intermediate Roll Bending Block Cylinders
120
Left Project Block
121
Right Project Block
122
Mill Housing
123
Flat Rolled Metal Product, Rolling Passline
124
Cylinder Housing (typical example)
125
Bolts
130a, b
Intermediate Roll Chocks (Lower and Upper)
131a, b
Work Roll Chocks (Lower and Upper)
In FIG. 1A , the backup rolls 101 a,b are shown on the left and right side of the mill window elevation view in their maximum and minimum diameter respectively. This is a common way of illustrating a mill window. As is seen, the intermediate rolls 102 a,b and work rolls 103 a,b are also similarly shown. This provides perspective on typical maximum motions of the mill window equipment in normal operation. For a roll change, the pistons will move more to create clearance between the rolls. FIG. 1A is only one embodiment of the invention; other arrangements could be adapted and used, such as a two high (i.e. two work rolls) or a four high (two work rolls and two backup rolls).
The work roll ends have bearings which are inside work roll chocks 131 a,b . Similarly, the intermediate rolls have chocks 130 a,b as well. In this design, bending blocks 104 a,b , 105 a,b , 106 a,b , and 107 a,b , also called bending project blocks or chock holding blocks, are used to guide the work roll or intermediate rolls into the mill as well as provide the force needed to bend the rolls for roll crown management and for strip shape control. When a roll is bent in a way that causes the roll to appear thicker in the middle, it is called ‘crown in’ or positive bending. This would occur when the ends of the upper work roll, for example, are pushed upwardly and the middle of the roll bows into the strip. The opposite way of bending it is called ‘crown out’ or negative bending.
The force needed to create roll bending effects in the present invention is developed by hydraulic cylinders that are rigidly attached to project blocks 120 , 121 that are, in turn, attached to the mill housing 122 . The roll bending hydraulic cylinders are explained further in FIG. 2 . There are sixteen cylinders per mill side, or a total of thirty two per mill stand. The Work roll lower left bending block cylinders 111 a,b , for example, on the operator side of the mill, comprise two cylinders in line, and attached to the mill left project block 120 . They are used to push the lower work roll bending block 105 a up and down to provide both crown out and crown in roll bending respectively.
Similarly, the roll bending hydraulic cylinders 110 a,b , 112 a,b , and 113 a,b are also attached to the left project block 120 . They are used to push the lower intermediate roll bending block, upper work roll bending block, and upper intermediate roll bending block up and down to provide crown management. Similarly, the roll bending hydraulic cylinders 114 a,b , 117 a,b , 115 a,b , and 116 a,b are also attached to the right project block 121 . They provide lower/upper intermediate roll bending block movement, and lower/upper work roll bending block movement respectively.
The force needed to create roll bending effects in the present invention is developed by hydraulic cylinders that are designed with maintenance in mind. In one embodiment, the cylinders are double rod, and designed in a manner that allows for easy maintenance and replacement by utilizing a standard cylinder or a modularized cylinder design. This provides for rapid replacement and repair as opposed to custom design and repair where in place repair is complicated. Methods of attachment to the project block, consider such things as power tools and accessibility. The bending block design is such that the cylinders can be unbolted, removed, and replaced easily.
A typical cylinder housing 124 is rigidly attached to the project block 120 , though the method of attaching is not illustrated. A mechanical attaching method is preferred, such as by bolts or a hardware method.
The project blocks 120 , 121 are rigidly attached to the mill housing 122 in this illustration by a bolt method 125 , though other rigid methods could equally be used. The flat metal product 123 , such as steel or aluminum, is aligned to the rolling mill centerline, i.e. strip passline, or rolling passline, and is defined location (typically a specific elevation or a small range of elevations) for a particular mill housing pair 122 . Typically, only one housing is illustrated and a second mill housing on the other side of the rolling passline is implied by the illustration for a rolling mill stand unless otherwise explained. Both mill housings for a rolling stand are typically set on a rigid foundation.
Similarly, FIG. 1B shows a four high mill stand arrangement with a pair of work rolls and supporting backup rolls. The intermediate rolls and back up rolls in FIG. 1A (and backup rolls in FIG. 1 b ) could also be called support (or supporting) rolls. The associated equipment such as chocks, etc. are called associated supporting chocks, etc.
FIGS. 2A-2D illustrate a shifting work roll 201 a - d , but would also illustrate a shifting intermediate roll. In FIG. 2A the forces created by the bending cylinders, F 1 and F 2 are shown through the bending blocks 202 a , 203 a , which result in the forces and applied torsion in FIG. 2B . The hydraulic cylinders are interconnected by piping in a manner so that the forces F 1 and F 2 are created as shown (and will be discussed in FIG. 4 ). In consideration of the bending and deflection of the ends of the actual work roll, the two torsions shown in FIG. 2B will actually improve the bearing mounting on the work roll end, and avoid issues with higher maintenance caused by the shifting work roll. Also, the torsion will also counteract the shifting location of the applied overall bending force location.
Similarly, FIGS. 2C , 2 D illustrate a work roll that has shifted somewhat to the left of the mill center. Even though the roll is close to center, the same issue of roll bearing and mounting still applies, even if the torsion amount is relatively smaller.
FIG. 2E shows how the bending moments affect the rotation of the end bearing blocks for a crown in bending force when the roll is above the metal strip (in an exaggerated illustration). The applied bending force is ultimately resisted by the inherent stiffness of the roll itself. As shown, the chocks ‘rock’, that is, they are allowed to rotate slightly with the roll ends to avoid bearing stress concentrations.
FIGS. 3A-3B illustrates a method where the work roll chock 301 a,b (or alternately, intermediate roll chock) along with a right bending block 303 a,b and left bending block 302 a,b , are designed to provide a small amount of rotational movement with respect to the mill housing face. To this end, Guide Pins 304 a,b are rigidly attached to the bending blocks (along with an alternative guide plate 305 as illustrated in FIG. 3A only) to allow the bending block to move vertically, but allow rotational freedom of movement so that the work roll chock 301 a,b rotates when the bending force is applied, which in turn, will allow the work roll bearing (not shown) to rotate with the bending work roll end shaft. Matching machined grooves for the guide pins are added to the mill housing faces, as well as a machined surface for the guide plate with suitable vertical side plates along the edges of the guide plate to capture it next to the mill housing face. This design is only one embodiment. The Guide Pins 304 a,b (and guide plate 305 ) might be a variety of geometric shapes, or, might be a different number such as a minimum of three to a large number of pins, such as sixteen so as to allow an even distribution of surface stress.
In one embodiment, the interface between the work roll chock and the bending blocks is a dovetail arrangement 306 a,b and a particular dovetail design may be adapted as is suitable to the task. Such interface designs include standard rectangular to a base with sides angled up to 15 degrees.
FIG. 3C shows a free body diagram of a Bending Block to illustrate how the Guide Pins counter balance the applied bending force. Bending Cylinders (not shown) oriented vertically apply bending forces 310 a,b to the Bending Block (in this example downward direction). The force is applied to the Work Roll Chock 314 along an edge of the Bending Block resulting in an edge pressure 313 . These forces create a moment which is counter balanced by the Upper Guide Pin forces 312 a,b and lower Guide Pin Forces 311 a,b . A force applied to the Guide Pins may be in either direction due to the method by which the Guide Pins are held against the project block—a slot with a groove, which allows the head of the pin to carry either a tensile or a compressive load. The slot is wide enough to allow the bending block to rotate along with the work roll chock rotation due to roll end deflection, but the slot is narrow enough to keep the head of the Guide Pins captured.
FIGS. 4 and 5 illustrate an abbreviated piping schematic of the hydraulic pressure system that provides the needed pressure in the bending cylinders for the work roll and intermediate rolls. As seen in FIG. 4 , the pressure P 1 + is commonly interconnected by piping to the cylinders as shown in a manner that will develop the forces as previously illustrated in FIG. 2 . The applied bending force between the left and right sides as viewing the mill window is carried out by repetition of the pattern shown in FIG. 4 . The bending pressure P 2 +, is applied similarly to the positive bending pressure P 1 + as shown. Similarly, the negative bending pressures P 1 −, and P 2 −, are applied as illustrated. The piping schematic illustrates the odd-even counting method of connecting the cylinders together, where the cylinders 1 and 3 (when counting in line from the left) are connected, and the cylinders 2 and 4 are connected together. The net result is that the odd numbered bending cylinders in the bending blocks are operated with a common pressure (and also the even numbered cylinders). By similarly designing bending block cylinders, the applied forces are the same. The cylinders in the bending blocks are set at a predetermined distance apart based on rolling mill parameters, such as the rolling width, gauge, material to be rolled, work roll diameter, intermediate roll diameter, and roll shifting dimensions.
As seen in FIG. 5 , the pressures P 3 +/− and P 4 +/− are interconnected to the bending cylinders as shown in a manner similar to FIG. 4 , so that forces will develop in the manner as previously illustrated in FIG. 2 . It should be noted that the hydraulic pressures for the intermediate bending block cylinders are connected separately from the work roll system sufficiently so as to allow the intermediate rolls to develop different pressures and bending forces.
FIGS. 6A-6E show a latching method whereby a roll is easily and readily inserted into the mill, and also withdrawn when it is time to pull the roll out of service. The method applies to either a work roll or intermediate roll. This latching system is particularly useful for rolling mills where the rolls are shifted for the rolling operation, and devices like keeper plates have little use for containing the rolls in place.
In FIG. 6A , a roll 606 with associated chock 605 , is being pushed into the mill. The equipment being used to latch the roll into its operating position includes: a hydraulic cylinder 601 , C-Frame stop blocks 602 , a C-Frame 603 , Latch frames 604 a,b , and Latch Frame Open Block 607 . These elements are used to capture the roll chock and hold it for the rolling operation. The C-Frame 603 is already fully retracted against the stop blocks 602 by use of the hydraulic cylinder 601 .
In FIG. 6B , the roll is pushed by the roll changer further against the latch frames, which rotate due to the end of the roll contact, and this causes the latch frames to rotate enough to lock one protrusion into a machined groove in the roll chock. This allows the latch frame to capture the chock, and, only allows the chock to leave when the hydraulic cylinder is actuated. This is also the minimum shifting position.
In FIG. 6C , the normal operational position of the work roll and C-Frame is shown. The work roll shifts horizontally in normal operation and the C-Frame will shift along with it because it is engaged/latched. To remove the roll and chocks, the hydraulic cylinder 601 is activated. In FIG. 6D , the C-Frame is additionally pushed by the hydraulic cylinder until the latch frame is pressed into the latch frame stop block. Additional push will generate a reaction from the stopper 607 , which will introduce a large moment to open the latch frame. This mechanism releases the roll chocks from the latch frame by causing the latch frames to rotate as illustrated in FIG. 6E . FIGS. 6C-6E shows the cylinder pushing the latching frame to open. Alternately, the cylinder is an auxiliary device which allows the roll changer to pull out the roll and to open the latching frame.
This method applies to individual non-driven rolls, but could easily be adapted to a driven roll (i.e. motor with coupling on the end of the roll), by varying the geometry of the C-Frame in three dimensional space to provide room for the motor shaft and coupling, and alternately, any mill stand gearing. Another possibility is to provide a shaft connection between the Latch Frames and C-Frame rather than a simple pivot point so as to allow the C-Frame and Latch Frames to be at different elevations. Another method is to make the Latch Frame three dimensional so that the groove capture comes from extended arms from a higher (or lower) elevation. The latching mechanism is also locatable to the operator side of the mill, that is, the opposite side of the mill from where the motor/coupling are.
While various embodiments of the present invention have been described, the invention may be modified and adapted to various operational methods to those skilled in the art. Therefore, this invention is not limited to the description and figure shown herein, and includes all such embodiments, changes, and modifications that are encompassed by the scope of the claims. | An improved roll bending system is described for the work rolls and intermediate rolls in a six high mill. New bending blocks apply improved roll bending forces to the roll chocks, and additionally, are designed to move vertically and rotate, which provide important benefits to maintenance and enhance the rolling operation. Additionally, important related details to the mill operation and bending blocks provide operational improvements during roll changing. | 1 |
BACKGROUND OF THE INVENTION
This invention relates to an apparatus for attaching implements to earth moving vehicles.
Heretofore attaching an implement to or replacing it from an earth moving vehicle required complicated and time consuming procedures. For example, when it is required to replace an implement from the vehicle, it is generally necessary to move the implement by means of a crane, etc. in order to align pin holes of the implement with those of lift arms of the vehicle. After aligning pin holes, pins are inserted therethrough so as to attach the implement to the vehicle. It is difficult to align pin holes formed in the implement and the lift arms of the vehicle by moving the vehicle itself without moving the implement by the crane or the like.
SUMMARY OF THE INVENTION
It is, therefore, an object of the present invention to provide an apparatus for attaching implements to an earth moving vehicle wherein replacement of the implements can be carried out easily.
Another object of the present invention is to provide an apparatus for attaching implements to an earth moving vehicle wherein replacement of the implements can be carried out from the driver's cab.
According to one aspect of the present invention, there is provided an apparatus for attaching implements to an earth moving vehicle, comprising a pair of lift arms for lifting the implement, a pair of tilt rods for effecting tilting motion of the implement, a pair of lower couplers pivotally connected to said lift arms at one end thereof, and a pair of upper couplers pivotally connected to said pair of tilt rods. Said upper couplers are pivotally connected with said lower couplers. A pair of connecting beams are provided so as to interconnect said pair of lower couplers and said pair of upper couplers, respectively. Said connecting beams are adapted to engage with C-shaped hooks fixedly secured to the rear surface of the implement.
Lock means is provided either on said upper couplers or said lower couplers so as to block pivotal movement of said upper couplers relative to said lower couplers when said couplers are engaged with the hooks of the implement.
Lock releasing means may be provided on said lift arms of the vehicle so as to release said lock means from the driver's cab when it becomes necessary.
Other objects, features and advantages of the present invention will be readily apparent from the following description taken in conjunction with the accompanying drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a perspective view of the present invention;
FIG. 2 is a partial back elevational view of FIG. 1;
FIG. 3 is a cross-sectional view taken along the line III--III in FIG. 2;
FIG. 4 is a front elevational view partially in cross-section of lower couplers according to the present invention;
FIG. 5 is a side elevational view of FIG. 4;
FIG. 6 is similar to FIG. 4 but showing upper couplers according to the present invention;
FIG. 7 is a side elevational view of FIG. 6;
FIG. 8 is an enlarged cross-sectional view of lock means according to the present invention;
FIG. 9 is a front elevational view of FIG. 8;
FIG. 10 is a plan view thereof;
FIG. 11 is a perspective view of an implement according to the present invention;
FIG. 12-I to FIG. 12-V are explanational views showing procedures for removing the implement from the vehicle according to the present invention;
FIG. 13 is a side elevational view partially in cross-section of lock releasing means according to the present invention; and
FIG. 14 is a plan view partially in cross-section of FIG. 13.
DETAILED DESCRIPTION OF THE INVENTION
The present invention will now be described in detail below with reference to drawings. Reference numeral 1 denotes a lower coupler having a beam 2. Fixedly secured to both ends of the beam 2 are inner plates 3. Referring to FIG. 4, each of the inner plate 3 has a pin hole 4 formed in the upper part thereof. Further, the upper edge of the inner plate is formed in a circular cam portion 5 defined about the pin hole 4. Each of the inner plate 3 is connected through a connecting plate 6 with an outer plate 7 disposed in parallel therewith. The outer plate 7 has a pin hole 4' formed in the upper part thereof. Further, the outer plate 7 has a stopper 8 formed in the upper edge portion thereof. The inner and outer plates 3 and 7 have pin holes 9 and 9' formed in the lower parts thereof, respectively.
Connected to the lower coupler 1 having pins 10 inserted into the pin holes 9 and 9' are a pair of lift arms 11 of a vehicle.
Reference numeral 12 denotes an upper coupler having a beam 13. Fixedly secured to both ends of the beam 13 are inner plates 14. Each of the inner plate 14 is fixedly secured through a connecting plate 15 to an outer plate 16 disposed in parallel therewith. Further, each of the inner and outer plates 14 and 16 has pin holes 17, 17' and 18, 18' formed in the upper and lower parts thereof, respectively. (refer to FIG. 6).
The upper part of the lower coupler 1 is inserted into the lower part of the upper coupler 12. The upper and lower couplers 12 and 1 are interconnected by means of pins 19 each being inserted into the pin holes 18, 18', 9 and 9'. The stopper 8 is adapted to contact with the connecting plate 15 when the upper coupler 12 is aligned with the lower coupler 1.
Connected to the upper coupler 12 having pins 20 inserted into the pin holes 17 and 17' are tilt rods 21 of the vehicle.
Referring to FIG. 8, the inner plate 14 of the upper coupler 12 have a lock means 22 fixedly secured thereto. The lock means 22 comprises a block 23 fixedly secured to the inner plate 14. The block 23 has vertically extending holes 24 and 25 formed therein. Inserted into the hole 24 is a lock pin 26 having a spring seat 26 formed thereon. The lock pin 26 has a notch 28 formed in the upper end thereof, and also has a pin 29 attached to the lower part thereof. The block 23 has a spring retainer plate 30 fixedly secured thereto, and a spring 31 is interposed between the spring retainer plate 30 and the spring seat 27. Inserted into the hole 25 is a rod 32 urged downwardly by the biasing force of a spring 33. A yoke 34 is attached to the upper end of the rod 32. The block 23 has in the upper part thereof a lever 35 pivotally mounted by means of a pin 36. The leading end of the lever 35 is connected through a pin 37 to the yoke 34. A claw 38 is fitted to the lever 35.
In FIG. 11, reference numeral 39 denotes an implement comprising a bucket. The implement 39 has a pair of C-shaped hooks 40 fixedly secured to the rear surface thereof.
The implement 39 is fitted to the lift arms 11 by allowing the beam 13 of the upper coupler 12 to engage with upper portions 40a of the hooks 40 and the beam 2 of the lower coupler 1 to engage with the lower portions 40b of the hooks 40. In this case, the lock pin 26 of the lock means 22 is inserted into stopper grooves 41 of the circular cam parts 5 of the inner plates 3.
The operation of the apparatus of the present invention will now be described below.
The lock pin 26 is lifted by the operator against the biasing force of the spring 31 by pulling up a tool 42 engaged by him with the pin 29 of the lock pin 26 so that the notch 28 of the lock pin 26 can be engaged with the claw 38 of the lever 35 thereby disengaging the lock pin 26 from the stopper groove 41. (Refer to FIG. 12-I)
Then, the implement 39 is tilted back to allow the stopper face 43 of the upper coupler 12 to abut against the stopper 44 of the lift arms 11. Subsequently, the implement is dumped to allow stopper face 45 of the lower coupler 1 to abut against a connecting rod 46 of the lift arms 11. (refer to FIG. 12-II)
Thereafter, when the lift arms 11 are lifted and the implement 39 is dumped continuously further, the upper portions 40a of hooks 40 of implement 39 are engaged with the beam 13 of the upper coupler 12, whilst the beam 2 will move along the guide until the lower coupler 1 is allowed to abut against the implement 39. If the implement 39 is dumped continuously further, point "B" on the upper coupler 12 will move to point "B'"; point "C" on the implement 39 will move to point "C'"; and point "D" will move to point "D'" so that the upper and lower couplers 12 and 1 are kept at an angle of about seventy degrees by the connecting plates 6 and 15. (Refer to FIG. 12-III) At that time the rod 32 of the lock means 22 is allowed to abut against the circular cam portions 5 of the inner plates 3 thereby actuating the lever 35 so that the claw 38 can be disengaged from the notch 28 of the lock pin 26. As a result, the lock pin 26 is urged by the resilient force of the spring 31 against the abovementioned circular cam portions 5.
If the implement 39 is dumped further, the point "B" will move towards point "B"".
In the next place, the implement 39 is dumped further while it is placed on the ground and the vehicle is moved backwards. (Refer to FIG. 12-IV)
Next, dumping of the implement is stopped when the beam 13 has been disengaged from the hooks 40, and the vehicle is moved back further so as to detach the implement 39. (Refer to FIG. 12-V)
The implement 39 can be mounted on the vehicle by effecting the abovementioned sequence reversely.
In the above-mentioned embodiment of the present invention, unlocking of the lock means 22 is made manually; however another embodiment of the invention which will be mentioned below is of a type wherein the arrangement is made such that the lock means can be unlocked by the operator in the driver's cab effecting its remote controls.
The aforementioned lift arms 11 have unlocking means 50 fixedly secured on the upper surfaces thereof. The unlocking means 50 comprises a spring loaded cylinder 51 fixedly mounted on the lift arm 11. Slidably mounted in the spring loaded cylinder 51 is a piston 52. The piston 52 has a rod 53 connected to a member 54 having an inclined face 55 formed thereon. Each of the lift arms 11 has a stopper 56 fixedly secured thereto. Accommodated within the spring loaded cylinder 51 is a spring 57 which urges the piston 52 thereby allowing the member 54 to urge against the stopper 56. The piston 52 is connected to a cable 58 which extends to the driver's cab so as to be connected to a control lever (refer to FIG. 13).
Thus, if the control lever is operated to pull the cable 58 to the right hand, the piston 52 is moved against the biasing force of the spring 57, the member 54 is moved through the rod 53 and the unlocking pin 29 is pushed upwardly by the inclined face 55 of the member 54, the lock pin 26 can be disengaged from the grooves 41, and the notch 28 of the lock pin 26 can be engaged with the claw 38 of the lever 35. In this condition, the upper and lower couplers 12 and 1 becomes capable of swinging freely relative to each other.
It is to be understood that the foregoing description is merely illustrative of the preferred embodiments of the present invention and that the scope of the present invention is not to be limited thereto, but is to be determined by the scope of the appended claims. | An apparatus for attaching an implement to an earth moving vehicle, comprising a pair of lift arms for lifting the implement, a pair of tilt rods for effecting tilting motion of the implement, a pair of lower couplers pivotally connected to said lift arms at one end thereof, and a pair of upper couplers pivotally connected to said pair of tilt rods, the upper and lower couplers being pivotally connected with each other. The pair of lower couplers and pair of upper couplers are transversely connected by connecting beams, respectively. The connecting beams are adapted to engage with C-shaped hooks fixedly secured to the rear surface of the implement. | 4 |
BACKGROUND OF THE INVENTION
The present invention relates to rotary motors, and, more particularly, to rotary hydraulic motors which drive a cantilevered shaft.
Rotary auger shredders, such as the auger shredder disclosed in Koenig U.S. Pat. No. 4,253,615, include a housing which is divided into a grinding chamber and a motor cabinet. A rear wall separating the grinding chamber and cabinet supports a bearing on which is mounted a radial piston hydraulic motor and an auger screw which is cantilevered into the grinding chamber. The hydraulic motor includes a stationary part and a rotating part which is bolted to a mounting plate or disc which supports the screw.
The stationary motor part is connected to a hydraulic pump which supplies pressurized hydraulic fluid to drive the motor. The stationary part is connected to the housing framework within the cabinet by a single torque arm which extends radially from the rotational axis of the motor. The torque arm is attached to the housing by a link which is pivotally connected at one end to a clevis mounted on the housing, and at its other end to a clevis formed in the end of the link arm.
A problem with such a design is that torque forces transmitted to the link arm through the motor are unbalanced and create unwanted reactive radial loads, which may shorten the life of the motor and bearing. Further, the link connection between the torque arm and frame lacks means for absorbing shocks which may be created during reversal of the motor and auger screw rotation, or which occur when the auger encounters a relatively hard object such as a block of metal or hardened concrete. Accordingly, there is a need for an auger shredder having a motor and torque arm assembly which minimizes bending moments applied to the hydraulic motor and bearing, and which is capable of absorbing shocks encountered by the auger shredder during operation, and is balanced to minimize the radial reactive load occurring within the motor and bearing.
SUMMARY OF THE INVENTION
The present invention is a rotary motor having a counterbalanced torque arm which is connected to the motor housing such that reactive radial loads normally generated during operation of such an motor are substantially eliminated. Further, the torque arm of the present invention includes opposing pairs of hydraulic cylinders which are interconnected to distribute torque loads evenly between the ends of the torque arm and the housing, and in addition, absorb shock loads imparted to the auger drive motor. The invention is used with a rotary auger of the type having a housing, a drive motor having a stationary part and a rotary part attached to a bearing mounted on a wall of the housing, and an auger screw mounted on the bearing for rotation relative to the housing and stationary part of the motor.
The torque arm is attached to the stationary part of the motor and extends radially outwardly from the axis of rotation of the auger screw. The torque arm preferably includes a pair of opposing arm members which are oriented diametrically opposite to each other and are connected to the wall separating the grinding chamber of the auger shredder and the motor cabinet.
Also in the preferred embodiment, the torque arm members of the invention each include pairs of opposing hydraulic cylinders which provide the connection between the torque arm and the housing. Each of the cylinders is in fluid communication with a diametrically opposite cylinder in the opposing arm member. Consequently, for both clockwise and counterclockwise rotation of the auger and motor, the resistive torque borne by the torque arm will be transmitted to the housing through a pair of cylinders which are interconnected to equalize the pressure force transmitted from opposite ends of torque arm to the housing. Further, the use of the cylinders serves to cushion shock loading.
Accordingly, it is an object of the present invention to provide a counterbalanced torque arm for rotary machines which minimizes the reactive radial load exerted on the rotary machine by the torque arm during operation of the auger; a rotary motor in which shock loads transmitted to the housing enclosing the motor by the torque arm are minimized; a rotary motor in which the torque arm connecting the motor stationary part and rotary part is balanced to transmit torque loads evenly between the two torque arm members; a rotary motor in which the torque arm comprises a pair of diametrically opposed torque arm members which are connected to the housing enclosing the motor by cylinders which are interconnected to balance the loads transmitted; and a rotary motor having a torque arm which is relatively simple to construct, attach, detach and maintain.
Other objects and advantages will be apparent from the following description, the accompanying drawings and appended claims.
BRIEF DESCRIPTION OF THE DRAWING
FIG. 1 is a somewhat schematic, exploded perspective view of a rotary auger embodying the torque arm design of the present invention;
FIG. 2 is a perspective detail of the rotary auger of FIG. 1 showing the torque arm mounted on the motor and bulkhead;
FIG. 3 is a detail of the auger of FIG. 1, showing a mounting block in section;
FIG. 4 is an exploded, perspective view of the detail of FIG. 2;
FIG. 4A is a detail of an alternate embodiment of the mounting boss of the embodiment of FIG. 4; and
FIG. 5 is a hydraulic schematic of the cylinder circuit of the torque arm of FIG. 1.
DETAILED DESCRIPTION
As shown in FIG. 1, the rotary motor of the present invention is incorporated within a rotary auger, generally designated 10, which includes a housing 12 having a superstructure or framework 14. The housing includes a grinding chamber 16 and a motor cabinet 18. The motor cabinet 18 typically is enclosed, but is shown open in FIG. 11 for purposes of clarity. A wall or bulkhead 20 separates the grinding chamber 16 from the motor cabinet 18 and is attached to the framework 14.
The bulkhead 20 includes a circular central opening 22 which receives a circular bearing 24. The bearing 24 supports and is attached to a tapered auger screw 26, such as the auger screw disclosed in U.S. Pat. No. 5,108,040, the disclosure of which is incorporated herein by reference. The bearing 24 includes an outer race 28 which is attached to the bulkhead 20 by bolts 30, and an inner race 32.
As shown in FIGS. 1, 2 and 4, a hydraulic motor, generally designated 34, is attached to the inner race 32 by bolts 36 (see also FIG. 2). The motor is of the radial piston type, having a central, stationary cylinder block part 38 and an outer, rotary housing or cowling part 40. It is the outer cowling 50 which is attached to the inner race 32 by bolts 36. In operation, the cylinder block 38 remains stationary and the cowling 40 rotates, thereby rotating the inner race 32 of the bearing 24 and the auger screw 26 (see FIG. 1). The cylinder block 38 includes hydraulic oil ports 42 to power the motor 34. The ports 42 are connected to supply and return lines (not shown) from a hydraulic pump mounted within the cabinet 18 (see FIG. 1).
As shown in FIG. 1, the bearing 24 is mounted on a carriage, generally designated 44, which rides on the lower flanges of rails 46 extending rearwardly from the cabinet 18 and facilitates the assembly and disassembly of the auger 10. The carriage includes a support frame 48 having a cradle 50 that supports the outer race 28 of the bearing and includes a screw jack 52 which is attached to the upper portion of the outer race so that the bearing and auger screw 26 can be adjusted to engage central opening 22 for attachment and removal for maintenance.
As shown in FIGS. 2 and 4, a torque arm 54 is attached to the cylinder block 38 by a ring of bolts 56 and includes a pair of diametrically opposed, unitary arm members 58, 60. Arm members 58, 60 terminate in mounting blocks 62, 64. Mounting blocks 62, 64 include pairs of opposing cylinders 66, 68 and 70, 72, respectively (see FIG. 5). It is within the scope of the invention to provide a motor with a stationary case and a rotating central shaft. In such case, the torque arm would be attached to the stationary case.
As shown in FIG. 3 for mounting block 62, cylinders 66, 68 include sleeves 74, 76 which enclose pistons 78, 80 that have protruding stub shafts 82, 84, respectively. Although shown only schematically in FIG. 5, the structure for cylinders 70, 72 is the same as for cylinders 66, 68 in mounting block 64. Cylinder 70 includes piston 86 and stub shaft 88, and cylinder 72 includes piston 90 and stub shaft 92.
As shown in FIGS. 2 and 5, the cylinders 68 and 70 are interconnected by hydraulic line 94, and cylinders 66 and 72 are interconnected by hydraulic line 96. Hydraulic lines 94, 96 are fed by supply line 98 which is connected to a hydraulic accumulator 100 and hydraulic pump 102. Check valves 104, 106 are connected between supply line 98 and lines 96 and 94, respectively, to prevent reverse flow of fluid during operation.
As shown in FIGS. 2 and 4, the bulkhead 20 includes bosses 106, 107 which project into the motor cabinet 18 (see FIG. 1) and include upper and lower cam plates 108, 110, 112, 114, respectively. Cam plates 108, 110 are spaced to receive mounting block 62 between them, and similarly, cam plates 112, 114 are spaced to receive mounting block 64 between them. The spacing is such that stub shafts 82, 84 of cylinder 66, 68 engage cam plates 108, 110, and stub shafts 88, 92 engage cam plates 112, 114. Accordingly, the only contact between the torque arm 54 and bulkhead 20 is the camming engagement between the stub shafts 82, 84, 88, 92 and their respective cam plates 108, 110, 112, 114, respectively.
As shown in FIG. 4A, an alternate boss 106' includes an L-shaped locking member 116 which is removably bolted to a base 118 at an upper end rand to the end of the lower cam plate 110 at a lower end. Locking member 116 includes an upper cam plate 108' and a transverse portion 120 interconnecting the upper and lower cam plates 108', 110. Although not shown, boss 107 preferably is modified in the same manner. Accordingly, maintenance and repair of the cylinders 66, 68, 70, 72 is facilitated since removal of the locking member of the bosses allows the torque arm 54 to be rotated out of engagement with the bosses to expose the cylinders.
In operation, material to be ground is deposited through the open top of the grinding chamber 16 and the motor 34, powered by pump 102, is actuated to rotate the inner bearing race 32 which, in turn, rotates screw 26. The reactive force encountered by the screw 26 in grinding the material in chamber 16 has a tendency to rotate the cylinder block 38 of the motor 34 in a direction counter to the direction of rotation. This reaction force is transmitted from the motor 34 to the bulkhead 20 through the torque arm 54.
With the screw configuration shown for screw 26 in FIG. 1, the initial rotation will occur in a clockwise direction, creating a counterclockwise reaction force which will tend to make the torque arm 54 rotate in a counterclockwise direction. This causes the cylinders 66 and 72 to be compressed against their respective cam plates 108, 114, which pressurizes the cylinders. This pressurizing causes hydraulic fluid in line 96 to equalize the pressure exerted upon the cylinders as a result of the compressive force exerted between the mounting blocks 62, 64 and their respective bosses 104, 106.
When the screw 26 is reversed in rotation, which may be a part of a normal programmed operation, the reverse occurs; namely, the torque arm 54 is urged in a clockwise direction so that cylinders 68, 70 are pressurized by the compressive force exerted between the mounting blocks 62, 64 and cam plates 110, 112 of bosses 104, 106, respectively. This causes fluid to flow through line 94 until the cylinders 68, 70 are pressurized at equal pressures. Jolts and shocks sustained by the auger screw 26 during operation are absorbed somewhat by the hydraulic system shown in FIG. 5, since the hydraulic fluid has a measure of compressibility.
In a preferred embodiment, the lines 94, 96 are pressurized by pump 102 to approximately 250 psi. These lines 94, 96 preferably are made of stainless steel tubing.
While the form of apparatus herein described constitutes a preferred embodiment of this invention, it is to be understood that the invention is not limited to this precise form of apparatus and that changes may be made therein without departing from the scope of the invention. | A rotary motor with a counterbalanced torque arm adapted to be mounted within an auger housing. The torque arm is mounted on the stationary cylinder block of the motor which extends radially outwardly from the access of the cowling and is attached to the auger housing. The torque arm includes a pair of diametrically opposed torque arm members which support pairs of cylinders. The cylinders engage the housing and are interconnected such that diametrically opposed pairs of cylinders are in fluid communication. Accordingly, rotational torques exerted on the torque arm by the cylinder block, for auger screw rotation both in the clockwise and counterclockwise directions, are born equally by the opposing torque arm members. | 1 |
FIELD OF INVENTION
This is a continuation of U.S. application Ser. No. 29/002,596 filed Dec. 17, 1992 now U.S. Pat. Des. No. 343,756.
This invention relates to a restrainer device for infants, and more particularly, relates to a pair of support cushions of which at least one is releasably affixed to a planar surface one on each side of an infant to prevent the infant from rolling while sleeping.
BACKGROUND OF THE INVENTION
Infant safety while sleeping has always been a concern for parents. The occurrence of Sudden Infant Death Syndrome (SIDS) has heightened that concern. At present, the cause of SIDS is unknown. It has been theorized that SIDS may be due to infants suffocating by rotating or rolling face down on a mattress or into an obstacle which blocks their breathing, and then not having enough strength to raise their heads or move away from the obstacle.
A support pillow is described in U.S. Pat. No. 5,193,238 by Clute. The support pillow comprises two elongated right triangular members which have thin sheeting material extending from and beyond one lateral edge of each elongated triangular member with mating hook and loop fastening strips on the sheeting material to attach the elongated triangular members together. The vertical walls of the elongated triangular members oppose each other defining a channel. The infant lies lengthwise on its side in the channel on top of the sheeting material. Another fastening strip joins the triangular members above the infant and secures the infant in place. The infant's head projects out one end of the channel and its legs project out the other end of the channel. This ensures that the infant's breathing is not hampered since the infant's face cannot be pressed against a vertical sidewall.
Another embodiment of support pillow is disclosed in U.S. Pat. No. 5,216,772 by Clute in which an elongated recess is formed lengthwise in each vertical sidewall of the support pillow shown in the above-mentioned U.S. Pat. No. 5,193,238 with excluding means to prevent a child's face from entering the recess.
Patent Cooperation Treaty Application No. PCT/CA90/00145 (WO91/16842) discloses a restrainer for maintaining an infant on its side. One weighted chock member normally is placed on a mattress against the back of the infant and a second weighted chock member is placed on the mattress against the infant's chest and stomach. The chock members are joined to each other by a band of quilted fabric which wraps around the infant.
The above patents relate to complex infant support pillow structures which require the joining together of pillows by fastening strips for interaction of the two support pillows to prevent movement of an infant.
SUMMARY OF THE INVENTION
The disadvantages of the prior art may be overcome by providing a relatively simple restrainer device which does not require connector straps for the joining together of the two support pillows which can be readily positioned as desired to restrict an infant's movement.
In its broad aspect, the restrainer of the present invention for limiting human body movement on a planar surface comprises two support cushions of open-cell foam in a spaced-apart relationship to each other on the planar surface, and means for releasably attaching at least one of the support cushions to said planar surface.
According to a preferred aspect of the invention, the support cushions are elongated with a planar base, the planar surface is a sheet or panel of pliable fabric, such as a brushed nylon, and the means for releasably attaching the support pillows to the planar surface is formed on the planar base and the planar surface and comprises at least one strip of elongated hook fasteners on the planar base engageable with mating loop fasteners formed on the planar surface. It is further desirable to envelop each cushion in a thin, permeable fabric enclosure and to provide apertures extending through the support pillow to allow enhanced air flow to an infant supported by the support cushions.
BRIEF DESCRIPTION OF THE DRAWINGS
The present invention will now be described with reference to the accompanying drawings, in which:
FIG. 1 is a perspective view of an embodiment of the device of the invention showing the support cushions in an operative position releasably affixed to a panel;
FIG. 2 is an end view of the device of the invention with support cushions as shown in FIG. 1;
FIG. 3 is a perspective view of the underside of a support cushion;
FIG. 4 is a top plan view of the support cushions typified in FIG. 1;
FIG. 5 is a side view thereof;
FIG. 6 is a bottom plan view of an embodiment of the panel;
FIG. 7 is a perspective view of another operative position of the invention;
FIG. 8 is a perspective view of a preferred embodiment of foam rubber cushion insert;
FIG. 9 is a fragmentary perspective view, partly cut away, of a foam rubber cushion with fabric enclosure; and
FIG. 10 is a perspective view of a still further embodiment of the invention.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
Referring to FIGS. 1-5 of the drawings, each of elongated support cushions 10 having a planar base 12 is releasably attached to upwardly facing loop fasteners 14 formed on planar surface 16, such as provided by brushed nylon fabric, by at least one strip of downwardly facing elongated hook fastens 18, such as VELCRO™ hook fasteners, attached to the planar base 12. Hook fasteners 18, can be used to enable support cushions 10 to be releasably attached to planar surface 16 in desired arrangements, such as typified in FIGS. 1 and 7. FIG. 3 shows a pair of spaced-apart elongated hook fastener strips 18 secured longitudinally in proximity to opposite side edges of the planar base 12, but it will be understood that hook fastener strips 16 can be disposed transversely on base 12.
Elongated support cushions 10 preferably are made of resilient, open-cell foam rubber with a removable, thin, permeable fabric enclosure 19 enveloping each cushion foam rubber insert. Enclosure 19 may be opened at one end or opened along its base 12 to allow insertion of the foam rubber insert. The combination of open-cell foam and permeable fabric enclosure allows air to flow through the cushions.
The embodiment of elongated cushion shown in FIGS. 1-5 has a planar, i.e. flat, base 12 with a generally cylindrical or arcuate upper surface 20 with opposite upstanding lower sidewalls 22, 24 substantially perpendicular to the plane of base 12. With reference now to FIG. 8 and 9, the embodiment of elongated cushion 30 illustrated therein has a planar base 32, upstanding opposite lower side walls 34, 36 substantially perpendicular to the plane of base 32, a flat upper surface 37, and longitudinal bevelled upper corners 38, 40. The bevelled longitudinal upper corners 38, 40 of cushion 30 impart a generally arcuate shape to the upper portions thereof. Cushion 30 comprises resilient, open-cell rubber insert 31 with removable, thin, permeable fabric enclosure 33 which can be opened at an end or at the bottom for removal of insert 31.
Planar surface 16 preferably is composed of a sheet or panel of a pliable fabric such as nylon fabric (tricot) and is formed in a rectangular, circular, elliptical or the like shape having the loop fasteners 14 formed thereon to which the hook fasteners 18 will releasably attach. The loop fasteners are formed by brushing of the nylon fabric to develop the loops over the full surface of planar surface 16. A soft and aesthetic planar surface 16 can be provided by quilting a pair of co-extensive sheets of nylon fabric, as shown in FIG. 10, to be described, and brushing one side of the quilt to develop the loop fasteners.
Planar surface 16 may also comprise a bed sheet, mattress or the like having loop fasteners formed thereon to which the elongated hook fasteners will releasably engage. Loop fasteners 14 may be formed co-extensive with the planar surface 16 or may be formed in strips attached to the planar surface.
The use of such planar surfaces allows for the placement of a pair of support cushions 10 in various configurations as shown in FIGS. 1 and 7. The pair of spaced-apart support cushions 10 in cooperation with each other, with attachment of the support cushions 10 to planar surface 16, maintains the infant lying between the cushions generally stationary and effectively prevents the infant from rolling over.
In the preferred embodiment, support cushions 10 are arranged as shown in FIG. 1 in which the support cushions 10 are substantially parallel to each other to ensure that the infant's movement is restrained. However, embodiments such as that shown in FIG. 7 are acceptable since the infant will still be able to be restrained while propped in an inclined or seating position.
In the preferred embodiment of the invention, support cushions 10 contain a plurality of equispaced apertures 50 which extend transversely through the support cushions to further facilitate air flow through the support pillows. The light, permeable enclosure 19 enveloping support pillows 10 maintains apertures 50 unblocked.
Planar surface 16, such as a rectangular sheet or panel 17 illustrated, may also be releasably attached to an undersurface such as a bed or to a sheet on a bed by a strip 52 of elongated hook fasteners such as VELCRO™ fasteners secured to the underside thereof, as shown in FIG. 6. Strip 52 also conveniently allows panel 17 to be rolled into a bundle enveloping cushions 10, with strip 52 secured to the loops 14 on surface 16.
FIG. 10 shows another embodiment of support cushions in which cushion enclosure 51 of cushion 53 is permanently attached to an end of pliable rectangular panel 54 by stitching 56. Cushion 58 having enclosure 60 to which transverse hook fasteners 62 are attached is removably attached to panel 54 a desired distance from cushion 53 by engagement of hook fasteners 62 to loop fasteners 64 formed on panel 54. Panel 54 preferably is formed of two layers 66, 68 of quilted nylon fabric having loop fasteners formed on the upper side of layer 16 by brushing.
It will be understood that modifications can be made in the embodiment of the invention described here without departing from the scope and purview of the invention as defined by the appended claims. | A restrainer device for infants for maintaining an infant generally stationary to prevent the infant from rolling while sleeping comprising a planar surface and two support cushions arranged in a spaced-apart relationship to each other on the planar surface. The planar surface preferably is a sheet or panel of fabric and at least one of the support cushions are releasably attached to the planar surface. | 8 |
BACKGROUND OF THE INVENTION
This invention relates to an efficient energy storage flywheel possessing a benign failure mode. The invention relates particularly to flywheels with rotors fabricated from single crystals, microcrystalline solids, glasses or glass ceramics, which materials possess both high strength and low density and which fail at high stress in a brittle manner, thereby assuring rapid and complete fragmentation of the rotor in the event of rotor burst.
Flywheel based energy storage devices have long been regarded as having considerable promise for a variety of automotive, spacecraft, utility power and other applications due to their intrinsic simplicity, non-polluting nature, high efficiency and long cycle life compared to chemical batteries and other conventional energy storage means. A flywheel stores energy as the kinetic energy of a rapidly rotating body. The stored kinetic energy is proportional to the square of the rotation rate which is limited by the strength of the centrifugally stressed rotor. As a consequence, the energy stored per unit weight, or the specific energy of a flywheel, is directly proportional to the specific strength of the rotor material σ/ρ, where σ is the breaking strength and ρ is the density of the material. Hence, high strength, low density materials are preferred for flywheel rotor construction.
A wide variety of geometrical and mechanical designs have been proposed for energy storage flywheel rotors but most of these can be conveniently grouped into two categories based on the directionality, or lack thereof, of the rotor material mechanical properties. Isotropic materials possess nearly equal strengths in all mechanical properties. Isotropic materials possess nearly equal strengths in all directions whereas anisotropic materials, such as fiber reinforced composites, have strong directionality of mechanical properties. In the present invention, the term "isotropic" shall refer to materials in which the variation of strength with direction in the plane of rotation is less than 25%.
The simplest rotor designs employ materials with substantially isotropic mechanical properties, typically metallic alloys such as steel, titanium or aluminum, fabricated into disc-like shapes. The optimal designs for disc-like isotropic flywheel rotors are based on the so called Stodola or "optimized" shapes in which the thickness of the rotating disc decreases hyperbolically or exponentially with increasing radius in such a way that the magnitude of the centrifugally generated stress is only weakly position dependent or constant throughout the rotor body. The mathematical basis of constant stress rotor designs is described by Kulkarni and Stone in U.S. Pat. No. 4,408,500 and by J. P. Den Hartog in the book Advanced Strength of Materials, McGraw-Hill, 1952, pp. 49-69, all incorporated herein by reference. Since the ideal Stodola shape extends to infinity in the radial direction and is thus not suited for practical use, Kulkarni and Stone teach a modification to the Stodola design in which the rotating disc is truncated at a finite radius and the thin edges are thickened to increase the total kinetic energy relative to a truncated but not edge thickened Stodola design. The maximum energy storage per unit mass of a Stodola flywheel is numerically equal to σ/ρ.
Unfortunately, the performance and safety of isotropic rotors are limited by the mechanical properties and fracture behaviors, respectively, of conventionally chosen rotor materials. For example, the highest performance steels may have tensile strength values σ approaching 300,000 lb/in 2 and density ρ is near 0.283 lb/in 3 . The cyclic fatigue behavior of high strength steels limits design stresses to about 90,000 lb/in 2 , giving an available specific strength for energy storage applications of about 318,000 inches, equivalent to 856,000 ftlb/slug maximum specific energy. Marginally higher specific strength can be obtained using certain titanium alloys but the improved properties come at significantly higher cost compared to steel.
Metal alloys for structural applications are generally processed to possess significant ductility so that tensile crack propagation is impeded and stabilized, giving rise to predictable fracture characteristics. However, these otherwise favorable mechanical behaviors of ductile metallic alloys give rise to problems in high speed rotor applications. Catastrophic rotor burst failures have been associated with the use of ductile isotropic metal alloy rotors at high rotational speeds. In a typical failure of this nature, the ductile rotor fractures into several relatively large ballistic particles which, as a group, carry the entire stored energy of the rotor, and are individually capable of inflicting very severe damage and/or injury in the surrounding area. This potential for ballistic damage and injury has heretofore limited the practical applications of isotropic rotors to relatively low energy applications such as in momentum control wheels for spacecraft.
Anisotropic flywheel rotor designs typically start with a rotating tensile ring or tube made from carefully wound fiber-reinforced uniaxial composite. This design concentrates mass at the largest radius and directs fiber strength in the tangential or hoop stress direction. Carbon fibers are often chosen because of their high specific strengths. Carbon fibers with strengths as high as 750,000 lb/in 2 and density near 0.065 lb/in. 3 are available commercially. Carbon fibers typically have round cross-sections and, with careful winding, packing density in the wound fiber composites up to 78% can be achieved. The remaining space in the composite is filled with matrix resin. The composite matrix resin contributes weight but not strength to the rim thereby diluting the properties of the high strength fiber. This factor limits the strength of the resulting carbon fiber composite to about 585,000 lb/in 2 . Assuming that the resin density is approximately equal to that of the carbon fibers, the specific strength of the carbon fiber composite rotor is still approximately 9.000,000 inches equivalent to 24,000,000 ftlb/slug or more than an order of magnitude better than that of high strength steels.
However, difficulties in the design of composite rotors are introduced by the extremely low transverse strength of uniaxial composites. This weakness can lead to delamination under the significant radial stresses experienced by the rotor if it has significant thickness in the radial direction. Thus, while the energy storage efficiency of a rotating anisotropic rim can be large on a per unit weight basis, it difficult to achieve high volumetric efficiencies. Moreover, high levels of energy storage imply high elastic strain values in rotating rim flywheel designs. Centrifugal stress and strain values in the hub and axle sections of the rotor are much lower due to the smaller radius of rotation. Means for mechanical coupling the rim to the hub and axle sections of the rotor must be sufficiently compliant to accommodate this large radial differential in elastic strain while, at the same time, sufficiently stiff to resist input/output torques and gyroscopic twisting forces and to maintain stability with respect to potentially destructive vibratory modes. Many complex mechanical constructions have been advanced to meet these requirements. For example, Friedericy et. al., in U.S. Pat. No. 4,036,080, show a flywheel rotor with multiple nested composite rims which frictionally couple inertial torques to a hub while largely decoupling radial stresses. Additionally, Bakholdin et. al., in U.S. Pat. No. 5,628,232, teach the use of conical sections combined with cylindrical hubs to mechanically couple a rotating annular cylinder to a rotating shaft while Bitterly, in U.S. Pat. No. 5,124,605 intersperses a series of compliant tubes between the hub and the rim. All of these structures typically comprise multiple mechanical elements, adding considerable complexity, cost and reliability issues to the basic rotating rim flywheel design.
There have been several attempts to create safe, high performance flywheel rotors by combining the use of composite materials with classical isotropic rotor designs. For example, Rabenhorst et. al., in U.S. Pat. No. 3,788,162, show a rotor of the constant stress design comprising multiple fiber reinforced composite laminations to build up the radially contoured shape. Unfortunately, such a construction makes only limited use of the highly directional strength properties of the fibers and thus cannot offer the full performance advantage of the fiber properties. Gilman, in U.S. Pat. No. 4,186,245, shows a similar constant stress disc construction built up using high specific strength metal alloy strips. Gilman's design has high volumetric efficiency due to the efficient packing of the strips but the design fails to take into account the poor fatigue characteristics of the chosen glassy metal alloy materials. Kulkarni and Stone in U.S. Pat. No. 4,408,500 show an isotropic constant stress disc flywheel rotor with an outer rim of uniaxial fiber reinforced composite intended to improve the safety of the device. While incipient failure in the rim of Kulkari and Stone's rotor may give some warning, full rotor burst will still generate the large and destructive ballistic particles characteristic of conventional isotropic rotors.
Thus, as a result of the aforementioned limitations and despite the efforts over several decades of many workers skilled in the art, energy storage flywheels have still not been adopted for widespread use in the transportation, space and utility power industries.
SUMMARY OF THE INVENTION
The present invention addresses the problem of safe and efficient rotational energy storage in a different and unexpected way. Instead of relying on the delamination or fibrillation of fiber or strip reinforced anisotropic composites to achieve a benign rotor failure mode, as in the above referenced U.S. Patents, this invention utilizes the stored elastic energy in a highly stressed, perfectly brittle solid to assure benign disintegration of the flywheel rotor in the event of a rotor burst. The term "brittle" as used in the present context, is taken to refer to a material with negligible ductility having a fracture toughness value less than about 3 ksi√in, preferably less than 1 ksi√in. A flywheel rotor formed from a brittle, high specific strength and substantially isotropic material provides the desired combination of high energy storage efficiency and safety required for the above mentioned energy storage applications.
Brittle failure at sufficiently high tensile stress always results in complete fragmentation, creating a multitude of small particles which are harmless relative to burst fragments of ductile, isotropic flywheels. This dramatic fragmentation effect results from prolific crack tip branching which draws energy from the stored elastic strain field and converts it directly into the surface energy of the newly created small particles. Thus, a higher density of stored elastic energy density will tend to result in the creation of more and smaller particles. This feature is advantageous for flywheel design since degree and speed of rotor fragmentation will increase in direct proportion to the degree of hazard.
A number of relatively conventional high strength, low density materials are suitable for construction of brittle isotropic flywheel rotors. These include, but are not limited to, single crystals of silicon, metal oxide single crystals, as of sapphire (Al 2 O 3 ) or oxide garnets (e.g., yttrium aluminum garnet, Y 3 Al 5 O 12 ), and graphite, oxide silicate glasses such as silica glass, s-glass, e-glass and Pyrex and microcrystalline materials such as Pyroceram™ and pyrolytic graphite. It should be noted that sapphire, graphite and pyrolytic graphite have isotropic properties within the planes perpendicular to their respective crystallographic c-axes. The desired combination of brittle failure at high stress in such materials can be routinely achieved by first carefully processing the rotor material to eliminate bulk mechanical defects and subsequently removing stress concentrating surface flaws in the final stages of rotor fabrication. Mechanical flaws in the bulk of the rotor materials are effectively removed by careful melting practice in the case of silicate glasses or slow and stable crystallization processes for single crystals. Surface flaws are effectively removed by means of chemical or chemo-mechanical polishing of the final rotor surfaces. The strikingly high strengths readily achieved by such processing in low density silica and silicate glasses are discussed by C. J. Phillips in American Scientist, 53, pp.20-51, 1965.
The high strength states achieved by elimination of mechanical flaws are effectively preserved and protection from strength degradation due to handling or in-service damage is effected by application of protective polymer or metal coatings or by creation of surface compression layers. The latter is accomplished either by suitable tempering heat treatments or surface ion exchange treatments in the cases of glasses, or by application of a compressively loaded epitaxial layer on the surfaces of single crystal rotors. Surface compressive stresses are created in glass ceramic bodies by laminating layers of differing thermal expansion properties.
It is therefore the object of this invention to provide safe, low cost and efficient energy storage flywheels which take maximum advantage of the relatively high specific strength, excellent processability and unique fracture properties of brittle, high strength isotropic solids, thereby avoiding the performance and safety limitations of conventional isotropic flywheel designs and the design complexities associated with the use of composite rotors.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 shows a simple disc shaped isotropic flywheel rotor;
FIG. 2 shows a section through the rotor of FIG. 1 illustrating the attachment of axially located axles;
FIG. 3 shows an annular ring isotropic flywheel rotor with conical end plates and a central axle; and
FIG. 4 shows a constant stress design isotropic flywheel rotor.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
Since the invention relies on stored elastic energy in a brittle solid to fragment the rotor in the event of a failure, the shape of the rotor and the resulting stress distribution under centrifugal loading are of prime importance. In particular, it is preferable that variation of the magnitude of the total stress within the rotor body be as small as possible so that the fragmentation process operates uniformly on all portions of the rotor.
A rotating, solid, flat disc 1 with no central hole, as illustrated in FIG. 1, has a stress distribution with maximum tangential and radial stress magnitudes at the center of the disc which is also the rotation axis 2. According to J. P. Den Hartog in Advanced Strength of Materials, McGraw-Hill, 1952, pp. 53, the tangential stress parabolically decreases to 43% of the maximum value at the outer radius while the radial stress decreases to zero at this location. In this stress distribution the majority of the volume of the brittle rotor body is highly stressed leading to moderately effective fragmentation at rupture. This degree of stress magnitude variation is the maximum permitted by the invention.
The presence of a small central hole in a larger flat disc, which may be desired to fit an axle, immediately concentrates the stress local to the hole by a factor of approximately two on top of the flat disc stress distribution. This stress distribution is not favorable for performance or safety since the most highly stressed portion of the rotor body is a small volume surrounding the central hole. Failure of the rotor in this local high stress region will limit energy storage performance and may result in the formation of large fragments in the more lightly stressed outer portions of the rotor. Thus, flat disc shaped rotors with central holes smaller than about 0.4 times the overall disc diameter are not suitable for fabrication from brittle materials. Therefore, axle or bearing attachment to a flat disc rotor must be accomplished in a manner similar to that illustrated in FIG. 2, where axle or bearing mounting elements 3 are affixed to the surface of the rotor using adhesive means. The rotor in FIG. 2 is supported by rolling element or magnetic bearings 4.
The stress concentrating effect of a central hole decreases as the hole diameter approaches the disc diameter, and, in the limit, a thin rotating ring or tube has a uniform tangential or hoop stress. Thus, flat annular ring shaped rotors in which the inner diameter is greater than about 0.4 times the outer diameter are suitable for fabrication from brittle materials. These annular ring designs are similar to designs using wound, fiber-reinforced composite rotors except that the annular ring made from a brittle isotropic solid can be much thicker in the radial direction due to the isotropic strength property. FIG. 3 shows a cross-section of a flywheel rotor comprising a brittle annulus 5 attached to a rotatable shaft 6 by means of two conical elements 7.
The most preferable rotor shapes for fabrication from brittle materials are the constant stress or Stodola designs referred to above. In this case, the centrifugal stress and the elastic energy density is substantially constant throughout the rotor body and, at rupture, brittle fracture will uniformly fragment the rotor into small, relatively harmless particles. FIG. 4 shows a constant stress rotor 8 with axial protrusions 9 for mounting of bearings.
The potential of isotropic rotors fabricated from brittle materials for high performance can be illustrated by using the example of monocrystalline silicon. Cylindrical silicon single crystals up to 12 inches in diameter are produced routinely and utilized commercially in the semiconductor industry, as is well known to those skilled in the art. These crystals are remarkably perfect and free of interior mechanical defects. Conventional chemical polishing techniques can be used to remove surface flaws resulting in tensile strength levels of about 1,000,000 lb/in 2 (see K. E. Peterson, Proc. IEEE 70, p. 420, 1982). The density of silicon is 0.083 lb/in 3 , giving a specific strength of about 12,000,000 inches, equivalent to 32,000,000 ftlb/slug specific energy, which is marginally greater than that of uniaxially stressed carbon fiber composites. Since the strength of single crystal silicon is substantially isotropic, there is no problem withstanding centrifugal radial stresses as there is in the case of tangentially wound fiber reinforced composite rotors.
Other isotropic and brittle materials, including but not limited to sapphire, garnet and other oxide single crystals, sintered ceramics, oxide glasses such as silica glass, lithium alumino-silicate glasses, s-glass, e-glass and Pyrex and microcrystalline solids such as Pyroceram™, offer a wide design space within which flywheel performance and cost can be traded off to meet the requirements of particular applications. For example, lowest possible weight will be of prime concern in designing an energy storage flywheel for use in a spacecraft while cost may be less important. The cost-performance relationship may be reversed in the case of an automotive regenerative braking application.
While very high strengths can be achieved in silicon and other hard materials by chemically polishing or other means to remove surface defects, the strong objects formed in this way are subject to strength degradation if the polished surface is damaged by contact with other hard objects, as may easily happen during assembly or operation of a flywheel. The need for mechanical damage resistance can be met in several ways. As-drawn quartz optical fibers have pristine surfaces and strength values near 1,000,000 lb/in 2 . Immediately after drawing they are coated with a polymeric material to protect the surface and preserve the high strength. Other methods rely on the creation of surface compressive stresses to preserve strength even in the presence of mechanical damage.
U.S. H000557, "Epitaxial strengthening of crystals," and related U.S. Pat. Nos. 5,572,725 and 5,573,862, all assigned to the same assignee as the present invention and all incorporated herein by reference, teach enhancement of the mechanical damage tolerance of chemically polished garnet crystals by application of an epitaxial surface compression layer comprising garnet film compositions with a compressive elastic strain in the range of 0.02 to 0.4%. Specific illustrative embodiments of the present invention include rotors fabricated from yttrium-aluminum-garnet (Y 3 Al 5 O 12 ) coated with a surface compression layer of Y 3 Al 5 O 12 in which a portion of the yttrium is replaced by another Rare earth element such as holmium, dysprosium, terbium, gadolinium, europium, samarium, neodymium, praseodymium, or lanthanum. This epitaxial strengthening technique could also be used to preserve the strength of monocrystalline silicon objects. A suitable epitaxial layer on silicon would consist of a silicon-germanium alloy with a lattice constant 0.01 to 0.5% greater than that of silicon. The epitaxial layer would be applied by standard liquid or vapor phase epitaxy techniques as are known to those skilled in the art.
Of particular interest to the present invention are certain alkali containing silicate glasses which can be chemically strengthened using ion exchange processes to impart surface compressive stresses. C. J. Phillips in American Scientist, 53, pp.20-51, 1965 reports strength values greater than 100,000 psi in chemically strengthened glasses. U.S. Pat. No. 4,255,199, to Richard Reade and incorporated herein by reference, teaches lithium alumino-silicate based glass compositions which can be very effectively chemically strengthened by immersion in molten NaNO 3 to achieve tensile strength values up to 90,000 lb/in 2 . Given a density value near 0.09 lb/in 3 , the specific strength of such glass is 1,000,000 inches or about three times the value for high strength steel.
An illustrative example of one preferred embodiment assumes a flywheel rotor fabricated from a simple 1 inch thick, 12 inch diameter single crystal silicon flat disc, weighing 9.4 lb. At a rotation rate of 120,000 rev/min. the rotor would be subjected to tensile stresses of magnitude a little less than 1,000,000 lb/in 2 and would store a little more than 1 kWhr of kinetic energy, giving a specific energy storage value about 234 Whrs/kg. This is comparable to anisotropic flywheel designs using high strength carbon fibers. Moreover, the angular momentum of the 1" by 12" silicon rotor would be about 229 ft lbs sec, offering potential utility for spacecraft pointing and attitude control application.
It will be appreciated by those skilled in the art that the specific energy storage value for a Stodola shaped or constant stress silicon disc will be substantially higher than that of the flat disc in this example, an advantage that can be traded for design safety margin while maintaining relatively high energy storage efficiency. The energy density of an infinite Stodola disc would be just σ/ρ or 833 Whr/kg. For finite radius approximations to the Stodola shape the energy density will be intermediate between that of the flat disc and the ideal value. Also, a constant stress design is preferable from a safety point of view since, at rupture, the entire volume of the disc will fragment equally, thereby simplifying containment of the fragments. The containment of the released small fragments, while not as difficult as in the case of a steel wheel, is still an issue. The total energy of approximately 1 kWhr or 3.6 MJ is released suddenly in the form of the kinetic energy of radially outward direct high velocity particles. This energy may be contained using a ring of Spectra® brand polyethylene fiber which is capable of dissipating about 50J/gm in ballistic interactions. A Spectra® ring weighing about 200 pounds would be needed to contain the burst of the silicon rotor in this example. For unmanned spacecraft applications this weight penalty is probably unacceptable and the flywheel would be used without containment.
Another illustrative example assumes a flywheel rotor fabricated from a 1 inch thick, 12 inch diameter flat disc of lithium alumino-silicate glass and chemically strengthened by immersion in molten NaNO 3 to achieve a fracture stress of 90,000 lb/in 2 . The weight of the rotor would be about 10.2 lb (4.62 kg). At fracture, the lithium alumino-silicate glass rotor would store about 85 Whr of kinetic energy or about 1/12 the energy of the higher performing monocrystalline silicon rotor. This can be compared to the kinetic energy of a 1000 kg passenger car traveling at a typical suburban speed limit of 35 miles per hour, which is 34 Whr. Thus, two such glass discs, rotating in opposite directions to cancel gyroscopic forces, and operating up to about half the fracture stress, could store 42.5 Whr or 153 kJ, providing the energy storage needed for a passenger car regenerative braking system. In this lower energy example, a seven to ten pound Spectra® fiber ring would contain the energy release from a rotor burst. As in example 1, a constant stress disc of similar dimensions is preferred over a flat disc for both performance and safety. | An energy storage flywheel having a benign failure mode, the rotor of which is constructed of a brittle, high specific strength, isotropic solid. | 5 |
FIELD OF THE INVENTION
This invention relates generally to industrial loss events. More particularly, aspects of the invention provide methods and systems for predicting loss events, impacts of loss events, and/or providing potential corrective measures to reduce or eliminate the occurrence or impact of the loss events.
DESCRIPTION OF RELATED ART
Businesses are increasingly utilizing automation technologies to monitor specific components of an industrial system. For example, in the oil and gas industry it is quite common to monitor the specific components that are required to extract crude oil and/or natural gas. By doing so, workers may be notified when the component, such as a pump, fails or otherwise ceases to operate at full capacity. Indeed, unanticipated and preventable production losses due to plant equipment failure, production chemistry anomaly, pipeline corrosion, etc. can be a significant source of waste, environmental pollution, and profit erosion.
While automated monitoring systems may notify workers of specific failures in regards to an individual component, current monitoring systems cannot adequately predict loss events. For example, the repair of a broken pump may readily be associated with a cost for labor, downtime, and a replacement pump, however, other costs, such as environmental, and/or health and safety of the workers are not considered or calculated. Furthermore, other loss events related to the pump failure are not indicated. For example, the failure of the pump may be indicative of another failure event that is not directly related to the operation of the pump. Also, data regarding the pump's functioning may indicate that the pump is fully operational, however, slight variations within the normal operating range of the pump may foretell the failure of other equipment. Indeed, in the oil and gas industry a very small rise in temperature over an extended period of time in pipes extracting crude oil could be considered a normal fluctuation within predefined limits and often goes unnoticed by workers. This is especially true when workers often change shifts every 8 to 12 hours and have other tasks besides monitoring the output of the sensor reporting the temperature. The small fluctuation in temperature, however, may foretell the failure of other equipment or an indication of contamination in the pipe, which leads to loss in the terms of economic loss, environmental contamination, and/or pose a risk for the health and safety of the plant workers or surrounding people.
Therefore, current systems may provide an insight to the failure of a single component, but do not provide an estimate that failure's impact upon the business. Nor do the current systems provide an avenue for the business to predict the loss, as well as its impact, and make an educated decision of mitigating the loss based upon g economic, environmental, and health and safety considerations. Therefore, there is a need in the art for systems and methods for predicting loss events, impacts of loss events, and/or providing potential corrective measures to reduce or eliminate the impact of the loss events.
BRIEF SUMMARY OF THE INVENTION
Aspects of the invention overcome problems and limitations of the prior art by providing systems and methods that may focus on key business concerns. One aspect relates to the use of system-wide information to predict variables that are directly linked to business impact, such as production loss. In one embodiment, operational data from a plurality of sensors, and transactional data are collected and utilized. Yet in other embodiments, only a subset of the total data is utilized. In certain embodiments, the subset of data selected for utilization may be based upon one or more thresholds. In certain embodiments, the collected data is utilized to determine which, if not all, of the collected data is considered. In yet other embodiments, extraneous data is also utilized. A plurality of statistical models may be applied to the selected system-wide data to determine a best-fit model in regards to the correlation among the operational data and extraneous data with the transactional data to predict events and impacts of the predicted events. In further embodiments, features may be applied to at least a portion of the selected data to amplify patterns before applying the data to the predictive model. In further embodiments, occasional sensor anomalies with little business impact may be ignored.
In another aspect, systems and methods may utilize the best-fit model to determine at least one intervention to reduce or eliminate the impact of the predicted events. The models may also be updated with additional collected data. In one embodiment, one or more predictions directly or indirectly based upon the best-fit model may be compared to an outcome to determine the accuracy of the best-fit model. In yet other embodiments, the actual outcome may be compared to other models, such as the models not considered as accurate as the best-fit model, to determine if another model is more accurate than the best-fit model initially chosen.
The systems and methods may be stored and/or distributed on computer-executable mediums. The systems and methods may also utilize one or more computer-readable instructions on computer-readable mediums for performing one or more of the disclosed methods. The computer-executable instructions may be stored on any tangible computer-readable medium, such as a portable memory drive or optical disk.
BRIEF DESCRIPTION OF THE DRAWINGS
The present invention is illustrated by way of example and not limited in the accompanying figures in which like reference numerals indicate similar elements and in which:
FIG. 1 is a flowchart demonstrating an exemplary method according to one embodiment of the invention;
FIG. 2 shows a computing environment a may be utilized in accordance with one or more embodiments of the invention;
FIG. 3 shows an exemplary industrial system that one or more embodiments of the invention may be applied to;
FIGS. 4A , 4 B and 4 C illustrate exemplary displays that may be utilized in accordance with one or more embodiments of the invention; and
FIGS. 5A and 5B show exemplary displays that may be utilized in accordance with one or more embodiments of the invention.
DETAILED DESCRIPTION
FIG. 1 is a flowchart demonstrating an exemplary method according to one embodiment of the invention. As seen in FIG. 1 , a method according to one or more embodiments of the invention collects system-wide information comprising operational data from a plurality of sensors, extraneous data, and transactional data (step 102 ). As used herein, a “system” refers to a plurality of components and/or subsystems utilized in the production of a good or service. The system may be spread throughout several geographic locations and/or include one or distinct subsystems. For example, an oil and gas collection system may comprise several subsystems, such as: reservoirs, wells, plants, and/or export subsystems. Thus, “system-wide information” includes information regarding one or more components throughout several subsystems. In this regard, embodiments of the invention view the production of the goods or services at the process or business level rather than single discrete components.
As used herein, operational data includes data originating at or otherwise obtained (directly or indirectly) from any of a plurality of sensors throughout a system that measures one or more operation parameters within the system. In one such embodiment, the operational data may be collected substantially upon being received or measured at the sensor. For example, one or more sensors may measure data on a consistent basis over a period of time. As one example, in the oil and gas industry it may be desirable to collect data regarding oil pressure of a collection point every second. In that scenario, the sensor may consistently provide operational data for collection. In yet other embodiments, operational data may be stored on one or more computer-readable mediums in one or more formats for subsequent collection.
In certain embodiments of the invention, not all of the operational data measured at one or more sensors is collected. For example, only a fraction of the total detected parameters from a specific sensor may be included in any collection efforts. For example, merely because a parameter is measured every second, there is no requirement that every data point is collected. Rather, in one embodiment, only a predetermined fraction of the data (e.g., one data point per minute) may be collected in step 102 . Indeed, while the operational data may be collected in a. “system-wide” manner, there is no requirement that the collected data include data from every sensor in the system. Rather, the collection of “system-wide” operational data as used herein is data that is received from a plurality of sensors that are located in different components within a system, and wherein at least one datum is collected from a sensor that is considered part of a different component than at least another sensor and is not directly connected to the other component mechanically, hydraulically, or electrically or otherwise directly dependent on at least one other component. For example, the failure of one component having a sensor would not directly impact the working order of another component. Indeed, some components within the system may, in the minds of those skilled in the art, not even be considered to have a tangential relationship with another component. As explained below, however, the inventors have discovered novel methods and systems for discovering relationships between components throughout a system and predicting loss events based upon the measurements of sensors within the system.
As used herein, the term “collect” also encompasses the storage on one or more computer-readable mediums. Indeed, the collection of data is not required to be a single event, rather the collection of data may encompass irregular storage of data across several computer-readable mediums. Furthermore, various embodiments of the invention may be implemented with computer devices and systems that exchange and process data. In feet, with the benefit of this disclosure, those skilled in the art will readily appreciate that several computing and/or networking environments may be utilized to carry out one or more embodiments of the invention. For discussion purposes, FIG. 2 provides an exemplary environment for performing one or more embodiments of the invention.
Elements of an exemplary computer system are illustrated in FIG. 2 , in which the computer 200 is connected to a local area network (LAN) 202 and a wide area network (WAN) 204 . Computer 200 includes a central processor 210 that controls the overall operation of the computer and a system bus 212 that connects central processor 210 to the components described below. System bus 212 may be implemented with any one of a variety of conventional bus architectures.
Computer 200 can include a variety of interface units and drives for reading and writing data or files. In particular, computer 200 includes a local memory interface 214 and a removable memory interface 216 respectively coupling a hard disk drive 218 and a removable memory drive 220 to system bus 212 . Examples of removable memory drives include magnetic disk drives and optical disk drives. Hard disks generally include one or more read/write heads that convert bits to magnetic pulses when writing to a computer-readable medium and magnetic pulses to bits when reading data from the computer readable medium. A single hard disk drive 218 and a single removable memory drive 220 are shown for illustration purposes only and with the understanding that computer 200 may include several of such drives. Furthermore, computer 200 may include drives for interfacing with other types of computer readable media such as magneto-optical drives.
Unlike hard disks, system memories, such as system memory 226 , generally read and write data electronically and do not include read/write heads. System memory 226 may be implemented with a conventional system memory having a read only memory section that stores a basic input/output system (BIOS) and a random access memory (RAM) that stores other data and files.
A user can interact with computer 200 with a variety of input devices. FIG. 2 shows a serial port interface 228 coupling a keyboard 230 and a pointing device 232 to system bus 212 . Pointing device 232 may be implemented with a hard-wired or wireless mouse, track ball, pen device, or similar device.
Computer 200 may include additional interfaces for connecting peripheral devices to system bus 212 . FIG. 2 shows a universal serial bus (USB) interface 234 coupling a video or digital camera 236 to system bus 212 . An IEEE 1394 interface 238 may be used to couple additional devices to computer 200 . Furthermore, interface 238 may be configured to operate with particular manufacture interfaces such as FireWire developed by Apple Computer and i.Link developed by Sony. Peripheral devices may include touch sensitive screens, game pads scanners, printers, and other input and output devices and may be coupled to system bus 212 through parallel ports, game ports, PCI boards or any other interface used to couple peripheral devices to a computer.
Computer 200 also includes a video adapter 240 coupling a display device 242 to system bus 212 . Display device 242 may include a cathode ray tube (CRT), liquid crystal display (LCD), field emission display (FED), plasma display or any other device that produces an image that is viewable by the user. Sound can be recorded and reproduced with a microphone 244 and a speaker 246 . A sound card 248 may be used to couple microphone 244 and speaker 246 to system bus 212 .
One skilled in the art will appreciate that the device connections shown in FIG. 2 are for illustration purposes only and that several of the peripheral devices could be coupled to system bus 212 via alternative interfaces. For example, video camera 236 could be connected to IEEE 1394 interface 238 and pointing device 232 could be connected to USB interface 234 .
Computer 200 includes a network interface 250 that couples system bus 212 to LAN 202 . LAN 202 may have one or more of the well-known LAN topologies and may use a variety of different protocols, such as Ethernet. Computer 200 may communicate with other computers and devices connected to LAN 202 , such as computer 252 and printer 254 . Computers and other devices may be connected to LAN 202 via twisted pair wires, coaxial cable, fiber optics or other media. Alternatively, radio waves may be used to connect one or more computers or devices to LAN 202 .
A wide area network 204 , such as the Internet, can also be accessed by computer 200 . FIG. 2 shows a modem unit 256 connected to serial port interface 228 and to WAN 204 . Modem unit 256 may be located within or external to computer 200 and may be any type of conventional modem, such as a cable modem or a satellite modem. LAN 202 may also be used to connect to WAN 204 . FIG. 2 shows a router 258 that may connect LAN 202 to WAN 204 in a conventional manner. A server 260 is shown connected to WAN 204 . Of course, numerous additional servers, computers, handheld devices, personal digital assistants, telephones and other devices may also be connected to WAN 204 .
The operation of computer 200 and server 260 can be controlled by computer-executable instructions stored on a computer-readable medium 222 . For example, computer 200 may include computer-executable instructions for transmitting information to server 260 , receiving information from server 260 and displaying the received information on display device 242 . Furthermore, server 260 may include computer-executable instructions for transmitting hypertext markup language (HTML) and extensible markup language (XML) computer code to computer 200 .
As noted above, the term “network” as used herein and depicted in the drawings should be broadly interpreted to include not only systems in which remote storage devices are coupled together via one or more communication paths, but also stand-alone devices that may be coupled, from time to time, to such systems that have storage capability. Consequently, the term “network” includes not only a “physical network” 202 , 204 , but also a “content network,” which is comprised of the data—attributable to a single entity—which resides across all physical networks.
Returning now to specific implementations, FIG. 3 more clearly shows an exemplary system that may benefit from one or more embodiments of the invention. As shown on the top left side of the figure, pump 302 is operatively connected to pipe 304 , which terminates at separator 306 . Pump 302 may be used to pump a liquid, such as crude oil being excavated from an underwater drilling facility. As the liquid is passed to separator 306 , sensor 308 may measure temperature of the liquid within pipe 304 . Those skilled in specific arts, such as oil and gas production, understand that specific processes of pumping oil may not utilize the structures shown in FIG. 3 , however, the basic teachings of FIG. 3 are shown to demonstrate that the systems and methods of the invention may be applied to a vast array of multi-component systems. Likewise, pump 310 may be used to pump the same or different material than the material being pumped by pump 302 , such as crude oil. As the gas travels through pipe 312 to separator 314 , sensor 316 measures a parameter, such as pressure, temperature, estimated flow rate, etc. The functionality of pump 302 is not dependent upon the functionality of pump 310 and vice-versa. Specifically, each pump ( 302 , 310 ) may pump a different gas or liquid to a different separator and does not rely on an output of the other to function. Thus, in the embodiments shown in FIG. 3 , pumps 302 and 310 are considered part of different subunits within the system and that the failure of pump 302 would not directly impact the functionality of pump 310 . Thus, some components of the system (e.g., such as pumps 302 and 310 ), may, in the minds of those skilled in the art, not even be considered to have a tangential relationship with each other. To the contrary, the failure of a cooling system, for example, for one of the pumps 302 , 310 may directly impact the output of the pump, such as lower output and or the failure of the pump, resulting in no output. Like pumps 302 and 310 , separators ( 306 , 314 ) may also be geographically spaced apart and thus considered different subunits or subsystems of the overall system. FIG. 4B (discussed in more detail later) shows further subsystems that may be within the system shown in FIG. 3 .
As further seen in FIG. 3 , each of the separators 306 , 314 may be used to separate the natural gas from the oil. For example, extracted gas from separators 306 , 314 may travel by pipes 318 , 320 , respectively to field gas compressors (see element 322 ). Pipe 318 may comprise sensor 324 that measures a parameter and pipe 320 may comprise sensor 326 that measures a parameter, such as flow rate, compression, temperature, and/or combinations thereof. Conversely, the remaining oil product may travel by pipes 328 and 330 to a different processing subunit or subsystem (see element 332 ). As explained in more detail later in the Specification, subsystems utilized in processing the extracted gas from pipes 318 and 320 are distinct from subsystems utilized for processing the oil, however, information one subsystem may be used to predict loss event and/or the severity of a loss event that may occur in another subsystem.
As discussed above in regards to step 102 , extraneous data may also be collected. As used herein, extraneous data excludes any data directly regarding the creation, processing, or manufacturing of the goods or services being produced by the system. For example, extraneous data may include data that either 1) originated outside the system, or 2) data originating inside the system regarding the measurement of an external impact source upon the system and would exclude any man-made intended input or output of the system or data regarding the processing or manufacturing of the goods and/or services. Using the system of FIG. 3 as an example, the output, electrical consumption, and or working parameters of the pumps 302 , 310 and/or the separators 306 , 314 would not be considered extraneous data. Outside forces acted upon one or more of the components of FIG. 3 , however, would be considered extraneous data.
In one embodiment, extraneous data may include event data, such as environmental data. The extraneous data may be collected directly from a plurality of sensors connected to or associated with the system. Yet in other embodiments, the sensors are not associated with the system. In either embodiment, the sensors would measure extraneous data, as opposed to system operational data. Yet in other embodiments, the data, such as weather data may be historical and obtained after the occurrence of the event from which the data relates to. In this regard, there is no requirement that the data utilized be received from a sensor. Rather, the extraneous data may be already modified or otherwise manipulated, for example subjected to statistical analysis before collection at step 102 . The data may be stored on one or more computer-readable mediums. In yet other embodiments, the extraneous data may be modeled from an event and not be actual results or information received at one or more sensors during the event.
Step 102 further includes the collection of transactional data. As used herein, transactional data includes any data comprising information regarding the intentional modification of the system. In one embodiment, the transactional data comprises maintenance data. Maintenance data (or any type of transactional data) may include what component was added or removed from the system of FIG. 3 , such as one or more of the pumps 302 , 310 and/or separators 306 , 314 . Maintenance data may also include the part number, the manufacturer of the component, the individual who made the addition or removal of the component, the time and/or date of the modification, or other situational data surrounding the intentional input or output to the system.
As shown in FIG. 1 , the method may further include step 104 which comprises the selection of at least a portion, if not all, of the information from the system-wide information collected at step 102 to conduct statistical analysis upon. In one embodiment, it may be determined that all the data collected may be utilized, however, in other embodiments it may not be either feasible and/or desirable to utilize all of the collected data. For example, several industries, including the oil and gas industry, employ complex systems that comprise thousands of sensors in a plurality of different configurations. For example, a pump, such as pump 302 may report a measured parameter every second or even several parameters every second, whereas another sensor located either upstream or downstream front the pump, such as sensor 224 may only report a sensor parameter every minute or hour. As would be appreciated by those skilled in the art, it may not be feasible to utilize every value from every sensor given the large quantity of sensors and/or parameter values for those sensors. Therefore, in one embodiment, the step of selecting which of the collected system-wide information to conduct statistical analysis on comprises the utilization of a threshold.
A threshold may be any value point in which parameters either above or below that value point are not considered in further analysis. For example, the utilization of every data point may introduce errors from impacts that are not likely to occur again. Using collected extraneous data as an example, the exclusion of event data regarding weather that is unlikely to occur again through a predefined time-period may be beneficial. A frequency threshold may also be utilized to exclude data associated with such an event or any event that did not occur above a certain frequency. For example, parameters obtained from a sensor regarding the wind (e.g., speed and/or duration), rainfall (e.g., speed, duration, accumulation), or combinations thereof may be utilized. Either taken individually or in combination, such sensor parameters may define a time period for Which to exclude operational data and/or transactional data correlating to that particular time of the event.
In yet another embodiment, an impact threshold may be utilized remove a portion of the collected data from further analysis. For example, if a repetitive occurrence routinely or consistently provides an impact below a significant amount, data associated with the impact may be excluded. In yet another embodiment, the impact is considered unavoidable. The impact threshold may be environmental, economic, relate to health and safety, and combinations thereof.
Further embodiments of the invention may include step 106 , where one or more features or attributes are built from operational data from at least one of the plurality of sensors in the system. Such a process may be useful, for example, to investigate what sensors provide data of interest, how to best amplify the signals with transformations or features, and determine what transformation or features are most pertinent for a given sensor. Those skilled in the art will readily appreciate that there are a wide variety of features that may be used in the various embodiments of the invention. Some exemplary features and their descriptions are provided in Table 1. The inventors have found the features provided in Table 1 to provide successful and favorable results, however, the scope of the invention is not limited to the disclosed features. Furthermore, those skilled in the art will readily appreciate that one or more different features may be applied to specific groups of sensor data while other features are applied to another group. Still yet, in certain embodiments, specific sensor data may not have features applied.
TABLE 1
Exemplary Features
Features
Descriptions
Mean amplitude
1 st order moment from interpolated series
Std dev amplitude
2 nd order moment
Skewness amplitude
3 rd order moment
Kurtosis amplitude
4 th order moment
Fraction of outliers
Mean, Std dev,
1 st , 2 nd , 3 rd , and 4 th order moment from the Fast
Skewness and
Fourier Transform (FFT) spectrum
Kurtosis spectrum
Peak freq
Non-zero fraction
Non-zero fraction of time samples
# of diff
The number of different sampling rates in raw
sampling rates
time series
Singular 12
From the SVD of data matrix, the ratio of the
value ratio
largest singular value to the next largest
Singular 34
value ratio
Sval exp slope
Least squares slope estimate of log singular
value vs. # of singular values ordered from the
largest to the smallest
Sval reg R{circumflex over ( )}2
R-squared value of the slope estimator
Sval reg F statistic
F-statistic of the slope estimator
# of thrU crossings
@ of samples that are above up threshold (mean +
k * sigma) from interpolated time series after
constant false alarm rate (CFAR) processing
@ of thrD crossings
# of samples that are below down threshold
DWF coeff
The four most important DWT coefficients with
1, 2, 3, & 4
Villasenor DWT filter
In certain embodiments, step 106 may be incorporated into step 104 , yet in other embodiments, step 106 is independent from step 104 . For example, in one instance where step 106 is incorporated into step 104 , the features are applied to data before step 104 , and thus the results of step 106 may be used in determining which of the sensor data is utilized in one or more further steps. In another embodiment, step 106 may be conducted after 104 , however, the results of step 106 may be used in subsequent processes utilizing step 104 . Specifically, in one embodiment, upon the application of the features, it may be determined to alter the selection of the portion of the collected system-wide information that is utilized. Thus, step 104 may be repeated. Yet in embodiment where steps 104 and 106 are independent, step 106 may only be used on a subset of the data selected in step 104 . Yet, in other embodiments, step 106 may be omitted.
As shown in step 108 , a plurality of statistical models may be applied to the selected operational data, extraneous data, and transactional data (whether with, partially with, or without one or more features applied to at least a portion of the selected data). Specifically, the models are applied to determine a best-fit model in regards to the correlation among the operational data and extraneous data with the transactional data to predict events and impacts of the predicted events. In one embodiment, each of a selected group of statistical models are applied to the data. Yet in another embodiment, only one or more specific statistical models are applied to specific data. For example, if one statistical model is more accurate at predicting a specific event and/or the impact of that loss when applied to data specific to one or more sensors, then the model(s) may only be applied to that data. In yet further embodiments, as systems change or extraneous forces upon the systems change, one model that was highly accurate when applied to specific data may no longer be the best model, thus according to certain embodiments, the models may be used to further test the accuracy of selected models. Furthermore, step 108 may further comprise the investigation of any correlation of specific sensor data with other sensor data.
Those skilled in the art will readily appreciate that there are a wide variety of statistical models that may be used in the various embodiments of the invention. Some exemplary models that may be used in accordance with one or more embodiments of the invention include a Baysean Network which provides a probabilistic approach where a structured model is created with conditional probabilities defined for relationships between nodes in the model. Similarity Based Modeling (i.e., SmartSignal SBM) may be also be used as a non-parametric technique that constructs a function surface entirely based on training data by using interpolation to produce estimates for every point. Decision Trees may also be used, where internal nodes are simple decision rules on one or more attributes and leaf nodes are predicted class labels. Other algorithms that may be used include Multivariate Linear Regression and Support Vector Machines. The inventors have also discovered that Multivariate Gaussian models are especially accurate in specific embodiments of the invention to predict loss events in the oil and gas extraction industry.
The models may be used to provide an outcome for predicting events and impacts of the predicted events. The predicted events are events which will cause a loss in terms of economic, environmental, and/or health and safety. In one embodiment, impacts are measured in regards to specific economic impact, environmental impact, and health and safety impact. In certain embodiments, step 110 may be utilized to apply the best-fit model to predict events and impacts of the predicted events. For example, FIGS. 4A and 4B show exemplary displays of predicted events. FIG. 4A shows an exemplary display that graphically presents predicted loss events. The display may also include historical and substantially recent or present events. FIG. 4B shows an exemplary display that schematically presents the predicted loss events shown in FIG. 4A , such as for conveying information of where within the system the predicted event may occur. Those skilled in the art will readily understand that FIG. 4B may be presented in conjunction with, or independently of FIG. 4A , and vice-versa.
Looking first to FIG. 4A , display 400 extends along an x-axis and a y-axis. In one embodiment, the y-axis is divided into discrete components or subunits of a system, such as the system shown in FIGS. 3 and/or 4 B. In another embodiment, each element of the y-axis comprises a category of loss. Thus, in both exemplary embodiments, the elements of the y-axis does not show data collected from a sensor, but rather specific loss(es) that are predicted (or have occurred). For example, the first component along the y-axis is component 402 . Component 402 may represent what is referred to in the oil and gas industry as a Mono-Ethylene Glycol System (“MEG system”). Specifically looking to FIG. 4B , exemplary display 410 shows a portion of a system having a MEG subsystem (element 412 ). For example, any gas transported to element 332 of FIG. 3 may enter through element 408 shown in FIG. 4B , pass through various components and subsystems and be delivered to the MEG system 412 . Indeed, in one embodiment, the entire system including all the subsystems shown in FIG. 3 may be provided in display 410 , thereby providing a user with a system overview. In certain embodiments, the user may zoom into or otherwise select groups of subsystems or individual subsystems. As shown within element 412 . Which represents the MEG system, the system typically comprises an injection unit 411 that injects material having anti-freeze like properties into the flow lines transporting gas to limit or prevent gumming. Thus, by using a MEG system, more oil and/or gas may be extracted over a set period of time. Historically, however, it is hard to predict the failure of the MEG system and even more difficult to predict the impact of the failure on a process or business level.
Returning to FIG. 4A , the x-axis of display 400 represents time. The time may be divided into any measurement of time, such as days, hours, minutes, seconds, or combinations thereof. For discussion purposes only, each time division in display 400 is 1 day. In one embodiment, the display may be adjusted or manipulated by a user. For example, a user may expand upon the predicted loss event, such as altering the time scale to determine a specific hour or minute the predicted loss event is to occur. Looking to display 400 , the majority of the display is a uniform shade, indicating that a loss event is not predicted (or has not occurred). There are, however, some different shades in the chart that are indicative of a loss event. Looking specifically to component 402 (representing the MEG system), a loss event is not expected for several days, however, as indicated by element 404 , there is a predicted loss event. For example, while the MEG system prevents gumming of the lines, too much water in the flow lines may result in salt build up within the lines. Thus, the shading and/or coloring of element 404 may be used to indicate the estimated loss or the severity of the loss. Indeed, knowing an estimated time-frame for a predicted loss event may be advantageous in further reducing the impact. For example, most industrial processes have “planned kisses.” For example, production facilities may have scheduled down times where the production of products or services are reduced or ceased. For example, systems may need to be flushed and/or refueled on a routine basis. Thus, by knowing the timing of the planned losses and the estimated timing of the predicted loss, it may be feasible to take corrective or remedial measures during the planned loss events to prevent the unplanned loss event. In one embodiment, a cheaper corrective measure may be feasible as a short-term fix to allow the system to operate until taking a second more-intensive corrective measure during the planned loss period. Furthermore, in the embodiment shown in FIG. 4A , both historical data and predictive data are displayed. The user may “click on” or otherwise select past data to determine what the loss event was, the severity of the loss event, and/or the corrective measure taken in an attempt to mitigate or eliminate the loss event. In this regard, if another loss event for that category or component is predicted, the user may readily view the past corrective measures to determine the effectiveness of past actions.
FIG. 4C shows another exemplary display 420 that may be used in conjunction with one or more embodiments of the invention. Specifically, upon conducting step 110 shown in FIG. 1 , where the best fit model is applied to determine loss events and the predicted impact of the loss events, display 420 may be used to provide information regarding the timing, location, severity, and cause(s) of the loss event. As seen in the upper portion of display 420 , the shading of element 404 indicates that there is a severe predicted loss event within a specific time-frame for the MEG system (represented by row 402 ). The bottom portion of display 420 provides a schematic diagram of one or more subsystems of the system that may be used to more clearly show where the predicted loss is likely to occur. In one embodiment, visual cue 422 may be associated with one or more components of the MEG system 412 to indicate the location of the predicted loss event. In other embodiments, a user may zoom into or otherwise view information regarding individual pieces within specific components that are likely to fail, so the user can determine if one is readily available or be ordered.
In another embodiment, the potential cause(s) of the predicted loss event may also be graphically displayed. Specifically, element 424 (labeled “Temperature sensor”) may represent a temperature sensor on a pipe carrying gas or oil. Temperature sensor 424 may be highlighted or otherwise marked to indicate a potential cause of a loss. The marking may be used to indicate that the temperature within the pipe has exceeded a predefined limit or has risen at a pace that is above a predefined limit. For example, as discussed above, an increase in the temperature of the pipes carrying oil and/or gas may indicate an elevated concentration or volume of water within the pipes. In one embodiment, the user may “click on” or otherwise select temperature sensor 424 to determine the temperature, the rate of increase, or other information. Furthermore, display 420 may also be associated with displays 500 and 510 of FIGS. 5A and 5B , as discussed in more detail below, to view potential preventative measures.
While the use of coloring and/or shading has been described to convey exemplary embodiments, any indicia that visually conveys a severity of the loss is within the scope of this invention. Furthermore, those skilled in the art will readily understand that other cues, such as sounds, may be used in conjunction with or independent of the visual cues to indicate a loss or severity of said loss. For example, another exemplary view of predicted losses is shown in FIG. 5A . Display 500 extends along an x-axis and a y-axis. The y-axis represents the predicted loss based upon millions of barrels of oil (abbreviated in the oil and gas industry as “MBOE”). The x-axis of display 500 represents the estimated costs based upon business impact. For example, element 502 , labeled “MEG System O” is predicted to result in a loss of about 54 to about 59 millions of barrels of oil and an estimated total cost of about 3200 to about 3450. Utilizing the exemplary view in FIG. 5A may be useful when users want to quickly determine what subsystems or components are likely to result in a loss event. Display 500 may also be adjusted to show specific time periods, for example, to display any predicted loss events until the next planned shutdown of a process (planned loss event).
Yet in another embodiment, the user may be able to determine more information regarding the loss event, such more specific information regarding the component or subunit expect the fail, and/or the impacts of the loss event in regards to the economic impact, the environmental impact, and/or the impact on the health and safety. For example, FIG. 5B shows an exemplary display ( 510 ) that may provide information regarding a predicted loss event and actions to correct or remedy the loss event. For example, display 510 may be presented to a user that “clicks on” or otherwise selects to view the loss event 502 shown in FIG. 5A . In another embodiment, display 510 may be presented to a user upon “clicking on” or otherwise selecting a portion of the MEG system 412 of FIG. 4B .
As shown in FIG. 5B , display 510 extends along an x-axis and a y-axis. The y-axis represents the predicted average loss based upon millions of barrels of oil. The x-axis represents the estimated costs for each of the displayed preventative measures. As seen, preventative measures 512 , 514 , and 516 , are each shown by way of the average loss in oil and average total costs. For example, performing either “Corrective” measure (element 512 ) costs slightly less than performing “Preventative Maintenance” measure (element 514 ), however, “Preventative Maintenance” ( 514 ) results in losing much less in terms of MBOE. Conversely, “Predictive Measure” (element 516 ) costs more than both of the above alternatives (elements 512 and 514 ), however, results in much less loss when measuring MBOE. In certain embodiments, the preventative measures ( 512 , 514 , and 516 ) may also be viewed in context of not performing any action to eliminate or reduce the impact of the predicted loss event. For example, element 518 (labeled “Breakdown”) indicates the predicted loss due to not taking any corrective or preventative action.
As would be appreciated by those skilled in the art, the determination of the severity of the loss event may be tailored to a specific business' need. For example, corporations are becoming increasingly aware that consumer's purchasing decisions may be based on how the company is perceived on impacting the environment. Therefore, in one embodiment, even a slight environmental impact coupled with a large economic impact, may be treated as significantly more important than even an economic impact that is twice as large. Likewise, any predicted loss regarding the health and safety of workers or surrounding residents may be treated significantly more important, even when not coupled with an economic and/or environmental impact.
Step 112 may then be applied to determine at least one intervention that may reduce or eliminate the impact of the predicted event(s). In select embodiments, the intervention(s) may be displayed on a display device, such as being associated with display 510 . In one embodiment, interventions are displayed on a display device, wherein at least one intervention differs from another intervention in regards to at least on impact selected from the impact group consisting of: environmental, economic, health and safety; and combinations thereof. For example, a first intervention that calls for repairing a first component may dramatically reduce the economic impact, however, may not substantially reduce an environmental impact, in contrast, a second intervention may reduce the economic impact to a lesser extent, however, will substantially reduce an environmental impact. In certain situations, the second intervention will require different actions and/or components to be repaired than if the first intervention is undertaken. Yet in other situations, the interventions may differ in only the time and/or worker to conduct at least a portion of the intervention.
As seen in FIG. 1 , as an intervention is applied (for example, following the determination in step 112 ), more data could be collected, such as by repeating step 102 . While the repetition of step 102 is shown in FIG. 1 as following step 112 , the collection of data may be continuous throughout the process and be conducted before, during, or after any of the other steps shown in FIG. 1 . Furthermore, other methods may be utilized in conjunction with or independently of the preceding steps. For example, step 114 may be conducted following the preceding steps.
At step 114 , the accuracy of the best fit model may be determined, specifically, the actual outcome in terms of economic, environmental, and health and safety can be compared with the predicted outcome according to the predictions based upon the best fit model Not only can the impacts be measured and compared, but the time period in which the loss event was predicted to occur may be compared with the actual timing of a loss event. Indeed, any prediction directly or indirectly based upon the best-fit model may be compared at step 114 . In addition or as an alternative to determining the accuracy of the best fit model, the actual outcome may be compared to other models, such as the models from step 108 , to determine if another model is more accurate than the best-fit model initially chosen at step 108 .
The present invention has been described herein with reference to specific exemplary embodiments thereof. It will be apparent to those skilled in the art that a person understanding this invention may conceive of changes or other embodiments or variations, which utilize the principles of this invention without departing from the broader spirit and scope of the invention as set forth in the appended claims. All are considered within the sphere, spirit, and scope of the invention. | Current monitoring systems often provide the operating condition of a specific component and do not consider the impact of a specific failure upon an entire system or a business. Nor do the current systems provide an avenue for the business to predict the loss, as well as its impact, and make an educated decision of mitigating the loss based upon economic, environmental, and health and safety considerations. Methods and systems are provided for predicting loss events, impacts of loss events, and providing potential corrective measures to reduce or eliminate the occurrence or impact of the loss events. One aspect relates to the use of system-wide information to predict variables that are directly linked to business impact, such as production loss. Extraneous and transactional data are also utilized according to other aspects of the invention. | 6 |
STATEMENT REGARDING FEDERALLY SPONSORED RESEARCH OR DEVELOPMENT
[0001] This invention was made with Government support under Contract DE-AC0576RL01830 awarded by the U.S. Department of Energy. The Government has certain rights in the invention.
BACKGROUND
[0002] In the context of information analysis, analysts are challenged not only by the vast amounts of data that they must sift and refine, but also by the different types and sources of data that they must reconcile. For example, data requiring analysis can be in the form of text, imagery, audio, maps, sensor data, and others, and can come from any variety of sources including, but not limited to, the Internet, media outlets, telephone conversations, the intelligence community, and digital communications. During the analysis process, effective analysts fuse relevant information and identify connections between the seemingly disparate data. However, oftentimes, the fusion process is performed manually and the analyst is required to juggle in his/her mind various pieces of data. In the least, information loss and traceability in developing the analytic product can occur as a result.
[0003] Analysts having an effective fusion solution can focus on exploring and analyzing data, rather than integrating it. Accordingly, a need for automated approaches and tools for generating fusible signatures of information contained in two or more corpora of data exists.
SUMMARY
[0004] Embodiments of the present invention include methods, computer-executable instructions on computer-readable media, and systems for generating fusible signatures for information contained in two or more corpora of data. The fusible signatures can allow the information from the separate corpora of data to be merged, or fused, into a single information space that allows analysts to explore, analyze, and/or process the fused data. Prior to manipulation by the embodiments of the present invention, the information contained in at least one of the individual corpora of data is typically represented by initial signatures that are not directly fusible with information in the other corpora of data because of differences, for example, in dimensionality, source, data type, basis, and/or the space in which the initial signatures reside.
[0005] While a variety of embodiments of the present invention are contemplated, in a preferred embodiment, two or more corpora of data that are of interest each comprise documents characterized by initial signatures. A set of reference points is determined for each corpus of data, and all of the sets have the same number of reference points. Each reference point is characterized by a reference signature, and each reference point has an equivalent reference point in the other sets as determined by pre-defined criteria. A similarity measure can then be quantified for each combination of one initial signature from a given corpus of data with one reference signature from its associated set of reference points. The similarity measure represents the similarity between the initial signature and the reference signature. A fusible signature having a dimensionality equal to the number of reference points is generated by populating a vector for each document, wherein the vector for a given document comprises all of the similarity measures quantified from combinations involving the initial signature for the given document. In some embodiments, a new signature, which is also fusible, is generated for each reference signature in the same manner. The new reference signature is referred to herein as a fusible reference signature.
[0006] As used herein, a “document” refers to the smallest information unit that is represented by a signature. Documents are not limited to information in the form of text, but can broadly include audio, video, imagery, map, sensor data, and other forms of information that can be represented by a signature.
[0007] A collection of documents is referred to as a corpus of data. A corpus of data does not have to be static, but can be dynamic, evolving over time as information is added or removed. An example of a dynamic corpus of data can be a real-time stream of data. Each corpus of data exists in an information space. An information space is a set of information encoded into a specific representation. The information space for dynamic corpora can either evolve with the data or it can remain static in a static context based, for example, on features of importance. It is important to note that, an information space is not necessarily a mathematical construct in the same way as a signature space or vector space. A signature space is an information space in which the representations are signatures. Similarly, a vector space is an information space in which the representations are vectors.
[0008] “Signatures” refer to mathematical representations of documents that characterize aspects of the documents (e.g., content, semantic significance, object properties or features, etc.) and allow for computational analysis and/or visualization of the documents. An exemplary signature can comprise an N-dimensional vector representing, in signature space, a document on a semantic basis. However, not all signatures are necessarily vectors, nor are they necessarily based on semantics. The initial signatures can have a basis including, but not limited to, temporal, sentiment, events/activities, transactions, geospatial, and network topologies. Fusible signatures, as used herein, are ones that have been transformed from their original dimensionality, space, and/or basis, which may have been initially different, into ones that can be directly fused into a common dimensionality, space, and/or basis. For example, without transformation, initial signatures from a first corpus of data may not be fusible with initial signatures from a second corpus of data because they differ in terms of dimensionality, meaning, basis, the type of data represented by the initial signature, and/or the information space in which the signatures reside. However, according to the embodiments described elsewhere herein, the initial signatures can be transformed into a common form that is fusible.
[0009] “Reference points” are objects represented by reference signatures in the same information space as their associated initial signatures. According to pre-defined criteria, reference points in one set have corresponding and equivalent reference points in each of the other sets, which provides an ability to join, or fuse, the separate corpora of data together as described elsewhere herein. For purposes of conceptual clarification, but not for determination of the scope of the invention, the collective sets of reference points can be viewed metaphorically as a Rosetta stone. The equivalence between reference points across sets provides points of commonality across the information spaces containing the corpora of data to enable fusion. Exemplary reference points can, but do not necessarily, comprise documents within a corpus of data. The origin in three-dimensional space can serve as a weak analogy of reference points for two different data sets, whether or not a data point exists in one of the two data sets.
[0010] “Similarity measures” and “difference measures” as used herein, refer to types of statistical distance measures. Examples of statistical distance measures can include, but are not limited to, Euclidean, Mahalonobis, and Bhattacharyya distances. In the context of vectors as signatures, similarity can be quantified, for example, using distances or cosine measures between vectors.
[0011] In some embodiments, the fusion of the corpora of data can be accomplished using the fusible signatures as well as representations of relationships between the reference points. More specifically, for each set of reference points, a representation of relationships between the reference points in the set is constructed, wherein the representations are based on the respective fusible reference signatures. Furthermore, distances between fusible signatures and fusible reference signatures are determined in a space containing the fusible signatures. The separate representations of relationships are joined into a combined representation while altering at least one value in at least one reference signature to minimize difference measures between equivalent reference signatures. The documents are arranged in the combined representation according to each document's fusible signature while altering at least one value in at least one fusible signature to minimize changes to the distances between fusible signatures and fusible reference signatures previously determined. A new vector can then be populated for each document to generate a fused signature. The new vector for a given document comprises values from the fusible signature of the given document after the document had been arranged in the combined representation and the fusible signature had been altered as necessary to enable its arrangement in the combined representation. The fused signature (i.e., the new vector) replaces the initial signature as the representation of the document.
[0012] Representations of relationships, as used herein, can refer to computer-implemented constructs that describe relationships among signatures. Accordingly, one example of a representation includes graphs and/or the data structures representing them. Exemplary data structures can include, but are not limited to, list structures, matrix structures, and combinations thereof. In a particular embodiment, a graph is N-dimensional and can use N-dimensional signatures, wherein nodes represent the signatures, and the spacing between nodes is related according to a known function (e.g., proportional) to the similarity between documents represented by the signatures. In embodiments where the representations of relationships are graphs, the individual representations can be joined into a combined representation using one or more graph algorithms. Exemplary and appropriate graph algorithms can include, but are not limited to, force-based algorithms, neural network algorithms, self-organizing map (SOM) algorithms, simulated annealing algorithms, and genetic algorithms. Generally, appropriate algorithms optimize an objective function, which, for the present embodiment, is to reduce the stresses and/or errors in the graph layout. Alternative objective functions can include, but are not limited to, maintaining neighborhoods and maintaining global structures.
[0013] The purpose of the foregoing summary is to enable the United States Patent and Trademark Office and the public generally, especially the scientists, engineers, and practitioners in the art who are not familiar with patent or legal terms or phraseology, to determine quickly from a cursory inspection the nature and essence of the technical disclosure of the application. The summary is neither intended to define the invention of the application, which is measured by the claims, nor is it intended to be limiting as to the scope of the invention in any way.
[0014] Various advantages and novel features of the present invention are described herein and will become further readily apparent to those skilled in this art from the following detailed description. The preceding and following descriptions show and describe preferred embodiments of the invention by way of illustration. As will be realized, the invention is capable of modification in various respects without departing from the invention. Accordingly, the drawings and descriptions of the preferred embodiments set forth hereafter are to be regarded as illustrative in nature, and not as restrictive.
DESCRIPTION OF DRAWINGS
[0015] Embodiments of the invention are described below with reference to the following accompanying drawings.
[0016] FIG. 1 is an illustration depicting the generation of fusible signatures, and the fusion, of two different corpora of data according to one embodiment of the present invention.
[0017] FIG. 2 is an illustration depicting a visualization of a corpus of data.
[0018] FIG. 3 is an illustration depicting a visualization of a corpus of data.
[0019] FIG. 4 is an illustration depicting a visualization of the fused signatures.
DETAILED DESCRIPTION
[0020] The description provided herein includes the best mode of one embodiment of the present invention. It will be clear from this description of the invention that the invention is not limited to these illustrated embodiments, but that the invention also includes a variety of modifications and embodiments thereto. Therefore the present description should be seen as illustrative and not limiting. While the invention is susceptible of various modifications and alternative constructions, it should be understood, that there is no intention to limit the invention to the specific form disclosed, but, on the contrary, the invention is to cover all modifications, alternative constructions, and equivalents falling within the spirit and scope of the invention as defined in the claims.
[0021] FIGS. 1-4 present graphically a variety of embodiments and/or aspects of the present invention. Referring first to FIG. 1 , an illustration depicts an embodiment of the present invention wherein fusible signatures are generated for two different corpora of data and are then fused into a single space. Initially, each of the two corpora of data comprises a plurality of documents characterized by initial signatures, which are represented by dots 101 , 102 in their respective visualizations 100 , 103 . The initial signatures from one corpus of data exist in a signature space 105 that is different than the signature space 106 of the initial signatures from the other corpus of data. Five reference points 104 , 112 have been pre-defined and are numbered 1 through 5 . Equivalent reference points between the sets of reference points are assigned the same number label. Several criteria have been applied in selecting the reference points. For example, the signature spaces 105 , 106 will have specific dimensionalities, and the number of reference points must be at least one more than the maximum dimensionality of either of the signature spaces. Furthermore, the reference points should ideally span both spaces. In other words multiple reference points should not be substantially co-located (e.g., characterize similar aspects) because in that instance, they will likely not provide the resolution necessary to generate fusible signatures that accurately represent the documents in the corpora of data.
[0022] One way to minimize the occurrence of co-located reference points is to compute both signature spaces with a set of reference points of desire and then use a mapping of clusters to determine whether the reference points reflect the diversity of the spaces or whether additional reference points are needed in certain areas. An alternative approach involves examining the reference points in relation to the initial signatures and each respective space and identifying those reference points that maximize the values in all the dimensions. Once a base set of reference points is determined, it can be increased, as appropriate, to be a distribution of the signature spaces.
[0023] Having selected the two sets of reference points and defined their equivalents, the initial signatures can be transformed into fusible signatures. The transformation can involve defining an order for each of the reference points that becomes a definition of the dimensions in new spaces containing the fusible signatures. The similarity measures are then quantified for each initial signature-reference signature combination. In other words, for a given initial signature representing a document in one of the corpora of data, similarities are quantified to each of the reference points in the corresponding set. The quantification occurs for every document in both corpora of data with respect to the corresponding set of reference data. Accordingly, each document has five similarity measures that characterize the similarity of that document to the five reference points in the corresponding set. The fusible signature is populated with the five similarity measures in the order defined previously.
[0024] The same approach is taken to transform the reference signatures from their respective signature spaces 105 , 106 into the fusible signature spaces 108 , 109 . In other words, similarity measures are quantified for each reference signature with respect to all of the reference signatures in the same set. For example, the fusible reference signature of a particular reference point comprises similarity measures from its reference signature to all five of the reference signatures in its set. The similarity measures are then used to populate a fusible reference signature 111 in the order defined previously for the fusible signatures. Accordingly, one similarity measure in each of the fusible reference signatures will indicate complete similarity because each reference signature is completely similar to itself. As used herein, reference signatures after being transformed into the space containing fusible signatures, are referred to as fusible reference signatures.
[0025] Whereas the initial signatures 101 , 102 in the two corpora of data were different based on dimensionality, the space in which they existed, and/or on their basis, the fusible signatures have been transformed to enable fusion, where common operators (e.g., visualizations, QBE, etc.) can still apply and synergies between datatypes can be exploited. It is significant to note that extensive knowledge databases are not required, but only the documents within the corpora of data, and their initial signatures.
[0026] Having transformed the initial signatures 101 , 102 and the reference signatures 104 , 112 into fusible signatures and fusible reference signatures, respectively, the corpora of data can now be merged, or fused. Referring still to the embodiment illustrated in FIG. 1 , graphs 113 , 114 can be constructed for each set of reference points reflecting the distances between reference points in their respective fusible signature spaces. For each corpus of data, distances between fusible signatures and reference signatures are determined in the spaces 108 , 109 containing the fusible signatures. Accordingly, in one respect, the two graphs represent the layout in their respective fusible signature spaces. The graphs are then joined at equivalent reference points by applying a non-linear mapping based on a forced directed layout graph algorithm, thereby creating a single, combined graph 116 . Regardless of the particular graph algorithm applied, the fundamental aim is to rearrange the layout of both fusible signature spaces such that equivalent reference points, as represented by fusible reference signatures, between the two sets are proximally located, or even co-located, while maintaining the relationships between reference points within each set. Once the fusible reference signatures have been arranged, the fusible signatures are laid out against the combined graph using the same, or a similar, graph algorithm. While laying out the fusible signatures on the combined graph, only the fusible signatures are allowed to move (i.e., fusible signature values are allowed to change) against the fusible reference signatures, which are now fixed, in order to minimize changes to the distances between fusible signatures and reference signatures. After being joined, the fixed, fusible reference signatures are referred to as fused reference signatures and represented 117 , 118 on the combined graph. Regardless of the particular graph algorithm applied to layout the fusible signatures on the combined graph, the fundamental aim of allowing at least some values within at least some fusible signatures to be altered is to maintain relationships between the fusible signatures and the fused reference signatures, as the relationships were first determined in the context of the fusible signatures and the fusible reference signatures. The final state of the fusible signatures, having been altered as necessary for optimal arrangement on the combined graph, become fused signatures. The fused signatures from both corpora of data are now in a common basis, exist in the same space, and have the same dimensionality. Furthermore, they can be used in a multitude of analytic and visualization processes. For example, clustering and visualization processes can be applied to generate a two-dimensional representation 119 of the documents and reference points according to the fused signatures and the fused reference signatures, respectively.
Example
Generation of Fusible Signatures, and Fusion, of English and Spanish Texts
[0027] Fusible signatures were generated, and subsequently fused, from two different corpora of data comprising English and Spanish documents. The corpora of data 200 , 300 were both generated from a set containing 2228 Associated Press English news stories from 1988 (AP88). The news stories were translated into Spanish by a machine translator. The English corpus 200 and the Spanish corpus 300 each totaled 1000 news stories, wherein each news story comprised a document. However, only 710 documents in each corpus were direct translations of each other. The remaining 290 documents in each corpus were not corresponding translations of each other, but were judged to be similar based on characterizing and clustering of the entire 2228 English news stories. The two corpora are depicted as clustered visualizations in FIGS. 2 and 3 , respectively. Signatures for the documents in both corpora were generated using a term-frequency-multiplied-by-inverse-document-frequency (TF-IDF) approach. The resultant initial signatures had a dimensionality of 200 (i.e., N=200).
[0028] Embodiments of the present invention were then applied to the corpora of data by first identifying an ordered list of N+1 (e.g., 201) reference point pairs of documents from the test corpora. Each pair consisted of an English document and a Spanish document. The corresponding English and Spanish documents were defined as equivalent reference points spanning the two corpora of data. Since each document had one associated initial signature, it follows that each reference point had two associated reference signatures, one relevant for the English corpus and one relevant for the Spanish corpus.
[0029] As part of selecting reference points, k-means clustering was performed to cluster each corpus's signatures. The reference points were then chosen such that each cluster contained at least one reference signature associated with a reference point. Additional reference points and their associated reference signatures were chosen to meet the minimum desired number of pairs (e.g., 201) for the sets of reference points. This approach to choosing reference points ensured that the reference points were well distributed within the information spaces of the corpora of data, thereby minimizing significant repetition of content among reference points.
[0030] From each document's initial signature vector, which was generated by the TF-IDF approach, a new signature vector was derived consisting of rank-ordered distances of the initial signature to each reference point's relevant reference signature. Distances between initial signatures and reference signatures were determined according to a Euclidean distance measure. The resultant “fusible” signatures comprised vectors all having a common representational basis (i.e., rank-ordering from reference points). Fusible signatures of the reference points were similarly generated.
[0031] A refined fusion of the fusible signatures was then performed using a graph layout strategy. The fusible vectors for the reference points were used as nodes in two mathematical graphs, one for the English corpus and one for the Spanish corpus. Each reference point pair was represented by two nodes, one corresponding to the English document and its fusible reference vector, and one corresponding to the Spanish document and its fusible reference vector. The nodes were considered to be located in a vector space, with their fusible vectors being coordinates in their respective spaces. An edge was added to connect each English-Spanish reference point pair. Edges were also added between all pairs of English nodes and all pairs of Spanish nodes.
[0032] Target lengths were then associated with each edge. For intra-language edges (e.g., within each set of reference points), the target length was the initial length (i.e., distance between the nodes). For the inter-language edges (e.g., spanning the sets of reference points), the target length was zero, since the goal in applying the layout algorithm was to have each reference point's two nodes pulled together, since they were previously defined as being equivalent.
[0033] To optimize the node positions, a force-directed graph layout algorithm was employed, wherein each edge of the graph was treated as an idealized spring with force proportional to the difference between its actual length and its target length. These simulated forces were applied to nodes, causing them to be repositioned, thereby modifying the lengths of edges between nodes. A fixed number of iterations of this algorithm was executed, and then the actual length of the English-Spanish edges was measured. Had any actual length exceeded an arbitrary preset maximum tolerance, that edge would have been removed prior to resuming the iterations. The repositioned fusible reference signature was considered to be a fused reference signature.
[0034] Having fused all of the fusible reference signatures into a common graph, all of the fusible signatures representing the documents in the corpora were added in the same fashion, as nodes in the common graph. For each fusible signature, edges were added to all relevant reference point nodes (e.g., from an English fusible signature node to an English fused reference point node). The target lengths for these edges were the actual node-to-node distances in the English-only or Spanish-only graph.
[0035] The same force-directed graph layout algorithm was then applied to the new nodes and edges, again treating each new edge as an idealized spring. The existing reference point nodes and edges were held in fixed positions, and simulated forces were applied to the new nodes and edges. Again, a fixed number of iterations were executed. The final vector space coordinates of the nodes were considered to be the fused signatures.
[0036] The final vectors were clustered to verify that corresponding English-Spanish documents were occurring in the same clusters at a rate significantly higher than what would be expected from random grouping. The clustered visualization 400 is depicted in FIG. 4 .
[0037] While a number of embodiments of the present invention have been shown and described, it will be apparent to those skilled in the art that many changes and modifications may be made without departing from the invention in its broader aspects. The appended claims, therefore, are intended to cover all such changes and modifications as they fall within the true spirit and scope of the invention. | Methods, computer-executable instructions on computer-readable media, and systems for generating fusible signatures for information contained in two or more corpora of data. The fusible signatures can allow the information from the separate corpora of data to be merged, or fused, into a single information space that allows information analysts to explore, analyze, and/or further process the fused data. Prior to manipulation by the embodiments of the present invention, the information contained in at least one of the individual corpora of data is typically represented by initial signatures that are not directly fusible with information in the other corpora of data because of differences, for example, in dimensionality, source, data type, basis, and/or the space in which the initial signatures reside. | 6 |
TECHNICAL FIELD
The present invention is concerned with a novel class of inhibitors of fibrin cross-linking and/or of transglutaminase activity, and in particular, with such inhibitors which may be, for example, derived from leech tissue and/or from leech secretions.
BACKGROUND OF THE INVENTION
Enzymes known as transglutaminases are primarily responsible for the stabilisation of many protein aggregates, such as for example, in blood clot formation. The cross-linking of proteins by the action of transglutaminases is the major way in which, for example, fibrin clots are stabilised. In mammals, stabilisation of blood clots is brought about by a transglutaminase, known as Factor XIIIa, which catalyses the formation of cross-linking between the fibres of fibrin. Cross-linked blood clots are not as susceptible to the action of fibrinolytic enzymes and are virtually insoluble in denaturing solvents, such as 5M urea.
Factor XIIIa is an atypical coagulation enzyme since it is not a serine protease but rather a cysteine-containing, transamidating enzyme which catalyses the reaction between the amino acid side chains of lysine and glutamine to form an amide link with the elimination of ammonia according to the following scheme; ##STR1## When fibrin is the substrate, R 1 --CONH 2 and R 2 --NH 2 are glutamine and lysine side chains respectively in different chains of the fibrin polypeptide.
Factor XIIIa can also catalyse the cross-linking of other proteins. For example Factor XIIIa is known to link α 2 antiplasmin to fibrin and increase resistance to fibrinolysis. Moreover it can cause cross-links between a range of disparate structural and contractile proteins such as collagen, laminin actin, myosin, thrombospondin, vinculin and vitronectin or the like. It is believed that this property is part of the wound healing process and may have a role in the pathology of a number of diseases of tissue remodelling.
It is therefore desirable to provide an inhibitor of transglutaminases which inhibitor could be used, for example, in the treatnment of various pathological or thromboembolic events. Inhibitors of translutaminases have been described previously and these generally fall into four main categories:
(a) immunoglobulins directed at the enzyme;
(b) low molecular weight substrates that compete with the natural protein substrates;
(c) reagents that react with the active site of the enzyme; and
(d) peptide fragments of Factor XIII itself.
These inhibitors are not suitable, for use in, for example, pharmaceutical formulations. for a variety of reasons, as follows:
Naturally circulating transglutaminase inhibitors have been identified previously as immunoglobulins directed at the sub-units of the transglutaminase. Such inhibitors give rise to a haemorrhagic condition caused by reduction in circulating factor XIII. U.S. Pat. No. 5,470,957 discloses using such immunoglobulins therapeutically by raising monoclonal antibodies to the transglutaminase enzyme sub-units by known techniques. A disadvantage associated with such antibodies as transglutaminase inhibitors is that they have high molecular weights and it is typically necessary to produce chimeric human analogues of the immunoglobulins before they can be used, for example, therapeutically in man.
WO91/10427 discloses transglutaminase inhibitors that are amines which act by linking to glutamine residues in one substrate to prevent cross-linking to another substrate. Such inhibitors are not very potent because they need to be present at the same concentrations as, or higher concentrations than, the natural substrate in order to have any significant inhibiting effect. Therefore they are only effective at concentrations in the region of approximately 50 μM and above.
WO92/13530 discloses using various transglutaminase inhibitors which rely on the activity of transglutaminase being largely dependent on a reactive sulfhydryl group. Therefore any reagent that alkylates or oxidises this sulfhydryl group should inhibit the activity of the transglutaminase. Such reagents are, however, very reactive and also very unstable and are therefore particularly unsuitable for use in, for example, pharmaceutical or therapeutic treatment.
Attempts to provide peptidic inhibitors which might be expected to be more specific and less toxic has so far resulted only in compounds of low potency. For example, such inhibitors are described in U.S. Pat. No. 5,328,898 and by Achyuthan K E, Slaughter T F, Santiago M A et al; in J. Biol. Chem. 268: pp. 21284-21292, 1993; "Factor XIIIa derived peptides inhibit transglutaminase activity: localisation of substrate recognition sites".
Therefore, it is the purpose of one aspect of the present invention to provide a potent inhibitor of transglutaminase enzymes and which inhibitor can be used in, for example, pharmaceutical or therapeutic use.
SUMMARY OF THE INVENTION
We have now isolated a novel polypeptide which inhibits transglutaminase activity and/or fibrin crosslinking, which polypeptide has the following amino acid sequence:
______________________________________1 10NH.sub.2 -Lys-Leu-Pro-Cys-Lys-Glu-X.sub.1 -His-Gln-Gly- 20Ile-Pro-Asn-Pro-Arg-Cys-X.sub.2 -Cys-Gly-Ala-Asp-Leu- 30Glu-X.sub.3 -Ala-Gln-Asp-Gln-Tyr-Cys-Ala-Phe-Ile-Pro- 40Gln-Z.sub.1 -Arg-Pro-Arg-Ser-Glu-Leu-Ile-Lys-Pro-Met- 50Asp-Asp-Ile-Tyr-Gln-Arg-Pro-Val-Z.sub.2 -Phe-Pro-Asn-60 66Leu-Pro-Leu-Lys-Pro-Arg-Z.sub.3 -COOH (Sequence ID NO:2).______________________________________
wherein X 1 , X 2 and X 3 each represent any amino acid residue; Z 1 , Z 2 and Z 3 each represent, simultaneously or alternatively Cys or Glu; or a pharmaceutically acceptable salt, a derivative (such as a chimeric derivative) or a bioprecursor of said amino acid sequence, or a homologue or analogue thereof of substantially similar activity. By homologue, we mean a polypeptide in which no more than 23% of the amino acids in the polypeptide chain differ from those listed. The figure of 23% is based on the fact that many homologues of hirudin occurring naturally in Hirudo medicinalis are described in the literature; the most diverse of these differ in 15 of the 65 amino acids in the polypeptide chain. By analogue, we mean that one or more additional amino acids may be interposed in the polypeptide chain, provided that they do not significantly interfere with the pharmacological activity of the polypeptide. The invention also encompasses truncated forms of the polypeptide having the above-mentioned amino acid sequence.
The polypeptides according to the invention are highly potent inhibitors of transglutaminase activity and/or fibrin cross-linking. The ability of the polypeptides according to the invention to prevent formation of protein cross-links has a dramatic effect on the instability of, for example, blood clots. The inhibitory effect of the polypeptides according to the invention on factor XIIIa can be measured by the increased solubility of fibrin clots in 5M urea. In addition the inhibitory effect of the polypeptides may be measured by utilising the fact that the polypeptides inhibit ammonia release by incorporation of ethylamine into casein and also by incorporating biotinamidopentylamine into casein.
The amino terminal domain is believed to be a particularly potent inhibitor of transglutaminase activity. The invention therefore further comprises a polypeptide which specifically inhibits transglutaminase activity, which polypeptide comprises the following amino acid sequence:
NH.sub.2 -Lys-Leu-Leu-Pro-Cys-Lys-Glu-Y-His-Gln-Gly-Ile-Pro-Asn-Pro-Arg-
wherein Y represents any amino acid residue or a pharmaceutically acceptable salt, derivative or bioprecursor thereof, or a homologue or analogue thereof of substantially similar activity (sequence ID No: 1).
The polypeptides according to the invention (which will hereinafter be referred to as the "Tridegins"), advantageously inhibit transglutaminase activity directly at concentrations in the 1-50 nanomolar range (a difference by at least a factor of 1000 relative to the known transglutaminase inhibitors of categories (b), (c) and (d) described above).
The Tridegins can advantageously form pharmaceutically acceptable salts with any suitable non toxic, organic or inorganic acid. Examples of such inorganic acids include hydrochloric, hydrobromic, sulfuric or phosphoric acid and acid metal salts such as sodium monohydrogen orthophosphate and potassium hydrosulfate. Examples of organic acids include the mono, di and tri carboxylic acids such as acetic, glycolic, lactic, pyruvic and sultonic acids or the like. Salts of the carboxy terminal amino acid moiety include the non toxic carboxylic acid salts formed with any suitable inorganic or organic bases.
The Tridegins according to the invention may be extracted from leech tissue or secretions by, for example, homogenisation of substantially the whole leech, the salivary glands or the proboscis or the like, in a suitable buffer. Transglutaminase inhibitors had not previously been identified in, or extracted from, leeches; the present invention therefore comprises an inhibitor of transglutaminase activity derivable from leech tissue or leech secretions. The term "derivable" as used herein encompasses the material which is directly derived, as well as material which is indirectly derived or converted to a chemically modified derivative.
The Tridegins according to the invention are typically extracted or purified using a combination of known techniques such as, for example, ion-exchange, gel filtration and/or reverse phase chromatography.
Leeches of the same genus, or even the same species, often have polypeptides in their saliva which have similar biochemical effects and are highly homologous in their amino acid structure. In the same species of leech, several different isoforms may exist differing by only a few amino acids.
The Tridegins according to the invention are derivable from leech tissue or leech secretions, typically from leeches of the order Rhynchobdellida. However, because many of the components of the salivary gland or tissue secretions from leeches which have similar biochemical specificity are members of such homologous families of polypeptides, the present invention also comprises such isoforms and analogues of the Tridegins according to the invention derivable from leeches. Furthermore, post-translational modification of leech polypeptides is frequently observed, and in view of the fact that some of the residues in the Tridegins could not be assigned to a known amino acid structure, the present invention also includes such post-translationally modified polypeptides corresponding to the polypeptides of the abovementioned sequences.
According to a second aspect of the present invention, there is provided an inhibitor of fibrin crosslinking and/or transglutaminase activity, which inhibitor is derivable from leech tissue or leech secretions, typically from leeches of the order Rhynchobdellida, more preferably from leeches of the genus Haementeria.
The inhibitor according to the invention preferably has an apparent molecular weight in the range between approximately 7000 daltons and 8000 daltons, as measured by polyacrylamide gel electrophoresis (PAGE), and has the ability to inhibit the factor XIIIa catalysed release of ammonia from the incorporation of amines into casein, and the factor XIIIa catalysed incorporation of biotinamidopentylamine into casein.
In addition to the effect on factor XIIIa, the Tridegins are inhibitors of many different transglutaminases as they inhibit the activity of both plasma and platelet factor XIIIa and tissue transglutaminase from guinea pig liver albeit with different potency. They are therefore also general transglutaminase inhibitors and can be expected to inhibit many different types of this group of enzymes.
The invention also comprises a diagnostic method of measuring the degree of inhibition of transglutaminase activity for an inhibitor according to the invention (as defined above), which method comprises measuring the amount of ammonia liberated from the transglutaminase catalysed incorporation of amines into casein in the presence of the inhibitor, wherein the amount of ammonia liberated and/or amine incorporation provides a measure of the level of inhibition of the transglutaminase activity by the inhibitor.
According to a further aspect of the present invention, there is provided a pharmaceutical formulation comprising an inhibitor according to the first or second aspect of the invention (as described above) and a pharmaceutically acceptable carrier, diluent or excipient therefor.
Because of the low level of toxicity and the high level of inhibition of transglutaminase activity associated with the Tridegins, they can advantageously be incorporated into pharmaceutical formulations, which formulations may be, for example, administered to a patient either parenterally or orally.
The term "parenteral" as used herein includes subcutaneous. intravenous, intraarticular and intratracheal injection and infusion techniques. Other means of administration such as oral administration or topical application may also be used. Parenteral compositions and combinations are preferably administered intravenously either in a bolus form or as a constant infusion according to known procedures.
The term "pharmaceutically acceptable carrier" as used herein should be taken to mean any inert, non toxic, solid or liquid filler, diluent or encapsulating material, which does not react adversely with the active compound or with a patient. Preferred liquid carriers which are well known, include sterile water, saline, aqueous dextrose, sugar solutions, ethanol, glycols and oils. Tablets and capsules for oral administration may contain conventional excipients such as binding agents, fillers, lubricants and wetting agents etc. Oral liquid preparations may be in the form of aqueous or oily suspensions, solutions, emulsions, syrups, elixirs or the like, or may be presented as a dry product for reconstitution with water or other suitable vehicle for use.
Such liquid preparations may contain conventional additives such as suspending agents, emulsifying agents, non-aqueous vehicles and preservatives. Topical applications may be in the form of aqueous or oily suspensions, solutions, emulsions, jellies or, preferably, emulsion ointments.
Unit doses of pharmaceutical formulations according to the invention may contain daily required amounts of the Tridegin, or sub-multiples thereof to make a desired dose. The optimum therapeutically acceptable dosage and dose rate for a given patient (which may be a mammal such as a human) depend on a variety of factors, such as the activity of the specific active material employed, the age, body weight, general health, sex, diet, time and route of administration, rate of clearance, the object of the treatment, i.e. treatment or prophylaxis and the nature of the disease treated.
It is expected that systemic doses in the range 0.05 to 50 mg/kg body weight, preferably between 0.05 and 10 mg/kg and more preferably 0.1 to 1 mg/kg will be effective. According to the nature of the disease to be treated, one single dose may contain from 0.05 to 10 mg/kg body weight whether applied systemically or topically.
The Tridegins can potentially be used to inhibit the stabilisation of forming thrombi in, for example, acute coronary syndromes, venous thrombosis or strokes and thereby enhance the effect of thrombolytic therapy or indeed the natural lytic processes. In this context the inhibition of the incorporation of fibrinolysis inhibitors like α 2 -antiplasmin into fibrin clots could provide an additional benefit.
The fact that the Tridegins also inhibit other transglutaminases very potently indicates additional potential uses anywhere that transglutaminase activity causes a pathological event. Such a role for transglutaminases has been hypothesised in Crohn's disease, tumour implantation, vessel wall thickening in atherosclerotic processes, thrombotic microangiopathy in, for example, the kidneys, fibrous growths of the skin such as scleroderma, membranous glomerulonephritis, repair of retinal damage, cataracts, acne, the formation of scar tissue and infection by various filarial nematodes. Not only can the Tridegins be used for their therapeutic action against the above or related syndromes but their high potency will allow lower doses.
This possibility is illustrated very well in WO93/18760, which describes the use of impotent inhibitor putrescine to treat hypertrophic scars with a preferred dose of 50 mM. The preferred concentration of a Tridegin in a similar circumstance is 1-100 μM.
A formulation according to the second aspect of the invention may advantageously be administered in combination with an anticoagulant, a thrombolytic, fibrinolytic, or fibrinogenolytic agent, or the like, which advantageously may increase the ability of the formulation to digest or inhibit, for example, blood clots. The anti-coagulant may comprise a polypeptide such as hirudin or heparin. Hirudin is disclosed in EP 0347376 and EP 0501821 and is a generic term for a family of homologous polypeptides found in a variety of leeches which specifically and potently inhibit thrombin and subsequently inhibit blood clotting. Similarly, a fibrinolytic/fibrinogenolytic agent such as hementin may be used whose activity is in digestion of fibrinogen, rendering it unclottable. Hementin is a fibrinolytic agent found in various leech species, and is disclosed in, for example, U.S. Pat. No. 4,390,630 and WO 91/15576.
A particular effect of Tridegins is to decrease the lysis time of both platelet-free and platelet-rich human plasma clots when lysis is induced by any fibrinolytic enzyme. The combination of either tissue plasminosen activator or hementin with a Tridegin results in more rapid lysis than the Tridegin alone. Since the Tridegin has no effect on its own, this shows a synergy between the two active materials. Tridegins can be used in combination with fibrinolytic agents that directly lyse fibrin (such as hementin, plasmin or Eminase) or with plasminogen activators that act through plasmin (such as streptokinase, urokinase, staphylokinase, tissue plasminogen activator or their derivatives) or with truncated forms or hybrid molecules that possess features of two or more of these agents.
Thrombolytic agents which may be included in the formulation according to the invention may comprise one or more of tissue plasminogen activator, streptokinase, Eminase, urokinase and staphlyokinase, as well as derivatives, truncated forms and hybrids thereof. Advantageously, the formulation when comprising, in addition to the Tridegins, the anticoagulant, thrombolytic or fibrinolytic agent, markedly decreases the time taken for blood clots to be digested. Therefore, Tridegins can potentially be used to inhibit the stabilisation of forming thrombi in, for example, acute coronary syndromes, venous thrombosis, or the like, and thereby enhance the effect of thrombolytic therapy. Typically the time required for 50% lysis of fibrin clots in the presence of plasmin is approximately halved if cross-linking is inhibited with one or more of the Tridegins.
Furthermore, the time for 50% lysis of plasma clots in the presence of tissue plasminogen activator is reduced by up to 40%, and similarly that by streptokinase by an amount greater than 25%.
The term "in combination", as used throughout the specification should be taken to mean the simultaneous or sequential administration of the Tridegins, according to the invention, together with any of or all of the anticoaculant, fibrinolytic, fibrinogenolytic or thrombolytic agents.
The Tridegins according to the invention may advantageously be used for the preparation of a medicament for the treatment of thromboembolic disease. Other pathological events which may be treated using the Tridegins according to the invention include Crohn's disease, tumour implantation, vessel wall thickening in atherosclerotic processes, thrombotic microangiopathy, in for example the kidney, fibrous growths of the skin, membranous glomerulonephritis, cataracts, acne and the formation of scar tissue, as well as infections with microfilarial nematodes. Advantageously, not only should the Tridegins according to the invention be useful in therapeutic treatment or prevention of such syndromes, but the high potency of the Tridegins should permit lower doses to be used.
The present invention further comprises a polypeptide produced by a recombinant DNA technique, which polypeptide is equivalent to the polypeptide defined above; the invention further comprises a synthetic or protein-engineered equivalent to the polypeptide according to the invention.
BRIEF DESCRIPTION OF THE DRAWINGS
Exemplary processes for isolation and characterisation of the polypeptide according to the invention will now be described with reference to the accompanying drawings which are given, by way of example only, wherein;
FIG. 1 is a graphic illustration of the elution of the inhibitory activity of the polypeptides according to the invention isolated according to Example 3 described below;
FIG. 2 is a graphic illustration of the results of Example 4 for the elution of the inhibitory activity of the polypeptide according to the invention in comparison to hementin and ghilantin;
FIG. 3 is a graphic illustration of the results of Example 6 of the inhibitory activity of the polypeptide according to the invention;
FIG. 4 is a chromatograph of the inhibitory activity from FIG. 3;
FIG. 5 is a chromatograph of the active fractions obtained from FIG. 4;
FIG. 6 is an illustration of the results of sodium dodecyl sulfate polyacrylamide gel electrophoresis from Example 7;
FIG. 7 is an illustration of the results obtained from Example 22;
FIG. 8 is an illustration of the results obtained from Example 24; and
FIG. 9 is an illustration of the results obtained from Example 25.
DETAILED DESCRIPTION OF THE INVENTION
EXAMPLE 1
In a first experiment A, the proboscis, anterior and posterior salivary glands of a leech of the species Haementeria ghilianii were homogenised together in a Potter homogeniser in 10 mM Tris HCl, 0.85% w/v NaCl pH7.0 (1 ml), and centrifuged at 13000 rpm. The supernatant was assayed in a clot solubility assay similar to that of Tymiak, Tuttle, Kimball, Wang and Lee "A simple and rapid screen for inhibitors of factor XIIIa". J. Antibiotics 46 (1993) pp. 204-206. In a second experiment B, the proboscis, anterior and posterior salivary glands were dissected from a leech of the species Haementeria ghilianii and homogenised separately in 0.2 ml aliquots of the buffer. The effect was compared with extracts of the proboscis, anterior and posterior salivary glands from two leeches of the species Haementeria officinalis prepared in 0.2 ml buffer. The test samples (30 μl) were added to a solution of 10 mg/ml crude bovine fibrinogen which contains factor XIII (30 μl). The reaction was started by adding 6.25 units/ml bovine thrombin containing 9 mM CaCl 2 (40 μl). A clot formed in 15 min when 8M urea (160 μl) was added and left in contact with the clot. After 30 min, the absorbance resulting from the clot's opalescence was read at 405 nm. Lowered absorbance indicates solubility of the clot resulting from inhibition of cross-linking. Table 1 shows the inhibitory effect (absorbance at 405 nm) of the various extracts on the solubility of fibrin clots compared with iodoacetamide (a known inhibitor of factor XIIIa). The numerical values quoted in the table are absorbance at 405 nm.
TABLE 1______________________________________ Experiment ExperimentTest Sample A B______________________________________Tris buffer 0.74 0.83Iodoacetamide (100 μM) 0.26 0.42H. ghilianii complete salivary 0.29 --complex extractH. ghilianii anterior gland extract -- 0.43H. ghilianii posterior gland extract -- 0.43H. ghilianii proboscis extract -- 0.53H. officinalis anterior gland extract -- 0.64H. officinalis posterior gland extract -- 0.55H. officinalis proboscis extract -- 0.09______________________________________
EXAMPLE 2
In order to confirm the presence of an inhibitor of factor XIIIa, the effect of the extracts on the ability of human factor XIIIa to catalyse the incorporation of biotinamidopentylamine into casein was measured by the microtitre plate method described by Slaughter T F, Achyuthan K E, Lai T-S and Greenberg C S. (1992). ("A microtitre plate transglutaminase assay utilizing 5-(biotinamido)pentylamine as substrate"; Anal Biochem 205: 166-171). Extracts of the proboscis, anterior and posterior salivary glands of leeches of the Haementeria species were prepared as in experiment A in Example 1. Those from Haementeria depressa were lyophilised. As the salivary glands are not easily removable from leeches of the species, Hirudo medicinalis and Hirudinaria manillensis, the extracts were prepared by removing the anterior one third of single leeches and homogenising in 1 ml 10 mM Tris HCl containing 0.85% NaCl. The supernatant following centrifugation at 13000 rpm was used in the assay. N,N dimethylcasein was dissolved in 0.1M Tris HCl pH8.5 by stirring at 85° C. for 30 min 2000 g for 20 min. A concentration of 10-20 mg/ml (0.2 ml) was used to coat the wells of a microtitre plate by incubation at 37° C. for 1 h. The excess casein was discarded and the wells blocked with 0.5% non fat dry milk in 0.1M Tris HCl pH8.5 for 30 min. The plate was then washed twice with 0.35 ml aliquots of the Tris buffer. Factor XIIIa was prepared from citrated human plasma by defibrinogenation by addition of solid bentonite (40 mg/ml), incubation for 10 min and centrifugation at 12000 g for 2 min. The supernatant (0.5 ml) was activated by the addition of 1000 U/ml bovine thrombin (0.05 ml) and 200 mM CaCl 2 (0.025 ml) and incubation at 37° C. for 15 min. The thrombin was neutralised by addition of 2000 ATU/ml hirudin (0.5 ml). Microtitre plate wells (total volume 0.2 ml) contained 5 mM CaCl 2 , 10 mM dithiothreitol, 0.5 mM biotinamidopentylamine, test sample (0.05 ml) and of the activated plasma (0.05 ml). After incubation at 37° C. for 30 min, the liquid was discarded and the reaction stopped by two washes in 0.2M EDTA (0.35 ml each) followed by two washes with 0.1M Tris HCl pH8.5 (0.35 ml each). 0.25 mg/ml streptavidin-alkaline phosphatase was diluted 1:150 with 0.5% non fat dry milk in the Tris buffer and 0.25 ml was added to each well and incubated for 1 h at 20° C. The plate was washed once with 0.1% Triton X-100 (0.35 ml) followed by 3 washes with the Tris buffer (0.35 ml).
Bound alkaline phosphatase was measured by addition of 1 mg/ml p-nitrophenyl phosphate. 5 mM MgCl 2 in the Tris buffer (0.05 ml) plus Tris buffer (0.2 ml) and the absorbance measured after 30 min using a Titertek Uniskan II microtitre plate reader at 405 nm. Table 2 confirms, in a different and more sensitive assay, that the Factor XIIIa inhibitory activity (measured by the incorporation of biotinamidopentylamine into casein catalysed by human plasma factor XIIIa) is found in the salivary organs of both Haementeria ghilianii and Haementeria officinalis. Moreover, significant but low inhibitory activity is detectable in the salivary glands of Haementeria depressa and in the anterior portions of both Hirudo medicinalis and Hirudinaria manillensis.
TABLE 2______________________________________ Factor XIIIa inhibitory activity (unit/complete salivary complex orTest Sample unit/leech)*______________________________________Buffer control 0.00Haementeria ghilianii 128.7Haementeria officinalis 10.2Haementeria depressa 0.5Hirudo medicinalis 1.5Hirudinaria manillensis 2.1______________________________________ *1 unit is defined as double the amount of transglutaminase inhibitor required to inhibit human factor XIIIa in 1 ml normal human plasma by 50% A pool of plasma from seven healthy donors was utilised for this standardisation.
EXAMPLE 3
A homogenate was prepared in phosphate-buffered saline from five sets of the complete salivary complex (anterior, posterior glands and the proboscis) from Haementeria ghilianii in the same way as that described in Example 1 and the supernatant was applied to a 1.6×80 cm column of Superdex G-200 and run in phosphate-buffered saline pH7.2 at a flow rate of 1 ml/min. The eluant was monitored at 280 nm and the inhibitory activity was determined by the same assay as that described in Example 1. FIG. 1 shows the separation and the position where the inhibitory activity elutes. The bar indicates the fractions which contain the Tridegin activity.
EXAMPLE 4
A homogenate of the complete salivary complex from five Haementeria ghilianii was prepared in 20 mM Tris HCl pH8.0 as in Example 1. The supernatant was applied to a 0.8×7.5 cm column of Express-Ion Exchanger Q (Whatman) and eluted with a linear gradient to 20 mM Tris HCl pH8.0 containing 0.3M NaCl. The eluate was monitored by absorption at 280 nm and the Tridegin activity was determined by the clot solubility assay as in Example 1. In addition the activity of hementin was measured by a fibrinogenolytic assay and the factor Xa inhibitory activity by a chromogenic substrate assay. The hementin activity was assessed by incubating 2 mg/ml bovine fibrinogen (50 μl) with 20 mM HEPES buffer containing 10 mM CaCl 2 and 0.1% w/v Brij 35 pH 7.5 (25 μl) and serial dilutions of the column fractions (25 μl) at 37° C. for 60 min. Then 100 U/ml thrombin (10 μl) was added to cause clotting and the clot was measured by the turbidity at 405 nm after 30 min. Reduction in the turbidity indicated the amount of fibrinogen digested. The factor Xa chromogenic substrate assay was carried out by incubating 2 mM S2765 in 50 mM Tris HCl pH 8.3 in a spectrophotometer and measuring the rate of absorbance change at 405 nm. The reaction was started by the addition of human factor Xa.
FIG. 2 shows the elution profile on a column of SP Sepharose eluted with a linear gradient to 0.3M NaCl. The positions where the Tridegin (T), the hementin and the factor Xa inhibitory activity appears are shown; there is a very clear separation of the Tridegin from the other two salivary components, namely hementin (H) and ghilanten (G), known to be in the salivary glands of this species of leech, confirming that Tridegin differs from the known components. The fractions containing the inhibitory activity are marked with a bar and the respective letters T,G and H.
EXAMPLE 5
A homogenate of the complete salivary complex from Haementeria ghilianii was prepared in 20 mM ammonium formate pH3.5 (5 ml) in a similar way to that in Example 1 and applied to a 0.8×7.5 cm column of Express-Ion Exchanger S (Whatman).
Fractions were eluted with a linear salt gradient to 20 mM sodium formate containing 1M NaCl pH3.5. The eluate was monitored by absorbance at 280 nm and assayed as in Example 1. The inhibitory fraction eluted at about 0.6M.
EXAMPLE 6
By combining similar chromatography steps to those exemplified in Examples 3, 4 and 5, a large batch was prepared. The complete salivary complex of fifty leeches of the species Haementeria ghilianii which had not been fed for at least 3 months were homogenised in 20 mM Tris HCl pH8.0 (50 ml) and centrifuged as in Example 1. The supernatant was applied to a 60×10 cm column of Q Sepharose Fast Flow (Pharmacia). Fractions were eluted with a linear gradient from the starting buffer to one containing 0.1M NaCl. The eluate was monitored at 280 nm and the active fraction was found to elute at about 0.09M NaCl (see FIG. 3 in which the fractions containing inhibitory activity are marked with a bar). The active fractions (145 ml) were adjusted to pH 4 by addition of formic acid and applied to a 5×12 cm column of SP Sepharose Fast Flow (Pharmacia) which had been equilibrated in 20 mM. sodium formate buffer pH 3.5. The column was eluted with a linear gradient from the equilibration buffer to the same buffer containing 1M NaCl. The active fraction eluted in a peak at about 0.57M NaCl (see FIG. 4 in which the fractions containing inhibitory activity are again marked with a bar). This was lyophilised and reconstituted in a final volume of 2.4 ml water and applied to a 1.6×60 cm column of Superdex G-75 which had been equilibrated in phosphate-buffered saline pH7.2. The elution profile is shown in FIG. 5 in which the fractions containing inhibitory activity are again marked with a bar. The pooled active fractions contained 715 μg protein and these were stored frozen.
Polyacrylamide gel electrophoresis in sodium dodecyl sulfate and staining with either Coomassie Blue or silver stain demonstrated that the protein was substantially pure after this step and that by comparison with standards of known molecular weight, the major band had an apparent molecular weight of about 7800 daltons with minor bands at higher molecular weight which were only detectable by the more sensitive silver staining method.
EXAMPLE 7
For sequencing work, a further purification step was performed. 0.3 ml of the active fraction from Example 6 was applied to a 0.5×10 cm column of ProRPC equilibrated in 0.1% trifluoroacetic acid and was eluted with a gradient from 0 to 100% acetonitrile containing 0.1% trifluoroacetic acid. A major peak was found which contained the inhibitory activity and this was followed by and widely separated from, two very much smaller, inactive peaks. The active fraction showed a single band on sodium dodecyl sulfate polyacrylamide gel electrophoresis with an apparent molecular weight of about 7800 in comparison with peptidic standards of known molecular weight which are illustrated in FIG. 6.
FIG. 6 is a polyacrylamide gel electrophoresis in sodium dodecyl sulfate of the pure polypeptide on a PhastGel high density gel (Pharmacia). The left hand lane (lane 1) and lane 7 are low molecular weight marker kit (Pharmacia) of 94, 67, 43, 30, 20.1 and 14.4 kD plus aprotinin (molecular weight 6.5 kD). Lanes 2 and 7: peptide marker kit (Pharmacia) of molecular weights 16.9, 14.4 10.7, 8.2 and 6.2 kD plus aprotinin (6.5 kD). Lane 3: water blank. Lane 4: Purified Tridegin. Lane 5 and 6: minor peaks from reverse phase chromatography column. The lowest molecular weight components migrate nearest the top of the gel.
A single, clean, amino acid sequence was found from the amino terminus by an Applied Biosystems 473A automatic protein sequencer indicating that only one peptide was present. The amino acid sequence was found to be:
NH.sub.2 -Lys-Leu-Leu-Pro-X-Lys-Glu-Y-His-Gln-Gly-Ile-Pro-Asn-Pro-Arg-
where X and Y were not identified positively and therefore could be any amino acid. The cysteines in this sample were not derivatised and therefore could not be assigned. The sequencing was repeated after pyridylethylation and this showed residue X to be a cysteine whereas Y gave no peak at all and could not be assigned to any common amino acid.
EXAMPLE 8
In order to produce enough material for amino acid sequencing, a sample of the transglutaminase inhibitor was prepared from the posterior salivary glands only of fifty leeches of the species Haementeria ghilianii by an identical method to that used in Examples 6 and 7. Aliquots were denatured, amidocarboxymethylated and digested by either trypsin or AspN endoprotease by the standard methods described in Matsudaira ("A practical guide to protein and peptide purification for microsequencing" Academic Press. 2nd Edition pp. 45-67), and the fragments were separated on a 0.5×10 cm column of ProRPC equilibrated in 0.06%, trifluoroacetic acid and eluted with sequential linear gradients from 2 to 38%. 38 to 75% and 75 to 98% elution buffer where the elution buffer was 80% acetonitrile in 0.0675% trifluoroacetic acid and monitored at 210 nm. The sequence of the isolated fragments was determined by an Applied Biosystems 473A automatic protein sequencer. The amino acid sequence of the whole polypeptide was deduced from this and the overlapping peptides that were found:
__________________________________________________________________________ 1 10NH.sub.2 -Lys-Leu-Leu-Pro-Cys-Lys-Glu-X.sub.1 -His-Gln-Gly- 20Ile-Pro-Asn-Pro-Arg-Cys-X.sub.2 -Cys-Gly-Ala-Asp-Leu- 30Glu-X.sub.3 -Ala-Gln-Asp-Gln-Tyr-Cys-Ala-Phe-Ile-Pro- 40Gln-Z.sub.1 -Arg-Pro-Arg-Ser-Glu-Leu-Ile-Lys-Pro-Met- 50Asp-Asp-Ile-Tyr-Gln-Arg-Pro-Val-Z.sub.2 -Phe-Pro-Asn-60 66Leu-Pro-Leu-Lys-Pro-Arg-Z.sub.3 -COOH__________________________________________________________________________
wherein amino acids X 1 , X 2 and X3 were not identifiable and may represent residues that have been modified post translationally and Z 1 , Z 2 and Z 3 represents amino acids that could not be distinguished between Cys or Glu. The polypeptide having this sequence is designated as Tridegin variant 1.
EXAMPLE 9
Besides the assays which demonstrate the ability of factor XIIIa to incorporate amines into casein and the effects of Factor XIIIa on clot solubility, the specificity of the inhibitory action can be shown by an assay which measures the production of ammonia from casein when amines are incorporated. The transglutaminase activity of human plasma factor XIIIa was measured spectrophotometrically by a modification of the method of Muszbek, Polgar and Fesus; "Kinetic determination of blood coagulation factor XIII in plasma." Clin Chem 31 (1985) pp. 35-40. This method measures the production of ammonia by linking it through the glutamate dehydrogenase reaction to NADH oxidation which can be monitored by the change in absorption at 340 nm. Factor XIII was activated by incubating defibrinated human plasma (2 ml) and 200 mM CaCl 2 (0.1 ml) with 1000 unit/ml bovine thrombin (0.1 ml) at 37° C. After 15 min the reaction was stopped by the addition of 260 antithrombin units of hirudin. The reaction cuvette contained: 2.5 mM dithiothreitol (0.1 ml), 40 mg/ml dephosphorylated β-casein (0.05 ml), 70 mM ethylamine (0.1 ml), 12 mM sodium 2-ketoglutarate (0.1 ml), 4 mM NADH (0.1 ml), 1.2 mM ADP (0.1 ml), 40 unit/ml glutamate dehydrogenase (0.1 ml), 70 mM HEPES buffer pH7.5 (0.25 ml) and this was placed in a spectrophotometer at 20° C. All components were dissolved in 70 mM HEPES buffer pH 7.5 where possible. The reaction was started by the addition of the activated factor XIII (0.2 ml) and monitored at 340 nm. The assay was validated with the use of factor XIII-deficient plasma (Sigma). Replacement of the normal plasma with the deficient plasma resulted in a rate of reaction that was 88% lower (1.87 versus 11.3 mAbs/min) demonstrating that the assay actually measures factor XIIIa.
Test samples were added in 0.1 ml of the HEPES buffer to the reaction cuvette. The inhibitory effect of Tridegin variant 1 was compared to that of iodoacetamide, a known inhibitor of the sulfhydryl group-dependent factor XIIIa and EGTA, an inhibitor of factor XIII activation and activity by virtue of its chelation of essential calcium as shown in Table 3. The Tridegin lowered the rate of ammonia production by about 93%, that is the inhibition was equivalent to that of iodoacetamide (as shown in Table 3). This is additional evidence which shows that Tridegins, as well as being inhibitors of clot solubilisation, are inhibitors of plasma transglutaminase or factor XIIIa.
TABLE 3______________________________________Test Sample Change in absorbance(concentration in cuvette) (mAbs/min)______________________________________Control 4.14EGTA (77 mM) 0.024Iodoacetamide (0.077 mM) 0.356Tridegin (3.89 μg/ml) 0.28______________________________________
EXAMPLE 10
The effect of Tridegin variant 1, purified as in Example 6, on the ability of human factor XIIIa to catalyse the incorporation of biotinamidopentylamine into casein was measured by the microtitre plate method described by Slaughter T F, Achyuthan K E, Lai T-Sand Greenberg C S. (1992). ("A microtitre plate transglutaminase assay utilizing 5-(biotinamido)pentylamine as substrate". Anal Biochem 205: 166-171). N,Ndimethylcasein was dissolved in 0.1M Tris HCl pH 8.5 by stirring at 85° C. for 30 min and then centrifugation at 12000 g for 20 min. A concentration of 10-20 mg/ml (0.2 ml) was used to coat the wells of a microtitre plate by incubation at 37° C. for 1 h. The excess casein was discarded and the wells blocked with 0.5% non fat dry milk in 0.1M Tris HCl pH 8.5 for 30 min. The plate was then washed twice with 0.35 ml aliquots of the Tris buffer. Purified human platelet factor XIII (0.6 unit/0.12 ml) was activated by addition of 150 U/ml thrombin in 15 mM CaCl 2 (0.18 ml) and incubation at 37° C. for 15 min. The thrombin was then inhibited by addition of 140 ATU/ml natural hirudin (0.3 ml). Nicrotitre plate wells (total volume 0.2 ml) contained 5 mM CaCl 2 , 10 mM dithiothreitol, 0.5 mM biotinamidopentylamine, Tridegin sample prepared in a similar way to that described in Example 6 and 0.25 unit/ml of the activated factor XIIIa in 0.1M Tris HCl pH 8.5. After incubation at 37° C. for 30 min, the liquid was discarded and the reaction stopped by two washes in 0.2M EDTA (0.35 ml each) followed by two washes with 0.1M Tris HCl pH8.5 (0.35 ml each). 0.25 mg/ml streptavidin-alkaline phosphatase was diluted 1:150 with 0.5% non fat dry milk in the Tris buffer and 0.25 ml was added to each well and incubated for 1 h at 20° C. The plate was washed once with 0.1% Triton X-100 (0.35 ml) followed by 3 washes with the Tris buffer (0.35 ml). Bound alkaline phosphatase was measured by addition of 1 mg/ml p-nitrophenyl phosphate, 5 mM MgCl 2 in the Tris buffer (0.05 ml) plus Tris buffer (0.2 ml) and the absorbance measured after 30 min using a Titertek Uniskan II microtitre plate reader at 405 nm.
Tridegin variant 1 clearly inhibited the incorporation of the amine with an IC50 of 0.026±0.002 μg/ml (3.4 nM) confirming its very potent inhibitory activity on platelet factor XIIIa.
In a separate experiment using an identical protocol except replacing the purified factor XIII with plasma from a healthy human volunteer and varying the concentration of the Tridegin, the IC50 was determined to be 0.07±0.003 μg/ml (9.2 nM) for the plasma form of factor XIIIa.
EXAMPLE 11
The effect of Tridegin variant 1 purified as in Example 6 was tested on the coagulation enzyme, thrombin. with a chromogenic substrate assay. 1 mM S2238 was incubated in 50 mM Tris HCl pH 8.3 and the reaction was started by adding thrombin 0.15 U/ml final concentration. The reaction was monitored in a spectrophotometer at 405 nm. Table 4 shows that Tridegin had no effect on thrombin at a concentration of 4.6 μg/ml whereas hirudin at a concentration of 0.046 μg/ml had a marked inhibitory effect (95%).
TABLE 4______________________________________ Rate of Concentration ReactionTest Sample (μg/ml) (mAbs/min)______________________________________Control -- 49.8Tridegin 4.6 51.8Hirudin 0.046 2.63______________________________________
EXAMPLE 12
The effect of the Tridegin purified as in Example 6 was tested on factor Xa. 2 mM S2765 was incubated in 50 mM Tris HCl pH 8.3 and the reaction was started by adding human factor Xa. The assay was performed as in Example 11. The transglutaminase inhibitor at 4.6 μg/ml had no effect on factor Xa whereas recombinant tick anticoagulant peptide (rTAP), a known inhibitor of factor Xa (Waxman L. Smith D E, Arcuri K et al. "Tick anticoagulant peptide (TAP) is a novel inhibitor of blood coagulation factor Xa" Science 248: 593-596: 1990), inhibited by 89.9% at a concentration of 0.046 μg/ml (Table 5). This confirms that, not only is the transglutaminase inhibitor different from previously known inhibitors of factor Xa, but the methods exemplified to purify the transglutaminase inhibitor successfully remove the factor Xa inhibitors.
TABLE 5______________________________________Test Concentration Reaction RateSample (μg/ml) (mAbs/min)______________________________________control 49.8Tridegin 4.6 56.1rTAP 0.046 5.53______________________________________
EXAMPLE 13
In order to ascertain if Tridegins have a hementin-like fibrinogenolytic activity, the ability of the purified material from Example 6 to direst fibrinogen was evaluated by assessing the clottability of fibrinogen after incubating it with the inhibitor. 2 mg/ml bovine fibrinogen (50 μl) was incubated with the Tridegin, purified hementin or vehicle (50 μl) and 20 mM HEPES buffer containing 10 mM CaCl 2 and 0.1% w/v Brij 35 pH 7.5 (50 μl) at 37° C. for 60 min. Then 100 U/ml thrombin (10 μl) was added to cause clotting and the clot was measured by the turbidity at 405 nm after 30 min. Table 6 shows that the transglutaminase inhibitor had no effect on the clot formation whereas purified hementin had clearly digested the fibrinogen and little clot resulted. This indicates that Tridegins have no proteolytic action on fibrinogen and therefore are not hementin as described in WO 91/15576 ("Treatment of thrombotic events") and U.S. Pat. No. 4,390,630, ("Hementin--a fibrinolytic agent"). In addition, this example adds further confirmation that the hementin which is found in Haementeria ghilianii is separated from the transglutaminase inhibitor during the purification procedures exemplified.
TABLE 6______________________________________Test Sample Absorbance Absorbance______________________________________buffer control 0.238 0.224Tridegin (35 μg/ml) 0.226 --Hementin (30 unit/ml) -- 0.007______________________________________
EXAMPLE 14
The activity of the enzyme, destabilase, can be measured by its effect in causing the release of p-nitroaniline from the chromogenic substrate, L-γ-glutamyl p-nitroanilide. In order to ascertain whether destabilase and the Tridegins have similar properties, the effect of the two agents on the chromogenic substrate was compared. The absorbance of cuvettes containing 0.45 mg/ml L-γ-glutamyl p-nitroanilide in 50 mM Tris HCl, 10 mM CaCl 2 pH 8.0 (0.9 ml) was continuously recorded at 405 nm in a spectrophotometer. Either 0.046 mg/ml Tridegin variant 1 (0.1 ml) or the supernatant from an extract of Hirudo medicinalis (0.1 ml), a known source of destabilase, prepared as in Example 2, was added and the rate of generation of nitroaniline measured. Table 7 shows the effect of Tridegin on the destabilase substrate, L-γ-glutamyl p-nitroanilide, and indicates that although Hirudo medicinalis extract contains an activity which causes an increase in the rate of absorbance indicating cleavage of this substrate attributable to destabilase, the Tridegin had no such effect and in fact results in a slight decrease in absorbance over time.
TABLE 7______________________________________ Reaction Rate (mAbs/min)______________________________________Hirudo medicinalis extract 2.04Tridegin (4.6 μg/ml) -1.17______________________________________
EXAMPLE 15
Tridegin was tested for its effect on the clotting of plasma by comparing a sample of normal plasma to which had been added 0.1 volumes of of the inhibitor purified as in Example 6 (46 μg/ml) in phosphate-buffered saline with one that had buffer alone. Standard clotting tests were carried out on an automated analyser. The results in Table 8 show that there was no difference in the two samples so Tridegin has no effect on the clotting time of normal human plasma. This property is expected since inhibitors of fibrin cross-linking have no effect on clot formation and only influence its physical and chemical properties after it has formed. Moreover this confirms, in a different test, the absence of any other anticoagulant activity such as inhibition of factor Xa or thrombin in Tridegin.
Platelet aggregation was assessed in human citrated platelet-rich plasma in a Bio/Data aggregometer in response to either 6.7 μg/ml collagen, 6.3 μM ADP or 0.4 U/ml thrombin. Tridegin from Example 6, at a final concentration of 4.6 μg/ml was compared to buffer controls. Table 8 shows that the Tridegin clearly has no effect on platelet aggregation under these conditions.
TABLE 8______________________________________ TrideginParameter Control (4.6 μg/ml)______________________________________Thrombin clotting time (sec) 9.8 9.8One stage prothrombin time (sec) 15.2 14.7Kaolin cephalin clotting time (sec) 28.5 27.9Collagen-induced aggregation (%/min) 23 28ADP-induced aggregation (%/min) 11 14Thrombin-induced aggregation (%/min) 73 82______________________________________
EXAMPLE 16
The effect of the inhibitor on guinea pig liver tissue transglutaminase was measured in an assay similar to that described in Example 10 where the activated factor XIIIa was substituted with tissue transglutaminase. Tridegin (4.5 μg/ml) inhibited the incorporation of the amine into casein catalysed by this enzyme by 95.5%. By using different concentrations of Tridegin the IC50 was found to be 1.55 μg/ml. This assay indicates that the Tridegin is an inhibitor of tissue transglutaminase as well as of the plasma transglutaminase factor XIIIa and that it is likely to be an inhibitor of many of the transglutaminase enzymes.
EXAMPLE 17
The transglutaminase inhibitor is measurable in the glands of the salivary system and in salivary secretions of Haementeria ghilianii by the amine incorporation assay of Slaughter T F, Achyuthan K E, Lai T-S and Greenberg C S. (1992). ("A microtitre plate transglutaminase assay utilizing 5-(biotinamido)pentylamine as substrate". Anal Biochem 205: pp. 166-171). The anterior and posterior salivary glands and the proboscis together with the hind sucker were removed from a starved third-fed stage animal. The samples were homogenised in a glass homogeniser in 1 mM Tris HCl pH8.0 (1 ml or 0.5 ml in the case of the posterior glands) and centrifuged at 12000 rpm. The supernatant was used for the assay. For collection of the salivary secretion the complete salivary apparatus (proboscis, anterior and posterior glands) of each of eight starved third-fed stage Haementeria ghilianii was removed after chilling the leeches at 5° C. for 2-3 h. It was pinned out on to a Sylgard base and bathed in physiological saline solution (65 mM NaCl, 50 mM NH 4 Cl, 4 mM KCl, 1 mM EGTA, 11 mM glucose, 10 mM HEPES pH 7.4) at 20° C. for 15 min. By cutting the wall of the proboscis longitudinally, the lumen was accessed and secretions contained therein were collected by micropipette.
Table 9 shows the inhibition of human plasma factor XIIIa by these extracts and secretions of the leech Haementeria ghilianii. The inhibitory activity is found in both salivary glands, in the salivary secretion and in the proboscis. The very low activity detectable in the hind sucker is of very low specific activity, being 0.35% that in the posterior salivary gland, and in fact the apparent activity detected may well result from the very high protein concentration extracted from this large piece of tissue.
TABLE 9______________________________________ Specific activityTissue (unit/mg).sup.# % inhibition______________________________________Anterior salivary gland 19.0 99.7Posterior salivary gland 93.3 100Proboscis 11.7 95.5Hind sucker 0.33 48.5Luminal secretion from proboscis* --.sup.+ 61.9______________________________________ .sup.# 1 unit is defined as double the amount of transglutaminase inhibitor required to inhibit factor XIIIa in 1 ml normal human plasma by 50% in the amine incorporation assay described in Example 10. *mean of eight separate experiments. .sup.+ the protein concentration was too low to measure (the specific activity is very high).
EXAMPLE 18
The potentiating effect of the Tridegin on fibrinolysis induced by plasmin was demonstrated by an absorbance method. 10 mg/ml bovine fibrinogen (0.1 ml) was incubated with 50 U/ml bovine thrombin (0.01 ml) with either buffer or Tridegin from Example 6 (0.04 ml) for 2 h at 37° C. in a microtitre plate. 2.56 U/ml plasmin (0.05 ml) was added and the plate was incubated at 37° C. The absorbance was measured every 15 min on a Titretek Uniskan II microtitre plate reader. The clot was viewed every 15 minutes and the time taken for the clot to completely dissolve was recorded. At all the concentrations tested, the transglutaminase inhibitor shortened the time for lysis to occur as illustrated in Table 10.
TABLE 10______________________________________[Tridegin] (μg/ml) Time for lysis (h)______________________________________0 3.02.0 1.01.0 1.250.2 1.250.1 2.50.04 1.5______________________________________
EXAMPLE 19
The accelerating effect of Tridegin on fibrinolysis induced by tissue plasminogen activator was also shown on human plasma clots. Human plasma (0.1 ml) was incubated with 5 U/ml bovine thrombin in 0.18M CaCl, containing 0.14M KCl (0.01 ml) and either buffer or Tridegin prepared as in Example 6 but from the posterior salivary glands of Haementeria ghilianii (0.04 ml) for 2 h at 37° C. in a microtitre plate in replicates of six. Tissue plasminogen activator (0.05 ml) was then added to a final concentration of 10 IU/ml and the plate was incubated at 37° C. and absorbance readings were taken every 30 min at 405 nm using a Titretek Uniskan II microtitre plate reader. The reduction in absorbance indicated lysis of the plasma clots. The time taken for 50% lysis in the control wells was 12.9±1.1 h and in the wells containing the transglutaminase inhibitor, 7.9±0.7 h, a statistically significant reduction. This example confirms that the transglutaminase inhibitor dramatically accelerates the action of tissue plasminogen activator on human plasma clots.
EXAMPLE 20
Singe platelets invariably become associated with thrombi in vivo, it is of interest to see if the transglutaminase inhibitors allow more rapid lysis of platelet-rich clots, a more physiological test. Platelets are a rich source of the plasma transglutaminase, factor XIII, as well as inhibitors of fibrinolysis so they severely reduce the efficacy of fibrinolytic agents. Human platelet-rich or platelet-poor plasma prepared from the same donor (0.1 ml) was incubated with 5 U/ml bovine thrombin in 0.18M CaCl 2 containing 0.14M KCl (0.01 ml) and either buffer or Tridegin (prepared as in Example 6 but from the posterior salivary glands of the species Haementeria ghilianii, 0.04 ml) for 2 h at 37° C. in a microtitre plate in replicates of six. Tissue plasminogen activator (0.05 ml) was added to a final concentration of 10 IU/ml and the plate incubated at 37° C. Absorbance readings were taken every 30 min for 72 h at 405 nm using a Molecular Devices Thermomax kinetic microtitre plate reader (lowered absorbance showing lysis of plasma clots). Table 11 shows that in the presence of platelets the clots did not achieve 50% lysis in a 72 hour incubation period. Tridegin is even more effective at reducing the effect of platelets when present as it reduces the time from >72 h to 24.9 h in their presence and from 2.5 h to 18.0 h in their absence in this Example.
TABLE 11______________________________________ control buffer Tridegin (time for 50% lysis (time for 50% lysis in hours) in hours______________________________________Platelet-poor plasma 22.5 ± 1.99 18.0 ± 1.03Platelet-rich plasma >72 24.9 ± 5.57______________________________________
EXAMPLE 21
The effect of Tridegin to decrease clot lysis times is a general effect and can be shown when streptokinase is used as the lytic agent. Human plasma (0.1 ml) was incubated with 5 U/ml bovine thrombin in 0.18M CaCl 2 containing 0.14M KCl (0.01 ml) and either buffer or Tridegin prepared as in Example 6 but from the posterior salivary lands of Haementeria ghilianii (0.04 ml) for 2 h at 37° C. in a microtitre plate in triplicate. Streptokinase was then added to a final concentration of 30 U/ml and the plate was incubated in an iEMS kinetic microtitre plate reader at 37° C. and absorbance readings were taken every 30 min for 47.5 h at 405 nm. Although the wells containing streptokinase alone had not lysed sufficiently to obtain a time for 50% lysis, all the wells that contained the Tridegin lysed by 50% in 36.1±1.6 h demonstrating again the accelerating effect when used in combination with fibrinolytic agents like streptokinase is shown in FIG. 7 (which shows the effect of Tridegin on plasma clot lysis induced by streptokinase). The results are ±SEM (n=3).
EXAMPLE 22
The combination of Tridegin and hementin was investigated as described in Example 21, where the tissue plasminogen activator was replaced with 110 U/ml hementin. In this Example both platelet-free and platelet-rich plasma samples from the same donor were used in order to ascertain if there was an difference. Table 12 shows the times taken for 50% lysis to occur in the samples. There is a clear effect of platelets which increase the time required for lysis from 34 h to >56 h yet clearly the Tridegin reduces the time for 50% lysis to occur whether platelets are absent or present. The Tridegin seems to largely overcome the effect of the platelets by decreasing the lysis time close to that of the control.
TABLE 12______________________________________ Buffer Tridegin (time for 50% lysis (time for 50% lysis in hours) in hours)______________________________________Platelet-free 34 ± 3.5 24 ± 0.8plasmaPlatelet-rich >56 ± 7.8 36 ± 2.2plasma______________________________________
EXAMPLE 23
In order to investigate the properties of Tridegin derived from the Mexican leech. Haementeria officinalis, an extract was chromatographed on gel filtration followed by reverse phase high pressure liquid chromatography. The salivary glands and probosces were dissected from five specimens of Haementeria officinalis that had been starved to a point where no blood was found in the foregut. These were homogenised in phosphate buffered saline pH 7.2 (1 ml) in a Teflon/glass homogeniser and centrifuged at 12000 g for five minutes in order to obtain a clear supernatant. The supernatant was applied to a 1.6×60 cm column of Superdex G75 and the eluate was monitored at 280 nm and all fractions were collected and assayed in a clot solubility assay as in Example 1. The inhibitory activity was found in a single peak as indicated in FIG. 8 (in which again the fractions containing the inhibitory activity are marked with a bar).
The active fraction was lyophilised and redissolved in water (1 ml). Part of this (0.3 ml) was applied to a 0.5×10 cm column of Pro-RPC which had been equilibrated in 0.1% trifluoroacetic acid (TFA). Elution with a linear gradient of 0.1% TFA to acetonitrile containing 0.1% TFA resulted in the elution of a large number of peaks which absorbed at 280 nm. Each was assayed in the clot solubility assay as described in Example 1 and a single peak was found to contain activity.
Comparison of the elution positions on the two columns with that for similar extracts of Haementeria ghilianii indicated the close similarity with the elution position of Tridegin variant 1. The inhibitory activity purified from the salivary glands of Haementeria officinalis has very similar physicochemical properties in terms of molecular weight, as determined by gel filtration, and partition coefficient, as determined by reverse phase high pressure liquid chromatography to those of Tridegin variant 1.
EXAMPLE 24
To determine the behaviour of Tridegin variant 1 in vivo, a dose of 0.207 mg/kg i.v. formulated in 0.01M sodium phosphate, 0.027M KCl, 0.137M NaCl pH 7.4 (4.7 ml) was administered intravenously to a group of four rats. Blood samples (approx. 0.3 ml) were taken from the tail vein both before and 2 or 5 and 10, 20, 30, 60 and 120 minutes after administration and mixed immediately with 0.04 ml 3.8% w/v trisodium citrate. The samples were immediately centrifuged at 12000 g for 5 min and the supernatants removed and flash frozen on dry ice. No side effects of the Tridegin administration were noted.
The Tridegin in the samples was assayed by a modification of the amine incorporation assay used in Example 2 where the intrinsic factor XIII was activated in each sample (0.097 ml) by addition of 0.1M Tris HCl pH 8.5 (0.03 ml) and 1000 U/ml bovine thrombin (0.01 ml) and incubation at 37° C. for 15 minutes. The fibrin clot was removed by centrifugation and the serum used for the assay. Samples for the standard curve were prepared by addition of known concentrations of pure Tridegin variant 1 to citrated rat plasma and activation of the factor XIIIa in an identical way. The Tridegin concentration in each sample was then determined by the percentage inhibition of the factor XIIIa as in Example 2 by comparison with the standard curve.
FIG. 9 shows Tridegin's pharmacokinetics in the rat. The time course is clearly multiphasic: the terminal half life is 30-60 minutes indicating significant duration of action and that Tridegin's pharmacokinetics make it suitable for pharmaceutical use.
__________________________________________________________________________# SEQUENCE LISTING- (1) GENERAL INFORMATION:- (iii) NUMBER OF SEQUENCES: 2- (2) INFORMATION FOR SEQ ID NO: 1:- (i) SEQUENCE CHARACTERISTICS:#acids (A) LENGTH: 16 amino (B) TYPE: amino acid (C) STRANDEDNESS: (D) TOPOLOGY: linear- (ii) MOLECULE TYPE: peptide- (v) FRAGMENT TYPE: N-terminal#1: (xi) SEQUENCE DESCRIPTION: SEQ ID NO:- Lys Leu Leu Pro Cys Lys Glu Xaa His Gln Gl - #y Ile Pro Asn Pro Arg# 15- (2) INFORMATION FOR SEQ ID NO: 2:- (i) SEQUENCE CHARACTERISTICS:#acids (A) LENGTH: 66 amino (B) TYPE: amino acid (C) STRANDEDNESS: (D) TOPOLOGY: linear- (ii) MOLECULE TYPE: peptide- (ix) FEATURE: (A) NAME/KEY: Peptide (B) LOCATION:37 (D) OTHER INFORMATION:/pro - #duct= "OTHER"#"Amino acid residue 37 represents, alternativel - #y, cysteine or glutamic acid."- (ix) FEATURE: (A) NAME/KEY: Peptide (B) LOCATION:56 (D) OTHER INFORMATION:/pro - #duct= "OTHER"#"Amino acid residue 56 represents, alternativel - #y, cysteine or glutamic acid."- (ix) FEATURE: (A) NAME/KEY: Peptide (B) LOCATION:66 (D) OTHER INFORMATION:/pro - #duct= "OTHER"#"Amino acid residue 66 represents, alternativel - #y, cysteine or glutamic acid."#2: (xi) SEQUENCE DESCRIPTION: SEQ ID NO:- Lys Leu Leu Pro Cys Lys Glu Xaa His Gln Gl - #y Ile Pro Asn Pro Arg# 15- Cys Xaa Cys Gly Ala Asp Leu Glu Xaa Ala Gl - #n Asp Gln Tyr Cys Ala# 30- Phe Ile Pro Gln Xaa Arg Pro Arg Ser Glu Le - #u Ile Lys Pro Met Asp# 45- Asp Ile Tyr Gln Arg Pro Val Xaa Phe Pro As - #n Leu Pro Leu Lys Pro# 60- Arg Xaa65__________________________________________________________________________ | The inhibitors, obtainable from tissue or secretions of leeches typically of the order Rhynchobdellida, has the following terminal sequence: NH 2 -Lys-Leu-Leu-Pro-Cys-Lys-Glu-Y-His-Gln-Gly-Ile-Pro-Asn-Pro-Arg- wherein Y represents any amino acid sequence; or a pharmaceutically acceptable salt, derivative or bioprecursor of said sequence, or an analogue or homologue thereof. Because of their extreme potency in the nanomolar range, they can be used to treat a number of diseases where protein cross-linking is important. They can be used for the treatment of Crohn's disease, tumor implantation, atherosclerosis, thrombotic microangiophathy, fibrous growths of the skin, acne, scar formation, membranous glomerulonephrits, cataracts, or infection with microfilarial nematodes. In particular, they can be used to reduce the stability of thrombi so that they are more susceptible to lysis by thrombolytic agents. | 2 |
In orthodontic practice there has been a steady improvement in the structures used in a patient's mount. The trend has been to miniaturization, enhanced appearance of the apparatus from a cosmetic viewpoint and increased simplification of installation and removal. At present small, slotted brackets are employed. These are bonded directly to the front or rear surfaces of the teeth. A curved archwire (conforming to the patient's dental arch) is formed of a special alloy, pretensioned by the orthodontist to produce desirable movement of the teeth and fitted into the slots in the brackets. After the archwire is tied down to each bracket by a much finer "ligating" wire or elastic "doughnut", the pretensioning forces come into play to achieve the desired tooth movement. Rotation wedges or like devices are used for teeth which are severely rotated. The finess of the ligating wire makes necessary considerable skill on the part of the orthodontist and long chair time for the patient. It is also normally required that the archwire be removed for retensioning or replacement a number of times during the course of the treatment. The ligating process must be repeated each time.
It is sometimes required that the archwire have play, i.e. that it be not fully seated. A loose ligation is therefore required. In other instances the archwire must be fully seated and have no play. This requires a tight ligation. In addition the ligations are sometimes broken during chewing or brushing and must be replaced. The rough edges generated by an accidental break or the "pigtails" which terminate the ligation wires create a dental emergency with inconvenience and discomfort for the patient. Often the surfaces of the tied, fine ligating wires or rotation wedges act as food traps which are hard to keep clean. When elastic "doughnuts" are used, they discolor and rapidly lose their elasticity. Their efficiency in securing the archwire to the base of the bracket falls off and they become ineffective. It would therefore by highly desirable if each bracket would incorporate a rapid clamping and unclamping device i.e. be "self-ligating" and also allow play or full seating of the archwire. In this way the use of ligating wires, elastic "doughnuts" and rotation devices could be greatly reduced.
Prior art directed to this problem has resulted in complex structures which are expensive to manufacture or contain separable parts which can accidentally be swallowed or are difficult to apply. Self-ligating brackets have been devised by Pletcher (U.S. Pat. Nos. 4,371337; 4,077,126; 4,419,178,; 3,444,621), Fostee (U.S. Pat. No. 4,268,249), Brader (U.S. Pat. No. 3,327,393), and Fujita (U.S. Pat. No. 4,355,975). My present invention as well as my copending "An Orthodontic Bracket Having Archwire Seating and Locking Mechanism", Ser. No. 852,452, are easily fabricated, convertible and easily applied.
SUMMARY OF THE INVENTION
This invention relates to an orthodontic bracket and its cover plate with built-in provision for archwire play, seating, rotation and in-out tooth movement (using adjacent teeth) after locking. The bracket is an assembly of two components: a base and a cover plate. The base contains an archwire slot in its center and a transverse, semi-cylindrical section on both its upper and lower ends. The cover plate is formed into a hollow, semi-cylinder at its upper end to make up a hinge with the upper base, semi-cylindrical section. A clip at the lower end of the cover plate permits a firm hold on the lower semi-cylindrical section of the base. In the center of the cover plate is a flat spring or two indentations. When the plate is rotated on the hinge to a closed position flat against the front of the base, the clip of the cover plate engages and locks over the lower semi-cylindrical section while the flat spring or pair of indents exert adjustable pressure on the archwire in its slot.
In use, an archwire is introduced into the slot of a tooth-mounted bracket; the cover plate is then swung into its closed position. The flat spring or pair of indents is brought to bear on the archwire by a desired amount and the cover plate locked into position. Whe the archwire is to be removed, the end of a sharp instrument is brought under the clip and it is sprung free. The plate can now be rotated open through 120 or more degrees so as to allow free access to the slot. Hinge friction or gravity serves to hold the cover plate open while the orthodontist alters the archwire prior to reinstallation. The plate serves to block the entry of food particles while it is closed. It may be coated with a pigment similar in color to tooth enamel or made of a synthetic tooth-colored material for cosmetic blending. In the above description the cover plate swings out and away from the base to reveal the slot. In another embodiment of the invention the cover plate is mounted by a rivet perpendicular to the base. In this embodiment the opening takes place in a plane parallel to the base.
DESCRIPTION OF THE DRAWINGS
FIG. 1 is an isometric view of the invention showing the base attached one version of the cover plate with the latter in an open position.
FIG. 2 is a side view of the invention of FIG. 1 showing an archwire being held in place by a closed and latched cover plate.
FIG. 3 is an isometric view of a second variation of a cover plate prior to assembly to a slotted base.
FIG. 4 is an isometric view of the invention with another version of a cover plate in closed position holding an archwire within its slot to its base.
FIG. 5 is an isometric view of a second embodiment of the invention prior to assembly.
FIG. 6 is an isometric view of a third embodiment of the invention.
FIG. 7 is an isometric view of a simplified version of the embodiment of FIG. 5.
FIG. 8 is an isometric view of a fourth embodiment of the invention prior to assembly.
FIG. 9 is an isometric view of the embodiment of FIG. 8 assembled and in an open position.
FIG. 10 is a cross section of the embodiment of FIG. 8 taken along the line X--X'.
DESCRIPTION OF THE INVENTION
The operation of the invention will be explained with reference to FIGS. 1 through 10. The bracket body 14 (FIGS. 1 and 2) incorporates the semi-cylindrical segment 1 at its upper end and the semi-cylindrical segment 3 at its lower end, both integral with the base 11. The semi-cylindrical segment 1 is undercut at 13 as shown in FIGS. 1 and 2. A slot 7 is provided to fit an archwire 6. The cover plate is rolled at one end into the semi-cylindrical form 15 and is provided with the confining tabs 5'. A cylindrical bar 9 is attached or may be formed of the material of the flat plate. Leaf springs 8' are formed from the tabs 8 by bending.
Assembly of the bracket body to the cover plate is accomplished by sliding the semi-cylindrical portion 15 of the plate over the semi-cylindrical segment 1 and bending down the tab 5. FIGS. 1 and 3. The tab 5' is bent during manufacture. This confines the plate laterally while permitting rotation in the vertical direction. The position of the spring 8' is such as to be in alignment with the slot 7 when the plate is rotated to a closed position.
In use, brackets of this construction are bonded to the teeth as in prior art. After the preflexed archwire 6 is successively pushed into each slot, step A in FIG. 1, each cover plate 2 is then rotated and its clip 4' is forced over the lower semi-cylindrical segment 3, step B. This brings the leaf springs 8' to bear on the archwire, locking it and seating it to its base (FIGS. 1 and 2). It is also possible by selection of archwire size and spring tension to bring about play when desired. If the slot 7 is of graded depth (laterally), the bracket cover plate can also be used to apply tooth rotating forces. The cover plate 2 and other parts of the bracket can be finished in various shades of white so as to decrease the visibility of the bracket when installed. It can also be made of synthetic, tooth-colored materials such as plastics.
The undercut 13, shown in FIGS. 1, 2 and 4 retains the cylindrical bar 9 when cover plate 2 is in the open position. Frictional force or gravity (depending on the initial positioning of the bracket when it is cemented on to a tooth) thus keeps each cover plate open so that the orthodontist has adequate accessibility to all the slots.
In the cover plate construction pictured in FIG. 4 a block 20 of an inert material such as Teflon or Nylon is attached to the underside of the cover. When the cover plate is closed and locked, the resulting flexion forces 20 against archwire 6, again locking and seating it. This effect could also be accomplished by indenting the cover plate in its central region to create a notch in line with the archwire slot so that the high side of the notch enters the slot. Depending on the size of the archwire and the depth of the indentation, play of the archwire or solid contact may be achieved.
The bracket and cover plate shown in FIGS. 5 and 7 make use of an extended upper cylindrical section 1a in the bracket body and the tabs 17 on the cover plate. The tabs 17 are formed into the hollow cylinders 17' which together with the extended cylindrical section 1a make up a hinge on which cover plate 2 can rotate. The advantage of this embodiment is the provision of a larger angle of opening of the cover plate and increased accessibility to the slot. The hollow cylinders 17' are made sufficiently close fitting to cylindrical section 1a that the cover plate is held at any angle of opening by friction or gravity.
Increased angle of opening can also be achieved by the embodiment of FIG. 6. An aperture 22 is formed in the support portion of the upper semi-cylindrical section 1b. A central tab 21 is shaped into the hollow cylinder 21' which fits around the central section of 1b and emerges through aperture 22. Again the fit is such as to retain the cover plate by friction or gravity at any desired angle of opening.
FIG. 7 illustrates a simplified version of the embodiment of FIG. 5. A central support block 33 serves as a mounting for the cylindrical sections 1c and an upper surface of the archwire slot.
The unlocking of clip 4' from the lower semi-cylindrical sections 3 of any of the embodiments of FIGS. 1 through 6 is done by inserting a scaler pick or similar dental tool behind the clip and pulling it away from the bracket. This frees the cover plate.
FIGS. 8, 9 and 10 illustrate an embodiment of the invention in which the cover plate opens parallel to the face of the bracket. The cover plate 2' is held in place by the rivet 30 which is shrink fitted into the hole 2. The cover plate turns on the rivet in the open position shown in FIG. 9. The indentations 26 will contact an appropriately sized archwire and provide seating force, while allowing smaller archwires the necessary play often required in the beginning stages of treatment. To use a fixed diameter or linear dimension of archwire requires various cover plate having a gradation of indent depths. Rotation may be accomplished by the use of a varying-depth slot and cover plates having indents of unequal length. The underside of the cover plate may be color coded for indentification of the indent depth. After the archwire is placed in the slot 7, the cover plate is rotated in the direction C to close the bracket slot, lock the cover plate and secure the archwire. The segment 32 engages the rounded surface 33 to hold the cover closed.
An additional feature of the embodiment shown in FIGS. 8, 9 and 10 may be added by cutting the slot 34 in the cover plate. This slot will permit the removal of the cover plate with the bracket bonded to a tooth and its replacement with a plate having longer or shorter indentations to accommodate various sizes of archwires. The embodiments of FIGS. 1 through 7 can also be modified to incorporate partial hinge cylinders to permit removal and replacement of the cover plate.
The present invention, used in combination over two or more teeth, can provide in and out (i.e. tongue to cheek) orthodontic movements.
The construction of the invention is such that the cover plate cannot unlock or be separated from its hinge during mastication or brushing.
The cover plate prevents accummulation of food particles within the bracket base while its smooth, tooth-colored surface promotes patient comfort and acceptance.
The rear surface of the base 37 in FIG. 10 is of mesh design to facilitate effective cementing to a tooth as in prior art. | An orthodontic bracket with self-ligating features is described. A cover plate is rotatably attached to the bracket base. Turning of the cover plate to the open position provides access to an archwire slot. After archwire placement, returning of the cover plate to its closed position achieves various degrees of play and seating depending on archwire size and cover plate configuration. The over plate promotes cleanliness and provides cosmetic advantages. | 0 |
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to the bonding of metals, the bonding of ceramics or the bonding of ceramics to metals and the like, and in particular to a bonding apparatus suitable for the bonding of parts of precision machines.
2. Description of the Related Art
It is known that the pressure welding of, for example, metals is possible by moving spaced apart surfaces to be pressure welded toward each other, at which an inter-atomic force of gravity can act.
However, since a surface coat such as an oxidized coat or a nitrified coat usually exists on a metal surface, it is difficult to pressure weld metals to each other.
Thus, a method, in which surfaces to be pressure welded are held at high temperatures and the diffusion bonding of materials having a surface coat that does not have strong chemical bonds therein is carried out by utilizing the diffusion phenomenon of said surfaces to be pressure welded, has been proposed as a general pressure welding method. This method is defective in that since the materials to be pressure welded are heated to temperatures near the recrystallization temperatures thereof, metallographical change and thermal strain are produced in the portion bonded and as a result, it is unsuitable for the bonding of parts of precision machines requiring high accuracy.
On the other hand, a method has been proposed in which the surface coat layer is removed by friction between the surfaces to be pressure welded or by brushing the surfaces to be pressure welded with a metal brush instead of heat treating the surfaces and thus, pressure welding at high temperatures is rapidly carried out before the surface coat has formed again.
However, this method is also defective in that since a large strain and a great amount or heat are induced on the surfaces to be pressure welded, the dimensional change of the portions to be pressure welded is inevitable.
As described above, pressure welding is remarkably dependent upon the surface state of metals, so that it is almost impossible to perform in the event that the surface coat layer exists. Accordingly, pressure welding is possible if a clean surface, on which the surface coat layer does not exist, can be obtained. It is, however, remarkably difficult to remove a surface coat without imparting any strain to the surface, and it is difficult to remove the surface coat layer while imparting only a very remarkably small surface strain.
One of the present inventors found from his various investigations that metals can be readily bounded to themselves without any metallographical change or increase in thermal strain of the material pressure welded, or without any dimensional change of the portion pressure welded, or without requiring any special means such as means for heat treating the metals, by pressure welding them in a superhigh vacuum of 10 -9 mmHg or more, after removing a metal surface coat by spattering using inert gas ions (Japanese Patent Application No. 53-32416).
However, since a bonding chamber must be returned to an almost atmospheric pressure condition when the substances to be bonded are put in or removed from the bonding chamber, it takes considerable amount of time to return the pressure inside of the bonding chamber to 10 -9 mmHg or more when the substances are to be bonded. Accordingly, an improvement in productivity cannot be expected.
SUMMARY OF THE INVENTION
It is an object of the present invention to eliminate the above described defects and to provide an apparatus for bonding metals or ceramics or ceramics to metals and the like more effectively within a superhigh vacuum bonding chamber.
According to the invention a bonding apparatus comprising holding means for holding a substance to be bonded and a pressing means for pressure welding substances to be bonded to each other, is characterised by a superhigh vacuum bonding chamber provided with said holding means and said pressing means, a superhigh vacuum bonding preparatory chamber connected with said superhigh vacuum bonding chamber through a gate valve and a conveying means for conveying the substances to be bonded between said superhigh vacuum bonding preparatory chamber and said superhigh vacuum bonding chamber.
BRIEF DESCRIPTION OF THE DRAWINGS
The invention will now be described, by way of example with reference to the accompanying drawings, in which:
FIG. 1 is a plan view of an embodiment of the invention;
FIG. 2 is a side view of the apparatus of FIG. 1 taken along line A--A in FIG. 1;
FIG. 3 is a diagram showing a superhigh vacuum evacuating apparatus used in an embodiment of the present invention; and
FIG. 4 is a fragmented perspective view of the principal parts explaining the operation of an embodiment of the present invention.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
The present embodiment is mainly comprised of the following four portions:
The first portion is a superhigh vacuum bonding chamber (hereinafter referred to simply as a bonding chamber) 1. The bonding chamber 1 is maintained under a superhigh vacuum of 10 -9 mmHg or more and is provided with a holding means 3 for fixedly holding two substances 2 to be bonded, a pressing means 4 for generating a minute pressure, a differential pressure type spatter-etching means 5 capable of spatter-etching surfaces to be bonded with inert gas when the vacuum of 10 -9 mmHg is maintained in order to make the surfaces to be bonded clean surfaces, and substantially ideal ones, prior to the bonding operation.
The second portion is a superhigh vacuum preparatory chamber (hereinafter referred to simply as a preparatory chamber) 6. The preparatory chamber 6 is maintained under a high vacuum of 10 -8 mmHg or more and is cut off from the bonding chamber 1 by a gate valve 7. The preparatory chamber 6 communicates with an atmosphere when the substance 2 to be bonded is put in or removed but can be held under a superhigh vacuum after the substance 2 to be bonded has been mounted on a plurality of holders 8. Additionally, the preparatory chamber 6 is provided with a spatter-vapour coating apparatus 9 capable of coating a thin film on the surface of the substance 2 to be bonded.
The third portion is a conveying means 10 for conveying the substance 2 to be bonded from the preparatory chamber 6 and for mounting it on the holding means 3 of the bonding chamber 1.
The fourth portion is a superhigh vacuum evacuating apparatus 11 for producing a superhigh vacuum within the preparatory chamber 6 and the bonding chamber 1, as shown in FIG. 3.
These portions will now be described in more detail. The bonding chamber 1 is generally cylindrical in shape and is provided with a rotary table 12 therein which is controlled so as to be rotatable through suitable angles by a rotary apparatus 17 arranged outside of the bonding chamber 1, if need arises. This rotary table 12 is provided with a stage 13 having an upwardly facing channel-shaped section fixedly mounted thereon as shown in FIG. 4. The holding means 3 for holding the substance 2 to be bonded is constructed to hold the substance 2 within the bonding chamber 1 by engaging a collar member 14a of a substance holder 14 with a groove 13a in stage 13. In addition, the bonding chamber 1 is provided in the upper portion thereof with a second stage 15 comprising a part of the holding means 3 facing the stage 13. The stage 15 has an inverted channel shape section, which is opposed to that of the lower stage 13, and is provided with a groove 15a so as to hold a holder 14 in the opposite direction. This stage 15 is connected with the pressing means 4, and is movable up and down, and is provided with a closing apparatus 16 for opening and closing the arms of the channel section stage 15.
The cylindrical preparatory chamber 6 is provided with a rotary table 23, which is similar to the rotary table 12 provided in the bonding chamber 1, four holders 8 being fixedly mounted on the rotary table 23 at regular intervals of 90°. These holders 8 have a channel-shaped section, which is generally the same as that of said substance to be bonded stage 13, as shown in FIG. 4. The holders 8 are fixedly mounted so that the open side of the channel-shape is directed sidewards, and the substance to be bonded 2 is held by engaging the collar member 14a of a holder 14 with a groove 8a of the holder 8. The preparatory chamber 6 is provided with the spatter-vapour coating apparatus 9 on the side thereof facing the holders 8, as the table 23 is turned, whereby a thin film can be coated on the surface of the substances 2 to be bonded which are mounted on a holder 8.
Also, the bonding chamber 1 is provided with the differential pressure type etching means 5 for etching the surface of the substance to be bonded 2 if necessary. Said differential pressure type etching means 5 has an upper spatter-etching apparatus 5a provided in the upper portion of the bonding chamber 1 at a side opposite to said stage 13 while a lower spatter-etching apparatus 5b is provided in the lower portion of the bonding chamber 1 facing the second stage 15. Additionally, the bonding chamber 1 is provided with an exhaust port 18 connected to said superhigh vacuum evacuating apparatus 11, operation-monitoring ports 19,20, an instrument port 21, a surface analysis port 22 and the like.
The conveying means 10 is provided with a movable shaft 10a which is rotatable and movable in an axial direction, said movable shaft 10a passing through the side wall of the preparatory chamber 6. The shaft 10a is extendable to the stage 13 in the bonding chamber 1 through said holder 8 and said gate valve 7. This movable shaft 10a is provided with a screw member 10b at the forward end thereof, the substance 2 to be bonded being conveyed between the preparatory chamber 6 and the bonding chamber 1 by turning this screw member 10b in a complimentary screw member 14b of the holder 14. Furthermore, an exhaust port 24 is connected with the superhigh vacuum evacuating apparatus 11.
The superhigh vacuum evacuating apparatus 11, as shown in FIG. 3, comprises superhigh vacuum pumps P 1 ,P 2 capable of producing a vacuum of about 10 -2 to 10 -10 mmHg, a high vacuum pump P 3 capable of producing a vacuum of about 10 -4 mmHg, vacuum gauges G 1 ,G 2 , valves B 1 ,B 2 ,B 3 ,B 4 ,B 5 ,B 6 ,B 7 ,B 8 arranged between the pumps P 1 ,P 2 ,P 3 , the bonding chamber 1, the preparatory chamber 6 and an argon gas bomb 25. The inside of the bonding chamber 1 and the preparatory chamber 6 are maintained at the desired vacuum and the bonding chamber 1 and the preparatory chamber 6 are simultaneously fed with argon gas used for ion-etching or ion-spatter vapour coating by appropriate opening and closing the various valves.
The operation of apparatus according to the present embodiment will now be described. At first, a superhigh vacuum atmosphere is produced in the bonding chamber 1 and the preparatory chamber 6. Then the preparatory chamber 6 is subjected to atmospheric pressure and a plurality of holders 14, on which the substance 2 to be bonded is mounted, are mounted on respective holders 8. After a plurality of substances to be bonded 2 are fixedly mounted on the holders 8, the desired superhigh vacuum is again produced in the preparatory chamber 6.
The surface of the substance 2 to be bonded can be subjected to the spatter-vapour coating within the vacuum preparatory chamber 6 if necessary. In this case, an inert gas such as argon gas is introduced into the preparatory chamber 6 under a vacuum of about 10 -5 mmHg and a substance, a desired thin film, can be coated on the surface as a spatter-vapour coated film by use of this inert gas. After the spatter-vapour coated film is applied, a high vacuum of 10 -8 mmHg is again produced within the preparatory chamber 6.
Upon completion of the operation in the preparatory chamber 6, the screw member 10b is turned within the screw member 14b of a holder 14 by rotating the movable shaft 10a and the holder 14 is removed from the holder 8 by axially moving the movable shaft 10a. Then the holder 14 is fixedly engaged with the stage 13 in the bonding chamber 1 by rotating the rotary table 23 in the preparatory chamber 6 by 45°, rotating the movable shaft 10a by 90°, and simultaneously opening the gate valve 7 to pass the holder 14 through the gate valve 7 and until the holder 14 engages the stage 13. After the holder 14 is fixed, the movable shaft 10a is rotated in the reverse direction to remove it from the holder 14 and the shaft 10a is returned to the original position in the preparatory chamber 6. Next, the rotary table 23 is further rotated by 45° and the pointed end of the movable shaft 10a is screwed into another holder 14, the movable shaft 10a being axially moved to remove the holder 14 from the holder 8, and the movable shaft 10a being rotated by 90°. At this juncture, in the bonding chamber 1, the rotary stage 12 has been rotated by 180° and the stage 15 has been lowered to a fixed position in alignment with the path of the shaft 10a. Subsequently, the movable shaft 10a is axially moved to fixedly mount the holder 14 onto the stage 15, the movable shaft 10a being rotated to be removed from the holder 14, the movable shaft 10a being returned to the original position in the preparatory chamber 6, and simultaneously the gate valve 7 being closed. Under this condition, one of the substances 2 to be bonded in the bonding chamber 1 is mounted on the pointed end portion of the pressing means 4 and the other one is mounted on the rotary stage 12. Accordingly, the surfaces of the substances 2 to be bonded are fixed at positions facing the upper and lower differential pressure type spatter-etching apparatus 5a,5b, respectively, so that the surfaces of the substances 2 to be bonded are subjected to the spatter-etching until a clean surface, which is substantially an ideal one, is obtained.
The substances 2 to be bonded, having the substantially ideal clean surfaces, are positioned face to face with each other by rotating the rotary stage 12 by 180°. Under this condition, minute pressure is imparted to both surfaces to be bonded by means of the pressing means 4 to carry out the bonding operation. After the completion of the bonding operation, the gate valve 7 between the bonding chamber 1 and the preparatory chamber 6 is opened and the movable shaft 10a is inserted and screwed in the holder 14 while the pressure is removed by the pressing means 4.
Such a conventional spatter-etching apparatus 5a,5b can carry out the spatter-etching by using an inert gas under a superhigh vacuum of 10 -9 mmHg and can spatter-etch an area of a certain extent or more by surface-scanning.
Then, both arms of the stage 15 are opened by means of the closing apparatus 16 to loosen the engagement of the holder 14 with the stage 15, the movable shaft 10a being returned to the preparatory chamber 6, the holder 14 being engaged with the holder 8 in the preparatory chamber 6, and simultaneously the gate valve 7 being closed. Thus, both of the substances bonded are brought into the preparatory chamber 6 in a bonded condition and can be taken out of it by returning the pressure inside the preparatory chamber 6 to an atmospheric pressure.
Thus, the procedure occurring from the time the substance to be bonded is placed in the bonding chamber to the time it is removed from the bonding chamber is complete. A large number of bonded products can be obtained by repeating the above described procedure. Although the preparatory chamber 6 disclosed is provided with four holders 8 therein, so that two bonding operations can be carried out without returning the pressure inside the preparatory chamber 6 to atmospheric pressure, it goes without saying that a larger number of bonding operations can be continuously carried out by increasing the number of the holder 8 in the preparatory chamber 6.
As described above, according to the present invention, a bonding chamber can always be maintained under a superhigh vacuum and the inside of the bonding chamber can always be kept clean, so that not only can the inside of the bonding chamber be free from contaminated air but the time required for producing a superhigh vacuum atmosphere can also be shortened thereby effectively carrying out a superhigh vacuum bonding process. | The bonding apparatus has a holding device, a pressing device for pressure welding substances to be bonded to each other, and a superhigh vacuum bonding chamber provided with the holding device and the pressing device. A superhigh vacuum bonding preparatory chamber is connected with the superhigh vacuum bonding chamber through a gate valve and a conveyor is arranged for conveying the substances to be bonded between the superhigh vacuum bonding preparatory chamber and the superhigh vacuum bonding chamber. The preparatory chamber is provided with a rotary preparatory table having a plurality of stages for releasably supporting holders for holding the substances to be bonded, the preparatory table being moved to successive positions to register with the conveyor. | 1 |
BACKGROUND OF INVENTION
1. Field of the Invention
The present invention relates to digital electronics, and more specifically, to computer-based programming tools and software for handheld digital electronic devices.
2. Description of the Prior Art
Protecting computer software from misuse has been a concern since computers were first developed. One form of misuse, software piracy, normally only results in lost revenue for software developers and publishers, but can have more significant consequences. Software piracy and misuse has conventionally been fought with various protection schemes employing encryption or activation methods.
A typical software protection scheme validates a user password before enabling and executing a software application. This type of scheme is useful for database access where different users have different access rights. Another conventional protection scheme common with commercial software applications is a hardware key. Hardware keys can take the form of a CD being inserted into a CD drive for protecting a home-user application, or a specialized hardware lock (dongle) used for protecting high-end professional applications. Besides resulting in inconveniences to users, typical protection schemes are easily worked around and circumvented.
When applied to programming software used to program electronic devices, such as programming tools used by service providers to program mobile phones, typical software protection schemes offer few advantages. First, these schemes are easily defeated, and it can generally be assumed that any individual who desires to obtain such protected programming tools can obtain them and negate the protection scheme. Second, these schemes simply passively protect the software programming tools from access or unauthorized copying, and offer no further means of protecting against actual misuse while the programming tools are functioning. This is a particularly notable shortcoming in the case of mobile phone cloning.
Once a protection scheme for a set of programming tools has been defeated, programming a mobile phone is straightforward. Parameters can be sent to the phone indiscriminately. If these parameters contain errors, the mobile phone may operate incorrectly or even cease to operate. When these parameters are stolen or duplicated a mobile phone can be cloned. Thus, the capabilities of these programming tools need to be protected to safeguard the functionality of individual mobile phones and entire mobile phone networks.
Conventionally, programming tools for mobile phones or other electronic devices have been protected against unauthorized copying and use by conventional software protection schemes, such as the hardware key or password validation schemes. The disadvantages of these schemes require that an improved method be developed.
SUMMARY OF INVENTION
It is therefore a primary objective of the present invention to provide a method for providing active protection to programming tools for programmable devices to provide security, and further, to prevent errors in programming, accordingly solving the abovementioned problems of the prior art.
Briefly summarized, a method according to the present invention includes providing a programmable device having a plurality of operational modes and a key data, and providing a computer system having configuration data corresponding to the plurality of operational modes of the programmable device. An authorized portion of the configuration data corresponds to the key data and to at least one authorized operational mode. The method further includes, first, establishing a data connection between the computer system and the programmable device and sending the key data from the programmable device to the computer system over the data connection, then, activating the authorized configuration data at the computer system referencing the received key data, before finally, programming the programmable device with the authorized configuration data through the data connection to enable a predetermined authorized operational mode.
According to the present invention, the method can further include locking configuration data not corresponding to the key data at the computer system. Locked configuration data being unusable when programming the programmable device.
According to the present invention, the method can further include confirming the authorized configuration data by referencing the key data with the programmable device and rejecting configuration data received not corresponding to the key data before programming the programmable device with the authorized configuration data.
It is an advantage of the present invention that the programmable device supplies critical information, namely the key data, to the computer system. And, the computer system is unable to program the programmable device without this critical information.
It is a further advantage of the present invention that the key data includes limitations to how the programmable device can be programmed, in effect, reducing the probability that the programmable device is programmed erroneously or in an unauthorized manner.
It is a further advantage of the present invention that misuse of software embodying the method is prevented by information contained in a specific programmable device.
These and other objectives of the present invention will no doubt become obvious to those of ordinary skill in the art after reading the following detailed description of the preferred embodiment that is illustrated in the various figures and drawings.
BRIEF DESCRIPTION OF DRAWINGS
FIG. 1 is a schematic diagram of a computer system for programming a mobile phone according to the present invention.
FIG. 2 is a flowchart of a method according to a first embodiment of the present invention.
FIG. 3 is a flowchart of a method according to a second embodiment of the present invention.
DETAILED DESCRIPTION
The present invention is described in the following as applied to programming a mobile phone. The present invention can be applied to other programmable electronic devices as well.
Please refer to FIG. 1 showing a computer system 10 for programming a mobile phone 30 . The computer system 10 includes a processor 12 and a memory 14 , such as a random access memory, in a combination well known in the art. The computer further comprises a mass storage device 16 , such as a hard drive, and a user interface 18 including a monitor, keyboard, pointing device, etc. A data cable 24 , or similar data transmission device such as radio transmitters and receivers, connects the computer system 10 to the mobile phone 30 . The mass storage device 16 stores configuration information 20 for the mobile phone 30 .
The configuration information 20 includes operating data and parameters required for the mobile phone 30 to function such as mobile phone operating software, network information, service provider information, hardware settings, and other similar information for supporting a wide variety of mobile phones. The configuration information 20 can be in the form of discrete files, each for a distinct mobile phone model, serial number, or unique identification number, or can have a more generalized data structure. A user can modify or amend the configuration data 20 thought the user interface 18 , however, the user cannot select and transmit configuration information to the phone 30 . A portion of the configuration information 20 , or a single file in the case of discrete files, is authorized (by a service provider, vendor, or manufacturer) for loading to the mobile phone 30 , and is represented in FIG. 1 as authorized configuration data 22 . The authorized configuration data 22 present in a memory of a mobile phone means the mobile phone is effectively programmed into a corresponding authorized operational mode. In practical application there is one set of authorized configuration data for each mobile phone to be programmed, only one authorized configuration data 22 being shown for clarity.
The mobile phone 30 includes a processor 32 and a memory 34 . The memory 34 stores key data 36 and phone data 38 , and is capable of storing authorized configuration data 22 . The phone data 38 includes hardware information such as manufacturer ID, serial number, time and date from an internal clock of the processor 32 , unique phone identification number, and other generally non-configurable information. The processor 32 acts on the authorized configuration data 22 stored in the memory 34 to realize the functions of the mobile phone 30 . That is, the authorized configuration data 22 is essential to the operation of the mobile phone 30 and provides the authorized operational mode. For example, the authorized configuration data 22 can comprise a service provider identification number, so that the processor 32 can instruct related systems of the phone 30 to communicate with cellular base stations of the correct service provider. Before the phone 30 is programmed with the authorized configuration data 22 , it is nonfunctional. When the mobile phone 30 is connected to the computer system 10 through the cable 24 and a data connection is established, the mobile phone 30 is ready to be programmed with the authorized configuration data 22 .
Please refer to FIG. 2 showing a flowchart of a method according a first embodiment of the present invention. The flowchart of FIG. 2 is described as follows with reference to FIG. 1 .
Step 100 : Start;
Step 102 : Establish a data capable connection between the computer 10 and the mobile phone 30 through the connection cable 24 . Once the cable 24 is connected, the processor 12 of the computer 10 initiates the connection with the processor 32 of the phone 30 ;
Step 104 : The mobile phone 30 , detecting the completion of the established connection, sends the key data 36 stored in the memory 34 to the computer 10 ;
Step 106 : The computer 10 receives and processes the key data 36 correlating it to the configuration information 20 to determine the authorized configuration data 22 ;
Step 108 : The computer 10 sends the authorized configuration data 22 to the mobile phone 30 ;
Step 110 : The mobile phone 30 receives the authorized configuration data 22 and becomes programmed;
Step 112 : End.
In this way, the above method as illustrated in FIG. 2 programs the mobile phone 30 with only a preauthorized configuration to realize a predetermined operational mode. The above method requires very little user interaction, and does not support a user directed transfer of configuration data to the mobile phone 30 . Limited non-critical user interaction is allowed through the user interface 18 . As a result, the mobile phone 30 is prevented from being given erroneous or prohibited configuration information, even though such information may be stored in the computer 10 . Further programming can occur in step 110 according to other programming tools on the computer system 10 , which unlocks these tools based on the key data 36 received.
Please refer to FIG. 3 showing a flowchart of a method according to a second embodiment of the present invention. The flowchart of FIG. 3 is described as follows with reference to FIG. 1 .
Step 200 : Start;
Step 202 : Establish a data capable connection between the computer 10 and the mobile phone 30 through the connection cable 24 . Once the cable 24 is connected, the processor 12 of the computer 10 initiates the connection with the processor 32 of the phone 30 ;
Step 204 : The computer 10 sends a request to the mobile phone 30 for the key data 36 ;
Step 206 : The mobile phone 30 , receiving and verifying the request from the computer 10 , sends the key data 36 stored in the memory 34 to the computer 10 ;
Step 208 : The computer 10 receives and processes the key data 36 correlating it to the configuration information 20 to determine the authorized configuration data 22 ;
Step 210 : The computer 10 sends the authorized configuration data 22 to the mobile phone 30 ;
Step 212 : The mobile phone 30 receives the authorized configuration data 22 and compares it to expected data, effectively confirming the configuration data 22 using the key data 36 . The mobile phone 30 rejects any data received that does not correspond to the key data 36 . This provides another layer of protection and also verifies the success of the data transfer. If the configuration data 22 is confirmed as correct go to step 214 , otherwise return to step 206 ;
Step 214 : Upon confirming the received authorized configuration data 22 , the mobile phone 30 becomes programmed;
Step 216 : The processor 32 of the mobile phone 30 determines how many times the mobile phone 30 has been programmed. If the mobile phone 30 has been programmed more than a predetermined number of times, a new key data is required, go to step 218 . If a new key is not required, go to step 220 ;
Step 218 : The processor 32 of the mobile phone 30 generates a new key data from the phone data 38 ;
Step 220 : End.
As described above, the method shown in FIG. 3 programs the mobile phone 30 with only a preauthorized configuration. The request step 204 allows for another layer of protection, via a password or similar well-known method. That is, the computer 10 is idle until a correct password is entered to initiate the programming of the mobile phone 30 . The confirmation step 212 effectively confirms or verifies the configuration data 22 using the key data 36 as a reference. This can be accomplished, for instance, by including the key data 36 or a derivative of the key data 36 (such as a checksum) in the configuration data 22 , and provides additional protection and verification of data transfer success. When the configuration data 22 is not properly confirmed, the mobile phone 30 resends the key data 36 to the computer 10 . In steps 216 and 218 , after the same key data is used to program the phone 30 a predetermined number of times, the phone 30 generates a new key data. The phone 30 generates this new key data using internal information, such as the phone data 38 , in the same way the original key data 36 was determined. Alternatively, the computer 10 can keep track of the number of times the phone 30 has been programmed and prompt the phone 30 to generate a new key data accordingly. Regardless, the key data 36 and any new replacement key data should originate from the mobile phone 30 to ensure security. Furthermore, in step 214 additional programming can occur according to other programming tools on the computer system 10 , the computer system 10 unlocking these tools after the key data 36 is received. The method illustrated in FIG. 3 accomplishes the same task as the method of FIG. 2 with enhanced protection.
In practical application, the present invention of protecting programming the tools of a programmable device such as a mobile phone can be realized with software and related hardware as illustrated in FIG. 1 . The present invention is compatible with state of the art programming tools and programmable devices.
In contrast to the prior art, the present invention provides an active protection method for programming tools of programmable devices. A programmable device sends a key data to a computer system, which then unlocks corresponding configuration data (programming instructions) and sends this authorized configuration data to the programmable device. The computer system is incapable of programming the programmable device without receiving valid key data. Thus, the present invention method ensures that a programmable device cannot be programmed erroneously or in an unauthorized manner.
Those skilled in the art will readily observe that numerous modifications and alterations of the device may be made while retaining the teachings of the invention. Accordingly, the above disclosure should be construed as limited only by the metes and bounds of the appended claims. | A method includes providing a programmable device, such as a mobile phone, having a plurality of operational modes and a key data, and providing a computer system having configuration data corresponding to the plurality of operational modes. An authorized portion of the configuration data corresponds to the key data and to at least one authorized operational mode of the mobile phone. The method further includes sending the key data from the mobile phone to the computer system over a data connection, then, activating the authorized configuration data at the computer system referencing the received key data, before finally, programming the mobile phone with the authorized configuration data through the data connection to enable a predetermined authorized operational mode. Protection from errors in programming and device cloning is insured, as the computer system is prevented from programming the mobile phone until receiving the key data from the mobile phone. | 6 |
CROSS-REFERENCE TO RELATED APPLICATION
This application claims priority from Korean Patent Application No. 10-2005-0077439, filed on Aug. 23, 2005, in the Korean Intellectual Property Office, the entire disclosure of which is incorporated herein by reference.
BACKGROUND OF THE INVENTION
(a) Field of the Invention
The present invention relates to an online FLASH game protection system, a web server, a web page provision method, an online FLASH game protection method, and a storage medium for recording the method execution program. More particularly, the present invention relates to an online FLASH game protection system including a web server that is accessed by a user terminal for performing a FLASH game and a game server for transmitting and receiving game information to/from the user terminal when playing a FLASH game and providing and protecting FLASH games, a web server, a web page provision method, an online FLASH game protection method, and a storage medium for recording the method execution program.
(b) Description of the Related Art
As the Internet has become widely used, various services have been provided over the Internet. Accordingly, services of various categories, such as Internet-based online game services and various community services, in addition to the mail services in the earlier popularization stage of the Internet, have become available. Particularly, many users use Internet game services, and the market volume of such services has gradually increased. For example, Go-Stop card games with 1:1 competition rules and various FLASH games have been provided through the Internet.
A FLASH game is a computer game generated by using ADOBE FLASH (“FLASH”), which is an Internet moving picture producing software program, and the FLASH game is generated by applying the action script and motion graphics of the FLASH program. The categories of FLASH games range from the elementary and fun ones for children to those for testing personality and mental states. Representative games include sports games such as bowling and baseball, adventure games, puzzle/board games, games for women such as make up games, slide games, picture finding games, and maze games.
FLASH games have been recently provided by Internet game service providers so that they may be used on line, and they are accordingly used by many users. Particularly, some FLASH games are provided without payment as a service policy for corresponding web page visitors.
In this instance, the respective FLASH games are configured to show URL information indicating existence of corresponding files by simply checking source codes of web pages for providing FLASH game services, and the FLASH games can be copied or linked by unknown users without permission, and hence the existing FLASH game service providers or FLASH game producers may meet with a financial loss.
Particularly, some FLASH games are provided without fee for the purpose of increasing the number of visitors to the corresponding web pages, and when a user copies or links a FLASH game and plays the same game on a different web page, the corresponding FLASH game provider may suffer a greater loss.
The above information disclosed in this Background section is only for enhancement of understanding of the background of the invention and therefore it may contain information that does not form the prior art that is already known in this country to a person of ordinary skill in the art.
SUMMARY OF THE INVENTION
The present invention has been made in an effort to prevent online FLASH games from being copied or linked without permission, and to protect the rights of game producers and game service providers.
In one aspect of the present invention, an online FLASH game protection system for providing and protecting FLASH games, wherein the system includes a web server that is accessed by a user terminal so as to perform a FLASH game and a game server for transmitting/receiving game information to/from the user terminal when performing the FLASH game, includes: a game view FLASH module for providing a game view FLASH for realizing game contents as a FLASH on a FLASH game screen displayed on the user terminal; and a game skin FLASH module for providing a game skin FLASH that is a frame to the FLASH-based game contents, the game skin FLASH module being performed when the user selects performance of a predetermined FLASH game through the web server, and controlling the game view FLASH module to perform the FLASH game contents selected by the user by referring to pre-stored FLASH game execution information according to a game ID of the selected FLASH game so that the game view FLASH source information is provided from the FLASH game execution information.
In another aspect of the present invention, an online FLASH game protection method for providing and protecting FLASH games in a system that includes a web server that is accessed by a user terminal so as to perform a FLASH game and a game server for transmitting/receiving game information to/from the user terminal when performing the FLASH game includes: a) when predetermined FLASH game performance is selected, a game skin FLASH module controlling a game skin FLASH that is a frame on a FLASH game screen to be realized on a user terminal screen; b) the game skin FLASH module checking whether a URL of the web page on which the game skin FLASH performance is started is a predetermined URL; and c) when the URL is not a predetermined URL in b), the game skin FLASH module forcibly moving the web page displayed on the user terminal to a web page having a predetermined URL, or terminating realization of the game skin FLASH.
In another aspect of the present invention, an online FLASH game protection method for providing and protecting FLASH games in a system that includes a web server that is accessed by a user terminal so as to perform a FLASH game and a game server for transmitting/receiving game information to/from the user terminal when performing the FLASH game includes: a) selecting performance of a FLASH game in which a game view FLASH that is a game contents FLASH in the FLASH game and a game skin FLASH that is a frame of the game view FLASH are respectively realized by a game view FLASH module and a game skin FLASH module, and realizing a game view FLASH; b) the game view FLASH module checking whether the game skin FLASH is realized; and c) the game view FLASH module terminating realization of the game view FLASH when no game skin FLASH is realized.
In another aspect of the present invention, an online FLASH game protection method for providing and protecting FLASH games in a system that includes a web server that is accessed by a user terminal so as to perform a FLASH game and a game server for transmitting/receiving game information to/from the user terminal when performing the FLASH game includes: a) selecting performance of a FLASH game in which a game view FLASH that is a game contents FLASH in the FLASH game and a game skin FLASH that is a frame of the game view FLASH are respectively realized by a game view FLASH module and a game skin FLASH module, and realizing a game view FLASH; b) the game view FLASH module checking whether a URL of the web page on which the game view FLASH realization is performed is a predetermined URL; and c) the game view FLASH module terminating game view FLASH realization when the URL is not a predetermined URL in b).
In another aspect of the present invention, a method for providing a web page for performing a FLASH game to a user terminal connected through a network in a system that includes a web server that is accessed by the user terminal so as to perform a FLASH game and a game server for transmitting/receiving game information to/from the user terminal when performing the FLASH game includes: a) the web server providing a web page on which source information of a game skin FLASH that is a frame on a FLASH game screen is recorded, and driving the game skin FLASH on the web page; and b) the game skin FLASH checking game view FLASH source information that is game contents of a FLASH game corresponding to a game ID of the selected FLASH game from pre-stored FLASH game execution information, and realizing the game view FLASH at a predetermined position of the web page.
In another aspect of the present invention, provided is a storage medium for recording a program for controlling the method disclosed by any one of the above-described methods, to be performed in a computer.
In another aspect of the present invention, provided is a web server configuring a network with a game server for transmitting/receiving game information to/from a user terminal and being accessed by the user terminal so as to perform a FLASH game wherein when a predetermined FLASH game performance is selected by the user terminal, the web server includes game skin FLASH source information that is a frame on a FLASH game screen and provides a web page including script that is driven on the web page, and the web server includes FLASH game execution information for storing game view FLASH source information that is game contents in the FLASH game for respective FLASH game IDs so that the game skin FLASH may check corresponding game view FLASH source information from the FLASH game execution information and perform the game view FLASH at a predetermined position of the web page.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 shows a schematic diagram for performing a FLASH game at a client in an online FLASH game protection system according to an embodiment of the present invention.
FIG. 2 shows a web page configuration provided by an online FLASH game protection system according to an embodiment of the present invention.
FIG. 3 shows a client screen configuration when a FLASH game is performed by an online FLASH game protection system according to an embodiment of the present invention.
FIG. 4 shows a flowchart for an online FLASH game protection method according to an embodiment of the present invention.
DETAILED DESCRIPTION OF THE EMBODIMENTS
Embodiments of the present invention will now be described in detail with reference to the accompanying drawings.
As shown in FIG. 1 , the online FLASH game protecting system according to the embodiment of the present invention is connected to a user terminal through the Internet, and it includes a web server and a game server.
The use terminal is a communication terminal for accessing the online FLASH game protecting system through the Internet and for performing FLASH games, and for example, a mobile communication terminal, a desktop computer, a portable computer, and other various communication devices are applicable to the user terminal.
In this instance, the game includes a game skin FLASH and a game view FLASH. The game skin FLASH functions as a FLASH game launcher, it is initially performed when the user attempts to perform the FLASH game, and it can perform or terminate the game. The game view FLASH is the substantial game contents in which the user plays a game through a user terminal, and it includes an interface (e.g., a start button when a game is loaded, a game rank provision unit, and an event notice unit) provided to the user on the FLASH game screen.
The game skin FLASH and the game view FLASH will be described in further detail later.
The web server functions as an interface for the user terminal to access the online FLASH game protecting system, converts various pieces of information provided by respective servers into predetermined communication standard data to provide the data to a plurality of user terminals, or receives information from the user terminal through the Internet and provides the information to the respective servers.
The web server provides various and selectable FLASH games to the user terminal through the Internet, and it includes a game skin FLASH module as a game skin FLASH realization file into the user terminal, and FLASH game execution information.
The FLASH game execution information includes a plurality of pieces of FLASH game execution information that can be provided by the online FLASH game providing system, and it can be stored as a CONFIG.XML file. For example, the FLASH game execution information includes a game name of a FLASH game, a game ID, version information, game view FLASH module information realizing game view FLASHes configuring a FLASH game, corresponding server information, and port information.
The web server includes a game skin FLASH module, and it controls the game skin FLASH to be performed on the user terminal and receives a game ID of a specific FLASH game selected by the user when the user selects the FLASH game.
The game skin FLASH module receives game view FLASH module information on the corresponding FLASH game from FLASH game execution information, and controls the game view FLASH to be performed on the user terminal.
The game view FLASH is the substantial game contents in which the user plays the game through the user terminal, and it includes an interface (e.g., a start button when a game is loaded, a game rank provision unit, and an event notice unit) provided to the user on the FLASH game screen. In this instance, the game view FLASH may include a substantial game contents FLASH and a UI FLASH for realizing an interface with the user.
The game server is a real-time server compared to the general request and answer servers. That is, the game server consecutively checks game results that are transmitted irrespective of the status of requests given by the user terminal having accessed the game server, and transmits/receives information to front the user terminal.
In this instance, the game server includes a game view FLASH module so that the game view FLASH ma be performed on the user terminal by control of the game skin FLASH module, and the game may be played.
Therefore, as shown in FIG. 2 , the FLASH game together with the game skin FLASH and the game view FLASH is displayed on the user terminal screen.
When the user accesses the web server to select execution of a predetermined FLASH game, the web server executes the game skin FLASH on the user terminal including the game skin FLASH module.
The game skin FLASH module controls the game skin FLASH to be loaded on to the user terminal irrespective of the FLASH game type selected by the user. Next, with reference to stored FLASH game execution information, corresponding information is received so as to perform a game view FLASH corresponding to a game ID of the corresponding FLASH game ({circle around (1)}).
For example, based on the game ID, the game skin FLASH module receives URL information including a game view FLASH module, server information for the user terminal to access the server including the game view FLASH module, and port information from the FLASH game execution information.
In this instance, the URL information of the game view FLASH module substantially configuring the game contents is included in the game execution information, is referred to by the game skin FLASH module, and is not directly displayed by the web page source codes providing the FLASH game.
Therefore it is prevented to drain URL information where the FLASH game files exist through the web page source codes, and to randomly set links or download the game files.
Next, as an example, the game skin FLASH module controls the game view FLASH module to be executed based on the information provided from FLASH game execution information such as CONFIG.XML so that the game FLASH may be displayed on the FLASH game screen of the user terminal.
In this instance, the game view FLASH module includes at UI FLASH module and a game contents FLASH module, it is an interface (e.g., a start button when a game is loaded, a game rank provision unit, and an event notice unit) provided to the user on the FLASH game screen, and it is possible to separately perform the UI FLASH and the substantial game contents FLASH.
In this case, the game skin FLASH module per the FLASH module based on the information provided from the FLASH game execution information so that the UI FLASHes including a loading screen and a game start button may be displayed on the FLASH game screen of the UI user terminal ({circle around (2)}).
The game skin FLASH module performs the game contents FLASH module based on the information provided from the FLASH game execution information so as to perform the substantial FLASH game ({circle around (3)}). For example, on receiving a selection signal on the game start button from the user terminal, the game skin FLASH module performs the game contents FLASH module so that the game contents FLASH may be displayed on the user terminal screen.
In this instance, the game skin module performs the game view FLASH module and checks whether the URL of the corresponding web page corresponds to the predefined URL when configuring the web page for performing the FLASH game.
That is, on configuring the web page for substantially performing the FLASH game, the game skin module can terminate the execution of the corresponding game when the address of the web page is changed not by the predefined URL but by an unknown user without any permission. Also, the game skin module can forcibly move the user terminal's screen to a predetermined URL, for example, a web page of a FLASH game service provider.
As a result, it is prevented for the unknown user to transfer the corresponding FLASH game including the game skin module and the game view module without permission, and to perform the FLASH game at a changed web page and not at a predetermined address.
Further, the game view FLASH module checks the existence of the game skin FLASH when the game view FLASH is performed on the user terminal. That is, the game view FLASH module checks whether the game skin FLASH is performed on the web page on which the FLASH game is performed, and can terminate the performance of the game when there is no game skin FLASH.
Further, when there is a game skin FLASH, the game view FLASH module checks whether the web page standing by for game performance corresponds to the predetermined URL, and can terminate performance of the game when the web page does not correspond to the predetermined URL.
Therefore, it is prevented for the users to transfer the substantial game contents except the game skin without permission.
FIG. 3 shows a FLASH game screen configuration displayed on the user terminal screen by a game skin FLASH module and a game view FLASH module.
The FLASH game screen includes a game skin FLASH and a game view FLASH.
The game skin FLASH is initially performed on the user terminal when a FLASH game is performed, and the game skin FLASH can be displayed to include the subsequent game view FLASH in a like manner of a frame.
In this instance, the game skin FLASH can control the game view FLASH to be loaded onto the game skin FLASH in a like manner in which the conventional web browser loads a web page onto the web browser. Also, the game skin FLASH is provided on the user terminal and is performed thereon depending on the game types, and the game skin FLASH module controls the game view FLASH module and it is possible to configure the game skin FLASH in an invisible manner.
The game view FLASH is substantial game contents played by the user, and realizes the performance of a game, that is, the original function of the game. In this instance, the game view FLASH can include a UI FLASH and a game contents FLASH.
The UI FLASH can realize common parts included by other FLASH games (e.g. a game start button, a rank display blank, and an event display blank) or additional functions, and the game contents FLASH can realize the original function of the game.
Referring to FIG. 4 , an online FLASH game protecting method according to an embodiment of the present invention will now be described.
First, when the user accesses the online FLASH came providing web server through the user terminal to select a specific FLASH game, the game skin FLASH module controls the game skin FLASH to be performed on the screen of the user terminal irrespective of the type of the FLASH game selected by the user (S 100 ).
In this instance, when the corresponding web page on which the FLASH is performed is not the predefined URL, the game skin FLASH module can forcibly move the user to a predetermined web page. In addition, the game skin FLASH module can terminate game screen loading for FLASH game performance (S 110 and S 190 ).
Therefore, it is prevented for the unknown user to transfer the corresponding FLASH game including the game skin module and the game view module without permission, and to perform the FLASH game at a changed web page and not at a predefined address.
When the FLASH execution web page is the predetermined URL, the game skin FLASH module checks FLASH game information corresponding to the FLASH game ID selected by the user based on the FLASH game execution information such as CONFIG.XML (S 120 ).
The game skin FLASH module controls the game view FLASH module so that the game may be loaded on the screen of the user terminal while the substantial game screen of the corresponding FLASH game is displayed (S 130 ). When the user clicks the game start button displayed on the screen of the user terminal the game starts (S 140 ).
That is, the game skin FLASH module receives information for performing the corresponding FLASH game including game view FLASH module information from the stored FLASH game execution information. Therefore, transfer the FLASH game without permission is prevented by checking the URL of the FLASH game files shown in the source codes since no user can check UL, information of the corresponding FLASH game files by checking the source codes of the web page for providing the FLASH game.
The game view FLASH module checks whether the game skin FLASH is performed by the game skin FLASH module (S 150 ). The game view FLASH module terminates setting the corresponding web page (S 200 ) when determining that no game skin FLASH is provided.
Also, the game view FLASH module can terminate setting the corresponding web page for performing the FLASH game when the web page on which the FLASH game is performed is not a predefined web page's URL while there is a game skin module (S 160 and S 200 ).
Therefore, it is prevented to transfer the game view FLASH for substantially performing the FLASH game.
The game view FLASH module controls game information for substantially performing the FLASH game to be loaded on to the user terminal and performs the game (S 160 -S 180 ) when there is a game skin module and the URL of the web page set for performing the FLASH game corresponds to the predefined URL.
While this invention has been described in connection with what is presently considered to be practical exemplary embodiments, it is to be understood that the invention is not limited to the disclosed embodiments, but, on the contrary, is intended to cover various modifications and equivalent arrangements included within the spirit and scope of the appended claims.
For example, the server configuration of the above-described online FLASH game protection system can be further classified or combined according to functions, and the functions are not restricted according to their titles.
According to the present invention, it is prevented for an undesired user to check the source codes of the web page for providing various online FLASH games and transfer specific FLASH games without permission.
Particularly, protection for the FLASH game provided on the Internet is further reinforced since a single FLASH game is divided into modules depending on the functions, and the modules can crosscheck the URLs of web pages on which the corresponding FLASH game is performed. | Disclosed is a system for providing and protecting online FLASH games, the system including: a game view module configured to provide a FLASH game view for realizing game content as a FLASH application on a game screen displayed on a user terminal; and a game skin module configured to provide a FLASH game skin comprising a frame of FLASH game content, wherein the game skin module is configured to operate in response to, at least in part, selecting performance of a predetermined FLASH game through a web server, and configured to control the game view module to perform the FLASH game content by referring to pre-stored FLASH game execution information based at least in part on a game ID of the selected FLASH game, so that the game view FLASH source information is provided from the FLASH game execution information. | 0 |
This application is a continuation-in-part of pending U.S. Ser. No. 617,255, filed Mar. 18, 1996 now U.S. Pat. No. 5,667,962.
BACKGROUND OF THE INVENTION
This invention relates to several new pyruvate compounds and methods of treating (i) ischemia in mammalian hearts, lungs, veins, arteries and other organs or tissues, (ii) accelerating ethanol oxidation/preventing acute toxic effects of ethanol on the liver, and (iii) other recognized uses of pyruvates including, but not limited to, treating of secondary effects of diabetes, lowering of cholesterol and lipid levels, as a nutrition source which can provide as much as 100% of caloric requirements and to treat injured organs requiring a readily accessible energy source.
DESCRIPTION OF THE ART
Ischemia is defined herein as the interruption of oxygen supply, via the blood, to an organ or to part of an organ. Examples of ischemic events include (i) myocardial, cerebral, or intestinal infarction following obstruction of a branch of a coronary, cerebral, or mesenteric artery, and (ii) removal and storage of an organ prior to transplantation. In the case of myocardial infarction, prompt restoration of blood flow to the ischemic myocardium, i.e. coronary reperfusion, is a key component of the treatment. This is because mortality is directly related to infarct size (tissue necrosed) which is related to the severity and duration of the ischemic event.
Notwithstanding the need to supply an organ cut-off from a normal blood supply with oxygen, it has been found that reperfusion injury may occur upon restoration of blood flow. This results from-the production of reactive oxygen species (ROS), namely, hydrogen peroxide, hydroxyl radicals and superoxide radicals which are formed from both extracellular and intracellular sources. ROS are highly reactive species that, under normal conditions, are scavenged by endogenous defense mechanisms. However, under conditions of post-ischemic oxidative stress, ROS interact with a variety of cellular components, causing peroxidation of lipids, denaturation of proteins, and interstitial matrix damage, resulting in increase of membrane permeability and release of tissue enzymes.
In an attempt to minimize these undesirable side effects of perfusion, researchers Simpson, et al., (Free Radical Scavengers and Myocardial Ischemia, Federation Proceedings, Volume 46, No. 7 May 15, 1987) suggest the use of an inhibitor of ROS production to protect the reperfused myocardium. The Simpson, et al. disclosure is particularly directed to the use of agents and inhibitors (ex. allopurinol) that reduce ROS levels. In a similar context, Brunet, et al., (Effects of Acetylcysteine, Free Radical Biology and Medicine, Volume XX, No. X 1995) suggest the use of acetylcysteine to reperfuse hearts. In particular, the article concludes that acetylcysteine treatment decreases the production of ROS in reperfused rat hearts.
In a further effort directed to protecting reperfused heart tissue, U.S. Pat. No. 5,075,210, herein incorporated by reference, discloses a process for reperfusing a heart for transplantation. The patent discloses a cardioplegic solution containing sodium chloride, potassium chloride, calcium chloride, sodium bicarbonate, sodium EDTA, magnesium chloride, sodium pyruvate and a protein.
U.S. Pat. No. 5,294,641, herein incorporated by reference, is directed to the use of pyruvate to prevent the adverse effects of ischemia. The pyruvate is administered prior to a surgical procedure to increase a patient's cardiac output and heart stroke volume. The pyruvate is administered as a calcium or sodium salt. The pyruvate can alternatively be an ester of pyruvic acid such as ethylamino pyruvate. Similarly, U.S. Pat. No. 5,508,308, herein incorporated by reference, discloses the use of pyruvyl glycine to treat reperfusion injury following myocardial infarction.
U.S. Pat. No. 4,988,515 and 5,705,210, herein incorporated by reference, use pyruvate salts in cardioplegic solutions and in preservation solutions for the heart before transplantation. U.S. Pat. No. 4,970,143, herein incorporated by reference, discloses the use of acetoacetate for preserving living tissue, including addition of the pyruvate to the preservation solution.
U.S. Pat. No. 5,100,677 herein incorporated by reference, discloses the composition of various parenteral solutions. Of interest is a recommendation to include pyruvate anions (apparently from metal salts) in intravenous solutions. In U.S. Pat. No. 5,183,674, herein incorporated by reference, pyruvate compounds are used as foodstuff. U.S. Pat. No. 5,134,162 herein incorporated by reference, focuses on the use of pyruvate to lower cholesterol and lipid levels in animals. U.S. Pat. No. 5,047,427, deals with the use of pyruvate for improving the condition of diabetics, while U.S. Pat. No. 5,256,697 suggests the use of pyruvyl-aminoacid compounds, each of which is herein incorporated by reference.
In addition, U.S. Pat. No. 5,283,260, herein incorporated by reference, is directed to treatment of diabetes with a physiologically acceptable form of pyruvate. The patent discloses a pyruvate compound in the form of a covalently linked pyruvyl-amino acid. By utilizing this type of a pyruvate delivery system, the negative effect of pyruvate salt is avoided. However, administration of large amounts of pyruvate-amino acid may result in nitrogen overload which could harm patients with liver and/or kidney pathology.
Notwithstanding the acceptance of pyruvate as an effective component of a reperfusion solution or other varied applications, pyruvic acid is a strong and unstable acid which cannot be infused as such. Furthermore, it has been recognized that traditional pharmacological pyruvate compounds, such as salts of pyruvic acid, are not particularly physiologically suitable. For example, these compounds lead to the accumulation of large concentrations of ions (ex. calcium or sodium) in the patient's body fluids. Similarly, amino acid compounds containing pyruvate can lead to excessive nitrogen loads. It has also been proposed to infuse pyruvylglycine, the amide function of which is presumably hydrolyzed in plasma and/or tissues, thus liberating pyruvate. However, at the high rates of pyruvylglycine infusion required to achieve 1 mM pyruvate in plasma, the glycine load may be harmful to patients suffering from hepatic or renal pathologies. Also, flooding plasma with glycine may interfere with the transport of some amino acids across the blood-brain barrier. Accordingly, while potentially suitable to organ preservation, these pyruvate compounds are less suited to treating an organ in vivo, and it is recognized that a need exists to provide a pyruvate delivery compound which is more physiologically acceptable.
Therefore, it is desirable in this field to have an alternate physiologically compatible therapeutic pyruvate compound. In this regard, the novel pyruvate compounds of this invention permit the use of pyruvate to treat ischernic events, ethanol poisoning, acetaminophen poisoning and other recognized pyruvate effective treatments because sufficiently high loads of pyruvate can be administered without a toxic constituent.
SUMMARY OF THE INVENTION
Accordingly, it is a primary object of this invention to provide a new and improved pyruvate compound(s).
It is an advantage of this invention to provide a new and improved method for organ reperfusion. It is still a further advantage of this invention to provide a new and improved method for treating ethanol intoxication. An additional advantage of this invention is to provide a pyruvate compound which can provide nutritional benefits.
To achieve the foregoing objects and in accordance with the purpose of the invention, as embodied and broadly described herein, one novel pyruvate compound of this invention comprises a pyruvate thiolester. Preferably, the thiol is cysteine or homocysteine. In a particularly preferred form, the compound is a N-acetyl ethyl ester of the cysteine or homocysteine amino acid.
One preferred compound is: ##STR1##
A further novel compound of the present invention is a glycerol-pyruvate ester. A particularly preferred form of a glycerol-pyruvate ester will be of the formula: ##STR2## where one, two, or three groups are pyruvyl ##STR3## and one or two R may be a short-chain acyl such as acetyl or propionyl. and more preferably ##STR4##
Another novel compound of the present invention is a dihyroxyacetone-pyruvate ester. A particularly preferred form of this compound is of the formula: ##STR5## where one or two R groups are pyruvyl ##STR6## and one R may be a short-chain acyl such as acetyl or propionyl. and more preferably ##STR7##
The invention is also directed to use of the novel pyruvate compounds in reperfusion of tissue and organs both in vivo and in storage. Accordingly, the invention includes a method for the preservation of tissue deprived of oxygen through events including, but not limited to, coronary infarction, stroke, mesenteric infarction, organ transplant (during preservation and intravenously after grafting of the organ) including amputated limbs. The compound is also believed well suited to treatment of acetaminophen poisoning of the liver which depletes liver glutathione stores leading to acute hepatic necrosis.
This invention is also directed to the use of the novel pyruvate compounds to assist a patient's body in ethanol oxidation. In fact, the novel pyruvate compounds of this invention are suited to use as nutritional supplements, preventing body fat deposition, lowering high blood cholesterol levels, and treatment for secondary diabetes effects.
It is believed that pyruvate acts as a NADH trap and a trap for ROS generated upon reperfusion. In addition, the thiol group from cysteine, for example is believed to scavenge ROS. Similarly, the carbonyl group of dihydroxyacetone acts as a NADH trap. Accordingly, the subject novel compounds provide stable, and physiological compounds with the beneficial result of delivering pyruvate and an additional NADH and ROS trapping moiety.
BRIEF DESCRIPTION OF THE DRAWINGS
The invention consists of the novel parts, construction and arrangements, combinations and improvements shown and described. The accompanying drawings, which are incorporated in and constitute a part of the specification illustrate one embodiment of the invention and together with the description explain the principals of the invention.
Of the drawings:
FIGS. 1 and 2 are graphical representations of the results of the experiments on ischemia of isolated rabbit hearts set forth hereinbelow;
FIGS. 3-7 show the results of experiments or ethanol oxidation in livers;
FIGS. 8 and 9 show the results of experiments directed to pyruvate concentrations in arterial blood; and
FIG. 10 shows the results of experiments on the effect of DPAG on ethanol uptake.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
For the purposes of this disclosure, the following abbreviations are used: ADH, alcohol dehydrogenase; ALDH, aldehyde dehydrogenase; DCA, dichloroacetate; DHA, dihydroxyacetone; DHAP, dihydroxyacetone phosphate; DPAG, dipyruvyl-acetyl-glycerol; FAEE, fatty acid ethyl esters; GC, gas chromatography; GCMS, gas chromatography-mass spectrometry; LAD, left anterior descending coronary artery; MPE, molar percent enrichment; MS, mass spectrometry; NAC, N-acetylcysteine; NEFA, non-esterified fatty acids; PADA, pyruvyl-acetyl-dihydroxyacetone; PDH, pyruvate dehydrogenase; PNACE, pyruvate N-acetylcysteine ethyl ester; ROS, reactive oxygen species.
Reperfusion
As described above, timely coronary reperfusion as treatment for acute myocardial infarction reduces myocardial infarct size and improves survival rates. However, there is concern that reperfusion may cause further injury to the myocardium, called "reperfusion injury". More particularly, experimental studies have demonstrated that myocardium reperfused after reversible ischemia exhibits prolonged depression or "myocardial stunning". There is evidence that reperfusion of ischemic myocardium results in the generation of ROS and that a burst of ROS production at the time of reperfusion causes myocardial damage. Accordingly, attempts have been made to provide pyruvate compounds which trap and/or prevent the formation of ROS.
One form of the present invention is a novel compound including a pyruvate moiety which also traps reducing equivalents (NADH) and ROS, and a thiol moiety which traps ROS. Accordingly, the present compound provides dual functionality in an effective and highly efficient manner and in a physiologically soluble molecule. In addition, the compounds are degraded to physiological and safe metabolites (pyruvate, cysteine or homocysteine). Lastly, the present inventive compound is equally applicable to use in the preservation of organs removed for transplantation.
In summary, the novel compounds are redox chimeras whose molecules contain a trap for reducing equivalents (NADH) and a trap for ROS.
The inventive compounds demonstrate the following characteristics;
(i) water solubility;
(ii) no ionic charge, to facilitate diffusion through cell membranes and to avoid the need to administer a counter-ion, such as Na + ;
(iii) metabolizable to physiological compounds; and
(iv) stability in solution.
PNACE
One preferred group of the inventive compounds is a thiolester of pyruvate and a sulfur amino acid, for example cysteine or homocysteine. Preferably, any ionizable functions on the amino acid molecule are blocked by easily removable radicals, such as ethyl and N-acetyl groups. The most preferred compound is formed of pyruvate and N-acetylcysteine ethyl ester.
The invention will now be described with reference to the following examples, intended to describe, but not limit the invention.
Recovery of isolated rabbit hearts following 25 min of warm ischemia
Hearts were removed from anesthetized New Zealand rabbits (2.5-3.0 kg) and perfused in the working mode at 37° with non-recirculating Krebs-Ringer bicarbonate (KRB) buffer containing 5 mM glucose and 5 units/l of insulin, and equilibrated with a gas mixture containing 95% O 2 +5% CO 2 . In the working mode, which simulates physiological conditions, hearts pump the buffer against a 85 cm hydrostatic pressure in the aorta. The mechanical performance of the hearts was assessed by monitoring heart rate, cardiac output, coronary flow, left ventricular pressure, and dP/dt max . The latter parameter reflects the capacity of the heart to increase hydrostatic pressure in the left ventricle.
Following 30 minutes of equilibration, the hearts were made ischemic for 25 minutes by clamping the aortic and left atrial canulas. Then, the clamps were removed to allow reperfusion with oxygenated KRB buffer containing either no additive (n=7, control group), or 20 μM pyruvate-N-acetyl-cysteine ethyl ester (PNACE) (n=7). PNACE was infused via a syringe pump into the inflowing perfusate. In the syringe, PNACE was dissolved in 0.1 mM HCl to prevent hydrolysis of the thiolester.
None of the control group hearts recovered any function. In contrast, hearts reperfused with buffer containing 20 μM PNACE recovered 75 to 95% of their mechanical function after reperfusion was instituted (see FIGS. 1 and 2). Functional recovery lasted throughout the 30 minute reperfusion experiment.
Recovery of isolated rabbit hearts following massive catecholamine injury
Rabbit hearts were perfused in the working mode as in the above example. However, after the 30 minutes of equilibration, 50 μM isoproterenol was added to the inflowing perfusate for 10 min. Isoproterenol is a catecholamine, which, at the dose administered, induces a marked increase in heart rate and cardiac output. After 10 minutes, the mechanical performance of the hearts decreased markedly to the point where cardiac output was almost zero. Then, isoproterenol infusion was stopped, and perfusion was continued for 30 minutes with oxygenated KRB buffer containing either no additive (n=7, control group), or 20 μM PNACE (n=7). The hearts perfused with plain buffer did not show recovery of cardiac function. In contrast, hearts perfused with buffer containing 20 μM PNACE recovered 75 to 95% of their mechanical function.
The data of these experiments proved substantially similar to that shown in FIGS. 1 and 2.
Improved function of preserved rat livers
Livers from overnight-fasted rats were surgically removed and flushed at 37° C. with non-recirculating KRB buffer containing 5 mM glucose and equilibrated with a gas mixture containing 95% O 2 +5% CO 2 The first group of livers (n=7, control group) was not preserved, but was perfused at 37° C. for 45 minutes. The second group of livers (n=8, preserved group) was flushed with ice-cold University of Wisconsin (UW) preservation solution and stored for 24 hours in ice-cold UW solution. Next, the livers were reperfused at 37° C. with non-recirculating KRB buffer containing 5 mM glucose. The third group of livers (n=8, preserved+PNACE group) was treated as the second group except that 20 μM PNACE was added to the UW preservation solution and to the reperfusion KRB buffer. During the last 45 min of (re)perfusion, the function of the three groups of livers was assessed by (i) the release of three cellular enzymes, i.e. lactate dehydrogenase, aspartate aminotransferase, and alanine aminotransferase, (ii) oxygen consumption, and (iii) the production of ketone bodies, ie β-hydroxybutyrate+acetoacetate, after addition of 1 mM octanoate to the perfusate.
The data depicted in the Table, show that, in preserved reperfilsed rat livers, PNACE (i) markedly decreases the initial release of tissue enzymes, (ii) restores partially the capacity of the liver to oxidize fatty acids to ketone bodies, and (iii) restores oxygen consumption to the level of non-preserved livers.
______________________________________Effect of PNACE on metabolic integrity of preserved rat liversupon reperfusionAll data from group III are statistically different from thecorresponding data of group II. Group I Group II Group IIIParameter Control non- Control Preserved +measured preserved (8) PNACE (8)______________________________________Release of lactate 1.9 21.8 4.5dehydrogenase (U/L · g)10-14 min.Release of aspartate amino- 0.28 3.4 0.73transferase (U/L · g)25-30 min.Release of alanine 0.21 3.7 0.33aminotransferase (U/L · g)25-30 min.Ketone body production 3.1 0.9 1.4(μmol/min · g) 25-30 min.Oxygen consumption 2.1 1.3 2.4(μmol/min · g) 25-30 min.______________________________________
Synthesis of PNACE
As understood in the art, pyruvate has proven to be a relatively unstable compound with very limited mechanism for satisfactory delivery to subjects. However, the present inventive compound has proven to be readily manufacturable and very effective in the prevention of organ damage associated with reperfusion injury. The compound has been prepared in pure form and in gram amounts. Its formula has been confirmed by elemental analysis and gas chromatography-mass spectrometry. The compound is stable in slightly acidic solutions (pH 4-5). At pH 7.4, it is slowly hydrolyzed to pyruvate and N-acetylcysteine ethyl ester. The compound has also been synthesized labeled with three deuterium 2 H atoms on the N-acetyl moiety. This deuterated compound is used as an internal standard for the assay of the compound by isotope dilution gas chromatography-mass spectrometry.
In a three-neck flask of 500 ml, freshly distilled pyruvic acid (9.06 g., 0.102 mol) and N-hydroxy-succinimide (11.82 g., 0.102 mol) in dry tetrahydrofurane (THF) (180 ml) was stirred under nitrogen and was cooled in a ice bath. Dicyclohexylcarbodiimide (21.2 g., 0.102 mol) dissolved in dry THF (150 ml) was added slowly to the stirred cooled mixture over approximately 1 hr. Then, the reaction mixture was stirred at room temperature for 2.5 hr, followed by slow addition of N-acetyl-L-cysteine ethyl ester (6.81 g., 0.033 mol) dissolved in 20 ml dry THF over approximately 1 hr. The reaction mixture was stirred overnight at room temperature under a nitrogen atmosphere.
After evaporating the THF, the residue was suspended in ethyl acetate (750 ml) and was kept for 4-6 hr at 0° C. Dicyclohexyl urea (DCU) was then filtered and discarded, the ethyl acetate solution was washed three times with water (3×100 ml). It was then dried over anhydrous sodium sulfate and concentrated under vacuum.
The product (17-18 g.) was further purified by using column chromatography. A column of 5 cm. diameter was filled with silica gel (180-200 g., 60 Angstrom flash chromatography from Aldrich). The product was dissolved first in a minimum quantity of ethyl acetate:hexane (60:40) and was loaded on the column. The column was developed under gravity (rather than flash chromatography) with ethyl acetate:hexane (60:40). Fifty ml fractions were collected and monitored by TLC using either iodine or UV light. The fractions containing the product were combined and solvents were removed under reduced pressure. The residue was dissolved in chloroform (300 ml), first washed with 5% HCl (2×30ml) and then saturated NaCl (3×60 ml). The organic layer was dried over anhydrous sodium sulfate, filtered, and the solvent evaporated. The residue was dissolved in a minimum quantity of chloroform, and petroleum ether was added until the solution became turbid. The suspension was kept overnight in the refrigerator and then filtered to get the pure crystallized product. The compound was dried under vacuum over P 2 O 5 to a yield of 6.5 g. (75%, based on the N-acetyl-L-cysteine), m.p. 76°-77° C.
Alternative Synthesis of PNACE
To a 250 ml three neck flask fitted with a thermometer, a magnetic stirrer, a 50-ml pressure-compensated addition funnel, and a Friedrich's condenser under nitrogen, was added 10 g (52.3 mmoles) of N-acetyl-L-cysteine ethyl ester, 8.0 ml of dry pyridine and 60 ml of dry benzene.
Pyruvoyl chloride (0.104 mole, 2 eq) was added dropwise over a period of 0.5 hr. while maintaining a temperature of 5° C. to 10° C. Then, the reaction mixture was allowed to warm to 25° C. and stirred for 2 hours at this temperature. The benzene solvent was then evaporated under vacuum. The crude product was purified as above to yield 11.15 g of the desired compound (82%).
Synthesis of Deuterated PNACE
Pyruvate-N- 2 H 3 !acetyl-L-cysteine ethyl ester
Synthesized wherein the above procedure was followed using N- 2 H 3 ! acetyl-L-cysteine ethyl ester to form (d 3 -PNACE). The latter was prepared by reacting L-cysteine ethyl ester with 2 H 6 !acetic anhydride.
Set forth hereinbelow are certain analytical characteristics of the composition of the invention provided to facilitate identification thereof, but not intended to limit the scope.
Characteristics of Compounds
I. Pyruvate-N-acetyl-L-cysteine ethyl ester: PNACE (unlabeled)
mp: 65° C. Rf (ethyl acetate/petroleum ether: 3/2): 0.52 IR (Nicolet 300, CCl 4 ) (cm -1 ) 3435 (V N--H) 3000 (v C--H) 1747 (v CO--O) ester 1731 (v CO--S) thioester 1687 (v CO--CO,CO--N) ketoester, amide 1497, 1378.3, 1210.1
NMR 1 H, 300 MHz (Varian, CDCl 3 , TMS) (ppm): 1.33 (t, 3 J=7.13, 3H, OCH 2 CH 3 ) 2.10 (s, 3H, COCH 3 ) 2.50 (s, 3H, CH 3 COCO) 3.45 (dd, 3 J=4.10 Hz, 3 J=8.95 Hz, 2H, CH 2 --S) 4.23 (dd, 3 J=7.13 Hz, 2H, CH 2 CH 3 ) 4.83 (m, 1H, CH) 6.50 (sl, 1H, NH) Mass spectrum, electron ionization (m/z): 190 (M-CH 3 COCO,33); 118(26); 102(56); 76(33), 60(90), 43 (CH 3 CO + , 100)
NMR 13 C, 100.12 MHz (Bruker, CDCl 3 , TMS)(ppm): 190.6; 188.08 keto, ketoester 168.6, 168.08 ester, amide 60.1 (OCH 2 ) 49.5 (CH 2 S) 28.4 (CHNH) 21.9 (CH 3 COCO) 20.8 (CH 3 CO) 12.1 (CH 3 CH 2 ) Mass spectrum, ammonia chemical ionization (m/z): 279 (M+18, 100);262(M+1, 93);209(49);192(60) 175(18), 158(26)
II. Pyruvate-N- 2 H 3 !acetyl-L-cysteine ethyl ester: d 3 -PNACE (deuterated)
NMR 1 H, 300 Mhz (Varian, CDCl 3 , TMS) (ppm): 1.34 (t, 3 J=7.13, 3H, OCH 2 CH 3 ) 2.50 (s, 3H, CH 3 COCO) 3.42 (dd, 3 J=4.10 Hz, 3 J=8.95 Hz, 2H, CH 2 --S) 4.25 (dd, 3 J=7.13 Hz, 2H, CH 2 CH 3 ) 4.90 (m, 1H, CH) 6.50 (sl, 1H, NH) Mass spectrum, electron ionization (m/z): 193 (M- CH 3 COCO, 17); 121(4);103(29); 77(12); 63(26); 43 (CH 3 CO, 100)
NMR 13 C, 100 MHz (Bruker, CDCl 3 , TMS) (ppm): 190.5; 187.08 keto, ketoester 168.5, 168.10 ester, amide 60.1 (OCH 2 ) 49.1 (CH 2 S) 28.1 (CHNH) 20.8 (CH 3 COCO) 19.9 (CH 3 CO) 12.0 (CH 3 CH 2 ) Mass spectrum, ammonia chemical ionization (m/z): 282(M+18, 42); 265(M+1, 47); 212(23), 195(37); 178(53), 161(100); 106(23); 89(15).
Ethanol Metabolism
The following is believed to represent aspects of the human system for ethanol oxidation, but is supplied only as a representation of the theory, and is not intended to limit the invention in any way.
Ethanol is oxidized to acetate in the liver and the stomach by two reactions catalyzed by alcohol dehydrogenase (ADH) and aldehyde dehydrogenase (ALDH) which use NAD + as coenzyme. The bulk of ADH activity is in the liver. ALDH activity appears to occur in most tissues.
The ADH reaction is reversible; the mid-potential of the ethanol/acetaldehyde couple is -230 mV, which is very close to that of the lactate/pyruvate couple (-225 mV). In the absence of ALDH, the plasma ethanol/acetaldehyde ratio would be similar to the lactate/pyruvate ratio (about 10). However, the equilibrium of ADH is displaced by ALDH, the equilibrium of which is far toward acetate because of the very negative mid-potential of the acetaldehyde/acetate couple (-265 mV). As a result, the ethanol/acetaldehyde ratio is very high (>1000) and the acetaldehyde concentration difficult to measure (in the low μM range) unless ALDH is inhibited by disulfiram. In this invention, strategies for accelerating ethanol oxidation target the ADH pathway, but may have an impact on some of the toxic effects derived from non-ADH pathways.
Ingestion of alcoholic beverages leads to ethanol concentrations in body fluids that are much higher than the Km of liver ADH for ethanol. For example, in many US states, the legal limit of blood ethanol concentration compatible with driving a car, is 0.75 g/l or 17 mM. Drunkenness occurs at concentrations above 30 mM, and alcoholic coma at variable concentrations above 40 mM.
Reducing equivalents generated in the cytosol by ethanol oxidation are transferred to the mitochondria via the malate/aspartate and the citrate/malate shuttles. In mitochondria, reducing equivalents are oxidized in the respiratory chain. Ethanol oxidation can be seen as a sequence of three processes catalyzed by ADH, the reducing equivalent shuttles and the respiratory chain. It is possible to set up in vitro conditions where ethanol oxidation is limited either by ADH, the shuttles or the respiratory chain. However, in the intact in vivo liver, ethanol oxidation appears limited by the capacity of the respiratory chain to oxidize reducing equivalents, which itself is set by the ATP turnover. Under extreme conditions, most of the liver O 2 uptake is used to oxidize the reducing equivalents derived from ethanol.
Since the rate of ethanol oxidation is limited by the ATP turnover, an increase in this turnover raises the capacity to oxidize ethanol. In chronic ethanol ingestion (before liver decompensation), hyperthyroidism and chronic exposure to cold, the liver ATP turnover and the capacity of ethanol oxidation increase. In fact, a single gavage of ethanol induces (i) an increase in the rate of O 2 uptake by the rat liver perfused in the absence of ethanol, and (ii) an increase in the in vivo capacity of rats and humans to oxidize a second dose of ethanol.
In isolated livers, one can accelerate ethanol oxidation by imposing a drain on ATP with ureogenic substrates (NH 4 Cl+ornithine+asparagine for example), gluconeogic substrates or uncoupler of the respiratory chain. In dogs, an intragastric gavage of NH 4 HCO 3 increases the rate of ethanol oxidation. However, the toxicity of uncouplers precludes their use in vivo.
The liver of an adult human accounts for only 2% of body weight. However, the liver receives 100% of water-soluble nutrients absorbed from the gut. In addition, it must handle part of the lipid material (i) absorbed from the gut via the lymphatic system and (ii) released by adipose tissue lipolysis. Only a small fraction of nutrients' energy is used in the liver. Most of this energy is exported as substrate molecules to peripheral tissues.
The O 2 uptake of the 1.5 kg liver of a 75 kg subject is about 3 mol/day. Thus, the maximum ATP production of the liver is 18 mol/day. If all this O 2 uptake were used to oxidize ethanol to CO 2 , only 1.1 mol of ethanol (51 g) could be oxidized per day. This would leave no room for (i) the obligatory hepatic ATP production from protein catabolism, (ii) ATP production from carbohydrate and fat catabolism. The liver manages this energy plethora by exporting most of the potential energy of ethanol as acetate, thus decreasing by 80% the hepatic ATP production from ethanol. Acetate is well used in peripheral tissues.
While most ethanol can be exported from the liver, there is no large-scale mechanism for exporting reducing equivalents from the liver. One obvious export mechanism would (i) trap reducing equivalents in the conversion of pyruvate to lactate, and (ii) export lactate to peripheral tissues. However, plasma pyruvate concentration is very low (0.05-0.1 mM). Pyruvate could be generated from glucose and amino acids, but these processes would further increase the liver's ATP burden. For these reasons the exogenous pyruvate compounds of the present invention are particularly suited to assist the body with ethanol oxidation.
The unregulated production of reducing equivalents in the liver increases the cytosolic and mitochondrial NADH!/ NAD + ! ratios. This redox shift inhibits gluconeogenesis from proteins and the recycling of glucose in the Cori cycle by displacing the equilibrium of lactate, malate and α-glycero-P dehydrogenases. If the hepatic glycogen reserves are exhausted (for example after more than 12 hr of fasting), inhibition of gluconeogenesis can induce alcoholic hypoglycemia which can lead to hypoglycemic coma, brain damage and death. In addition, the redox shift inhibits the citric acid cycle at α-ketoglutarate dehydrogenase, lowering CO 2 production and the respiratory quotient sometimes to almost zero. Then, all the liver O 2 uptake is used to oxidize the reducing equivalents derived from ethanol.
Other processes are involved in the hepatic toxicity of ethanol: binding of acetaldehyde to proteins, damage to proteins by free radicals (superoxide, hydroxyl) probably generated by cytochrome P450 IIE1, which is induced by chronic alcohol ingestion. There is evidence that ethanol generates pro-oxidant reactive species in both the liver and the central nervous system. This leads to depletion of glutathione and to the covalent binding of hydroxyethyl radicals to liver microsomal proteins. Free radical damage and malnutrition are most likely implicated in the cirrhotic process.
Fatty acid ethyl esters (FAEE) have been identified in liver and in organs where oxidative metabolism of ethanol is minimal or absent, but which are commonly damaged by ethanol abuse: brain, pancreas, myocardium, and in cells cultured in the presence of ethanol. FAEE are formed by a synthase and an acyl-CoA:ethanol acyltransferase activity present in microsomes and cytosol of these organs. FAEE synthase activity is also present in white blood cells. After ethanol ingestion, FAEE are found in LDLs. Serum FAEE concentrations, assayed by GCMS, correlate with ethanol concentration. The half-life of plasma FAEE is ˜1 min; they undergo hydrolysis in plasma and uptake by organs. FAEE bind to myocardial mitochondria in vitro and in vivo. The mitochondria hydrolyze FAEE to fatty acids, which are uncouplers of oxidative phosphorylation. This may account for the impaired mitochondrial function and inefficient energy production associated with the toxic effects of ethanol on the heart. Also, the accumulation of FAEE in embryos of rats given ethanol has been linked to the fetal-alcohol syndrome.
Amethystic agents could be used to treat alcoholic coma. Ethanol concentrations are typically in the 50 to 70 mM range. This condition is life threatening because it can mask alcoholic hypoglycemia leading to brain damage and possibly death. In addition, anesthesia of the respiratory center by ethanol depresses respiration and coughing, leading to respiratory acidosis and pulmonary infection. Sometimes, respiratory depression leads to respiratory arrest. Also, general alcoholic anesthesia induces hypothermia which itself can be lethal. Patients in alcoholic coma brought to the Emergency Room could be infused with amethystic agents until they regain some consciousness and show no depression of respiration. Similarly, if safe oral amethystic agents were available, their ingestion between alcoholic drinks, or sometimes before driving an automobile, could dramatically decrease the rate of accidents or violence while under the influence.
Ethanol oxidation in liver is limited by the capacity of the respiratory chain to oxidize reducing equivalents derived from the conversion of ethanol to acetate. The administration of pyruvate will accelerate ethanol oxidation by exporting the reducing equivalents in the form of lactate. This export will shift the burden of disposing of reducing equivalents from the liver (2% of body weight) to the bulk of peripheral tissues. Lactate is well used by peripheral tissues, particularly by muscle and kidney. In these tissues, lactate oxidation to CO 2 will probably result in an underutilization of fatty acids, glucose and glycogen. The notion of Cori cycle, in which lactate derived from glycolysis in erythrocytes is recycled to glucose in the liver, does not exclude oxidation of a large fraction of this lactate in peripheral tissues.
Pyruvic acid is a strong, unstable ketoacid which cannot be administered orally or parenterally. Sodium pyruvate is stable in dry form and could be dissolved as an isotonic solution just before use. However, the sodium and water loads would kill the patient. The effects of the sodium load is compounded by the difference between the volumes of distribution of sodium (20% of body wt) and of ethanol (67% of body wt). Consider a numerical example: suppose we want to decrease the ethanol concentration by 20 mM in a 75 kg patient. The ethanol pool must decrease by 20×75×0.67=1,000 mmol. Since the oxidation of 1 mol ethanol generates 2 NADH, we need to supply 2×1,000=2,000 mmol of sodium pyruvate as 2,000/150=13.3 liters of isotonic solution (150 mM). Such volume cannot be administered safely. In addition, the 2,000 meq of sodium supplied is similar to the patient's original sodium pool: 140×75×0.2=2,100 meq. Therefore, sodium pyruvate cannot be used.
However, esters of pyruvate are stable and pH neutral. Esters of glycerol and/or dihydroxyacetone are preferred forms of amethystic agents for this invention. The ester will be hydrolyzed to pyruvic acid by non-specific esterases present in plasma, tissues and the gastrointestinal tract. Pyruvic acid will be neutralized by the body's buffers. Then, pyruvate will be reduced in the liver to lactate which will be oxidized to CO 2 in peripheral tissues. Overall, the strong pyruvic acid will be replaced by a weak acid which is eliminated by the lungs. From an acid-base point of view, this is similar to the oxidation to CO 2 of neutral compounds such as glucose and triacylglycerols. These oxidations pass through strong acids: pyruvic, lactic, acetoacetic and R-β-hydroxybutyric which are converted to weak and volatile CO 2 . Thus, as long as the rate of pyruvate ester infusion matches the capacity of peripheral tissues to oxidize lactate, the concentration of the latter could be kept at a safe level (<10 mM), without major acid-base disturbance. The transient increase in the anion gap would not be greater than what occurs after strenuous muscular exercise.
DPAG and PADA
A second set of the inventive compounds are dipyruvyl-acetyl-glycerol (DPAG) and pyruvyl-acetyl-dihydroxyacetone (PADA). As with PNACE, these compounds are metabolizable substrates which counteract the effects of reperfusion injury. Glycerol is a physiological substrate which is well tolerated in large amounts and although DHA is not known to exist as such in body fluids, it is quickly phosphorylated by liver glycerol kinase to dihydroxyacetone phosphate (DHAP) which is a glycolytic intermediate. Similarly DPAG and PADA can be infused in vivo to deliver a therapeutic concentration of pyruvate without lactic acidosis and sodium overload. However, because DPAG and PADA can be administered in very high doses, they are also agents for accelerating ethanol oxidation in the liver, via transfer of reducing equivalents to peripheral tissues in the form of lactate.
Glycerol is a physiological substrate. It is released by adipose tissue lipolysis and is taken up by the liver, which is the major site of glycerol kinase activity (some glycerol kinase is also present in kidney). Glycerol kinase generates glycerol-phosphate which has 3 fates: glucose, glycerides/phospholipids, and lactate. DHA is converted to physiological dihydroxyacetone-phosphate (DHAP) by glycerol kinase. Then, DHAP has the same fates as glycerol. DHA is the oxidized counterpart of glycerol.
The rate of administration of pyruvate esters should be adjusted to keep lactate concentration below 10 mM. Such lactate concentrations, in the 5 to 10 mM range, favor the competition for oxidation with other fuels such as fatty acids and glucose. One can favor lactate oxidation by infusing a small amount of dichloroacetate (DCA, final concentration 1 mM), an activator of pyruvate dehydrogenase (PDH). This drug is used for the treatment of various types of lactic acidosis, in particular those resulting from congenitally low activities of PDH in peripheral tissues.
Because of the particular benefits of the thiol in PNACE, a dual strategy to prevent and/or treat reperfusion injury is considered advantageous. Moreover, to safely deliver large amounts of pyruvate without sodium or nitrogen load, esters of pyruvate with either glycerol or dihydroxyacetone, i.e. or DPAG can be used. PNACE is not a means to supply large amounts of pyruvate, since pharmacologically NAC concentrations of below 0.1 mM are often desirable, while effective pyruvate concentrations are 1-2 mM. Thus, pyruvate-glycerol or pyruvate-DHA ester is infused in large amounts together with smaller amounts of PNACE.
Acceleration of ethanol oxidation
Rat livers were infused with ethanol and the components of the esters of glycerol-and-DHA pyruvate to represent the conditions that will occur after ester hydrolysis. Livers from 24 h-fasted rats were perfused with non-recirculating buffer containing 4 mM glucose and 2 mM ethanol (20 times the Km of ADH for ethanol, to insure zero order kinetics). After 10 min baseline, the influent perfusate was enriched with various equimolar concentrations of the components of the esters, ie DHA+Na-pyruvate, or glycerol+Na-pyruvate (up to 2.2 mM). These conditions simulated infusion and hydrolysis of glycerol- or DHA-monopyruvate. The uptakes of ethanol, pyruvate, DHA and glycerol, as well as the productions of lactate and glucose were measured.
Addition of the components of the pyruvate esters increased ethanol uptake up to 5 fold (FIGS. 3 and 4). As expected, the uptake of ethanol was greater in the presence of DHA than in the presence of glycerol. This clearly shows that DHA contributes to the trapping of reducing equivalents derived from ethanol oxidation. In perfusions with glycerol+pyruvate, correlation between pyruvate uptake and lactate output was linear with a slope of 0.7 (FIG. 5, solid circles). Thus, 70% of the pyruvate taken up was converted to lactate. In perfusions with DHA+pyruvate (FIG. 5, open circles), the correlation had also a slope of 0.7 up to a pyruvate uptake of 13 μmol/min.g dry wt (corresponding to influent DHA and pyruvate concentrations of 0.7 mM). At higher DHA and pyruvate concentrations, the slope increased to 1.45. However, at the highest DHA and pyruvate concentration used, the ratio (lactate release)/(pyruvate uptake) was 0.96. The fraction of pyruvate uptake not accounted for was presumably converted to glucose and CO 2 . FIG. 6 shows that the uptake of glycerol and DHA increased with their concentration in the perfusate. As long as the (lactate production)/(pyruvate uptake) ratio was less than 1.0, there was no net conversion of glycerol or DHA to lactate. This occurred only at high DHA concentration. Thus, most of the glycerol and DHA were converted to glucose, glycerides, CO 2 or to a combination of these species. FIG. 7 shows the relationship between ethanol uptake and lactate production. Lactate yield was lower when pyruvate was infused with DHA rather than glycerol.
Before the infusion of the components of the pyruvate esters, the effluent lactate!/ pyruvate! ratio could not be measured with precision, but must have been very high given the presence of ethanol. As the concentrations of the ester components increased from 0.4 to 2.2 mM, the lactate!/ pyruvate! ratio went down from about 12 to about 2. Thus, essentially all reducing equivalents generated from ethanol were exported as lactate. The oxidized status of the liver NADH/NAD + system may have allowed oxidation of part of the substrates, including acetate derived from ethanol.
In summary, these experiments confirmed that ethanol oxidation is stimulated by the components of DHA-pyruvate and glycerol-pyruvate. DHA is preferred as it acts not only as an esterifying group for pyruvate but also as a trap for reducing equivalents in its own right.
Therapeutic pyruvate concentration in vivo with DPAG
After preparing pure DPAG, experiments were performed to test whether it could be used to impose a therapeutic concentration of 1 mM pyruvate in arterial blood. Overnight-fasted rats, anesthetized with halothane, were infused in the jugular vein with DPAG at 90 μmol.min -1 .kg -1 for 90 min. This rate corresponds to about 120% of the rats' caloric requirement. Five blood samples (70 μl) were taken from the carotid artery between 60 and 90 min. The arterial concentrations of pyruvate, lactate, and glycerol were clamped at 1.0, 2.5, and 0.8 mM, respectively. Corresponding portal vein concentrations at 90 min were 0.6, 2.5, and 1.0 mM, respectively. FIGS. 8 and 9 show blood concentrations of metabolites in rats infused with DPAG (panel A) and in control rats infused with saline (panel B). Control rats show normal arterial concentrations of pyruvate (0.05 mM) and lactate (0.3 to 0.6 mM; normal values for lactate are up to 1.5 mM). In rats infused with DPAG, the arterial concentrations of pyruvate and lactate were clamped at 1.0, and 2.5 mM, respectively. Corresponding portal vein concentrations at 90 min were 0.6 and 2.5 mM, respectively. Arterial glucose remained at 5-6 mM. Final samples of aortic blood showed normal acid-base and electrolyte parameters. Thus, DPAG can be safely used to set up the 1 mM target concentration of pyruvate expected to be beneficial for the treatment of reperfusion injury. Similar data were obtained when PADA was infused to rats. This was achieved without sodium overload and/or acid-base perturbations. Second, the lack of major increases in glucose and lactate concentrations shows that administration of DPAG at 120% of the caloric requirement spares endogenous energy sources, probably including proteins. Third, during peripheral administration of DPAG at 90 μmol.min -1 .kg -1 , portal pyruvate concentration was about 2/3 that which yielded a 3 to 6-fold increase in ethanol uptake by perfused rat livers. A portal pyruvate concentration of 1 mM could be achieved (i) by increasing the peripheral infusion of DPAG to 120 μmol.min -1 .kg -1 , or (ii) by administering DPAG enterally to better target portal vein concentrations.
DPAG can thus be safely used to set up the 1 mM target concentration of arterial pyruvate expected to be beneficial for the treatment of ethanol overdose and reperfusion injury. This was achieved without sodium overload and/or acid-base perturbations. Also, the lack of major increases in glucose and lactate concentrations shows that administration of DPAG at 120% of the caloric requirement spares endogenous energy sources, probably including proteins.
The effect of DPAG on the rate of ethanol uptake by perfused rat livers was also tested. Livers were perfused with non-recirculating buffer containing 4 mM glucose, 2 mM ethanol and variable concentrations of DPAG (0 to 1.5 mM). FIG. 10 shows that the uptake of ethanol by the liver increases 2.5 fold when DPAG concentration is raised from zero to 0.5 mM. Note that 0.5 mM DPAG corresponds to 1 mM pyruvate after hydrolysis. Thus, to accelerate ethanol oxidation in vivo, the rate of DPAG administration should be adjusted to achieve a 1 mM concentration of free pyruvate in the portal vein. When DPAG was infused to live rats at 90 μmol.min -1 .kg -1 , the portal vein concentration of pyruvate was 0.6 mM. A portal pyruvate concentration of 1 mM could be achieved in vivo (i) by increasing the peripheral infusion of DPAG to 120 μmol.min -1 .kg -1 , or (ii) by administering DPAG enterally to better target portal vein concentrations.
Accordingly, DPAG and PADA are effective in the treatment of alcoholic coma to prevent complications such as brain damage, hypothermia, respiratory depression, and pulmonary infection and in the oral intake of the esters in conjunction with ingestions of alcoholic beverages, to accelerate ethanol oxidation and restore the capacity to drive a vehicle or operate machinery.
Synthesis of DPAG
DPAG was prepared by esterification of 1-acetyl-glycerol (1-monoacetin) with pyruvyl chloride. To a 250 ml three-neck flask fitted with a thermometer, a mechanical stirrer, a 25 ml dropping funnel, and flushed with dry nitrogen, one adds 5.0 g of anhydrous monoacetin (dried for 2 days under vacuum), 8.0 ml of anhydrous pyridine, and 100 ml of anhydrous benzene. The flask is cooled below 10° C. with an ice+salt slurry. Freshly distilled pyruvyl chloride (6.0 ml, 1 equivalent) is added dropwise over 15 min, while maintaining the temperature below 10° C. Then, the reaction mixture (showing a white precipitate of pyridinium chloride) is stirred for 1 hr at room temperature. The reaction mixture is filtered, to remove the pyridinium salt, and concentrated at 30° C. on a rotavapor under high vacuum. The crude yellow product is dissolved in 50 ml of chloroforn, washed once with 10 ml of HCl 1N, and stirred with 4 g of Amberlyst-15 for 4 hr. The solvent is evaporated on a rotavapor under high vacuum at 30 ° C. maximum. The yield of DPAG (light yellow oil) is 9.6 g (94%).
The formula of DPAG was verified by (i) NMR -1 H and 13 C, (ii) infrared spectra, (iii) enzymatic assay of the components of DPAG after hydrolysis, and (iv) HPLC before and after hydrolysis.
NMR 1 H (200 MHz Varian), solvent CDCl 3 , reference TMS (δ in ppm): 5.30 (m, 1H, CH); 4.50-4.00 (m, 4H, CH 2 O); 2.40 (s, 6H, CH 3 COCO); 2.00 (s, 3H, CH 3 CO)
NMR 1 H in agreement with the formula and the theoretical NMR spectra software ACD/LABS DEMO. NMR 13 C (200 MHz Varian), solvent CDCl 3 , reference TMS (δ in ppm): 188.9, 188.7 (2C, carbonyls); 170.2 (1C, acetyl); 157.8, 157.9 (2C, pyruvyl); 68.9 (1C, CH); 61.5, 59.4 (2C, CH 2 O); 24.6 (2C,CH 3 ); 18.4 (1C, CH 3 ) in agreement with the formula and the theoretical NM spectra software ACD/LABS DEMO. IR (cm -1 , CCl 4 ): 3537 (OH bonds from hydrated C═O), 2984; 1756, 1751, 1740, 1736, 1729 (C═O); 1383, 1231.
The NMR and IR spectra show that two molecules of water are fixed on carbonyl groups to form stable hydrated keto esters.
Incubation of DPAG with pig liver esterase liberates the components of the ester which were determined by enzymatic assays, thus confirming the formula of DPAG.
Synthesis of PDAG
PDAG was prepared in 81% yield by reacting diacetyl-glycerol with pyruvyl chloride, using the above procedure.
The formula of PDAG was verified by (i) NMR 1 H and 13 C, (ii) infrared spectra, (iii) enzymatic assay of the components of DPAG after hydrolysis, and (iv) HPLC before and after hydrolysis.
NMR 1 H (200 MHz Varian), solvent: CDCl, reference TMS (δ in ppm): 5.28 (m, 1H, CH); 4.38-4.14 (m, 4H, CH 2 O); 2.41 (s, 3H, CH 3 COCO); 2.01 (s 6H, CH 3 CO). NMR 1 H in agreement with the formula. NMR 13 C (200 MHz Varian), solvent: CDCl 3 , reference TMS (δ in ppm): 190.9 (1C, carbonyl); 170.4 (2C, acetyl); 159.8 (1C, pyruvyl); 71.5 (1C, CH acetyl); 68.6 (1C, CH pyruvyl); 61.9, 61.8 (2C, CH 2 O); 24.7 (1C, CH 3 pyruvyl); 20.6 (2C, CH 3 acetyl) in agreement with the formula. IR (cm -1 , CCl 4 ): 3593 (OH bond, from hydrated C═O), 2973, 1762 (C═O bond), 1752 (C═O bond), 1744(C═O bond), 1736 (C═O bond), 1374, 1242.
The NMR and IR spectra show that on a small fraction of the molecules, one molecule of water is fixed on a carbonyl group to form a stable hydrated keto ester.
Synthesis of PADA
PADA was prepared in 95% yield by esterification of dihydroxyacetone monoacetyl with pyruvyl chloride, as above.
TLC on silica (developed with chloroform/methanol/hexane 12/1/1 and revealed with iodine) showed one spot corresponding to PADA (Rf 0.45-0.50), and no dihydroxyacetone, dihydroxyacetone monoacetate, or dihydroxyacetone diacetate.
The formula of PADA was verified by (i) NMR 1 H and 13 C, (ii) infrared spectra, (iii) enzymatic assay of the components of PADA after hydrolysis, and (iv) HPLC before and after hydrolysis.
NMR 1 H (200 MHz Varian), solvent CDCl 3 , reference TMS (δ in ppm): PADA (keto form): 4.94 (s, 2H, CH 2 OCOCO); 4.74 (CH 2 OCO); 2.49 (s, 3H, CH 3 COCO), 2.08(s, 3H, CH 3 CO). NMR 13 C (200 MHz Varian), solvent CDCl 3 , reference TMS (δ in ppm): PADA (keto form): 198.0 (1C, keto of DHA); 192.9 (1C, keto of pyruvyl); 170.1 (1C, acetyl); 159.1 (1C, pyruvyl); 67.3, 66.3 (2C, CH 2 O); 26.7 (1C, CH 3 , pyruvyl); 20.3 (1C, CH 3 acetyl). Spectra in agreement with the formula. Enzymatic assay of pyruvate after hydrolysis was in agreement with the formula
Thus it is apparent that there has been provided, in accordance with the invention, a novel pyruvate compound and a method of treating ischemia that fully satisfies the objects, aims and advantages set forth above. While the invention has been described in conjunction with specific embodiments thereof, it is evident that many alternatives, modifications, and variations will be apparent to those skilled in the art in light of the foregoing description. Accordingly, it is intended to raise all such alternatives, modifications and variations as fall within the spirit and broad scope of the appended claims. | The invention comprises a novel pyruvate compound for the treatment or prevention of reperfusion injury following ischemia, diabetic effects, cholesterol levels, injured organs, ethanol intoxication or as a foodstuff. The novel pyruvate compound is particularly a pyruvate thiolester, a glycerol-pyruvate ester or a dihydoxyacetone-pyruvate ester. | 2 |
BACKGROUND OF THE INVENTION
1. Field of the Invention
This invention relates to nutritional supplements for livestock. More specifically, the invention relates to a combination of Macrocystis algae, yeast, calcite, and other minerals, and methods of supplementing animal feed to promote growth and productivity.
2. Related Art
Throughout history, people tending livestock have sought to provide a nutritious feed that provides good growth, health, and productivity of the animal. With ruminants such as cows, certain nutritional supplements are added to a feed blend to promote milk production, calving, and so on. Those raising horses try to optimize size and health by selecting a wholesome blend of food such as hay and oats and supplements. Poultry farmers use a feed blend that is intended to maximize the number, quality, and size of eggs, or to maximize growth.
U.S. Pat. No. 5,085,874 relates to a feed product comprising whey, dry yeast, and fat together with proteins, starch, and other components. U.S. Pat. No. 5,000,964 describes feedstuffs with low levels of yeast together with a carrier and other components. U.S. Pat. No. 5,211,980 discloses a lipid pellet having an algin component such as sodium alginate and other nutritive elements.
The prior art does not include a combination of natural components including Macrocystis algae, yeast, and calcite that is adjusted to the needs of a particular type of livestock, and provides excellent growth and performance.
SUMMARY OF THE INVENTION
A nutritional supplement according to the invention is prepared from algae, yeast, and a mineral component. The supplement acts as a metabolic corrector and improves the health and growth of dairy and beef cattle, horses, and chickens, and improves milk and egg production. Minerals and vitamins may be added to the supplement where desired to counteract metabolic deficiencies in the animal.
According to the invention, a nutritional supplement for animals contains Macrocystis algae meal, dry yeast, and a mineral component. Preferably, the algae is dried and crushed to a meal, the yeast is Cepa Sc in microcapsules, and the mineral component is powdered calcite from sea shells. In preferred formulations the Macrocystis algae comprises about 25-75% by weight, the yeast comprises about 10-50% by weight, and the powdered calcite comprises about 10-30% by weight. In an especially preferred formulation, the Macrocystis algae comprises about 50% by weight, the yeast comprises about 30% by weight, and the powdered calcite comprises about 20% by weight.
The invention also comprises a method of improving the health of an animal comprising combining crushed calcite with Macrocystis algae meal and microcapsulated yeast to provide a nutritional supplement, and feeding the supplement to the animal. The method may also comprise (a) measuring metabolite levels in a stable tissue of the animal; (b) identifying metabolites whose levels are lower than desired; (c) adding the identified metabolites to crushed calcite; (d) combining the calcite with Macrocystis algae meal and microcrystalline yeast to provide a nutritional supplement; and (e) feeding the supplement to the animal. The method preferably involves providing the supplement in an amount of about 0.1 g to 1.0 g per kg body weight.
The metabolic corrector has other beneficial applications. It can prevent and treat viral infections in animals, particularly poultry, when a therapeutically effective dose of a combination of the metabolic corrector is administered orally. It can also promote physical and mental health in humans.
BRIEF DESCRIPTION OF THE DRAWINGS
The accompanying drawing figures are provided to facilitate understanding the invention.
FIG. 1 illustrates milk production records for dairy cattle fed with the metabolic corrector as compared to controls.
FIG. 2 illustrates milk fat content for dairy cattle fed with the metabolic corrector compared to controls.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
In describing preferred embodiments of the present invention, specific terminology is employed for the sake of clarity. However, the invention is not intended to be limited to the specific terminology so selected, and it is to be understood that each specific element includes all technical equivalents which operate in a similar manner to accomplish a similar purpose.
In its preferred form, the metabolic corrector is prepared from three basic ingredients. Other minerals and supplements may be added according to the specific needs of particular animals. The metabolic corrector is preferably made up as follows:
1) edible marine algae genus Macrocystis, crushed into a meal form--about 25-75% by weight, preferably about 50%;
2) yeast culture, preferably a live yeast such as Cepa Sc 47 in microcapsules--about 10-50% by weight, preferably about 30%; and
3) calcite, preferably from pulverized sea shells, as an excipient--about 10-30% by weight, preferably about 20%.
A preferred dosage is about 0.1 to about 1 gram per kg live weight of the animal in question, most preferably about 0.25 grams per kg. Other amounts, lower or higher, may be desirable depending on the animals' particular needs.
In dry form, the metabolic corrector typically comprises about 85% dry matter and about 15% water. These proportions may vary depending on climate and storage conditions. It is typically fed dry, but may be added to warm water for consumption, in which case it forms a viscous, gelatinous preparation.
Mineral elements may be added to the calcite excipient as indicated in each case depending on the nutritional requirements of the animal. The calcite component generally contains substantial amounts of calcium, sodium, phosphorous, potassium, magnesium, and sulfur. Other minerals in the excipient may include cobalt, silver, boron, bromine, chromium, copper, iron, iodine, mangasese, molybdenum, nickel, strontium, vanadium, and zinc. Typically, slow growing animal tissue such as poultry feathers, hair, hoof, or blood are sampled and analyzed by an assay for mineral content. The quantities of these elements are determined in each particular case by an analysis of blood, hair or feather samples. The qualitative and quantitative mineral content of the sampled tissues are compared to a standard source, such as the U.S. Department of Agriculture Minimum Daily Requirement Tables for the particular species, referred to as Cantidad Suficiente Para 100, or quantity sufficient to reach 100% of the desired level, by weight or volume. If the level of a particular mineral in a test animal is below the recommended level, then an extra quantity of that mineral is added to the calcite excipient as a supplement to meet the animal's minimum requirements. The supplemental minerals are easily obtainable anywhere in the world without restriction.
Using the metabolic corrector in proportions adequate to each animal species in general optimizes the utilization of the available nutrients and coenzymes in the feed ration vital to normal metabolism. The metabolic corrector apparently acts as a nutritional "buffer," and allows for the adequate absorption of the metabolites in the feed ration, i.e. , glucids, proteins (amino acids), vitamins, and macro and microelements.
The metabolic corrector of the invention has been found to have many beneficial effects with various animals. These benefits are described here in terms of numerical observations made during the course of recent experimental procedures.
Each animal species has different nutritional requirements that are carefully monitored in the process of formulating the metabolic corrector. Minerals are added as necessary to the calcite excipient, to supplement the mineral content of animals whose levels fall below the currently updated USDA Minimum Daily Requirement Tables.
Dairy Cattle
Ruminants more often than not present digestive disturbances as a result of man's constant interference in their feed formulation. This exposes the milking cow to nutritional factors and conditions which tend to limit optimum milk production and often is the cause for toxic and semi-toxic levels of certain elements. When incorporated into the feed ration, the interaction of the metabolic corrector in the ruminal medium modifies the metabolism of the intestinal flora. This interaction increases the pH of the digestive medium to 6.9, a level which is considered to be normal.
Cows under pasture feeding conditions tend to have a ruminal pH in the order of 5.9/6.2. This acid ruminal medium causes an alteration of the ruminal flora and therefore an alteration of the metabolic process with special emphasis on proteins. Approximately 80% of the protein in the ration is broken down in the rumen, and through the cellulitic (or cellular) action of the flora, is converted into bacterial protein. The undigested protein is transformed into ammonia (hepatotoxic ammonia).
The high level of ammonia overtaxes the liver as ammonia is absorbed through the walls of the rumen in transit to the circulatory system. These conditions result in a loss of protein in the diet and predominant toxic state in the animal. The optimum ammonia concentration content for an acceptable protein metabolism is in the order of 5 grams per every 100 milliliters of ruminal fluid. Cows in the above examples have been found to have levels of 30 to 40 grams per 100 milliliters of ruminal fluid.
When the metabolic corrector is added to the daily ration, in an amount of about 100 grams per day for a cow of 1,100 lbs. live weight, after a period of time, the pH becomes adjusted to a desirable level. Thereafter, bacteria and protozoans will function adequately in the breakdown of proteins thereby reducing the levels of ammonia and thus increasing bacterial protein.
From the actions detailed above we can make the following observations:
There is an increase in milk production of between 10 to 12%.
Milk fat content increases between 18 to 20%.
Protein content increases from 3 to 5%.
There is a high concentration of vitamins and minerals in the milk.
As a result of less toxemia there is a higher degree of assimilation of nutrients of high biological value, better intestinal passage which results in a more vigorous feeding. Herds have been observed to have a higher proportion of cows in heat as well as an increased response to successful artificial insemination.
Beef Cattle
Certain observations have been made in beef cattle as a result of using this metabolic corrector, the most important being as follows:
More rapid weight gain and overall growth is observed in young weaning animals, when fed the metabolic corrector together with their milk.
Cattle in pens have been observed to increase their weight between 30 to 40% more than the untreated norm.
Use of the metabolic corrector provides a higher carcass weight of the animals at slaughter.
Horses
Sporting horses often live in an artificial environment (a box), with little or no light and are fed a ration which is brought by man. Generally horses under this medium live under a permanent state of stress. This medium often results in lack of appetite (anorexia); disturbances in the color and odor of the fecal matter; and exposure to colic. It is commonly observed, when exposed to a competitive environment, that these animals show a general lack of appetite and stress.
The use of the metabolic corrector in the ration results in a stabilization of the digestive process as shown in the normalization of the fecal matter, an increase in appetite shown under voluntary feeding and better performance under a training environment.
In addition, it has been observed that horses have improved their red blood cell formation (erythropoiesis), red blood cell count as well as an increase in the relative red blood cells in the plasma (hematocritical), which can be traced to the action of the metabolic corrector on the overall process of blood formation (hematopoiesis).
High Performance Laying Hens
This is the sector where the metabolic corrector has been proven and tested the most, showing the following results:
An increase of 5 to 6% in quantity of eggs laid
A distinct difference in the distribution of egg size:
15 to 35% more large size eggs
20% less medium size eggs
15 to 18% less small size eggs
2 to 4.5% increase in the weight of the egg
Mortality due to viruses affecting the laying hen population was reduced by 50% on those hens being fed the corrector. It is felt that the utilization of the metabolic corrector stimulates immune mechanisms, thus increasing the animal's natural defenses.
Uniformity of weights (according to figures recommended by the developers of the genetic string of laying hens) is obtained more readily. The uniformity of weight on those treated hens was observed to be 20% higher than for the untreated hens.
The analytical content of Component A has been determined. It is made up of 15% water and 85% dry matter. The following details are based on the dry matter only:
______________________________________A) Metabolites: (approximately)Proteins 34.80%Fats 4.35%Mineral Ashes 17.40%Carbohydrates 39.10%Fiber Content 4.35%B) Vitamins: (in Milligrams per Kg. Dry Matter)Vitamin A (Beta Carotene) 40Vitamin D (Calciferol) 5Vitamin E (Tocopherol) 70Vitamin B1 (Thiamine) 15Vitamin B12 (Riboflavin) 6Vitamin C (Ascorbic Acid) 200Panthotenic Acid 12Niacin 50Folic Acid 0.5Biotin 0.5C) Amino Acids: (in Milligrams/100 gr. Protein)Alanine 6Arginine 5.5Aspartic Acid 8.5Cisteine 0.5Glutamic Acid 12Glicine 3Histidine 8.8Triptophane 0.9Tyrosine 1.8Isoleucine 2.5Leucine 3.5Lysine 5.0Methionine 1.0Pheniialanine 2.5Preline 2.7Serene 3.5Treonine 2.8Valline 3.0Cisteine 0.5Citruline 2.0Omitine 1.5Tyrosine 0.4Treonine 0.3D) Mineral Content: (in Milligrams/Kg. Dry Matter)Calcium 7,000Sodium 11,000Phosphorus 6,000Cobalt 3.5Silver 0.5Boron 70Bromium 1Chromium 1Copper 4Iron 35Iodine 450Potassium 12,000Magnesium 1,800Manganese 26Molybdenum 0.1Nickel 10Sulfur 2,800Strontium 1Vanadium 1Zinc 35______________________________________
The amounts of these components may vary. However, it is important that the algae, yeast, and calcite components of the metabolic corrector be used in their essentially intact form. For example, a synthetic combination of the analytically determined components of Component A does not achieve the results claimed heretofore. Likewise, the use of less than all three of the ingredients of the metabolic corrector may be beneficial but does not provide the optimal results according to the invention. Preferably, the algae, yeast, and calcite must all be present together to provide the surprising effectiveness of the metabolic corrector.
The genus Macrocystis is the largest algae in the family Lessoniaceae. It includes M. pyrifera L., M. integrifolia Bory, and M. angustifolia Bory. M. pyrifera is preferred, although it is expected that other species may be employed pursuant to the invention. Algaes of related genuses include Dictyoneurum, Pelagophycus, and Nereocystis. The blades of the algae are the preferred components, although the entire plant may be used.
EXAMPLE 1
An experiment was conducted with cattle to determine whether the metabolic corrector provided a marked improvement in the general metabolism (specifically in the ruminal metabolism) of cattle through the use of human medical techniques, thereby improving the production of beef and milk. The specific objective of the experiment was to determine the correction of the digestive media through the use of diagnosed metabolic correctors in a milking herd in Argentina. The breed of cattle was Holstein Fresian cows.
METHODOLOGY
Criteria in Selecting the Test Group
The process of selection of the Test Group was based on the diagnosis of existing needs in the herd at a time where maximum milk production was required.
This period, between 0 to 90 days after calving, demands from the cow the use of all of its reserves to meet the highest nutritional requirements imperative at the time of maximum lactation.
By the same token, it is during this period that the cow must call on all its resources in order to replace tissue lost during parturition, thus preparing itself for the coming period of heat and pregnancy essential for the animal to be considered an economically productive unit.
As a first step, these were the criteria used in selecting the Test Group from the herd. No first pregnancy heifers were selected and were left for a later study of this same type. Thence two lots of ten (10) animals each were picked at random, each animal with an individual I.D. number. These two (2) groups are herein known as "Test Group" and "Control Group," respectively.
Initial Diagnosis
The diagnostic process began with the extraction of serum and blood samples from each individual animal. These samples provided a mineral content profile for each individual Group at the onset of the experience.
The minerals tested were those considered most lacking in the region. These minerals are: Calcium (Ca); Phosphorus (P); Magnesium (Mg); and Copper (Cu) as well as Total Protein and Albumin.
These profiles were analyzed taking into account the lab results and a diagnosis of the amounts lacking was effected.
Treatment
A metabolic corrector was prescribed for the test herd in view of this diagnosis and taking into consideration the lactating period previously mentioned. The same formulation was used for all the cows in the test group. This metabolic corrector was fed twice a day at a rate of 100 grams/animal/day. The amount of metabolic corrector fed (100 grams/animal/day) remained the same any time that the feed quantity was either changed or modified thus establishing a new relationship between the feed ration and the corrector.
Feed Management
This experiment began on Dec. 11th, 1992 with the analysis of each cow's milking record since Oct. 15th, 1992, in order to determine the adjustments necessary as to productions liters/day/cow as well as milk fat content. This was performed on each of the two Groups to avoid any misinterpretation of the final results.
Both Groups were handled jointly with the rest of the heard at milking time but were separated from the milking herd when they were put out to pasture. This insured that both test Groups were first to be on new pasture. This mode was used until Dec. 30th, 1992 when due to extreme drought conditions prevalent in the region since end November, required that the test Groups be handled together with the rest of the herd.
Pasture time on a daily rotating basis was set from 0800-1500 hrs--then milking; and from 1800-0400 hrs.--then milking. As of Dec. 30th, 1992 the Groups were put into pens at night where good quality hay was provided after pasturing on grass.
Good quantity and volume of forage was provided both Groups during pasture; as the drought began to set in, this was changed to low volume-good quality forage during daytime and high volume-lower quality forage during the evening time when cows were in their pens.
During the milking, the cows were fed normal well balanced commercial feed (16% protein). The ration provided each animal depended on their milk production; both the "Test Group" as well as the "Control Group" were fed 5 Kg/cow/day (11 lbs./cow/day). This daily ration was divided in two, half being fed at each milking. The "Test Group" was fed the additional 100 grams per day of the prescribed metabolic corrector.
Normal sanitary conditions were kept during the whole experience; no cases of clinical mastitis were recorded in either Group.
The grazing sequence is shown in Table 1. The feed plants found in the Argentinean pastures are as follows:
Trebol Rojo--Red Clover (trifolium pratensis)
Pasto Ovillo--Sheep Grass (dactylis glomerata)
Sorgo Forrajero--Sorgum (sorgum sacaratum)
Agropiro (agrophrum alongatum)
Melilotus--Lotus (mililotus officinalis)
Moha de Hungria (satarea italium pratensis)
Phalaris (phalaria bulbosa)
TABLE 1______________________________________Grazing (pasture) Sequence during the Experience.Daytime Grazing Nighttime GrazingDate Type Date Type______________________________________Nov. 02 to #91 R. Clovr + Nov. 2 to #90 AgropiroNov. 10, 1992 Sheep Past Nov. 8, 1992 & LotusNov. 11 to #90 R. Clovr + Nov. 9 to #90 R.Nov. 19, 1992 Sheep Past Nov. 16, 1992 Clover* Falaris.Nov. 20 to #91 R. Clovr + Nov. 17 to #89 AgropiroNov. 27, 1992 Sheep Past Nov. 29, 1992 & LotusNov. 28 to #90 R. Clovr + Nov. 30 to Bale of MohoDec. 2, 1992 Sheep Past Dec. 13, 1992 8.816 lbs./ day/cowDec. 3 to #89 R. Clovr + Dec. 14 to Bale of R.Dec. 18 1992 Sheep Past Jan. 6, 1993 Clover 8.816 lbs./day/cowDec. 19 to #91 R. Clovr +Dec. 26, 1992 Sheep PastDec. 27 to SorghumJan. 6, 1993 Feed______________________________________
Data Acquisition
The following Data Acquisition scheme was designed taking into account the specific objectives set forth at the onset:
A) Individual milk production per cow in both Test as well as Control Groups.
1 ) Initial Sampling
2) Monthly Sampling
B) Milk Fat content (Grasa Albumina) in both Test as well as Control Groups.
1 ) Initial Sampling
2) Monthly Sampling
The Initial Milk Production Sample (under A-1 ) was obtained from the Control Sheets kept by CASTELMAR, the local dairy farmer's coop.
Subsequent Monthly Samples (under A-2) were taken in the same manner for the months of November, December (1992) and January 1993.
Table "2" provides a comparison of Milk Production in the "Test Group," the "Control Group" as well as the whole of the milking herd. A graph is provided as FIG. 1.
TABLE 2__________________________________________________________________________Milk Production Records - Test Group & Control Group - comparedCow Calving No. of Lactat. MILK PRODUCTION CONTROLI.D. No.Date Calves Days Oct. 14 Nov. 16 Dec. 12 Jan. 15__________________________________________________________________________***"CONTROL GROUP"***508 9/01/92 7 43 33.4 24.0 20.6 20.0755 8/23/92 3 52 34.6 29.6 16.6 20.0862 8/09/92 2 66 25.4 25.2 14.8 19.4878 7/26/92 2 80 23.8 26.0 13.8 13.8893 9/01/92 2 43 27.4 25.8 14.6 18.6896 9/25/92 2 19 24.7 26.4 20.2 19.8979 9/23/92 3 21 28.4 19.8 16.2 18.21129 9/05/92 5 39 22.0 19.6 16.4 14.41131 8/01/92 3 74 28.4 21.2 14.2 16.41145 7/30/92 3 76 30.2 20.0 14.8 20.0Ave. Milk Production 52 27.8 23.7 16.2 18.0***"TEST GROUP"***541 9/02/92 7 35 33.8 30.0 21.0 23.2694 8/16/92 3 59 33.8 28.4 19.0 26.0738 9/15/92 3 28 33.0 27.4 17.2 21.2764 8/15/92 3 60 27.6 23.4 17.2 18.4818 9/05/92 2 39 34.6 30.0 20.4 22.2964 8/16/92 2 59 27.3 24.6 17.0 21.6989 9/25/92 2 19 26.8 27.0 20.8 20.41000 9/22/92 5 22 26.6 22.4 17.4 19.81093 7/20/92 5 86 31.6 27.4 16.4 17.81141 7/21/92 3 85 26.6 24.2 17.2 18.4Ave. Milk Production 52 29.8 26.6 18.5 21.0DIFFERENCES FOUND IN %: +7.2% +12.2% +13.6% +16.6%__________________________________________________________________________
At the onset of the Experiment the Lactation Period for the "Control Group" was 52 days and 50 days for the "Test Group". These periods have been adjusted for variances using tables provided by the S.R.A.--Sociedad Rural Argentina--which take into consideration adjustment of lactation periods of 305 days as related to age. Table "3" contains the relevant information from these tables.
TABLE 3______________________________________Lactation Periods to 305 days - Conversion Table used AGE AT AGE ATNo. OF PARTUM No. OF PARTUMLACT. (in yrs. & decimals) LACT. (in yrs. & decimals)DAYS <3 years >3 years DAYS <3 years >3 years______________________________________15 16.67 14.63 165 1.62 1.5135 9.99 8.9 175 1.54 1.4435 7.13 6.36 185 1.47 1.3845 5.54 4.96 195 1.41 1.3355 4.53 4.07 205 1.35 1.2865 3.85 3.48 215 1.3 1.2475 3.35 3.02 225 1.25 1.285 2.97 2.69 235 1.21 1.1695 2.68 2.43 245 1.17 1.14105 2.44 2.22 255 1.13 1.1115 2.25 2.05 265 1.1 1.07125 2.08 1.91 275 1.07 1.05135 1.94 1.79 285 1.05 1.03145 1.82 1.68 295 1.02 1.02155 1.72 1.59 305 1 1______________________________________
______________________________________Conversion Factors - To Equivalent Age(in months)Age at Last Age at LastPartum FACTOR Partum FACTOR______________________________________21 1.44 72 1.0124 1.35 78 130 1.31 84 132 1.26 90 133 1.21 96 136 1.15 102 142 1.1 108 1.0248 1.06 114 1.0254 1 120 1.0360 1.04______________________________________
Cows were not given their feed rations from Dec. 9 through Dec. 12, 1992. Coincidental with this lack of feed, the month of December shows a marked decline in milk production during this period. Regardless of this fact, the Milk Production Control for this month was kept as scheduled. It was felt that, in order not to affect the results of the experiment, the recordings were to be kept as initially programmed.
Table "4" provides a comparison in Milk Fat Content for the "Test Group," the "Control Group" as well as the whole of the milking herd. A graph depicting these quantities is also provided as FIG. 2.
TABLE 4__________________________________________________________________________Milk Fat Content - Test Group & Control Group - compared. (Grass/Fat) October November December January 14/92 16/92 12/92 15/92LOT Gr. % Fat Gr. % Fat Gr. % Fat Gr. % Fat__________________________________________________________________________Control Group 867 3.11 831 3.50 515 3.17 559 3.10Test Group 1009 3.39 875 3.29 622 3.38 688 3.27 +142 +44 +107 +129DIFFERENCE +16.4% +5.8% +20.8% +23.2%Total Milk Pool 595 507 500__________________________________________________________________________
Several conclusions can be drawn from this Example. First, the palatability of the metabolic corrector added to the ration was acceptable to the "Test Group." Second, judging from the results obtained from this Experiment the differences between the "Test Group" and the "Control Group" both in milk production as well as in fat content gradually increased with time. Thus, one can conclude that, in time, the metabolic corrector has a cumulative beneficial effect in the animal's rumen. Third, there was a definite residual effect on the "Test Group." Independent sources recorded this effect as far as Feb. 5th, 1993 before the rest of the herd was fed the metabolic corrector.
Finally, from the results of this Experiment one can definitely conclude that the metabolic corrector does have utility and economic potential in larger dairy herds.
EXAMPLE 2
An experiment was conducted with beef cattle to determine the effect of the metabolic corrector on weight increase. A test group consisting of 70 head of steers was divided out of a herd, of which 353 head remained as the control group. All animals were fed on a winter pasture of barley grass and rye grass, at a load of about 400 kg/hectare, or about 616 lbs/acre. The test group was fed with fresh forage plus 2.2 lbs of corn per day, and 20 grams of the metabolic corrector, as with the dairy cattle. The control animals had the same diet, but without the metabolic corrector.
The test animals were slightly lighter, on average, than the control group, but they were otherwise comparable. The average weights of the animals at the beginning of the experiment is shown in Table 5.
The experiment began Sep. 14 and ended Dec. 7, 1993, 84 days later. The final comparative analysis in Table 5 shows that the average daily increase and total increase in weight for the test group, in terms of percentage, was more than double the increases for the control group. The total increase averaged 142 lbs, or about 60% for the test animals, as compared to 93.8 lbs, or 28% for the control animals.
This experiment demonstrates that the metabolic corrector can increase the rate of weight gain for beef cattle, at least over the course of several months.
TABLE 5______________________________________Results of the Beef ExperienceGROUP TEST GROUP CONTROLDate Day Wt(Lb) Gain % Wt(Lb) Gain %______________________________________ 9/14 0 236.5 0 0 335.2 0 010/08 24 275.5 39 16.5 360.8 25.8 7.711/06 29 329.8 54.25 19.7 390 29.36 8.1312/07 31 378.5 48.7 14.77 429 38.68 9.91______________________________________
______________________________________Final Comparative Analysis Test Group Control Group______________________________________Daily Increase 1.69 Lbs. 1.117 Lbs.% Increase 0.7% 0.3%Total Increase 142 Lbs. 93.8 Lbs.% Increase 60.04% 28%______________________________________
Modifications and variations of the above-described embodiments of the present invention are possible, as appreciated by those skilled in the art in light of the above teachings. It is therefore to be understood that, within the scope of the appended claims and their equivalents, the invention may be practiced otherwise than as specifically described. | A nutritional supplement is prepared from Macrocystis algae meal, microcapsules of yeast, and powdered calcite from sea shells. The supplement improves the health and growth of dairy and beef cattle, horses, and chickens, and improves milk and egg production. Minerals and vitamins may be added to the supplement where desired to counteract metabolic deficiencies in the animal. | 0 |
BACKGROUND OF THE INVENTION
The present invention relates to a roller bearing and a method for the production thereof. In particular, the invention relates to a method for producing a bearing ring of the roller bearing and an associated roller body.
Various roller bearings are known from the prior art. For example, roller bearings are known in which a bearing ring, i.e. the outer ring and/or the inner ring, has a rim in order to absorb axial forces acting on the bearing. In methods for producing roller bearings which are known from the prior art, the respective bearing rings are produced by means of a turning method and subsequently what is referred to as a grinding undercut is provided in a still unhardened state in a corner region between the raceway of the bearing ring and the lateral rim. This grinding undercut is required to be able to subsequently grind the raceway and the rim running face.
This grinding undercut results in a sharp edge in the rim running face. This edge, in turn, in combination with unsuitable lubricants, can damage roller end faces due to the axial running on of the roller end faces. To be more precise, due to the edge it is possible for minor damage to occur to the roller bodies and their end faces. In particular when roller bodies are used with planar roller end faces, such damage to these faces by the edge is likely to occur.
SUMMARY OF THE INVENTION
The present invention is based on the object of making available a method for producing a roller bearing with which a roller bearing can be made available with a prolonged service life compared to the prior art. In addition, the intention is to increase the axial load-bearing capacity of bearings.
The present invention is also aimed at a roller bearing which achieves improved contact between the end faces of the roller bodies on the one hand and the inner wall of the rim on the other.
The aforesaid objects are achieved by means of the subject matters of the independent claims. Advantageous embodiments and developments are the subject matter of the subclaims. However, it is to be noted that the subject matters of all the subclaims do not solve all the inventive problems to the same degree.
Furthermore, it is to be noted that the subject matters of all the independent claims are based on the same problem, namely of increasing the service life of the roller bearings.
In the inventive method for producing a bearing ring for a roller bearing, wherein the bearing ring has a raceway for a roller body and at least one lateral rim for axially guiding the roller body, in one method step a notch is made in a wall of the bearing ring facing the roller body. According to the invention, the end contour of the bearing ring is produced by a hard turning process.
The rim is preferably also used for absorbing loads acting axially on the roller bearing.
An end contour of the bearing ring is understood to be a contour which only still requires fine processing for completion, the formation of the notch also being considered to be fine processing.
The bearing ring which is already hardened is processed by means of the hard turning process according to the invention. In this case, there is no need to grind the rim running face further.
A notch is understood to be a groove or recess which is preferably formed essentially in the radial direction in the bearing ring. This notch, which performs the function of a grinding undercut, is preferably located in a corner region between the rim running face and the raceway.
The present invention is also aimed at a method for producing a bearing ring for a roller bearing, wherein the bearing ring has a raceway for a roller body and at least one lateral rim for axially guiding the roller body. In this context, in one method step, a notch is made in a wall of the bearing ring facing the roller body. According to the invention, in this method the notch is produced by forming a groove with a groove body in essentially the radial direction of the roller bearing.
The groove body can be used to form a groove in the radial direction of the roller bearing if the lateral rim or its inner wall no longer needs to be subsequently ground. Forming a groove with the groove body in the radial direction of the roller bearing prevents an edge being produced in the rim running face and damaging the individual roller bodies during later operation.
In a further method step the raceway is preferably ground. The notch in the corner region between the raceway and the lateral rim is used to carry out this grinding. The notch prevents damage to the rim face by the grinding tool. In a further preferred embodiment, the rim is hard turned with a rim angle of aperture of more than 90°. After this hard turning, in a last work step the notch or the grinding undercut is formed in order to permit the raceway to be ground.
The rim angle of aperture is preferably between 90° and 92°. The contact geometry between the roller body and the rim running face is improved by this rim angle of aperture.
To be more precise, the run up between the roller bodies and the rim is improved by this rim angle of aperture which is slightly above 90°, for example 90.5°, therefore increasing the service life of the roller bearing.
The present invention is, as stated above, also aimed at a method for producing a roller body for a roller bearing, wherein the roller body has at least one end face which is curved in sections. As stated above, planar end faces, which are subject to high stresses when in contact with the rim, are used in the prior art. Provision of a curved end face ensures that instead of a contact face, known from the prior art, between the roller and the rim, only essentially a point of contact occurs between the roller body and the rim. The lubrication between the roller body and the rim can also be improved.
In this way, the service life and the axial load-bearing capacity of the bearing according to the invention can also be increased. The end face of the roller body is understood to be that face which is turned towards the rim. According to the invention, the roller body is also produced by means of a hard turning process. Using a hard turning process facilitates the production of a curved end face according to the invention.
The end face is preferably curved at least in sections, in particular is curved logarithmically or in a toroidal shape.
A toroidal body is understood to be a body which is produced as a result of the turning of a circle about an axis lying in the circular plane outside the circle. With respect to the roller body, a toroidal end face is understood to mean that the end face produces a line in a projection in a radial direction of the roller body, and this line is curved in particular in a circular or ellipsoidal shape in its end regions. In this context, the geometric centre point of this circular or ellipsoidal curvature does not lie on the geometric axis of symmetry of the roller body but rather is spaced apart from it.
This curved, in particular toroidal, surface has proven particularly suitable in complex trials for reducing damage produced by the running up of the end face against the rim running face.
The present invention is also aimed at a roller bearing with a raceway for roller bodies which has at least one lateral rim for axially guiding the roller bodies, wherein the rim has a rim running face which is turned toward the roller body, and a notch is provided in a corner region between the raceway and the rim running face. According to the invention, the notch and the wall of the rim merge one into the other essentially without an edge.
In other words, a tangent to an end point or end region of the notch extends essentially parallel to the rim running face. In contrast, this parallelism does not occur in the prior art, in other words there is an edge. This edgeless transition means that the roller body and its end face cannot be damaged by the edge when they run up.
In a further preferred embodiment, the notch has at least in sections a circular-segment-shaped profile, wherein this circular-segment-shaped profile has a radius of curvature which is between 0.5 mm and 2 mm, and preferably between 1 mm and 1.5 mm. This notch serves, as stated above, as a grinding undercut which permits the raceway to be ground. Since the profile between the notch and the wall is edgeless, it is not possible to grind the rim running face.
The notch preferably has an end region facing the raceway of the bearing ring, and in this end region said notch extends at an angle with respect to the raceway which is between 20° and 40°, preferably between 25° and 37°, and particularly preferably between 30° and 34°.
The present invention is also aimed at a roller body, wherein according to the invention the roller body has at least one and preferably two end faces which are curved at least in sections, in particular are curved logarithmically or in a toroidal shape.
This end face which is curved in particular in a toroidal shape ensures that the contact between the rim and the roller body is not punctiform or linear but rather over a surface. This contact over a surface permits improved lubrication of the roller bearing.
The roller body preferably has, in at least one end region, a lateral face which is curved in the axial direction of the roller body. In this way it is also possible to improve the running up of the roller body with respect to the raceway. The lateral face is preferably curved convexly.
The present invention is also aimed at a roller bearing having a bearing ring of the type described above, and at a roller bearing having at least one roller body of the type described above.
BRIEF DESCRIPTION OF THE DRAWINGS
Further advantages and embodiments of the present invention emerge from the appended drawings, in which:
FIG. 1 shows a partial illustration of a hearing ring according to the prior art;
FIG. 2 shows a partial illustration of a bearing ring according to the invention;
FIG. 3 shows an illustration of the production method for a bearing ring according to the invention;
FIG. 4 shows a partial illustration of a hearing ring according to the prior art with a roller body;
FIG. 5 shows an enlarged partial illustration of a bearing ring according to the invention with a roller body;
FIG. 6 shows an illustration of a hearing ring with a roller body;
FIG. 7 shows an enlarged illustration of a bearing ring with a roller body according to the invention;
FIG. 8 shows an enlarged illustration of a roller bearing according to the invention;
FIG. 9 shows a detailed illustration of a bearing ring with a roller body;
FIG. 10 shows a roller body; and
FIG. 11 shows a further embodiment of a roller body according to the invention.
DETAILED DESCRIPTION OF THE INVENTION
FIG. 1 shows a detail illustration of a bearing ring 2 manufactured using a method known from the prior art. The reference symbol 4 here refers to a central region of the bearing ring and the reference symbol 6 refers to a lateral rim. The rim running face 6 a of the rim is facing a roller body (not shown).
As mentioned at the beginning, in the method known from the prior art the notch 7 or the grinding undercut is formed in the material before the hardening process. The material is hardened only after this. In this method it is also still necessary to grind the rim running face 6 a . Therefore, the notch 7 , as shown in FIG. 1 , is formed in an oblique direction with respect to the rim 6 and the central region 4 . As a result, an edge 30 is produced in the rim running face 6 a in the prior art. This sharp edge 30 can have unfavorable effects on the start of axial movement, in particular of planar roller end faces.
FIG. 2 shows a bearing ring manufactured according to the inventive method. In this context, the material of the bearing ring is firstly hardened and the end contour, in particular the end contour of the rim running face 6 a , is then produced by hard turning. In this case, subsequent grinding of the rim running face 6 a is not necessary, but only the raceway 4 a of the central region 4 needs to be ground. In this case, the tool for producing the grinding undercut is introduced into the notch 7 in the radial direction P 1 of the bearing ring 2 , avoiding an edge 30 being formed as in FIG. 1 .
To be more precise, the hard turning of the rim face 6 a is finished by complying with a necessary mean value for the rim aperture in the region between 90° and 92°, for example 90.5°, and in a final work step the grinding undercut is formed in order to permit the raceway 4 a to be ground.
The reference symbol 9 refers to an end region of the notch 7 facing the raceway 4 a . This end region runs in an axial direction at an angle of approximately 32° with respect to the raceway.
FIG. 3 illustrates the production of the notch 7 or of the grinding undercut in a method according to the invention. For this purpose, a tool 13 is pushed into the bearing ring 2 in an essentially radial direction (arrow P 1 ) after the hard turning of the bearing ring. The reference symbol 12 characterizes a groove body of the tool 13 . The reference symbol d denotes the grinding dimension, which is in the vicinity of 0.5 mm. The angle β between the edge 12 b of the groove body 12 and the raceway 4 a is in a range between 30° and 35°.
The rim running face 6 a does not extend at an angle of precisely 90° with respect to the raceway 4 a but rather at a slightly larger angle. The angle γ between the edge 12 a of the groove body 12 and the rim running face 6 a is between 3° and 4°.
FIG. 4 is an illustration of a detail of a bearing ring according to the prior art with a roller body 5 which runs up against it. In this context, the rim angle is not illustrated to scale here. It is apparent that the roller body 5 can make contact with the edge 30 of the grinding undercut at the notch 7 . Since the roller body moves with respect to this sharp edge 30 , the small damage which was mentioned at the beginning can occur to the roller body and therefore accelerated wear thereof may occur. The reference symbol 11 refers to the end face of the roller body.
FIG. 5 shows a bearing ring with a roller body in which the bearing ring has been manufactured with the methods according to the invention. It is apparent that in this case there is no edge 30 and therefore the roller body 5 is treated in a correspondingly gentler way.
FIG. 6 shows an illustration of a bearing ring 2 with a roller body 5 . This concerns a hard-turned bearing ring also. The end face 11 of the roller body 5 has a central region 11 a which can be implemented in essentially any desired way since it does not run up against the rim 6 . It is also conceivable for the central region 11 a of the end face 11 to have a trough or the like. As a result of the special configuration of the edge regions 11 b of the end face 11 it is possible to ensure that only a single contact point occurs between the rim and the end face, which is explained in more detail below.
The contact point between the end face 11 of the roller body and the rim face 6 a is denoted by 8 . The radius of curvature of the corner region 15 of the roller body is between 0.5 mm and 4 mm, preferably between 1 mm and 2 mm, and particularly preferably in the vicinity of 1.5 mm.
The reference sign L refers to the rotational axis or axis of symmetry of the roller body 5 . The reference symbol 14 denotes a toroidal center point line on which, given a toroidal curvature of the roller body, the groove point 16 or center point for the toroidal curvature lies. The line 14 , and therefore the groove point for the toroidal curvature, is preferably located at the level of the end face 17 of the rim 6 .
FIG. 7 shows an enlarged illustration of the arrangement shown in FIG. 6 . Here, the reference symbol TV denotes the distance by which the toroidal center point line 14 is displaced with respect to the axis L of symmetry. This means that in the embodiment shown in FIG. 7 the curvature in the edge region 11 b of the end face 11 of the roller body lies on a circle whose circle center point (which is equal to the groove point 16 ) lies in turn on the line 14 . Here, the edge region 11 b is a single curved region continuously curving in an axial direction away from the central region 11 a.
The reference symbol LW max refers to the maximum length of the roller body, and the reference symbol LW refers to the length of the roller body in the vicinity of the contact point 8 between the roller body and the rim running face 6 a . This contact point 8 is at the distance BA from the raceway 4 a of the bearing ring 2 . In the embodiment shown here, the contact point 8 is approximately at the same distance, in the radial direction, from the end face 17 of the rim 6 and from the raceway 4 a of the bearing ring.
FIG. 9 shows an enlarged illustration of a bearing ring according to the prior art with a roller body 5 . Here, the illustration has been enlarged to different degrees in the x and y directions.
It is apparent that when the roller body according to the prior art is used, an edge 32 of the roller body runs up against the rim face 6 a of the rim. This running up of the edge also leads over time to an adverse effect on the rim face. The notch 7 is not shown in FIG. 9 .
As mentioned at the beginning, the present invention is based on the object of increasing the service life of such roller bearings, and in particular of improving the running up of the roller bodies against the rims of the bearing ring or rings.
FIG. 8 shows a bearing ring 2 which is used with a roller body 5 which is improved according to the invention. Here too, the illustration has been enlarged to different degrees in the x and y directions.
This roller body does not have any sharp corner edges but rather has rounded edge regions 11 b which are embodied in this case in the manner of a torus. The grinding undercut or the notch is not shown in the illustration in FIG. 8 . It is apparent that as a result of the toroidal embodiment of the edge region 11 b , sharp-edged contact does not occur between the rim running face 6 a and the end face 11 or the end face region 11 b of the end face 11 . As a result, during operation it is possible to avoid wear on the end face and therefore the roller body as well as the rim running face 6 a . Ideally, in the embodiment shown in FIG. 8 essentially one contact face 8 is provided between the roller body and the rim running face 6 a.
FIG. 10 shows a roller body. It is apparent that the end face 11 in this embodiment is of essentially spherical shape. The center point of this sphere or spherical segment face is located on the rotational axis L or axis L of symmetry of the roller body. The radius R of the spherical configuration is between 300 mm and 800 mm, preferably between 500 mm and 700 mm, and particularly preferably between 570 mm and 620 mm. However, the selection of this radius also depends on other geometries of the roller body, for example its length Lw and its diameter Dw. In the corner region 15 , the roller body preferably has, as mentioned above, a radius between 1 mm and 2 mm. The use of a roller body 5 in the embodiment shown in FIG. 10 requires a rim angle of aperture in the vicinity of 92°. The reference sign DW characterizes the diameter of the roller body.
FIG. 11 shows a further embodiment of the roller body according to the invention. In contrast to the embodiment shown in FIG. 10 , the end face in the embodiment shown in FIG. 11 is of toroidal design This means that here the center point of the circular faces 11 b does not lie on the axis L of symmetry but rather is offset with respect to it by a predefined distance a. This is illustrated by the circular line K for the lower edge region 11 b . In the embodiment shown in FIG. 11 , the radius of the curvatures is in the regions 11 b over the length L of the roller body.
In the point of intersection S between the toroidal center point line 14 and the end face 11 , the central region 11 a and the edge region 11 b merge with one another without an edge.
The central region 11 a of the end face can also have a planar profile in this embodiment. From FIG. 11 it is apparent that the geometric location of all the center points of the respective circular lines K is located itself on a circular ring around the axis of symmetry with the radius a.
The method according to the invention or the bearing components according to the invention result in a larger effective rim height and therefore an improved running up of the roller end face onto the rim face since the sharp edge of the notch 7 is dispensed with, and therefore this region can also be used for the running up of the roller body. Since the dressing, for example the grinding, takes place after the heat treatment, the cooling does not result in any distortion due to heat treatment of the individual bearing components.
Subsequent to this process, the lateral line and/or the roller end face or the roller end faces can preferably be honed.
Since production can occur in a clamped region between tips, it is also possible to avoid run-out errors with the respectively produced or processed roller bodies, which may arise due to remounting.
All the features disclosed in the application documents are claimed as essential to the invention insofar as they are novel compared to the prior art, either individually or in combination.
LIST OF REFERENCE SYMBOLS
2 Bearing ring
4 Central region of the bearing ring
4 a Raceway
5 Roller body
6 Lateral rim of the bearing ring
6 a Rim running face
7 Notch
8 Contact point between end face 11 and rim running face 6 a
9 End region of the notch
11 End face of the roller body
11 a Central region of the end face 11
11 b Edge region of the end face 11
12 Cutting body
12 a , 12 b Edge of the cutting body 12
13 Tool
14 Toroidal center point line
15 Corner region of the roller body 5
16 Groove point
17 End face of the rim
19 Circular line
30 Edge of the notch (prior art)
32 Edge of the roller body (prior art)
P 1 Radial direction
L Axis of symmetry of the roller body
TV Toroidal connection
LW Length of the roller body
LW max Maximum length of the roller body
DW Diameter of the roller body
BA Distance between contact point and raceway
TR Toroidal radius
R Radius
S Point of intersection between toroidal center point line 14 and end face 11
a Distance between toroidal center point line 14 and axis L of symmetry. | A method for producing a bearing ring for a roiling bearing, the bearing ring comprising a raceway for a rolling member as well as at least one lateral rim for axially guiding the rolling member. In one step of said method, a notch is introduced into a running surface of the bearing ring which faces the rolling member. The final contour of the bearing ring is created by means of a hard turning process. | 8 |
STATEMENT OF GOVERNMENT INTEREST
The invention described and claimed herein may be manufactured and used by or for the Government of the United States of America for governmental purposes without the payment of royalties thereon or therefor.
BACKGROUND OF THE INVENTION
The present invention relates to a mobile cofferdam and to a method for building elongated structures in a body of water using the mobile cofferdam. In accordance with the invention, construction of the elongated structure takes place in a dewatered or still water enclosure. The method of construction is most applicable to a long, repetitive structure such as a concrete sill or massive wall to be built within the body of water.
BRIEF DESCRIPTION OF THE PRIOR ART
Typically, major construction within the river, lake, or other body of water is performed inside a cofferdam of cellular sheet pile cells and granular fill. These conventional cofferdams are costly and time consuming to build. Their construction is subject to delay and cost increases arising from unknown foundation conditions at the bottom of the body of water, from unpredictable weather and water conditions, and from difficult dewatering problems.
In addition, these structures require movement and placing of massive quantities of material to fill the sheet pile cells and stabilizing berms where required. Following construction, this same material must then be degraded and spoiled in order to remove the cofferdam, which disturbs the surrounding environment.
SUMMARY OF THE INVENTION
Accordingly, it is a primary object of the present invention to provide a mobile cofferdam structure for use in building elongated sills or walls on the bottom of a body of water. The cofferdam includes a rectangular shell having spaced inner and outer walls which define a first chamber between the walls and a second chamber within the interior of the shell. A bottom wall is connected with the bottom edges of the inner and outer walls for closing the bottom of the first chamber. A pump is connected with the shell for controlling the water depth within the first and second chambers. Thus, when water is removed from the second chamber, a construction area for building a segment of the sill or other elongated structure is defined. When water is removed from the first chamber, the shell is floated for repositioning with respect to a previously built segment of the sill. The shell also includes an anchoring mechanism for anchoring the shell to the previously built portion of the sill.
According to a more specific embodiment of the invention, one side wall of the shell is contoured to match the contour of the sill under construction. In this fashion, the cofferdam can be positioned in sealing relation along the contoured side wall with the previously constructed segment of the sill, and anchored thereto, with construction of the next segment of the sill taking place within the second chamber of the shell.
A further object of the invention is to provide a method for building elongated structures in a body of water. In accordance with the method, the mobile cofferdam is positioned at the bottom of a body of water. Using the pump, water is removed from the interior of the cofferdam to define a dry working environment. Next, a segment of the sill is constructed within the cofferdam on the bottom of the body of water. Following construction, the interior of the cofferdam is flooded with water and the first chamber of the cofferdam is evacuated so that the cofferdam floats above the bottom of the body of water. Next, the cofferdam is repositioned laterally along the length of the previously constructed segment of the sill. The first chamber is again flooded whereby the cofferdam will sink into relation with the previously constructed sill segment. The cofferdam is then anchored to the segment and the next segment of the cofferdam is built.
The cofferdam is anchored in place either by using a hydraulic gripping mechanism which secures the cofferdam to the previously constructed sill segment, or by using the underwater Tremie placement method wherein concrete is delivered through a tube, the end of which is kept submerged in the fluid concrete mass. The weight of the concrete and/or foundation piles or temporary piles can be used to anchor the cofferdam in abutting relation with the existing sill segment.
BRIEF DESCRIPTION OF THE FIGURES
Other objects and advantages of the subject invention will become apparent from a study of the following specification when viewed in light of the accompanying drawing in which:
FIG. 1 is a perspective view of the mobile cofferdam for constructing an elongated sill within a body of water;
FIG. 2 is a front plan view of the cofferdam according to the invention;
FIG. 3 is a top plan view of the mobile cofferdam of FIG. 2; and
FIG. 4 is a partial sectional perspective view of cofferdam positioned for construction of a subsequent segment of the sill.
DETAILED DESCRIPTION
As shown in FIG. 1, the mobile cofferdam 2 is used for the construction of an elongated structure such as a sill 4 beneath a body of water. More particularly, the bottom of the body of water is first dredged out along the dredge lines 6 to define a channel in which the sill 4 is to be constructed. As will be developed in greater detail below, the sill is constructed in segments within the interior of the mobile cofferdam. After a segment of the sill has been completed, the cofferdam is repositioned laterally to define a working area for construction of one or more subsequent segments of the sill. The cofferdam is repositioned as many times as necessary so that the entire elongated sill can be constructed.
As shown in FIGS. 1-3, the mobile cofferdam comprises a rectangular shell 8 having spaced inner and outer walls 10, 12 which define a first chamber 14 between the walls and a second chamber 16 within the interior of the shell. For structural rigidity, the shell is preferably formed by space truss structures (not shown) with skin plates on the inner and outer surfaces thereof to define the inner and outer walls 10, 12, respectively. A bottom wall 18 (FIG. 2) is connected with the bottom edges of the inner and outer walls for closing the bottom of the first chamber. If desired, a top wall 20 may be provided for connection with the top edges of the inner and outer walls for closing the top of the first chamber as well. However, no walls are provided at the top and bottom of the second chamber 16, whereby the second chamber is open at both its top and bottom ends for placement over an existing portion of the sill, as will be set forth in greater detail below.
One side wall of the cofferdam shell is contoured along a line 22 to match the contour of the sill segment previously constructed. Preferably, this wall of the cofferdam shell is provided with a rubber gasket or seal to mate with the previously constructed sill segment, thereby preventing any leakage therethrough.
A pumping mechanism 24 is connected with the cofferdam shell for adding or removing water from the first and second chambers, respectively. Accordingly, when water is removed from the second chamber within the interior of the shell, a construction area for construction of a segment of the elongated sill is defined as shown in FIGS. 1 and 4. When water is removed from the first chamber between the inner and outer walls, the shell is floated for repositioning with respect to a previously built segment of the sill.
With the second chamber 16 filled with water and the first chamber 14 evacuated from water, the shell has a tendency to float in the body of water in which the sill is being constructed. By pumping water into the first chamber 14 between the inner and outer shell walls, the shell gradually sinks within the body of water. By using cables or other guide mechanisms, the mobile cofferdam shell can be accurately positioned on the bottom surface of the body of water. Next, the second chamber 16 can be evacuated using the pumping mechanism 4 to define a construction area free from water within which a sill segment can be constructed.
In order to anchor the mobile cofferdam shell in place, gripping jacks 26 are provided within the interior of the shell. Upon actuation of a hydraulic mechanism 28, the gripping jacks are extended into a pressing engagement with the previously constructed sill segment, thereby fixing the shell to the previously constructed sill segment, with the contoured rubber seal mating against the contour of the pre-existing sill segment.
Movable forms 30 are also connected with the cofferdam shell. These forms are positioned upon operation of the hydraulic mechanism 28 to define the outer surface of the sill segment to be constructed within the interior of the dewatered cofferdam shell. Next, steel is positioned within the forms following which concrete is poured within the form to construct the next sill segment. Once the concrete has cured, the forms 30 are removed from the newly constructed sill segment upon operation of the hydraulic mechanism 28, and the second chamber 16 is flooded by the pumping mechanism 24. Next, the grippers 26 are disengaged from the previously constructed sill segment, and water is removed from the first chamber 14 by the pumping mechanism 24 to re-float the mobile cofferdam. Using the guide mechanism (not shown) the mobile cofferdam is laterally shifted down along the length of the just completed sill segment and repositioned for construction of a further segment of the sill.
The mobile cofferdam shell may be quite large. For example, the shell may have an interior chamber 16 approximately 200 feet in length and of any suitable width, such as, for example, 50 feet so that long segments of a sill may be constructed at any particular time. This is necessary for the construction of complex sill structures including complex machinery for positioning movable wickets relative to the completed concrete sill.
The method for building elongated structures such as sills or walls within a body of water in accordance with the invention will now be described.
A special fixed cell is constructed to serve as a truss support for the mobile cofferdam for the first segment of sill to be constructed or to define a temporary end fill section which is necessary for the trailing end of the mobile cofferdam. This trailing end is the end of the sill which has a configuration conforming with the perimeter of the sill under construction. The initial section of the sill or wall is constructed inside the dewatered cofferdam. Once this is done, subsequent segments of the sill are constructed as set forth below. The mobile cofferdam is slightly floated by pumping water out of the first chamber 14 following which the cofferdam is advanced along a previously constructed sill segment. Next, the first chamber is flooded to sink the mobile cofferdam to the bottom of the body of water. The mobile cofferdam is then anchored to the previously constructed segment of the sill. This anchoring step may be performed in one of two ways. Preferably, the mobile cofferdam shell includes gripping members which are extendable from the shell for gripping grooves or other recesses provided in the sill. Alternatively, in accordance with the "Tremie" method, a thick (approximately 5 feet) layer of concrete is poured within the second chamber 16 of the shell. This concrete is poured by placing concrete through a tube or hose until the thick layer of concrete is formed on the floor of the body of water. If the interior wall of the cofferdam shell is tapered, it can be broken loose from the concrete base formed in the second chamber. However, this base prevents lateral displacement of the shell whereby the shell can only be moved vertically by floating the shell relative to the base, and then repositioning it laterally beyond the base.
With the mobile cofferdam anchored in place, the pumping mechanism is activated to dewater the interior of the shell. The pumping mechanism can comprise a dewatering system which is installed around the perimeter of the mobile cofferdam. Once the second chamber of the cofferdam shell has been dewatered, forms can be positioned to define the contour of the sill under construction. Concrete is poured into the forms to physically construct the sill segment. After the concrete has been set, the forms are withdrawn and the interior of the cofferdam is flooded with water. Next, the cofferdam is repositioned along the length of the segment of the sill by pumping water out of the first chamber and floating the sill for lateral displacement.
Of course, in the event that the sill under construction is designed to have a hollow structure, as shown for example in FIG. 4, it is necessary to place bulkheads at the end of a completed sill segment prior to flooding the interior of the cofferdam shell. Once the shell has been repositioned to construct the next segment, the interior of the cofferdam shell is evacuated or dewatered, and the bulkheads are removed before the next sill segment is constructed.
In this manner, the sill is constructed in segments as the mobile cofferdam is displaced laterally along the length of previously constructed sill segments as shown in FIGS. 1 and 4. For example, approximately 100 feet of sill or wall are constructed during each cycle. At the leading end, approximately 50 feet of the structure will be built, from driving piles if required, through placing the concrete. Immediately behind that, on the previously built 50 foot section, the remaining structural appurtenances 30, wickets 32, and operating equipment 34 for the the sill are installed. The mobile cofferdam is anchored to the section during the dewatered period to resist the unbalanced hydrostatic forces between the leading and trailing ends thereof.
Using the inventive method and mobile cofferdam structure, substantial cost savings are provided. Moreover, in rivers a smaller restriction of flow area than is necessary with conventional cofferdam construction allows concurrent construction of structures and shortens the overall project construction time. Environmental disturbance is also minimized when compared with conventional cofferdam construction, which requires moving more material to fill cells and construct berms, and results in greater noise and activity associated with placing and pulling the cells. The placement of concrete for construction of the sill is accomplished with a mechanized repetitive slip-form technology for increased efficiency. Finally, since a small area is dewatered at any given time, the total pumping requirements are less than with conventional technology.
While in accordance with the provisions of the patent statute the preferred forms and embodiments of the invention have been illustrated and described, it will be apparent to those of ordinary skill in the art that various changes and modifications may be made without deviating from the inventive concepts set forth above. | A mobile cofferdam for use in the construction of elongated structures win a body of water is characterized by a water-tight rectangular shell which is guided and supported off the previously constructed segment of the sill or wall structure being built. The mobile cofferdam shell is floated into place, sunk, dewatered, and used as a cofferdam during construction of the sill. The mobile cofferdam is guided and supported off the previous placed concrete sill or wall and proceeds in a horizontal slip-form fashion. The walls of the mobile cofferdam are designed as spaced truss structures with skin plate on the inner, outer, top and bottom surface thereof to define a chamber which can be filled or evacuated with water to float the shell structure. The trailing end of the shell conforms to the sill or wall under construction and includes seals along the contact area for mating with the previously constructed sill portion. | 4 |
CROSS-REFERENCE TO RELATED APPLICATION
[0001] The present application is a continuation of International Application No. PCT/KR2012/008091 filed on Oct. 5, 2012, which claims priority to Korean Application No. 10-2011-0101421 filed on Oct. 5, 2011, which applications are incorporated herein by reference.
TECHNICAL FIELD
[0002] The present invention relates to a lighting method of an LED lighting apparatus, and more particularly to a lighting method of an LED lighting apparatus which can provide an optimized illumination to a road or an interior of a building while minimizing consumption of energy.
BACKGROUND ART
[0003] In recent years, development of lighting apparatuses using an LED as a light source has been accelerated, considering that existing lighting apparatuses consume much electric power and should be frequently replaced due to their short life spans.
[0004] The lighting apparatuses currently using an LED as a light source employ lenses having various shapes or for various purposes to satisfy light distribution patterns ruled according to the use purposes of the lighting apparatuses.
[0005] For example, efforts are made to divide a board to which LEDs are mounted to divide the shape of a housing to which boards are coupled into a plurality of parts in order to adjust installation angles of the boards. However, when the board surface of the housing is divided into a plurality of parts, the thickness of the lighting apparatus becomes relatively larger and the weight of the lighting apparatus increases.
[0006] Further, although a method of using lenses to satisfy the ruled light distribution patterns is also widely used, a relatively high power LED should be used to satisfy a ruled intensity of illumination due to loss of light when the lens is used.
[0007] In particular, street lamps are installed at sides of a road to be spaced apart from each other and an area of the road which should be illuminated by one street lamp is wide.
[0008] A general street lamp has a light distribution pattern having an elliptical shape a length of which is longer along a lengthwise direction of a road, that is, toward an adjacent street lamp thereof. Further, when a street lamp is installed, an intensity of illumination on a road surface of a road is ruled.
[0009] The street lamp having the elliptical light distribution pattern has a difference between the intensity of illumination on a road surface adjacent to the street lamp and the intensity of illumination on a road surface farthest away from the street lamp. In this way, when the intensity of illumination at an edge of the light distribution pattern farthest from the street lamp agrees with the ruled intensity of illumination of a road surface, the intensity of illumination at a central portion of the light distribution pattern adjacent to the street lamp is higher than the rule.
[0010] In this way, the high intensity of illumination may cause a glare in the eyes of a driver, and may influence the driver of a vehicle travelling on another adjacent road. Further, power consumption may increase unnecessarily as the intensity of illumination is higher than the rule.
[0011] Furthermore, when a factory lamp illuminates a space having a wide interior area, the factory lamp disposed at an edge of the interior of the factory, for example, the factory lamp disposed near a wall of the factory unnecessarily illuminates the wall, decreasing efficiency.
[0012] Korean Patent Application Publication No. 10-2011-0008522 (published on Jan. 27, 2011) discloses an invention in which a light distribution pattern for illuminating a road is divided such that an LED lighting apparatus illuminates corners of the divided areas.
[0013] However, since the LED chips emit light at a light emission angle of 120 degrees and the difference between the intensities of illumination according to the distances from the LED chips to the locations of the light distribution chips is not considered, the difference between the intensities of illumination according to the locations of the light distribution pattern cannot be overcome.
[0014] Hereinafter, the problems of the illumination apparatuses according to the related art will be described in detail with reference to the accompanying drawings.
[0015] FIG. 1 is a view for explaining a problem of a lighting method of a lighting apparatus according to the related art.
[0016] Referring to FIG. 1 , street lamps SL 1 and SL 2 are generally installed to be spaced apart from each other by a separation of 50 m, and a maximum diameter of a light distribution pattern of one street lamp is theoretically 50 m.
[0017] However, the light distribution patterns LP 1 and LP 2 of the street lamps SL 1 and SL 2 are elliptical, and some portions of the adjacent light distribution patterns LP 1 and LP 2 overlap each other to prevent a blind spot area of the light pattern. Accordingly, a maximum diameter of the light distribution patterns SL 1 and SL 2 exceeds 50 m.
[0018] Although the intensity of illumination on a road surface may agree with a ruled intensity of illumination, the intensity of illumination of an area B 1 adjacent to the light source of the street lamp SL 1 exceeds the ruled value to be a higher intensity of illumination.
[0019] As described above, the road surface whose intensity of illumination exceeds the rule may cause a glare in the eyes of the driver, and the other areas B 2 and B 3 may be mistaken as dark places and power consumption may become excessive.
[0020] FIG. 2 is a view for explaining a problem of Korean Patent Application Publication No. 10-2011-0008522.
[0021] Referring to FIG. 2 , Korean Patent Application Publication No. 10-2011-0008522 (hereinafter, ‘Prior Art 1’) is configured such that LEDs are disposed in a matrix form in a lamp mechanism of a street lamp and an illumination area also is divided into a matrix form so that each of the LEDs illuminates one section.
[0022] Then, an LED LEDA located at the most distant location from a lamp pole illuminates the divided road surfaces A 1 , A 2 , A 3 , and A 4 at the farthest distance from the lamp pole.
[0023] However, since the road surface A 4 which is more distant from the lamp pole is more distant from the road A 1 , their intensities of illumination are different even though the LEDs arranged in a row of the LED LEDA illuminate the road surfaces A 1 to A 4 .
[0024] In addition, since road surfaces B 1 , B 2 , B 3 , and B 4 adjacent to the pole of the street lamp are illuminated by an LED LEDB, the road surfaces B 1 , B 2 , B 3 , and B 4 have the same problem as that of the road surfaces A 1 to A 4 . Further, since all the divided road surfaces A 1 to A 4 and B 1 to B 4 are divided into the same area, the intensities of illumination of the road surfaces B 1 to B 4 adjacent to the pole of the street lamp and the most distant road surfaces A 1 to A 4 also are different.
SUMMARY
[0025] The present invention has been made in an effort to solve the above-mentioned problems, and it is an object of the present invention to provide a lighting method of an LED lighting apparatus in which set surfaces of a divided road surface are illuminated by an LED or a group of LEDs, and the areas of the set surfaces of the divided road surfaces are different such that the set surfaces of the divided road surfaces may be illuminated by adjusting illumination angles and radiation angles of the LEDs.
[0026] In accordance with an aspect of the present invention, there is provided a lighting method of an LED lighting apparatus wherein a plurality of LEDs illuminate divided patterns of light distributed patterns, and the divided light distribution patterns are illuminated by adjusting illumination angles and radiation angles of light radiated from the LEDs.
[0027] In the lighting method of an LED lighting apparatus according to the present invention, an LED illuminating an edge of a light distribution pattern distant from a street lamp has a relatively large illumination angle and a small radiation angle and a central portion of a light distribution pattern near the street lamp and an edge of a light distribution pattern adjacent to the street lamp have relatively small illumination angles and large radiation angles, so that the areas or interior areas of the roads illuminated by the LEDs are different, making it possible to uniformly secure the intensities of illumination of the entire light distribution patterns.
[0028] In this way, power consumption can be further reduced by securing the uniformity in the intensities of illumination of the light distribution patterns. Further, a road surface or an interior surface which is determined to be relatively dark by the driver or the user in spite that the intensities of illumination agree with a rule can be prevented from being generated due to the partial differences of illumination, which helps safe driving.
[0029] Further, a glare due to a higher intensity of illumination in some areas can be prevented from being generated. In addition, the driver of another vehicle traveling on another adjacent road can be prevented from being influenced, by concentrating light only on an illuminated area, which helps safe driving.
[0030] In addition, illumination efficiency can be increased by concentrating light on a surface which requires illumination other than a wall in a factory located near the wall of an interior of a building.
BRIEF DESCRIPTION OF THE DRAWINGS
[0031] FIG. 1 is a view for explaining a problem of a lighting method of a lighting apparatus according to the related art.
[0032] FIG. 2 is a view for explaining a problem of prior art 1.
[0033] FIG. 3 is a view for explaining a lighting method according to an exemplary embodiment of the present invention.
[0034] FIGS. 4 and 5 are views for explaining a relationship between radiation angles and illumination angles according to distances in the present invention.
DETAILED DESCRIPTION
[0035] Hereinafter, an LED light apparatus and a lighting method using the same according to the present invention will be described in detail with reference to the accompanying drawings.
[0036] FIG. 3 is a view for explaining a lighting method according to an exemplary embodiment of the present invention.
[0037] Referring to FIG. 3 , in the lighting method according to the embodiment of the present invention, a light distribution pattern (LPxy) of a street lamp 1 , in which a plurality of LEDs L 11 to L 15 , L 21 to L 25 , L 31 to L 35 , L 41 to L 45 , and L 51 to L 55 (hereinafter, the entire LEDs are denoted by Lxy) are arranged in a matrix form, is divided into a plurality of parts corresponding to the number of the plurality of LEDs Lxy such that the LEDs Lxy light the divided light distribution patterns LPxy, and areas of the divided light distribution patterns which are more distant from the street lamp 1 are smaller than areas of the light distribution patterns which are closer to the street lamp 1 .
[0038] Although the street lamp arranged in a matrix form is exemplified in the embodiment of the present invention, the present invention is not limited thereto and may be applied to any lighting lamp having an arbitrary arrangement.
[0039] Although installation surfaces of the LEDs Lxy of the street lamp 1 are shown to be excessively large as compared with the light distribution patterns LPxy for convenience' sake, the street lamp 1 is very small as compared with the light distribution patterns LPxy, and thus light of the LEDs Lxy may be illuminated from one point to the divided areas of the light distribution patterns LPxy.
[0040] The light distribution patterns LPxy are divided into 25 areas corresponding to the number of the LEDs Lxy, and as shown in the drawing, the light distribution patterns LPxy are formed on the left and right sides and the front side of the street lamp 1 . For convenience' sake, the front side of the street lamp 1 corresponds to the x direction and the lateral side thereof corresponds to the y direction, and the divided light distribution patterns LPxy (x and y are integers of 1 to 5) are shown.
[0041] The areas of the two divided light distribution patterns LP 51 and LP 55 which are most distant from the street lamp 1 are narrowest and the areas of the divided light distribution pattern LP 13 adjacent to the street lamp 1 are largest, and the areas of the light distribution patterns become gradually smaller as they go from the largest light distribution pattern LP 13 toward the left and right sides and the front side.
[0042] Since the two LEDs L 51 and L 55 lighting the divided light distribution patterns LP 51 and LP 55 having the smallest areas should light the most distant areas, their intensities of light are low due to a difference between distances of light for reaching a road surface as compared with the other areas of the light distribution patterns LPxy in the same condition.
[0043] Then, since the areas of the light distribution patterns LP 51 and LP 55 are smallest, the radiation angles of the LEDs L 51 and L 55 may be smaller than the radiation angles of the other LEDs Lxy (x and y are 1 to 5 except that xy is 51 or 55), and when the radiation angles are small, a higher intensity of illumination may be obtained as compared with the wide radiation angles in a condition in which the same distance is illuminated.
[0044] Thus, by adjusting the radiation angles of the divided light distribution patterns LP 51 and LP 55 located at the farthest distance, the light distribution patterns LP 51 and LP 55 may provide the same intensity of illumination as that of the other areas of the light distribution patterns LPxy.
[0045] FIG. 4 is a view for explaining a relationship between radiation angles and illumination angles according to distances in the present invention.
[0046] Referring to FIG. 4 , the LEDs L 13 , L 23 , L 33 , L 43 , and L 53 in the central row of the LEDs Lxy illuminate the divided light distribution patterns LP 13 , LP 23 , LP 33 , LP 43 , and LP 53 .
[0047] Then, the illumination angle GA 5 of the LED L 53 illuminating the light distribution pattern LP 53 which is farthest in the corresponding row from a pole of the street lamp 1 is larger than those of the LEDs L 13 to L 43 , and the radiation angle RA 5 which is a light emission angle of the LED L 53 is the smallest of the radiation angles RA 1 to RA 5 of the LEDs L 13 to L 43 .
[0048] Thus, among the intensities of illumination at locations spaced from the LEDs L 13 to L 53 by the same distance, the intensity of illumination of the LED L 53 is highest and the intensity of illumination of the LED L 13 emitting light at the largest radiation angle RA 1 is lowest.
[0049] The differences in the intensities of illumination become uniform on the road surface having the light distribution patterns LP 13 , LP 23 , LP 33 , LP 43 , and LP 53 due to the differences in the distances from the street lamp 1 to the divided light distribution patterns LP 13 , LP 23 , LP 33 , LP 43 , and LP 53 .
[0050] Due to this, the areas of the light distribution patterns LP 13 , LP 23 , LP 33 , LP 43 , and LP 53 become smaller as they go far away from the street lamp 1 . This can be regarded as the differences in the areas according to the radiation angles RA 1 to RA 5 of the LEDs L 13 , L 23 , L 33 , L 43 , and L 53 .
[0051] As described above, FIG. 4 is an exploded view of a surface on which the LEDs L 13 , L 23 , L 33 , L 43 , and L 53 are disposed and is substantially the same as the case in which the LEDs L 13 , L 23 , L 33 , L 43 , and L 53 illuminate light to the light distribution patterns LP 13 , LP 23 , LP 33 , LP 43 , and LP 53 .
[0052] In FIG. 5 , the height H of the lighting lamp 1 and the total width of the light distribution patterns LP 13 , LP 23 , LP 33 , LP 43 , and LP 53 are fixed values in design of the road, and the illumination angles GA 1 to GA 5 and the radiation angles RA 1 to RA 5 of the LEDs L 13 , L 23 , L 33 , L 43 , and L 53 are adjusted to obtain a uniform intensity of illumination while the light of the LEDs L 13 , L 23 , L 33 , L 43 , and L 53 do not overlap each other.
[0053] In this way, according to the present invention, the entire light distribution patterns can be illuminated at a uniform intensity of illumination by adjusting the radiation angles of the LEDs as well as the illumination angles of the LEDs.
[0054] It will be appreciated by those skilled in the art to which the present invention pertains that the present invention is not limited to the embodiments and can be variously adjusted and modified without departing from the technical spirit of the present invention.
[0055] Since the present invention can secure a uniform intensity of illumination of the entire light distribution patterns by making the areas of a road illuminated by a plurality of LEDs in an LED lighting apparatus, it is industrially applicable. | The present invention relates to a lighting method for an LED lighting apparatus, in which e.g. an LED for illuminating an edge of a light distribution pattern far away from a street lamp has a relatively larger illumination angle and a smaller radiation angle, and an LED for illuminating the center of a light distribution pattern near the street lamp and an edge of a light distribution pattern adjacent to the street lamp has a relatively smaller illumination angle and a smaller radiation angle. Thus, each LED illuminates different areas of the road, thereby ensuring the uniformity of illumination of an overall light distribution pattern. | 5 |
BACKGROUND OF THE INVENTION
The present invention relates to mass spectrometers.
Orthogonal acceleration time of flight (“oaTOF”) mass spectrometers sample ions travelling in a first (axial) direction by periodically applying a sudden accelerating electric field in a second direction which is orthogonal to the first direction. Because the ions have a non-zero component of velocity in the first direction, the result of the pulsed electric field is that ions are accelerated into the field free or drift region of the time of flight mass analyser at an angle θ with respect to the second direction. If the ions have an initial energy eVa in the first direction, and they are accelerated to an energy eVo in the orthogonal direction, then tan(θ)=(Va/Vo) 0.5 . For a continuous stream of ions travelling in the axial direction, all with the same energy eVa, the ion sampling duty cycle of the orthogonal acceleration time of flight mass analyser is typically of the order of 20-30% for ions having the maximum mass to charge ratio. The duty cycle is less for ions with lower mass to charge ratios. For example, if it is assumed that the length of the pusher region of the time of flight mass analyser is L 1 , the length of the detector is at least L 1 (to eliminate unnecessary losses at the detector) and the distance between the pusher and the detector is L 2 , then if ions with the maximum mass to charge ratio have an mass to charge ratio mo, then the duty cycle Dcy for ions with a mass to charge ratio m is given by: Dcy=L 1 /(L 1 +L 2 ).(m/mo) 0.5 . Accordingly, if L 1 =35 mm and L 2 =120 mm, then L 1 /(L 1 +L 2 )=0.2258. Hence the maximum duty cycle is 22.6% for ions with the maximum mass to charge ratio mo, and is correspondingly less for ions with lower mass to charge ratios.
SUMMARY OF THE INVENTION
According to a first aspect of the present invention, there is provided a mass spectrometer comprising:
an ion guide wherein in use a DC potential travels along a portion of the ion guide.
As will be explained in more detail below, the ion guide with a travelling DC wave is particularly advantageous in that all the ions preferably exit the ion guide with essentially the same velocity. The ion guide can therefore be advantageously coupled to an orthogonal acceleration time of flight mass analyser which can be operated in conjunction with the ion guide so as to have an ion sampling duty cycle of nearly 100% across the whole mass range i.e. the ion sampling duty cycle is improved by a factor of approximately ×5 and furthermore is substantially independent of the mass to charge ratio of the ions. This represents a significant advance in the art.
Most if not all of the electrodes forming the ion guide are connected to an AC or RF voltage supply. The resulting AC or RF electric field acts to radially confine ions within the ion guide by creating a pseudo-potential well. According to less preferred embodiments, the AC or RF voltage supply may not necessarily output a sinusoidal waveform, and according to some embodiments a non-sinusoidal RF waveform such as a square wave may be provided. Preferably, at least 10%, 20%, 30%, 40%, 50%, 60%, 70%, 80%, 90%, or 95% of the electrodes are connected to both a DC and an AC or RF voltage supply.
According to the preferred embodiment, a repeating pattern of DC electrical potentials is superimposed along the length of the ion guide such as to form a periodic waveform. The waveform is caused to travel along the ion guide in the direction in which it is required to move the ions at constant velocity. In the presence of a gas the ion motion will be dampened by the viscous drag of the gas. The ions will therefore drift forwards with the same velocity as that of the travelling waveform and hence ions will exit from the ion guide with substantially the same velocity, irrespective of their mass.
The ion guide preferably comprises a plurality of segments. The ion guide is preferably segmented in the axial direction such that independent transient DC potentials can be applied, preferably independently, to each segment. The DC travelling wave potential is preferably superimposed on top of the AC or RF radially confining voltage and any constant or underlying DC offset voltage which may be applied to the segment. The DC potentials at which the various segments are maintained are preferably changed temporally so as to generate a travelling DC potential wave in the axial direction.
At any instant in time a moving DC voltage gradient is generated between segments so as to push or pull the ions in a certain direction. As the DC voltage gradient moves along the ion guide, so do the ions.
The DC voltage applied to each of the segments may be independently programmed to create a required waveform. The individual DC voltages on each of the segments are preferably programmed to change in synchronism such that the waveform is maintained but shifted in the direction in which it is required to move the ions.
The DC voltage applied to each segment may be programmed to change continuously or in a series of steps. The sequence of DC voltages applied to each segment may repeat at regular intervals, or at intervals that may progressively increase or decrease. The time over which the complete sequence of voltages is applied to a particular segment is the cycle time T. The inverse of the cycle time is the wave frequency f. The distance along the RF ion guide over which the waveform repeats itself is the wavelength λ. The wavelength divided by the cycle time is the velocity v of the wave. Hence, the wave velocity, v=λ/T=λf. Under correct operation the velocity of the ions will be equal to that of the travelling wave. For a given wavelength, the wave velocity may be controlled by selection of the cycle time. The preferred velocity of the travelling wave may be dependent on a number of parameters. Such parameters may include the range of ion masses to be analysed, the pressure and composition of the bath gas and the maximum collision energy where fragmentation is to be avoided. The amplitude of the travelling DC waveform may progressively increase or decrease towards the exit of the ion guide. Alternatively, the DC waveform may have a constant amplitude. In one embodiment the amplitude of the DC waveform grows to its full amplitude over the first few segments of the ion guide. This allows ions to be introduced and caught up by the travelling wave with minimal disruption to their sequence.
One application of the preferred ion guide is to convert a continuous ion beam into a synchronised pulsed beam of ions. The ability to be able to convert a continuous beam of ions into a pulsed beam of ions is particularly advantageous when using an orthogonal acceleration time of flight mass analyser since it allows the pulsing of an orthogonal acceleration time of flight mass spectrometer to be synchronised with the arrival of ions at the orthogonal acceleration region. The delay time between the time the ions exit the travelling wave ion guide and the pulsing of the orthogonal acceleration stage of the time of flight mass spectrometer depends on the distance to be travelled and the ion velocity. If all the ions have the same velocity, irrespective of their mass, then the ion sampling duty cycle will be optimised for all ions simultaneously, irrespective of their mass.
Another application of the preferred ion guide is to convert an asynchronous pulsed ion beam into a synchronous pulsed ion beam. The travelling wave ion guide may be used to collect and organise an essentially random series of ion pulses into a new series with which an orthogonal acceleration time of flight mass analyser may be synchronised. Again, if all the ions have the same velocity, irrespective of their mass, then the ion sampling duty cycle may be optimised for all ions simultaneously, irrespective of their mass.
Preferably, ions are not substantially fragmented within the ion guide so that all the ions received by the ion guide are essentially onwardly transmitted. The ion guide is therefore preferably not used as a fragmentation cell.
The ion guide may comprise a plurality of rod segments (i.e. electrodes which do not have apertures) or more preferably the ion guide may comprise an ion tunnel ion guide. An ion tunnel ion guide comprises a plurality of electrodes having apertures through which ions are transmitted in use. The electrodes may comprise ring, annular, plate or substantially closed loop electrodes. Preferably, at least 50%, 60%, 70%, 80%, 90% or 95% of the electrodes forming the ion guide have apertures which are substantially the same size or area.
The diameter of the apertures of at least 50% of the electrodes forming the ion guide is preferably selected from the group consisting of: (i) ≦20 mm; (ii) ≦19 mm; (iii) ≦18 mm; (iv) ≦17 mm; (v) ≦16 mm; (vi) ≦15 mm; (vii) ≦14 mm; (viii) ≦13 mm; (ix) ≦12 mm; (x) ≦11 mm; (xi) ≦10 mm; (xii) ≦9 mm; (xiii) ≦8 mm; (xiv) ≦7 mm; (xv) ≦6 mm; (xvi) ≦5 mm; (xvii) ≦4 mm; (xviii) ≦3 mm; (xix) ≦2 mm; and (xx) ≦1 mm.
According to a preferred embodiment, the ion guide may comprise a plurality of segments wherein each segment comprises a plurality of electrodes having apertures through which ions are transmitted and wherein all the electrodes in a segment are maintained at substantially the same DC potential and wherein adjacent electrodes in a segment are supplied with different phases of an AC or RF voltage. Such a segmented design simplifies the electronics associated with the ion guide.
The ion guide may consist of 10-20, 20-30, 30-40, 40-50, 50-60, 60-70, 70-80, 80-90, 90-100, 100-110, 110-120, 120-130, 130-140, 140-150, >150, ≧5 or ≧10 electrodes. Preferably at least 50% of the electrodes forming the ion guide are ≦3 mm, ≦2.5 mm, ≦2.0 mm, ≦1.5 mm, ≦1.0 mm or ≦0.5 mm thick. The ion guide preferably is <5 cm, 5-10 cm, 10-15 cm, 15-20 cm, 20-25 cm, 25-30 cm or >30 cm long.
A gas may be introduced into the ion guide for causing the motion of ions to be dampened preferably without substantially causing fragmentation of the ions. Alternatively, the ion guide may be located within a vacuum chamber maintained at a pressure such that the motion of ions is dampened without substantially causing fragmentation of the ions. According to all embodiments of the present invention at least a portion of the ion guide is preferably maintained, in use, at a pressure selected from the group consisting of: (i) 0.0001-100 mbar; (ii) 0.001-10 mbar; (iii) 0.01-1 mbar; (iv) >0.1 mbar; 0.1 mbar; (viii) >1 mbar; (ix) >10 mbar; and (x) <100 mbar. According to an embodiment the whole ion guide is maintained at such pressures. However, according to other embodiments only part of the ion guide is maintained at such pressures.
The travelling wave ion guide is preferably used at intermediate pressures between 0.0001 and 100 mbar, further preferably between 0.001 and 10 mbar, at which pressures the gas density will impose a viscous drag on the ions. The gas at these pressures will appear as a viscous medium to the ions and will act to slow the ions. The viscous drag resulting from frequent collisions with gas molecules helps to prevent the ions from building up excessive velocity. Consequently, the ions will tend to ride on the travelling DC wave rather than run ahead of the wave and execute excessive oscillations within the travelling potential wells.
The presence of the gas helps to impose a maximum velocity at which the ions will travel through the ion guide for a given field strength. The higher the gas pressure, the more frequent the ion-molecule collisions and the slower the ions will travel for a given field strength.
The energy of ions is dependent on their mass and the square of their velocity, and if fragmentation is to be avoided then it is desirable to keep the energy of the ions less than approximately 5-10 eV.
The preferred embodiment further comprises a time of flight mass analyser, preferably an orthogonal acceleration time of flight mass analyser. Time of flight mass analysers are discontinuous devices in that they are designed to receive a packet of ions rather than a continuous beam of ions. The time of flight analyser comprises a pusher and/or puller electrode which ejects packets of ions into a substantially field free or drift region wherein ions contained in a packet of ions are temporally separated according to their mass to charge ratio. The time taken for an ion to reach a detector is used to give an accurate determination of the mass to charge ratio of the ion in question.
Ions which exit the preferred ion guide can advantageously be arranged to reach the pusher and/or puller electrode of a time of flight mass analyser at substantially the same time. Since the ion guide produces a pulsed beam of ions, the repetition rate of the mass analyser may be matched to the waveform cycle time i.e. the repetition frequency of the DC waveform may be synchronised with the pusher pulses of the time of flight mass analyser to maximise the ion sampling duty cycle.
Since ions emitted from the ion guide will have substantially the same axial velocity, then ions of differing mass will have differing energies. If necessary, a slightly larger detector may be used in the time of flight mass analyser to accommodate ions having a spread of initial energies. Additionally and/or alternatively, the ions may be accelerated once they exit the ion guide almost immediately before reaching the pusher/puller region of the orthogonal acceleration time of flight mass analyser in order to reduce the relative energy spread of the ions. For sake of illustration only, if the ions emerge from the ion guide with constant velocity and have a range of energies from 1-10 eV then there is a 10:1 difference in axial energies between the most energetic ions and the least energetic ions. However, if all the ions are accelerated and given an additional 10 eV of energy, then the ions will have a range of energies from 11-20 eV and hence there will then only be a 1.8:1 difference in the spread of energies.
Either a continuous or pulsed ion source may be used. The ion source may comprise an Electrospray (“ESI”), Atmospheric Pressure Chemical Ionisation (“APCI”), Atmospheric Pressure Photo Ionisation (“APPI”), Matrix Assisted Laser Desorption Ionisation (“MALDI”), Laser Desorption Ionisation, Inductively Coupled Plasma (“ICP”), Electron Impact (“EI”) or Chemical Ionisation (“CI”) ion source.
According to the preferred embodiment, no additional (static) axial DC voltage gradient is required. However, according to less preferred embodiments a constant axial DC voltage gradient may be maintained along at least a portion of the ion guide. The travelling DC waveform would therefore be superimposed upon the underlying static axial DC voltage gradient. If an axial DC voltage gradient is maintained in use along at least a portion of the length of the ion guide, then an axial DC voltage difference of 0.1-0.5 V, 0.5-1.0 V, 1.0-1.5 V, 1.5-2.0 V, 2.0-2.5 V, 2.5-3.0 V, 3.0-3.5 V, 3.5-4.0 V, 4.0-4.5 V, 4.5-5.0 V, 5.0-5.5 V, 5.5-6.0 V, 6.0-6.5 V, 6.5-7.0 V, 7.0-7.5 V, 7.5-8.0 V, 8.0-8.5 V, 8.5-9.0 V, 9.0-9.5 V, 9.5-10.0 V or >10V may be maintained along a portion of the ion guide. Similarly, an axial static DC voltage gradient may be maintained along at least a portion of ion guide selected from the group consisting of: (i) 0.01-0.05 V/cm; (ii) 0.05-0.10 V/cm; (iii) 0.10-0.15 V/cm; (iv) 0.15-0.20 V/cm; (v) 0.20-0.25 V/cm; (vi) 0.25-0.30 V/cm; (vii) 0.30-0.35 V/cm; (viii) 0.35-0.40 V/cm; (ix) 0.40-0.45 V/cm; (x) 0.45-0.50 V/cm; (xi) 0.50-0.60 V/cm; (xii) 0.60-0.70 V/cm; (xiii) 0.70-0.80 V/cm; (xiv) 0.80-0.90 V/cm; (xv) 0.90-1.0 V/cm; (xvi) 1.0-1.5 V/cm; (xvii) 1.5-2.0 V/cm; (xviii) 2.0-2.5 V/cm; (xix) 2.5-3.0 V/cm; and (xx) >3.0 V/cm. A static axial DC voltage gradient may be used to help urge ions within the ion guide towards the downstream exit region of the ion guide. Alternatively, a static axial DC voltage gradient may be arranged which opposes the ions and helps to confine the ions to a region close to the travelling DC potential(s).
According to a second aspect of the present invention, there is provided a mass spectrometer comprising:
an ion source for emitting a beam of ions;
an ion guide comprising at least five electrodes having apertures for guiding the ions; and
a voltage supply for supplying a voltage wave along the electrodes for modulating the velocity of ions passing through the ion guide.
Preferably, the phase difference between two adjacent electrodes is selected from the group consisting of: (i) <180°; (ii) <150°; (iii) <120°; (iv) <90°; (v) <60°; (vi) <50°; (vii) <40°; (viii) <30°; (ix) <20°; (x) <15°; (xi) <10°; and (xii) <5°.
Preferably, the voltage wave is a ripple or other waveform which modulates the velocity of ions passing through the ion guide so that the ions emerge with substantially the same velocity.
Preferably, ions enter the ion guide as a substantially continuous beam but emerge as packets of ions due to the voltage wave.
According to a third aspect of the present invention, there is provided a mass spectrometer comprising:
an ion source;
an ion bunching device comprising a plurality of electrodes having apertures wherein trapping potentials are not applied to either the front or rear of the ion bunching device; and
a voltage supply for modulating the voltage seen by each electrode so that ions passing through the ion bunching device are urged forwards and emerge from the ion bunching device as packets of ions, each ion in the packet having substantially the same velocity.
According to a fourth aspect of the present invention, there is provided a mass spectrometer comprising:
an atmospheric pressure ion source;
an ion bunching device for receiving a substantially continuous stream of ions and for emitting packets of ions;
a voltage supply for supplying a voltage to the ion bunching device; and
a time of flight mass analyser arranged downstream of the ion bunching device for receiving packets of ions emitted by the ion bunching device;
wherein the voltage supply is arranged to supply a voltage waveform which travels along at least a part of the length of the ion bunching device, the voltage waveform causing ions to be bunched together into packets of ions.
According to a fifth aspect of the present invention, there is provided a mass spectrometer comprising:
an ion guide comprising ≧10 ring or plate electrodes having substantially similar internal apertures between 2-10 mm in diameter and wherein a DC potential voltage is arranged to travel along at least part of the axial length of the ion guide.
According to a sixth aspect of the present invention, there is provided a mass spectrometer comprising:
an ion guide comprising at least three segments,
wherein in a mode of operation:
electrodes in a first segment are maintained at a first DC potential whilst electrodes in second and third segments are maintained at a second DC potential; then
electrodes in the second segment are maintained at the first DC potential whilst electrodes in first and third segments are maintained at the second DC potential; then
electrodes in the third segment are maintained at the first DC potential whilst electrodes in first and second segments are maintained at the second DC potential;
wherein the first and second DC potentials are different.
Preferably, ions are not substantially fragmented within the ion guide.
According to a seventh aspect of the present invention, there is provided a mass spectrometer comprising:
a continuous ion source for emitting a beam of ions;
an ion guide arranged downstream of the ion source, the ion guide comprising ≧5 electrodes having apertures through which ions are transmitted in use, wherein the electrodes are arranged to radially confine ions within the apertures, wherein a travelling DC wave passes along at least part of the length of the ion guide and wherein ions are not substantially fragmented within the ion guide; and
a discontinuous mass analyser arranged to receive ions exiting the ion guide.
Preferably, an additional constant axial DC voltage gradient is maintained along at least 5%, 10%, 15%, 20%, 25%, 30%, 35%, 40%, 45%, 50%, 55%, 60%, 65%, 70%, 75%, 80%, 85%, 90% or 95% of the length of the ion guide.
Preferred ion sources such as Electrospray or APCI ion sources are continuous ion sources whereas a time of flight analyser is a discontinuous device in that it preferably requires a packet of ions. The ion guide according to the preferred embodiment is effective in essentially coupling a continuous ion source with a discontinuous mass analyser such as a time of flight mass analyser.
According to an eighth aspect of the present invention, there is provided a method of mass spectrometry, comprising:
travelling a DC potential along at least a portion of an ion guide.
According to a ninth aspect of the present invention, there is provided a mass spectrometer comprising:
an ion guide comprising a plurality of electrodes, wherein the following voltages are applied to at least five of the electrodes:
(i) an AC or RF voltage so as to radially confine ions within the ion guide;
(ii) a constant DC offset voltage; and
(iii) an additional DC voltage which varies with time.
Each of said electrodes may have substantially the same constant DC offset voltage (which may be OV or a positive or negative DC value) or alternatively at least some of the electrodes may be maintained at different DC offset voltages so that a constant axial DC voltage gradient is generated along at least part of the ion guide.
According to a tenth aspect of the present invention, there is provided a mass spectrometer comprising:
an RF ion guide having a plurality of segments;
an orthogonal acceleration time of flight mass analyser; and
a controller which generates a DC potential which travels along at least part of the RF ion guide so as to cause ions of different mass to be ejected from the ion guide with essentially the same velocity so that they arrive at the orthogonal acceleration time of flight mass analyser at essentially the same time.
According to an eleventh aspect of the present invention, there is provided a mass spectrometer comprising:
a continuous ion source;
an ion guide having a plurality of segments wherein a DC potential is progressively passed along at least some of the segments so that a DC wave having a first frequency passes along at least a portion of the ion guide; and
an orthogonal acceleration time of flight mass analyser having an injection electrode for injecting ions into a drift region, wherein the injection electrode is energised at a second frequency.
Preferably, the first frequency differs from the second frequency by less than 50%, 40%, 30%, 20%, 10%, 5%, 1% or 0.1%. According to a particularly preferred embodiment, the first frequency substantially matches the second frequency. According to other embodiments either the first frequency is substantially a harmonic frequency of the second frequency or the second frequency is substantially a harmonic frequency of the first frequency.
The DC wave may have a frequency in the range: (i) 1-5 kHz; (ii) 5-10 kHz; (iii) 10-15 kHz; (iv) 15-20 kHz; (v) 20-25 kHz; (vi) 25-30 kHz; (vii) 30-35 kHz; (viii) 35-40 kHz; (ix) 40-45 kHz; (x) 45-50 kHz; (xi) 50-55 kHz; (xii) 55-60 kHz; (xiii) 60-65 kHz; (xiv) 65-70 kHz; (xv) 70-75 kHz; (xvi) 75-80 kHz; (xvii) 80-85 kHz; (xviii) 85-90 kHz; (xix) 90-95 kHz; or (xx) 95-100 kHz. A frequency of approximately 10 kHz is particularly preferred.
Similarly, the injection electrode of the time of flight mass analyser may be energised with a frequency in the range: (i) 1-5 kHz; (ii) 5-10 kHz; (iii) 10-15 kHz; (iv) 15-20 kHz; (v) 20-25 kHz; (vi) 25-30 kHz; (vii) 30-35 kHz; (viii) 35-40 kHz; (ix) 40-45 kHz; (x) 45-50 kHz; (xi) 50-55 kHz; (xii) 55-60 kHz; (xiii) 60-65 kHz; (xiv) 65-70 kHz; (xv) 70-75 kHz; (xvi) 75-80 kHz; (xvii) 80-85 kHz; (xviii) 85-90 kHz; (xix) 90-95 kHz; or (xx) 95-100 kHz. A frequency of 5-50 kHz is preferred and a frequency of 10-40 kHz is particularly preferred.
In all embodiments of the present invention, the DC wave may have an amplitude selected from the group consisting of: (i) 0.2-0.5 V; (ii) 0.5-1 V; (iii) 1-2 V; (iv) 2-3 V; (v) 3-4 V; (vi) 4-5 V; (vii) 5-6 V; (viii) 6-7 V; (ix) 7-8 V; (x) 8-9 V; (xi) 9-10 V; (xii) 10-11 V; (xiii) 11-12 V; (xiv) 12-13 V; (xv) 13-14 V; (xvi) 14-15 V; (xvii) 15-16 V; (xviii) 16-17 V; (xix) 17-18 V; (xx) 18-19 V; and (xxii) 19-20 V. The amplitude is preferably the relative amplitude compared to any constant bias DC voltage applied to the ion guide. A relative amplitude in the range 1-15 V is preferred and asks a relative amplitude in the range of 5-10 V is particularly preferred.
Preferably, the ion guide comprises at least 4, 5, 6, 7, 8, 9, 10, 11, 12, 13, 14, 15, 16, 17, 18, 19, 20, 21, 22, 23, 24, 25, 26, 27, 28, 29 or 30 segments.
Preferably, the DC wave comprises: (i) a potential barrier; (ii) a potential well; (iii) a potential well and a potential barrier; (iv) a repeating potential barrier; (v) a repeating potential well; (vi) a repeating potential well and potential barrier; or (vii) a repeating square wave.
Preferably, the DC wave has an amplitude and the amplitude: (i) remains substantially constant; (ii) decreases with time; (iii) increases with time; or (iv) varies non-linearly with time.
According to a twelfth aspect of the present invention, there is provided a method of mass spectrometry comprising:
passing ions to an RF ion guide having a plurality of segments; and
generating a DC potential which travels along at least part of the RF ion guide so as to cause ions of different mass to be ejected from the ion guide with essentially the same velocity so that they arrive at an orthogonal acceleration time of flight mass analyser at essentially the same time.
BRIEF DESCRIPTION OF THE DRAWINGS
Various embodiments of the present invention will now be described, by way of example only, and with reference to the accompanying drawings in which:
FIG. 1 shows a preferred ion tunnel ion guide wherein the DC voltage supply to each ion tunnel segment is individually controllable;
FIG. 2 ( a ) shows a front view of an ion tunnel segment;
FIG. 2 ( b ) shows a side view of an upper ion tunnel section;
FIG. 2 ( c ) shows a plan view of an ion tunnel segment;
FIG. 3 ( a ) shows a schematic of a segmented RF ion guide;
FIG. 3 ( b ) shows a DC travelling potential barrier;
FIG. 3 ( c ) shows a DC travelling potential well;
FIG. 3 ( d ) shows a DC travelling potential well and potential barrier; and
FIG. 3 ( e ) shows a square wave DC travelling wave.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
A preferred ion guide will now be described with reference to FIGS. 1 and 2. The ion guide is preferably an ion tunnel ion guide 1 comprising a housing having an entrance aperture 2 and an exit aperture 3 . The entrance and exit apertures 2 , 3 are preferably substantially circular apertures. The plates forming the entrance and/or exit apertures 2 , 3 may be connected to independent programmable DC voltage supplies (not shown).
Between the plate forming the entrance aperture 2 and the plate forming the exit aperture 3 are arranged a number of electrically isolated ion tunnel segments 4 a , 4 b , 4 c . In one embodiment fifteen segments 4 a , 4 b , 4 c are provided. Each ion tunnel segment 4 a ; 4 b ; 4 c comprises two interleaved and electrically isolated sections i.e. an upper and lower section. The ion tunnel segment 4 a closest to the entrance aperture 2 preferably comprises ten electrodes (with five electrodes in each section) and the remaining ion tunnel segments 4 b , 4 c preferably each comprise eight electrodes (with four electrodes in each section). All the electrodes are preferably substantially similar in that they have a central substantially circular aperture (preferably 5 mm in diameter) through which ions are transmitted. The entrance and exit apertures 2 , 3 may be smaller e.g. 2.2 mm in diameter than the apertures in the electrodes or the same size.
All the ion tunnel segments 4 a , 4 b , 4 c are preferably connected to the same AC or RF voltage supply, and different segments 4 a ; 4 b ; 4 c may be provided with different offset DC voltages. A time varying DC potential wave is also applied to the various segments 4 a , 4 b , 4 c so that a travelling DC voltage wave is generated. The two sections forming an ion tunnel segment 4 a ; 4 b ; 4 c are connected to different, preferably opposite, phases of the AC or RF voltage supply.
A single ion tunnel section is shown in greater detail in FIGS. 2 ( a )-( c ). The ion tunnel section has four (or five) electrodes 5 , each electrode 5 having a 5 mm diameter central aperture 6 . The four (or five) electrodes 5 depend or extend from a common bar or spine 7 and are preferably truncated at the opposite end to the bar 7 as shown in FIG. 2 ( a ). Each electrode 5 is typically 0.5 mm thick. Two ion tunnel sections are interlocked or interleaved to provide a total of eight (or ten) electrodes 5 in an ion tunnel segment 4 a ; 4 b ; 4 c with a 1 mm inter-electrode spacing once the two sections have been interleaved. All the eight (or ten) electrodes 5 in an ion tunnel segment 4 a ; 4 b ; 4 c comprised of two separate sections are preferably maintained at substantially the same DC voltage. Adjacent electrodes in an ion tunnel segment 4 a ; 4 b ; 4 c comprised of two interleaved sections are connected to different, preferably opposite, phases of an AC or RF voltage supply i.e. one section of an ion tunnel segment 4 a ; 4 b ; 4 c is connected to one phase (RF+) and the other section of the ion tunnel segment 4 a ; 4 b ; 4 c is connected to another phase (RF−).
Each ion tunnel segment 4 a ; 4 b ; 4 c is mounted on a machined PEEK support that acts as the support for the entire assembly. Individual ion tunnel sections are located and fixed to the PEEK support by means of a dowel and a screw. The screw is also used to provide the electrical connection to the ion tunnel section. The PEEK supports are held in the correct orientation by two stainless steel plates attached to the PEEK supports using screws and located correctly using dowels. These plates are electrically isolated and have a voltage applied to them. Gas may optionally be supplied to the ion guide 1 via a 4.5 mm ID tube.
An AC or RF voltage supply provides phase (RF+) and anti-phase (RF−) voltages at a frequency of preferably 1.75 MHz and is coupled to the ion tunnel sections 4 a , 4 b , 4 c via capacitors which are preferably identical in value (100 pF). According to other embodiments the frequency may be in the range of 0.1-3.0 MHz.
The DC voltage supplied to the plates forming the entrance and exit apertures 2 , 3 is also preferably independently controllable and preferably no AC or RF voltage is supplied to these plates.
The transient or time varying DC voltage applied to each segment may be above and/or below that of the constant or time invariant DC voltage offset applied to the segment so as to cause movement of the ions in the axial direction. FIG. 3 ( a ) shows a simplified diagram of a segmented RF ion guide and shows the direction in which ions are to move. FIGS. 3 ( b )-( e ) show four examples of various DC travelling waves superimposed upon a constant DC voltage offset. FIG. 3 ( b ) shows a waveform with a single potential hill or barrier, FIG. 3 ( c ) shows a waveform with a single potential well, FIG. 3 ( d ) shows a waveform with a single potential well followed by a potential hill or barrier, and FIG. 3 ( e ) shows a waveform with a repeating potential hill or barrier (square wave).
Although the present invention has been described with reference to preferred embodiments, it will be understood by those skilled in the art that various changes in form and detail may be made without departing from the scope of the invention as set forth in the accompanying claims. | An ion guide is disclosed wherein a travelling DC wave is passed along the length of the ion guide so that ions exit the ion guide having substantially the same velocity. | 7 |
FIELD OF THE INVENTION
[0001] The instant invention is directed to a curb inlet filter, and more particularly to a curb inlet filter for filtering out sediments and the like flowing into a curb inlet.
RELATED ART
[0002] Ground water from heavy rains or melted snow is normally collected in a storm sewer or in a curb inlet and then flows into an underground storm sewer line. Water flows into the basin through openings in a grate on top of the basin, or into a curb inlet through an opening along the vertical portion of the curb.
[0003] It is important that water entering a sewer line should be free of suspended solids, such as sediments, debris or the like. If stormwater, for example, flows into a curb inlet, in a construction site where soil has been disturbed, a great deal of sediment or other solids (including debris) may flow into the curb inlet and thus, into the storm sewer lines. When too much sediment or solid materials flow into the storm sewer lines, they become clogged.
[0004] Accordingly, in the past, numerous products have been used to prevent sediment or other solids from flowing into curb inlet storm drains. Products such as straw wattles have been used to filter out sediment and other solids flowing into a curb inlet storm drain. Hay bails have also been used to filter out sediment and other solids from stormwater flowing into a curb inlet. Additionally, stones have been wrapped in chicken wire and placed in front of a curb inlet type storm drain. The straw wattle and hay bail type of sediment filters often get clogged and are often not reusable. Also, they may decompose and slip into the storm drain. This could cause further clogging. Furthermore, the method using stones and chicken wire (stone bundles) does not filter out as large amount of sediment and other solids as do other methods. Also, these stone bundles break and fall into the drains, and can also be a safety hazard for children.
SUMMARY OF THE INVENTION
[0005] The instant invention is a curb inlet filter for filtering out sediments, solids and the like flowing into a curb inlet type of storm drain. Generally, the term sediment, when used in connection in this application refers to solid particles that are suspended in water flowing into a curb inlet. Sediment may originate from earth, grass, and other sources, and any other type of material suspended in water flowing into a curb inlet. Generally, a curb inlet refers to an opening in a vertical face of a curb (with or without a grade level storm sewer catch basin with a grating on top) which leads to a drain unit that directs stormwater into a storm sewer. While focused on use with a curb inlet type of drain, the instant invention may also be used with a combination type of drain which joins a curb inlet drain with a catch basin type of drain with a horizontal grate.
[0006] The instant invention includes a frame and a filter cover formed on at least part of the frame. For example, such types of curb inlet filters are often used in and around construction sites where earthen materials have been moved around and under heavy rains become sediment suspended in runoff water. As the runoff water (with sediment or the like suspended therein) flow into a curb inlet type of storm drain, the instant invention covers the mouth of the curb inlet and filters out many of the sediment or solid particles suspended in the stormwater.
[0007] A curb inlet filter, in accordance with the instant invention, is provided for filtering out sediments, solids and the like flowing into a curb inlet. The curb inlet filter has a filter body which includes a water permeable, substantially rigid, elongated frame having an upstream side and a downstream side thereof, and an elongated filter cover formed around at least one of the sides of the frame, wherein the filter cover is formed of a filtration material to filter out sediments and the like. Additionally, the curb inlet filter includes a weight support attached to the bottom of the filter body for supporting a weight, and a support strap connecting the weight support to an upper portion of the filter body. The support strap helps to pull the top of the filter body snug with the top of the curb inlet. It is contemplated that the weight support can be attached rigidly or flexibly to the filer body. It is then possible that the support straps could be connected to different portions of the filer body, rather than just the upper portion, although the upper portion is preferable. It is also possible that there are no support straps. For example, a weight support may be attached more rigidly to filter body, so that support straps are not necessary.
[0008] Additionally, the curb inlet filter may include a plurality of spacers, wherein at least one spacer is formed at each end of the frame. Spacers are formed on the downstream side thereof, in order to form a gap between the spacers and the downstream side of the frame. This allows the water to flow over the top of the frame, through the gap formed between the spacers, and into the curb inlet.
[0009] The filter cover of the filter body preferably entirely surrounds the frame. However, it is possible to mount the filter cover on only one side of the frame. While the filter cover is preferably a woven fabric, it may also be formed of a non-woven material. This non-woven material could be a mat-type material, or it may be some type of metal grill or other type of filter. The preferred woven fabric is multidimensional, and even more preferably a three dimensional fabric. A preferable fabric is Pyramat® manufactured by SI Geosolutions. For the same size of frame, a three dimension fabric has a larger surface area than a conventional two dimensional fabric. Accordingly, a filter using a three dimensional fabric will be able to filter more sediment than a conventional two dimensional fabric. Another reason a three-dimensional fabric is preferable is that flowing water tends to bounce off of a two-dimensional fabric easier than a three-dimensional fabric. Additionally, when the filter cover entirely surrounds the frame, in envelop fashion, it presents two surfaces for filtering, one on the upstream side and one on the downstream side of the frame.
[0010] The weight support may be removably attached or fixedly attached to a bottom portion of the filter body. In other words, it may be located in a lower area of the filter body for pulling the filter snug against the curb. More specifically, the weight support may be removably attached to a bottom portion of the filter body by using connectors to make the connection. Furthermore, the weight support may be a bag for receiving a weight therein. When in use, it is easy for the user to put a portion of a steel or other type of weight in the bag. Additionally, the bag may be waterproof with a closable filling hole therein. A user could simply fill the bag with water and close the filing hole in order to provide the weight for the curb inlet filter.
[0011] The filter cover may be formed of a cylindrical sleeve, into which the frame is axially inserted, wherein the sleeve is closed up at opposing ends thereof. Alternately, the filter cover may have a closeable seem running along a longitudinal side thereof. The frame may be inserted into the filter cover and the seam simply closed up. Any other appropriate arrangement for covering the sleeve is also appropriate.
[0012] The frame may be a single unit, or it may be made of a plurality of individual units attached together. They may be permanently attached at they may be detachably attached to one another. Using a plurality of individual elements, the frame may be built up in modules for use with different sized curb inlets. Also, when a frame is composed of a plurality of individual elements (each one shorter than the total length of the frame) the frame may be broken down for easier shipping. Preferably, each of the individual elements of the frame would include one or more spacers. A frame element, whether it is one or a plurality of elements, may also be formed to be snapped together for easy assembly. Thus, the frame elements could be interlocking with one another. For example, each end of a frame element may have a dovetail or other equivalent type joint. In other words, one end of the frame would have a dovetail projection, and the opposite end of the frame element would have a dovetail recess, such that a frame may be formed of the plurality of individual elements in which the dovetail portions are nested with one another. Also, a key/keyway combination (or any other conventional means) may be used to join individual frame elements together.
[0013] The frame may also be a collapsible type of frame. The plurality of individual elements may be connected together by hinges, or the like, to provide an easily collapsible frame for ready transportation. Additionally, the frame may have a telescoping structure that makes for easy storage or shipping when in a collapsed state.
[0014] Additionally, the frame (whether a single unit or a plurality of individual elements) may also include a flexible insert formed on a bottom portion thereof, in order to adjust to the contours of the road surface on which the filter sets. The flexible insert may simply be a type of foam or foam rubber formed on the bottom of the frame. Additionally, the flexible insert may be an extruded rubber insert of any type which is fixed to the bottom of the frame or inserted into a groove or keyway.
[0015] For ease of transporting, a handle may also be formed on an upper portion of the curb inlet filter. Tieback straps may also be formed on the upper portion of the filter body in order to stabilize the curb inlet filter when in position in front of a curb inlet.
[0016] Furthermore, the curb inlet filter according to the instant invention may include an additional layer to absorb metals, oils and other containments. For example a coconut mat or organic layer may be added to absorb contaminants or other undesirable substances.
[0017] Also, the curb inlet according to the instant invention is easy to clean and reuse. It may simply be washed off and repositioned for subsequent use. As such, it provides great labor savings for a user, such as a contractor. It is reusable and, may be easily replaced if damaged. The frame may be easily replaced if it is damaged, while retaining the filer cover. Conversely, if the filter cover is damaged, it may easily be replaced while retaining the frame.
BRIEF DESCRIPTION OF THE DRAWINGS
[0018] The advantages of the invention will become apparent in the following description taken in conjunction with the drawings, wherein:
[0019] FIG. 1 is a perspective view of a downstream side of the curb inlet filter in accordance with the instant invention;
[0020] FIGS. 2 ( a )- 2 ( c ) are views of a curb inlet filter;
[0021] FIG. 3 is a perspective view of a curb inlet;
[0022] FIG. 4 is a perspective view of the curb inlet of FIG. 3 , with the curb inlet filter in position;
[0023] FIG. 5 is a cross-sectional view of a curb inlet and storm sewer drain with a curb inlet filter in position;
[0024] FIG. 6 is a top plan view showing a curb inlet filter in position in front of a curb inlet;
[0025] FIG. 7 is a partial cutaway view of a curb inlet filter showing the frame thereof;
[0026] FIGS. 8 ( a )- 8 ( b ) illustrate insertion of the frame into filter covers;
[0027] FIG. 9 illustrates different weight bags for attaching to the filter body;
[0028] FIGS. 10 ( a ) and 10 ( b ) illustrate flexible inserts usable with the curb inlet filter;
[0029] FIG. 11 is an illustration of the curb inlet filter, demonstrating woven and non-woven fabrics thereon;
[0030] FIG. 12 is a perspective view of a single frame structure;
[0031] FIG. 13 is an illustration of a plurality of individual elements which make up a single elongated frame; and
[0032] FIG. 14 is an illustration of dovetail type connectors between individual elements.
DETAILED DESCRIPTION OF THE INVENTION
[0033] FIG. 1 is a perspective view of a downstream side of the curb inlet filter in accordance with the instant invention. FIGS. 2 ( a )- 2 ( c ) are additional views of the stormwater filer. As illustrated in FIGS. 1 and 2 , curb inlet filter 10 includes a filter body 12 , a weight support 16 , and support straps 18 . A handle 20 is attached to the top of filter body 12 for ease of transportation from one location to another. Tieback straps 22 may or may not be used. They may be used to tie the upper portion of filter body 12 back to keep it snug with the curb inlet. Arrow 24 represents the inflow of water toward the curb inlet filter 10 . Arrow 26 represents the outflow of water after it has passed through stormwater filter 10 . Accordingly, arrow 24 represents the upstream side of curb inlet filter 10 , while arrow 26 represents the downstream side of curb inlet filter 10 .
[0034] FIG. 3 is a perspective view of a typical curb inlet. Specifically, curb inlet 28 is formed in a curb 36 , adjacent a road surface 30 . Normally, such curb inlets have a top portion 32 with a manhole (or access) cover 34 located therein, in order to provide access to the drain below. A curb inlet opening 40 provides a passage for the inflow of water, represented by arrow 24 , into the storm drain itself.
[0035] FIG. 4 illustrates the curb inlet filter 10 in place, in front of a curb inlet. FIG. 5 illustrates a cross-section of the curb inlet with the curb inlet filter 10 in place. In FIG. 4 , filter body 12 is in place in front of curb inlet opening 40 . In this illustration, tieback straps 22 extend rearwardly to the ground surface behind curb 36 . The tieback straps 22 are staked into the ground by stakes 42 .
[0036] FIG. 5 is a cross-section of the curb inlet 28 of FIG. 4 , with the curb inlet filter 10 in place. As illustrated in FIG. 5 , the structure of the curb inlet 28 includes a curb inlet housing 48 formed in the ground and adjacent to road surface 30 . Curb inlet 28 has a top portion 32 formed on top of the curb inlet housing 48 . An access opening 35 is formed in top cover 32 for allowing access to the curb inlet 28 for removing clogs and the like. An access cover 34 covers the access opening 35 . A curb inlet opening 40 is formed for allowing stormwater to enter the curb inlet. Drain pipe 46 is formed on the lower portion of the curb inlet housing 48 for directing the stormwater down to the storm sewer.
[0037] Curb inlet filter 10 is shown in place in front of curb inlet opening 40 . Filter body 12 sets on the road surface 30 with weight support 16 extending in the downstream direction into curb inlet housing 48 . As illustrated in FIG. 5 , weight support 16 also contains a weight 17 therein. Furthermore, support strap 18 extends from weight support 16 to an upper portion of filter body 12 . Furthermore, filter body 12 includes a water permeable, substantially rigid, elongated frame 50 and an elongated filter cover 54 . Frame 50 also includes a spacer 52 formed on a downstream side thereof. Because the thickness of the filter body 12 is substantially less than the width, this filter does not project very far from the curb, and thus does not extend substantially out into the road.
[0038] FIG. 6 is a plan view showing the curb inlet filter 10 in place against curb inlet 28 . As illustrated in FIGS. 5 and 6 , arrow 24 represents the inflow of stormwater. This inflow of stormwater is normally laden with suspended solids such as sediment, debris and the like. As the stormwater or sediment laden water impinges on the upstream side of curb inlet filter 10 , suspended solids such as sediment and the like are trapped by the filter material of filter cover 54 . The water flows through filter cover 54 , and the water permeable frame 50 . The outflow of water on the downstream side of the curb inlet filter 10 is represented by arrow 26 . This outflow has been filtered by the curb inlet filter 10 and flows through curb inlet housing 48 into drain pipe 46 and down into the storm sewer system.
[0039] When the curb inlet filter 10 becomes clogged, or if the water level rises above the top of the curb inlet filter 10 , overflow water, represented by arrows 44 , flows over the top of stormwater 10 and into curb inlet opening 40 . This is possible because spacers 52 space the frame 50 apart from the front of curb inlet 28 . Frame 50 and spacers 52 form a gap therebetween in order to allow the overflow water to flow into opening 40 of inlet 28 . The overflow capability is often specified by engineers when specifying requirements for filters for curb inlets.
[0040] FIG. 7 illustrates a partial cutaway view of the curb inlet filter 10 . As illustrated, filter body 12 includes a frame 50 . The frame 50 is a water permeable, substantially rigid, elongated structure. A spacer 52 is formed near an end thereof on a downstream side thereof. As illustrated in FIG. 7 , the frame is made of elongated rails 58 connected together by cross members 60 . This forms openings 56 which allow water to flow therethrough. It should be noted that the frame 50 disclosed in FIG. 7 is only one example of such a frame. Frame 50 may be made of plastic, metal, wood, recycled material or any other suitable material that provides the necessary water permeability, and the rigidity necessary to support the filter cover 14 . It is even possible that the frame may be made of a substance such as coconut mat, so long as it has sufficient rigidity and water permeability. Frame 50 is formed as an elongated structure, and generally has a long and thin shape. The shape may be board like so that it does not take up a great deal of space in front of the curb inlet.
[0041] Filter cover 14 , as illustrated in FIG. 7 , entirely surrounds frame 50 . Although it is possible for the filter cover to be formed on only a single side of frame 50 . Preferably, however, filter cover 14 entirely surrounds frame 50 .
[0042] While filter cover 14 is preferably formed by a fabric, it may also be formed by a grill or grating. Preferably though, a fabric is used for the filter cover. The fabric may be a woven fabric, a non-woven fabric, or another type of non-woven material. It is also preferable to use a multidimensional, woven fabric such as a three dimensional fabric, as illustrated in FIG. 7 . A three dimensional fabric used as a filter cover is found to be efficient in filtering out solids, such as sediment and the like. Because a three dimensional fabric has a greater surface area than a two dimensional fabric, more sediment may be filtered out of the stormwater flowing through the filter.
[0043] FIGS. 8A and 8B illustrate different forms of filter covers 14 . In FIG. 8A , filter cover 14 is formed of a tubular shape of fabric 62 . In assembling curb inlet filter 10 in FIG. 8A , frame 50 is inserted into tubular fabric 62 and ends 64 , 64 are closed. FIG. 8B illustrates an alternate version of how curb inlet filter 10 is assembled. Flat fabric 66 is provided with seams 68 along the edges thereof. For assembly, frame 50 is positioned in the fold of fabric 66 and seams 68 , 68 are closed-up by way of zipper, velcro, thread, or any other conventional way.
[0044] FIG. 9 illustrates different weight bags for removably attaching the weight bag to the weight support of the storm filter. In FIG. 9 , weight support 16 is attached to a lower portion of filter body 12 of curb inlet filter 10 . Weight bags may also be considered to be part of the weight support 16 . Weight bag 76 or waterproof weight bag 78 may alternately be attached to the weight support 16 . The detachability of the weight bags increases adaptability and convenience for the user. For ease of attaching and detaching a weight, weight support 16 , as illustrated in FIG. 9 , includes male clips 70 , 70 , attached to weight support 16 by way of straps, 72 , 72 . Male clips 72 , 72 are attachable with female clips 74 a , 74 a of weight bag 76 , or female clips 74 b , 74 b of waterproof weight bag 78 .
[0045] Weight bag 76 is attached to female clips 74 a , 74 a by way of straps 86 , 86 . Weight bag 76 includes a front flap 82 folded over front panel 88 and secured on the edges. Accordingly, this allows a weight such as weight 17 to be inserted under front flap 82 and behind front panel 88 and thus to securely remain there in order to serve as a weight for curb inlet filter 10 . Weight 17 may be a steel bar, or any other suitable material for weighing down the stormwater filer. Weight bag 76 may also be part of weight support 16 , since weight bag 76 also supports weight 17 . Additional clips 90 , 90 are attached to a lower portion of weight bag 6 in order to connect with cooperative male clips (not shown) attached to support straps 18 .
[0046] Waterproof weight bag 78 , as illustrated in FIG. 9 , also attaches to weight support 16 by way of female clips 74 b , 74 b cooperatively engaging male clips 70 , 70 . Female clip 74 b , 74 b are attached to waterproof weight bag 78 by way of straps 86 , 86 . A closeable filling hole 80 is formed in a front panel 92 of waterproof weight bag 78 . Closeable filling hole 80 may have a screw top or any other type of closable filling hole suitable for enabling waterproof bag 78 to be filled with water, and then closed-up, in order to provide the sufficient weight for curb inlet filter 10 . As with weight bag 76 , waterproof weight bag 78 may be part of weight support 16 , since waterproof weight bag 78 supports the water therein for providing weight to hold the curb inlet filter 10 in place. Also, waterproof weight bag 78 may include female clips 94 , 94 to cooperatively engage with male clips (not shown) of support straps 18 . While clips are illustrated in FIG. 9 , any suitable type of connecting device may be employed to connect a bag to the weight support 16 .
[0047] FIGS. 10 ( a ) and 10 ( b ) illustrate flexible inserts used with the curb inlet filter 10 . Specifically, FIG. 10 ( a ) illustrates a flexible extruded rubber insert 96 attached to a lower portion of frame 50 by way of a slot 98 formed in the bottom of the frame 50 . A projection 100 formed axially along the length of extruded rubber insert 96 is engaged with slot 98 of frame 50 for securing the extruded rubber insert 96 to the bottom thereof. While it is preferable that extruded rubber insert 96 is located within filter cover 14 , other arrangements are also possible.
[0048] FIG. 10 ( b ) illustrates another version of the flexible insert. In FIG. 10 ( b ), a foam portion 102 is fixed to a lower part of frame 50 . Form portion 102 is affixed to the bottom of frame 50 by adhesives or any other appropriate method. As with extruded rubber insert 96 , foam portion 102 is preferably formed on the bottom of frame 50 , inside of filter cover 14 .
[0049] FIG. 11 illustrates two type of fabrics used for filter cover 14 of filter body 12 . Filter cover 14 is split into two different types of covers for illustration purposes only. On the left side of FIG. 11 , a woven fabric 104 is illustrated, while a non-woven fabric 106 is illustrated on the right side of FIG. 11 . Woven fabric 104 is illustrated as a multidimensional fabric. Specifically, woven fabric 104 is a three dimensional fabric. While a two dimensional fabric may be used for filter cover 14 , a three dimensional fabric is preferable because it presents a larger surface area to filter the sediment laden stormwater. With a greater surface area, the three dimensional woven fabric takes longer to clog up than a similar two dimensional fabric. Non-woven fabric 106 may be a water permeable matt fabric. A perforated sheet may also be used as a filter cover.
[0050] FIG. 12 illustrates a single frame structure with elongated frame 50 having spacers 52 formed on the downstream side thereof, one each positioned at opposite ends thereof. As illustrated, frame 50 contains generally parallel rails 58 which are connected together by cross members 60 . Frame 50 provides substantial rigidity and is water permeable, so that the substantially rigid frame supports filter cover 14 and allows water to pass therethrough.
[0051] FIG. 13 is an illustration of a plurality of individual elements which make up a single elongated frame. In FIG. 13 , frame portions 50 a , 50 b and 50 c can be detachably attached to one another. In FIG. 13 , each individual frame element has a male and female connector. For example, frame element 50 a has a male connector projection 108 and a female connector recess 110 . Furthermore, each individual frame element 50 a may be supplied with individual spacers 52 a , 52 a on a downstream side thereof. Thus, frames of different length may be assembled by connecting individual frame elements together. While any number of individual frame elements may be combined to result in a desired length frame, individual elements are often easier and less expensive to ship.
[0052] FIG. 14 illustrates a different style of connector compared with male and female connectors 108 , 110 of FIG. 13 . In FIG. 14 , a male dovetail projection 112 is formed on an end of frame element 50 d . Male dovetail projection 112 enables frame element 50 d to be attached to frame element 50 e by being coupled with female dovetail recess 114 . Additionally, individual frame elements may be detachably attached to one another by screwing individual elements together.
[0053] Although a specific form of embodiment of the instant invention has been described above and illustrated in the accompanying drawings in order to be more clearly understood, the above description is made by way of example and not as a limitation to the scope of the instant invention. It is contemplated that various modifications apparent to one of ordinary skill in the art could be made without departing from the scope of the invention which is to be determined by the following claims. | A curb inlet filter for filtering out sediments and the like flowing into a curb inlet, includes a filter body, including a water permeable, substantially rigid, elongated frame having an upstream side and a downstream side thereof, and an elongated filter cover formed around at least one of the sides of the frame. The filter cover is formed of a filtration material to filter out sediments and the like. Further, a weight support attached to a bottom of said filter body for supporting a weight, and a support strap connects the weight support to an upper portion of the filter body. | 4 |
RELATED APPLICATIONS
The present application claims priority from U.S. Provisional Patent Application Ser. No. 60/282,875, filed Apr. 11, 2001.
FIELD OF THE INVENTION
The present invention relates to game feeders, and in particular, to game feeders having an improved feed dispensing mechanism.
DESCRIPTION OF RELATED ART
Game feeders are used primarily to attract wild animals into certain areas and to supplement wild animals' diets. Game feeders are used to feed a variety of species ranging from large animals, such as deer, to fur bearing animals and even fish. During times when natural food sources are scarce, such as during a severe winter or a population boom, it is difficult for a herd of deer, or other animals, to find adequate food, and game feeders are used to supplement their natural diet. Game feeders are also used for recreational purposes to increase the likelihood of spotting a certain species in a certain area.
Major disadvantages of current game feeders are their high visibility, difficulty to set up, difficulty to fill, and uncontrolled feed dispersion pattern. These problems result from the feed dispersion mechanism, which must be kept out of wild animals' reach in order to prevent the animals from having unfettered access to the feed stored in the game feeder.
Wild animals are very sensitive to new and strange items appearing in their habitat, and, although a game feeder contains and disperses feed for the wild animals, its presence can disturb animals' natural habits and even frighten them away. Current game feeders are difficult to camouflage because their design requires a large structure that does not fit in well with animals' natural habitat. Available game feeders have a feed storage area that narrows at the bottom, usually into an inverted cone shape. The bottom portion of the feed storage area is positioned a slight distance away from the feed dispensing mechanism. Feed dispensing mechanisms typically have a motor and power source connected to a paddle, which is usually a flat disc that is roughly parallel to the ground and has raised paddles thereon, and a control element such as a timer or simple computer. Such feed mechanisms are well known in the art, and disperse small amounts of feed intermittently. Feed in the feed storage area is prevented from draining out by the close proximity of the feed dispensing mechanism to the opening at the bottom of the feed storage area
When the feed dispensing mechanism is operated, the motor spins a disc with fins thereon to disperse feed randomly in a circular area. While the feed dispensing mechanism is operating, feed flows from the feed storage area to replace the feed that was resting on the disc, thus providing a constant supply of feed to be dispersed. When the feed dispensing mechanism stops, the feed resting on the disc prevents further feed from flowing out of the feed storage area. Such feed dispensing mechanisms need to be kept out of wild animals' reach because an animal could eat all of the feed in the feed storage area simply by eating the feed from the disc. One solution to prevent wild animals from having access to the feed on the disc was to place a wire cage around the feed dispensing mechanism, however some animals such raccoons and squirrels can reach through the cage to the feed, thus depriving other animals such as deer of the feed.
Another solution to prevent access to the feed on the disc is to keep the entire game feeder out of reach of wild animals. This requires either hanging the feeder in a tree, or supporting the game feeder on long poles above the ground. For example, see U.S. Pat. No. 5,862,777. Hanging feeders in trees typically results in poor feed dispersion because of the proximity to the tree and the uncontrollable, circular feed dispersion that results in feed becoming caught in the tree or piled at the base of the tree. The major disadvantage of supporting the game feeder on poles is that the game feeder must be kept seven to twelve feet above the ground, resulting in a large structure that is difficult to camouflage. Additionally, game feeders on long poles are difficult to set up, especially in remote areas and/or on uneven terrain, and are difficult to fill with feed because of their height above the ground.
There is a need for reducing the visibility of a game feeder. There is also a need to provide a game feeder that delivers feed in a controlled direction. There is an additional need to provide a game feeder that is easy to set up and easy to refill.
SUMMARY OF THE INVENTION
The above needs, and others, are addressed by the present invention, which provides a game feeder with an improved feed dispersion mechanism. A paddle, for example a disc with raised fins thereon, is aligned to be substantially perpendicular to the ground when the game feeder is set up. The improved feed dispersion mechanism is also configured to prevent access to the feed without requiring the use of a cage and without requiring suspension of the game feeder at a great height above the ground.
Accordingly, one aspect of the invention relates to an improved feed dispensing mechanism. The improved feed dispensing mechanism comprises a housing and a paddle contained within the housing. A feed connector connected to the housing is configured to deliver feed to the paddle, and an agitator connected to the paddle is configured to prevent feed from flowing through the feed connector when the paddle is not moving and to enable feed to flow through the feed connector to the paddle when the paddle is moving.
Accordingly, another aspect of the invention relates to a game feeder. The game feeder comprises a feed source with a feed conduit connected to the feed source. A feed dispensing mechanism is connected to the feed conduit and comprises a housing and a paddle contained within the housing. The housing also comprises a feed connector that connects to the feed conduit. The feed conduit is configured to deliver feed to the paddle through the feed connector, and an agitator connected to the paddle is configured to prevent feed from flowing through the feed conduit when the paddle is not moving and to enable feed to flow through the feed conduit to the paddle when the paddle is moving.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 depicts a front view of a housing of an embodiment of the present invention.
FIG. 2 depicts a rear view of the housing depicted in FIG. 1 .
FIG. 3 depicts the housing depicted in FIG. 1 pivoted about a hinge to display the left and right sides of the housing.
FIG. 4 depicts a left side of the housing depicted in FIG. 1 .
FIG. 5 depicts a front and side view of a bracket used with the embodiment of the present invention depicted in FIG. 1 .
FIG. 6 depicts a front and side view of a motor-mount used with the embodiment of the present invention depicted in FIG. 1 .
FIG. 7 depicts an assembly view of an agitator and paddle used with the embodiment of the present invention depicted in FIG. 1 .
FIG. 8 depicts a top and front view of a paddle used with the embodiment of the present invention depicted in FIG. 1 .
FIG. 9 depicts an electric motor used with the embodiment of the present invention depicted in FIG. 1 .
FIG. 10 depicts a feed dispensing mechanism in accordance with the embodiment depicted in FIG. 1 .
DETAILED DESCRIPTION OF THE INVENTION
An improved game feeder and feed dispensing mechanism are described. In the following description, for the purposes of explanation, numerous specific details are set forth in order to provide a thorough understanding of the present invention. It will be apparent, however, to one skilled in the art that the present invention may be practiced without these specific details. In other instances, well-know structures and devices are shown in blocked-diagram form in order to avoid unnecessarily obscuring the present invention.
Current feed dispensing mechanisms allow direct access to the feed source and must be kept away from wild animals. The present invention prevents wild animals from accessing feed through the feed dispensing mechanism without requiring that the feed dispensing mechanism be kept out of wild animals' reach.
FIG. 1 depicts a housing 100 utilized with an embodiment of the present invention. The housing 100 comprises two halves, 306 and 308 (see FIG. 3 ), attached by a hinge 202 (see FIG. 2) and are held together in the closed position through internal resistance of the hinge 202 . Housing 100 is made using a rigid material, for example, metal, plastic, wood, lucite, fiberglass, etc. Housing 100 also comprises a feed connector 102 . The feed connector 102 is a structure that is configured to attach a feed conduit 1004 / 1002 (see FIG. 10) to the housing 100 .
Housing halves 306 and 308 are separable, or movably connected to one another, in order to permit a paddle 800 to be placed in the interior of housing 100 . The paddle depicted in FIG. 8 comprises a disc 802 with fins 804 attached to one face of the disc 802 . The fins 804 are attached to the disc 802 by rivets 806 . Fins 804 can also be attached in any other manner, for example, by welding, screws, gluing, or can be formed integrally as part of disc 802 . An aperture 808 in the center of disc 802 allows the paddle 800 to be attached to driveshaft extension 702 (see FIG. 7) as described in detail below. Paddle 800 is placed between housing halves 306 and 308 so that the fins 804 project towards housing half 308 . Paddle 800 is made using a rigid material, for example, metal, plastic, wood, lucite, fiberglass, etc.
Referring to FIG. 7, attachment of the paddle 800 to the driveshaft extension 702 is described. For clarity, the housing 100 is not shown, however paddle 800 is placed proximate to housing half 306 so that the face of disc 802 without fins 804 thereon is adjacent the interior portion of housing half 306 . Nut 710 is spun onto the threaded portion 708 of driveshaft extension 702 . Driveshaft extension 702 is then inserted, threaded portion 708 first, through aperture 302 (see FIG. 3) in housing half 306 , then through aperture 808 (see FIG. 8) in paddle 800 . The nut 710 can be spun along the threaded portion 708 of driveshaft extension 702 to adjust the projection of driveshaft extension 702 through housing half 308 and paddle 800 . Nut 710 directly contacts paddle 800 . Once the driveshaft extension 702 has been properly adjusted using nut 710 , nut 712 is spun onto the threaded portion 708 of driveshaft extension 702 and tightened against paddle 800 in order to lock paddle 800 into place. Driveshaft extension 702 is made using a rigid material, for example, metal, plastic, wood, lucite, fiberglass, etc., as are the nuts 710 and 712 .
Still referring to FIG. 7, an agitator 700 is attached to driveshaft extension 702 . The agitator 700 comprises an elongate, flexible portion 706 and an attachment portion 704 . In the depicted embodiment, attachment portion 704 is a nut that is spun onto threaded portion 708 of driveshaft extension 702 . Agitator 700 is made using a material that undergoes plastic deformation, i.e., will bend and return to its original position and shape once the bending force has been removed, for example, spring steel, plastics, rubber, etc.
Once paddle 800 , agitator 700 and driveshaft extension 702 have been assembled, or otherwise placed together, housing halves 306 and 308 are brought together. Housing halves 306 and 308 may be fastened to one another, but such fastening is not required.
Referring to FIGS. 6 and 10, motor-mount 600 is attached to housing half 306 . Apertures 604 in flange 602 are aligned with apertures 304 (see FIG. 3) on housing half 306 . Screws, rivets or other fasteners are passed through apertures 304 / 604 to secure motor-mount 600 to housing half 306 . The inner portion 610 of motor-mount 600 is dimensioned to allow driveshaft extension 702 to pass therethrough. Driveshaft extension 702 rotates within portion 610 . Grease can be used to reduce friction between portion 610 and driveshaft extension 702 . Motor-mount 600 is made using a rigid material, for example, metal, plastic, wood, lucite, fiberglass, etc.
Referring to FIGS. 7 and 9, driveshaft extension 702 is attached to an electric motor 900 . The non-threaded end of driveshaft extension 702 is affixed to the driveshaft 904 of electric motor 900 , for example, using a press fit or internal threads in a bore in the non-threaded end of driveshaft extension 702 and a threaded driveshaft 904 (preferably the threaded connection is such that when electric motor 900 turns driveshaft 904 the load on driveshaft extension 702 tightens the connection). When driveshaft extension 702 is connected to driveshaft 904 , flange 608 (see FIG. 6) is placed against electric motor 900 . Motor-mount 600 is attached to electric motor 900 by flange 608 just as flange 602 is attached to housing half 306 , or in any well-known manner.
Referring to FIGS. 5 and 10, the housing/motor assembly described above is attached to a feed source 1006 . Bracket portion 502 , which is T-shaped, is attached to the bottom of feed source 1006 in any well-known manner, for example, using screws 508 , or bolts, rivets, welds, glue, etc. Bracket portion 506 is placed over motor-mount 600 and then fastened to bracket portion 502 in any well-known manner, for example, using bolts 510 , or screws, rivets, welds, glue, etc. Bracket 1010 is attached to bracket 500 in any well-known manner, for example, welds, rivets, screws, bolts, glue, etc. Bracket 1010 contains a power source and controller 1000 such as a battery and timer, or other power source for electric motor 900 and controller, such as a simple computer. Power source and controller 1000 is connected to electric motor 900 in any well-known manner. Brackets 500 and 1010 are made using a rigid material, for example, metal, plastic, wood, lucite, fiberglass, etc.
Referring to FIG. 10, feed from feed source 1006 is connected to the housing/motor assembly through a feed conduit comprising fitting 1004 and elbow 1002 . Fitting 1004 is attached to the bottom of feed source 1006 , for example, using threads, welds, glue, a flange and rivets/screws, etc. An aperture in the bottom of feed source 1006 opens the interior of feed source 1006 to the interior of fitting 1004 . Elbow 1002 is attached to fitting 1004 in any well-known manner, for example, using threads, welds, glue, a flange and rivets/screws, etc. Elbow 1002 is then attached to feed connector 102 in any well known manner, for example, using threads, welds, glue, a flange and rivets/screws, etc. allowing feed to flow from the interior of feed source 1006 into housing 100 .
Agitator 706 extends through housing 100 and feed connector 102 into elbow 1002 . When electric motor 900 is off, agitator 706 prevents feed from flowing out of feed source 1002 , through fitting 1004 , elbow 1002 , feed connector 102 and housing 102 . Agitator 706 does not need to project all the way through feed connector 102 as long as it prevents feed from flowing. Because the feed is held in place by the agitator 706 in elbow 1002 , it is safely out of reach of wild animals who would have to reach through housing 100 , feed connector 102 and into elbow 1002 in order to reach the feed. A lid (not shown) on top of feed source 1006 prevents access by wild animals through the top of the game feeder.
When the controller in 1000 activates the power source in 1000 and causes electric motor 900 to start, agitator 706 turns, vibrates and loosens the feed within elbow 1002 /feed connector 102 . The turning and vibrating of agitator 706 causes feed to flow into housing 100 . Because electric motor 900 is on, paddle 800 is also turning and disperses the feed out of housing 100 in a substantially linear pattern.
The feed dispensing mechanism depicted in FIG. 10 is easily attached to the bottom of a feed source 1006 (for example a 50 gallon drum, a 5 gallon bucket or other container for holding feed) and does not project far below the bottom of the feed source 1006 (less than 6 inches). Because wild animals cannot reach the feed through the feed dispensing mechanism, there is no need to support feed source 1006 high above the ground. All that is needed is enough clearance for the feed dispensing mechanism, ideally ½ a foot to 2 feet. Feed source 1006 is supported using any well-known structure (not shown) such as legs, a cylindrical structure with a cut out to allow feed dispensing, etc.
In alternate embodiments, the housing halves 306 and 308 are held together using any mechanism that does not interfere with the paddle 800 (see FIG. 8) that is surrounded by the housing 100 . For example, clasps, buckles, VELCRO, posts on one half that mate with holes in the other half, etc. are used to secure housing halves 306 and 308 together. Additionally, the housing halves 306 and 308 do not need to be held together as the assembled feed dispensing mechanism will hold the housing halves 306 and 308 together.
In another embodiment, the housing halves 306 and 308 are not hinged together, but are releasable with respect to one another in order to permit access to the interior of housing 100 .
In other embodiments the paddle comprises a series of flattened spokes attached about a hub.
In yet other embodiments, the feed connector 102 ranges from a fitting as depicted in FIG. 1 to a series of apertures that permit a feed conduit 1004 / 1002 to be attached to the housing 100 .
Further embodiments comprise a driveshaft extension 702 attached to paddle 800 in other manners from that described above. For example, a small flange welded onto driveshaft extension 702 , or formed as part of driveshaft 702 , that fits through aperture 302 is used to either weld paddle 800 to the flange, or attach paddle 800 with fasteners such as rivets or screws. Paddle 800 is welded directly to driveshaft extension 702 or formed integrally with driveshaft extension 702 in other embodiments, which then requires insertion of driveshaft 702 through housing half 308 in a manner reverse to that described above.
In other alternate embodiments, attachment portion 704 is welded or otherwise attached to driveshaft extension 702 . Alternatively, agitator 700 is formed integrally with driveshaft extension 702 .
In further embodiments, motor-mount 600 is attached to housing half 306 in any well-known manner, for example studs on the housing half 306 are passed through apertures 604 and used to secure flange 602 , or flange 602 is welded or glued to housing half 306 . In additional embodiments, ball bearings are inserted within portion 610 to reduce friction between portion 610 and driveshaft extension 702 .
In yet other embodiments, power sources and motors other than a battery and an electric motor are used. For example, a fuel-cell, solar cells and electric motor, etc.
Other, alternate embodiments utilize any conduit structure that conveys feed from the feed source 1006 to the feed dispensing mechanism. For example, flexible hosing, piping, etc. Conduit materials include rigid materials such as polyvinylchloride (PVC), metal, plastics, wood, etc., and flexible materials such as rubber, polyethelyne, etc.
A game feeder according to the present invention can be placed close to the ground and have the feed dispersed in a predictable manner. This allows a game feeder according to the present invention to be easily concealed, to be easily filled, and easily set up. Because the direction of the feed dispersion is known, a game feeder according to the present invention can be placed close to, or suspended from, flora without having the feed becoming accumulated in the flora.
While this invention has been described in connection with what is presently considered to the most practical and preferred embodiments, the invention is not limited to the disclosed embodiments, but on the contrary, is intended to cover various modifications and equivalent arrangements included within the spirit and scope of the appended claims. | A game feeder utilizes an improved feed dispensing mechanism that allows feed to enter the feed dispensing mechanism from the side. A game feeder utilizing the improved feed dispensing mechanism prevents access to the feed through the feed dispensing mechanism thereby eliminating the need to keep the game feeder out of the reach of wild animals. | 0 |
CROSS-REFERENCE TO RELATED APPLICATIONS
This application claims the benefit under 35 U.S.C. §119(e) of U.S. Provisional Application No. 61/476,847 filed Apr. 19, 2011, which application is incorporated herein by reference.
TECHNICAL FIELD
The present disclosure relates to an assembly for a torque converter that links a turbine to a damper assembly and eliminates a turbine hub. Specifically, a hardened plate links the turbine and the damper assembly and provides a surface to receive a thrust bearing.
BACKGROUND
Commonly owned U.S. Pat. No. 6,142,272 discloses a torque converter including a plate welded to a turbine shell and connected to cover plates for a damper assembly. A thrust bearing is located between the plate and a stator. The patent also discloses a turbine hub to which the damper assembly is connected. The turbine hub receives torque from the turbine or the damper assembly and transmits the torque to an input shaft for a transmission.
SUMMARY
According to aspects illustrated herein, there is provided an assembly for a torque converter, including: a damper assembly including a cover plate including a first plurality of openings, a flange, and at least one spring in contact with the flange and the cover plate; a turbine including at least one first blade and a shell including a portion disposed radially inward of the at least one blade, and a second plurality of openings in the portion; a turbine plate with a third plurality of openings; and a plurality of fasteners passing through the first, second, and third pluralities of openings. The plurality of fasteners: fixedly secure the cover plate, the portion of the turbine shell, and the turbine plate to one another; or fixed securing the portion of the turbine shell to the turbine plate and restricting rotation of the cover plate with respect to the portion of the turbine shell to the turbine plate.
According to aspects illustrated herein, there is provided a torque converter, including: a turbine including at least one first blade and a shell including a portion disposed radially inward of the at least one blade, and a first plurality of openings in the portion; an impeller with at least one second blade; a stator with at least one third blade, the stator axially disposed between to the turbine and the impeller; a damper assembly including a cover plate including a second plurality of openings, a flange, and at least one spring in contact with the flange and the cover plate; and a turbine plate assembly including: a turbine plate with a third plurality of openings; a plurality of fasteners passing through the first, second, and third pluralities of openings and fixedly securing the portion of the turbine shell to the turbine plate; and a resilient element in contact with the plurality of fasteners and the cover plate and urging the cover plate toward the turbine plate. The torque converter includes a bearing axially disposed between the turbine plate and the stator and in contact with the turbine plate and the stator to enable relative rotation of the turbine shell with respect to the stator. A radially inner circumference of the turbine plate is in contact with the flange to radially center the turbine with respect to the flange. Torque from the turbine is transmitted from the portion of the turbine shell to the cover plate through the plurality of fasteners and from the cover plate to the flange of the damper through the at least one spring. The portion of the turbine shell and a radially outward portion of the turbine plate are aligned in an axial direction. For each fastener in the plurality of fasteners, a first portion of said each fastener passing through the cover plate has a first diameter. Each opening in the first plurality of openings has a radial extent and a circumferential extent each greater than the diameter such that relative rotation of the cover plate and the plurality of fasteners is enabled.
According to aspects illustrated herein, there is provided a torque converter, including: a turbine including at least one first blade and a shell including a portion disposed radially inward of the at least one blade, and a first plurality of openings in the portion; an impeller with at least one second blade; a stator with at least one third blade, the stator connected to the turbine and the impeller; a damper assembly including a cover plate including a second plurality of openings, a flange, and at least one spring in contact with the flange and the cover plate; and a turbine plate assembly including: a turbine plate with a third plurality of openings; and a plurality of fasteners passing through the first, second, and third pluralities of openings and fixedly securing the portion of the turbine shell to the turbine plate. The torque converter includes a bearing axially disposed between the turbine plate and the stator and in contact with the turbine plate and the stator to enable relative rotation of the turbine shell with respect to the stator. Torque from the turbine is transmitted from the portion of the turbine shell to the cover plate through the plurality of fasteners and from the cover plate to the flange of the damper through the at least one spring. The portion of the turbine shell and a radially outward portion of the turbine plate are aligned in a radial direction. A radially inner circumference of the turbine plate is in contact with the flange to radially center the turbine with respect to the flange; or the turbine plate assembly includes a seal element sealed against a radially inner circumference of the turbine plate and arranged to seal against an input shaft for a transmission.
BRIEF DESCRIPTION OF THE DRAWINGS
Various embodiments are disclosed, by way of example only, with reference to the accompanying schematic drawings in which corresponding reference symbols indicate corresponding parts, in which:
FIG. 1A is a perspective view of a cylindrical coordinate system demonstrating spatial terminology used in the present application;
FIG. 1B is a perspective view of an object in the cylindrical coordinate system of FIG. 1A demonstrating spatial terminology used in the present application; and,
FIG. 2 is a partial cross-sectional view of a torque converter with a turbine plate assembly;
FIG. 3 is a front view generally along line 3 - 3 in FIG. 2 ;
FIG. 4 is a partial cross-sectional view of a torque converter with a turbine plate assembly;
FIG. 5 is a front view generally along line 5 - 5 in FIG. 4 ;
FIG. 6 is a partial cross-sectional view of a torque converter with a turbine plate assembly;
FIG. 7 is a back view generally along line 7 - 7 in FIG. 6 .
DETAILED DESCRIPTION
At the outset, it should be appreciated that like drawing numbers on different drawing views identify identical, or functionally similar, structural elements of the disclosure. It is to be understood that the disclosure as claimed is not limited to the disclosed aspects.
Furthermore, it is understood that this disclosure is not limited to the particular methodology, materials and modifications described and as such may, of course, vary. It is also understood that the terminology used herein is for the purpose of describing particular aspects only, and is not intended to limit the scope of the present disclosure.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood to one of ordinary skill in the art to which this disclosure belongs. It should be understood that any methods, devices or materials similar or equivalent to those described herein can be used in the practice or testing of the disclosure.
FIG. 1A is a perspective view of cylindrical coordinate system 80 demonstrating spatial terminology used in the present application. The present invention is at least partially described within the context of a cylindrical coordinate system. System 80 has a longitudinal axis 81 , used as the reference for the directional and spatial terms that follow. The adjectives “axial,” “radial,” and “circumferential” are with respect to an orientation parallel to axis 81 , radius 82 (which is orthogonal to axis 81 ), and circumference 83 , respectively. The adjectives “axial,” “radial” and “circumferential” also are regarding orientation parallel to respective planes. To clarify the disposition of the various planes, objects 84 , 85 , and 86 are used. Surface 87 of object 84 forms an axial plane. That is, axis 81 forms a line along the surface. Surface 88 of object 85 forms a radial plane. That is, radius 82 forms a line along the surface. Surface 89 of object 86 forms a circumferential plane. That is, circumference 83 forms a line along the surface. As a further example, axial movement or disposition is parallel to axis 81 , radial movement or disposition is parallel to radius 82 , and circumferential movement or disposition is parallel to circumference 83 . Rotation is with respect to axis 81 .
The adverbs “axially,” “radially,” and “circumferentially” are with respect to an orientation parallel to axis 81 , radius 82 , or circumference 83 , respectively. The adverbs “axially,” “radially,” and “circumferentially” also are regarding orientation parallel to respective planes.
FIG. 1B is a perspective view of object 90 in cylindrical coordinate system 80 of FIG. 1A demonstrating spatial terminology used in the present application. Cylindrical object 90 is representative of a cylindrical object in a cylindrical coordinate system and is not intended to limit the present invention in any manner. Object 90 includes axial surface 91 , radial surface 92 , and circumferential surface 93 . Surface 91 is part of an axial plane, surface 92 is part of a radial plane, and surface 93 is a circumferential surface.
FIG. 2 is a partial cross-sectional view of torque converter 100 with turbine plate assembly 102 .
FIG. 3 is a front view generally along line 3 - 3 in FIG. 2 . The following should be viewed in light of FIGS. 2 and 3 . Torque converter 100 includes damper assembly 104 including cover plate 106 with a plurality of openings 108 , flange 110 , and at least one spring 112 in contact with the flange and the cover plate. The torque converter also includes turbine 114 including at least one blade 116 and shell 118 including portion 120 disposed radially inward of blade 116 . Portion 120 also includes a plurality of openings 122 . Turbine plate assembly 102 includes turbine plate 126 with a plurality of openings 128 , and a plurality of fasteners 130 passing through the openings 108 , 122 , and 128 . Fasteners 130 fixedly secure cover plate 106 , portion 120 , and the turbine plate to one another.
In an example embodiment, radially inner circumference 132 of the turbine plate is in contact with the flange to radially center the turbine with respect to the flange. In an example embodiment, radially inner circumference 134 of the flange is arranged to contact input shaft 136 for a transmission (not shown) to radially center the flange with respect to the input shaft and to transmit torque to the input shaft as further described below.
In an example embodiment, radially inner circumference 135 of portion 120 of the turbine shell and radially outer circumference 138 of the turbine plate are aligned in a radial direction, advantageously minimizing an axial extent of the turbine plate assembly. In an example embodiment, openings 122 and 128 are at least partially aligned in a circumferential direction such that fasteners 130 are at a uniform radial distance R from axis of rotation 139 for the torque converter. Having fasteners 130 at a single radius reduces the radial space requirements for assembly 102 . For example, if respective fasteners for the turbine plate and portion 120 were at different radii, greater radial space would be needed to accommodate the two rings of fasteners. In an example embodiment, portion 120 includes a plurality of radially inwardly projecting protrusions 140 and the turbine plate includes a plurality of radially outwardly projecting protrusions 142 . Protrusions 140 and 142 are interleaved. By interleaved, we mean that protrusions 140 and 142 are at least partially aligned in circumferential direction C and protrusions 140 and 142 alternate in direction C.
In an example embodiment, torque converter 100 includes impeller 144 with at least one blade 146 , stator 148 with at least one blade 150 , and bearing 152 . The stator is axially disposed between the turbine and the impeller, and the bearing is axially disposed between the turbine plate and the stator and in contact with the turbine plate and the stator to enable relative rotation of the turbine shell with respect to the stator. In an example embodiment, bearing 152 is a thrust bearing and axial force associated with axial displacement of the damper assembly or the turbine toward each other is transmitted to the bearing. The most radially inward segment of the portion of the turbine shell is radially outward of the bearing.
Advantageously, the configuration shown for torque converter 100 eliminates the need for a separate turbine hub to center the turbine and the damper assembly and to connect the turbine and the damper assembly to an input shaft. Eliminating the hub reduces the cost, size, weight, and complexity of the torque converter. For example, torque path 156 (for operation in torque converter mode) extends from the turbine to the input shaft via portion 120 , fasteners 130 , cover plate 106 , spring 112 , and the flange. In lock-up mode, torque path 158 extends from lock-up clutch 160 to the input shaft via at least one spring 162 , cover plates 106 and 164 , spring 112 , and the flange.
FIG. 4 is a partial cross-sectional view of torque converter 200 with turbine plate assembly 202 . Torque converter 200 includes damper assembly 204 including cover plate 206 with a plurality of openings 208 , flange 210 , and at least one spring 212 in contact with the flange and the cover plate. The torque converter also includes turbine 214 including at least one blade 216 and shell 218 including portion 220 disposed radially inward of blade 216 . Portion 220 also includes a plurality of openings 222 . Turbine plate assembly 202 includes turbine plate 226 with a plurality of openings 228 , and a plurality of fasteners 230 passing through the openings 208 , 222 , and 228 . Fasteners 230 fixedly secure cover plate 206 , portion 220 , and turbine plate 226 to one another.
Assembly 224 includes seal element 232 sealed against radially inner circumference 234 of turbine plate 226 and arranged to seal against input shaft 236 for a transmission (not shown). Radially inner circumference 238 of cover plate 206 is in contact with portion 240 of flange 210 and radially inner circumference 242 of the flange is arranged to contact input shaft 236 to radially center the flange and cover plate 206 with respect to the input shaft and to transmit torque to the input shaft as further described below.
In an example embodiment, radially inner circumference 243 of portion 220 of the turbine shell and radially outer circumference 244 of the turbine plate are aligned in a radial direction, advantageously minimizing an axial extent of the turbine plate assembly. In an example embodiment, openings 222 and 228 are at least partially aligned in circumferential direction C such that fasteners 230 are at a uniform radial distance R from axis of rotation 245 for the torque converter. In an example embodiment, portion 220 includes a plurality of radially inwardly projecting protrusions 248 and the turbine plate includes a plurality of radially outwardly projecting protrusions 250 . Protrusions 248 and 250 are interleaved. By interleaved, we mean that protrusions 248 and 250 are at least partially aligned in circumferential direction C and protrusions 248 and 250 alternate in direction C.
In an example embodiment, torque converter 200 includes impeller 252 with at least one blade 254 , stator 256 with at least one blade 258 , and bearing 260 . The stator is connected to the turbine and the impeller, and the bearing is axially disposed between the turbine plate and the stator and in contact with the turbine plate and the stator to enable relative rotation of the turbine shell with respect to the stator. In an example embodiment, bearing 260 is a thrust bearing and axial force associated with axial displacement of the damper assembly or the turbine toward each other is transmitted to the bearing.
Advantageously, the configuration shown for torque converter 200 eliminates the need for a separate turbine hub to provide a seal, to center the turbine and the damper assembly, and to connect the turbine and the damper assembly to an input shaft. Eliminating the hub reduces the cost, size, weight, and complexity of the torque converter. For example, torque path 264 (for operation in torque converter mode) extends from the turbine to the input shaft via portion 220 , fasteners 230 , cover plate 206 , spring 212 , and the flange. In lock-up mode, torque path 266 extends from lock-up clutch 268 to the input shaft via plates 206 and 270 , spring 212 , and flange 210 .
FIG. 6 is a partial cross-sectional view of torque converter 300 with turbine plate assembly 302 .
FIG. 7 is a back view generally along line 7 - 7 in FIG. 6 . The following should be viewed in light of FIGS. 6 and 7 . Torque converter 300 includes damper assembly 304 including cover plate 306 with a plurality of openings 308 , flange 310 , and at least one spring 312 in contact with the flange and the cover plate. The torque converter also includes turbine 314 including at least one blade 316 and shell 318 including portion 320 disposed radially inward of blade 316 . Portion 320 also includes a plurality of openings 322 . Turbine plate assembly 302 includes turbine plate 326 with a plurality of openings 328 , and a plurality of fasteners 330 passing through the openings 308 , 322 , and 328 .
Segment 331 of portion 320 and segment 332 of turbine plate 326 are aligned in axial direction A 1 . Fasteners 330 fixedly secure portion 320 and turbine plate 326 to one another and restrict rotation of cover plate 306 with respect to portion 320 and turbine plate 326 . To enable the fixing of plate 306 and portion 320 , portion 334 of fasteners 330 , passing through the cover plate, is engaged with radial surface 336 of plate 306 . Portion 334 has a diameter D 1 and each opening 328 is in the form of a circumferentially curved slot with radial extent R 1 greater than D 1 and circumferential extent C 1 greater than D 1 . Thus, fasteners 330 have a limited degree of circumferential motion within openings 328 and with respect to turbine plate 326 and the turbine. Specifically, rotation of fasteners 330 , and turbine plate 326 and the turbine, is limited by contact of the fasteners with ends E 1 and E 2 of openings 328 . Assembly 324 also includes resilient element 338 which urges cover plate 306 in axial direction A 1 against turbine plate 326 , creating frictional contact, or hysteresis between cover plate 306 and turbine plate 326 , which is beneficial to the operation of damper assembly 304 . For example, the hysteresis can be used to tune the damper assembly to attenuate undesirable vibration.
In an example embodiment, radially inner circumferences 340 and 341 of the turbine plate and cover plate 306 , respectively, are in contact with flange 310 to radially center turbine 314 and cover plate 306 with respect to the flange. In an example embodiment, radially inner circumference 342 of the flange is arranged to contact input shaft 344 for a transmission (not shown) to radially center the flange with respect to the input shaft and to transmit torque to the input shaft as further described below.
In an example embodiment, torque converter 300 includes impeller 346 with at least one blade 348 , stator 350 with at least one blade 352 , and bearing 354 . The stator is connected to the turbine and the impeller, and the bearing is axially disposed between the turbine plate and the stator and in contact with the turbine plate and the stator to enable relative rotation of the turbine shell with respect to the stator. In an example embodiment, bearing 354 is a thrust bearing and axial force associated with axial displacement of the damper assembly or the turbine toward each other is transmitted to the bearing.
Advantageously, the configuration shown for torque converter 300 eliminates the need for a separate turbine hub to center the turbine and the damper assembly and to connect the turbine and the damper assembly to an input shaft. At the same time assembly 302 provides the desired frictional and rotational contact between cover plate 306 and turbine plate 326 . Eliminating the hub reduces the cost, size, weight, and complexity of the torque converter. For example, torque path 356 (for operation in torque converter mode) extends from the turbine to the input shaft via portion 320 , fasteners 330 , cover plate 306 , spring 312 , and the flange. In lock-up mode, torque path 358 extends from lock-up clutch 360 to the input shaft via at least one spring 362 , cover plates 106 and 364 , spring 112 , and the flange.
The following should be viewed in light of FIGS. 2 through 7 . Advantageously, when turbine shell 118 , 218 , or 318 is formed by a stamping process, the respective turbine plate can be formed from the portion of the blank for the turbine shell left over from the stamping process, reducing cost for the turbine plate. Since a separate stamping operation with its attendant costs and complexities is not required, using the left over portion even further reduces costs and complexity for the turbine plate.
Advantageously, the turbine shell and the turbine plate shown in the figures can be subjected to differing fabrication processes once the pieces are formed by stamping. For example, it is usually not necessary to harden the turbine shell because of the added “rib” strength from the plurality of blades. Furthermore, if hardened, the shell would likely lose much of the strength gained during exposure to the elevated temperatures necessary to braze the blades. On the other hand, the turbine plate acts as a receiving surface for a thrust bearing and it is desirable to harden the turbine plate, for example, by heat treating, so that the turbine plate has better wearing properties. If the receiving surface for the bearing and the turbine shell are formed of a single piece, the wearing properties of the plate would be sacrificed during the turbine manufacturing process. Further, if a receiving surface for a thrust bearing is integral to the shell, characteristics of the receiving surface can be undesirably modified by the brazing oven, for example, the receiving surface can be distorted. Advantageously, by the use of a separate turbine plate, the turbine plate can be withheld from the brazing oven when the turbine is formed.
Although torque converters 100 , 200 , and 300 , and assemblies 102 , 202 , and 302 have been shown with respective particular configurations of components, it should be understood that torque converters 100 , 200 , and 300 , and assemblies 102 , 202 , and 302 are not limited to the respective particular configuration of components shown and that other respective configurations of components are possible.
It will be appreciated that various of the above-disclosed and other features and functions, or alternatives thereof, may be desirably combined into many other different systems or applications. Various presently unforeseen or unanticipated alternatives, modifications, variations, or improvements therein may be subsequently made by those skilled in the art which are also intended to be encompassed by the following claims. | A torque converter, including: a damper assembly including a cover plate including a first plurality of openings, a flange, and at least one spring in contact with the flange and the cover plate; a turbine including at least one first blade and a shell including a portion disposed radially inward of the at least one blade, and a second plurality of openings in the portion; a turbine plate with a third plurality of openings; and a plurality of fasteners passing through the first, second, and third pluralities of openings. The plurality of fasteners: fixedly secure the cover plate, the portion of the turbine shell, and the turbine plate to one another; or fixed securing the portion of the turbine shell to the turbine plate and restricting rotation of the cover plate with respect to the portion of the turbine shell to the turbine plate. | 5 |
FIELD OF THE INVENTION
The invention relates to a method and apparatus for perforating a liner of an oil or gas production well and for subsequently fracturing an underground formation surrounding the liner.
BACKGROUND OF THE INVENTION
In may well completion operations it is not possible to install a slotted liner at the well intake. In those situations it is common practice to install an unslotted liner in the well, and subsequently perforating the liner using a perforation gun. Such a gun contains a mass of explosives which shoot perforations through fragile spots of the liner. After retrieval of the gun from the well the formation surrounding the perforation may be fractured by pumping a fluid at an elevated pressure through the perforations into the formation.
The conventional perforating and fracturing procedures are time consuming. They also involve the risk that during or after the shooting of perforations well fluids enter the reservoir formation thereby causing formation impairment.
It is an object of the present invention to provide a method and apparatus for perforating a well liner and subsequently fracturing an underground formation surrounding this liner which remedy the above-mentioned drawbacks of the conventional perforation and fracturing procedures.
SUMMARY OF THE INVENTION
The method according to the invention comprises: inserting into a well a liner having along at least a selected interval of its length a series of fragile spots; lowering through the liner a perforating and fracturing tool comprising a pipe string which carries at its outer surface a pair of packers and which has at least one port in the area between the packers, the pipe being equipped near its lower end with a bottom valve for closing off the pipe interior at a location below the packers; positioning the tool in the liner such that the packers span at lest one of said spots; closing the bottom valve; spotting a fluid via the pipe and the ports into an annular space around the pipe and between the packers, thereby perforating each fragile spot of the liner around said annular space; injecting fluid at an elevated pressure into the pipe, thereby actuating the packers to form fluid tight seals adjacent said annular space and creating fractures in the formation surrounding each perforated spot; and reducing the fluid pressure in the pipe, annular space and fractures.
The apparatus according to the invention comprises: a pipe string which can be lowered through the well liner; a pair of packers being mounted at a selected mutual distance on the outer surface of the pipe; at least one port formed in the pipe wall in the area between the packers; and a bottom valve being arranged near a lower end of the pipe for closing off the pipe interior below the packers.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a longitudinal view of a well in which an apparatus according to the invention is located.
FIG. 2 shows in larger detail a section of the well and of the tool shown in FIG. 1.
DETAILED DESCRIPTION OF THE INVENTION
Referring now to FIG. 1 there is shown a well with a horizontal lower section in which a well liner 1 is arranged. The well extends from the earth surface into an oil and/or gas containing reservoir formation which surrounds the liner 1.
A perforating and fracturing tool 2 has been lowered into the well through a blow out preventer at the well head 3. The tool 2 comprises an elongate pipe 4 which is equipped with bell nipple 5 for a production safety valve, two packers 7, 8, and a bottom valve 9, and a latching sub 10 which carries a hydraulically actuated packing plug 11.
As shown in FIG. 2 the pipe 4 contains ports 20 in the area between the packers 7 and 8. The ports 20 create fluid communication between the pipe interior 21 and an annular space 22 between the pipe 4 and the liner 1 in the area between the packers 7 and 8. The packers 7 and 8 are secured to the pipe by clamp rings 24 in which openings 25 are arranged via which the pressure within the annular space 22 may enter the inner surface of the elastomeric sliding or fixed packers 7 and 8 so as to inflate the packers to form fluid tight seals in response to pressurizing the pipe interior 21.
A one way valve 27 is mounted near the uppermost packer 7 for enabling fluid to flow from the annulus 28 between the liner 1 and the section of the pipe above the packer 7 into the annular space 22. A hydraulic conduit 29 for actuating the bottom vale 9 passes through the annulus 28, the annular space 22, and the pipe wall underneath the packers 7 and 8.
In the context of this specification "lower" parts of the well and the tool are parts having a larger distance to the wellhead, when measured along the well path than "upper" parts of the well and the tool. Accordingly the uppermost packer 7 is located closer to the wellhead 3 than the lowermost packer 8.
The liner 1 consists of a steel tubular body in which a series of fragile spots 30 are present throughout its length. In the embodiment shown the spots 30 are created by machining cup-shaped recesses 31 at regular intervals into the outer surface of the body. If desired the fragile spots 30 may be formed by aluminum or other acid soluble inserts (not shown) which can perform as shear discs and which can be dissolved by an acid.
The normal operation of the apparatus is as follows. Before running the apparatus into the well the liner 1 has been cleaned up, tagged, and gauged and the well has been filled with a non-water based liquid.
The tool is then lowered into the well until the packing plug 11 has reached the bottom of the well. The tool may then be pulled to position the packers 7 and 8 such that they span at least one of the fragile spots 30. Then the bottom valve 9 is closed. If the fragile spots 30 consist of acid soluble discs they can be dissolved by lowering a coiled tubing through the interior of the pipe 4 via which acid is spotted into the pipe interior and the annular space 22 between the packers 7 and 8 in order to dissolve the discs. After spotting the acid fluid in injected at elevated pressure into the pipe interior 21. The resulting positive pressure difference between the annular space 22 between the packers 7 and 8 and the other annuli around the pipe 4 will cause the packers to expand and to form fluid tight seals against the inner surface of the liner. At the same time a positive pressure difference is created between the annular space 22 and the pores of the surrounding reservoir formation. This causes the remaining parts of the possibly only partly dissolved discs to be sheared and fractures to be formed in the formation around the sheared discs in the area between the packers 7 and 8.
The fluid which is injected at elevated pressure via the pipe interior 21 into the fractures may contain an acid in order to etch channels in the formation and/or a propping agent, such as sand, for forming a permanently permeable core inside the fractured channels.
After this the pressure in the pipe interior 21 and annular space 22 is reduced which causes the packers 7 and 8 to be released from the wall of the liner 1 and at lest part of the fracturing fluid and propping agent to be produced back into the well. As the returned fracturing fluid, which may contain formation particles, and the returned propping agent may contaminate the well interior they are preferably subsequently flushed away by pumping a cleaning fluid at an elevated pressure into the annulus 28 which causes the one way valve 27 to open and cleaning liquid to circulate down through the annulus 28, one way valve 27 into the annular space 22 and subsequently up via the ports 20 and the pipe interior 21.
At this moment a production test can be carried out after which a decision can be made to fracture again, to leave it as it is, to further etch channels by acidizing or to close the created fractures by pumping cement into the created fractures.
Then the tool 2 is pulled until the packers span other fragile spots 30 than the already removed spots and the cycle of spotting acid to dissolve the discs, elevating the pressure in the pipe interior 21 and annular space 22 so as to fracture the formation, reducing the pressure again, and optionally injecting propping agent into the fractures and flushing a cleaning fluid through the well is repeated again one or more times until the whole interval of the liner where fragile spots are present has been perforated.
It will be appreciated that the procedure according to the invention enables perforating a small section of the liner and subsequently fracturing the formation surrounding this section of the liner. This procedure of perforating the liner section by section enables an accurate control of the fracturing process which is particularly important of the liner has a large length, which is usually the case in a horizontal or nearly horizontal well.
After the required number of liner perforations and formation fractures has been made the pipe is pulled up through the well and the temporary packing plug 11 is set at the top of the perforated liner by actuating the latching sub 10. Then the pipe 4 is removed from the well.
The well can now be completed with a permanent packer and production tubing, whereupon the well may be circulated to nitrogen to allow the temporary packer to open and to allow oil and/or gas to flow through the perforated liner and fractures in the surrounding formation. | A liner at the bottom of an oil or gas well is perforated and the surrounding formation is subsequently fractured by inserting into the liner a perforating and fracturing apparatus comprising a pair of packers that can be positioned around fragile spots of the liner, and subsequently injecting a fluid or fluids at an elevated pressure into the area between the packers in order to perforate the liner at the locations of the fragile spots and to create fractures in the formation surrounding these spots. | 4 |
BACKGROUND OF THE INVENTION
1. Field of the Invention
This invention relates to improvements in concrete mixing apparatus and more particularly, but not by way of limitation, to a concrete batch plant adapted for either stationary or portable operation.
2. Description of the Prior Art
Many sites wherein concrete is to be poured are located a substantially great distance from the concrete plant, and it is the usual practice to load a concrete mixer vehicle at the plant site and mix the concrete batch in the vehicle mounted mixer during transport to the remote site. This procedure has disadvantages in that it is usually desirable to mix the concrete batch for a particularly selected time period in order to assure an efficient end product, and there is also usually an optimum time for dumping the mixed concrete into the forms, or the like, to insure that the concrete does not "set up" or begin to harden before the pouring and spreading operation can be completed. The time of travel of the mixer vehicle from the plant site to the ultimate use location may vary greatly, depending upon conditions which may be completely out of the control of the operator of the vehicle, such as snarled traffic conditions, vehicle break down, and the like. In addition, there are many instances wherein a plurality of concrete batches may be required, with some of the batches being smaller than other batches, which is difficult and expensive to arrange with present day methods and means.
SUMMARY OF THE INVENTION
The present invention contemplates a concrete batch plant which may be transported to or near the site wherein the concrete is to be utilized. The novel apparatus comprises a main cement storage bin or silo, a water weigh bin, a cement weigh bin, and an aggregate weigh bin mounted on support means which may be transported by a wheeled vehicle, or the like, from site to site in accordance with the location wherein it is desired to utilize concrete. The support means is disposed in a substantially horizontal position during transporting thereof, and is elevated to a substantially vertical position for operation thereof during a concrete batching operation. The cement storage bin or silo is in communication with the cement weigh bin through any suitable means whereby a preselected quantity of the dry cement may be deposited within the cement weigh bin according to weight. A preselected quantity of water is deposited in the water weigh bin in accordance with weight, said proportions being selected in accordance with the desired end result of the concrete mixture. The aggregate weigh bin is carried by a suitable lifting apparatus whereby the bin may be charged or loaded in a lowered position of the bin and discharged or dumped in a raised position of the bin. The aggregate bin is moved from the lowered position to the raised position by the same means which raises and lowers the support means, and is moved through an overhead arc whereby the bin remains in its normal upright position at all times, thus precluding accidental loss of material therefrom, and in the raised position thereof, the aggregate may be readily discharged into the mixer truck in accordance with the desired weight thereof. Of course, the truck mixer is utilized in the usual or well known manner for mixing the ingredients to provide the desired concrete batch.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a side elevational view of a portable concrete batch plant embodying the invention and depicted in the substantially horizontal transporting position thereof.
FIG. 2 is a side elevational view of a portable concrete batch plant embodying the invention and depicted in the raised operating position thereof, with portions shown in dashed lines for purposes of illustration.
DESCRIPTION OF THE PREFERRED EMBODIMENT
Referring to the drawings in detail, reference character 140 generally indicates a portable concrete batch plant comprising a cement silo 142, a water weigh bin 144, a cement weigh bin 146, an aggregate weigh bin 148, and a mixer 147 of a usual concrete mixer type vehicle 149. The silo 142 may be of any suitable construction, and as shown herein is provided with a main housing portion 143 which may be either substantially cylindrical or of a rectangular cross-sectional configuration, and a lower portion 150 as viewed in FIG. 2 in intimate communication with the main portion 143. The portion 150 is provided with a tapered portion 152 extending between the main portion 143 and a discharge opening or outlet 154 having a suitable gate member 156 cooperating therewith for selectively discharging dry cement from the silo 142 in a manner as will be hereinafter set forth. One side plate 153 of the silo 142, and which is conterminous with the tapered portion 152, becomes a bottom plate in the horizontal position shown in FIG. 1. An upper plate 155 of a tractor fifth wheel (not shown) is welded or otherwise suitably secured to the plate 153 and a king pin 157 is welded to the plate 155 as is well known and for a purpose as will be hereinafter set forth. The silo 142 is secured to a pair of spaced first support beams 158 (only one of which is shown in the drawings), and a second pair of spaced support beams 160 (only one of which is shown in the drawings) in any suitable manner, such as by welding, or the like.
The support beams 158 and 160 are preferably mutually parallel and are spaced apart by suitable cross members generally indicated at 162 to provide a tower-type support structure for a purpose as will be hereinafter set forth. The beams 158 are pivotally secured at 164 to a pair of spaced support legs 166 (only one of which is shown in the drawings), and the legs 166 cooperate with a plurality of additional spaced support legs 168 which form a part of a framework 170 which supports the entire apparatus 140 as will be hereinafter set forth. In addition, each leg 166 and 168 is provided with an adjustable or telescopically arranged foot member 172 which may be selectively moved into engagement with the surface 174 of the ground, or elevated with respect thereto, as desired. A pair of axially aligned wheels 176 (only one of which is shown in the drawings) are suitably journalled on the frame 170 for supporting the apparatus 140 when the feet 172 are raised from engagement with the surface 174, and for providing portability for the apparatus 140 during transport thereof, as will be hereinafter set forth. A foot member 178 is adjustably or telescopically secured to the outer end of each of the support beams 160 for a purpose as will be hereinafter set forth.
The water weigh bin 144 may be of any suitable construction, and as shown herein is preferably of an elongated tank-type configuration secured to one of the beams 158 in any suitable manner (not shown), and preferably disposed inboard thereof, as shown in the drawings. A suitable discharge pipe 180, or the like, is provided at one end of the water weigh bin 144 and is provided with a suitable hose or conduit 182 extending therefrom for a purpose as will be hereinafter set forth. In addition, it is preferable to provide a suitable valve (not shown) or the like in combination with the discharge pipe 180 and/or hose 182 for selectively controlling the discharge of water from the bin 144. A suitable supply or filler means (not shown) is also provided for charging of the water bin 144 with water, and suitable load cells (not shown) are provided in conjuntion with the water weigh bin 144 and in operable connection with a central electronic weigh control system (not shown). Of course, any suitable electronic weigh control system may be utilized, but it is preferable to use the type known as the Weigh Systems Inc. system which includes a suitable control center or control box (not shown) conveniently mounted on the apparatus 140 for facilitating access thereto by the operator of the equipment, and suitable load cells connected between the water weigh bin, the aggregate weigh bin, the cement weigh bin and the control box. Prior to a concrete batching operation, the desired ratio of the components of the concrete by weight are dialed into the control box. In this manner, the actuation of the apparatus 140 is automatically controlled by the electronic system to provide optimum concrete batching in accordance with the desired end result.
The cement weigh bin 146 may be of any suitable type construction and as shown herein is of a tank-type construction rigidly secured to the other leg 150 oppositely disposed from the water weigh bin 144. One end of the cement weigh bin 146 is in communication with the cement silo 142 through a suitable delivery conduit 184, and the opposite end thereof is open for discharge of the contents thereof, but is provided with a suitable gate (not shown) for selective discharge of the contents from the cement weigh bin as is well known.
The aggregate weigh bin 148 may be of any suitable construction and as shown herein the upper end thereof is open for receiving material therein and the lower end thereof is provided with a suitable discharge gate member 186. In addition, it may be preferable to provide at least one angularly disposed bottom plate 187 for facilitating directing of the material within the bin 148 to the discharge gate 186, as is well known. The bin 148 is suitably suspended from three load cells (not shown) and a visual system (not shown) is provided in the electronic control system for indicating the percentage of filling of the bin 148, by weight, continually during loading of the aggregate bin 148 as will be hereinafter set forth.
The aggregate bin 148 is carried by a suitable support frame 188 which is pivotally secured at 190 to a beam 192 having the opposite end thereof pivotally secured at 194 to one of the support legs 166. A similar beam (not shown) is pivotally secured between the frame 188 and other support leg 166 in spaced aligned relation to the beam 192. A pair of removable strap members 196 (only one of which is shown) is pivotally secured between the frame 188 and the support beams 158 for a purpose as will be hereinafter set forth. A pair of suitable bracket members 197 (only one of which is shown) are provided on opposite sides of the frame 188 and the outer end of each bracket 197 is pivotally secured as shown at 198 to one end of an arm 200 (only one of which is shown). The opposite ends of the arms 200 are pivotally secured as shown at 201 to a pair of spaced blocks 202 rigidly secured to a portion 204 of the frame 170 in the proximity of the support legs 166. A pair of suitable hydraulic cylinders 206 (only one of which is shown) are pivotally secured between the frame 170 and the beams 192 whereby extension or expansion of the cylinders 206 will pivot the beams 192 in a counterclockwise direction about the pivot connections 194 as viewed in the drawings, and contraction of the cylinders 206 will pivot the beams 192 in a clockwise direction about the pivot points 194.
Of course, the cylinders 206 may be operably connected with a suitable fluid reservoir (not shown) and the fluid reservoir may be powered by a suitable motor and pump (not shown). Whereas the cylinders 206 are preferably hydraulic cylinders, it is to be understood that they may be pneumatic cylinders, if desired.
When the portable concrete plant 140 is to be transported along a highway, or the like, to the site wherein it is desired to produce concrete batches, the beams 158 and 160 are disposed in the horizontal position therefor as shown in FIG. 1, and the usual or standard type highway tractor vehicle (not shown) provided with a fifth wheel (not shown) is backed into a position whereby the fifth wheel is disposed beneath the silo 142 in order that the king pin 157 is engaged and locked in the fifth wheel in the usual or well known manner. Of course, the feet 172 may then be suitably retracted within the respective legs 168 whereby the wheels 176 are in engagement with the surface 174 of the ground, and the tractor may be moved forwardly in the usual manner for pulling the plant 140 along the highway.
When the apparatus 140 has reached the site wherein it is desired to produce concrete batches, the feet 172 may be set in place in the usual manner for engagement with the surface 174 of the ground, and for elevating the wheels 172 from engagement with the ground. The hydraulic cylinders 206 may then be activated in the usual manner for extending thereof in order that the beams 192 will be pivoted in a counterclockwise direction about the pivot points 194, as viewed in the drawings. The movement of the beams 192 is transmitted to the beams 158 through the connecting members 196, and the beams 158 are pivoted simultaneously with the beams 192. Of course, the cross members 162 cause the beams 160 to pivot simultaneously with the beams 158, and the pivoting may be continued until the lowermost end of the beams 158 rest against the uppermost ends of the support legs 166 as shown at 208 in FIG. 2. The feet 178 may then be extended and pinned or locked with respect to the beams 160 for engagement with the upper ends of the respective support legs 168 as shown in FIG. 2. In this manner, the apparatus 140 is supported in a vertical position, which is preferable during the batching operation.
It is to be noted that during the movement of the apparatus 140 from the horizontal position to the vertical position, the aggregate bin 148 remains in a substantially upright or vertical orientation due to the pivotal connection between the frame 188 and the beams 192. When the apparatus 140 has been raised or elevated to the vertical position, the removable straps 196 may be disconnected from the frame 188, and the cylinders 206 may be contracted whereby the beams 192 are pivoted in a clockwise direction about the pivot connections 194, as viewed in the drawings. The aggregate bin 148 is moved simultaneously with the beams 192 due to the pivotal connection of the frame 188 with the beams 192 until the bin 148 is lowered to the position shown in dashed lines in FIG. 2. It is again to be noted that the bin 148 will remain in the upright or vertical orientation thereof during both the raising and lowering thereof, and moves in an overhead arc during the raising and lowering whereby the accidental loss of the contents thereof is substantially eliminated.
In the lowered position of the bin 148, the sand and gravel may be loaded and weighed therein by the usual front end loader (not shown), or in any other suitable manner. As hereinbefore set forth, the aggregate bin 148 is suspended from three load cells (not shown) in any well known manner, and weighs at all times during operation of the apparatus. The operator of the loader (not shown) begins dumping gravel into the bin 148 while watching two rows of lights (not shown) provided on the side of the control housing of the electronic weighing system. When 80% of the desired quantity of gravel by weight, is accumulated within the bin 148, the first or bottom amber colored light automatically illuminates. When 90% of the quantity of gravel has accumulated within the bin 148, the second amber colored light illuminates. When 98% of the gravel has been loaded into the bin 148, the third amber light illuminates, and when 100% of the gravel has been loaded in the bin 148, the fourth or white light illuminates. Thus, the operator is provided with a visual indication of the progress of the loading operation. The loader operator then ceases the dumping of gravel into the bin 148, and starts dumping sand in the bin 148 on top of the gravel loaded therein. The operator watches the second row of lights and goes through the same sequence of 80%, 90%, 98% and 100% loading of the sand, by weight. When both white lights are on, the loader operator stops dumping sand into the bin 148, and preferably moves to a position away from the bin 148 in order that the bin 148 may be elevated from its loading position.
Subsequent to the loading or charging of the bin 148, the cylinders 206 may be extended for elevating the bin 148 to a position as shown in solid lines in FIG. 2 wherein the discharge gate 186 thereof will be in alignment with the charge hopper 210 of the mixer 147.
Of course, it is preferable to load or charge the cement silo 142 with dry bulk cement from a suitable tanker or tank truck (not shown). The dry bulk cement may be discharged from the silo 142 into the cement weight bin 146 by gravity through the discharge conduit 184. When the preselected quantity of cement, by weight, has been loaded into the cement weigh bin 146, the flow of cement from the silo 142 is stopped.
Water may be loaded into the water weigh bin 144 in any well known manner, such as through a hose from a suitable water source, with the flow of water to the bin 144 being stopped when the preselected weight of the water has been loaded therein. The weighed cement and weighed water may be discharged into the hopper 210 of the mixer 147 for discharge thereof into the mixer 147 as is well known. The sand may be measured, by weight, into the hopper 210 and discharged into the mixer 147, and the gravel may also be measured, by weight, into the hopper 210 for discharge into the mixer 147. The mixer 147 may then be operated in the usual manner for mixing a concrete batch from the ingredients which have been loaded therein. Of course, the concrete batch may be discharged from the mixer 147 for use in the usual manner.
When the apparatus 140 is to be transported to another site for further concrete batching operations, the strap members 196 may be replaced, and the cylinders 206 contracted for moving the apparatus 140 to the horizontal position therefor, whereupon the entire apparatus may be towed along the highway to the new site. It is to be noted that the cylinders 206 provide both the raising and lowering of the support frame and the raising and lowering of the aggregate bin.
From the foregoing it will be apparent that the present invention provides a novel portable concrete batching plant which may be moved from location to location, as desired, whereupon an entire concrete batching operation may be completed at the site wherein the concrete is to be used. The novel apparatus comprises a dry bulk cement silo, a water weigh bin, a cement weigh bin, an aggregate weigh bin mounted on a framework which permits transporting of the concrete batching plant from site to site. The aggregate bin is adapted for movement between a lowered position for loading thereof and a raised position for discharging the contents therefrom into the mixer whereby the cement, water and aggregate, all of which have been measured by weight ratios, may be mixed to provide the desired concrete batch or batches. The support frame is adapted to be raised to a vertical operating position, and is raised and lowered by the same elevating apparatus which raises and lowers the aggregate bin. Repeated concrete batches may be mixed at the site, as required, subsequent to which the entire portable plant may be moved to an additional site for producing still additional concrete batches.
Whereas the present invention has been described in particular relation to the drawings attached hereto, it should be understood that other and further modifications, apart from those shown or suggested herein, may be made within the spirit and scope of this invention. | A concrete batch plant designed and constructed for transport to the site wherein the concrete is to be used, said plant being disposed in a substantially horizontal position during transport thereof and in a substantially vertical position during operation thereof for producing concrete batches. The apparatus comprises cement storage means for storing a quantity of dry bulk cement therein, weigh bin means for receiving a preselected quantity of the dry cement from the cement storage means, water bin means for receiving a preselected quantity of water therein, aggregate weigh bin means for containing a quantity of aggregate therein and discharging the same in preselected quantities, and means for elevating the aggregate storage bin means from the charging or loading position to the dumping or discharging position for discharging the contents thereof into a suitable mixer means such as a Ready-mix truck, said elevating means also being utilized for elevating the apparatus from said horizontal position to said vertical position and return to horizontal position. Electronic means is also provided for automatic loading of the water weigh bin and cement weigh bin with said preselected quantities of material according to weight for the desired concrete mixture, as well as visual electronic means for loading of the aggregate weigh bin means. | 1 |
FIELD OF THE INVENTION
[0001] The present invention relates to printing industry field, and more particularly to a printing process and printing auxiliary agent used therein
BACKGROUND
[0002] Significant development has been made in printing technology since its origin as one of the Four Great Inventions in ancient China.
[0003] The present printing process generally includes the following steps: 1. substrate transport and printing preparation for single-color or multi-color printing process; 2. first color (or background color) printing: transfer the printing ink of a first printing station to the substrate by printing plate (or screen); 3. drying by forced or natural evaporation to remove water and organic solvents from the printing ink by heating, ventilation and so on; 4. second color printing: transferring the printing ink in a second printing station to the suitable positions of the substrate by printing plate (or printing screen) followed by drying; 5. performing other printing processes.
[0004] With regard to the current printing technology, poor surface flatness of substrates (e.g., paper, fabrics, nonwoven paper and plastic thin film) would directly influence the printing quality. As for substrates with rough surface, such as kraft paper, fabrics and nonwoven paper, the surface is generally not in complete contact with the printing plate, resulting undesirable consequences such as discontinuous and white leak after printing, significantly affecting printing precision and hindering further progress.
[0005] Generally, the problems mentioned above are solved by improving papermaking process to increase paper flatness. However, such measures increase manufacturing cost, yet not completely resolving the problems of printing quality.
[0006] The printing of nonwoven fabric material, a high-end product in architectural decoration industry, also encounter the same problems because such materials have irregular surface with fiber structure designed to catch people's eyes as elegant works of art. And yet it is exactly the surface irregularity that results in poor contact between the concave portion on the surface and the printing roller during substrate inking and therefore causes small breaks or large areas of white points in the printed portion, especially for patterns with dark background, greatly deteriorating the printing effect as a whole.
SUMMARY OF THE INVENTION
[0007] An object of the present invention is to overcome the defects of the prior art by providing a printing process and printing auxiliary agent used therein so as to solve the technical problems of the prior art, namely breaks, white leak or missing coating.
[0008] In order to solve the foregoing technical problems, the present invention adopts the following printing process.
[0009] The present invention disclosed a printing process including steps of mounting a plate, applying ink, conveying an object to be printed, and impressing. The printing auxiliary agent is applied on the substrate to be imprinted (i.e., the substrate waiting to be imprinted at the selected printing station) before the print impression points of any selected printing station. The printing auxiliary agent includes water and/or organic compounds that are liquid under normal conditions.
[0010] The process of plate mounting, inking, substrate transport and imprinting are performed by conventional procedures.
[0011] The term “printing station” refers to a unit on the printing press that has functions such as substrate transport, inking, imprinting and drying, and includes components such as printing plate, impression roller, inking device, drying device and transmission device. A printing press usually comprises one or more printing stations.
[0012] The term “print impression points” are the place at a printing station where the printing plate and impression roller contact with the substrate.
[0013] The printing auxiliary agent could be applied separately on the substrate, which means that the printing auxiliary agent is applied independently on the substrate, a way different from conventional method by which the printing auxiliary agent is required to be mixed as an auxiliary material into the printing ink to be applied on the substrate.
[0014] The process of applying the printing auxiliary agent on the substrate to be imprinted separately before the print impression points of any selected printing station, refers to any one of the following situations: for a printing process involving only one printing station, applying the printing auxiliary agent separately on part or whole of the substrate to be imprinted before the substrate to be imprinted reaches the print impression points of the printing station; or for a printing process involving multiple printing stations and one or more printing stations being selected, for each printing station selected, applying the printing auxiliary agent separately on part or whole of the part of the substrate that has not been imprinted at this specific printing station before the substrate that is not imprinted at said printing station reaches the print impression points of said printing station.
[0015] The method of independently applying a printing auxiliary agent on a substrate can be selected from printing, coating, spraying or immersion.
[0016] After being applied with a printing auxiliary agent, the substrate should be kept moist so as to have it imprinted at the selected printing station before the printing auxiliary agent applied being completely dried.
[0017] After being independently applied with a printing auxiliary agent, the impression procedure should be conducted with the total amount of the water and organic compounds which is liquid under normal conditions contained in the substrate being ranging from 0.5˜105 g/m 2 (that is, 0.5˜105 g per square metre of the substrate), preferably 2.5˜30 g/m 2 on substrate. This total amount of the water and organic compounds which is liquid under normal conditions contained in each square metre of the substrate refers as the “total retention amount”. For the substrates made of different materials, the preferable total retention amount may change on a slight basis. Such as, for nonwoven substrate, a preferable total retention amount is 1˜96 g/m 2 on substrate; as for textile substrate, a preferable total retention amount is 5˜105 g/m 2 on substrate; as for paper substrate, a preferable total retention amount is 1˜20 g/m 2 on substrate; as for plastic substrate, a preferable total retention amount is 0.5˜15 g/m 2 on substrate; as for rubber substrate, a preferable total retention amount is 0.5˜20 g/m 2 on substrate; as for ceramic substrate, a preferable total retention amount is 5˜50 g/m 2 on substrate. The control of the total retention amount can be realized by the application amount of printing auxiliary agent or by proper drying after application.
[0018] During the printing process of the present invention, the step of the printing, coating, spraying, or immersion of the printing auxiliary agent is arranged before the print impression points of the first printing station, and can be adjusted according to the printing pattern features and the sequence of each kind of single-color printing. The process can work effectively to the most extent when it is conducted before the step of imprinting at the printing station where missing printing or missing coating is most likely to occur. Moreover, the steps of printing, coating, spraying or immersion of the printing auxiliary agent is not limited to only once and, if necessary, further application may be made completely or partially at appropriate positions according to actual requirements.
[0019] Upon the completion of imprinting at all printing stations, various conventional steps, such as drying, solidification, trimming, slitting and packaging, can be performed subsequently.
[0020] In the present invention, the substrates can be various kinds of conventional substrates, including but not limited to nonwoven substrate, textile substrate, paper substrate, plastic substrate, rubber substrate, ceramic substrate and so on, such as kraft paper, newsprint paper, book paper, decorating paper, dowling paper, coated paper, wrapping paper, poster paper, deckle-edged paper, banknote paper, fiber fabrics, nonwoven fabrics, building board, floor tile and wall tile. The printing process of the present invention is particularly suitable for the foregoing substrates with uneven surface.
[0021] The printing process of the present invention can be applied to many printing fields, such as but not limited to, relief printing, gravure printing, permeographic printing (screen or rotary screen) and flexographic printing.
[0022] The key point for the printing process of the present invention lies in that a crucial printing auxiliary agent which can greatly enhance the printing ink transfer ratio is used before the step of imprinting at printing station.
[0023] The printing ink can be various kinds of conventional printing ink. The term of “printing ink” is a general concept of, for example but not limited to, solvent ink, water-based ink, ultraviolet (UV) ink and other liquid inks, and can be colored or colorless.
[0024] The printing auxiliary agent should meet the following features: Able to moisten the surface (layer) of substrate. Having appropriate volatility to enable proper drying condition as substrate is formally printed, therefore ensuring the improvement effect on printing. Having appropriate surface tension to support the printing ink and transfer the ink to the concave portion of substrate in time, therefore fulfilling the purpose of improving the printing quality.
[0025] The present invention provides a printing auxiliary agent meeting the features above, wherein said printing auxiliary agent comprises one or more of water and organic compounds that are liquid under normal conditions.
[0026] Said printing auxiliary agent could be, for example but not limited to, in forms of solution, suspension or emulsion.
[0027] Said printing auxiliary agent comprising water and/or organic compounds that are liquid under normal conditions means that, the printing auxiliary agent comprises water or organic compounds that are liquid under normal conditions, or the printing auxiliary agent comprises water and organic compounds that are liquid under normal conditions. For example, the printing auxiliary agent can be water, or only one kind of organic compound that is liquid under normal conditions, or more kinds of organic compounds that are liquid under normal conditions, and, of course, also can be water and one or more kinds of organic compounds that are liquid under normal conditions in combination simultaneously. Water and/or organic compounds that are liquid under normal conditions can be mixed in any ratio.
[0028] The sum of the weight percents of said water and organic compounds that are liquid under normal conditions is 50%-100%, preferably 70%-100%, and more preferably 80%-100%.
[0029] Preferably, the printing auxiliary agent is a homogeneous liquid.
[0030] The organic compounds that are liquid under normal conditions are organic solvents that are liquid under normal conditions. Organic solvents that are liquid under normal conditions are one or more selected from aromatic hydrocarbon, aliphatic hydrocarbon, alicyclic hydrocarbon, halide, alcohol, ether, ester, ketone, phenol and diol derivative that are liquid under normal conditions. For example, said organic solvents that are liquid under normal conditions can be one or more selected from methanol, ethanol, isopropanol, ethanediol, propanediol, diethylene glycol, dipropylene glycol, dipropylene glycol monomethyl ether, dipropylene glycol monoethyl ether, dipropylene glycol monopropyl ether, dipropylene glycol monobutyl ether, diethylene glycol monomethyl ether, diethylene glycol monoethyl ether, diethylene glycol monopropyl ether, diethylene glycol monobutyl ether, benzene, methylbenzene, dimethyl benzene, propanone, butanone, cyclohexanone, ethyl acetate, propyl acetate and butyl acetate. Each of the solvents listed above can be used individually with the printing quality of uneven substrate improved. The selected solvents could be mixed with each other and the mixture could also improve the printing quality of uneven substrate.
[0031] Said printing auxiliary agent can be further added with one or more of resin, cosolvent, surface active agent, antifoaming agent, screening agent and rheological agent according to requirements. Said printing auxiliary agent can comprise resin for printing ink use or not.
[0032] Preferably, said printing auxiliary agent is water, one kind of organic compound that is liquid under normal conditions, a homogeneous mixture of more kinds of organic compounds that are liquid under normal conditions, or a homogeneous mixture of water and one or more kinds of organic compounds that are liquid under normal conditions.
[0033] Printing auxiliary agents having water and/or organic compounds that are liquid under normal conditions can improve the printing quality of any kind of substrate with uneven surface. For optimal printing effect, the proportion of ingredients in printing auxiliary agent is not fixed and can be changed according to factors such as substrate properties, heating temperatures in printing machine, hot wind conditions, coating thickness, printing speed, and the space between coating and printing positions.
[0034] Printing auxiliary agents having multiple ingredients can be produced by uniformly mixing the selected ingredients according to the proportion.
[0035] The printing auxiliary agent and printing process in the present invention can be applied to the printing of various kinds of substrates, and is particularly suitable for the improvement of the printing quality of substrates. The inventor is surprised to find that the phenomenon of missing printing or missing coating can be effectively prevented or improved, without adjusting the original printing process sequence, simply by adding a step of independently applying a printing auxiliary agent with certain fluidity before the printing station where missing printing or missing coating occurs during pre-printing or before the printing station where missing printing or missing coating is expected to occur.
[0036] Said substrate is nonwoven substrate, fabric substrate, paper substrate, plastic substrate, rubber substrate, or ceramic substrate, such as kraft paper, newsprint paper, book paper, glazed paper, decorating paper, art paper, packing paper, poster paper, deckle-edged paper, banknote paper, fiber fabrics, nonwoven fabrics, building board, floor tile and wall tile.
[0037] Said printing auxiliary agent can improve the transfer of the printing ink on substrate and thus improving the problem of printing quality of substrate.
[0038] Improving the problem of printing quality of substrate refers to improving the quality problem of missing printing or missing coating occurring during the printing of substrate due to uneven surface.
[0039] Said printing auxiliary agent can be used before the print impression points of any selected printing station during the printing of various kinds of substrates.
[0040] Said printing auxiliary agent can be used in the following ways: before the print impression points of any selected printing station, a printing auxiliary agent alone is applied on substrate, wherein the application method can be selected from printing, coating, spraying or immersion.
[0041] Preferably, an additional step of independently applying a printing auxiliary agent on the substrate to be imprinted (i.e., substrate waiting to be imprinted at the selected printing station) before the print impression points of the printing station where missing printing or missing coating occurs during the original printing process.
[0042] After being applied with a layer of printing auxiliary agent, the substrate should be kept moist as much as possible so as to have it imprinted at the selected printing station without the printing auxiliary agent being completely dried.
[0043] After being independently applied with a printing auxiliary agent, the substrate is imprinted with the total retention amount of water and organic compounds that are liquid under normal conditions in printing auxiliary agent at 0.5-105 g/m 2 on substrate. As for substrates made of different material, the preferable total retention amount may change on a slight basis, wherein as for nonwoven substrate, a preferable total retention amount is 1-96 g/m 2 on substrate; as for fabric substrate, a preferable total retention amount is 5-105 g/m 2 on substrate; as for paper substrate, a preferable total retention amount is 1-20 g/m 2 on substrate; as for plastic substrate, a preferable total retention amount is 0.5-15 g/m 2 on substrate; as for rubber substrate, a preferable total retention amount is 0.5-20 g/m 2 on substrate; as for ceramic substrate, a preferable total retention amount is 5-50 g/m 2 on substrate. The total retention amount can be controlled by the application amount of printing auxiliary agent or by proper drying after application for those skilled in the art.
[0044] Said printing auxiliary agent can be applied by printing using the printing station or device existing on the printing press or additionally provided, or by coating, spraying or immersion manually or using the device existing on the printing press or additionally provided.
[0045] The method for printing said substrate can be selected from various kinds of printing methods such as relief printing, gravure printing, flexographic printing, or permeographic printing (screen or rotary screen printing).
[0046] In the printing process of the present invention, the use of printing auxiliary agent can greatly improve the printability of substrate and the transfer of printing ink on substrate. The printing auxiliary agent gives consideration to the physical and chemical properties of both printing ink and substrate, and the best modification effect can be obtained simply by choosing proper printing auxiliary agent according to the material and property of the printing ink and substrate being used, and by adjusting the amount of coating according to the site conditions during printing such as temperature and humidity conditions, heating and drying conditions, and printing speed
BRIEF DESCRIPTION OF THE DRAWINGS
[0047] FIG. 1 is a 25-fold enlargement for comparison of the printing effects in embodiment 2.
[0048] The left picture shows the printing effect without printing auxiliary agent, the right picture shows the printing effect with printing auxiliary agent.
[0049] FIG. 2 is a 25-fold enlargement for comparison of the printing effects in embodiment 3.
[0050] The left picture shows the printing effect without printing auxiliary agent, the right picture shows the printing effect with printing auxiliary agent.
[0051] FIG. 3 is a 25-fold enlargement for comparison of the printing effects in embodiment 4.
[0052] The left picture shows the printing effect without printing auxiliary agent, the right picture shows the printing effect with printing auxiliary agent.
DETAILED DESCRIPTION
[0053] The present invention is further detailed below with reference to the embodiments. It should be understood that theses embodiments are not used to limit the protection scope of the present invention
Embodiment 1
Printing Auxiliary Agent Preparation
[0054] Prepare printing auxiliary agent according to the following composition by weight percent.
[0055] Method of preparation: have all ingredients uniformly mixed according to the proportion.
[0000]
1
2
3
4
5
6
7
8
9
10
11
12
Water (%)
40
30
30
100
35
20
30
Methanol (%)
10
25
30
25
30
Ethanol (%)
10
35
30
100
20
20
Propanol (%)
10
30
Isopropanol (%)
50
Ethanediol (%)
30
30
Propanediol (%)
10
5
Dipropylene
10
Glycol (%)
Dipropylene
5
Glycol
Monomethyl
Ether (%)
Methylbenzene
30
Butanone
20
50
Cyclohexanone
25
Ethyl Acetate
50
50
Butyl Acetate
64
Resin (%)
48
28
18
Oleoresin (%)
11
Antifoaming
0.5
0.5
0.5
Agent (%)
Rheological
0.5
0.5
0.5
Agent (%)
Cosolvent (%)
0.5
0.5
0.5
Active Agent (%)
0.5
0.5
0.5
Embodiment 2
[0056] Print by a gravure printing press with a substrate of kraft paper, a printing ink of WA-20, and a printing speed of 60 m/min. The printing process adopted is as follow:
[0057] 1. Uncoiling.
[0058] 2. Coating and printing the printing auxiliary agent:
[0059] 3. Take use of the original first printing station of the printing press to print the printing auxiliary agent of composition 1 in embodiment 1 on the substrate at an amount of 5.3 g/m 2 , and then no heated drying is arranged before turning to step 3.
[0060] 4. First color (or background color) printing:
Transfer the printing ink from the color disc to the substrate by printing plate.
[0062] 5. Performing subsequent process according to conventional process
[0063] 6. Printing process for comparison: all steps except step 2 are the same as that of the printing process mentioned above.
[0064] 7. The printing results are as shown in FIG. 1 . The coloring rate for the printed material that is not applied with the printing auxiliary agent is only 42% by taking the coloring power for the printed material that is coated with the printing auxiliary agent as 100% (please refer to the picture for comparison, wherein the tinting strength test is conducted by X-Rite SP-62 spectrophotometer). As it turns out, the use of printing auxiliary agent can significantly improve the problems of surface white points and missing printing for substrates with rough surface after printing.
Embodiment 3
[0065] Print by a gravure printing press with a substrate of art paper, a water-based printing ink of mat WA plus 2% blue, and a printing speed of 80 m/min The printing process and that for comparison are the same as that of embodiment 2 except for the use of the printing auxiliary agent of composition 3 in embodiment 1 at an amount of 2.5 g/m 2 .
[0066] The printing results are as shown in FIG. 2 . The coloring rate for the printed material that is not applied with the printing auxiliary agent is only 76% by taking the coloring rate for the printed material that is coated with the printing auxiliary agent as 100% (please refer to the picture for comparison, wherein the tinting strength is tested by X-Rite SP-62 spectrophotometer). As it turns out, the use of printing auxiliary agent can improve the problems of surface white points and missing printing for substrates with rough surface after printing.
Embodiment 4
[0067] Print by a gravure printing press with a substrate of newsprint paper, a water-based printing ink of WA-20 plus 2% blue, and a printing speed of 50 m/min The printing process and that for comparison are the same as that of embodiment 2 except for the use of the printing auxiliary agent of composition 2 in embodiment 1 at an amount of 3.1 g/m 2 .
[0068] The printing results are as shown in FIG. 3 . As shown in FIG. 3 , for the printed material that has been applied by the printing auxiliary agent, the dye uptake is 100%. However, for those has not been applied by the printing auxiliary agent, the dye uptake is 80%. (please refer to the picture for comparison, wherein the relative tinting strength is tested by X-Rite SP-62 spectrophotometer). As it turns out, the use of printing auxiliary agent can significantly improve the problems of surface white points and missing printing for substrates with rough surface after printing.
Embodiment 5
Gravure Printing on Book Paper
[0069] A four-color gravure printing press is adopted to perform single-color (of blue) printing on book paper of 90 g/m 2 . A 180-mesh gravure printing roller is mounted at the first machine position of the same gravure printing press before printing so as to perform printing progress in a regular printing mode by using the printing auxiliary agent (of 100% water) at an amount of 6.2 g/m 2 , and no heated drying process is arranged before the next step of full printing of blue with a 180-mesh gravure anilox roller by the second printing plate. The printed material is fully and uniformly finished in blue without obvious white leak upon visual inspection, while obvious white leak can be found upon visual inspection for the printed material that is not applied with the printing auxiliary agent by the first printing plate. The coloring rate for the printed material that is not applied with the printing auxiliary agent is only 57% by taking the coloring rate for the printed material that is coated with the printing auxiliary agent as 100% (wherein the relative tinting strength is tested by X-Rite SP-62 spectrophotometer).
Embodiment 6
Gravure Printing on Nonwoven Fabrics
[0070] A four-color gravure printing press is adopted to perform single-color (of brown) printing on nonwoven fabrics of 147 g/m 2 . A 100-mesh gravure printing roller is mounted at the first machine position of the same gravure printing press before printing so as to print the printing auxiliary agent (of ethanol) in an regular printing mode at an amount of 12 g/m 2 , and no heated drying process is arranged before the next step of full printing of brown with a 150-mesh gravure anilox roller by the second printing plate. The printed material is fully and uniformly finished in blue without obvious white leak upon visual inspection, while obvious white leak can be found upon visual inspection for the printed material that is not applied with printing auxiliary agent by the first printing plate. The coloring rate for the printed material that is not applied with the printing auxiliary agent is only 39% by taking the coloring rate for the printed material that is coated with the printing auxiliary agent as 100% (wherein the relative coloring power is tested by X-Rite SP-62 spectrophotometer).
[0071] The same method is used, with ethanol being respectively replaced by methanol, isopropanol, ethanediol, propanediol, diethylene glycol, dipropylene glycol, dipropylene glycol monomethyl ether, dipropylene glycol monoethyl ether, dipropylene glycol monopropyl ether, dipropylene glycol monobutyl ether, diethylene glycol monomethyl ether, diethylene glycol monoethyl ether, diethylene glycol monopropyl ether, or diethylene glycol monobutyl ether to be used as the printing auxiliary agent, the printing results turn out to be that the coloring rates for the printed material that is not applied with the printing auxiliary agent is only ranging from 35% to 65% by taking the coloring rate for the printed material that is coated with the printing auxiliary agent as 100%
Embodiment 7
Screen Printing on Nonwoven Fabrics
[0072] A screen printing press is adopted to print dark blue on nonwoven fabrics with a 300-mesh screen. A spraying device is used to spray the printing auxiliary agent (of composition 6 in embodiment 1) on the surface of nonwoven fabrics at an amount of 12 g/m 2 before printing to wet the substrate surface, and no heated drying process is arranged before the next regular full printing of dark blue and the immediate drying by hot wind. The printed material is finished in bright color and no white leak is found upon visual inspection, while obvious white leak can be found upon visual inspection for the printed material that is not applied with the printing auxiliary agent. The coloring rate for the printed material that is not applied with the printing auxiliary agent is only 54% by taking the coloring rate for the printed material that is coated with the printing auxiliary agent as 100% (wherein the relative tinting strength is tested by X-Rite SP-62 spectrophotometer).
[0073] The same method is used, with composition 6 being respectively replaced by water, methanol, ethanol, isopropanol, ethanediol, propanediol, diethylene glycol, dipropylene glycol, dipropylene glycol monomethyl ether, dipropylene glycol monoethyl ether, dipropylene glycol monopropyl ether, dipropylene glycol monobutyl ether, diethylene glycol monomethyl ether, diethylene glycol monoethyl ether, diethylene glycol monopropyl ether, or diethylene glycol monobutyl ether to be used as the printing auxiliary agent, the printing results turn out to be that the coloring rate for the printed material that is not applied with the printing auxiliary agent is only ranging from 41% to 67% by taking the coloring rate for the printed material that is coated with the printing auxiliary agent as 100%
Embodiment 8
Flexographic Printing on Kraft Paper
[0074] A three-color sheet-fed flexographic printing press is adopted to print dark block on kraft paper with a 200-mesh anilox roller. Before printing, take use of the position of the first printing plate of the same flexographic printing press to transfer the printing auxiliary agent (of composition 4 in embodiment 1) on the portion to be printed in a regular flexographic printing mode at an amount of 6.7 g/m 2 , and no heated drying process is arranged before the next step of overprinting black block at the second printing plate. The finished color block is clear and rich without any white leak. The coloring rate for the printed material that is not applied with the printing auxiliary agent is only 51% by taking the coloring rate for the printed material that is coated with the printing auxiliary agent as 100% (wherein the relative tinting strength is tested by X-Rite SP-62 spectrophotometer).
[0075] When the same method is used, except that the printing auxiliary agent is respectively replaced by methanol, ethanol, isopropanol, ethanediol, propanediol, diethylene glycol, dipropylene glycol, dipropylene glycol monomethyl ether, dipropylene glycol monoethyl ether, dipropylene glycol monopropyl ether, dipropylene glycol monobutyl ether, diethylene glycol monomethyl ether, diethylene glycol monoethyl ether, diethylene glycol monopropyl ether, or diethylene glycol monobutyl ether, the printing results turn out to be that the coloring rate for the printed material that is not applied with the printing auxiliary agent is only 43%-69% by taking the coloring rate for the printed material that is coated with the printing auxiliary agent as 100%.
Embodiment 9
Rotary Screen Printing on Nonwoven Fabrics
[0076] A six-color gravure rotary screen combination printing press is adopted to print dark red on nonwoven fabrics with a 150-mesh rotary screen. An 80-mesh gravure printing roller is mounted at the first machine position of the same rotary screen combination printing press before printing so as to coat the printing auxiliary agent (of composition 6 in embodiment 1) at an amount of 30 g/m 2 by lifting the blade, and no heated drying process is arranged before the next step of full printing red by a 150-mesh rotary screen at the second printing station and the immediate drying by hot wind. The printed material is fully and uniformly finished in red without obvious white leak upon visual inspection, while obvious white leak can be found upon visual inspection for the printed material that is not applied with the printing auxiliary agent. The coloring rate for the printed material that is not applied with the printing auxiliary agent is only 63% by taking the coloring rate for the printed material that is coated with the printing auxiliary agent as 100% (wherein the relative tinting strength is tested by X-Rite SP-62 spectrophotometer).
[0077] When the same method is used, except that the printing auxiliary agent is respectively replaced by water, methanol, ethanol, isopropanol, ethanediol, propanediol, diethylene glycol, dipropylene glycol, dipropylene glycol monomethyl ether, dipropylene glycol monoethyl ether, dipropylene glycol monopropyl ether, dipropylene glycol monobutyl ether, diethylene glycol monomethyl ether, diethylene glycol monoethyl ether, diethylene glycol monopropyl ether, or diethylene glycol monobutyl ether, the printing results turn out to be that the coloring rate for the printed material that is not applied with the printing auxiliary agent is only 52%-74% by taking the coloring rate for the printed material that is coated with the printing auxiliary agent as 100%.
Embodiment 10
[0078] The method used is the same as that of embodiment 9, except that the substrate is replaced by 120-thread count cotton. As it turns out, the coloring rate for the printed material that is not applied with the printing auxiliary agent is only 82% by taking the coloring rate for the printed material that is coated with the printing auxiliary agent as 100%.
Embodiment 11
[0079] The method used is the same as that of embodiment 3, except that the substrate is replaced by uneven foamed PVC coating paper. As it turns out, the coloring rate for the printed material that is not applied with the printing auxiliary agent is only 65% by taking the coloring rate for the printed material that is coated with the printing auxiliary agent as 100%.
Embodiment 12
[0080] The method used is the same as that of embodiment 7, except that the substrate is replaced by floor tile. As it turns out, the coloring rate for the printed material that is not applied with the printing auxiliary agent is only 78% by taking the coloring rate for the printed material that is coated with the printing auxiliary agent as 100%.
Embodiment 13
[0081] The method used is the same as that of embodiment 3, except that the printing auxiliary agent is replaced by composition 7 in embodiment 1. As it turns out, the coloring rate for the printed material that is not applied with the printing auxiliary agent is only 93% by taking the coloring rate for the printed material that is coated with the printing auxiliary agent as 100%.
Embodiment 14
[0082] The method used is the same as that of embodiment 3, except that the printing auxiliary agent is replaced by composition 8 in embodiment 1. As it turns out, the coloring rate for the printed material that is not applied with the printing auxiliary agent is only 86% by taking the coloring rate for the printed material that is coated with the printing auxiliary agent as 100%.
Embodiment 15
[0083] The method used is the same as that of embodiment 3, except that the printing auxiliary agent is replaced by composition 9 in embodiment 1. As it turns out, the coloring rate for the printed material that is not applied with the printing auxiliary agent is only 79% by taking the coloring rate for the printed material that is coated with the printing auxiliary agent as 100%.
Embodiment 16
[0084] The method used is the same as that of embodiment 4, except that the printing auxiliary agent is replaced by composition 10 in embodiment 1 (at an amount of 3.5 g/m 2 ). As it turns out, the coloring rate for the printed material that is not applied with the printing auxiliary agent is only 76% by taking the coloring rate for the printed material that is coated with the printing auxiliary agent as 100%.
[0085] When the same method is used, except that the printing auxiliary agent is replaced by benzene, methylbenzene, dimethyl benzene, propanone, butanone, cyclohexanone, ethyl acetate, propyl acetate, or butyl acetate, the printing results turn out to be that the coloring rate for the printed material that is not applied with the printing auxiliary agent is only 73%-88% by taking the coloring rate for the printed material that is coated with the printing auxiliary agent as 100%.
Embodiment 17
[0086] The method used is the same as that of embodiment 4, except that the printing auxiliary agent is replaced by composition 11 in embodiment 1 (at an amount of 3.3 g/m 2 ). As it turns out, the coloring rate for the printed material that is not applied with the printing auxiliary agent is only 79% by taking the coloring rate for the printed material that is coated with the printing auxiliary agent as 100%.
Embodiment 18
[0087] The method used is the same as that of embodiment 4, except that the printing auxiliary agent is replaced by composition 12 in embodiment 1 (at an amount of 4 g/m 2 ). As it turns out, the coloring rate for the printed material that is not applied with the printing auxiliary agent is only 83% by taking the coloring rate for the printed material that is coated with the printing auxiliary agent as 100%.
[0088] Given the disclosure of the present invention, it is apparent to those skilled in the art that further modifications based on the printing process of the present invention can be made to the printing auxiliary agent according to the printing speed, heating conditions, and gas supply and exhaustion conditions so as to obtain the optimal effect. These modifications are also within the protection scope of the present invention. | A printing process and a printing auxiliary agent used therein are disclosed. The printing process comprises mounting a plate, applying ink, conveying an object to be printed, and impressing. The printing auxiliary agent is applied to the object to be printed before an impressing point in an optional printing station. The printing auxiliary agent includes water and/or an organic substance which is in liquid state under normal temperature and normal pressure. The use of the printing auxiliary agent is also disclosed. The printing process and the printing auxiliary agent can be used in printing of all kinds of objects to be printed, thus improving printing quality. | 1 |
BACKGROUND OF THE INVENTION
This application claims priority from European Patent Application No. EP 02257846.2, filed Nov. 13, 2002, herein incorporated by reference in its entirety.
1. Field of the Invention
The present invention relates to lithographic projection apparatus and more particularly to a lithographic device manufacturing method.
2. Description of the Related Art
Lithographic projection apparatus can be used, for example, in the manufacture of integrated circuits (ICs). In such a case, the patterning device may generate a circuit pattern corresponding to an individual layer of the IC, and this pattern can be imaged onto a target portion (e.g. comprising one or more dies) on a substrate (silicon wafer) that has been coated with a layer of radiation-sensitive material (resist).
The term “patterning device” as employed herein should be broadly interpreted as referring to a mechanism that can be used to endow an incoming radiation beam with a patterned cross-section, corresponding to a pattern that is to be created in a target portion of the substrate; the term “light valve” can also be used in this context. Generally, the pattern will correspond to a particular functional layer in a device being created in the target portion, such as an integrated circuit or other device (see below). Examples of such a patterning device include:
mask: the concept of a mask is well known in lithography, and it includes mask types such as binary, alternating phase-shift, and attenuated phase-shift, as well as various hybrid mask types. Placement of such a mask in the radiation beam causes selective transmission (in the case of a transmissive mask) or reflection (in the case of a reflective mask) of the radiation impinging on the mask, according to the pattern on the mask. In the case of a mask, the support structure will generally be a mask table, which ensures that the mask can be held at a desired position in the incoming radiation beam, and that it can be moved relative to the beam if so desired; programmable mirror array: an example of such a device is a matrix-addressable surface having a visco-elastic control layer and a reflective surface. The basic principle behind such an apparatus is that (for example) addressed areas of the reflective surface reflect incident light as diffracted light, whereas unaddressed areas reflect incident light as undiffracted light. Using an appropriate filter, the said undiffracted light can be filtered out of the reflected beam, leaving only the diffracted light behind; in this manner, the beam becomes patterned according to the addressing pattern of the matrix-addressable surface. The required matrix addressing can be performed using suitable electronic means. More information on such mirror arrays can be gleaned, for example, from U.S. Pat. Nos. 5,296,891 and 5,523,193, which are incorporated herein by reference. In the case of a programmable mirror array, the said support structure may be embodied as a frame or table, for example, which may be fixed or movable as required; and programmable LCD array: an example of such a construction is given in U.S. Pat. No. 5,229,872, which is incorporated herein by reference. As above, the support structure in this case may be embodied as a frame or table, for example, which may be fixed or movable as required.
For purposes of simplicity, the rest of this text may, at certain locations, specifically direct itself to examples involving a mask and mask table; however, the general principles discussed in such instances should be seen in the broader context of the patterning device as set forth above.
In general, a single wafer will contain a whole network of adjacent target portions that are successively irradiated via the projection system, one at a time. In current apparatus, employing patterning by a mask on a mask table, a distinction can be made between two different types of machine. In one type of lithographic projection apparatus—commonly referred to as a wafer stepper—each target portion is irradiated by exposing the entire mask pattern onto the target portion in one go. In an alternative apparatus—commonly referred to as a step-and-scan apparatus—each target portion is irradiated by progressively scanning the mask pattern under the projection beam in a given reference direction (the “scanning” direction) while synchronously scanning the substrate table parallel or anti-parallel to this direction. Because, typically, the projection system will have a magnification factor M (generally <1), the speed V at which the substrate table is scanned will be a factor M times that at which the mask table is scanned. More information with regard to lithographic devices as here described can be gleaned, for example, from U.S. Pat. No. 6,046,792, incorporated herein by reference.
In a manufacturing process using a lithographic projection apparatus, the pattern is imaged onto a substrate that is at least partially covered by a layer of radiation-sensitive material (resist). Prior to this imaging step, the substrate may undergo various procedures, such as priming, resist coating and a soft bake. After exposure, the substrate may be subjected to other procedures, such as a post-exposure bake (PEB), development, a hard bake and measurement/inspection of the imaged features. This array of procedures is used as a basis to pattern an individual layer of a device, e.g. an IC. Such a patterned layer may then undergo various processes such as etching, ion-implantation (doping), metallization, oxidation, chemo-mechanical polishing, etc., all intended to finish off an individual layer.
If several layers are required, then the whole procedure, or a variant thereof, will have to be repeated for each new layer. Eventually, an array of devices will be present on the substrate (wafer). These devices are then separated from one another by a technique such as dicing or sawing, whence the individual devices can be mounted on a carrier, connected to pins, etc. Further information regarding such processes can be obtained, for example, from the book “Microchip Fabrication: A Practical Guide to Semiconductor Processing”, Third Edition, by Peter van Zant, McGraw Hill Publishing Co., 1997, ISBN 0-07-067250-4, incorporated herein by reference.
For the sake of simplicity, the projection system may hereinafter be referred to as the “lens”; however, this term should be broadly interpreted as encompassing various types of projection system, including refractive optics, reflective optics, and catadioptric systems, for example. The radiation system may also include components operating according to any of these design types for directing, shaping or controlling the projection beam of radiation, and such components may also be referred to below, collectively or singularly, as a “lens”. Further, the lithographic apparatus may be of a type having two or more substrate tables (and/or two or more mask tables). In such “multiple stage” devices the additional tables may be used in parallel, or preparatory steps may be carried out on one or more tables while one or more other tables are being used for exposures. Twin stage lithographic apparatus are described, for example, in U.S. Pat. No. 5,969,441 and WO 98/40791, incorporated herein by reference.
In a lithography apparatus, it is important to align the mask with the substrate wafer. In other words, alignment is the process of positioning the image of a specific point on the mask to a specific point on the wafer which is to be exposed. Typically one or more alignment marks, such as a small pattern, are provided on each of the substrate and the mask. A device may consist of many layers which are built up by successive exposures with intermediate processing steps. Before each exposure, alignment between the markers on the substrate and the mask is performed to minimize any positional error between the new exposure and the previous ones, which error is termed overlay error.
For some devices, e.g. micro-electro-mechanical systems (MEMS) and micro-opto-electro-mechanical systems (MOEMS), it is desirable to be able to create structures on both sides of a substrate using lithographic processes and, in many cases, the structures on opposite sides of the substrate need to be aligned with each other. This means that it is necessary for the lithographic apparatus to align the pattern being projected onto the front side of a substrate to alignment markers on the backside.
To achieve this alternate side imaging, various efforts have employed additional hardware, e.g. optics to project an image of a backside marker to the front side of the substrate or using a special substrate that is transparent. Infra-red radiation can be used with a silicon substrate but has limited accuracy and may undesirably heat the wafer.
SUMMARY OF THE INVENTION
Principles of the present invention, as embodied and broadly described herein, provide for a device manufacturing method which can image structures on one side of a substrate aligned to markers on the other side without the need for additional hardware and with improved accuracy. One embodiment of the present invention comprises providing a first substrate having first and second surfaces, patterning the first surface of the substrate with at least one reversed alignment marker, providing a protective layer over the alignment marker, and bonding the first surface of the first substrate to a second substrate. The embodiment further includes locally etching the first substrate as far as the protective layer to form a trench around the reversed alignment marker, and forming at least one patterned layer on the second surface using a lithographic projection apparatus having a front-to-backside alignment system while aligning the substrate to the alignment markers revealed in each trench.
The reversed alignment marker formed in the first surface is revealed by the etch as a normally oriented alignment marker to which the lithographic projection apparatus can readily align. Patterns directly aligned to the marker printed on the front side can therefore be printed on the backside of the substrate.
The protective layer which conforms to the shape of the marker is preferably formed of a material, e.g. SiO 2 , selective against the etch used to form the trench(es) and hence forms an etch stop layer. A reflective layer, e.g. of Al, can be formed over the protective layer (before bonding) to increase the visibility of the marker when revealed in the trench.
The etch step can be localized by forming an etch-resistant layer, e.g. of oxide, on the second surface; providing a layer of radiation-sensitive resist on the etch-resistant layer; patterning and developing said resist so as to form openings above said marker(s); and removing said etch-resistant layer in said openings. To pattern the resist to form the openings, the markers only need to be located coarsely, which can be done to sufficient degree of accuracy using an infra-red mark sensor from the second side of the substrate.
Before the substrate is bonded to the second (carrier) substrate, devices may be formed in and/or on the first surface using known techniques. The protective layer and optional reflective layer may be formed as part of device layers, with any intervening layers locally removed as necessary, rather than being specially formed.
Normal alignment markers for use in aligning the structures in or on the first surface can be printed in the same step as the reverse alignment markers used to align the structures formed on the second surface. In this way, the positional relationship of the normal and reversed markers and hence of the structures on the first and second surfaces can be assured.
After bonding, the first substrate may be reduced in thickness, e.g. by grinding.
Although specific reference may be made in this text to the use of lithographic apparatus in the manufacture of ICs, it should be understood that the lithographic apparatus described herein may have other applications, such as the manufacture of integrated optical systems, guidance and detection patterns for magnetic domain memories, liquid-crystal displays (LCDs), thin-film magnetic heads, etc. The skilled artisan will appreciate that, in the context of such alternative applications, any use of the terms “wafer” or “die” herein may be considered as synonymous with the more general terms “substrate” or “target portion”, respectively.
The substrate referred to herein may be processed, before or after exposure, in for example a track (a tool that typically applies a layer of resist to a substrate and develops the exposed resist) or a metrology or inspection tool. Where applicable, the disclosure herein may be applied to such and other substrate processing tools. Further, the substrate may be processed more than once, for example in order to create a multi-layer IC, so that the term substrate used herein may also refer to a substrate that already contains multiple processed layers.
The terms “radiation” and “beam” used herein encompass all types of electromagnetic radiation, including ultraviolet (UV) radiation (e.g. having a wavelength of 365, 248, 193, 157 or 126 nm) and extreme ultra-violet (EUV) radiation (e.g. having a wavelength in the range of 5-20 nm), as well as particle beams, such as ion beams or electron beams.
The term “projection system” used herein should be broadly interpreted as encompassing various types of projection system, including refractive optical systems, reflective optical systems, and catadioptric optical systems, as appropriate for example for the exposure radiation being used, or for other factors such as the use of an immersion fluid or the use of a vacuum. Any use of the term “lens” herein may be considered as synonymous with the more general term “projection system”.
The illumination system may also encompass various types of optical components, including refractive, reflective, and catadioptric optical components for directing, shaping, or controlling the projection beam of radiation, and such components may also be referred to below, collectively or singularly, as a “lens”.
The lithographic apparatus may be of a type having two (dual stage) or more substrate tables (and/or two or more mask tables). In such “multiple stage” machines the additional tables may be used in parallel, or preparatory steps may be carried out on one or more tables while one or more other tables are being used for exposure.
The lithographic apparatus may also be of a type wherein the substrate is immersed in a liquid having a relatively high refractive index, e.g. water, so as to fill a space between the final element of the projection system and the substrate. Immersion liquids may also be applied to other spaces in the lithographic apparatus, for example, between the mask and the first element of the projection system. Immersion techniques are well known in the art for increasing the numerical aperture of projection systems.
BRIEF DESCRIPTION OF THE DRAWINGS
Embodiments of the invention will now be described, by way of example only, with reference to the accompanying schematic drawings in which:
FIG. 1 depicts a lithographic projection apparatus depicts, which can be used in one embodiment of the invention;
FIG. 2 is a plan view of a substrate showing the location of alignment markers used in one embodiment of the invention; and
FIGS. 3 to 8 illustrate steps in accordance with an embodiment of the invention.
In the Figures, corresponding reference symbols indicate corresponding parts.
DETAILED DESCRIPTION
Lithographic Projection Apparatus
FIG. 1 schematically depicts a lithographic projection apparatus according to a particular embodiment of the invention. The apparatus comprises:
a radiation system Ex, IL: for supplying a projection beam PB of radiation (e.g. UV radiation such as for example generated by an excimer laser operating at a wavelength of 248 nm, 193 nm or 157 nm, or by a laser-fired plasma source operating at 13.6 nm). In this particular case, the radiation system also comprises a radiation source LA; a first object table (mask table) MT: provided with a mask holder for holding a mask MA (e.g. a reticle), and connected to first positioning mechanism PM for accurately positioning the mask with respect to item PL; a second object table (substrate table) WT: provided with a substrate holder for holding a substrate W (e.g. a resist-coated silicon wafer), and connected to second positioning mechanism PW for accurately positioning the substrate with respect to item PL; and a projection system (“lens”) PL: (e.g. a quartz and/or CaF 2 lens system or a catadioptric system comprising lens elements made from such materials, or a mirror system) for imaging an irradiated portion of the mask MA onto a target portion C (e.g. comprising one or more dies) of the substrate W.
As here depicted, the apparatus is of a transmissive type (i.e. has a transmissive mask). However, in general, it may also be of a reflective type, for example (with a reflective mask). Alternatively, the apparatus may employ another kind of patterning mechanism, such as a programmable mirror array of a type as referred to above.
The source LA (e.g. a UV excimer laser, a laser-fired plasma source, a discharge source, or an undulator or wiggler provided around the path of an electron beam in a storage ring or synchrotron) produces a beam of radiation. This beam is fed into an illumination system (illuminator) IL, either directly or after having traversed conditioning mechanism, such as a beam expander Ex, for example. The illuminator IL may comprise adjusting mechanism AM for setting the outer and/or inner radial extent (commonly referred to as σ-outer and σ-inner, respectively) of the intensity distribution in the beam. In addition, it will generally comprise various other components, such as an integrator IN and a condenser CO. In this way, the beam PB impinging on the mask MA has a desired uniformity and intensity distribution in its cross-section.
It should be noted with regard to FIG. 1 that the source LA may be within the housing of the lithographic projection apparatus (as is often the case when the source LA is a mercury lamp, for example), but that it may also be remote from the lithographic projection apparatus, the radiation beam which it produces being led into the apparatus (e.g. with the aid of suitable directing mirrors); this latter scenario is often the case when the source LA is an excimer laser. The current invention and claims encompass both of these scenarios.
The beam PB subsequently intercepts the mask MA, which is held on a mask table MT. Having traversed the mask MA, the beam PB passes through the lens PL, which focuses the beam PB onto a target portion C of the substrate W. With the aid of the second positioning mechanism PW (and interferometric measuring mechanism IF), the substrate table WT can be moved accurately, e.g. so as to position different target portions C in the path of the beam PB. Similarly, the first positioning mechanism PM can be used to accurately position the mask MA with respect to the path of the beam PB, e.g. after mechanical retrieval of the mask MA from a mask library, or during a scan.
In general, movement of the object tables MT, WT will be realized with the aid of a long-stroke module (coarse positioning) and a short-stroke module (fine positioning), which are not explicitly depicted in FIG. 1 . However, in the case of a wafer stepper (as opposed to a step-and-scan apparatus) the mask table MT may just be connected to a short stroke actuator, or may be fixed. Mask MA and substrate W may be aligned using mask alignment marks M 1 , M 2 and substrate alignment marks P 1 , P 2 .
The depicted apparatus can be used in two different modes:
step mode: the mask table MT is kept essentially stationary, and an entire mask image is projected in one go (i.e. a single “flash”) onto a target portion C. The substrate table WT is then shifted in the x and/or y directions so that a different target portion C can be irradiated by the beam PB; and scan mode: essentially the same scenario applies, except that a given target portion C is not exposed in a single “flash”. Instead, the mask table MT is movable in a given direction (the so-called “scan direction”, e.g. the y direction) with a speed v, so that the projection beam PB is caused to scan over a mask image; concurrently, the substrate table WT is simultaneously moved in the same or opposite direction at a speed V=Mv, in which M is the magnification of the lens PL (typically, M=¼ or ⅕). In this manner, a relatively large target portion C can be exposed, without having to compromise on resolution.
Embodiment 1
FIG. 2 shows a wafer W which is to be provided with devices on both sides and on which are provided normal markers (not shown) and reversed markers 1 - 8 . The reversed markers 1 - 8 are mirror images—about the axis about which the wafer is to be rotated, in this case the Y axis—of the normal markers. The normal markers may take any convenient form, such as a grating, a group of gratings, box-in-box, frame-in-frame, chevrons, etc., as known in the art, and may form the primary markers used for global alignment of the substrate prior to a series of exposures.
In FIG. 2 , examples of a reverse primary marker and, for reference, a normal primary marker, each formed by four gratings, are shown. Of the four gratings, a pair are horizontal and a pair vertical and, though not apparent from the drawing, the two gratings of each pair have different periods in a known manner. In the present example the markers are provided at symmetrical positions on the wafer axes. The present invention may of course also be applied to other markers, e.g. markers adjacent each target area or die.
FIGS. 3 to 8 illustrate steps in an example of the method of the invention. Firstly, normal markers (not shown) and reversed markers 1 - 8 are etched into first surface 10 a of wafer W in a known manner and covered by a protective layer 11 of SiO 2 and a reflective layer 12 of Al, as shown in FIG. 3 , which is a partial cross-section along the Y axis of FIG. 2 . The substrate W is then flipped over and bonded to carrier substrate CW with a layer of adhesive 13 . FIG. 4 shows the substrate W bonded to the carrier substrate CW, with the second surface 10 b uppermost.
As shown in FIG. 5 , the wafer W is ground to a desired thickness, T, e.g. of about 70 μm, and the upper surface 10 b ′ finished as required for the devices to be formed on it.
To locally etch through the first substrate to reveal the reversed markers 1 - 8 , the second surface 10 b ′ is first covered with a layer of oxide 14 , e.g. by deposition, as shown in FIG. 6 and a layer of resist 15 which is exposed to open primary flood windows 16 above the reversed markers 1 - 8 . Since the primary flood windows 16 are rather larger than the markers they do not have to be accurately located and the exposure step to form them can be carried out after the markers have been located using a coarse alignment tool, such as a mark sensor using infra-red, that can detect the reversed markers through the substrate W.
The oxide layer 14 is removed in the windows 16 by a dry etch RIE or wet etch (Buffered Oxide Etch Containing HF) step to form a hardmask and a deep trench etch using an etchant selective to Si is performed to form trenches 17 . The deep trench etch ends on the SiO 2 layer and so the trenches 17 extend down to the reversed primary markers 1 , 5 to reach the position shown in FIG. 8 . Thereafter, device layers can be formed on the second surface 10 b ′ with alignment to the reversed markers 1 - 8 revealed in trenches 17 . The trenches have a width d 1 at their tops that is sufficient, e.g. 1200 μm, to ensure that the width d 2 at their base is large enough, e.g. 1000 μm, to accommodate comfortably the markers 1 - 8 . The oxide layer 14 is then removed prior to continued processing.
The first step in continued processing of the bonded substrate may be to print further markers, at known positions relative to the revealed markers, on the second surface 10 b ′, now uppermost, of the wafer. The further markers can be aligned to in the further processing of the second surface more conveniently than the revealed markers.
Whilst specific embodiments of the invention have been described above, it will be appreciated that the invention may be practiced otherwise than as described. The embodiments described above may, instead, be implemented in different embodiments of software, firmware, and hardware in the entities illustrated in the figures.
As such, the description is not intended to limit the invention. The configuration, operation, and behavior of the present invention has been described with the understanding that modifications and variations of the embodiments are possible, given the level of detail present herein. Thus, the preceding detailed description is not meant or intended to, in any way, limit the invention—rather the scope of the invention is defined by the appended claims. | A device manufacturing method capable of imaging structures on one side of a substrate aligned to markers on the other side, is presented herein. One embodiment of the present invention comprises providing a first substrate having first and second surfaces, patterning the first surface of the substrate with at least one reversed alignment marker, providing a protective layer over the alignment marker, and bonding the first surface of the first substrate to a second substrate. The embodiment further includes locally etching the first substrate as far as the protective layer to form a trench around the reversed alignment marker, and forming at least one patterned layer on the second surface using a lithographic projection apparatus having a front-to-backside alignment system while aligning the substrate to the alignment markers revealed in each trench. | 6 |
BACKGROUND OF THE INVENTION
This invention relates to sanding devices and in particular to a pad assembly for a rotary disc sander of the vacuum type.
In my U.S. Pat. No. 4,058,936 issued Nov. 22, 1977, I have described several embodiments of a vacuum sanding device of the double-acting type. The present invention is directed specifically to a pad assembly for a rotary vacuum operated disc sander but the means for driving the disc and the vacuum creating means for the disc assembly may be the same as that in U.S. Pat. No. 4,058,936.
Rotary sanding devices revolve at fairly high speeds and are used in grinding operations and heavy duty forms of work such as automobile bodies etc. Due to the nature of the work and the varied materials to be sanded or ground, it has until this time been difficult to obtain an efficient rotary sanding assembly having an attached vacuum arrangement. This is mainly due to the fact that the ground particles clog up small passages in the disc, particularly when the pad is flexed under pressure.
The present invention overcomes the deficiencies of the prior art by providing a vacuum rotary sander with a flexible pad body that is secured to a rigid head member which in turn is connectable to a pneumatic rotating device as described in U.S. Pat. No. 4,058,936. Additionally, the rigid head may be enclosed by a vacuum housing such as that shown in U.S. Pat. No. 4,058,936 whereby the particles ground by the pad assembly are quickly and efficiently carried away from the unit. A plurality of apertures in the head communicate with other apertures in the lower surface of the pad by way of internal channels in the pad body and these channels are angled toward the direction of rotation of the pad so that there is a leading action to the vacuum function applied to the apertures when the pad is being rotated. Apertures in the lower portion of the pad coincide with apertures in an abrasive disc which is removably secured to the assembly and, in a preferable form, the apertures in the lower part of the pad are elongated in the direction opposite to that of rotation so as to allow some slippage of the abrasive disc relative to the pad assembly without losing alignment of the apertures in either member.
SUMMARY OF THE INVENTION
According to one broad aspect therefor, the present invention relates to a pad assembly for a vacuum rotary sander, said assembly comprising (a) a circular upper pad portion of firm but resilient material and having a plurality of evenly spaced apertures concentrically arranged therein and positioned approximately midway between the centre of said upper pad portion and the circumferential edge thereof, (b) and an elongated channel extending from each said aperture angularly outwardly in the direction of rotation of the assembly, each said channel being open along its bottom edge, (c) a lower pad portion of relatively soft flexible material and having an inner and outer row of evenly spaced concentrically arranged apertures therein, said lower pad portion being bonded to said upper pad portion so that the inner row of apertures on the lower pad portion coincide with the apertures in the upper pad portion to form a plurality of inner vacuum holes and wherein the outer row of apertures on the lower pad portion coincide with outer terminal ends of the channels in the upper pad portion, the material of the lower pad intermediate the inner and outer rows of apertures therein forming a flexible bottom wall for said channels, (d) said upper pad portion having an inwardly and upwardly tapering circumferential sidewall with a groove adjacent the upper end thereof, said pad assembly being adapted to receive a sanding disc on the lower surface thereof with apertures therein coinciding with those in the lower pad assembly, and retained thereon by a flexible backing held in the sidewall groove by elastic retaining means, and (e) a circular rigid head member secured concentrically to the top of the upper pad portion and adapted for connection to rotative and vacuum means, said rigid member having a plurality of apertures therein somewhat larger than, and coinciding with the apertures in the upper pad portion. The inner and outer rows of apertures in the lower pad portion are elongated in the direction opposite to that of rotation of the assembly to provide each aperture with a leading and trailing end, the leading end of the inner row of apertures coinciding with the inner ends of the apertures in the upper pad prtion and the rigid head member.
In accordance with another aspect, the present invention relates to a vacuum sanding assembly having a circular pad and abrasive disc attachable thereto, the pad and disc having corresponding apertures therein for suction of sanded material into said assembly, a device for positioning and loading the abrasive disc onto the pad comprising a circular, planar member having a central upstanding primary pin thereon adapted to centre central apertures in the abrasive disc and pad, an upstanding side wall tapering inwardly on its outer surface and having an O-ring retaining lip at its upper end, and at least a pair of spaced secondary pins secured to and upstanding from the planar surface and corresponding to a selected pair of coincident apertures in the abrasive disc and pad.
BRIEF DESCRIPTION OF THE DRAWINGS
The invention is illustrated by way of example in the accompanying drawings wherein:
FIG. 1 is a partially sectioned, fragmented top view of the several elements of the pad assembly;
FIG. 2 is another fragmented top view with the elements in assembled condition;
FIG. 3 is a fragmented sectional view taken along the line 3--3 of FIG. 2;
FIG. 4 is a partially sectioned view of the pad assembly in operation;
FIG. 5 is a perspective view of a further embodiment of the lower pad assembly 12; and
FIG. 6 is a cross-sectional view similar to FIG. 3 illustrating the additional embodiment of FIG. 5.
DESCRIPTION OF THE PREFERRED EMBODIMENT
Referring to FIGS. 1 and 2, a pad assembly 10 has circular lower and upper pad portions 11 and 12 and a circular head member 14. In FIG. 1, the lower pad portion is shown as a single sheet of relatively soft, flexible material such as rubber and having a plurality of inner apertures 16 and outer apertures 18 in the surface thereof. The direction of rotation of the assembly is shown by arrow R. The inner row of apertures 16 is positioned approximately midway between the center aperture 58 in the lower pad portion 11 and the outer terminal edge thereof with the outer row of apertures 18 being positioned more or less adjacent to the outer circumferential edge of the assembly. The inner row of apertures are circumferentially, evenly spaced with respect to one another as are the apertures 18 of the outer row and while the apertures 16 and 18 may be circular, I prefer that they be elongated as shown.
In FIG. 1 the upper pad portion 12 is provided with channels 20 which interconnect the apertures 16 and 18 when the upper pad portion 12 is placed on a top surface of the lower pad portion 11 and bonded thereto as shown in FIG. 1. In the upper portion of FIG. 1, the position that the channels 20 will assume are shown in pecked line and in the central part of FIG. 1 which is a top view of the upper pad portion 12, the elongated channels 20 are shown providing a communication between the inner and outer rows of apertures 16 and 18 respectively. The inner terminal ends 22 and outer terminal ends 24 of the channels 20 coincide with the inner and outer apertures 16 and 18 respectively when the upper pad portion 12 overlays the lower pad portion 11.
The upper pad portion is manufactured from resilient material that is quite firm with respect to the material of the lower pad portion.
The head member 14 is of rigid material and is shown in the fragmented portion of FIG. 1. Head 14 has apertures 26 which, when head 14 is bonded to the upper surface of upper pad portion 12, coincide with the inner terminal ends 22 of the channels 20 and the inner row of apertures 16 in the lower pad portion as shown for example in FIG. 2. Preferably, apertures 26 in head 14 are slightly larger than the apertures which they overlay and also, they are preferably elongated as shown in FIG. 1 The head 14 is also provided with a central, threaded sleeve 28 for connection to suitable rotating means.
Referring to FIG. 2, the fragmentary top view of the assembly 10 shows the path of communication between the outer row aperture 18, channel 20, inner row aperture 16 and aperture 26 in the head 14. It will also be evident that because of the elongation of the inner and outer rows of apertures in a direction away from that of rotation R, the outer row of apertures 18 has a "leading" portion 30 and a trailing portion 32 and inner row aperture also has a leading portion 34 and a trailing portion 36.
The reason for providing leading and trailing portions to the above apertures is that when an abrasive disc having apertures therein coincident with those in the pad assembly, it is applied to a bottom surface of the lower pad portion of the pad assembly and held thereon by a flexible skirt and elastic retaining means, there is sometimes slippage between the surface of the abrasive disc and the supporting pad assembly due to the amount of torque applied to the abrasive disc by the surface being ground resulting from a lot of pressure being exerted on the disc by the operator. It will be appreciated that because of the elongation of the apertures and the leading and trailing portions thereof, the abrasive disc can slip rearwardly a substantial amount though the apertures therein will still be in communication with the trailing ends 32 and 36 of the outer apertures 18 and inner apertures 36.
It will also be noted from FIG. 1 and FIG. 2 that the outer apertures 18 are circumferentially offset from the inner apertures 16 and that the channels 20 interconnecting those apertures are angularly directed towards the direction of rotation R of the pad assembly and this angulation provides an improved grit gathering result when the pad is rotated at high speed.
Referring to FIG. 3, the upper pad portion 12 can be manufactured from a single disc member although I prefer to make it from two discs, an upper disc 12a and a lower disc 12b. Upper disc 12a of quite firm but resilient material and a lower disc 12b of softer, more flexible material. In either case, the upper pad portion 12 has an aperture 13 therein coincident with aperture 26 in the head 14 and with aperture 16 in the lower pad assembly 11. It will be seen from FIG. 3 that the construction of the upper pad portion 12 provides the channel 20 with upper and end walls and that the material 21 between the inner and outer rows of apertures 16 and 18 in the lower pad assembly provides the channel 20 with a flexible, bottom wall. In cross-section therefore channel 20 has two inlets, 18 and 16 and a large exhaust outlet, 13 and 26.
The abrasive disc 38 is provided with a flexible backing 40 adhesively secured thereto and which incorporates a flexible peripheral skirt 42 which is folded into a groove 44 in the sidewall of the lower pad assembly 12 and retained therein by the indicated taper to that sidewall as well as by a resilient O-ring or other suitable retaining means as shown in FIG. 4.
The abrasive disc 38 is provided with an inner row of apertures 46 and an outer row of apertures 48 and it will be evident from FIG. 3 that when the disc is mounted onto the lower face of the pad, inner apertures 46 are coincident with apertures 16 in the lower pad assembly 11 as well as apertures 13 in the upper assembly and 26 in the head 14 while the outer row of apertures 48 in the disc are coincident with apertures 18 in the lower pad assembly 11.
The present invention also provides for a loading means 50 for quickly and accurately positioning and applying the abrasive disc 38 to the lower face of the pad assembly. The loader 50 has a circular planar platform or surface 52 provided with a central pin 54 which aligns central aperture 56 in the abrasive disc and a central aperture 58 in the pad assembly 10. At least two and preferably three additional pins 60 are provided on the surface of the loader 50 and these pins are positioned so as to be coincident with the inner row of apertures 46 in the abrasive disc and apertures 16 in the lower pad assembly. Additionally, the pins 60 are long or high enough to enter the aperture 13 in the upper ends of the upper pad portion 12 and as aperture 13 does not have a trailing portion, the abrasive disc 38 will be so positioned that its apertures 46 and 48 will be aligned with the leading portions 30 and 34 of the outer apertures 18 and inner apertures 16 respectively.
The outer periphery of the loader 50 has an upstanding wall 62, the outer surface of which tapers inwardly as shown at 64 and is provided with a lip 66 for retaining an elasticized O-ring 68 or the like. It will be appreciated from FIG. 3 that the abrasive disc is first placed downwardly onto the floor or surface 52 of the loader 50 with the apertures being positioned over their respective pins and then the pad assembly is lowered down onto the pins as well. The O-ring 68 can then be moved upwardly and will automatically pull the flexible skirt 42 upwardly along the tapered sidewall of the pad assembly and will come to rest in the groove 44 as shown in FIG. 4.
Alternatively, a telescoping form of loader may be utilized as shown in my Canadian Pat. No. 772,369 of Nov. 28, 1967. Such a telescoping loader would of course have to utilize the pin assembly disclosed herein.
Referring now to FIG. 4, the pad assembly is shown in operation grinding the surface of a workpiece 70. Due to the relatively firm material of the upper pad portion 12, a substantial pressure may be applied to the outer peripheral area of the pad assembly and as most rotary sanding is done with this form of pressure on the peripheral area of the pad, the flexible lower wall in the channel 20 ensures that the maximum amount of surface of the lower pad 11 is in contact with the surface of the work 70.
It will be evident from FIG. 4 that by virtue of the position and size of the apertures and channels, that the grit 72 flows smoothly through the channel 20 and out through the exit apertures 26 into the vacuum housing H shown in pecked line.
Referring to FIGS. 5 and 6, an additional soft pad 73 formed of sponge material or the like is inserted between the lower pad 12b and the abrasive disc 38. As shown in FIG. 5, sponge pad 73 is provided with inner and outer rows of apertures to register with those in the pad member 12b. Sponge pad 73 is normally used in situations where a softer sanding application is required, the resiliency of the sponge pad providing more "give" to the abrasive disc when the operator is for example sanding an area of multiple contours. In the past, sometimes the sponge pads 73 slipped away from the lower pad 12b after prolonged use. In accordance with the embodiment of FIGS. 5 and 6, the lower pad assembly 12b is provided on its bottom surface with a plurality of small protuberances or projections 74 which, when the sponge pad 73 is placed against the lower pad assembly 12b, provides additional grip between the two faces of the members in question. While FIG. 5 illustrates only a small number of projections 74 on the lower surface of pad 12b, it will be appreciated that these projections can be applied in any density required and normally would cover the whole surface of pad 12b.
It will be appreciated that the projections 74 dig into the upper or juxtaposed surface of the sponge pad 73 particularly on the peripheral area that is against the surface being sanded and there is an actual clutch action provided between the two gripped surfaces. It will further be appreciated that even if the face of the sponge pad pulls away slightly from the face of the pad 12b, it will not rotationally slip because of the fact that the sponge pad is riding on top of the projections 74.
While the invention has been described in connection with a specific embodiment thereof and in the specific use, various modifications thereof will occur to those skilled in the art without departing from the spirit and scope of the invention as set forth in the attached claims. The terminology and expressions which have been employed in this disclosure are used as terms of description and not of limitation and there is no intention in the use of such terminology and expressions to exclude any equivalents of the features shown and described or portions thereof but it is recognized that various modifications are possible within the scope of the invention claimed. | A pad assembly for a vacuum rotary sander has a flexible pad body secured to a rigid head that is connectable to a vacuum housing and a pad rotating means. A plurality of apertures in the head communicate with other apertures in the lower surface of the pad by internal channels which are angled toward the direction of rotation of the pad. The apertures in the lower portion of the pad coincide with apertures in an abrasive disc removably secured to the assembly and may be elongated in the direction opposite to that of rotation so as to allow some slippage of the abrasive disc relative to the pad assembly. There is also disclosed a device for quickly positioning and loading an abrasive disc onto the pad assembly. | 1 |
BACKGROUND OF THE INVENTION
This invention relates to tufting machines and tufted fabrics and more particularly to a method and apparatus for forming a new fabric having tufted loops in the form of chain links disposed longitudinally in rows on the base fabric.
In the formation of tufted pile a plurality of laterally disposed yarn carrying needles are reciprocably driven through a base fabric longitudinally fed through the machine to form loops carried down below the fabric to be seized by loopers oscillating in timed relationship with the needles and which cross the needles just above the needle eye to seize the loop of yarn. In a loop pile machine the loopers point in the direction of feed of the base fabric and hold the seized loops while the needles are retracted from the base fabric, thereafter rocking away from the point of loop seizure to release the loops. When the needles start their next descent the loops have been released from the loopers and carried one stitch length away from the needle path. To form cut pile the loopers point in the direction opposite to the direction in which the fabric is being fed and cooperate with respective oscillating knives. Since the fabric and thus the loop is being fed toward the closed end of the looper the loop cannot be released and is not cut by the knife as the hook rocks away from the needle path, generally after about three loops have been so seized. The pile height of cut pile fabric depends solely upon the distance that the loopers are disposed below the backing fabric, while the pile height of loop pile depends upon the amount of yarn fed to the needle with the maximum being the distance from the loopers to the backing fabric.
The aesthetic appearance of a tufted fabric to a large extent depends upon what is known as the "cover" or "coverage" of the fabric. This is the amount of the yarn that appears on the base fabric, it being undesireable for the base fabric to be visable. Heretofor, the manner of obtaining greater cover has been to utilize more yarn, either by having higher pile heights or greater density, or both, the latter being determined by the lateral spacing or gauge between adjacent needles and loopers, and by the rate of fabric feed relative to the rate of needle reciprocation. Large utilization of yarn results from obtaining coverage in this manner. Since the largest single factor in the cost of producing tufted fabric is the amount, and thus the weight, of yarn in the fabric, the greater the coverage the higher the cost of the fabric. Consequently, it is highly desireable to have a high coverage product with a low face weight, i.e., small amount of yarn.
Tufted fabric is less expensive to produce than other known pile fabric producing methods and tufted fabric stylists are continually seeking attractive new patterning abilities and yarns for broadloom carpet, wall coverings, upholstery and drapery fabric. Thus, attempts have been made to produce various looks in a tufted fabric that are produced more expensively by for example, weaving and knitting. The knitted look and the crewel look are desireable for certain applications, particularly when the look can be obtained with the yarns of larger size or heavier deniers. No tufted fabric is presently known with these qualities nor with the unraveling characteristics of the product produced by those methods.
SUMMARY OF THE INVENTION
The present invention provides a tufted pile fabric having the pile tufts disposed on the base fabric in the form of chains extending longitudinally substantially parallel to the base fabric between stitching holes, and a method and apparatus for producing the fabric by concatenating successive tufting loops into a chain using a primary looper and a transfer looper oscillating out of phase with each other. Since the loops lie substantially flat against the base fabric a greater amount of yarn is capable of being placed on the face of the base fabric relative to the amount of yarn utilized, and the amount of yarn coverage while substantial does not result in the high face weight of yarn heretofor necessary for equivalent coverage. Moreover, adjacent rows of chains may be off set laterally to provide a fabric with exceptionally high coverage. The fabric has an attractive knitted appearance with berber or crewel effects suitable for use as a residential carpeting, automobile fabrics, wall coverings, upholstery and rugs. It also provides an excellent print base for carpeting and is ideal in public areas when used with heavier and/or larger yarn sizes because it will not unravel and has virtually no pile crushing possibilities.
In practicing the principles of the invention a base fabric is fed between a reciprocating needle and a pair of oscillating loopers. The needle penetrates the base fabric and forms a loop seized by the first or primary looper having a bill facing in the direction of fabric feed as the looper rocks toward the needle path. As the needle ascends the primary looper rocks away from the needle path and sheds the loop which is thereafter seized by the second or transfer looper having a bill facing oppositely to the direction of fabric feed and oscillating oppositely relatively to the primary looper. The transfer looper holds the loop for entry by the needle as it thereafter descends. The transfer looper thereafter rocks away from the needle path as the primary looper rocks into the needle path for seizing a subsequent loop. Thus, each loop is formed within a prior loop and as the needle begins to ascend the transfer looper releases the first loop which is concatenated about the subsequent loop.
The transfer looper has a loop seizing bill spaced above and overlying a portion of the bill of the primary looper and in transverse alignment therewith. The transfer loopers oscillate out of phase with the primary loopers. Preferably the transfer loopers are mounted on a common looper bar with the primary loopers and have mounting portions longitudinally intermediate adjacent primary loopers, the bill portions of the transfer loopers being bent into the aligned relationship with the primary loopers. The needle passes through the bend of the transfer looper at approximately bottom dead center, but is spaced from the transfer looper as it enters the loop held thereon.
Another feature of the invention contemplates the insertion of a loop pile tuft into each chain using another yarn system. The second yarn system may include a different type yarn with different twists, sizes and colors than that of the chain system. Moreover, it may be separately controlled and provide high and low loops in accordance with a pattern within the chain fabric. To provide this combination additional needles may be mounted for reciprocating into cooperation with loopers pointing in the direction of the fabric feed. The needles may be mounted in the needle bar with the chain producing needles and the loopers may be mounted in the same looper bar with the other loopers.
Consequently, it is a primary object of the present invention to provide a tufted pile fabric having concatenated loops and a method and apparatus for forming the fabric.
It is another object of the present invention to provide in a tufting machine apparatus for producing a pile fabric in the form of a chain against the base fabric and wherein the apparatus includes oscillating primary and secondary loopers, the primary loopers for seizing a loop from a reciprocating needle and subsequently shedding the loop onto the secondary loopers where it is held, concatenated with a subsequent loop and thereafter shed.
It is a further object of the present invention to provide in a tufting machine a pair of loopers cooperating with a reciprocating needle, in which the bill of a first of the loopers points in the direction of fabric feed for seizing a loop of yarn from the needle and in which the second looper points in the direction opposite to fabric feed for receiving a seized loop shed from the first looper and holding the loop for entry by the needle as it descends to form a subsequent loop.
It is a still further object of the present invention to provide in a tufting machine a first oscillating looper having a bill pointing in the direction in which the base fabric is fed and cooperating with a reciprocating needle to seize a loop of yarn and thereafter shed the loop, and a second looper having a bill pointing oppositely to the direction of fabric feed positioned closer to the base fabric than the first looper and aligned with the bill of the first looper in the direction of fabric feed for seizing the loop shed by the first looper, the second looper oscillating out of phase with the first looper and holding the loop for entry by the needle as it descends towards the loop seizing position of the first looper.
It is yet a further object of the present invention to provide in adjacent lateral rows in a tufting machine needles offset from each other in the direction of fabric feed, each needle cooperating with a respective primary looper for seizing a loop of yarn presented by the respective needle and thereafter shedding the loop, and a transfer looper associated with each primary looper for seizing the loop shed by the respective primary looper for concatenation with a subsequently formed loop to produce offset adjacent rows of concatenated loops.
It is yet a still further object of the present invention to provide a transfer looper for a tufting machine for use in combination with a loop pile looper for forming chain tufts wherein the transfer looper has a bill portion bent out of the plane of its mounting portion.
It is still yet a further object of the present invention to provide a fabric having tufted loops disposed within concatenated chain loops and a method and apparatus for forming the fabric.
BRIEF DESCRIPTION OF THE DRAWINGS
The particular features and advantages of the invention as well as other objects will become apparent from the following description taken in connection with the accompanying drawings, in which;
FIG. 1 is a vertical fragmentary sectional view taken transversely through a portion of a multiple needle tufting machine embodying apparatus construction in accordance with the principles of the present invention and illustrating portions of the machine in somewhat diagrammatic form;
FIG. 2 is a fragmentary perspective view of the stitch forming instrumentalities of the tufting machine illustrated in FIG. 1;
FIG. 3 is a perspective view of a transfer looper of the present invention;
FIG. 4 is a sectional view taken substantially along the line 4--4 of FIG. 1 but with the needles in a descended position;
FIG. 5 is a fragmentary plan view of a looper bar constructed in accordance with one aspect of the present invention;
FIG. 6 is a schematic representation of the chain forming instrumentalities in an operative position preparatory to forming a loop;
FIG. 7 is a view similar to FIG. 6 disclosing a second operative position of the chain pile forming instrumentalities;
FIG. 8 is a view similar to FIG. 7 disclosing a third operative position;
FIG. 9 is a view similar to FIG. 8 disclosing a fourth operative position;
FIG. 10 is a view similar to FIG. 9 disclosing a fifth operative position;
FIG. 11 is a fragmentary plan view of a tufted chain loop fabric produced in accordance with the present invention; and
FIG. 12 is a fragmentary plan view of a tufted fabric having loop pile within concatenated chain loops as produced in accordance with the present invention.
DESCRIPTION OF THE PREFERRED EMBODIMENT
Referring now to the drawings, there is illustrated in FIG. 1 a portion of a tufting machine 10 having a frame comprising a bed 12 and a head 14 disposed above the bed. The bed 12 includes a bed plate 16 across which a fabric F is adapted to be fed by a pair of take-off rolls 18 and feed rolls 20.
Mounted in the head 14 for vertical reciprocation is one of a plurality of push rods 22 to the lower end of which a needle bar 24 is carried and which in turn carries a first set of a plurality of needles 26 and 28 in a first pair of transverse rows and a second set of a plurality of needles 30 and 32 in a second pair of transverse rows spaced downstream of the needles 26 and 28 in the direction of fabric feed. The needles are adapted to penetrate the fabric through wire support fingers 34 positioned across an opening in the bed plate 16 upon reciprocation of the needle bar to carry yarn Y therethrough and projects loops of yarn from the fabric. Endwise reciprocation may be coventionally imparted to the push rods 22 and thus the needle bar by a link 36 pivotably connected at its lower end to the push rods and at its upper end to an eccentric 38 on a driven rotary main shaft 40 that is journalled transversely through the head 14. Yarn jerkers 42 and 44 are carried by the needle bar 24 and operate to engage yarn between the respective rows of needles 26, 28 and 30, 32 and respective conventional yarn feed mechanisms (not illustrated) for each transverse pair of needle rows.
Mounted within the bed for cooperation with the needles 26, 28 are a plurality of conventional loop pile loopers 46,48 which have bills which point in the direction of fabric feed, the loopers 46 cooperating with the needles 26 and the loopers 48 cooperating with the needles 28 to seize loops of yarn presented by the needles. The loopers 46,48 have mounting portions receivable within respective slots 50, 52 in a looper bar 54. Secured to the looper bar 54 is one half of a plurality of two piece clamps 56 which are secured by screws 58 about a looper shaft 60 journalled in the bed substantially parallel to the main shaft 40. The looper shaft 60 is conventionally oscillated or rocked in a back and forth manner in timed relationship with the reciprocation of the needles so that the hooks of the loopers 46,48 enter the respective loops presented by the needles 26,28, seize the loops, and as the loopers rock away from the needle path as the needles ascend, shed the loops which are moved downstream along with the fabric F. To simplify the disclosure, the means for oscillating the looper shaft is not illustrated since this is notoriously well known in the tufting art and any conventional means can be utilized with the present invention. One means for accomplishing this may be a cam and lever means driven off the main shaft 40.
In accordance with the present invention a second or transfer looper 62 is mounted to cooperate with the looper 46 and a second or transfer looper 64 is mounted to cooperate with the looper 48. The loopers 62 and 64 have respective free end portions 66,68 including bills 70,72 which point oppositely to the direction of fabric feed and thus oppositely to the bill portions of the loopers 46, 48. The loopers 62,64 are positioned downstream of respective loopers 46,48 as hereinafter described in further detail, and are oscillated out of phase with the loopers 46,48. Thus, as the loopers 46, 48 rock toward the center line of the needle path from a first side thereof the loopers 62 and 64 rock away from the center line of the needle path from the same direction. In the preferred embodiment of the invention this out of phase oscillation is simply provided by mounting the loopers 62,64 in the same looper bar 54 as the loopers 46,48.
With the exception of an undercut 74 the shank 76 to form the mounting portion of the loopers 62, for purposes hereafter described, the loopers 62 and 64 are identical in construction and only looper 62 will be described in detail.
As best illustrated in FIG. 3 the loopers 62 comprise an upstanding shank 76 the lower end of which is the mounting portion receivable within slots 78 in the looper bar 54, (slots 79 receiving the loopers 64) and from the top of which the free end 66 in the form of an arm or blade 80, angularly extends and terminates in the bill 70. The blade 80 has a bend 82 such that the plane of the bill 70 is laterally offset from the plane of the shank 76. The leading edge or tip 83 above the bill 70 is disposed downwardly from the top edge and the rear portion of the bill has an edge 84 disposed downwardly beyond the lower edge 86 of the tip of the bill. The edge 84 defines a throat beyond which a loop of yarn seized by the bill 70 is prevented from moving and the bottom edge 86 is the edge against which the loop is seized. The length of the shank 76 is longer than the shanks of the loopers 46 and 48 such that when the loopers 62 and 64 are inserted within their respective slots 78 and 79 in the looper bar 54 the bill 70 is disposed closer to the backing fabric F than the free end bill portions of the loopers 46 and 48. Moreover, the slots 78 and 79 are offset from the slots 50 and 52 with each slot 78,79 transversely intermediate but spaced downstream from respective adjacent slots 50 and 52, the bend 82 being such that although the shanks 76 of the loopers 62,64 are offset from the shanks of corresponding loopers 46,48, the bill portions 70 of the loopers 62,64 are aligned with the bills of planar loopers 46,48. The bill 70 is not only laterally aligned with the corresponding looper 46, 48 but is of a length such that it is superposed over at least the leading tip of the bill of those loopers. Preferably, the length of the bill 70 is such that it overlays a portion of the bill of the respective looper 46,48 by some finite amount; good results being obtained when the bill 70 overlays about half of the bill of the respective cooperating looper 46,48.
The operation of the machine can best be understood with reference to FIGS. 6 through 10 which illustrate schematically portions of the stitch forming cycle for the system comprising the needle 26, the looper 46, and the transfer looper 62. With reference to FIG. 6, the needle 26 has already penetrated the base fabric F and descended to its maximum or deepest penetration. The looper bar which at this time is rocking in the counter-clockwise direction as illustrated, carries the bill of the looper 46 toward the needle center line, and the looper 62, which has a previous loop 88 held thereon against the throat 84 and the edge 86 of the bill 70, is rocking away from the needle path. The needle 26 during its descent has entered the loop 88 held on the looper 62 and is at the bend 82 of the looper 62 in the position illustrated in FIG. 4. After the needle begins its ascent, as illustrated in FIG. 7, the bill of the looper 46 has entered the new loop presented by the needle 26 as the looper bar 54 continues to rock counter-clockwise. At this point in the cycle the loop 88 is being released from the bill 70 of the looper 62 by the action of the looper 62 being rocked further from the needle center line and the loop being restrained from movement with the looper by the needle 26 and by the needle pushing against the bill 70. In FIG. 8 the looper bar 54 is illustrated at approximately its maximum counter-clockwise extent, and the new loop 90 has been seized by the bill of the looper 46. The loop 88 has been completely shed by the looper 62 and is concatenated as a chain link about the new loop 90. FIG. 9 illustrates the position of the stitch forming instrumentalities just after the needle has begun its descent and the looper bar 54 is rocking clockwise. The looper 46 is illustrated in the position as shedding the loop 90 from its bill onto the bill of the looper 62, while the previously formed loop 88 is secure against the base fabric F. In FIG. 10 the looper bar is continuing to rock clockwise with the looper 46 moving away from the needle center line. The needle 26 as it continues its descent is rearwardly of the bend 82 so easily passes through the loop 90 which has been seized and is being held by the bill 70 of the looper 62. The process is continued to form a succession of concatenated loops.
It should be understood that the needles 28 cooperate with the loopers 48 and the loopers 64 in the same manner as the needles 26 cooperate with the loopers 46 and 62. The needles 28 are offset in the direction transverse to the feed line of the base fabric to provide a staggered needle arrangement. Thus, as best illustrated in FIG. 2 the needles 26 are received within needle holes 92 in the needle bar 24 and the needles 28 are received within holes 94 offset transversely from the holes 92 downstream along the line of fabric feed. Consequently, the loopers 48 are offset from the loopers 46 by an amount similar to the offset or stagger between the needles 28 and 26, and the loopers 62 and 64 are similarly offset. The slots 50,52 78 and 79 in the looper bar 54, for manufacturing simplicity are cut into the looper bar the same depth along the line of feed. Thus, the loopers 48 include an undercut at 96 so that the loopers 46 and 48 may be otherwise identical, and the loopers 60 include the undercut 74. The depth of the undercut 74 and 96 being substantially equal to the offset or stagger between respective adjacent loopers.
The apparatus thus far described produces a fabric as illustrated in FIG. 11 wherein the needles 26 produce the concatenated loops L 1 and the needles 28 produce the concatenated loops L 2 . This product has exceptional coverage for the weight of yarn utilized, and when the larger size yarns are tufted the product provides a berber or crewel effect with full coverage and no portions of the base fabric visible. Moreover, when heavier yarns are tufted one leg of each loop overlies the other leg (depending upon the twist of the yarn) and gives a knitted appearance, and with certain yarns a herringbone appearance. Thus, attractive patterns can be produces by the utilization of yarns having different weights, sizes, twists, etc.
Another aspect of the present invention is the provision of the second set of staggered needels 30,32 which cooperate with another set of loopers 98 and 100 respectively. The loopers 98 and 100 being conventional loop pile loopers such as the loopers 46 and 48 and have bills which point in the direction the fabric feed. The loopers 98 and 100 are mounted within slots 102 and 104 respectively in the looper bar 54 at substantially the same downsteam location as the loopers 62 and 64, but the slots 102 are substantially transversely aligned with the slots 50, and the slots 104 are similarly aligned with the slots 52, so that the slots 102 and 104 are intermediate the slots 78 and 79 as illustrated in FIG. 5. With this construction a loop pile is formed every stroke of the machine which of course is equal to one stitch, and by proper spacing between the needles 26 and 30 and the needles 28 and 32, a loop tuft may be placed intermediate each pair of chain tufts, which ideally is at the previous penetration point of the base fabric. Thus, a unique fabric may be produced as illustrated in FIG. 12 with a pile loop L 3 at the intersection of each loop L 1 and a pile loop L.sub. 4 may be produced at the intersection of each pair of loops L 2 .
Numerous alterations of the structure herein disclosed will suggest themselves to those skilled in the art. However, it is to be understood that the present disclosure relates to the preferred embodiment of the invention which is for purposes of illustration only and not to be construed as a limitation of the invention. All such modifications which do not depart from the spirit of the invention are intended to be included within the scope of the appended claims. | Two tufted pile fabrics have pile tufts disposed on the base fabric in the form of rows of chains, with the chains in adjacent rows offset, one of the fabrics including loop pile that extend from between the chains. A tufting machine and method for producing the fabrics includes two staggered rows of needles with each needle cooperating with a primary looper and a transfer looper. The primary looper points in the direction of fabric feed while the transfer looper points in the opposite direction and has a bill above the bill of the primary looper and overlying a portion of it, the bill of the transfer looper being in a plane offset from its shank. The loopers rock oppositely to each other and when the primary looper sheds each loop it is seized and held by the transfer looper and entered by the needle as it descends to the primary looper. The transfer looper thereafter releases the loop which is concatenated about the succeeding loop. Another set of needles and loop pile loopers downstream from the first set produce the loop pile in the chain loops. | 3 |
RIGHTS OF THE GOVERNMENT
The invention described herein may be manufactured and used by or for the Government of the United States for all governmental purposes without the payment of any royalty.
BACKGROUND OF THE INVENTION
The present invention relates generally to explosive charge formulations and configurations and more particularly to a dual explosive charge formulation and configuration for enhancing blast pressure and fragmentation in a munition.
Previously existing customized explosives used for enhancing the blast or fragmentation characteristics of munitions have primarily been based on features of a target or set of targets. Blast performance is compromised in order to obtain high velocity fragments from very brisant or nearly ideal explosives (i.e., binders with nitramines). Fragmentation performance is compromised in order to obtain enhanced blast characteristics by replacing a portion of the nitramines with oxidizers and/or metal powders in non-ideal explosives. Total energy theoretically achievable from the non-ideal formulations is seldom realized experimentally. The rate of energy release from these formulations is relatively slow and many of the reactions occur relatively late compared with more nearly ideal explosives.
The invention solves or substantially reduces in critical importance problems with conventional explosive charge formulations and configurations by providing a dual explosive charge that simultaneously enhances blast and fragmentation characteristics in munition systems that commonly employ high explosive charges. The dual charge of the invention includes a cylindrical inner driven charge of a non-ideal explosive containing an inter-molecular composite mixture which includes fuels and/or oxidizers such as metal powders and/or oxidizers with a near stoichiometric blend of intra-molecular fuel ingredients such as trinitrotoluene. The inner charge is surrounded by an outer charge sleeve of a more nearly ideal explosive. Detonation of the outer charge results in super-confinement and/or shock pressure over-driving the inner charge and extremely high temperature, high pressure environment that accelerates the reaction kinetics for the inner charge, thereby allowing more reaction products to be formed earlier than for an unconfined charge of the same composition. With the proper inner-charge diameter and outer charge thickness, the outer charge maintains the fragment acceleration characteristics of a charge containing only the outer charge composition and allows blast performance to be enhanced while maintaining fragmentation performance by accelerating the reaction rate of the non-ideal explosive.
It is therefore a principal object of the invention to provide an improved explosive charge.
It is a further object of the invention to provide an explosive charge configuration having optimum blast pressure and fragmentation characteristics.
It is a further object of the invention to provide an explosive charge configuration having enhanced blast and fragmentation performance by accelerating the reaction rate of the explosive.
It is another object of the invention to provide an explosive charge for enhancing the performance of blast and fragmentation warheads and deep earth penetrating munitions.
These and other objects of the invention will become apparent as a detailed description of representative embodiments proceeds.
SUMMARY OF THE INVENTION
In accordance with the foregoing principles and objects of the invention, a dual explosive charge is described that simultaneously enhances blast and fragmentation characteristics of the charge, including an inner driven charge of a non-ideal explosive surrounded by an outer charge sleeve of a more nearly ideal explosive, detonation of the outer charge resulting in an extremely high temperature, high pressure environment that accelerates reaction kinetics in the inner charge, resulting in enhanced blast and fragmentation performance of the explosive charge.
DESCRIPTION OF THE DRAWINGS
The invention will be more clearly understood from the following detailed description of representative embodiments thereof read in conjunction with the accompanying drawings wherein:
FIG 1a is a view in axial section of a representative charge configuration of the invention which was used for the first series of blast pressure arena tests in demonstration of the invention;
FIG 1b is a view of the FIG 1a charge configuration taken along line B-B;
FIG. 2a shows schematically the test equipment arrangement for the blast pressure arena tests on the FIG 1a,1b charges;
FIG. 2b shows the location of pressure transducers in the FIG. 2a test equipment arrangement;
FIG. 3 shows graphs of shock wave time of arrival versus distance at each transducer position for blast pressure arena shot tests conducted in demonstration of the invention;
FIG. 4 shows graphs of peak pressure versus distance at each transducer position for blast pressure arena shot tests conducted in demonstration of the invention;
FIG. 5 shows graphs of impulse versus distance at each transducer position for blast pressure arena shot tests conducted in demonstration of the invention;
FIG. 6 shows graphs of log impulse versus cube root of distance from the test item at each transducer position for blast pressure arena shot tests conducted in demonstration of the invention;
FIG. 7 shows graphs of shockwave positive phase duration versus distance at each transducer position for blast pressure arena shot tests conducted in demonstration of the invention;
FIGS. 8a and 8b show schematic views in axial section of the test charge configurations for the subscale blast pressure/fragment velocity arena tests in demonstration of the invention;
FIG. 9 shows schematically the test equipment arrangement for the blast pressure/fragment velocity tests on the FIGS. 8a,8b test items;
FIG. 10 shows graphs of shock wave time of arrival versus distance at each sensor position for the blast pressure/fragmentation velocity tests conducted in demonstration of the invention;
FIG. 11 shows graphs of peak pressure versus distance at each sensor position for the blast pressure/fragmentation velocity tests conducted in demonstration of the invention;
FIG. 12 shows graphs of impulse versus distance at each sensor position for the blast pressure/fragmentation velocity tests conducted in demonstration of the invention;
FIG. 13 shows graphs of positive phase duration versus distance at each sensor position for the blast pressure/fragmentation velocity tests conducted in demonstration of the invention; and
FIG. 14 shows charts of average fragment velocity for each formulation used in demonstration of the invention.
DETAILED DESCRIPTION
Referring now to the drawings, FIGS. 1a and 1b show respective schematic axial sectional and a cross sectional views of a representative charge configuration according to the invention. The invention comprises a dual explosive charge 10 including an inner (driven) core 11 comprising a first explosive formulation surrounded by an outer layer or sleeve 12 comprising a second explosive formulation. It may be stated at the outset that though core 11 and sleeve 12 are herein described and depicted as having cylindrical shape, other geometrical shapes may be used, such as spherical, cubical and other, as would occur to the skilled artisan guided by these teachings within the scope of the claims. In accordance with a principal feature of the invention, core 11 may comprise a non-ideal explosive and sleeve 12 may comprise a more nearly ideal explosive. Accordingly, core 11 may comprise a non-ideal explosive containing an inter-molecular composite mixture including fuels and/or oxidizers such as metal powders and/or oxidizers with a near stoichiometric blend of intra-molecular fuel ingredients. Preferred core 11 formulations may therefore include ammonium perchlorate (AP) and aluminum powder (AL) combined with trinitrotoluene (TNT) and/or a nitramine (RDX or HMX) with or without a polymeric HTPB/wax binder system, that is, such as CHEMCORE (26% TNT/37% AP/37% AL) or PBXN-111 (20% RDX/43% AP/25% AL12% wax binder) or PWX MOD 19 (25% RDX/30% AP/33% AL/12% wax binder. Sleeve 12 may comprise a more nearly ideal explosive including a nitramine-based explosive in an inert or energetic binder system, such as PBXN-110 (88% HMX/12% HTPB binder or COMP B (59.5% RDX/39.5% TNT/1% wax desensitizer). Detonation of the outer charge comprising sleeve 12 results in super-confinement and/or shock pressure over-driving of the explosive charge comprising core 11.
Core 11 and sleeve 12 may be of substantially any diametric size and length, the same not considered limiting of the invention. Explosive charges fabricated in the practice of the invention may typically have a core 11 having a diameter of from about 4 inches to about 12 inches, and sleeve 12 may have a thickness of from about 3/4 to about 11/2 inches. However, it should be noted that in a preferred arrangement where the dual charge of the invention is most effective, the ratio of the volume of core 11 to that of sleeve 12 is as large as possible, and preferably from about 0.75 to about 3.0. Factors which dictate the minimum thickness of sleeve 12 include failure diameter of the outer charge explosive formulation, containment material and thickness, and the confining pressure required to accelerate the reaction in the inner charge comprising core 11. The sleeve 12 explosive should have a higher (5-40%) detonation velocity than that of the core 11 formulation.
The dual explosive charge configuration of the invention may be prepared by casting and machining (if necessary) core 11 to the desired shape and dimensions, and placing core 11 concentrically within a tubular container of preselected size according to the outer dimension of sleeve 12. The sleeve 12 explosive is then cast around core 11 inside the container. It may be preferable to form core 11 with a slight taper in order to facilitate casting of the sleeve 12 explosive and to streamline the sleeve 12 detonation path.
A first series of blast pressure arena shot tests was conducted on explosive charges comprising substantially unconfined 7-inch diameter/16-inch long charges of PWX MOD 19, PBXN-110 and a dual explosive charge consisting of a 4-inch diameter core 11 of PWX MOD 19 surrounded by a sleeve 12 of PBXN-110. A schematic in axial section of the charge configuration for these tests is shown in FIG 1a and a cross section of a test charge 10 is shown in FIG 1b. In the tests, each test charge 10 was initiated using an RP-80 detonator 13, a 1-inch by 1-inch Comp A-5 pellet 14, a 2-inch diameter by 2-inch long Comp B booster 15, and a 7-inch diameter by 1-inch thick Comp B pad 16. Each dual explosive test charge 10 was contained in a thin 0.25 inch thick walled phenolic tube 17 which provided minimal confinement.
FIG. 2a shows schematically the test equipment arrangement 20 for the blast pressure arena tests on test charges 10. Test charge 10 was positioned vertically on wooden stand 21 on center 51 inches above ground level. Stand 21 was mounted on base 22 of 6 feet×6 feet×4 inch thick, rolled homogeneous armor plate. Piezoelectric pressure sensor transducers 23a-f,24a-f were placed substantially as shown in FIG. 2b along two orthogonal gauge lines at 25, 35, 35.5, 45, 55 and 65 feet from and along the centerline height (51 inches) of test charge 10. Barometric pressure, wind speed and direction and temperature were recorded using on-site monitors. Pre- and post-test calibrations were performed for each shot.
Table 1 is a summary of blast pressure shot test performance data comparisons for the blast pressure arena tests, and show the peak pressure obtained for the dual explosive charge to be the same as that for PWX MOD 19. The impulse derived from the dual explosive charges was only 93% of that obtained for PWX MOD 19. The peak pressure and impulse from the dual explosive charge were 4% and 5% greater than those obtained from the PBXN-110 charge. Success criteria for the tests was maintaining the blast performance of PWX MOD 19.
Blast pressure data from individual shots are shown in Tables 2-4. Table 2 shows data from Shot 1 comprising 39.4 lbs of PWX MOD 19, shot conditions, temperature 75° F., barometric pressure 30.15 inches, wind 10 mph ENE. Table 3 shows data from Shot 2 comprising 36.03 lbs of PBXN-110 with PWX MOD 19 core, shot conditions, temperature 73° F., barometric pressure 30.08 inches, wind 11 mph ENE. Table 4 shows data from Shot 3 comprising 36.30 lbs of PBXN-110, shot conditions, temperature 73° F., barometric pressure 30.02 inches, wind 5 mph ESE. Blast pressure data at each transducer position are shown in FIGS. 3-7. FIG. 3 shows graphs of shock wave time of arrival versus distance. FIG. 4 shows graphs of peak pressure versus distance. FIG. 5 shows graphs of impulse versus distance. FIG. 6 shows graphs of log impulse versus cube root of distance from the test item. FIG 7 shows graphs of shockwave positive phase duration versus distance.
Table 1 and FIGS. 3-6 show that shockwave time-of-arrival does not discriminate between the three test charges. Peak pressures from the dual charge system were equivalent to those from the PWX Mod 19 charge. Both the dual charge 10 system and the PWX Mod 19 charge showed 4-5% enhancement of peak pressure relative to PBXN-110. Impulses measured for the dual charge 10 system were about 7% below those from the PWX Mod 19 charge. Impulses for the dual charge 10 system were 5% greater than those from PBXN-110 while those from PWX Mod 19 were 13% greater than PBXN-110. Positive phase durations yield the same ranking of the three charges.
The dual charge 10 of the invention provides a promising approach for increasing blast performance of an ordnance package while maintaining metal acceleration characteristics. The impulses measured for confined charges of PBXW-114 (78% HMX/10% AL/12% HTPB binder) were 18±0.0003% greater than those from PBXN-110 and 2 ±0.0003% greater than those from PBXN-109 (64% RDX/20% AL/16% HTPB binder).
A series (13) of subscale blast pressure/fragment velocity arena test shots was conducted on seven explosive composition test charges 80,81 shown schematically in axial section in FIGS. 8a and 8b. Test item 80 comprised an inner four-inch diameter core 83 of PWX Mod 19 or CHEMCORE and a sleeve 84 of PBXN-110. Test charge 81 comprised an eight-inch diameter cylinder 86 of PWX MOD 19, PBXN-110, APET 257 (25% RDX/30% AP/33% AL/12% HTPB binder), APET 257-4 (25% ultrafine RDX/30% AP/33% AL/12% HTPB binder), or AFX-625 (25% HMX/25% NTO(3-nitro-1,2,4-triazol-5-one)/25% AL/25% TNT). Test charges 80,81 were encased in mild steel tubes 87,87' eight inches OD by 16 inches long and 0.5 inch wall thickness. It is noted that the inner core charge may also be enclosed in a metal tube to provide additional confinement of the inner charge and additional metal mass to be projected upon detonation. The formulations used are shown in Table 5 and air blast fragmentation velocity performance rankings for the tests are shown in Table 6. In the tests, each test charge was initiated using an RP-80 detonator, 1-inch by 1-inch Comp A-5 pellet, 2-inch diameter by 2-inch long Comp B booster, and 7-inch diameter by 1-inch thick Comp B pad similarly to the blast pressure arena tests described above.
FIG. 9 shows schematically test equipment arrangement 90 for the blast pressure/fragment velocity tests. Each test item 80,81 was positioned vertically on center 6 feet above ground level on a wooden stand 91 mounted on base 92 of 6 feet×6 feet ×4-inch thick, rolled homogeneous armor plate. Piezoelectric pressure sensors 93a-f,94a-f were placed similarly to sensors 23,24 of FIG. 2b along the centerline height (six feet) of test items 80,81. In addition, two fragment velocity screens 89 were placed 34 feet behind the test items substantially as shown in FIG. 9, and a one-foot high ricochet fence (not shown in the drawings) consisting of sandbags was positioned 25 feet from the test charges. Weather data (temperature, dew point, wind direction/speed, relative humidity, barometric pressure) were monitored and recorded.
Air blast and fragmentation velocity data from individual shots are shown in Tables 7-10. Data from each sensor position are shown in FIGS. 10-13. FIG. 10 shows graphs of shock wave time of arrival versus distance. FIG. 11 shows graphs of peak pressure versus distance. FIG. 12 shows graphs of impulse versus distance. FIG. 13 shows graphs of positive phase duration versus distance.
The weighted, average fragment velocity and velocity range for each formulation/configuration is shown in FIG. 14 and Table 11. Of the formulations tested in this series, AFX-625 generated the highest velocity fragments and superior air blast characteristics. The dual explosive charges accelerated the fragments to a higher velocity than the PBXN-110 charges. The results suggested that the ratio of non-ideal to ideal explosive must be large. (The PBXN-110 used in the test series herein contained HMX ground to 2 microns, which meets the specification for PBXN-110, but restricting the HMX particle size distribution in this manner could influence both performance and sensitivity characteristics). The dual explosive charges with a core of PWX Mod 19 and a shell of PBXN-110 provided enhanced fragment velocities relative to PWX Mod 19 alone. The dual explosive charges provided improved airblast characteristics when compared to PBXN-110. However, in the case of the PWX Mod 19 core charge with the PBXN-110 shell, the charge failed to achieve the airblast characteristics of PWX Mod 19 alone. This energy enhancement may contribute to the improved fragment velocities observed for the dual explosive charges, however, it did not result in enhanced air blast characteristics. The CHEMCORE composition was developed to maximize the AP/Al available in an energetic binder system, and in every instance outperformed the PWX Mod 19 Core charge of the same dimensions.
The invention therefore provides a dual explosive charge formulation and configuration for enhancing blast pressure and fragmentation in a munition. It is understood that modifications to the invention may be made as might occur to one with skill in the field of the invention within the scope of the appended claims. All embodiments contemplated hereunder that achieve the objects of the invention have therefore not been shown in complete detail. Other embodiments may be developed without departing from the spirit of the invention or from the scope of the appended claims.
TABLE 1______________________________________ Dual Charge/ Dual charge/ PWX Mod 19/Parameter PWX Mod 19 PBXN-110 PBXN-110______________________________________Shockwave Time of 1.00 ± 0.00 1.00 ± 0.01 1.01 ± 0.01Arrival RatiosPeak Pressure Ratios 1.00 ± 0.07 1.04 ± 0.10 1.05 ± 0.11Impulse Ratios 0.93 ± 0.07 1.05 ± 0.07 1.13 ± 0.05Positive Phase 0.93 ± 0.06 0.97 + 0.09 1.04 ± 0.08Duration Ratios______________________________________
TABLE 2______________________________________ Time of Peak Positive Phase Distance Arrival Pressure Impulse (psi- DurationGauge (ft) (msec) (psi) msec) (msec)______________________________________1 25 7.81 26.95 42.79 5.132 35 13.80 15.50 41.60 6.893 35.5 14.13 13.64 39.16 7.424 45 20.65 10.01 32.57 9.345 55 27.98 5.50 22.25 9.316 65 35.72 4.20 17.77 10.117 25 7.81 27.40 47.57 5.408 35 13.80 12.22 33.96 7.059 35.5 14.13 12.94 37.04 7.8810 45 20.65 8.17 27.89 8.9011 55 27.9812 65 35.72 11.30______________________________________
TABLE 3______________________________________ Time of Peak Positive Phase Distance Arrival Pressure Impulse (psi- DurationGauge (ft) (msec) (psi) msec) (msec)______________________________________1 25 7.75 28.52 43.68 4.922 35 13.66 14.01 35.00 6.413 35.5 14 12.19 32.81 6.394 45 20.5 9.34 29.1 7.625 55 27.836 65 35.6 4.22 16.45 10.107 25 7.77 28.15 5.098 35 13.84 13.29 33.57 6.929 35.5 14.17 13.61 35.81 6.8410 45 20.80 8.44 26.62 8.4411 55 28.22 6.25 25.68 10.9412 65 36.01 4.24 18.97 11.28______________________________________
TABLE 4______________________________________ Time of Peak Positive Phase Distance Arrival Pressure Impulse (psi- DurationGauge (ft) (msec) (psi) msec) (msec)______________________________________1 25 7.62 28.73 40.29 5.132 35 16.51 15.47 37.32 7.253 35.5 13.85 13.00 34.04 7.84 45 20.45 7.66 26.59 8.765 55 27.94 4.89 19.97 9.186 65 35.86 3.86 15.98 10.167 25 7.87 30.98 40.65 4.468 35 13.77 12.40 30.80 6.819 35.5 14.10 12.32 31.69 6.7810 45 20.70 7.72 25.14 8.6111 5512 65 35.96 4.04 17.84 10.93______________________________________
TABLE 5______________________________________Designation Composition/Configuration______________________________________PBXN-110 (2 micron HMX/HTPB (88/12)HMX)-2 shotsPWX Mod 19-2 shots Polywax/Al/AP/RDX (12/33/30/25)PWX Mod 19 Core/PBXN- 4.5-inch Diameter Core of PWX Mod 19110 Shell-2 shots Surrounded by PBXN-110 (See FIG. 8a)APET 257-4-2 shots HTPB/RDX/AP/Al (12/25/30/33), 4 micron RDXAPET 257-1 shot HTPB/RDX/AP/Al (12/25/30/33), Class V RDXCHEMCORE/PBXN-110 4.5-inch Diameter Core of CHEMCOREShell-2 shots TNT/AP/Al (26/37/37), Surrounded by PBXN-110 (see FIG. 8a)AFX-625-2 shots TNT/HMX/NTO/Al (25/25/25/25)______________________________________
TABLE 6______________________________________Performance Ranking______________________________________Peak Pressure APET 257-4 > AFX-625 > PWX Mod 19 > CHEM- CORE > APET 257 > PWX Mod 19 Core > PBXN-110Impulse AFX-625 > APET 257-4 > APET 257 > PWX Mod 19 > CHEMCORE > PWX Mod 19 Core > PBXN-110Shockwave AFX-625 > APET 257-4 > APET 257 > PBXN-110 >Velocity CHEMCORE > PWX Mod 19 > PWX Mod 19 CorePositive Phase AFX-625 > APET 257-4 > APET 257 > PWX Mod 19 >Duration CHEMCORE > PWX Mod 19 Core > PBXN-110Fragment AFX-625 > CHEMCORE > PWX Mod 19 Core >Velocity PBXN-110 > PWX Mod 19 > APET 257-4 > APET 257______________________________________
TABLE 7__________________________________________________________________________Distance PWX Mod PWX Mod APET CHEM-(feet)PBXN-110 19 19 Core 257-4 APET 257 CORE AFX-625__________________________________________________________________________25 9.02 ± 1.18 9.40 ± 9.40 9.73 ± 0.19 9.37 ± 0.08 9.56 ± 0.11 9.55 ± 0.09 9.09 ± 0.1135 16.19 ± 2.01 16.23 ± 0.16 46.59 ± 0.20 15.57 ± 0.51 15.54 16.28 ± 0.15 15.74 ± 0.1435.5 16.40 ± 2.06 16.55 ± 0.16 17.00 ± 0.18 16.26 ± 0.14 16.33 16.55 ± 0.21 15.88 ± 0.2145 21.91 ± 3.28 23.34 ± 0.28 23.96 ± 0.10 22.86 ± 0.11 22.84 ± 0.17 22.93 ± 0.76 22.21 ± 0.9255 31.25 ± 1.28 30.91 ± 0.15 31.64 ± 0.08 30.18 ± 0.61 30.77 ± 0.23 31.07 ± 0.02 29.68 ± 0.6765 39.66 ± 1.29 38.77 ± 0.10 39.55 ± 0.15 38.36 ± 0.12 38.70 ± 0.31 38.70 ± 0.19 37.68 ± 0.06__________________________________________________________________________
TABLE 8__________________________________________________________________________Distance PWX Mod PWX Mod APET CHEM-(feet)PBXN-110 19 19 Core 257-4 APET 257 CORE AFX-625__________________________________________________________________________25 10.94 ± 0.75 14.82 ± 2.30 13.38 ± 1.85 16.01 ± 2.58 14.64 ± 1.31 14.60 ± 2.69 15.93 ± 2.1135 8.96 ± 1.77 10.96 ± 0.82 9.12 ± 1.53 11.96 ± 2.09 8.44 10.21 ± 1.11 10.14 ± 2.3235.5 7.55 ± 0.82 9.70 ± 0.41 8.25 ± 0.40 10.88 ± 1.09 9.09 9.10 ± 0.32 9.69 ± 0.8745 5.87 ± 1.86 7.60 ± 0.76 6.48 ± 1.46 7.84 ± 0.40 6.80 ± 0.33 6.95 ± 0.46 8.63 ± 3.9755 3.79 ± 0.44 4.68 ± 0.51 4.13 ± 0.52 4.66 ± 0.17 4.16 ± 0.37 4.50 ± 0.10 3.97 ± 1.2565 2.88 ± 0.67 3.51 ± 0.38 3.10 ± 0.56 3.61 ± 0.26 3.50 ± 0.58 3.16 ± 0.19 3.69 ± 0.01__________________________________________________________________________
TABLE 9__________________________________________________________________________Distance PWX Mod PWX Mod APET CHEM-(feet)PBXN-110 19 19 Core 257-4 APET 257 CORE AFX-625__________________________________________________________________________25 27.09 ± 2.77 39.74 ± 0.79 33.19 ± 1.11 39.57 ± 1.04 42.60 ± 0.21 35.48 ± 0.83 41.18 ± 2.6335 21.40 ± 0.42 30.68 ± 1.43 25.77 ± 1.79 31.83 ± 4.15 29.82 27.72 ± 1.17 30.89 ± 2.8935.5 22.42 ± 1.39 30.16 ± 2.81 26.36 ± 0.57 30.42 ± 1.63 26.32 26.60 ± 0.60 28.59 ± 0.7045 15.26 ± 5.65 24.26 ± 0.91 22.89 ± 2.32 27.60 ± 3.32 29.17 ± 6.72 22.72 ± 6.21 27.85 ± 5.7555 13.71 ± 1.30 20.44 ± 0.76 17.32 ± 0.16 19.48 ± 0.35 20.91 ± 0.11 18.47 ± 0.39 23.02 ± 3.9665 10.24 ± 3.64 17.35 ± 0.93 14.35 ± 0.65 17.65 ± 0.73 17.43 ± 1.17 15.50 ± 0.44 17.77 ± 0.19__________________________________________________________________________
TABLE 10__________________________________________________________________________Distance PWX Mod PWX Mod APET CHEM-(feet)PBXN-110 19 19 Core 257-4 APET 257 CORE AFX-625__________________________________________________________________________25 5.73 ± 0.38 6.51 ± 0.34 5.91 ± 0.49 6.07 ± 0.18 5.76 ± 0.50 5.78 ± 0.53 6.20 ± 0.8035 6.58 ± 0.56 7.75 ± 0.63 7.09 ± 0.41 7.98 ± 1.41 8.02 7.33 ± 0.21 8.04 ± 0.7135.5 6.88 ± 0.17 8.15 ± 1.77 7.17 ± 0.58 7.86 ± 0.77 7.89 7.40 ± 0.17 7.87 ± 0.6545 7.07 ± 0.40 9.24 ± 0.06 9.27 ± 1.28 10.32 ± 1.88 11.77 ± 4.12 9.30 ± 0.45 10.33 ± 3.1255 8.06 ± 0.43 10.33 ± 0.44 9.53 ± 0.37 10.52 ± 0.50 10.25 ± 0.69 10.20 ± 0.24 11.40 ± 1.3565 9.39 ± 0.25 10.83 ± 0.83 10.28 ± 0.71 11.18 ± 0.49 10.48 ± 1.08 10.96 ± 0.76 10.82 ± 0.23__________________________________________________________________________
TABLE 11______________________________________Formulation/ Velocity Range Average NumberConfiguration (fps) of Hits per Screen______________________________________PBXN-110 4843-6317 16PWX Mod 19 4752-5504 12PWX Mod 19 4388-5820 14CoreAPET 257-4 3750-5426 11APET 257 3032-5395 11CHEMCORE 4012-5641 13AFX-625 3864-6148 15______________________________________ | A dual explosive charge is described that simultaneously enhances blast and fragmentation characteristics of the charge, including an inner driven charge of a non-ideal explosive surrounded by an outer charge sleeve of a more nearly ideal explosive, detonation of the outer charge resulting in an extremely high temperature, high pressure environment that accelerates reaction kinetics in the inner charge, resulting in enhanced blast and fragmentation performance of the explosive charge. | 5 |
CROSS-REFERENCE TO RELATED APPLICATIONS
This is a divisional of U.S. patent application Ser. No. 10/632,744, filed Aug. 1, 2003 now U.S. Pat. No. 6,966,157.
STATEMENT REGARDING FEDERALLY SPONSORED RESEARCH OR DEVELOPMENT
Not Applicable.
BACKGROUND OF THE INVENTION
1. Field of the Invention
The invention is generally related to roofing skylights and more specifically to modularly integrated skylights for standing seam roofs.
2. Description of the Related Art
Skylights installed in roofs are widely practiced. In roofs with a standing seam roofing system prior art skylights have been affixed to adjacent roof panels by utilizing the standing seams of those roof panels.
U.S. Pat. No. 4,649,680 issued to Weisner et al. on Mar. 17, 1987, discloses a skylight system for a standing seam roof in which plastic skylight sections are formed to have the same width as a standard metal roof panel and shaped to integrate into the standing seam roof in place of a standard metal roof panel between two standing seams. U.S. Pat. No. 4,117,638 issued to Kidd, Jr. et al. on Oct. 3, 1978, discloses a skylight panel where the transparent panel is shaped to clip into the standing rib interface in place of a metal central panel.
U.S. Pat. No. 4,730,426 issued to Weisner, et al. on Mar. 15, 1988 discloses a skylight for a barrel tile roof. The skylight is made of plastic and folded along the edges to mate with the standing seams on each side of the skylight. The width of the skylight is the width of an integral number of roof tiles, creating joints at each standing seam.
Other prior art skylights are installed into the flat portion of the roof panel between the standing seams.
U.S. Pat. No. 5,323,576 issued to Gumpert et al. on Jun. 28, 1994, discloses a skylight system for use on metal standing seam roofs. The skylight is curbless and integrates into the flat metal panel between two adjacent standing seams. The roof panel is cut and the edges are folded back to form a lip over which a bubble-shaped covering is placed and sealed. In this manner, material is shed off the roof between the two standing seams and able to flow past the skylight.
U.S. Pat. No. 4,848,051 issued to Weisner et al. on Jul. 18, 1989, discloses a low profile skylight for a shingled sloping roof with a unitary rectangular frame having an upstanding standing seam element along each longitudinal edge. Head and sill flashings are provided to seal the remaining perimeter of the skylight.
U.S. Pat. No. 4,860,511 issued to Weisner et al. on Aug. 29, 1989, discloses a curbless skylight having a central dome and a pair of standing seam edges suitable for installation in a metal standing seam roof, wherein the standing seam edges are joined to adjacent metal standing seams with the same covered by battens.
It would be an improvement to the field to provide a skylight for standing seam roofs that spans across at least one standing seam, and integrated into a section of the standing seam panels, so as to be installed into the roof as a unitary component. It would be an improvement to the field to have the skylight assembly match the color of the metal standing seam roof.
BRIEF SUMMARY OF THE INVENTION
Accordingly, the objects of my invention are to provide, inter alia, a skylight for a standing seam roof that:
integrates into the standing seam connection system of the remainder of the roof; accommodates a skylight panel that may span at least one standing seam; and integrates into different types of standing seam connectors.
Other objects of my invention will become evident throughout the reading of this application.
My invention is a skylight for a standing seam roof comprising a durable gauge skylight panel frame integrated into at least one section of the particular roofing material being used.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a top view of the preferred embodiment of the skylight assembly for a standing seam roof.
FIG. 2 is a cross-sectional view of the preferred embodiment of the skylight frame interlocking with modified standing seam roof panels.
FIG. 3 is an enlarged cross-sectional view of an embodiment of the skylight frame interface with a modified standing seam roof panel.
FIG. 4 is an enlarged cross-sectional view of an embodiment of the skylight frame interface with top end piece and a water diverter.
FIG. 5 is a perspective view of an embodiment of the skylight frame assembly.
FIG. 6 is a top view of a partially modified roof panel.
FIG. 7 is a top view of a partially modified roof panel.
FIG. 8 is a perspective view of a modified roof panel.
FIG. 9 is a perspective view of a notch and cap on the lower edge of the skylight assembly.
FIG. 10 is a perspective view of a prior art standing seam connection.
FIG. 11 is a side view of a prior art standing seam connection.
DESCRIPTION OF THE INVENTION
The preferred embodiment of my standing seam skylight assembly is shown in FIGS. 1-8 . The standing seam skylight assembly is depicted as 10 .
Referring to FIGS. 10 and 11 , a prior art typical standing seam 121 is shown. Typical standing seam 121 joins two typical roof panels 120 a and 120 b . Each roofing panel in a project has a typical inner connector 122 along one edge and a typical outer connector 123 along the opposing edge. FIG. 11 depicts typical standing seam 121 , which is created by inserting typical inner connector 122 along one side of typical roof panel 120 b into typical outer connector 123 of one side of typical roof panel 120 a in an interference fit. In this manner, many roofing panels can be joined to form a complete roof.
Referring to FIG. 1 , standing seam skylight assembly 10 is comprised of a skylight frame assembly 50 , two roof panels 20 a and 20 b , a top end piece 41 , and a bottom end piece 45 . Roof panels 20 a and 20 b are immediately adjacent opposing sides of skylight frame assembly 50 . Top end piece 41 and bottom end piece 45 are located between roof panels 20 a and 20 b and are immediately adjacent opposing ends of skylight frame assembly 50 . Top end piece 41 and bottom end piece 45 may partially overlap each roof panel 20 a and 20 b . Skylight assembly 10 has skylight assembly upper edge 12 and skylight assembly lower edge 15 . Skylight assembly upper edge 12 is at a higher elevation than skylight assembly lower edge 15 when skylight assembly 10 is integrated into a sloped roof.
Referring to FIG. 5 , the skylight frame assembly 50 comprises a skylight curb 70 and a translucent or transparent skylight panel 52 . Skylight frame assembly 50 has an upper end 62 , a lower end 64 , and two longitudinal sides 66 a and 66 b . Upper end 62 is that end with a higher elevation along the pitch of a sloped roof when skylight assembly 10 is installed in a sloped roof. Upper end 62 has a top frame width 63 . Lower end 64 has a lower frame width 65 . Lower end 64 and upper end 62 are along opposing ends of skylight frame assembly 50 . Each of the two longitudinal sides 66 a and 66 b extends between the extremities of upper end 62 and lower end 64 to form a rectangular frame shape. Skylight curb 70 houses skylight panel 52 . Skylight curb 70 has an inner periphery 69 defined as that part of skylight curb 70 immediately adjacent and surrounding skylight panel 52 . A skylight curb length 75 is the longitudinal length of skylight curb 70 .
Referring to FIGS. 3 and 5 , skylight curb 70 extends around skylight panel 52 and is C-shaped with the open portion of the “C” facing away from inner periphery 69 . In the exemplary embodiment, skylight curb 70 comprises a frame ledge 72 , a skylight curb side member 73 , a skylight curb top member 76 , and a skylight curb lip 77 . Skylight curb side member 73 encompasses inner periphery 69 of skylight curb 70 . Skylight curb side member 73 and frame ledge 72 are adjoined perpendicularly along a common edge while skylight curb top member 76 is adjoined perpendicularly to the opposing edge of skylight curb side member 73 . Frame ledge 72 and skylight curb top member 76 are positioned such that skylight curb top member 76 is parallel to and overhangs frame ledge 72 . A skylight curb height 74 is defined as the distance between facing surfaces of skylight curb top member 76 and frame ledge 72 . Skylight curb lip 77 is perpendicularly adjoined to skylight curb top member 76 along an outer coner 78 , distal skylight curb side member 73 and extends toward frame ledge 72 , thus forming a C-shape. A skylight curb width 79 is defined as the distance between facing surfaces of skylight curb side member 73 and skylight curb lip 77 .
Referring to FIGS. 2 and 3 , the exemplary embodiment of the interface, curb interface 30 , between skylight curb 70 and roof panels 20 a and 20 b is shown. Roof panels 20 a and 20 b are each adapted to interface with skylight curb 70 along longitudinal sides 66 a and 66 b.
Referring to FIGS. 6 and 7 , roof panels, 20 a and 20 b are shown. Roof panels 20 a and 20 b are selected from roofing panels that are to be used in the roofing project. Roof panels 20 a and 20 b are modified to accommodate skylight frame assembly 50 . As shown in FIG. 6 , to prepare roof panels 20 a and 20 b for assembly with skylight frame assembly 50 , the inner connector (not shown) of one roof panel 20 a is removed leaving an inner connector edge 24 , which is straight. An outer connector 23 remains along the edge opposing inner connector edge 24 . FIG. 7 shows roof panel 20 b with the outer connector (not shown) removed, leaving an outer connector edge 26 , which is also straight. An inner connector 22 remains along the edge opposite outer connector edge 26 . Outer connector 23 and inner connector 22 may be referred to herein as panel attachment members. Inner connector edge 24 and outer connector edge 26 may be referred to herein as frame interface edges.
Two slits 27 a and 27 b are cut into a panel surface 25 a of roof panel 20 a from inner connector edge 24 in a direction perpendicular to inner connector edge 24 . Similarly, two slits 27 c and 27 d are cut perpendicular to outer connector edge 26 from outer connector edge 26 into panel surface 25 b of roof panel 20 b . Some material along inner connector edge 24 outside slits 27 a and 27 b may be removed as may some material along outer connector edge 26 outside slits 27 c and 27 d.
The edge between slits 27 a and 27 b is a panel curb edge 88 a and the edge between slits 27 c and 27 d is a panel curb edge 88 b . The distance between slits 27 a and 27 b on roof panel 20 a is a panel curb length 87 a and between slits 27 c and 27 d on roof panel 20 b is a panel curb length 87 b . Panel curb lengths 87 a and 87 b are each equivalent to skylight curb length 75 plus an allowance for a curb thickness 35 , shown in FIG. 4 , which will be present at the interfaces between skylight curb 70 and top end piece 41 and skylight curb 70 and bottom end piece 45 , discussed below. The distance between panel curb edge 88 a and the ends of slit 27 a and 27 b is a slit length 28 , which is equivalent to the sum of skylight curb height 74 and skylight curb width 79 . Surface material between slits 27 a and 27 b and between slits 27 c and 27 d may have to be removed to accommodate top frame width 63 and lower frame width 65 while maintaining the proper slit length 28 . Panel surface 25 a between slits 27 a and 27 b on roof panel 20 a and panel surface 25 b between slits 27 c and 27 d on roof panel 20 b are bent to form a panel curb 80 , shown in FIG. 8 .
Referring to FIG. 8 , in the exemplary embodiment, panel curb 80 comprises a panel surface 25 a , a panel curb side 82 , and a panel curb lip 84 . Panel curb 80 is formed by bending roof panel 20 a along panel surface 25 a between slits 27 a and 27 b perpendicular to the panel surface 25 a to form panel curb side 82 . Panel surface 25 a is bent such that panel curb side 82 extends upwards, in the same direction as outer connector 23 along the edge opposite inner connector edge 24 of roof panel 20 a . Panel curb side 82 is then bent toward outer connector 23 of the roof panel 20 a so that it is parallel to and overhangs panel surface 25 a , thereby forming panel curb lip 84 . Thus, panel curb 80 is U-shaped. A panel curb end 86 is located along the free edge of panel curb lip 84 . Panel curb 80 has a height 83 and panel curb lip 84 has a width 85 . The height 83 of panel curb 80 and the width 85 of panel curb lip 84 are such that panel curb 80 has an edge shape firmly receivable within the shape of the skylight curb 70 . As shown in FIG. 3 , the U-shape of panel curb 80 fits within the C-shape of skylight curb 70 along longitudinal sides 66 a and 66 b . Roof panel 20 b is prepared in the same manner as roof panel 20 a with panel curb 80 formed along outer connector edge 26 between slits 27 c and 27 d.
Referring to FIG. 3 , the interface between roof panel 20 b panel curb 80 and skylight curb 70 is shown. Insulation 56 , which is optional, but preferably included, is also shown, snugly sandwiched between panel curb 80 and skylight curb 70 . Panel curb side 82 of panel curb 80 , abuts against the insulation 56 . The snug fit of insulation 56 against panel curb side 82 causes panel curb end 86 to press against the inside of skylight curb lip 77 at outer coner 78 . The tension between the U-shaped panel curb 80 and the C-shaped skylight curb 70 results in panel surface 25 b and frame ledge 72 abutting parallel, such that frame ledge 72 provides support and rigidity to panel surface 25 b.
Referring to FIG. 1 , top end piece 41 and bottom end piece 45 are shown along upper end 62 and lower end 64 of skylight frame assembly 50 . In the preferred embodiment, both top end piece 41 and bottom end piece 45 are made from one or more flat sheets of roofing material obtained with roof panels 20 a and 20 b for the roofing project. Thus, top end piece 41 and bottom end piece 45 match the color of the roofing project. Top and bottom end pieces 41 and 45 interface with top and lower ends 62 and 64 of skylight frame assembly 50 in a manner similar to the interface between roof panels 20 a and 20 b and skylight frame assembly 50 along longitudinal sides 66 a and 66 b.
FIG. 4 depicts the interface between top end piece 41 and skylight curb 70 . In the exemplary embodiment, top end piece 41 has a U-shaped curb section 42 along the side interfacing with skylight curb 70 and is otherwise flat. U-shaped curb section 42 of top end piece 41 interlocks with the C-shape of skylight curb 70 . Insulation 56 is preferably included between curb section 42 and skylight curb 70 . Curb thickness 35 is the thickness of insulation 56 plus the immediately adjacent surfaces of top end piece 41 and skylight curb side member 73 . The interface along lower end 64 of skylight frame assembly 50 with bottom end piece 45 is the same as that just described. Appropriate roofing sealer (not shown) is optional, but may be used where frame ledge 72 of skylight curb 70 and top and bottom end pieces 41 and 45 overlap. Roof panels 20 a and 20 b overlap top end piece 41 and bottom end piece 45 to provide additional support to the surface of roof panels 20 a and 20 b and to prevent leakage. Therefore, panel curb length 87 must allow for curb thickness 35 in addition to skylight curb length 75 .
Referring to FIGS. 1 and 4 , a water diverter 54 , also known as a cricket, may be affixed to top end piece 41 . Many types of water diverters 54 are practiced in the skylight industry and may be used to divert water around skylight frame assembly 50 . One type of water diverter 54 attaches to top end piece 41 at diverter attachment point 55 . From diverter attachment point 55 , water diverter 54 slants downward and is affixed to top end piece 41 . Water diverter 54 has a centrally-located fold 53 thereby forming two triangularly-shaped sloped surfaces 51 a and 51 b extending from fold 53 to top end piece 41 . Thus, water flowing down skylight assembly 10 is diverted from skylight frame assembly 50 , preventing leakage. Other styles of water diverters, which are not depicted, include components that have walls raised vertically from the roof panel surface rather than triangularly-shaped surfaces. The walls are positioned such that they direct flowing water away from the skylight frame assembly 50 .
Referring to FIGS. 1 and 9 , when skylight assembly 10 is used in a roofing project, skylight assembly lower edge 15 may be located such that it overlaps the top of other roofing panels (not shown) used in the project. Because skylight assembly 10 may be wider than the roofing panels in the project, one or more notches 59 are cut along the skylight assembly lower edge 15 to accommodate the standing seam(s) (not shown) of the lower adjacent roof panels (not shown). When skylight assembly 10 is the width of two roofing panels, one standing seam (not shown) is traversed by skylight assembly 10 and one notch 59 is cut along skylight assembly lower edge 15 . When skylight assembly 10 is the width of three roofing panels, two standing seams are traversed by the skylight assembly 10 and two notches 59 are cut along skylight assembly lower edge 15 and so on. Caps 58 are placed over the end of each of the lower adjacent standing seams. Other roofing panels in the project might be located such that they overlap skylight assembly upper edge 12 . When necessary, caps 58 are placed over the end of the standing seams of these roofing panels as well.
Referring again to FIG. 1 , skylight frame assembly 50 is constructed of material sufficiently rigid enough to support skylight panel 52 . Once skylight frame assembly 50 is integrated into roof panels 20 a and 20 b and top and bottom end pieces 41 and 45 , it can then be employed in a roofing project similar to other panels in the project, with outer connector 23 on roof panel 20 a connecting to an inner connector (not shown) of an adjacent roof panel (not shown) and inner connector 22 of roof panel 20 b connecting to outer connector (not shown) of an adjacent roof panel (not shown).
The foregoing disclosure and description of the invention is illustrative and explanatory thereof. Various changes in the details of the illustrated construction may be made within the scope of the appended claims without departing from the spirit of the invention. The present invention should only be limited by the following claims and their legal equivalents. | A skylight for a standing seam roof having a skylight panel housed in a frame with a vertically extending curb along two longitudinal and two lateral sides. The frame curb integrates on the longitudinal sides with U-shaped curbs formed into modified roof panels selected from the construction project. On the lateral sides, the frame curb integrates with curbs formed in two end pieces painted with the other roof panels in the project. Standing seams, which are raised above the surface of the roof, interconnect the regular roof panels. The modified roof panels interconnect with the standing seams of the regular roof panels. The lateral sides of the skylight assembly traverse at least one standing seam when integrated with the regular roof panels. | 4 |
BACKGROUND OF THE INVENTION
[0001] 1. Field of the Invention
[0002] The present invention relates to a method for manufacturing a groove of a substrate and a method for cutting off a substrate. In addition, the present invention relates to a method for manufacturing a semiconductor device. The semiconductor device corresponds to a device including a transistor.
[0003] 2. Description of the Related Art
[0004] In recent years, development of a semiconductor device including a transistor has been advanced. A semiconductor device is formed by forming a transistor over a substrate, and then cutting off the substrate.
[0005] In many cases, a substrate is cut off as follows. First, a groove (also referred to as a scribe line) is formed at the surface of the substrate by using a scribing device. Then, the substrate is forcibly cut off along the groove by using a cutting device. In addition, a substrate is cut off by using a laser beam (hereinafter, a laser beam is included in laser light) as follows. First, the substrate is selectively irradiated with a laser beam to locally heat the substrate. Then, the surface of the substrate which is heated is locally cooled by a cooling medium. Subsequently, a crack is formed by utilizing thermal stress which is generated in the substrate, and accordingly, the substrate is cut off (for example, see Patent Document 1)
[0000] [Patent Document 1] Japanese Patent Laid-Open No. 2001-64029
[0006] When a substrate is cut off by using a scribing device, there is a case where a groove is not formed in a desired shape due to a layer which is provided over the surface of the substrate. As a result, the substrate cannot be cut off in a desired shape, which results in reduction in a yield. In addition, the substrate is cut off by using press power; therefore, a crack is easily generated from the groove and the cutting surface is adversely affected (see a photograph showing a cutting surface of a glass substrate of FIG. 6D ). Also, a burr may arise when that the substrate is plastic. “Burr” is called a state that a corner of the substrate is unprocessed smoothly. The state is often beard-form. As described above, cutting off a substrate by using a scribing device has been a factor of generating an exterior problem of a cutting surface and reducing a yield. In addition, it has been difficult to form a scribe line in a polygonal shape or a rounded shape in cutting off a substrate by using a scribing device.
[0007] In addition, a cutter is used for a scribing device, and such a cutter becomes worn after using multiple times; therefore, it is necessary that the cutter is replaced. Since a cutter is expensive, it has been difficult to reduce manufacturing cost in using a cutter.
[0008] Moreover, when a substrate is cut off by using a laser beam, there are cases where the substrate is transformed due to heating and a crack is generated in the substrate due to stress which remains inside the substrate.
SUMMARY OF THE INVENTION
[0009] The present invention is made in view of the above problems. It is an object of the present invention to provide a method for manufacturing a groove of a substrate, a method for cutting off a substrate, and a method for manufacturing a semiconductor device, each of which can reduce a yield.
[0010] A method for manufacturing a groove of a substrate of the present invention includes steps of selectively emitting a laser beam to form the groove in the substrate. One feature of the present invention is that an ablation process is used. The ablation process utilizes a phenomenon in which a molecular bond in a portion irradiated with a laser beam, that is, the portion absorbing the laser beam is cut off, photodegraded, and evaporated is used. In other words, the method for manufacturing a groove of a substrate of the present invention is as follows. A substrate is irradiated with a laser beam, and then a molecular bond in a portion of the substrate is cut off, photodegraded, and evaporated; accordingly, the groove is formed.
[0011] A method for manufacturing a groove of a substrate of the present invention includes steps of selectively emitting a laser beam to form the groove in the substrate and selectively emitting a laser beam to the groove to cut off the substrate. An ablation process is used in the present invention, and a substrate is irradiated with a laser beam, a molecular bond in a portion of the substrate is cut off, photodegraded, and evaporated; accordingly, the substrate is cut off.
[0012] In addition, in the present invention, a substrate may be thinned by performing one or both of grinding and polishing to the substrate by using one or both of a grinding device and a polishing device. More specifically, the substrate may be thinned to be 100 μm or less by using one or both of the grinding device and the polishing device. By thinning the substrate, formation of a groove in the substrate and cutting off the substrate can be performed easily at short times.
[0013] According to one feature of the present invention, a method for manufacturing a semiconductor device uses the above method for manufacturing a groove of a substrate and the above method for cutting off a substrate. The method for manufacturing a semiconductor device of the present invention includes steps of forming a layer including a transistor over a substrate; forming a first insulating layer over the layer including the transistor; forming a conductive layer which is connected to a source region or a drain region of the transistor through an opening provided in the first insulating layer; forming a second insulating layer which covers the conductive layer; and cutting off the first insulating layer, the insulating layer which is provided in the layer including the transistor, the second insulating layer, and the substrate by selectively emitting a laser beam.
[0014] A method for manufacturing a semiconductor device of the present invention includes steps of forming a layer including a transistor over a substrate; forming a first insulating layer over the layer including the transistor; forming a conductive layer which is connected to a source region or a drain region of the transistor through an opening provided in the first insulating layer; forming a second insulating layer which covers the conductive layer; forming a groove in one or more of the first insulating layer, the insulating layer which is provided in the layer including the transistor, the second insulating layer, and the substrate by selectively emitting a laser beam; and cutting off the first insulating layer, the insulating layer which is provided in the layer including the transistor, the second insulating layer, and the substrate by selectively emitting a laser beam.
[0015] A method for manufacturing a semiconductor device of the present invention includes steps of forming a layer including a transistor over one of surfaces of a substrate; forming a first insulating layer over the layer including the transistor; forming a conductive layer which is connected to a source region or a drain region of the transistor through an opening provided in the first insulating layer; forming a second insulating layer which covers the conductive layer; polishing the other surface of the substrate; and cutting off the first insulating layer, the insulating layer which is provided in the layer including the transistor, the second insulating layer, and the substrate by selectively emitting a laser beam.
[0016] Note that a solid laser which can oscillate a laser beam having a wavelength of 1 to 380 nm which is a visible light region may be used for a laser. More preferably, an Nd: YVO 4 laser having a wavelength of an ultraviolet region may be used. It is because compared with other laser beams at a longer wavelength side, the Nd: YVO 4 laser beam having a wavelength of an ultraviolet region is more easily absorbed in a substrate and an ablation process can be performed.
[0017] Note that a glass substrate may be used for a substrate. It is because a glass substrate easily absorbs a laser beam of an ultraviolet region, and therefore, an ablation process is easily performed.
[0018] A method for cutting off the substrate or forming the groove in the substrate in the present invention can be applied to methods of fabricating a liquid crystal display device and an EL (OLED) display device or the like. Moreover, a method of cutting off the substrate or forming the groove in the substrate in the present invention can be applied to not only an active matrix type display device but also a passive matrix type display device. Note that the liquid crystal and the EL (OLED) display devices and the active matrix type and passive matrix type display devices also have insulating layers.
[0019] The present invention uses an ablation process; accordingly, forming a groove in an insulating layer which is provided in a substrate and over the substrate and cutting off the insulating layer which is provided in the substrate and over the substrate can be performed easily at short times, and a yield can be improved. Moreover, the present invention uses a laser beam; therefore, a process of such a desired shape as not only a simple square shape but also a polygonal shape or a rounded shape can be easily performed.
BRIEF DESCRIPTION OF THE DRAWINGS
[0000] In the accompanying drawings:
[0020] FIGS. 1A and 1B are views each explaining a semiconductor device of the present invention;
[0021] FIGS. 2A and 2B are views each explaining a semiconductor device of the present invention;
[0022] FIGS. 3A and 3B are views each explaining a semiconductor device of the present invention;
[0023] FIGS. 4A and 4B are views each explaining a semiconductor device of the present invention;
[0024] FIGS. 5A to 5 D are views each explaining a semiconductor device of the present invention;
[0025] FIGS. 6A to 6 D are photographs (SEM images) each showing a cutting surface of a glass substrate;
[0026] FIG. 7 is a view explaining a semiconductor device of the present invention;
[0027] FIGS. 8A to 8 F are views each explaining a semiconductor device of the present invention;
[0028] FIGS. 9A to 9 D are views each explaining a semiconductor device of the present invention;
[0029] FIGS. 10A to 10 C are views each explaining a semiconductor device of the present invention; and
[0030] FIGS. 11A and 11B are views each explaining a semiconductor device of the present invention.
DETAILED DESCRIPTION OF THE INVENTION
[0000] [Best Mode for Carrying Out the Invention]
[0031] Embodiment Mode of the present invention will be explained in detail using the accompanying drawings. However, the present invention is not limited to the description below, and it is easily understood by those skilled in the art that modes and details thereof can be modified in various ways without departing from the purpose and the scope of the present invention. Therefore, the present invention is not understood as being limited to the description in Embodiment Mode. Note that in the structure of the present invention which is hereinafter described, the reference numerals denoting the same portions are used in common in different drawings.
[0032] A method for manufacturing a semiconductor device of the present invention will be explained with reference to FIGS. 1A and 1B , FIGS. 2A and 2B , FIGS. 3A and 3B , FIGS. 4A and 4B , FIGS. 5A to 5 D, and FIGS. 6A to 6 D. Note that a case where six thin film integrated circuits are manufactured over a substrate 11 will be explained hereinafter. Further, a region where one thin film integrated circuit is provided in each of FIG. 1A , FIG. 2A , and FIG. 3A corresponds to a region 26 surrounded by a dashed line. FIG. 1B , FIG. 2B , and FIG. 3B correspond to cross-sectional views of point A to point B of FIG. 1A , FIG. 2A , and FIG. 3A , respectively.
[0033] First, an insulating layer 12 is formed over one of the surfaces of the substrate 11 (see FIG. 1B ). Next, a layer including a plurality of transistors 13 is formed over the insulating layer 12 , and then, insulating layers 15 and 16 are formed over the layer including the plurality of transistors 13 . Next, conductive layers 17 to 24 are formed, each of which is connected to a source region or a drain region of each of the plurality of transistors 13 through openings provided in the insulating layers 15 and 16 . Subsequently, an insulating layer 25 is formed so as to cover the conductive layers 17 to 24 .
[0034] The substrate 11 corresponds to a glass substrate, a plastic substrate, a silicon substrate, a quartz substrate, and the like. A glass substrate or a plastic substrate is preferably used as the substrate 11 . A glass substrate or a plastic substrate having 1 meter or longer on a side is easily manufactured, and a desired shaped glass substrate or plastic substrate is also easily manufactured. Therefore, when a large-sized square glass substrate or plastic substrate having 1 meter or longer on a side is used, for example, productivity can be considerably improved. Such merits are great advantages as compared with a case of using a circular silicon substrate.
[0035] The insulating layer 12 functions to prevent intrusion of an impurity from the substrate 11 . The insulating layer 12 is formed by a single layer or a stacked layer of a layer containing oxide of silicon or nitride of silicon by a sputtering method, a plasma CVD method, or the like. A material for the oxide of silicon is a substance containing silicon (Si) and oxygen (O), and silicon oxide, silicon oxide containing nitrogen, or the like corresponds thereto. A material for the nitride of silicon is a substance containing silicon and nitrogen (N), and silicon nitride, silicon nitride containing oxygen, or the like corresponds thereto. Note that the insulating layer 12 may not necessarily be formed when it is not necessary to be formed.
[0036] Each of the plurality of transistors 13 has a semiconductor layer 27 , an insulating layer 14 , and a conductive layer 29 which is a gate electrode. The semiconductor layer 27 has an impurity region 30 functioning as a source region or a drain region, and a channel formation region 31 . An impurity element imparting N-type or P-type is added to the impurity region 30 . Specifically, an impurity element imparting N-type (an element belonging to Group 15 of the periodic table, for example phosphorus (P) or arsenic (As)) or an impurity element imparting P-type (for example boron (B)) is added. The insulating layer 14 corresponds to a gate insulating layer.
[0037] Note that although only the plurality of transistors 13 are formed in the structure shown in the drawing, the present invention is not limited thereto. An element which is provided over the substrate 11 may be appropriately adjusted in accordance with an application of the semiconductor device. In a case of forming a semiconductor device having a function to transmit and receive electromagnetic waves, for example, only a plurality of transistors may be formed, or alternatively, a plurality of transistors and a conductive layer functioning as an antenna may be formed over the substrate 11 . Note that the conductive layer functioning as an antenna may not necessarily be formed by one layer but a multilayer. In addition, in a case of forming a semiconductor device having a function to store data, a plurality of transistors and a memory element (such as a transistor or a memory transistor) may also be formed over the substrate 11 . Also, in a case of forming a semiconductor device (such as a CPU or a signal generating circuit) having a function to control a circuit, generate a signal, or the like, a transistor may be formed over the substrate 11 . Moreover, other elements such as a resistor element and a capacitor element may be formed in addition to the above elements, if necessary. Note that in a case of forming a semiconductor device having a function to transmit and receive electromagnetic waves, only a plurality of transistors may be formed over the substrate 11 .
[0038] The insulating layers 15 and 16 are formed by a single layer or a stacked layer by an inorganic material or an organic material by using an SOG (spin on glass) method, a droplet discharging method, a screen printing method, or the like. For example, nitride of silicon containing oxygen may be formed as the insulating layer 15 , and oxide of silicon containing nitrogen may be formed as the insulating layer 16 .
[0039] Next, a laser beam is selectively emitted, that is, to a predetermined position, and grooves 32 are formed in one or more of the insulating layers 14 , 15 , 16 , and 25 that are provided in the layer including the substrate 11 , the insulating layer 12 , and the plurality of transistors 13 (see FIGS. 2A and 2B ). In the structure shown in the drawing, the insulating layers 12 , 14 , 15 , and 16 are cut off by a laser beam, and the grooves 32 are formed in the substrate 11 .
[0040] A laser medium, an excitation source, and a resonator are included in a laser. Any type of laser may be used in the present invention although a laser is classified into a gas laser, a liquid laser, and a solid laser according to a medium, and classified into a free electron laser, a semiconductor layer, and an X-ray laser according to the type of oscillation. Note that a gas laser or a solid laser is preferably used, and a solid laser is more preferably used.
[0041] A gas laser includes a helium-neon laser, a carbon dioxide laser, an excimer laser, and an argon ion laser. An excimer laser includes a rare gas excimer laser and a rare gas halide excimer laser. A rare gas excimer laser oscillates by three kinds of excite molecules: argon, krypton, and xenon. An argon iron laser includes a rare gas ion laser and a metal vapor ion laser.
[0042] A liquid laser includes an inorganic liquid laser, an organic chelate laser, and a pigment laser. In an inorganic liquid laser and an organic chelate laser, rare earth ions such as neodymium, which are utilized for a solid laser, are used as a laser medium.
[0043] A laser medium used in a solid laser is a solid base doped with active species functioning as a laser. The solid base is crystal or glass. The crystal is YAG (yttrium aluminum garnet crystal), YLF, YVO 4 , YAlO 3 , sapphire, ruby, or alexandrite. In addition, the active species functioning as a laser are, for example, trivalent irons (such as Cr 3+ , Nd 3+ , Yb 3+ , Tm 3+ , Ho 3+ , Er 3+ , and Ti 3+ ).
[0044] As a laser used in the present invention, a continuous wave laser or a pulse oscillation laser can be used. The irradiation condition of a laser beam (for example, frequency, power density, energy density, beam profile, or the like) are appropriately controlled in consideration of a thickness of the substrate 11 , the insulating layers 12 , 14 , and 15 , and a material thereof.
[0045] As a laser used when the substrate 11 is the glass substrate, a solid laser having a wavelength of 1 nm or more to 380 nm or less, which is an ultraviolet region, is preferably used. More preferably, an Nd:YVO 4 laser having a wavelength of 1 nm or more to 380 nm or less, which is an ultraviolet region, is used. It is because light is more easily absorbed in a substrate (especially a glass substrate) by using a laser having a wavelength of an ultraviolet region compared with other laser at a longer wavelength side, and an ablation process is easily performed. Moreover, it is because an ablation process is easily performed especially by using an Nd:YVO 4 laser. Also, a laser beam having a wavelength in a range of 1 nm or more to 350 nm or less may be used in case of a plastic substrate (for example, a substrate comprising polyethylene terephthalate). In this case, preferably an Nd:YVO 4 laser is also used.
[0046] Note that a laser irradiation device for emitting the above laser beam has a moving table, a substrate, a head portion, and a control portion. The moving table is provided with an adsorption hole. The substrate is held by the adsorption hole over the moving table. The head portion emits a laser beam which is emitted from a laser oscillation device through a laser head. The control portion positions the laser head at a random place over the surface of the substrate by moving one or both of the moving table and the head portion, and accordingly, a laser beam is emitted. Note that the control portion recognizes and determines a portion to be processed from a relative position on the basis of a mark for positioning over a substrate which is taken by a CCD camera.
[0047] Next, a laser beam is selectively emitted to cut off the substrate 11 , the insulating layers 12 , 14 , 15 , 16 , and 25 (see FIGS. 3A and 3B ). Or, these may dynamically be cut with a formed groove. Through the above process, a laminated body 33 including the substrate 11 and the plurality of transistors 13 can be obtained.
[0048] Subsequently, the laminated body 33 including the substrate 11 and the plurality of transistors 13 is sealed using films 34 and 35 if necessary (see FIG. 4A ). The films 34 and 35 are made of a material such as polyethylene, polycarbonate, polypropylene, polyester, vinyl, polyvinyl fluoride, vinyl chloride, ethylene vinyl acetate, urethane, or polyethylene terephthalate, or a fiber material (for example, paper). Each of the films may be a single layer or a stacked layer of a plurality of films. In addition, an adhesion layer may also be provided over the surface thereof. The adhesion layer corresponds to a layer containing an adhesive such as a polyester or polyolefin thermal flexible resin, a thermal curing resin, an ultraviolet curing resin, a vinyl acetate resin adhesive, a vinyl copolymer resin adhesive, an epoxy resin adhesive, a urethane resin adhesive, a rubber adhesive, or an acrylic resin adhesive.
[0049] Each surface of the films 34 and 35 may be coated with powder of silicon dioxide (silica). A waterproof property can be maintained even under a high temperature environment or a high humidity environment by coating. In other words, a function of humidity resistance can be obtained. In addition, the surface thereof may also be coated with a conductive material such as indium tin oxide. The material which is used for coating charges static electricity, and accordingly, the plurality of transistors 13 can be protected from static electricity. That is, a function of preventing static electricity can be obtained. Moreover, the surface thereof may also be coated with a material containing carbon as its main component (for example, diamond like carbon or carbon containing nitrogen). The strength is increased by coating, and accordingly, a semiconductor device can be prevented from deteriorating and being destroyed. In addition, the films 34 and 35 may also be formed from a material in which a material for a base material (such as a resin) and a material containing silicon oxide, a conductive material, or carbon as its main component are mixed. Moreover, the films 34 and 35 can obtain a function of preventing static electricity by applying a surface active agent over the surface, or alternatively, by directly adding the surface active agent into the films.
[0050] Each surface layer of the films 34 and 35 or each surface adhesion layer of the films 34 and 35 is melted by heat treatment, and accordingly, the plurality of transistors 13 are sealed with the films 34 and 35 . In addition, adhesion is performed by pressure treatment.
[0051] According to one feature of the present invention, a laminated body including the substrate 11 and the plurality of transistors 13 is provided between the films 34 and 35 . By the above feature, intrusion of harmful gas, water, or an impurity element can be suppressed. Therefore, deterioration or destruction of the plurality of transistors 13 is suppressed, and accordingly, the reliability can be improved.
[0052] Note that a conductive layer functioning as an antenna may be provided at one or both of the films 34 and 35 . When the laminated body 33 including the plurality of transistors 13 is sealed with the films 34 and 35 , the conductive layer over the films 34 and 35 and the plurality of transistors 13 may be electrically connected to each other. At this time, it is preferable to provide an exposed conductive layer for connection in the laminated body including the plurality of transistors 13 . Then, sealing is performed so that the conductive layer for connection and the conductive layer over the films 34 and 35 are in contact with each other. Accordingly, a semiconductor device capable of transmitting and receiving electromagnetic waves can be provided.
[0053] Note that the substrate 11 may be thinned by performing one or both of grinding and polishing to the other surface of the substrate 11 by using one or both of a grinding device (for example, a grinding machine) and a polishing device (for example, a grinding stone). Thereafter, a laser beam is selectively emitted to cut off the insulating layers 12 , 14 , 15 , and 16 , and the thinned substrate 11 . Subsequently, the laminated body 33 including the substrate 11 and the plurality of transistors 13 is sealed by using the films 34 and 35 (see FIG. 4B ). Note that one or both of grinding and polishing may be performed to the substrate 11 so that the thickness of the substrate 11 is 100 μm, preferably 50 μm or less, and more preferably 5 μm or less.
[0054] Note that when one or both of grinding and polishing is/are performed, a film aimed at protection may be provided over the insulating layer 25 to be fixed, and thereafter, one or both of grinding and polishing is/are performed to the other surface of the substrate 11 . Note that the film which is provided over the insulating layer 25 may be a film having a surface provided with an UV curing adhesive. In addition, after one or both of grinding and polishing is/are performed, the film provided over the insulating layer 25 may be left or removed.
[0055] As described above, by thinning the substrate 11 , the insulating layers 12 , 14 , 15 , and 16 , and the substrate 11 can be easily cut off at short times using a laser beam. In addition, by thinning the substrate, a semiconductor device having flexibility can be provided. By making a semiconductor device have flexibility, design can be improved, and the semiconductor device can be easily mounted on an object with a flexible shape; accordingly, the semiconductor device can be utilized in various fields.
[0056] In addition, although a shape of the cut substrate 11 is a simple square shape in the above process, the present invention is not limited thereto. For example, a hexagonal groove 32 may be formed in the laminated body including the substrate 11 by scanning and emitting a laser beam (see FIG. 5A ), and subsequently, the laser beam is emitted to cut off the laminated body including the substrate 11 (see FIG. 5B ). Accordingly, a hexagonal laminated body including the substrate 11 can be formed. Moreover, a circular groove 32 may be formed in the laminated body including the substrate 11 by emitting a laser beam (see FIG. 5C ), and the laser beam may be emitted to cut off the laminated body including the substrate 11 (see FIG. 5D ). Accordingly, a circular laminated body including the substrate 11 can be formed.
[0057] An interior angle of the top shape of the laminated body including the substrate 11 is set to be 90 degrees or more (for example, a polygonal shape such as hexagon), or eliminating corner of the laminated body including the substrate 11 (for example, a circular shape or an ellipse shape) by devising the shape as described above; accordingly, the semiconductor device can be easily treated in carrying. In addition, generation of a defect, a crack or a burr at the time of mounting on a product can be prevented.
Embodiment 1
[0058] Results of an experiment using the present invention will be explained with reference to FIGS. 6A to 6 D. Each of FIGS. 6A to 6 C shows a cutting surface of a glass substrate.
[0059] As a first experiment, it was attempted to selectively emit a laser beam to a glass substrate, form a groove in the glass substrate, and cut off the glass substrate dynamically. Note that the size of the glass substrate which was used was 126.6 mm×126.6 mm×thickness of 0.7 mm. An Nd:YVO 4 laser having a wavelength of 266 nm was used for a laser. The irradiation condition of the laser beam was as follows: output power of 2.0 W, frequency of 15 kHz, and feeding speed of 20 mm/sec.
[0060] As a result of selectively emitting a laser beam to the glass substrate, a V-shaped groove was formed in the glass substrate (see FIG. 6A ). Then, as a result of emitting a laser beam to the glass substrate again, a deeper groove was formed in a depth direction (see FIG. 6B ). Next, the feeding speed of 20 mm/sec was changed to 5 mm/sec, and a laser beam is emitted to the glass substrate again; accordingly, a deeper groove was formed in the depth direction (see FIG. 6C ). Subsequently, when it was attempted to dynamically cut off the glass substrate where the above groove was formed, the glass substrate could be easily cut off. In this case, the position of the groove to which the laser beam was emitted became the cutting surface.
[0061] As a second experiment, it was attempted to cut off the glass substrate only by selectively emitting a laser beam to the glass substrate. The laser beam was emitted 6 times. Note that the size of the glass substrate which was used was 126.6 mm×126.6 mm×thickness of 0.7 mm. An Nd:YVO 4 laser having a wavelength of 266 nm was used for a laser. The irradiation condition of the laser was as follows: output power of 2.0 W, frequency of 15 kHz, and feeding speed of 5 mm/sec. As a result of the experiment, the glass substrate could be easily cut off without generating a crack and the like.
[0062] As a third experiment, the glass substrate was polished to be 100 μm thick or less by using a polishing device. Then, it was attempted to cut off the glass substrate only by selectively emitting a laser beam to the glass substrate which was polished. Note that the size of the glass substrate which was used was 126.6 mm×126.6 mm×thickness of 0.7 mm. An Nd:YVO 4 laser having a wavelength of 266 nm was used for a laser. The irradiation condition of the laser was as follows: output power of 2.0 W, frequency of 15 kHz, and feeding speed of 30 mm/sec. As a result of the experiment, the glass substrate could be easily cut off without generating a crack and the like.
[0063] According to these results, it is found that it is necessary to control a thickness of a glass substrate and to appropriately adjust irradiation condition of a laser such as output power, feeding speed, and the number of irradiation in a case of emitting a laser beam to a glass substrate to form a groove in the glass substrate, and also, in a case of emitting a laser beam to a glass substrate to cut off the glass substrate.
[0064] In addition, when a laser beam is emitted to a glass substrate to form a groove in the glass substrate, a cutting surface of the groove is rounded (see FIGS. 6B and 6C ). In a case where the cutting surface is rounded as described above, a defect of a corner of the cutting surface or a crack can be prevented from being generated as compared with a case where there is a corner at a cutting surface. According to such an advantage, a glass substrate can be easily handled mainly when the glass substrate is carried using a robot or the like. Moreover, also in being mounted on a product, generation of a defect or a crack can be suppressed, and generation of a damage or destruction of a substrate can be suppressed.
Embodiment 2
[0065] A structure of a semiconductor device of the present invention will be explained with reference to FIG. 7 . A semiconductor device 100 of the present invention has an arithmetic processing circuit 101 , a memory circuit 103 , an antenna 104 , a power source circuit 109 , a demodulation circuit 110 , and a modulation circuit 111 . The antenna 104 and the power source circuit 109 are essential component parts of the semiconductor device 100 , and the other parts are appropriately provided in accordance with an application of the semiconductor device 100 .
[0066] The arithmetic processing circuit 101 analyzes an order, controls the memory circuit 103 , and outputs data which is transmitted to an exterior portion to the modulation circuit 111 on the basis of a signal which is inputted from the demodulation circuit 110 .
[0067] The memory circuit 103 has a circuit including a memory element and a control circuit which writes and reads data. At least an identification number of the semiconductor device itself is stored in the memory circuit 103 . The identification number is used to distinguish from other semiconductor devices. In addition, the memory circuit 103 has one or more kinds selected from an organic memory, a DRAM (Dynamic Random Access Memory), a SRAM (Static Random Access Memory), an FeRAM (Ferroelectric Random Access Memory), a mask ROM (Read Only Memory), a PROM (Programmable Read Only Memory), an EPROM (Electrically Programmable Read Only Memory), an EEPROM (Electrically Erasable Programmable Read Only Memory), and a flash memory. The organic memory has a structure in which a layer containing an organic compound is interposed between a pair of electrodes, and the structure is simple; therefore, the organic memory has at least two advantages. One advantage is that a manufacturing process can be simplified and cost can be reduced. The other advantage is that an area of a laminated body can be easily reduced and an organic memory with high capacity can be easily realized. Moreover, since an organic memory is a nonvolatile memory, a battery may be incorporated or may not necessarily be incorporated. Therefore, it is preferable to use an organic memory as the memory circuit 103 .
[0068] The antenna 104 converts a carrier wave which is supplied from a reader/writer 112 into an AC electrical signal. Also, load modulation is added by the modulation circuit 111 . The power source circuit 109 generates a power source voltage by using the AC electrical signal which is converted by the antenna 104 to provide a power source voltage for each circuit.
[0069] The demodulation circuit 110 demodulates the AC electrical signal which is converted by the antenna 104 and supplies the demodulated signal to the arithmetic processing circuit 101 . The modulation circuit 111 adds load modulation to the antenna 104 on the basis of a signal which is supplied from the arithmetic processing circuit 101 .
[0070] The reader/writer 112 receives the load modulation which is added to the antenna 104 as a carrier wave. Also, the reader/writer 112 transmits the carrier wave to the semiconductor device 100 . Note that the carrier wave is an electromagnetic wave transmitted and received by the reader/writer 112 , and the reader/writer 112 receives a carrier wave which is modulated by the modulation circuit 111 .
[0071] As described above, the semiconductor device of the present invention having a function to transmit and receive an electromagnetic wave wirelessly is referred to as an RFID (Radio Frequency Identification), an RF chip, an RF tag, an IC tag, an IC label, a wireless chip, a wireless tag, an electronic chip, an electronic tag, a wireless processor, or a wireless memory. This embodiment can be freely combined with other embodiment modes.
Embodiment 3
[0072] The semiconductor device 100 to which the present invention is applied can be used for various goods and various systems by utilizing a function to transmit and receive an electromagnetic wave. The goods are, for example, keys (see FIG. 8A ), bills, coins, securities, bearer bonds, certificates (such as a driver's license and a residence certificate; see FIG. 8B ), documents, containers (such as a petri dish; see FIG. 8C ), packing containers (such as wrapping paper and a bottle; see FIGS. 8E and 8F ), a recording medium (such as a disk and a video tape), vehicles (such as a bicycle), accessories (such as a bag and glasses; see FIG. 8D ), foods, clothes, livingwares, electronic devices (such as a liquid crystal display device, an EL display device, a television device, and a portable terminal), and the like. The semiconductor device of the present invention is attached or mounted on surfaces of the above described goods having various shapes to be fixed. Also, a system indicates a goods management system, an authentication function system, a distribution system, or the like, and high functionality, multi functionality, and high added value of the system can be attempted. This embodiment can be freely combined with other embodiment modes and embodiments.
Embodiment 4
[0073] In this embodiment, a method for manufacturing a transistor will be explained with reference to FIGS. 9A to 9 D, FIGS. 10A to 10 C, and FIGS. 11A and 11B .
[0074] First, an insulating layer 552 is formed over a substrate 551 (see FIG. 9A ). Then, an insulating layer 553 is formed over the insulating layer 552 . Next, a semiconductor layer 554 is formed over the insulating layer 553 . Subsequently, a gate insulating layer 555 is formed over the semiconductor layer 554 .
[0075] The insulating layers 552 and 553 , the semiconductor layer 554 , the gate insulating layer 555 , and the like may be formed by using plasma treatment. It is preferable that plasma treatment herein used is performed with electron density of 1×10 11 cm −3 or more and electron temperature of plasma of 1.5 eV or less. More specifically, it is preferable that the plasma treatment is performed with electron density of 1×10 11 cm −3 or more and 1×10 13 cm −3 or less and an electron temperature of plasma of 0.5 eV or more and 1.5 eV or less.
[0076] When the electron density of plasma is high and the electron temperature near a substance to be processed (for example, the insulating layers 552 and 553 , the semiconductor layer 554 , the gate insulating layer 555 , or the like), a damage due to plasma to the substance to be processed can be prevented. Also, since electron density of plasma is 1×10 11 cm −3 or more, which is high, oxide or nitride which is formed by oxidizing or nitriding a substance to be irradiated by using plasma treatment can be formed as a film which is excellent in uniformity of thickness or the like and is also fine, compared with a thin film which is formed by a CVD method, a sputtering method, or the like. Moreover, since electron temperature of plasma is 1.5 eV or less, which is low, the oxidizing or nitriding treatment can be performed at lower temperature compared with conventional plasma treatment or thermal oxidation method. For example, the oxidizing or nitriding treatment can be sufficiently performed even when the plasma treatment is performed at lower temperature by at least 100° C. than a strain point of a glass substrate.
[0077] Subsequently, a conductive layer 501 and a conductive layer 503 are stacked over the gate insulating layer 555 . Each of the conductive layer 501 and the conductive layer 503 is formed by using metal such as tungsten, chromium, tantalum, tantalum nitride, molybdenum, alloy or a compound containing the above metal as its main component. Note that the conductive layer 501 and the conductive layer 503 are formed by using different materials from each other. Specifically, in an etching process which is performed afterward, a material which generates difference in etching rate is used.
[0078] Next, a mask 506 made of a resist is formed over the conductive layer 503 . The mask 506 is formed by using an exposure mask including a light-shielding film and a translucent film. A specific structure of the mask will be explained hereinafter.
[0079] Then, the conductive layer 503 is etched using the mask 506 to form a mask 507 and a conductive layer 504 (see FIG. 9B ). The mask 507 is sputtered by ion which is accelerated in an electric field, divided into two patterns, and placed separately. Next, the conductive layer 501 is etched using the mask 507 and the conductive layer 504 to form a conductive layer 502 (see FIG. 9C ).
[0080] Subsequently, the mask 507 and the conductive layer 504 are selectively etched to form a mask 508 and a conductive layer 505 (see FIG. 9D ). The mask 508 is sputtered by ion which is accelerated in an electric field and the size is reduced. In this process, a bias voltage which is applied to the substrate side is adjusted so that the conductive layer 502 is prevented from being etched.
[0081] Then, an impurity element imparting one conductivity type is added to the semiconductor layer 554 to form first concentration impurity regions 509 , 516 , and 517 (see FIG. 10A ). At this time, an impurity element is added to the semiconductor layer 554 in a self-aligned manner by using the conductive layers 502 and 505 .
[0082] Next, an impurity element imparting one conductivity type is added to the semiconductor layer 554 to form second concentration impurity regions 510 and 511 (see FIG. 10B ). The second concentration is made to be higher than the first concentration. Note that an impurity element imparting one conductivity type is not added to the semiconductor layer 554 which is overlapped with the conductive layer 505 . Therefore, the semiconductor layer 554 which is overlapped with the conductive layer 505 functions as a channel formation region. Through the above process, a thin film transistor 520 is completed.
[0083] Next, insulating layers 512 and 513 are formed so as to cover the thin film transistor 520 (see FIG. 10C ). Then, conductive layers 514 and 515 connected to the second concentration impurity regions 510 and 511 are formed through openings provided in the insulating layers 512 and 513 .
[0084] According to one feature of the above process, the conductive layers 501 and 503 are etched using the mask 506 having a different thickness and a complicated shape. The masks 507 that are placed separately can be formed by using the mask 506 . Then, a distance between two channel formation regions can be shortened. Specifically, the distance between two channel formation regions can be set to be less than 2 μm. Therefore, in a case of forming a multigate thin film transistor having two or more of gate electrodes, the occupation area thereof can be reduced. Therefore, high integration can be realized and a high definition semiconductor device can be provided.
[0085] Next, a method for forming the mask 506 will be explained with reference to FIGS. 11A and 11B . FIG. 11A is a plan view in which part of an exposure mask is enlarged. Also, FIG. 11B is a cross-sectional view of part of the exposure mask corresponding to FIG. 11A and a cross-sectional view of the laminated body including the substrate 551 .
[0086] The exposure mask has a light-transmitting substrate 560 , light-shielding films 561 and 562 , and a translucent film 563 . The light-shielding films 561 and 562 are made of a metal film such as chromium, tantalum, or CrNx (x is a positive integer). It is necessary that a material for the translucent film 563 is appropriately selected with respect to an exposure wavelength, and for example, TaSixOy (x and y are positive integers), CrOxNy (x and y are positive integers), CrFxOy (x and y are positive integers), MoSixNy (x and y are positive integers), and MoSixOy (x and y are positive integers) may be used. The translucent film 563 functions as an assist pattern.
[0087] When a resist mask is exposed by using the exposure mask having the above structure, the resist mask is classified broadly into a region which is not exposed 521 and a region which is exposed 522 . When a development process is performed in this state, the resist of the region which is exposed 522 is removed, and part of the resist of a portion corresponding to the translucent film 563 in the exposure mask in the region which is not exposed 521 is removed. A mask having a shape as shown in FIG. 9A is formed.
[0088] This application is based on Japanese Patent Application serial No. 2005-156583 filed in Japan Patent Office on May 30 in 2005, the entire contents of which are hereby incorporated by reference. | It is an object to improve a yield of a step of cutting off a substrate. A substrate is cut off by using an ablation process. An ablation process uses a phenomenon in which a molecular bond in a portion irradiated with a laser beam, that is, a portion which absorbs the laser beam is cut off, photodegraded, and evaporated. In other words, a substrate is irradiated with a laser beam, a molecular bond in a portion of the substrate is cut off, photodegraded, and evaporated; accordingly, a groove is formed in the substrate. A method for cutting the substrate has steps of selectively emitting a laser beam and forming a groove in the substrate, and selectively emitting a laser beam to the groove and cutting off the substrate. Methods for manufacturing a groove in a substrate and cutting off a substrate are used for manufacturing a semiconductor device. | 1 |
BACKGROUND OF THE INVENTION
[0001] I. Field of the Invention
[0002] The present invention relates generally to adjustable lighting systems. More particularly, the present invention relates to deflectable and adjustable light mounting systems that assume multiple, yieldable, detented orientations, and thus may safely and reliably be moved from hidden, out-of-the-way positions to exposed highly visible positions.
[0003] II. Description of the Prior Art
[0004] It has long been recognized by those skilled in the art that light mounting assemblies may be movably mounted. Some systems use swivels, some use diverse other systems including flexible cabling or mounts. Known systems move between extended, highly visible positions, and retracted, out-of-the-way positions where they may be shrouded against impact damage and the like.
[0005] A variety of truck and trailer lighting systems exist in the art. For example, U.S. Pat. No. 4,473,868 issued to Moore Sep. 25, 1984 illustrates a light assembly for trucks. A light carrying portion is pivotally mounted to an attaching portion normally on the vehicle top. The light can be moved between exposed and retracted positions. The attaching portion includes a pair of bracket members adapted to be secured to the frame. The light carrying portion has two arms, each having a dog which cooperates with a notch in a respective cam for locking the dog in the notch. A spring urges the dogs and notches into locking engagement. Manual input overcomes the bias of the spring to permit the lights to pivot into the retracted position.
[0006] U.S. Pat. No. 4,703,398 issued Oct. 27, 1987 discloses an auxiliary brake light for vehicles. A socket is mounted securely on a frame and a light housing is pivotally mounted on the socket. The light housing is displaceably and pivotally connected with the socket with bolts engaging guide channels. At least one spring projects from the socket, which is adapted to be connected with the light housing in a detent-like manner.
[0007] U.S. Pat. No. 6,260,990 issued to Saunders Jul. 17, 2001 illustrates a retractable truck light assembly ideal for trailer towing. A retractable light housing is affixed to the truck bedside wall by a pivotal mount enabling the light housing to swivel outwardly to an extended, highly visible position, or inwardly towards the truck body to assume a retracted position.
[0008] U.S. Pat. No. 6,918,689 issued to Schmidt Jul. 19, 2005 shows a pivoting auxiliary light assembly for tractors. An upper support is pivotal with respect to a lower support that is attached to a frame. Detent recesses are formed in an upper end surface of the lower support. The upper support has a lamp housing attached to an end of a support rod, and a detent member. The detent member is selectively received by the recesses to releasably hold the upper support in selected positions relative to the lower support. A bushing member is received by the support members to maintain axial alignment thereof. A spring is received by the support members, and is biased to urge the support members towards each other.
SUMMARY OF THE INVENTION
[0009] A retractable light mounting assembly for trucks and/or trailers provides increased safety and reliability. The light mounting assembly can be quickly user-switched between retracted, out-of-the-way positions and highly visible exposed positions where increased lighting is achieved. Ideally the unit is deployed on trailers, where heightened visibility results when towing.
[0010] A light fixture of a selected configuration is coupled by a rotatable arm to a first hollow tube comprising a rigid stand. A second hollow tube comprises a rigid, tubular spring housing. The stand and spring housing can have different lengths and configurations. The stand is adjustable mechanically, coupled to the spring housing by an elongated bolt that is core drilled to allow the light wiring to pass through the entire assembly. A pair of friction washers, one on the stand and the other on the housing, mutually abut, and create friction resisting torsional displacements. In a preferred embodiment protrusions on one washer register with dimples on one another to cause a detent effect. The housing and the stands may in each embodiment be torsionally displaced against friction caused by the spring biased washers that interfit to form radially spaced-part semi-fixed “detented” positions.
[0011] Thus, it is an object of our present invention to provide a user-deployable and retractable light mounting assembly that can be quickly switched between hidden positions protected from impact, and highly visible exposed positions.
[0012] A related object of our present invention is to provide a user-deployable and retractable light mounting assembly of the character described that is ideal for trailers or trucks.
[0013] It is also an object of our invention to provide an auxiliary lighting system for vehicles.
[0014] Another object of the invention is to provide a retractable light mounting assembly of the character described that can be user mounted in a wide variety of locations.
[0015] Yet another object of our invention is to provide an adjustable light mounting assembly that easily and quickly retracts when hit or deflected by impact with an obstacle.
[0016] A related object is to provide a detented light mounting system that responds to sudden, forcible impacts with yieldable deflections to avoid damage.
[0017] A still further object of our invention is to provide a mounting system for lights built in a wide variety of shapes, that facilitates their orientation either horizontally or vertically. It is a feature of our invention that unique backing plate designs may accommodate different light shapes and configurations. although not necessary for every application such as when used with lights that do not require use of a backing plate.
[0018] A still further object of our present invention is to provide a mounting system for lights that facilitates the advantages discussed.
[0019] These and other objects and advantages of the present invention, along with features of novelty appurtenant thereto, will appear or become apparent in the course of the following descriptive sections.
BRIEF DESCRIPTION OF THE DRAWINGS
[0020] In the following drawings, which form a part of the specification and which are to be construed in conjunction therewith, and in which like reference numerals have been employed throughout wherever possible to indicate like parts in the various views:
[0021] FIG. 1 is a frontal isometric view of a preferred light mounting assembly constructed in accordance with the invention;
[0022] FIG. 2 is a rear isometric view of the light mounting assembly of FIG. 1 ;
[0023] FIG. 3 is a front plan view of the light mounting assembly of FIGS. 1 and 2 ;
[0024] FIG. 4 is a top plan view of the light mounting assembly taken from a position generally above FIG. 1 and looking down;
[0025] FIG. 5 is an exploded isometric assembly view of a preferred light mounting assembly constructed in accordance with the invention;
[0026] FIG. 6 is a longitudinal sectional view of the preferred light mounting assembly taken generally along line 6 - 6 in FIG. 4 ;
[0027] FIG. 7 is a frontal isometric view of an alternative embodiment of our light mounting assembly;
[0028] FIG. 8 is an exploded isometric assembly view of the alternative embodiment of FIG. 7 ;
[0029] FIG. 9 is a top plan view of alternative the light mounting assembly taken from a position generally above FIG. 6 and looking down;
[0030] FIG. 10 is a front plan view of the alternative light mounting assembly of FIGS. 7-9 ;
[0031] FIG. 11 is a left front isometric view of the alternative embodiment of FIGS. 7-10 ;
[0032] FIG. 12 is a rear isometric view of the alternative embodiment of FIGS. 7-11 ;
[0033] FIG. 13 is a longitudinal sectional view of the alternative light mounting assembly taken generally along line 13 - 13 in FIG. 9 ;
[0034] FIG. 14 is a bottom plan view of the alternative light mounting assembly;
[0035] FIG. 15 is a exploded isometric view of a second alternative embodiment;
[0036] FIG. 16 is a exploded isometric view of a third alternative embodiment;
[0037] FIG. 17 is a top plan view of a preferred first compression washer with circular dimples;
[0038] FIG. 18 is a sectional view of the preferred first compression washer, taken generally along line 18 - 18 of FIG. 17 ;
[0039] FIG. 19 is a top plan view of a preferred second compression washer with rectangular dimples that mates with the first compression washer;
[0040] FIG. 20 is a sectional view of the preferred second compression washer taken generally along line 20 - 20 of FIG. 19 ;
[0041] FIG. 21 is a top plan view of an alternative, third second compression washer with slotted dimples that can mate with the first compression washer; and,
[0042] FIG. 22 is a sectional view of the alternative third compression washer taken generally along line 22 - 22 of FIG. 21 .
DETAILED DESCRIPTION
[0043] Turning now to FIGS. 1-6 of the appended drawings, a light mounting system constructed in accordance with the best mode of our invention has been generally designated by the reference numeral 30 . In this embodiment, and those to be discussed hereinafter, an illuminated light is coupled to a first upright, hollow tube that is swiveled to a second hollow tube by a pair of cooperating friction washers described later. The friction washers abut one another in assembly, and their construction establishes a detented, pivotal connection, As a result, the light fixture can swivel or pivot to various radial positions against yieldable pressure established by the detents. The light mounting system can be employed in original equipment installations in new vehicles, or it can be retrofitted to diverse applications, such as truck bodies and trailers. On either case the maneuverability of the system allows adjustments to the lighting fixture for maximum visibility. Concurrently, due to the yieldable characteristics of the detented light mounting, a sudden impact against the light, such as might be experienced when backing up a truck trailer, for example, will only shift the position or orientation of the light, while not breaking or damaging it.
[0044] In the preferred embodiment of our light mounting system 30 , the luminaire 32 is coupled by an arm 34 to a rigid elongated, hollow tubular stand 38 that can house critical components. The second hollow tube in this embodiment comprises a rigid, generally tubular spring housing 40 (i.e., FIGS. 1 , 2 ) that is generally cubicle. The stand 38 is adjustably mechanically, coupled to the spring housing 40 by a pair of friction washers 45 , 47 that enable semi-rigid coupling, but which yieldably allow limited pivotal movement between detented positions. Luminaire 32 may thus be swiveled in the radial directions indicated by arrow 46 ( FIG. 1 ) which is established by the washers 45 , 47 .
[0045] Luminaire 32 comprises a rigid, protective housing 50 which, in FIGS. 1-6 , is generally cylindrical. Instead of being round or cylindrical, the light could be rectangular, square, triangular, oval or other desired geometries. The connection arm 34 is formed by an elongated, threaded shaft 52 fixed within housing 50 that extends into stand 38 and is mechanically secured thereto at a given angular orientation by an external nut 54 and an internal nut 56 disposed within stand 38 that secures the shaft 52 ( FIG. 6 ). When nut 54 is loosened, the luminaire 32 maybe rotated or radially adjusted in position about the plane indicated by arrow 56 ( FIG. 1 ).
[0046] As best seen in FIGS. 1 and 2 , the luminaire 32 comprises at least one generally translucent plastic or glass lens 60 at the light front. Preferably there is a similar lens 62 at the light rear ( FIG. 2 ) with a series of LED's or an incandescent bulb 64 disposed between the lenses 60 and 62 . Bulb wiring is routed through arm 34 , stand 38 , stand 69 and fastener 82 through bore 87 and connected conventionally to a source of power, which may be switched or unswitched.
[0047] The stand 38 (i.e., FIGS. 2 , 5 ) is elongated and rigid, and is generally in the form of a parallelepiped, with a generally rectangular profile. The bottom may be left open to enable assembly of bolt 82 ( FIG. 6 ). One side has a suitable orifice 67 that clears light arm 34 (i.e., FIG. 5 ) previously discussed. Compression washer 47 sits atop stand 38 and is centered with respect thereto. Washer 47 is welded to stand 38 and moves with it.
[0048] The preferred spring housing 40 is preferably shorter in length than stand 38 . The generally cubicle body 69 has a pair of integral sides that mater with and are integral with a base flange 70 that has mounting orifices 73 , 74 (i.e., FIG. 2 ). When the light is mounted to an application, the underside 71 ( FIG. 2 ) of the flange will abut the surface upon which the light is mounted. The second compression washer 45 is welded at the base of body 69 , and is centered with respect thereto. In assembly it can be seen that washers 45 , 47 are centered on their respective parts such that they are operationally disposed in a concentric relationship.
[0049] The spring housing 40 and the stand 38 are axially, forcibly spring-biased together. As best viewed in FIGS. 5 and 6 , an elongated core-drilled fastener 82 is concentrically inserted within spring housing 40 , and passes through aligned washers 45 , 47 , entering stand 38 . A compression spring 84 ( FIG. 5 ) is coaxially captivated on the shank 85 of the fastener 82 . The bottom of the fastener 82 threadably receives a hex nut 86 . Tightening of fastener 82 causes spring 84 ( FIG. 5 ) to be forcibly compressed by the head 83 of fastener 82 . It will be observed from FIGS. 5 and 6 that the preferred fastener 82 has an elongated through bore 87 extending from its head 83 all the way through its shank 85 . Bore 87 is coincident with the longitudinal axis of the fastener 82 .
[0050] Torsional friction between compressed washers 45 , 47 (and between housing 40 and stand 38 ) is increased as the fastener 82 is tightened. Rotational friction between washers must be overcome when the luminaire 32 is deflected or impacted. Pivoting results when stand 38 is torsionally displaced as indicated by arrow 46 in FIG. 1 . As explained later, means are provided for the coaxially aligned and abutting washers 45 , 47 to assume semi-permanent detented positions.
[0051] Referring now to FIGS. 8-14 , a first alternative embodiment 130 is shown. It is substantially similar to embodiment 30 discussed above. Here luminaire 132 is coupled by an arm 134 to the first hollow tube comprising a rigid elongated, hollow stand 138 constructed substantially as described before. The second hollow tube in embodiment 130 comprises a rigid, generally tubular spring housing 140 (i.e., FIG. 8 ) that is generally cubicle as before, but which lacks the flange 70 discussed earlier. As before, the stand 138 is adjustably mechanically, coupled to the spring housing 140 by a pair of friction washers 145 , 147 which yieldably allow pivotal movements. Luminaire 132 connects to stand 138 with shaft 152 extending into stand 138 and being mechanically secured thereto by nut 154 .
[0052] The spring housing 140 and the stand 138 are forcibly spring-biased together by the through-bored fastener 182 . As best viewed in FIG. 8 , the fastener 182 passes through washers 145 , 147 , entering stand 138 and captivating compression spring 84 ( FIG. 8 ). Hex nut 186 secures fastener 182 , compressing spring 154 to develop washer friction.
[0053] FIG. 15 shows a preferred second alternative embodiment 230 which is substantially similar to he previous embodiments discussed above. Luminaire 232 is coupled by arm 234 and nut 235 ( FIG. 15 ) to a rigid stand 238 constructed substantially as described before. Spring housing 240 is generally cubicle as before, but lacks an analogous flange 70 discussed earlier. Stand 238 is mechanically coupled to spring housing 240 by a pair of different friction washers 245 , 247 which again facilitate yieldable pivotal movements. Core drilled fastener 282 captivates pressure spring 284 and biases stand 238 and housing 240 together.
[0054] FIG. 16 shows a preferred third alternative embodiment 330 which is substantially similar to the previous embodiments. Luminaire 332 is secured by arm 333 and nut 334 to a rigid stand 338 . Spring housing 340 is biased to stand 338 by core-drilled fastener 382 that captivates compression spring 384 . Stand 338 is coupled to spring housing 340 by a pair of different friction washers 345 , 347 that facilitate yieldable pivotal movements.
[0055] With reference now directed to FIGS. 17 and 18 , the washers 45 and 47 mentioned in the discussion of the first embodiment above are generally circular and flat. All washers can be made from either plastic or metal. Each washer has a central orifice that clears the fasteners discussed earlier. Each washer has a plurality of raised projections on one side, and a plurality of aligned depressions on its opposite side. Interaction and registration between the projections of one washer with the depressions on an adjacent washer create the desired detent effect. The washer projections and depressions can vary in size and placement and shape.
[0056] In the first washer embodiment of FIGS. 17 and 18 . A plurality of radially spaced apart, generally convex and upwardly extending projections comprising protrusions 402 project upwardly from the upper face 401 of the washer 45 or 47 . The lower annular washer face 405 ( FIG. 18 ) has depressions formed by indented dimples 407 that are concave. Protrusions 402 align and register with dimples 407 on an opposite washer yieldably establishing radially spaced apart detented positions. In other words, when stand 38 ( FIG. 5 ) receives spring housing 40 , the upwardly extending convex protrusions on washer 47 can mate with and register with the lower dimples on washer 45 . Since the dimples are symmetrical with the protrusions, torsional displacements between the stand 38 and the housing 40 allow four separate, radially spaced apart detent positions where the dimples and protrusions mate, i.e., the convex upper protrusions are forced into the concave lower dimples by spring pressure. Of course, the washers can be reversed, with protrusions, for example, projecting downwardly, but the point is to establish detented positions when the protrusions and dimples register. When torsional displacements occur, friction is insured during twisting by the forces of spring 84 , that compressively urges mutually abutting faces of the dimpled washers together.
[0057] FIGS. 19 and 20 show washers 245 or 247 that can also establish pivoting, and are desired in heavy duty applications. Instead of dimples and protrusions like washers 45 , 47 discussed above, washers 245 , or 247 have machined grooves or valleys 411 on one side ( FIG. 20 ) and corresponding ridged (peaks) 413 on the other side. Here, abutting washers end up with valleys 411 receiving peaks 413 allowing the same nesting action as before. In both cases spring tension mates the washers together. However, more torsional force is necessary to overcome the spring-influenced detent positions.
[0058] FIGS. 21 and 22 show washers 345 and/or 347 . The upper washer surface 421 has radially spaced apart ridges 420 that are oriented ninety degrees from peaks 413 discussed with FIG. 19 . In other words, the upwardly projecting ridges 420 are separated radially by ninety degrees, and run from the center of the washer towards the circumference. The underside 430 ( FIG. 22 ) has corresponding slots 432 that are penetrated by ridges 420 when the washers are aligned in the same manner as discussed earlier.
[0059] The ability of the light mounts described herein to pivot when hit from either direction provides the operator the opportunity to simply flip the undamaged light back into position before proceeding onto the highway. The mount also maintains high visibility by allowing the operator to mount the light in a more visible location without the fear of being damaged and/or broken off and thus a loss in investment. It can also be visible to oncoming traffic either by the unique design option of mounting lights in a forward-facing position on a backing plate or by using lights designed with that inherent function. (i.e., dual faced pedestal lights)
[0060] Use of the mounts addresses a major safety issue and drastically reduces the risk of traffic accidents due to damaged, missing or obscured lights on trailers leading to unexpected medical costs, elevated insurance premiums, lawsuits as well as loss of life in some situation.
[0061] From the foregoing, it will be seen that this invention is one well adapted to obtain all the ends and objects herein set forth, together with other advantages, which are inherent to the structure.
[0062] It will be understood that certain features and subcombinations are of utility and may be employed without reference to other features and subcombinations.
[0063] As many possible embodiments may be made of the invention without departing from the scope thereof, it is to be understood that all matter herein set forth or shown in the accompanying drawings is to be interpreted as illustrative and not in a limiting sense. | Highly visible detented light mounts for trucks or trailers have light fixtures of selected configurations coupled by rotatable arms to rigid, tubular stands. Each stand is axially biased to a rigid, tubular spring housing by an internal core-drilled fastener that coaxially secures an internal spring. The stand and spring housing can have different lengths and configurations. A pair of friction washers, one on the stand and the other on the housing, mutually abut. Protrusions on one washer register with corresponding dimples or depressions on another washer to cause a detent effect. The housing and the stands may in each embodiment be torsionally displaced against friction caused by the spring biased washers that interfit to form radially spaced-part semi-fixed “detented” positions. Various washer configurations are proposed. | 1 |
This is a continuation-in-part of application Ser. No. 08/307,545 filed on Sep. 16, 1994 now U.S. Pat. No. 5,424,348, which is a continuation of 08/096,530, Jul. 22, 1993 abandoned.
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to solvent utilizing polymerization processes, and more particularly relates to solvent based delivery systems for phosphites.
2. DESCRIPTION OF RELATED ART
Solvent utilizing polymerization processes are generally known. Such processes are useful for manufacturing polymers such as homopolymers, block copolymers and graft copolymers, and include processes commonly referred to as bulk, mass, suspension and emulsion processes. Some of the processes attempt to incorporate antioxidants such as phosphites into the polymer material by introducing a solvent containing the antioxidant into the reaction process. These solvents generally need to be removed at some point in the process, and consequently there is at times a desire to minimize the amount of solvent in the process. Many phosphites, however, do not exhibit high levels of solubility in various organic solvents, for example, aliphatic or aromatic liquid (25° C.) hydrocarbons, for further example, cyclohexane.
Accordingly, there is a desire to provide a phosphite which exhibits high levels of solubility in organic solvents, and to provide a solvent delivery system for the phosphite which minimizes the amount of solvent required.
SUMMARY OF THE INVENTION
The present invention involves a polymerization process involving the delivery of a phosphite into the process via a solvent carrier, and further involves a solvent carrier solution containing a phosphite wherein the phosphite is of the formula: ##STR2## wherein Y 1 is an alkyl and Y 2 is selected from tert-butyl and sec-butyl. The solvent is an organic solvent.
DETAILED DESCRIPTION OF THE INVENTION
A process is provided for making polymeric materials. One embodiment of the process involves introducing a carrier solution into a reaction mass. The carrier solution contains an organic solvent and a phosphite that exhibits a high degree of solubility in the organic solvent.
The process is useful for making polymeric materials containing (desired from) diene compounds. The diene rubber polymers which can be used in the present invention are characterized by the following types (a) and (b): (a) ABA-type or ABA'-type copolymer (or their combination); (b) AB type di block copolymer.
In the aforementioned types, A and A' are blocks derived from comonomers consisting of unsaturated alkenyl aromatic compounds (e.g., styrene, α-methylstyrene, vinyltoluene, vinylxylene, vinylnaphthalene, etc.) or their mixtures, B is a block derived from comonomers consisting of diene compounds (e.g., butadiene, chlorobutadiene, isoprene, 1,3-pentadiene, 2,3-dimethylbutadiene, etc.) or their mixtures.
The ABA-type or ABA'-type copolymer may be a so-called "tapered" block copolymer, in which three blocks are directly connected to each other or via a "random copolymer" consisting of an alkenyl aromatic compound and a diene compound constituting each block, or a radial teleblock copolymer consisting of an alkenyl aromatic compound and a diene compound. The AB type di block copolymer is a "tapered" block copolymer in which two blocks are directly connected to one each other or via a "random copolymer" consisting of an alkenyl aromatic compound and a diene compound constituting each block.
Examples of especially desirable rubber polymers corresponding to the aforementioned type (a) include a styrene-ethylene-butadiene-styrene block copolymer, styrene-butadiene-styrene block copolymer, styrene-isoprene-styrene block copolymer, etc. Examples of especially rubber polymers corresponding to the aforementioned type (b) include a styrene-ethylene-propylene block copolymer, styrene-butadiene block copolymer, etc.
The aforementioned rubber polymers may be totally hydrogenated, partially hydrogenated, or acid-modified using maleic anhydride, etc. In particular, hydrogenated polymers are especially desirable in consideration of the thermal ageing resistance.
It is desirable that the quantity of rubber polymer content be 1-80 parts by weight (with respect to 100 parts by weight) of the resin composition of the present invention. Then, it is desirable that the relative quantities of components (a) and (b) be 3-97 wt % and 97-3-wt %, respectively.
If necessary, furthermore, other rubbers (e.g., ethylene-propylene rubber, etc.) may be used in combination with the aforementioned rubber polymers of components (a) and (b).
The process is also useful for making graft copolymer having a diene rubber component. Rubber modified monovinylidene aromatic resins comprising (a) a rubber modified monovinylidene aromatic graft copolymer and (b) an ungrafted rigid copolymer, are generally prepared by graft polymerization of a mixture of a monovinylidene aromatic monomer and one or more comonomers in the presence of one or more rubbery polymeric substrates. Depending on the amount of rubber present, a separate matrix or continuous rigid phase of ungrafted rigid (co)polymer may be simultaneously obtained along with the rubber modified monovinylidene aromatic graft polymer. The resins may also be produced by blending a rigid monovinylidene aromatic copolymer with one or more rubber modified monovinylidene aromatic graft copolymers. Typically, the rubber modified resins comprise the rubber modified graft copolymer at a level of from 5 to 100 percent by weight based on the total weight of the resin, more preferably from 10 to 95 percent by weight thereof, more preferably 20 to 90 percent by weight thereof, and most preferably from 15 to 85 percent by weight thereof; and the rubber modified resin comprises the ungrafted rigid polymer at a level of from 0 to 95 percent by weight based on the total weight of the resin, more preferably from 5 to 90 percent by weight thereof, more preferably from 10 to 80 percent by weight thereof and most preferably from 15 to 85 percent by weight thereof.
Monovinylidene aromatic monomers which may be employed include styrene, alpha-methyl styrene, halostyrenes i.e. dibromostyrene, mono or di alkyl, alkoxy or hydroxy substitute groups on the nuclear ring of the monovinylidene aromatic monomer i.e. vinyl toluene, vinylxylene, butylstyrene, parahydroxystyrene or methoxystyrene or mixtures thereof. The monovinylidenearomatic monomers utilized are generically described by the following formula: ##STR3## wherein X is selected from the group consisting of hydrogen, alkyl groups of 1 to 5 carbon atoms, cycloalkyl, aryl, alkaryl, aralkyl, alkoxy, aryloxy, and halogens. R is selected from the group consisting of hydrogen, alkyl groups of 1 to 5 carbon atoms and halogens such as bromine and chlorine. Examples of substituted vinylaromatic compounds include styrene, 4-methylstyrene, 3,5-diethylstyrene, 4-n-propylstyrene, α-methylstyrene, α-methyl vinyltoluene, α-chlorostyrene, α-bromostyrene, dichlorostyrene, dibromostyrene, tetrachlorostyrene, mixtures thereof and the like. The preferred monovinylidene aromatic monomers used are styrene and/or α-methylstyrene.
Comonomers which may be used with the monovinylidene aromatic monomer includes acrylonitrile, methacrylonitrile, C 1 to C 8 alkyl or aryl substituted acrylate, C 1 to C 8 alkyl, aryl or haloaryl substituted methacrylate, acrylic acid, methacrylic acid, iraconic acid, acrylamide, N-substituted acrylamide or methacrylamide, maleic anhydride, maleimide, N-alkyl, aryl or haloaryl substituted maleimide, glycidyl (meth)acrylates, hydroxy alkyl (meth)acrylates or mixtures thereof. The acrylonitrile, substituted acrylonitrile, or acrylic acid esters are described generically by the following formula: ##STR4## wherein R 1 may be selected from the same group set out for R as previously defined and Y is selected from the group consisting of cyano and carbalkoxy groups wherein the alkoxy group of the carbalkoxy contains from one or about twelve carbon atoms. Examples of such monomers include acrylonitrile, ethacrylonitrile, methacrylonitrile, α-chloroacrylonitrile, α-bromoacrylonitrile, methyl acrylate, methyl methacrylate, ethyl acrylate, butyl acrylate, propylacrylate, isopropyl acrylate and mixtures thereof. The preferred monomer is acrylonitrile and the preferred acrylic acid esters are ethyl acrylate and methyl methacrylate. It is also preferred that the acrylic acid esters, when included, are employed in combination with styrene or acrylonitrile.
The rubber modified graft copolymer comprises (i) the rubber substrate, and (ii) a rigid polymeric superstrate portion grafted to the rubber substrate. The rubber substrate is preferably present in the graft copolymer at a level of from 5 to 85 percent by weight based on the total weight of the graft copolymer, more preferably from 10 to 80 percent by weight thereof, and most preferably 20 to 70 percent by weight thereof; and the rigid superstrate is preferably present at a level of from 15 to 95 percent by weight based on the total weight of the graft copolymer, more preferably from 20 to 90 percent by weight thereof, and most preferably from 30 to 80 percent by weight thereof.
For high rubber graft emulsion resins, the rubber level will range from 50 to 85% by weight based on the total weight of the rubber modified resin. For mass polymerization, the rubber level ranges from 4 to 40% by weight based on the total weight of the rubber modified resin. For blends of an ungrafted rigid copolymer (such as styreneacrylonitrile copolymer) with an emulsion high rubber graft (HRG) copolymer (such as acrylonitrile-butadiene-styrene graft copolymers), the rubber loading will typically range from 10 to 40% rubber based on the total weight of the rubber modified resin.
Examples of rubbery polymers for the substrate include: conjugated dienes, copolymers of a diene with styrene, acrylonitrile, methacrylonitrile or C 1 to C 8 alkyl acrylate which contain at least 50% (preferably at least 65% by weight) conjugated dienes, polyisoprene or mixtures thereof; olefin rubbers i.e. ethylene propylene copolymer (EPR) or ethylene propylene non-conjugated diene (EPDM); silicone rubbers; or C 1 or C 8 alkyl acrylate homopolymers or copolymers with butadiene and/or styrene. The acrylic polymer may also contain up to 5% of one or more polyfunctional crosslinking agents such as alkylenediol di(meth)acrylates, alkylenetriol tri(meth)acrylates, polyester di(meth)acrylates, divinylbenzene, trivinylbenzene, butadiene, isoprene and optionally graftable monomers such as, triallyl cyanurate, triallyl isocyanurate, allyl (meth)acrylate, diallyl maleate, diallyl fumarate, diallyl adipate, triallyl esters of citric acid or mixtures of these agents.
The diene rubbers may preferably be polybutadiene, polyisoprene and copolymers of butadiene with up to 35% by weight of comonomers such as styrene, acrylonitrile, methylmethacrylate or C 1 -C 6 -alkylacrylate which are produced by aqueous radical emulsion polymerisation. The acrylate rubbers may be cross-linked, particulate emulsion copolymers substantially of C 1 -C 8 -alkylacrylate, in particular C 2 -C 6 -alkylacrylate, optionally in admixture with up to 15% by weight of comonomers such as styrene, methylmethacrylate, butadiene, vinyl methyl ether or acrylonitrile and optionally up to 5% by weight of a polyfunctional crosslinking comonomer, e.g. divinylbenzene, glycol-bis-acrylates, bisacrylamides, phosphoric acid triallylester, citric acid triallylester, allylesters of acrylic acid or methacrylic acid, triallylcyanurate, triallylisocyanurate. Also suitable are mixtures of diene- and alkylacrylate rubbers and rubbers which have a so-called core/sheath structure, e.g. a core of diene rubber and a sheath of acrylate or vice versa.
Specific conjugated diene monomers normally utilized in preparing the rubber substrate of the graft polymer are generically described by the following formula: ##STR5## wherein X 1 is selected from the group consisting of hydrogen, alkyl groups containing from one to five carbon atoms, chlorine or bromine. Examples of dienes that may be used are butadiene, isoprene, 1,3-heptadiene, methyl-1,3-pentadiene, 2,3-dimethylbutadiene, 2-ethyl-1,3-pentadiene 1,3- and 2,4-hexadienes, chloro and bromo substituted butadienes such as dichlorobutadiene, bromobutadiene, dibromobutadiene, mixtures thereof, and the like. A preferred conjugated diene is 1,3 butadiene.
The substrate polymer, as mentioned, is preferably a conjugated diene polymer such as polybutadiene, polyisoprene, or a copolymer, such as butadiene-styrene, butadiene-acrylonitrile, or the like. The rubbery polymeric substrate portion must exhibit a glass transition temperature (Tg) of less than about 0° C.
Mixtures of one or more rubbery polymers previously described for preparing the monovinylidene aromatic graft polymers, or mixtures of one or more rubber modified monovinylidene aromatic graft polymers disclosed herein may also be employed. Furthermore, the rubber may comprise either a block or random copolymer. The rubber particle size used in this invention as measured by simple light transmission methods or capillary hydrodynamic chromatography (CHDF) may be described as having an average particle size by weight of select one of the following: 0.05 to 1.2 microns, preferably 0.2 to 0.8 microns, for emulsion based polymerized rubber latices or 0.5 to 10 microns, preferably 0.6 to 1.5 microns, for mass polymerized rubber substrates which also have included grafted monomer occlusions. The rubber substrate is preferably a particulate, highly crosslinked diene or alkyl acrylate rubber, and preferably has a gel content greater than 70%.
Preferred graft superstrates include copolymers of styrene and acrylonitrile, copolymers of α-methylstyrene and acrylonitrile and methylmethacrylate polymers or copolymers with up to 50% by weight of C 1 -C 6 alkylacrylates, acrylonitrile or styrene. Specific examples of monovinylidene aromatic graft copolymers include but are not limited to the following: acrylonitrile-butadiene-styrene (ABS), acrylonitrile-styrene-butyl acrylate (ASA), methylmethacrylate-acrylonitrile-butadiene-styrene (MABS), acrylonitrile-ethylene-propylene-nonconjugated diene-styrene (AES).
The ungrafted rigid polymers (typically free of rubber) are resinous, thermoplastic polymers of styrene, α-methylstyrene, styrenes substituted in the nucleus such as ρ-methylstyrene, methyl acrylate, methylmethacrylate, acrylonitrile, methacrylonitrile, maleic acid anhydride, N-substituted maleimide, vinyl acetate or mixtures thereof. Styrene/acrylonitrile copolymers, α-methylstyrene/acrylonitrile copolymers and methylmethacrylate/acrylonitrile copolymers are preferred.
The ungrafted rigid copolymers are known and may be prepared by radical polymerisation, in particular by emulsion, suspension, solution or bulk polymerisation. They preferably have number average molecular weights of from 20,000 to 200,000 and limiting viscosity numbers [η] of from 20 to 110 ml/g (determined in dimethylformamide at 25° C.).
The number average molecular weight of the grafted rigid superstrate of the monovinylidene aromatic resin is designed to be in the range of 20,000 to 350,000. The ratio of monovinylidene aromatic monomer to the second and optionally third monomer may range from 90/10 to 50/50 preferably 80/20 to 60/40. The third monomer may optional replace 0 to 50% of one or both of the first and second monomers.
These rubber modified monovinylidene aromatic graft polymers may be polymerized either by mass, emulsion, suspension, solution or combined processes such as bulk-suspension, emulsion-bulk, bulk-solution or other techniques well known in the art. Furthermore, these rubber modified monovinylidene aromatic graft copolymers may be produced either by continuous, semibatch or batch processes.
The organic solvent may be any suitable organic solvent, which preferably has a melt temperature below 25° C., and suitable examples include C 3 to C 20 hydrocarbons, more preferably C 4 to C 10 hydrocarbons, such as benzene, tetrahydrofuran, dioxane, 1,2-dimethoxyethane and n-hexane, and most preferably is cyclohexane. Other suitable solvents include aliphatic or aromatic hydrocarbons, mineral oil, and hydrocarbon monomers such as styrene. The carrier solution is a solution of organic solvent and phosphite. The phosphite is preferably present at a level of from 1 to 50 percent by weight based on the total weight of the carrier solution, more preferably from 10 to 50 percent by weight thereof, and most preferably from 20 to 40 percent by weight thereof. The organic solvent is preferably present in the carrier solution at a level of from 50 to 99 percent by weight based on the total weight of the carrier solution, more preferably from 50 to 90 percent by weight thereof, and most preferably from 60 to 80 percent by weight thereof.
One embodiment of the process involves feeding the carrier solution into a reaction mass. The reaction mass comprises vinyl monomers and diene monomers and/or diene derived polymers. The phosphite serves to enhance the oxidative stability of the polymeric materials during processing and post-processing. Another embodiment of the process involves introducing the carrier solution into the polymeric material, and then removing the solvent therefrom.
Other suitable processes for using the present invention include processes for making vinylic polymers including, for example, polystyrene, polyvinylchloride, anionic polymers, polybutadiene, polyisoprene, and polymethylmethacrylate.
Mass, bulk, mass-suspension, suspension and emulsion processes are well known in the art. The present invention involves improving the phosphite delivery system of those processes by utilizing a carrier solution that contains a phosphite which exhibits high levels of solubility in organic solvents.
Polymeric material as used herein refers to either the final polymer product or the final polymeric product in solution or dispersion.
The phosphite preferably has a melt temperature above 25° C.
TABLE 1______________________________________Ex Phos Solubility %______________________________________1 Phos 1 50.1A Phos A <10B Phos B 15.7C Phos C 12.4______________________________________
Solubility for example 1 and comparative example A is measured as solubility in hexane with each percentage value being equal to grams of phos per milliliter of hexane (20%=2 g/ml, 10%=1 g/ml.
Phos A is Tetrakis(2,4-di-tert-butylphenyl)4,4'-diphenylylenediphosphonite.
Phos 1 is of the formula ##STR6##
The examples of Table 2 illustrate the in polymer solubility of the present phosphites which should facilitate phosphite dispersion in the polymer compositions.
Phos B is bis(2,4-di-t-butylphenyl) pentaerythritol diphosphite.
Phos C is tris(2,4-di-tert-butylphenyl) phosphite.
Phos D is trisnonylphenyphosphite.
CEX D-G were comparative examples and examples 2 and 3 were examples of the present invention.
Phos 2 was of the formula ##STR7##
Values are set out as concentration in parts per million based on the total weight of the linear low density polyethylene. The greatly increasing values with time for examples 2 and 3 compared to CEX D-G illustrates the greatly enhanced solubility of the present phosphites.
TABLE 2______________________________________Time CEXD CEXE CEXF CEXG EX2 EX3(Weeks) Phos B Phos C Phos D Phos A Phos 1 Phos2______________________________________0 0 0 0 0 0 01 -- -- -- -- 275 11713 -- -- 394 -- 1177 43665 35 33 789 97 1595 63757 99 41 1204 291 1992 81519 59 95 773 320 2269 903711 111 40 777 -- 2791 --13 114 37 -- -- 2348 900715 77 33 1003 365 2187 8971______________________________________ | A polymerization process is provided involving a carrier solution containing an organic solvent and a phosphite. The phosphite is highly soluble in the solvent and allows for an incorporation of a minimum of solvent in the carrier sohltion. The phosphite is of the formula: ##STR1## wherein Y 1 is an alkyl and Y 2 is selected from tert-butyl and sec-butyl. The process is useful for making polymers such as styrene-butadiene block copolymers which may then be molded to produce commercial articles or may be blended with other thermoplastics to enhance the impact strengths thereof. | 3 |
BACKGROUND OF THE INVENTION
A pulse motor is often employed to control the operation of various precision mechanisms because the rotation angle of the pulse motor is accurately determined by the number of input pulses, and the angular position can thus be accurately controlled without the need of a feedback control, thereby reducing cost. However, if the pulse motor is used to control the fabric feeding device of a sewing machine, the resolving precision of the rotation angle of the pulse motor must be considered. When such a pulse motor is utilized, feed amount per pulse varies discontinuously as is shown in FIG. 2, and can only be varied stepwise between two adjacent feed amounts when the pulse motor is pulsed. The rotation angle of the pulse motor is proportional to the number of pulses delivered to the pulse motor. But, as the motion of the pulse motor is transmitted to the feed dog through a linkage and an adjuster, the selected feed amounts vary non-linearly with the number of pulses as shown in FIG. 2. The stitch control follows the plots in FIG. 2 in accordance with by stitch information. However, in dependence upon the type of stitch utilized, it becomes necessary to employ feed amounts intermediate adjacent plots shown in FIG. 2. To do so, the number of steps of the pulse motor required for maximum feed may be increased. This results in increasing the number of rotations of the pulse motor for the maximum feed amount, since the resolving precision of the rotation angle of the pulse motor is fixed. As a result, the rotation inertia of motor increases and its response decreases. Further, the non-linear variation of feed rate unnecessarily increases the resolving precision in the range of the minimum feed in FIG. 2, thereby causing waste in the control of the pulse motor.
SUMMARY OF THE INVENTION
It is a primary object of the invention to increase the resolving precision of a pulse motor, instead of increasing the rotation angles of the pulse motor, to thereby obtain desirable feed rates in sewing machine.
In this invention, this object is achieved by the use of a micro-computer which operates the pulse motor in such a fashion as to cause the pulse motor to alternate between adjacent individual feed rates to produce an overall feed rate which is a composite of the individual feed rates and is, overall, intermediate them. Thus, if a required feed rate is intermediate two available feed rates and the pulse motor can only feed at one rate or the other at any one time, the micro-computer programs the pulse motor to execute a repeated sequence in which the pulse motor operates first at one rate and then at the other. By so operating, the pulse motor feeds both at an overall rate which is a composite of the two rates and is intermediate them.
The other features and advantages of the invention will be apparent from the following description of the invention in reference to the preferred embodiment as shown in the attached drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 an outline of a sewing machine provided with the invention disclosed herein;
FIG. 2 shows fabric feed amount for each of the steps of the pulse motor;
FIG. 3 is a block diagram of the control for the pulse motor;
FIG. 4 is a flow chart showing the operation of the invention;
FIG. 5 is an example of a stitch produced by the invention; and
FIG. 6 shows the relation between the adjusted values indicated on the dial, the position coordinates of the pulse motor, and feed amounts.
DETAILED DESCRIPTION OF PREFERRED EMBODIMENTS
In FIG. 1, a numeral 1 indicates a sewing machine housing containing a pulse motor for controlling a fabric feeding device, in which the pulse motor acts on a feed adjuster 5 via links 3 and 4. A numeral 6 indicates a lower shaft rotating in synchronism with rotation of an upper shaft (not shown) of the sewing machine, and a fork rod 8 engages a cam 7 fixedly mounted on the lower shaft 6 for controlling the horizontal movement of a feed dog 12. Therefore, the fork rod 8 is shiftable as the lower shaft 6 rotates. As is well known, the feed adjuster 5 is formed with a guide groove (not shown) in which a block is slidably received. The block is connected to fork rod 8. Thus, depending upon the inclination of the feed adjuster 5, the horizontal feeding amount of the feed dog 12 is varied or nullified through transmission links 9, 10, and 11. The inclination of the feed adjuster 5 is adjusted by the operation of the pulse motor 2. Numeral 13 indicates a feed adjusting dial manually operated to adjust the fabric feeding rate, and 14 indicates a variable resistor varied by the dial for converting a rotated position of the dial 14 into a resistance value. A numeral 15 collectively shows pattern selecting switches. The value of the adjusting dial 13 can be adjusted to provide an optimum feed rate specific to the patterns selected. 16 indicates a light emitting diode for indicating the pattern selecting switch which has been selected.
FIG. 3 is a block diagram of a control micro-computer, in which CPU is a central processing unit, ROM is a read only memory, RAM is a read-write memory temporarily storing information, and I/O is an input output port. A/D is an A/D converter which converts the resistance of the variable resistor 14 into a digital value, and DV is a pulse motor driving circuit which receives a control signal from the micro-computer and drives the fabric feed control pulse motor 2. If any one of the pattern selecting switches 15 is operated, its operation is registered in the RAM and calculations are performed in the central processing unit CPU. Subsequently corresponding light emitting diode 16 is lighted, and a pattern signal is simultaneously given to the driving circuit DV for each stitch from a specific data location within the ROM which corresponds to the operated switch, thereby driving the pulse motor 2. The feed adjusting dial 13 (shown in FIG. 1) can be manually rotated. The resultant resistance value of the variable resistor 14 is routed into the memory RAM and is passed into the CPU for determination of the proper stepping of the pulse motor 2 in response to this resistance value, independently of the pattern signals stored in the memory ROM by operation of the pattern selecting switches 15. FIG. 6 shows the values obtained when the adjusted positions of the feed adjusting dial 13 are A/D converted, and the corresponding position co-ordinates (signals showing the positions for setting the pulse motor) of the pulse motor. The resolving precision of A/D converted values as shown on the adjusting dial 13 is twice the resolving precision of the position co-ordinates of the pulse motor so that the feeding dial 13 indicates the average value between corresponding adjacent position coordinates of the pulse motor. Each of the position co-ordinates of the pulse motor, partially shown in FIG. 6, corresponds a corresponding one of the points plotted in FIG. 2. Thus, each of the feed amounts in FIG. 6 corresponds to one of the feed amounts shown in FIG. 2, and X3 and X4 are particularly shown therein. Thus, feed adjusting dial 13 indicates values identifying midpoints between adjacent points in FIG. 2. In FIG. 6, the feed amount 0 is made to correspond to the position co-ordinate 01111 of the pulse motor because the maximum reverse feeding amount is made to correspond to the position co-ordinate 00000 of the pulse motor.
Operation of the invention will be explained with reference to the flow chart in FIG. 4 in which dotted lines indicate possible omission of steps. Assume that the basic zigzag stitching as shown in FIG. 5 has been selected by one of the pattern selecting switches 15. Subsequently, when the machine operator rotates the feed adjusting dial 13, the sewing machine is so set that the adjusted position or value of the dial overrides the usual feed amount used for such stitches. When the dial 13 is adjusted to an even number, (i.e. when the last bit of the code of the dial value in FIG. 6 is 0) such as 00110, the code corresponds to the position coordinate 10010 of the pulse motor. In this case the basic zigzag stitches are fed by a constant feed amount X 3 . Subsequently, if the feed adjusting dial 13 is rotated to slightly increase the feed amount and set to the value corresponding to 00111, there is no corresponding position coordinate of the pulse motor. However, in this case, the micro-computer of this invention produces a discriminating signal N which alternates between 0 and 1 at each stitch. If N=1 at the first stitch, the micro-computer is so operated to calculate that the adjusted position or value of the dial 13 is (00111)-1 and to produce a position coordinate 10010 which would ordinarily correspond to the dial value 00110, and the pulse motor 2 is driven to produce feed amount X 3 . When N=0 at the subsequent stitch, (00111)+1 is calculated to produce a coordinate (01000), and the pulse motor 2 is driven to provide feed amount X 4 . As a result, zigzag stitches are produced with alternating feed amounts X 3 and X 4 , as is shown in FIG. 5.
In this example, it has been explained that the two feed amounts X 3 and X 4 are alternately provided in a series of stitches as shown in FIG. 5. However, it will be possible to further increase the resolving precision of the position coordinates of the pulse motor by repeatedly using one step (for example, X 3 ) in two stitches and another step (for example, X 4 ) in one stitch. The resolving precision will furthermore be increased if the pulse motor is so controlled as to execute a combination of three steps, for example, X 2 , X 3 , and X 4 .
Thus, when the pulse motor is pulsed at a constant feed rate, it has a resolving precision which can only be adjusted in steps. On the other hand, if the overall feed amount is a composite of adjacent feed rates, resolution is further increased, and the pulse motor is used more effectively to improve the control of the sewing machine. | A sewing machine which utilizes a pulse motor to vary feed rate in steps is equipped with a microcomputer that causes the pulse motor to operate in a repeated sequence in which two adjacent feed rates are alternated. By operating the computer in accordance with a manually-operable control, an overall feed rate can be produced which is intermediate the two adjacent feed rates. | 3 |
CROSS-REFERENCE TO RELATED APPLICATION
Ser. No. 333,199 Rudolph Metoff, "Circular Fluorescent Lamp Unit", filed concurrently herewith and assigned the same as this invention.
BACKGROUND OF THE INVENTION
The invention is in the field of circular lamp units, such as screw-in units having a circular fluorescent lamp and a ballast.
Various types of screw-in fluorescent lamp units have been devised, for taking the place of incandescent lamps in ceiling sockets and in table lamps and floor lamps, and are economical to operate and conserve electrical energy because they consume less than half the electrical energy than incandescent lamps for the same brightness. U.S. Pat. No. 4,258,287 to Frederick Hetzel and U.S. Pat. No. 4,278,911 to Rudolph Metoff each discloses a screw-in central hub containing a ballast, and a replaceable circular lamp assembly including a circular bulb and spokes, positioned on the hub. U.S. Pat. Nos. 4,161,020 to Miller; 2,525,022 to Dupuy; 3,059,137 to Reaves; 2,534,956 to Pistey; and 2,534,955 to Dazley disclose other typical techniques for holding a circular lamp bulb, in which the support arms are hinged or slotted.
SUMMARY OF THE INVENTION
Object of the invention are to provide an improved circular lamp unit which is attractive in appearance, economical to manufacture, and which readily accommodates replaceable circular fluorescent light bulbs of varying dimensions, and particularly the circular diameter, such as due to manufacturing tolerance variations.
The invention comprises, briefly and in a preferred embodiment, a circular fluorescent lamp unit having a central screw-in hub containing lamp ballast means, and a plurality of support arms extending from the hub to support a circular lamp. The support arms are metal or plastic strips which enter through slots of the hub and are bent at substantially right angles within the hub so as to be held in place while having limited radial movement with respect to the hub to enable them to accommodate and support circular lamp bulbs of varying dimensions such as due to manufacturing tolerance variations.
BRIEF DESCRIPTION OF THE DRAWING
FIG. 1 is a perspective view of a preferred embodiment of the invention, showing a lamp unit having support arms holding a circular light bulb and also having and electrical connector member connected to the light bulb.
FIG. 2 is a side sectional view of a portion of FIG. 1, taken on the line 2--2 thereof, showing details of the support arms and also showing the electrical connector member disconnected from the light bulb.
FIG. 3 is an electrical circuit diagram of the lamp unit.
DESCRIPTION OF THE PREFERRED EMBODIMENT
The circular lamp unit comprises a central hub 11 having a two-part plastic housing consisting of a tapered section 12 having a threaded screw base 13 attached to the small end thereof and adapted to fit household or other threaded sockets, and a cylindrical cap section 14 attached to the section 12 by suitable means such as is disclosed in the above-referenced Hetzel patent. The hub 11 is hollow and contains a ballast and starter switch, as will be described.
A pair of light bulb support arms 16, 17 of sheet metal or plastic extend laterally from the hub 11 at mutually opposite sides thereof, and support and hold in position a circular light bulb 18. The light bulb 18 is provided with a conventional four-pin connector base plug 19 having pairs of connector pins 21, 22 connected respectively to ends of cathodes 23, 24 contained in the lamp 18. The outer end regions 26, 27 of the support arms 16, 17 are curved to partly surround and snugly and resiliently hold the lamp 18, one of these end regions 26 preferably being at and partly around the lamp plug 19. The lamp 18 thus is removable from and replaceable in the support arm end regions 26, 27.
In accordance with the invention, one or both of the support arms 16, 17 extends through slots 28 in the wall of the hub cap 14 and are held in the hub cap 14 by a bent inner region 29, at approximately right angles to the lateral portions 16 and 17, of which the outer end 30 is fixedly supported in position by ribs 31, 32 of the cap 14, and the portion of the region 29 near the bend 33 is free to move so that the arm 16 (and/or arm 17) is slidable in and out from the hub 11 a short distance, such as about an eighth or a quarter of an inch, as indicated by the double arrow 34, so that the support arms can readily adjust in length to accommodate and hold circular lamps 18 of slightly varying diameters such as due to manufacturing tolerance variations. The slot 28, right angle bend 33, and anchoring of the bent end 30, function to prevent any substantial movement of the support arms 16, 17 in directions other than radially as indicated by double arrow 34, whereby the support arms hold the bulb 18 firmly in place.
The slots 28 for the support arms are at the rim of the hub cap 14, and the inner region lengths 29 of the support arms extend within the cap 14 and parallel to the hub axis. The hub cap ribs 31, 32 form a receptacle for the end 30 of the inner support arm length 29, preventing any substantial lateral movement of this end 30. The support arms 16, 17 are quickly and economically attached to the hub during manufacture, by sliding the inner length region 29 into the cap 14 so that its end 30 fits into the receptacle provided by ribs 31, 32 and its lateral portion fits into the slot 28; no screws or other fastening devices are required.
The hub 11 contains a conventional lamp ballast means 36, such as an inductor, resistor or capacitor, and may also contain a conventional glow starter switch 37 which alternatively may be contained with the lamp connector plug 19. At the end of the ballast 36 is connected to the button contact 41 of base 13, and the other end thereof is electrically connected, via a wire 42, to the connector terminal 22 of cathode 23. Another wire 43 connects the threaded shell 44 of base 13 to the connector terminal 22 of cathode 24, and wires 46 and 47 respectively connected the starter switch 37 across the connector terminals 21 of cathodes 23 and 24.
The connector wires 42, 43, 46, and 47 may be carried by and/or embeded in, and are a part of, an elongated resilient electrical connector member 51, preferably of rubber or plastic having a lateral groove 52 near an end thereof which fits into a slot 53 of the hub 11 and thus locks the connector member to the hub, with the connection wires 42, 43, 46 and 47 extending from the inner end of the connector member and into the hub for connection to the ballast 36 and starter switch 37. The hub locking slot 53 is located in the tapered hub section 12 adjacent to the flat side of support arm 16 so that the connector 51 is in alignment with and extends substantially along the support arm 16. The connector member 51 includes an angular socket portion 56 and its outer end which contains two pairs of connector receptacles 21' and 22' adapted to connect over the lamp plug pairs of terminals 21, 22 when the socket protion 56 is pushed over these terminals, to provide an operative lamp circuit as shown in FIG. 3, the pairs of connector receptacles 21', 22' being suitably connected to the ends of the wires 42, 43, 46 and 47 within the socket portion 56. The lamp 18 is easily replaceable by pulling the connector socket 56 from the lamp and removing the lamp from its support arms 16, 17. The hub and ballast unit outlasts the lives of several light bulbs. To facilitate the bending of the connector member 51 when connecting it to or disconnecting it from a lamp, its cross-section is preferably rectangular with its narrower dimension in the direction of its flexing, as shown in the drawing, thus making it more flexible and easier to bend when connecting and disconnecting lamps. The width or larger cross-section dimension of the connector 51 may be approximately the same as that of the support arm 16. The connector member 51 is disclosed and claimed in the above-referenced patent application.
The invention provides an arrangement of support arms for a replaceable circular light bulb which is easy to use, economical to manufacture, which accommodates bulbs of varying dimensions, and which is unobtrusive and neat in appearance.
While preferred embodiments and modifications of the invention have been shown and described, various other embodiments and modifications thereof will become apparent to persons skilled in the art and will fall within the scope of the invention as defined in the following claims. | A circular fluorescent lamp unit having a central screw-in hub containing lamp ballast means, and a plurality of support arms extending from the hub and having curved outer ends to support a circular lamp. The support arms are metal or plastic strips which enter through slots of the hub and are bent at substantially right angles within the hub so as to be held in place while having limited radial movement with respect to the hub to enable them to accommodate and support circular lamp bulbs of varying dimensions such as due to manufacturing tolerance variations. | 5 |
TECHNICAL FIELD OF THE INVENTION
The present invention is directed, in general, to processing systems and, more specifically, to a data processor implementing a unified memory architecture design that is accessible by external processor(s).
BACKGROUND OF THE INVENTION
The number of electronic systems which contain microprocessors continues to grow as the prices of microprocessors and memory continue to fall. Microprocessors are implemented not only in traditional desktop personal computers (PCs), but also in a wide variety of consumer electronic devices, including home appliances, and wireless communication devices. Increasingly, many of these systems contain more than one processor. For example, some PC designs contain a main central processing unit (CPU) and a second processor (or “coprocessor” or “peripheral processor”) that performs a specific secondary function, such as a digital signal processor (DSP) that handles digital subscriber line (DSL) communications.
The use of more than one processor in a system, however, has numerous drawbacks. Not only does each additional processor increase the overall cost of, for example, a personal computer, but in conventional processing architectures, each additional processor requires its own memory and memory interface to store data and instructions used by that processor. This increases the overall chip count and pin count of the system and further increases the cost of the system.
Therefore, there is a need in the art for improved processing systems that minimize the cost and the complexity of multiprocessor systems. In particular, there is a need in the art for improved processing systems that minimize the amount of memory used in a processing system containing a main processor and at least one additional processor.
SUMMARY OF THE INVENTION
The limitations inherent in the prior art described above are overcome by an advantageous embodiment of the present invention, which provides a processing system comprising: 1) a first data processor comprising a unified memory architecture capable of receiving memory access requests from an external bus coupled to the first data processor; 2) a memory coupled to the first data processor and controlled by the unified memory architecture, the memory capable of storing a first plurality of instructions executable by the first data processor; and 3) a second data processor coupled to the external bus and capable of sending the memory access requests to the first data processor, wherein the memory access requests access data used by the second data processor stored in the memory.
According to one embodiment of the present invention, the data used by the second data processor comprises a second plurality of instructions executable by the second data processor.
According to another embodiment of the present invention, the second data processor further comprises an on-chip memory capable of storing a third plurality of instructions executable by the second data processor.
According to still another embodiment of the present invention, the second processor is capable of controlling the external bus.
According to yet another embodiment of the present invention, the external bus is a peripheral component interconnect (PCI) bus.
According to a further embodiment of the present invention, the second data processor is disposed in a peripheral device associated with the first data processor.
According to a still further embodiment of the present invention, the peripheral device is a communication device and the second data processor is a digital signal processor.
The foregoing has outlined rather broadly the features and technical advantages of the present invention so that those skilled in the art may better understand the detailed description of the invention that follows. Additional features and advantages of the invention will be described hereinafter that form the subject of the claims of the invention. Those skilled in the art should appreciate that they may readily use the conception and the specific embodiment disclosed as a basis for modifying or designing other structures for carrying out the same purposes of the present invention. Those skilled in the art should also realize that such equivalent constructions do not depart from the spirit and scope of the invention in its broadest form.
Before undertaking the DETAILED DESCRIPTION OF THE INVENTION, it may be advantageous to set forth definitions of certain words and phrases used throughout this patent document: the terms “include” and “comprise,” as well as derivatives thereof, mean inclusion without limitation; the term “or,” is inclusive, meaning and/or; the phrases “associated with” and “associated therewith,” as well as derivatives thereof, may mean to include, be included within, interconnect with, contain, be contained within, connect to or with, couple to or with, be communicable with, cooperate with, interleave, juxtapose, be proximate to, be bound to or with, have, have a property of, or the like; and the term “controller” means any device, system or part thereof that controls at least one operation, such a device may be implemented in hardware, firmware or software, or some combination of at least two of the same. It should be noted that the functionality associated with any particular controller may be centralized or distributed, whether locally or remotely. Definitions for certain words and phrases are provided throughout this patent document, those of ordinary skill in the art should understand that in many, if not most instances, such definitions apply to prior, as well as future uses of such defined words and phrases.
BRIEF DESCRIPTION OF THE DRAWINGS
For a more complete understanding of the present invention, reference is now made to the following descriptions taken in conjunction with the accompanying drawings, in which:
FIG. 1 is a block diagram of a prior art processing system, which includes an integrated microprocessor;
FIG. 2 is a block diagram of a processing system, including an integrated microprocessor and an external coprocessor, according to one embodiment of the present invention;
FIG. 3 is a block diagram of a processing system, including an integrated microprocessor and an external coprocessor, according to an alternate embodiment of the present invention; and
FIG. 4 is a flow diagram illustrating the operation of the processing system in FIG. 2, according to one embodiment of the present invention.
DETAILED DESCRIPTION OF THE INVENTION
FIGS. 1 through 4, discussed below, and the various embodiments used to describe the principles of the present invention in this patent document are by way of illustration only and should not be construed in any way to limit the scope of the invention. Those skilled in the art will understand that the principles of the present invention may be implemented in any suitably arranged processing system.
FIG. 1 is a block diagram of prior art processing system 10 , which includes integrated microprocessor 100 and external coprocessor 170 . Integrated microprocessor 100 comprises central processing unit (CPU) 105 , graphics unit 110 , system memory controller 115 , and bus interface 125 , all of which are coupled to communication bus 106 . Graphics unit 110 and system memory controller 115 may be integrated onto the same die as microprocessor 100 .
Integrated memory controller 115 bridges microprocessor 100 to system memory 140 , and may provide data compression and/or decompression to reduce bus traffic over external memory bus 145 . Integrated graphics unit 110 may provide one or more of TFT, DSTN, RGB, and other types of video output to drive display 150 . Bus interface unit 125 connects integrated microprocessor 100 to chipset bridge 155 . Bus interface unit 125 may support the peripheral component interconnect (PCI) bus interface.
Chipset bridge 155 may provide a conventional peripheral component interconnect (PCI) bus interface to PCI bus 160 , which connects chipset bridge 155 to one or more peripherals, such as sound card 162 , LAN controller 164 , disk drive 166 , and peripheral processor 170 , among others. In some embodiments, chipset bridge 155 may integrate local bus functions such as sound, disk drive control, modem, network adapter, and the like.
Peripheral processor 170 may be anyone of a wide variety of processing devices that may be implemented in processing system 10 . For example, peripheral processor 170 may be a digital signal processor (DSP) that provides a capability for communicating with external devices, such as a digital subscriber line (DSL). Alternatively, peripheral processor 170 may be a dedicated microprocessor that performs only a limited set of function(s) and that is subordinate to microprocessor 100 . Peripheral processor 170 may also be a microcontroller device or an ASIC circuit that is capable of executing instructions retrieved from a memory.
Typically, peripheral processor 170 requires its own memory to store the code that it executes. If only a small amount of code is executed by peripheral processor 170 , then the memory may be a dedicated on-chip random access memory (RAM), such as RAM 172 , that is integrated into peripheral processor 170 . However, as the size of the executable code used by peripheral processor 170 grows, the use of on-chip RAM 172 becomes impractical. For this reason, peripheral processor 170 typically requires external memory 174 to store instructions and data used by peripheral processor 170 . Unfortunately, this increases the amount of memory required by processing system 10 . This increases the overall chip count and the number of pins used to interface with memory.
FIG. 2 is a block diagram of processing system 20 , including integrated microprocessor 100 , according to one embodiment of the present invention. Processing system 20 is similar in most respects to prior art processing system 10 in FIG. 1 . Integrated microprocessor 100 comprises central processing unit (CPU) 105 , graphics unit 110 , system memory controller 115 , and bus interface 125 , all of which are coupled to communication bus 106 . Graphics unit 110 and system memory controller 115 may be integrated onto the same die as microprocessor 100 .
Integrated memory controller 115 bridges microprocessor 100 to system memory 140 , and may provide data compression and/or decompression to reduce bus traffic over external memory bus 145 . Integrated graphics unit 110 may provide one or more of TFT, DSTN, RGB, and other types of video output to drive display 150 . Bus interface unit 125 connects integrated microprocessor 100 to chipset bridge 155 . Bus interface unit 125 may support the peripheral component interconnect (PCI) bus interface.
Chipset bridge 155 may provide a conventional peripheral component interconnect (PCI) bus interface to PCI bus 160 , which connects chipset bridge 155 to one or more peripherals, such as sound card 162 , LAN controller 164 , disk drive 166 , and peripheral processor 210 , among others. In some embodiments, chipset bridge 155 may integrate local bus functions such as sound, disk drive control, modem, network adapter, and the like.
Those skilled in the art will recognize that bus interface unit 125 and memory controller 115 in microprocessor 100 comprise what is frequently referred to as a “north bridge” architecture. Similarly, chipset bridge 155 and PCI bus 160 are frequently referred to as a “south bridge” architecture.
Peripheral processor 210 may be anyone of a wide variety of processing devices that may be implemented in processing system 20 . For example, peripheral processor 210 may be a digital signal processor (DSP) that provides a capability for communicating with external devices, such as a digital subscriber line (DSL) Alternatively, peripheral processor 210 may be a general purpose microprocessor that is dedicated to performing only a limited set of function(s) and that is subordinate to microprocessor 100 . Peripheral processor 210 may also be a microcontroller, an ASIC chip, a programmable logic array (PAL) chip, or similar device that is capable of executing instructions retrieved from a memory.
As in the case of peripheral processor 170 in prior art processing system 10 , peripheral processor 210 also requires memory to store the code executed by peripheral processor 210 . Again, if only a small amount of code is executed by peripheral processor 210 , then the memory may be a dedicated on-chip random access memory (RAM), such as RAM 220 , that is integrated into peripheral processor 210 . However, if the size of the executable code used by peripheral processor 210 is large, peripheral processor 210 also requires an external memory to store instructions and data used by peripheral processor 210 . Unlike the prior art system, however, peripheral processor 210 uses the same memory, namely system memory 140 , used by microprocessor 100 , to store data and instruction code used by peripheral processor 210 . This decreases the amount of memory required by processing system 20 and reduces the overall chip count and the number of pins used to access memory.
In an advantageous embodiment of the present invention, bus interface unit 125 is implemented as a unified memory architecture (UMA) design and at least a portion of system memory 140 comprises dedicated memory 230 . Dedicated memory 230 comprises graphics memory 240 . In prior art processing system 10 , dedicated memory 141 typically is used by graphics unit 110 to hold graphics data and instruction code, represented collectively as graphics memory 142 in dedicated memory 141 . In accordance with an advantageous embodiment of the present invention, the instructions and data used by peripheral processor 210 , represented collectively as peripheral processor memory 250 , are also stored in dedicated memory 230 . The use of dedicated memory 230 allows the code and data in peripheral processor memory 250 used by peripheral processor 210 to be accessed without the need for page tables. In other words, the instruction code and data in peripheral processor memory 250 is always in dedicated memory 230 at the same physical address.
In order to use system memory 140 to store and to retrieve data and instruction code that it needs, peripheral processor 210 takes advantages of the features of the PCI Local Bus Specification followed by chipset bridge 155 . The PCI bus standard describes the way that peripherals on PCI bus 160 are electrically connected and the structured and controlled manner in which those peripherals must behave. Specifically, peripheral processor 210 uses the “bus mastering” capability of the PCI bus standard. Bus mastering allows peripheral processor 210 , or any other device on PCI bus 160 , to take control of PCI bus 160 and perform transfers directly, without requiring CPU 105 to act a “middle man” for any data transfers. The bus mastering capability is facilitated by chipset bridge 155 , which arbitrates requests to take control of PCI bus 160 from the peripherals attached to PCI bus 160 .
When peripheral processor 210 takes control of PCI bus 160 , peripheral processor 210 can directly access peripheral processor memory 250 via the unified memory architecture (UMA) provided by bus interface unit 125 without requiring any action by CPU 105 . In a non-UMA system, data must be transferred between graphics, video and imaging memory located on separate memory boards. In a UMA design, main (or system) memory used by CPU 105 , frame buffer, z-buffer, texture memory, rendering memory, image memory, video memory are all implemented in system memory 140 . Bus interface unit 125 arbitrates memory requests from the different subsystems in processing system 20 , including CPU 105 , graphics unit 110 , and chipset bridge 155 . Thus, each one of CPU 105 , graphics unit 110 , and chipset bridge 155 has direct access to the contents of system memory 140 . Bus interface unit 125 is capable of automatically reallocating memory space in system memory 140 according to the relative needs of CPU 105 , graphics unit 110 , chipset bridge 155 , and other devices.
FIG. 3 is a block diagram of processing system 30 , including integrated microprocessor 100 and external coprocessor 210 , according to an alternate embodiment of the present invention. The operation of processing system 30 is similar in nearly all respects to the operation of processing system 20 in FIG. 2 . However, in processing system 30 , coprocessor 210 is implemented in chipset bridge 155 . In this type of configuration, coprocessor 210 may be an integral part of chipset bridge 155 that controls its operation. Alternatively, coprocessor 210 may be a distinct PCI device that is incorporated into chipset bridge 155 in order to save board space. Nonetheless, the operation of coprocessor 210 in FIG. 3 is substantially the same as the operation of coprocessor 210 in FIG. 2 .
FIG. 4 depicts flow diagram 400 , which illustrates the operation of processing system 20 , according to one embodiment of the present invention. Initially, peripheral processor 210 must make an access to system memory 140 in order to fetch instruction(s), to read data, to write data, or to perform some combination of these operations. Peripheral processor 210 begins a memory access cycle by requesting control of PCI bus 160 (i.e., bus master request) from chipset bridge 155 (process step 405 ). After chipset bridge 155 receives the request and arbitrates it with any other such requests, peripheral processor 210 becomes the bus master of PCI bus 160 (process step 410 ).
Next, peripheral processor 210 sends a memory access request through chipset bridge 155 and an I/O interface (not shown) to the unified memory architecture controlled by bus interface unit 125 (process step 415 ). Bus interface unit 125 arbitrates the memory access request received from peripheral processor 210 with any other pending memory access requests that may have been received from CPU 105 or any other device in processing system 20 (process step 420 ). Then, bus interface unit 125 processes the peripheral processor 210 memory access request by 1) fetching instructions from system memory 140 , 2) reading data from system memory 140 , or 3) writing data to system memory 140 , or some combination of two or more of these operations (process step 425 ).
When the memory access request is completed, peripheral processor 210 relinquishes control over PCI bus 160 and chipset bridge 155 again is bus master of PCI bus 160 (process step 430 ). Next, peripheral processor 210 processes any pending instructions, including instructions fetched during the memory access cycle, until the next memory access is needed (process step 435 ). Peripheral processor 210 then returns to process step 405 to begin the next memory access cycle.
Generally speaking, the memory access performed by coprocessor 210 into system memory 140 will be slower than the memory access performed by the prior art coprocessor 170 (which uses dedicated external memory 174 ). Therefore, on-chip RAM 220 should be designed to be large enough to contain the “inner loops” of performance-critical code. On-chip RAM 220 may also be used by coprocessor 210 to temporarily store intermediate calculation values during fast data manipulations before returning a final block of data to coprocessor memory 250 .
Although the foregoing text described an embodiment of the present invention in which peripheral processor 210 is coupled to the unified memory architecture of microprocessor 100 by means of a PCI bus, those skilled in the art will understand that this is by way of illustration only. The PCI embodiment described above should not be construed so as to limit the scope of the present invention in any way. In fact, peripheral processor 210 may be coupled to the unified memory architecture of microprocessor 100 by means of any external bus that may be controlled (or mastered) by a peripheral device coupled to that external bus.
Although the present invention has been described it detail, those skilled in the art should understand that they can make various changes, substitutions and alterations herein without departing from the spirit and scope of the invention in its broadest form. | There is disclosed a processing system comprising: 1) a first data processor comprising a unified memory architecture for receiving memory access requests from an external bus coupled to the first data processor; 2) a memory coupled to the first data processor and controlled by the unified memory architecture, the memory storing a first plurality of instructions executable by the first data processor; and 3) a second data processor coupled to the external bus and capable of sending the memory access requests to the first data processor, wherein the memory access requests access data used by the second data processor stored in the memory. | 6 |
CROSS-REFERENCE TO RELATED APPLICATION
This application hereby incorporates by reference and claims benefit of U.S. application Ser. No. 09/642,066, filed on Aug. 18, 2000, now U.S. Pat. No. 6,751,635.
BACKGROUND OF THE INVENTION
1. Field of the Invention
This invention relates to file server systems, including those file server systems in which it is desired to maintain reliable file system consistency.
2. Related Art
In systems providing file services, such as those including file servers and similar devices, it is generally desirable for the server to provide a file system that is reliable despite the possibility of error. For example, it is desirable to provide a file system that is reliably in a consistent state, regardless of problems that might have occurred with the file server, and regardless of the nature of the file system operations requested by client devices.
One known method of providing reliability in systems that maintain state (including such state as the state of a file system or other set of data structures) is to provide for recording checkpoints at which the system is known to be in a consistent state. Such checkpoints, sometimes called “consistency points,” each provide a state to which the system can retreat in the event that an error occurs. From the most recent consistency point, the system can reattempt each operation to reach a state it was in before the error.
One problem with this known method is that some operations can require substantial amounts of time in comparison with the time between consistency points. For example, in the WAFL file system (as further described in the Incorporated Disclosures), operations on very large files can require copying or modifying very large numbers of file blocks in memory or on disk, and can therefore take a substantial fraction of the time from one consistency point to another. In the WAFL file system, two such operations are deleting very large files and truncating very large files. Accordingly, it might occur that recording a consistency point cannot occur properly while one of these extra-long operations is in progress.
The fundamental requirement of a reliable file system is that the state of the file system recorded on non-volatile storage must reflect only completed file system operations. In the case of a file system like WAFL that issues checkpoints, every file system operation must be complete between two checkpoints. In the earliest versions of the WAFL file system there was no file deletion manager present, thus very large files created a problem as it was possible that such large files could not be deleted between the execution of two consistency checkpoints.
This problem was partially solved in later versions of the WAFL file system, where a file deletion manager was assigned to perform the operation of file deletion, and a consistency point manager was assigned to perform the operation of recording a consistency point. The file deletion manager would attempt to resolve the problem of extra-long file deletions by repeatedly requesting more time from the consistency point manager, thus “putting off” the consistency point manager until a last-possible moment. However, at that last-possible moment, the file deletion manager would be required to give way to the consistency point manager, and allow the consistency point manger to record the consistency point. When this occurred, the file deletion manager would be unable to complete the file deletion operation. In that earlier version of the WAFL file system, instead of completing the file deletion operation, the file deletion manager would move the file to a “zombie file” list to complete the file deletion operation. At a later time, a zombie file manager would re-attempt the file deletion operation for those files on the zombie file list.
While this earlier method achieved the general result of performing file deletions on very large files, it has the drawbacks that it is a source of unreliability in the file system. First, the number of files that could be processed simultaneously as zombie files was fixed in the previous version.
Second, the file deletion manager and crash recovery mechanism did not communicate. The file deletion manager did not notify the crash recovery mechanism that a file was being turned into a zombie and the crash recovery mechanism was unable to create zombie files. Thus, to allow a checkpoint to be recorded, a long file would have to be turned into a zombie. If the system crashed at this point, the crash recovery mechanism might not be able to correctly recover the file system since it is unaware that a zombie file should be created and was incapable of creating zombie files should the need arise.
Third, since the file deletion manager and replay mechanism did not communicate the free space reported could be inaccurately reported. Attempts to restore state could fail, because the amount of free space could be different than that actually available.
Fourth, the earlier method is non-deterministic in the sense that it is not assured whether any particular file deletion operation will be completed before or after a selected consistency point. Moreover, the earlier method does not resolve problems associated with other extra-long file operations, such as requests to truncate very large files to much smaller length.
Accordingly, it would be advantageous to provide a technique for extra-long operations in a reliable state-full system (such as a file system), that is not subject to the drawbacks of the known art. Preferably, in such a technique, those parts of the system responsible for recording of consistency points are fully aware of the intermediate states of extra-long operations, the performance of extra-long operations is relatively deterministic, and performance of extra-long operations is atomic with regard to consistency points.
SUMMARY OF THE INVENTION
The invention provides a method and system for reliably performing extra-long operations in a reliable state-full system (such as a file system). The system records consistency points, or otherwise assures reliability, notwithstanding the continuous performance of extra-long operations and the existence of intermediate states for those extra-long operations. Moreover, performance of extra-long operations is both deterministic and atomic with regard to consistency points (or other reliability techniques used by the system).
The file system includes a separate portion of the file system reserved for files having extra-long operations in progress, including file deletion and file truncation. This separate portion of the file system is called the zombie file space; it includes a separate name space from the regular (“live”) file system that is accessible to users, and is maintained as part of the file system when recording a consistency point. The file system includes a file deletion manager that determines, before beginning any file deletion operation, whether it is necessary to first move the file being deleted to the zombie file space. The file system includes a zombie file deletion manager that performs portions of the file deletion operation on zombie files in atomic units.
The file system also includes a file truncation manager. Before beginning any file truncation operation, the file truncation manager determines whether it is necessary to create a complementary file called an “evil twin” file. The truncation manager will move all blocks to be truncated from the file being truncated to the evil twin file. Moving blocks is typically faster and less resource-intensive than deleting blocks. The “evil twin” is subsequently transformed into a zombie file. The file system includes a zombie file truncation manager that can then perform truncation of the zombie file asynchronously in atomic units. Furthermore, the number of files that can be linked to the zombie filespace is dynamic allowing the zombie filespace the ability to grow and shrink as required to process varying numbers of files.
An additional advantage provided by the file system is that files having attached data elements, called “composite” files, can be subject to file deletion and other extra-long operations in a natural and reliable manner. The file system moves the entire composite file to the zombie file space, deletes each attached data element individually, and thus resolves the composite file into a non-composite file. If the non-composite file is sufficiently small, the file deletion manager can delete the non-composite file without further need for the zombie file space. However, if the non-composite file is sufficiently large, the file deletion manager can delete the non-composite file using the zombie file space.
The invention provides an enabling technology for a wide variety of applications for reliable systems, so as to obtain substantial advantages and capabilities that are novel and non-obvious in view of the known art. Examples described below primarily relate to reliable file systems, but the invention is broadly applicable to many different types of systems in which reliability and extra-long operations are both present.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 shows a block diagram of a portion of a system using a zombie file space.
FIG. 2 illustrates a file structure in a system using a zombie file space.
FIG. 3 shows a process flow diagram for file deletion in a method for operating a system for manipulation of zombie files and evil-twin files.
FIG. 4 shows a process flow diagram for file truncation in a method for operating a system Manipulation of Zombie Files and Evil-Twin Files.
LEXICOGRAPHY
The following terms refer to or relate to aspects of the invention as described below. The descriptions of general meanings of these terms are not intended to be limiting, only illustrative.
live filespace—This term generally refers to a storage area within a file server where flies are available to system users.
As noted above, these descriptions of general meanings of these terms are not intended to be limiting, only illustrative. Other and further applications of the invention, including extensions of these terms and concepts, would be clear to those of ordinary skill in the art after perusing this application. These other and further applications are part of the scope and spirit of the invention, and would be clear to those of ordinary skill in the art, without further invention or undue experimentation.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
In the following description, a preferred embodiment of the invention is described with regard to preferred process steps and data structures. Embodiments of the invention can be implemented using general-purpose processors or special purpose processors operating under program control, or other circuits, adapted to particular process steps and data structures described herein. Implementation of the process steps and data structures described herein would not require undue experimentation or further invention.
RELATED APPLICATIONS
Inventions described herein can be used in conjunction with inventions described in the following documents.
U.S. patent application Ser. No. 09/642,062, filed Aug. 18, 2000, in the name of Rajesh Sundaram, et al., titled “Dynamic Data Space,” now U.S. Pat. No. 6,728,922. U.S. patent application Ser. No. 09/642,061, filed Aug. 18, 2000, in the name of Blake Lewis et al., titled “Instant Snapshot.” U.S. patent application Ser. No. 09/642,065, filed Aug. 18, 2000, in the name of Douglas Doucette, et al., titled “Improved Space Allocation in a Write Anywhere File System,” now U.S. Pat. No. 6,636,879.
and
U.S. patent application Ser. No. 09/642,064, filed Aug. 18, 2000, in the name of Scott SCHOENTHAL, et al., titled “Persistent and Reliable Delivery of Event Messages.”
Each of these documents is hereby incorporated by reference as if fully set forth herein. This application claims priority of each of these documents. These documents are collectively referred to as the “Incorporated Disclosures.”
System Elements
FIG. 1 shows a block diagram of a portion of a system using a zombie file space.
A system 100 includes a file server 110 including a processor (not shown but understood by one skilled in the art), program and data memory (not shown but understood by one skilled in the art), network interface card 115 , and a mass storage 120
The network interface card 115 couples the file server 110 to a network. In a preferred embodiment, the network includes an Internet, intranet, extranet, virtual private network, enterprise network, or another form of communication network.
The mass storage 120 can include any device for storing relatively large amounts of information, such as magnetic disks or tapes, optical drives, or other types of mass storage.
File Structure Example
FIG. 2 illustrates a file structure in a system using a zombie file space.
A file structure 200 includes, a live file space 210 , an inode file 220 , a live file link 230 , a file 240 , a zombie file space 250 , and a zombie file link 260 .
The live file space 210 contains the root block and all associated blocks of data for live files (I.e. files that may be accessed by users).
The inode file 220 is associated with the file to be deleted and contains information about the file.
The live file link 230 , links a file to the live file space 210 .
The file 240 includes a plurality of file blocks 241 , and a plurality of block links 242 . The file blocks 241 are connected by the plurality of block links 242 . The file 240 is illustrative of a file to be deleted. The structure of the file as defined above is a hierarchical tree-like structure, however, there is no requirement in any embodiment of the invention that the invention be applied only to file structures of this type. The use of a hierarchical tree-like structure filing system is intended to be illustrative only and not limiting.
The zombie file space 250 contains the root block and all associated blocks of data for zombie files (I.e. files that are in the process of being deleted).
The zombie file link 260 , links a file to be deleted to the zombie file space 250 . A file that has been linked to the zombie file space 250 is referred to as a “zombie file” while it is so linked.
Method of Operation—File Deletion
A method 300 includes a set of flow points and a set of steps. The system 100 performs the method 300 . Although the method 300 is described serially, the steps of the method 300 can be performed by separate elements in conjunction or in parallel, whether asynchronously, in a pipelined manner, or otherwise. There is no particular requirement that the method 300 be performed in the same order in which this description lists the steps, except where so indicated.
At a flow point 310 , a system user selects the file 240 for deletion. User interfaces for this activity vary from system to system but are well known in the art.
At a flow point 320 , the file 240 is identified by the system as a large file requiring zombie processing. In a preferred embodiment, the specific size of a file necessary to trigger zombie processing is parameter-based, software-selectable, however, it can be any set of instructions supporting this functionality, such as instructions hard-coded on a computer chip.
At a flow point 325 , the file deletion manager determines whether the zombie filespace 250 needs to be enlarged to accommodate another zombie file, and if necessary enlarges the zombie filespace.
At a flow point 330 , the link connecting the file 240 to the live file space 210 is terminated. At this point the file 240 is no longer available to users connected to the file server 110 .
At a flow point 340 , the file 240 is linked to the zombie file space 250 via the zombie file link 260 . At this point, file 240 is referred to as a zombie file.
At a flow point 350 , the zombie file deletion manager starts deleting portions of the file 240 by terminating block links 242 at the outer leaves of the file tree. As file blocks 241 are deleted by the zombie deletion manager, they become available for storage of other data. This fact is reflected in the free space indicator of the mass storage 120 .
At a flow point 360 , the file 240 is moved from the zombie filespace to the live filespace.
Method of Operation—File Truncation
A method 400 includes a set of flow points and a set of steps. The system 100 performs the method 400 . Although the method 400 is described serially, the steps of the method 400 can be performed by separate elements in conjunction or in parallel, whether asynchronously, in a pipelined manner, or otherwise. There is no particular requirement that the method 400 be performed in the same order in which this description lists the steps, except where so indicated.
At a flow point 410 , a system user selects the file 240 for truncation. User interfaces for this activity vary from system to system but are well known in the art.
At a flow point 420 , the system identifies the amount of the file to be truncated as requiring evil twin/zombie processing. In the preferred embodiment, the specific amount of data to be truncated necessary to trigger evil twin/zombie processing is parameter-based software-selectable; however, it can be any set of instructions supporting this functionality, such as instructions hard-coded on a computer chip.
At a flow point 425 , the file deletion manager determines whether the zombie filespace 250 needs to be enlarged to accommodate another zombie file, and if necessary enlarges the zombie filespace.
At a flow point 430 , an evil twin file is created. At this point the file 240 is unavailable to the user.
At a flow point 440 , blocks of data to be truncated are moved from the file 240 to the evil twin file.
At a flow point 450 , file attributes for the file 240 are adjusted appropriately (E.g. The size of the file).
At a flow point 460 , the evil twin file is turned into a zombie file. It is connected to the zombie file space.
At a flow point 470 , the file 240 is marked as available in the live file space. At this point the file 240 is available to all users.
At a flow point 480 , the zombie deletion manager frees all blocks attached to the zombie file.
At a flow point 490 , the zombie file has been deleted and the link to the zombie file space is terminated.
At a flow point 495 , the file 240 is moved from the zombie filespace to the live filespace.
Generality of the Invention
The invention has general applicability to various fields of use, not necessarily related to the services described above. For example, these fields of use can include one or more of, or some combination of, the following:
The invention is applicable to all computer systems utilizing large files.
Other and further applications of the invention in its most general form, will be clear to those skilled in the art after perusal of this application, and are within the scope and spirit of the invention.
Although preferred embodiments are disclosed herein, many variations are possible which remain within the concept, scope, and spirit of the invention, and these variations would become clear to those skilled in the art after perusal of this application. | A method and system for reliably performing extra-long operations in a reliable state-full system (such as a file system). The file system includes a separate portion of the file system reserved for files having extra-long operations in progress, including file deletion and file truncation. This separate portion of the file system is called the zombie file space; it includes a separate name space from the regular (“live”) file system that is accessible to users, and is maintained as part of the file system when recording a consistency point. | 8 |
BACKGROUND OF THE INVENTION
(1) Field of the Invention:
This invention relates to a novel heterocyclic derivative of formula (I): ##STR5## wherein R 1 represents ##STR6## and R 2 represents a hydrogen atom or an acyl group; its preparation; and radiosensitizing agents and antiviral agents comprising the derivative as their active component.
(2) Description of the Background Art:
Hypoxic cells in tumor tissues are strongly resistant to radiation. This fact is considered to be one of key factors that explains the obstinacy or recrudescence after radiotherapy. In view that hypoxic cells do not exist in normal tissues, it is very important to enhance the radiosensitivity of the hypoxic cells in tumor tissues in order to obtain better results from radiotherapy.
Meanwhile, viral infectious diseases which attack mammals including humans are contagious and bring agony and economic loss to our society. Only limited viral infectious diseases are curable by currently available antiviral agents, and new synthetic antiviral agents stand in demand.
SUMMARY OF THE INVENTION
Under the above circumstances, the present inventors conducted intensive studies for developing agents capable of selectively sensitizing hypoxic cells without affecting the sensitivity of normal cells at the time of irradiation, in other words, radiosensitizing agents selectively directed to hypoxic cells (hereinafter referred to simply as radiosensitizing agents) and agents having antiviral activity. They found that compounds of formula (I) have low toxicity, high radiosensitizing effect, and antiviral activity even at a low concentration. The low toxicity of the compound is notable because toxicity has long been the most serious problem in this technical field.
Accordingly, it is an object of the invention to provide a heterocyclic derivative of formula (I) and a process for preparing the derivative. It is another object of the invention to provide a radiosensitizing agent and an antiviral agent comprising the derivative as their active component.
DETAILED DESCRIPTION OF THE INVENTION
When R 2 is acyl, compounds of formula (I) of this invention can be prepared, for example, by the following process: ##STR7## wherein R 4 represents an acyl group and R 1 has the same meaning as defined above.
In other words, compounds (Ia) of this invention can be prepared by reacting 1,3-diacyloxy-2-acyloxymethoxypropane (II) with a compound (III). The starting compound (II) is readily obtainable according, for example, to a method described in Proc. Nat. Acad. Sci. USA, 80, 4139 (1983) by A. K. Fielol et al.
The above reaction is carried out by melting a compound (II) and a compound (III) under a reduced pressure in the presence of a catalyst. As suitable catalyst, mention may be made of: protic acids such as p-toluenesulfonic acid, methanesulfonic acid and trichloroacetic acid; and Lewis acids such as anhydrous zinc chloride, anhydrous aluminum chloride and anhydrous stannic chloride. The proportion of compound (II) and compound (III) may be varied arbitrarily. Generally, it is recommended that the compound (II) be used in equivalent or a little excessive amount. The reaction temperature is preferably from 50° to 150° C. The reaction is preferably completed in between 30 minutes to 6 hours, depending on reagent, solvent, temperature, reaction accelerator, etc.
The compounds (Ia) of this invention can also be prepared according to the following process: ##STR8## wherein R 4 is as same as defined above and R 5 represents ##STR9##
In other words, compounds (Ia) of this invention can be obtained by reacting 1,3-diacyloxy-2-acyloxymethoxypropane (II) with compound (IV) which is sililated derivative of compound (III).
The compounds (IV) are readily obtainable by reacting their corresponding compounds (III) with excessive amounts of N,O-bis(trimethylsilyl)acetamide at room temperature or under heat while stirring. Unreacted silylation agents are removed by distillation under reduced pressure.
The reaction process according to this invention is carried out in the presence of a Lewis acid. Various Lewis acids are usable, and specific examples include anhydrous stannic chloride, anhydrous aluminum chloride, anhydrous zinc chloride, etc. They are preferably used in a catalystic amount or equivalent amount of compound (II).
The proportion of compound (II) and compound (IV) may be varied arbitrarily. In general, it is recommended that the compound (II) be used in an equimolar or a slightly excessive amount with respect to compound (IV). Various solvents can be used in this reaction, which include acentonitrile, methylene chloride, benzene, toluene, etc. The reaction proceeds at temperatures ranging from -30° to +50° C., and generally under water cooling conditions or at room temperature. The reaction is preferably completed in between 30 minutes to 6 hours, depending on reagent, solvent, temperature, reaction accelerator, etc.
After the reaction is completed, the objective products are separated from the reaction mixture and purified according to a conventional method. For instance, the reaction mixture is subjected to extraction process, followed by condensation after washing the extract, and the residue being purified by chromatography to obtain a compound (Ia) at a high yield.
Going back to the general formula (I), compounds (I) having hydrogen as R 2 can be prepared by deacylation of compounds (Ia) as shown below: ##STR10##
One example of the deacylation process is such that proceeds in absolute alcohol containing sodium alcoholate or in absolute alcohol saturated with ammonia, at a temperature ranging from 0° C. to room temperature over a few hours to overnight. Another example of suitable deacylation is hydrolysis in water-alcohol using an organic base such as triethylamine, pyridine, etc. at a temperature ranging from room temperature to 80° C. As suitable alcohol, lower alcohols such as methanol, ethanol and propanol may be mentioned.
Examples of the novel compounds (I) of this invention are:
(1) 1-[2-acetoxy-1-(acetoxymethyl)ethoxy]methyl-2-nitroimidazol,
(2) 1-[2-acetoxy-1-(acetoxymethyl)ethoxy]methyl-3-nitro-1,2,4-triazol,
(3) 1-[2-hydroxy-1-(hydroxymethyl)ethoxy]methyl-2-nitroimidazol,
(4) 1-[2-hydroxy-1-(hydroxymethyl)ethoxy]methyl-3-nitro-1,2,4-triazol.
In this specification, the above compounds (1) to (4) will hereinafter be referred to as compound (1), compound (2), compound (3) and compound (4).
Compounds (I) of this invention have low toxicity as shown by the test below, and have excellent radio-sensitizing ability as well as antiviral activity. They are preferably dosed 5 minutes to 5 hours prior to irradiation either orally or non-orally. They may be formed into tablets, capsules, granules, powders, sapositories or injections together with excipiens, stabilizers, preservatives, modifiers, etc. as required. The administration amount depends on the patient's age, the region where tumor is produced, species and types of tumor, conditions of the patient, etc., and is preferably 0.2 to 5.0 g/m 2 body surface.
ACTION AND EFFECT
Acute toxicity test and other tests regarding radiosensitising ability and antiviral activity were carried out using the compounds of the present invention.
(1) Acute toxicity test
ICR strain male mice of 5 week old were intravenously or intraperitoneally administered with various compounds each dissolved in a physiological saline or in a physiological saline containing 10% DMSO. The mice were observed over 14 days and 50% death rates (LD 50/14 ) were obtained. The results are shown in Table 1.
TABLE 1__________________________________________________________________________Compound DoseNos. Administration (mg/kg) Dead/Treated LD.sub.50/14 General Status__________________________________________________________________________1 intraperitoneal 720 0/2 >860 Calmed down " 860 0/22 intraperitoneal 600 0/2 790 Transient respiratory accelera- " 720 0/2 tion after administration, then " 860 2/2 calmed down3 intravenous 720 0/2 >860 Calmed down " 860 0/24 intravenous 720 0/2 860 Calmed down " 860 1/2__________________________________________________________________________
(2) Radiosensitivity test
(a) In vitro test 1
Cells used in the test: single cells of EMT-6
Irradiation: 60 Co - gamma rays
Cell treatment to hypoxia:
A mixture gas of 95% nitrogen and 5% carbon dioxide was passed through cell suspension.
Survival ratio of cells:
Determined by counting colonies.
Radiosensitivity enhancement ratio (ER): ##EQU1##
The results of this test are shown in Table 2.
TABLE 2______________________________________Compound Nos. Concentration (mM) ER______________________________________3 1.0 1.704 1.0 1.50______________________________________
(b) In vitro test 2
Cells used in the test: Spheroids of EMT-6
Irradiation: 60 Co - gamma rays
Tested compound: Compound (3), 1 mM
Determination of radiosensitivity enhancement:
Six particles of spheroid having a certain size were taken and placed in a culture solution containing compound (3) having a concentration of 1 mM, and incubated at 37° C. over 30 to 60 minutes, followed by irradiation. The spheroids were treated by trypsin and then the enhancement ratio (ER) was obtained by counting colonies.
The result obtained was:
ER of compound (3) at a concentration of 1 mM=1.55
(c) In vivo test
Animal: Balb/c mice
Tumor: EMT-6
Tested compound: compound (3), 200 mg/kg
Administration:
Compound (3) dissolved in a physiological saline was intraperitoneally administered 20 minutes prior to irradiation.
Irradiation: 60 Co - gamma rays, whole body irradiation
Determination of radiosensitivity enhancement:
Enhancement ratio (ER) was obtained from irradiation dose and reduction ratio of tumor cells.
The result obtained was:
ER of compound (3) (200 mg/kg)=1.55
(3) Antiviral activity test
Virus: Herpes simplex virus type I
Cells: Vero (monkey kidney cells)
Culture medium: 2% FBS MEM
A sample conditioned to contain 2×10 5 /ml of vero cells was cultured at 37° C. in an atmosphere of 5% CO 2 for 1 day to obtain a monolayer sample. The sample was infected by HSV virus diluted with PBS (phosphate buffer). Compound (I) was dissolved in DMSO, then adjusted to have concentrations of 100 μg/ml, 50 μg/ml, 10/μg/ml, 5,μ/ml and 1 μg/ml by 2% FBS MEM, and served as test agents. The culture cells were added with each agent separately and incubated at 37° C. in a Co 2 incubator for one day. The cytopathic effect was observed under microscope. Cells were stained by crystal violet and scored as follows:
0: almost all cells are dead
1: certain effect of test agent with some dead cells
2: normal
The results are shown in Table 3.
TABLE 3______________________________________ 100 50 10 5 1Compound Nos. μg/ml μg/ml μg/ml μg/ml μg/ml______________________________________3 2 2 1 0 04 2 2 1 0 0______________________________________
EXAMPLES
This invention may be more fully understood from the following examples.
EXAMPLE 1
1-[2-acetoxy-1-(acetoxymethyl)ethoxy]methyl-2-nitroimidazol: compound (1)
5.6 g of 2-nitroimidazol, 12.4 g of 1,3-diacetoxy-2-acetoxymethoxypropane and 0.5 g of p-toluenesulfonic acid monohydrate were placed in a flask connected with a trap for reducing pressure by an aspirator. The flask was heated by oil bath of 130°-140° C. under reduced pressure while stirred. Acetic acid was distilled out as the reaction proceeded. In about 15 minutes, the reaction was completed. After cooling down to room temperature, the content was added with about 300 ml ethyl acetate and subjected to extraction. The extract was washed with saturated aqueous sodium hydrogen carbonate, and with water in this order. Then it was dried over anhydrous sodium sulfate and concentrated under reduced pressure. The residue was purified by separable high performance liquid chromatography through silica gel columns using a mixture solvent (ethyl acetate - benzene) as an eluate to obtain 13.3 g of the title compound as a viscous oil material (yield: 88.6%).
MS(m/e): 301(M + ),
IR(cm -1 ): 1740 (CO), 1535 (NO 2 ), 1490 (NO 2 ),
NMR(δ, CDCl 3 ): 2.0 (s, 6H, CH 3 CO×2),
3.8-4.3 (m, 5H, --CH 2 OAc×2, ##STR11## 5.9 (s, 2H, ##STR12## 7.1 (s, 1H, ring proton), 7.4 (s, 1H, ring proton).
EXAMPLE 2
1-[2-acetoxy-1-(acetoxymethyl)ethoxy]methyl-3-nitro-1,2,4-triazol: compound (2)
General procedures of Example 1 were followed to obtain the title compound as a viscous oil material (yield: about 83%).
MS(m/e): 302(M + ).
IR(cm -1 ): 1740 (CO), 1555 (NO 2 ), 1500 (NO 2 ),
NMR(δ, CDCl 3 ): 2.0(s, 6H, CH 3 CO×2),
3.8-4.3 (m, 5H, --CH2OAc×2, ##STR13##
5.9 (s, 2H, ##STR14## 8.7 (s, 1H, ring proton).
EXAMPLE 3
1-[2-hydroxy-1-(hydroxymethyl)ethoxy]methyl-2-nitroimidazol: compound (3)
3.01 g of 1-[2-acetoxy-1-(acetoxymethyl)ethoxy]-methyl-2-nitroimidazol (compound (1)) was dissolved in 50 ml of absolute methanol, and stirred at room temperature while being added with 5% absolute ethanol solution of sodium ethoxide dropwise until pH reached 9.0. Stirred at room temperature over 3 hours. Then Dowex 50 W (H + , made by Dow Chemical) was slowly added until the liquid had a pH of 7.0. Dowex 50 W was removed by suction filtration, and the solvent was distilled off under reduced pressure. The residue was subjected to recrystallization by ethanol to obtain 2.83 g of the title compound as light yellow needles (yield: 94%).
Melting point: 88° C.
MS(m/e): 218 (M+1), 185, 114, 98
IR(cm -1 ): 3450 (OH), 1540 (NO 2 ), 1490 (NO 2 )
NMR [δ, DMSO(d 6 )]: 3.2-3.6 (m, 5H, --CH 20 H×2, ##STR15## 4.6 (t, 2H, OH×2), 5.9(s, 2H, ##STR16## 7.15(s, 1H, ring proton), 7.8 (s, 1H, ring proton).
EXAMPLE 4
1-[2-hydroxy-1-(hydroxymethyl)ethoxy]methyl-3-nitro-1,2,4-triazol: compound (4)
General procedures of Example 3 were followed to obtain the title compound as colorless needles (yield: 95%).
Melting point: 132° C.
MS(m/e): 219 (M+1), 205, 185.
IR(cm -1 ): 3450 (OH), 1560 (NO 2 ), 1500 (NO 2 )
NMR [δ, DMSO(d 6 )]: 3.3-3.8 (m, 5H, --CH 2 OH×2, ##STR17## 4.6 (t, 2H, OH×2), 5.8 (s, 2H, ##STR18## 9.0(s, 1H, H in 5th position). | A novel heterocyclic derivative of formula (I): ##STR1## wherein R 1 represents ##STR2## and R 2 represents hydrogen or acyl. When R 2 is acyl, the derivative can be prepared, for example, by the following process: ##STR3## wherein R 4 is acyl and R 1 is ##STR4## The derivative is less toxic and has radiosensitizing activity and antiviral activity even at a low concentration.
Radiosensitizing agents and antiviral agents containing the derivative as active component are also disclosed. | 2 |
CROSS-REFERENCE SECTION TO RELATED APPLICATION
[0001] This application claims the benefit of U.S. Provisional Patent Application No. 61/037,775, filed Mar. 19, 2008, which is hereby incorporated by reference in its entirety.
FIELD OF THE INVENTION
[0002] The invention provides a construct comprising an amino acid sequence attached to a luciferin substrate, wherein the amino acid sequence is not a substrate for either luciferase or a caspase to render the substrate inactive in the presence of luciferase. The construct is useful, for example, as a negative control for in vitro apoptosis assays and the bioluminescent imaging of drug-induced apoptosis in vivo. The invention also provides methods for screening for novel modulators of an apoptosis-related disease.
BACKGROUND OF THE INVENTION
[0003] Optical imaging is a noninvasive technique that utilizes bioluminescent and fluorescent endogenous reporters or exogenous probes to monitor molecular and biological processes. While both modalities detect levels of visible light, a clear distinction exists between them with respect to how this light is created. Bioluminescence (e.g. firefly luciferase using the substrate luciferin) is the production and emission of light resulting from a chemical reaction during which chemical energy is converted to light energy (560-660 nm). This is an enzymatic process that requires a chemical substrate in order for light to be produced. Alternatively, fluorescence (e.g. GFP, RFP and near-IR proteins) occurs when the molecular absorption of a photon at one wavelength (400-600 nm) triggers the emission of another photon with a longer wavelength (450-650 nm). Fluorogenic compositions for the detection of protease activity are known, for example, in WO 98/37226.
[0004] Imaging of drug-induced apoptosis has become a focal interest in both experimental and clinical research. Z-DEVD-aminoluciferin (VivoGlo™ Caspase-3/7), manufactured by Promgea, is a substrate for luciferase only when cleaved by a cysteine aspartic acid-specific protease. Typically, the cysteine aspartic acid-specific proteases are cysteine aspartic acid-specific protease-3 (“caspase-3”) and cysteine aspartic acid-specific protease-7 (“caspase-7”), molecular markers of apoptosis. Methods of monitoring caspase-3/7 activity in vivo would provide a vaulable tool for assessing preclinical drug efficacy, allowing for quicker development of therapies. U.S. Pat. No. 7,148,030 describes a sensitive bioluminescent assay to detect proteases including caspases. Use of aminoluciferins for in vivo imaging is also known. Shah et al. (Molecular Therapy, Vol. 11, No. 6: 926-931) describes the single time-point use of a caspase-3-activatable aminoluciferins for in vivo bioluminescent imaging. One hurdle that has to be overcome with the use of aminoluciferase agents is the need for an appropriate negative control that is not a substrate for either luciferase or caspase-3/7.
SUMMARY OF THE INVENTION
[0005] The invention provides a construct comprising an amino acid sequence attached to a luciferin substrate, wherein the amino acid sequence is not a substrate for either luciferase or a caspase, to serve as a negative control for a ZDEVD-aminoluciferin. Since the sequence is not a substrate for a caspase, even in apoptotic cells no light will be emitted. Thus, such a molecule would serve as a negative control for either in vitro apoptosis assays or for in vivo bioluminescent imaging studies utilizing, for instance, the VivoGlo™ Caspase-3/7 substrate.
[0006] In one embodiment, the present invention provides a construct comprising a sequence that is not a substrate for either luciferase or a caspase attached to a luciferin molecule. In another embodiment, the sequence is selected from the group consisting of DEVN, DDDD, FA, VEID, LEHD, and YVAD. In a more preferred embodiment, the sequence is DEVN. In another embodiment, the present invention comprises the construct as a negative control for an in vitro apoptosis assay. In another embodiment, the present invention comprises the construct as a negative control for in vivo bioluminescent imaging. In another embodiment, the luciferin molecule is an aminoluciferin. In one embodiment, the present invention comprises a method of identifying modulators of an apoptosis-related disease.
DETAILED DESCRIPTION
[0007] The present invention now will be described more fully hereinafter. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein; rather, these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the scope of the invention to those skilled in the art.
[0000] All amino acid abbreviations used in this disclosure are those accepted by the United States Patent and Trademark Office as set forth in 37 C.F.R. sctn. 1.822(b).
“apoptosis-related disease”—a disease whose etiology is related either wholly or partially to the process of apoptosis. The disease may be caused either by a malfunction of the apoptotic process (such as in cancer or an autoimmune disease) or by overactivity of the apoptotic process (such as in certain neurodegenerative diseases).
“Cancer” or “Tumor”—an uncontrolled growing mass of abnormal cells. These terms include both primary tumors, which may be benign or malignant, as well as secondary tumors, or metastases which have spread to other sites in the body.
“Modulator”—any molecule that is capable of modulation, i.e. that either increases (promotes) or decreases (prevents). The term is understood to include partial or full inhibition, stimulation and enhancement.
“Treatment”—the term “treatment” and corresponding terms “treat” and “treating” includes palliative, restorative, and preventative treatment of a subject. The term “palliative treatment” refers to treatment that eases or reduces the effect or intensity of a condition in a subject without curing the condition. The term “preventative treatment” (and the corresponding term “prophylactic treatment” refers to treatment that prevents the occurrence of a condition in a subject. The term “restorative treatment” refers to treatment that halts the progression of, reduces the pathologic manifestations of, or entirely eliminates a condition in a subject.
Embodiments of the Constructs
[0008] In one embodiment, the present invention comprises a construct comprising an amino acid sequence attached to a luciferin substrate, wherein the amino acid sequence is not a substrate for either luciferase or a caspase. Preferably, the caspase is caspase-3, caspase-7 or both caspase-3/7. Preferably, the sequence that is not a substrate for either luciferase or caspase-3/7 is four amino acids in length. More preferably, the sequence is four amino acids in length and has at least 25% homology to the sequence DEVD. More preferably, the sequence is four amino acids in length and has at least 50% homology to the sequence DEVD. Even more preferably, the sequence is four amino acids in length and has at least 75% homology to the sequence DEVD. In a preferred embodiment, the sequences are selected from the group consisting of DEVN, DDDD, FA, VEID, LEHD, and YVAD. In a more preferred embodiment, the sequences are selected from the group consisting of DEVN and LEHD. In a more preferred embodiment, the sequence is DEVN. In another embodiment, the present invention comprises the use of these sequences as a negative control for in vivo imaging.
[0009] In one embodiment, the luciferin molecule is selected from the group consisting of a bacterial luciferin, a dinoflagellate luciferin, a vargula luciferin, a coelenterasine luciferin, a firefly luciferin and a beetle luciferin. In another embodiment, the luciferin molecule is a beetle luciferin. In another embodiment, the luciferin molecule is an aminoluciferin. In a more preferred embodiment, the luciferin molecule is an aminoluciferin having the structure wherein the luciferin molecule is an amino luciferin having the structure
[0000]
[0010] In another embodiment, the construct is selected from the group consisting of
[0000]
Methods of Identifying Modulators of an Apoptosis-Related Disease
[0011] In one embodiment, the present invention comprises a method of identifying modulators of an apoptosis-related disease comprising
(a) administering a modulator of an apoptosis-related disease and a construct comprising a caspase-3/7 substrate attached to a luciferin molecule to luciferase-expressing apoptosis-related diseased cells in a first container; (b) measuring the photon emission of the first container with a photodetector device; (c) administering a modulator of an apoptosis-related disease and a construct comprising a sequence that is not a substrate for either luciferase or caspase-3/7 attached to a luciferin molecule to luciferase-expressing apoptosis-related diseased cells; (d) measuring the photon emission of the second container with a photodetector device; and (e) comparing the photon emission of the first container and the second container.
[0017] A modulator of an apopotosis-related disease, wherein the modulator is pro-apoptotic, will have increased the photon emission of the first container. A modulator of an apopotosis-related disease, wherein the modulator is anti-apoptotic, will have decreased the photon emission of the first container. It is understood that it is within the scope of the method for the first measure and the second measure to be taken in the reverse chronological order. The container can be, for instance, a well in a microtiter plate. In one embodiment, the plate is a 96-well plate. In another embodiment, the construct of step (c) is selected from the group consisting of DEVN, DDDD, FA, VEID, LEHD, and YVAD and the luciferin molecule is an amino luciferin having the structure
[0000]
[0018] In one embodiment of the methods of the present invention, the subject is a mammal. In another embodiment, the subject is a rat. In another embodiment, the subject is a mouse. In another embodiment, the subject is a human.
[0019] In one embodiment, the present invention comprises a method of identifying modulators of an apoptosis-related disease comprising
(f) administering to a first subject luciferase-expressing cells; (g) allowing the cells to achieve localization in the first subject; (h) administering a modulator of an apoptosis-related disease and a construct comprising a caspase-3/7 substrate attached to a luciferin molecule to the first subject; (i) imaging the photon emission of the first subject with a photodetector device; (j) administering to a second subject luciferase-expressing cells; (k) allowing the cells to achieve localization in the second subject; (l) administering a modulator of an apoptosis-related disease and a construct comprising a sequence that is not a substrate for either luciferase or caspase-3/7 attached to a luciferin molecule to the second subject; (m) imaging the photon emission of the second subject with a photodetector device; and (n) comparing the photon emission of the first subject and the second subject.
[0029] A modulator of an apopotosis-related disease, wherein the modulator is pro-apoptotic, will have increased the photon emission of the first subject. A modulator of an apopotosis-related disease, wherein the modulator is anti-apoptotic, will have decreased the photon emission of the first subject. It is understood that it is within the scope of the method for the first image and the second image to be taken in the reverse chronological order. In another embodiment, the construct of step ( 1 ) is selected from the group consisting of DEVN, DDDD, FA, VEID, LEHD, and YVAD and the luciferin molecule is an amino luciferin having the structure
[0000]
[0030] In another embodiment, the present invention comprises a method of identifying modulators of an apoptosis-related disease comprising
(a) administering to a subject luciferase-expressing cells; (b) allowing the cells to achieve localization in the subject; (c) administering a modulator of an apoptosis-related disease and a construct comprising a caspase-3/7 substrate attached to a luciferin molecule to the subject; (d) creating a first image of the photon emission of the subject with a photodetector device; (e) administering a modulator of an apoptosis-related disease and a construct comprising a sequence that is not a substrate for either luciferase or caspase-3/7 attached to a luciferin molecule to the subject; (f) creating a second image of the photon emission of the subject with a photodetector device; and (g) comparing the photon emission of the first image and the second image.
A modulator of an apopotosis-related disease, wherein the modulator is pro-apoptotic, will have increased the photon emission of the first image. A modulator of an apopotosis-related disease, wherein the modulator is anti-apoptotic, will have decreased the photon emission of the second image. In another embodiment, the construct of step (e) is selected from the group consisting of DEVN, DDDD, FA, VEID, LEHD, and YVAD and the luciferin molecule is an amino luciferin having the structure
[0000]
[0038] In another embodiment, the present invention comprises a method of identifying modulators of an apoptosis-related disease comprising
(a) administering to a subject luciferase-expressing cells; (b) allowing the cells to achieve localization in the subject; (c) administering a modulator of an apoptosis-related disease and a construct comprising a sequence that is not a substrate for either luciferase or caspase-3/7 attached to a luciferin molecule to the subject; (d) creating a first image of the photon emission of the subject with a photodetector device; (e) administering a modulator of an apoptosis-related disease and a construct (f) comprising a caspase-3/7 substrate attached to a luciferin molecule to the subject; (g) creating a second image of the photon emission of the subject with a photodetector device; and (h) comparing the photon emission of the first image and the second image.
[0047] A modulator of an apopotosis-related disease, wherein the modulator is pro-apoptotic, will have increased the photon emission of the second image. A modulator of an apopotosis-related disease, wherein the modulator is anti-apoptotic, will have decreased the photon emission of the first image.
[0000] In another embodiment of the methods of identifying modulators of an apoptosis-related disease, the construct comprising a sequence that is not a substrate for either luciferase or caspase-3/7 attached to a luciferin molecule comprises a sequence selected from the group consisting of DEVN, DDDD, FA, VEID, LEHD, and YVAD. In another embodiment of the methods of identifying modulators of an apoptosis-related disease, the construct comprising a sequence that is not a substrate for either luciferase or caspase-3/7 attached to a luciferin molecule comprises DEVN. In another embodiment of the methods of identifying modulators of an apoptosis-related disease, the construct comprising a sequence that is not a substrate for either luciferase or caspase-3/7 attached to a luciferin molecule, wherein the luciferin molecule is an amino luciferin having the structure
[0000]
[0000] In another embodiment of the methods of identifying modulators of an apoptosis-related disease, the construct comprising a sequence that is not a substrate for either luciferase or caspase-3/7 attached to a luciferin molecule comprises a sequence selected from the group consisting of DEVN, DDDD, FA, VEID, LEHD, and YVAD and the luciferin molecule is an amino luciferin having the structure
[0000]
[0000] In another embodiment of the methods of identifying modulators of an apoptosis-related disease, the construct comprising a sequence that is not a substrate for either luciferase or caspase-3/7 attached to a luciferin molecule is DEVN and the luciferin molecule is an amino luciferin having the structure
[0000]
[0048] In another embodiment, the apoptosis-related disease is a proliferative disease selected from the group consisting of a tumor disease (including benign or cancerous) and/or any metastases, wherever the tumor or the metastasis are located, including breast cancer including, for example, advanced breast cancer, stage 1V breast cancer, locally advanced breast cancer, and metastatic breast cancer, lung cancer, including, for example, non-small cell lung cancer (NSCLC, such as advanced NSCLC), small cell lung cancer (SCLC, such as advanced SCLC), and advanced solid tumor malignancy in the lung; ovarian cancer, head and neck cancer, gastric malignancies, melanoma (including metastatic melanoma), colorectal cancer, pancreatic cancer, and solid tumors (such as advanced solid tumors); hyperplasias, fibrosis (especially pulmonary, but also other types of fibrosis, such as renal fibrosis), angiogenesis, psoriasis, atherosclerosis and smooth muscle proliferation in the blood vessels, such as stenosis or restenosis following angioplasty. In another embodiment, the apoptosis-related disease is selected from the group consisting of ocular diseases such as cataracts or glaucoma, osteoporosis, bone fractures, epidermal lesions, restenosis, conditions linked to an incorrect proliferation or migration of the smooth muscle cells, inflammations of the respiratory system, asbestosis, silicosis, lupus erythematosus, Goodpasture's syndrome, granulomatosis, eosinophilic granulomatosis, gastric and duodenal ulcers, oesophagitis, enteritis, gastritis, septicaemia, dysfunctions of the haematopoiesis and/or lymphopoiesis, cystic fibrosis, myelopathies and arthropathies, hepatites (C, A, B, F), AIDS, immune deficiencies, cell aging, tissue degeneration phenomena, inflammation, infectious diseases, graft rejection, acute or chronic rheumatoid arthritis, ulcerative colitis, thrombocytopenic purpura, autoimmune erythronoclastic anaemia, juvenile (Type I) diabetes (insulin-dependent), myelodysplasic syndrome, Huntington's disease, prion diseases, ARDS, prostatic hypertrophy, asthma, atherosclerosis and its thrombo-embolic complications, renal diseases, glomerulonephritis, ischemic pathologies such as myocardial infarction, myocardial ischemia, coronary vasospasm, angina and cardiac failure, chronic pancreatitis, auto-immune gastritis, and primary biliary cirrhosis.
[0049] In another embodiment, the present invention comprises a modulator of an apoptosis-related disease identified by the methods of identifying modulators of an apoptosis-related disease. In another embodiment, the modulator is an anti-apoptotic drug. In another embodiment, the modulator is an anti-tumor drug. In another embodiment, the method is used to identify an appropriate efficacious dose of the modulator of an apoptosis-related disease.
[0050] In one embodiment, the localization of the luciferase-expressing cells takes from about 1 minute to about 1 hour. In another embodiment, the localization of the luciferase-expressing cells takes from about 5 minutes to about 30 minutes.
[0051] In one embodiment, the present invention comprises a method of evaluating the efficacy of modulators of an apoptosis-related disease comprising
(a) administering to a first subject luciferase-expressing cells; (b) allowing the cells to achieve localization in the first subject; (c) administering a modulator of an apoptosis-related disease and a construct comprising a caspase-3/7 substrate attached to a luciferin molecule to the first subject; (d) imaging the photon emission of the first subject with a photodetector device; (e) administering to a second subject luciferase-expressing cells; (f) allowing the cells to achieve localization in the second subject; (g) administering a modulator of an apoptosis-related disease and a construct comprising a sequence that is not a substrate for either luciferase or caspase-3/7 attached to a luciferin molecule to the second subject; (h) imaging the photon emission of the second subject with a photodetector device; and (i) comparing the photon emission of the first subject and the second subject.
In another embodiment, the construct of step (g) is selected from the group consisting of DEVN, DDDD, FA, VEID, LEHD, and YVAD and the luciferin molecule is an amino luciferin having the structure
[0000]
Experimentals
[0061] Compounds of the invention can be prepared using procedures that are generally known. For example, compounds of the invention can be prepared using standard solution phase chemistry.
Synthesis of Caspase-3/7 Inactive Substrate(s):
[0062] Compounds of the invention can be prepared using conventional peptide synthesis protocols. Similar chemical syntheses could be performed for the other inactive substrates.
[0000]
In Vivo Bioluminescent Imaging of VivoGlo™ Caspase-3/7 Substrate and Caspase-3/7 Inactive Substrate(s):
[0063] To test for the sensitivity and specificity of the caspase-3/7 inactive substrates in vivo, mice bearing tumors stably expressing luciferase will be treated with known apoptosis-inducing cytotoxic therapies (e.g. docetaxel). At timepoints post treatment, mice will be injected intraperitoneally with 62.5 mg/mL of VivoGlo™ Caspase-3/7 substrate or caspase-3/7 inactive substrate(s). A buffer comprising about 30% PEG 400, about 5% DMSO, about 5% Tween 80 and about 60% Dextrose 5% in Water (D5W) is used for the VivoGlo™ Caspase-3/7 substrate and caspase-3/7 inactive substrate(s). In luciferase-expressing cells undergoing apoptosis, caspase-3/7 will cleave the DEVD peptide from the VivoGlo™ Caspase-3/7 substrate, allowing it to be a substrate for luciferase photon production. In luciferase-expressing cells undergoing apoptosis, caspase-3/7 will be unable to cleave the peptide from the caspase-3/7 inactive substrate(s), preventing the substrate from being used for luciferase photon production. The photon emission will be detected with a photodetector device at timepoints from 5-30 minutes post injection and quantified. The VivoGlo Caspase-3/7 injected mice should yield significant bioluminescent signal, whereas the caspase-3/7 inactive substrate-injected mice should produce little to no bioluminescent signal, indicating specificity of the substrate. | The invention provides a construct comprising an amino acid sequence attached to a luciferin substrate, wherein the amino acid sequence is not a substrate for either luciferase or caspase-3/7 to render the substrate inactive in the presence of luciferase. The construct is useful, for example, as a negative control for in vitro apoptosis assays and the bioluminescent imaging of drug-induced apoptosis in vivo. The invention also provides methods for screening for novel modulators of an apoptosis-related disease. | 2 |
CLAIM OF PRIORITY UNDER 35 U.S.C. §119
[0001] The present Application for Patent claims priority to Provisional Application No. 60/731,024, entitled “System And Method For Improving Robust Header Compression (ROHC) Efficiency By Correct Interpretation Of Change In The Increment Of The RTP Timestamp,” filed Oct. 27, 2005, and assigned to the assignee hereof and hereby expressly incorporated by reference herein.
BACKGROUND
[0002] 1. Field
[0003] The invention relates to data compression and decompression in a communication system and, in particular, to a system and method for improving Robust Header Compression (ROHC) efficiency.
[0004] 2. Background
[0005] ROHC is an Internet Engineering Task Force (IETF) header compression framework that provides for high efficiency and robustness in wireless communication systems. Among other features, ROHC supports Real-time Transfer Protocol/User Datagram Protocol/Internet Protocol (RTP/UDP/IP) and UDP/IP compression profiles.
[0006] The ROHC working group is also specifying support for a Transmission Control Protocol/Internet Protocol (TCP/IP) compression profile.
[0007] ROHC exhibits robustness, i.e., the ability to tolerate errors on the wireless links. ROHC is useable with multi-media applications and provides for header compression for various applications, protocols, and wireless technologies. Header compression is a technique to reduce the packet size transmitted over a link thereby increasing the link efficiency and throughput. Header compression is particularly useful on slow links or when packet sizes are small where a reduction in the header size results in a significant decrease in the header overhead. Header compression achieves this by leveraging header field redundancies in packets belonging to the same flow. In particular, many packet header fields such as source and destination addresses remain constant throughout the duration of a flow while other fields such as sequence numbers change predictably to allow header compression to transmit only a few bytes of header information per packet. FIG. 1 illustrates a typical ROHC compression/decompression block diagram 100 of IP/UDP/RTP headers over a communication link. Typically, reference copies of the full headers are stored at a ROHC compressor 102 and a ROHC decompressor 104 in order to reliably communicate and reconstruct original packet headers. There is a need in the art, however, for a system and method for improving ROHC efficiency by correctly interpreting change in increment of the RTP Timestamp field either due to silence suppression for a voice flow or due to a change in sampling/frame rate of a video flow.
SUMMARY
[0008] The invention relates to the change in the increment of the RTP Timestamp field as occurring either due to silence suppression for a voice flow or due to change in sampling/frame rate of a video flow. By interpreting this change correctly, the value of the TS_STRIDE in ROHC may be correctly calculated leading to efficient header compression performance.
[0009] In one aspect, there is disclosed a method of improving ROHC between an Access Network (AN) having a compressor and an Access Terminal (AT) having a decompressor, comprising providing flow information to the compressor relating to a change in the increment of a Real-Time Transfer Protocol Timestamp (RTP TS) field of a header; determining the change in the increment of a RTP TS field as occurring either due to silence suppression or due to a change in sampling/frame rate based on the flow information; and sending an appropriate TS_STRIDE value from the access network to the access terminal to achieve efficient ROHC. If the ROHC compressor determines that the RTP TS field increment is changed due to silence suppression, then there is no change to the TS_STRIDE value; if the ROHC compressor determines that RTP TS field increment is changed due to a change in the sampling/frame rate, then the TS_STRIDE value is changed in accordance with the sampling/frame rate. With this aspect, silence suppression may occur only in voice flow, and the change in sampling/frame rate may occur only in video flow.
[0010] In another aspect, there is disclosed a system providing ROHC between an access network having a compressor and an access terminal having a decompressor, comprising means for providing flow information to the compressor relating to a change in the increment of an RTP TS field of a header; means for determining the change in RTP TS field increment as occurring either due to silence suppression or due to a change in sampling/frame rate based on the flow information; and means for sending an appropriate TS_STRIDE value from the access network to the access terminal to achieve efficient ROHC. The means for providing the flow information to the compressor may further comprise means for setting the TS_STRIDE value in response to a change in the increment of the RTP TS field. With this aspect, if the determining means determines that the RTP TS field increment is changed due to silence suppression, then there is no change to the TS_STRIDE value; and if the determining means determines that the RTP TS field increment is changed due to a change in the sampling/frame rate, then the TS_STRIDE value is changed in accordance with the sampling/frame rate.
[0011] It is appreciated that in the above aspects, the compressor may be at the access terminal and the decompressor may be at the access network and the system and method for improving ROHC efficiency by correctly interpreting change in the increment of the RTP TS would still work.
BRIEF DESCRIPTION OF THE DRAWINGS
[0012] FIG. 1 illustrates a block diagram of a typical ROHC compressor/decompressor in a communication system;
[0013] FIG. 2 illustrates an RTP header;
[0014] FIG. 3 is a flowchart illustrating the operations of the improved ROHC of the invention; and
[0015] FIG. 4 illustrates an apparatus to perform the method of FIG. 3 .
DETAILED DESCRIPTION
[0016] As explained above, ROHC is a header compression scheme that compresses RTP/UDP/IP headers efficiently. Referring to FIG. 2 , there is shown an RTP header 200 . One of the techniques ROHC uses to compress headers is to compress an RTP Sequence Number (RTP SN) field 202 and then use linear relations from the RTP SN field 202 to other changing fields such as an RTP Timestamp (RTP TS) field 204 . The RTP SN field 202 increases by one (1) for every transmitted packet, while the RTP TS field 204 increments according to a sampling rate. According to RFC 3550, available at URL www.faqs.org/rfcs/rfc3550.html, which is fully incorporated herein by reference, “[i]f an audio application reads blocks covering 160 sampling periods from the input device, the timestamp would be increased by 160 for each such block, regardless of whether the block is transmitted in a packet or dropped as silent.”
[0017] In order to compress headers, the ROHC compressor needs to estimate the increment in the RTP TS field 204 from packet to packet. The value of a parameter called TS_STRIDE is set equal to this increment in the RTP TS field 204 . Once this regular change is known, the ROHC compressor can compress a scaled value of the RTP TS field 204 , scaled by the regular jump from packet to packet. This allows it to achieve savings in the size of compressed headers. Moreover, in order to compress this scaled of the RTP TS field 204 , the ROHC compressor needs to communicate the value of TS_STRIDE to the ROHC decompressor.
[0000] Behavior of Voice Source with Silence Suppression
[0018] For voice carried over RTP/UDP/IP, the RTP TS field 204 in the RTP header 200 typically increases by a fixed amount from packet to packet. As an example, for a voice codec producing 20 msec packets sampled at 8 kHz, the RTP TS field 204 increases by the number of samples contained in 20 msec, e.g., 8000*0.02=160.
[0019] In order to conserve bandwidth when sending Voice over IP (VoIP), the sender can make use of a technique called Silence Suppression. This technique causes the frames generated when the user is silent (or equivalently, when the vocoder is generating ⅛ th rate frames, as in the case of a vocoder like EVRC) to not be transmitted. This translates into bandwidth savings and increased capacity for communication systems. However, as explained earlier, the RTP TS field 204 increments even during periods of Silence Suppression.
[0020] Thus, the first frame generated after the end of the Silence Suppression period will show a jump in the increment of the RTP TS field 204 . As an example, for a voice codec producing 20 msec packets sampled at 8 KHz, if say 5 “silent” packets have been suppressed, the RTP TS field 204 will increase by 160*(5+1)=960. In this case, even though there is now a change in the increment of the RTP TS field from 160 to 960, subsequent frames will still have increments of 160 and thus the ROHC compressor should continue using the TS_STRIDE value of 160.
[0000] Behavior of Video Source with Adaptive Sampling/Frame Rate
[0021] Certain video sources can adapt their sampling/frame rates dynamically during a flow, causing the increment of the RTP TS field 204 to change. As an example, the TS_STRIDE increment may be 50 for the first 10 packets of a video flow, but may change to 100 for the next 10 packets (due to a change in the video's sampling/frame rate). In this case, the ROHC compressor should change its value of the TS_STRIDE when the video's sampling/frame rate changes.
[0000] Calculation of the TS_STRIDE
[0022] The problem arises due to the requirement that the ROHC compressor needs to interpret the change in the increment of the RTP TS field 204 differently for voice and video flows. In particular, in the case of voice flows, it should not change the value of the TS_STRIDE when there is a change in the increment of the RTP TS field 204 due to silence suppression. For adaptive video flows, on the other hand, the ROHC compressor should change the value of the TS_STRIDE when there is a change in the increment of the RTP TS field 204 due to a change in the video's sampling/frame rate.
[0023] The invention identifies that in order to improve the current ROHC, the ROHC compressor should distinguish between the two different causes of change to the increment of the RTP TS field 204 . More specifically, the invention recognizes the following:
(1) For voice flows, only silence suppression may take place; typically there is no sampling rate change; and (2) For video flows, change in the increment of the RTP TS field may be caused only by a sampling/frame rate change; silence suppression never takes place (silence suppression is only for voice media).
[0026] From the above two observations, silence suppression and sampling or sampling/frame rate change are mutually exclusive; that is, neither silence suppression nor sampling/frame rate change happens in the same flow. Thus, the ROHC compressor can interpret the change in the increment of the RTP TS field 204 correctly if flow information is fed to it.
[0027] Such information about the type of flow may be known to the access network.
[0028] As an example, in 3GPP/3GPP2 systems, the RAN/PDSN typically has access to information about the type of flow and can feed this to the ROHC compressor located in the access network. The AT, on the other hand, may or may not have information about the type of flow. In case the AT does not have such information, one option may be for the AN to pass it such information.
[0029] Referring to FIG. 3 , there is shown a flowchart 300 illustrating the operations of the improved ROHC of the invention. In block 302 , the AN provides to the AT with flow information relating to a change in the increment of the RTP TS field 204 . In block 304 , the TS_STRIDE value is set equal to the increment in the RTP TS field 204 . In block 306 , the ROHC compressor determines the change in RTP TS field increment 204 as occurring either due to silence suppression or due to a change in sampling/frame rate. If the ROHC compressor determines that the RTP TS field increment 204 changes due to silence suppression, then there is no change in the value of TS_STRIDE in block 308 . On the other hand, if the ROHC compressor determines that the RTP TS field increment 204 changes due to a sampling or sampling/frame rate change, then there is a change in the value of TS_STRIDE in block 310 . In block 312 , the AN performs the appropriate behavior for TS_STRIDE, i.e., it sends the TS_STRIDE value to the AT if TS_STRIDE is changed due to a sampling or frame rate change and does not send TS_STRIDE if the change in increment of the RTP TS field is due to silence suppression. As stated above, silence suppression occurs only in voice flow, and the change in the sampling/frame rate occurs only in video flow. The invention also contemplates that the compressor may reside at the AT and the decompressor may reside at the AN. In this case, the AN needs to pass flow information to the AT since the compressor is at the AT.
[0030] It is appreciated that if the ROHC compressor does not interpret the change in the increment of the RTP TS field 204 differently based on the type of flow, its performance may suffer. For example,
(1) If the ROHC compressor always assumes that change in the increment of the RTP TS field 204 is due to sampling or a sampling/frame rate change, this may cause inefficiencies if the flow is voice. This may cause the ROHC compressor to send a new TS_STRIDE in a larger compressed header (typically an IR, IR-DYN or UOR-2 Ext3 packet) to the decompressor, when the first packet after silence suppression is received. Also, when a few packets subsequent to this first packet have been received, the ROHC compressor will need to revert back to the earlier TS_STRIDE and again communicate this change to the decompressor using a larger header. This will lead to inefficiencies in ROHC performance, particularly when talkspurts are small. (2) If the ROHC performance always assumes that change in the increment of the RTP TS field 204 is due to silence suppression, this may cause inefficiencies for adaptive video flows. For such flows, even when the sampling/frame rate changes, the ROHC compressor will never attempt to change its value of TS_STRIDE. This may again impact the header compression efficiency of ROHC since the correct TS_STRIDE is not being used for compression.
[0033] Accordingly, the invention discloses an improved system and method for the ROHC compressor to interpret changes in the increment of the RTP TS field correctly when either silence suppression takes place in voice flows or the sampling/frame rate changes in adaptive video flows. This leads to better compression efficiency for ROHC.
[0034] FIG. 4 illustrates an apparatus comprising means 402 - 412 to perform the method of FIG. 3 . The means 402 - 412 in FIG. 4 may be implemented in hardware, software or a combination of hardware and software.
[0035] One of skill would further appreciate that the various illustrative logical blocks, modules, and steps described in connection with the embodiments disclosed herein may be implemented as electronic hardware, computer software, or combinations of both. To clearly illustrate this interchangeability of hardware and software, various illustrative components, blocks, modules, and steps have been described above generally in terms of their functionality. Whether such functionality is implemented as hardware or software depends upon the particular application and design constraints imposed on the overall system. Skilled artisans may implement the described functionality in varying ways for each particular application, but such implementation decisions should not be interpreted as causing a departure from the scope of the present invention.
[0036] The various illustrative logical blocks, modules, and circuits described in connection with the embodiments disclosed herein may be implemented or performed with a general purpose processor, a Digital Signal Processor (DSP), an Application Specific Integrated Circuit (ASIC), a Field Programmable Gate Array (FPGA) or other programmable logic device, discrete gate or transistor logic, discrete hardware components, or any combination thereof designed to perform the functions described herein. A general purpose processor may be a microprocessor, but in the alternative, the processor may be any conventional processor, controller, microcontroller, or state machine. A processor may also be implemented as a combination of computing devices, e.g., a combination of a DSP and a microprocessor, a plurality of microprocessors, one or more microprocessors in conjunction with a DSP core, or any other such configuration.
[0037] The steps of a method or algorithm described in connection with the embodiments disclosed herein may be embodied directly in hardware, in a software module executed by a processor, or in a combination of the two. A software module may reside in Random Access Memory (RAM), flash memory, Read Only Memory (ROM), Electrically Programmable ROM (EPROM), Electrically Erasable Programmable ROM (EEPROM), registers, hard disk, a removable disk, a CD-ROM, or any other form of storage medium known in the art. An exemplary storage medium is coupled to the processor such the processor can read information from, and write information to, the storage medium. In the alternative, the storage medium may be integral to the processor. The processor and the storage medium may reside in an ASIC.
[0038] The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein. | The invention relates to interpreting the change in the increment of the RTP TS field as occurring either due to silence suppression for a voice flow or a change in sampling/frame rate of a video flow. By interpreting this change correctly, the value of the TS_STRIDE field in robust header compression may be correctly calculated leading to efficient header compression performance. In one aspect, there is disclosed a method of improving ROHC between an Access Network (AN) having a compressor and an Access Terminal (AT) having a decompressor, comprising providing flow information to the compressor relating to a change in the increment of an RTP TS field of a header; determining the change in the increment of an RTP TS field as occurring either due to silence suppression or due to a change in a sampling/frame rate; and taking appropriate action for TS_STRIDE. | 7 |
CROSS REFERENCE TO RELATED APPLICATION
This is a divisional of application Ser. No. 11/783,482, filed Apr. 10, 2007, which is incorporated herein by reference in its entirety.
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to a wafer stage of a photolithographic exposure apparatus. More particularly, the present invention relates to a magnetic levitation wafer stage which levitates a wafer to be exposed.
2. Description of the Related Art
Typically, a wafer used for fabricating a semiconductor device is repeatedly and selectively subjected to individual processes such as cleaning, diffusion, photo-resist coating, exposure, development, etching, and ion-implantation processes. These processes are performed by respective apparatuses. There are several types of exposure apparatus for performing the exposure process. Among these apparatus is a stepper. A stepper is used to direct light from a light source through a reticle, and to scan a layer of photo-resist on the surface of the wafer with the light directed through the reticle. The reticle bears a pattern corresponding to that of a circuit pattern or the like. The layer of photo-resist is thus exposed to an image of the pattern of the reticle. The exposed layer of photo-resist is then developed to remove the exposed (or non-exposed) regions of the layer and thereby pattern the layer of photoresist. The underlying layer is then etched using the patterned layer of photo-resist as a mask. Accordingly, a pattern corresponding to that of the reticle is formed on the wafer.
Generally, the wafers are exposed one-by-one in the stepper. To this end, a predetermined number of wafers coated with photo-resist are loaded in a carrier and the carrier is transferred to a loading/unloading station inside the stepper. Then, a robot arm having a blade is extended to insert the blade into the carrier beneath a wafer. Next, the table is moved down so that the wafer is supported by the blade, and the robot arm is retracted to remove the wafer from the carrier. Once the wafer is removed from the carrier, the wafer is transferred from the blade to a horizontally movable member of a transfer device. The horizontally movable member loads the wafer onto a wafer stage of the stepper. The wafer stage of the stepper aligns each die (region) of the wafer with the reticle whereupon the exposure of the die commences, and the wafer stage moves the wafer so that the dies are exposed sequentially.
The wafer stage has a ceramic chuck (table) and a driving device for moving the chuck. The ceramic chuck holds the wafer, and the driving device moves the ceramic chuck in X and Y (orthogonal) directions. A transfer arm unloads the wafer from the ceramic chuck once the exposure of the wafer has been completed.
During the above-described operation, particles are generated from the back of the wafer or elsewhere in a vacuum chamber in which the wafer stage is disposed. The particles accumulate on the ceramic chuck. Such particles may cause defocus, i.e., an inability of the exposure apparatus to properly focus the image of the pattern of the reticle on the wafer. Therefore, after a certain number of wafers have been exposed, an engineer stops the operation of the exposure apparatus whereupon the pressure in the vacuum chamber of the exposure apparatus is returned to atmospheric pressure. The engineer then takes the wafer stage out of the apparatus, and cleans the ceramic chuck to remove any particles on the chuck.
U.S. Pat. No. 5,196,745 discloses a positioning device (a stage) that can prevent defocus errors from occurring. The positioning device disclosed in U.S. Pat. No. 5,196,745 has a table (wafer chuck) that is magnetically suspended so as to be out of contact with a stationary member in which the table is received. Permanent magnets are arrayed in two dimensions on both top surface and bottom surface of the table. The permanent magnets are arranged, in each direction of the array, such that the adjacent poles of the magnets are of opposite polarity. Also, a multiphase coil array corresponding to the permanent magnets is mounted to the stationary member, in which the table is received, for suspending the table and driving the table in horizontal directions.
However, the table of the non-contact type of positioning device disclosed in U.S. Pat. No. 5,196,745 is relatively large and heavy because the table has a plurality of permanent magnets on the top and bottom surfaces thereof. Moreover, the multiphase coil array can only produce a considerably weak magnetic field in a vertical direction. Therefore, it is difficult to devise a working embodiment in which the multiphase coil array suspends such a heavy table satisfactorily.
SUMMARY OF THE INVENTION
Therefore, an object of the present invention is to provide a magnetic levitation stage having a relatively lightweight table.
Another object of the present invention is to provide a magnetic levitation stage which can obviate defocusing errors caused by particles in an exposure apparatus of photolithographic equipment.
Likewise, an object of the present invention is to provide a method for use in aligning a substrate in an exposure apparatus of photolithographic equipment, which method will not be subject to defocus errors when particles are produced in the equipment.
Still another object of the present invention is to provide a magnetic levitation stage that can be operated using relatively small amounts of power (mechanical or electrical).
Similarly, an object of the present invention is to provide a method for use in aligning a substrate in an exposure apparatus of photolithographic equipment, which method can be carried out using relatively small amounts of power (mechanical or electrical).
In accordance with one aspect of the present invention, there is provided a magnetic levitation stage comprising a base, a table supported on the base and whose entire top surface exhibits magnetism of a single polarity, and motors for moving the table in the X and Y directions relative to the base. In addition, Y-directional members each extending longitudinally in the Y direction are symmetrically disposed at opposite sides of an upper part of the base, and an X-directional member extending longitudinally in the X direction spans the Y-directional members. The X-directional member is supported so as to be movable in the Y direction. The table is engaged with the X-directional member so as to move therewith in the Y direction, and the table is supported so as to be movable in the X direction. The motors include a first motor connected to the X-directional member and operative to reciprocate the X-directional member in the Y direction, and a second motor connected to the table and operative to reciprocate the table in the X direction
A substrate, e.g., a wafer, is levitated by the stage. To this end, the bottom surface of the substrate has a coating of a magnetic substance exhibiting the same polarity as that at the upper surface of the table of the stage. Preferably, films comprising the magnetic substance are adhered to the bottom surface of the substrate and an upper surface of the body of the table, respectively.
In accordance with another aspect of the present invention, there is provided a magnetic levitation stage comprising a table including a main body and a number of electromagnets disposed in an upper portion of the main body, and electronics operatively connected to the electromagnets. Preferably, the electromagnets are arrayed in rows and columns in the upper surface of the main body of the table. The electronics are configured to supply current in either direction through coils of the electromagnets respectively and independently of one another.
Preferably, the electronics include a main control unit, a position controlling unit, and an electromagnetic driving circuit. The main control unit is configured to generate a command signal calculated to position a magnetic substrate at a desired location on the table. The position controlling unit is operatively connected to the main control unit to receive the command signal from the main control unit. The position control unit is also configured to determine on the basis of the command signal a polarity of each of the electromagnets, and to output signals corresponding to the polarity of each of the electromagnets. The electromagnetic driving circuit is operatively connected to the position controlling unit to receive the signals output by the position controlling unit. The electromagnetic driving circuit is also configured to supply electric current to the electromagnets in directions through the coils on the basis of the signals output by the position controlling unit. In the case in which the electromagnets are arrayed in rows and columns in the upper surface of the main body of the table, the command signal represents X and Y coordinates, in a Cartesian coordinate system, of the desired location of the substrate.
In accordance with another aspect of the present invention, there is provided a method for use in aligning a substrate in an exposure apparatus of photolithographic equipment, wherein a substrate having a magnetic substance at the bottom surface thereof is provided, the substrate is levitated above a table whose upper surface exhibits magnetism of the same polarity as that at the bottom of the substrate, and the substrate is moved horizontally while the substrate remains levitated above the table. Either the table can be moved while the substrate remains levitated above the table to thereby drag the wafer along with the table or the substrate itself can be moved relative to the table by changing the polarity of the magnetism exhibited at respective regions of the table.
BRIEF DESCRIPTION OF THE DRAWINGS
The above and other objects, features and advantages of the present invention will become more apparent to those of ordinary skill in the art by referring to the following detailed description of the preferred embodiments thereof made with reference to the attached drawings in which:
FIG. 1 is a perspective view of a wafer stage according to the present invention;
FIG. 2 is a side view of a wafer levitated above a table of the wafer stage of FIG. 1 ;
FIG. 3 a is a plan view of the table;
FIG. 3 b is a bottom view of the wafer;
FIG. 4 is a perspective view of a table of another embodiment of a wafer stage according to the present invention;
FIG. 5 is a block diagram of a driving device for driving the table of FIG. 4 ; and
FIG. 6 is an explanatory diagram illustrating an operation of moving a wafer magnetically levitated above the table of a wafer stage according to the present invention.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
The present invention will now be described more fully hereinafter with reference to the accompanying drawings. However, the function and constitution of those parts of the present invention and/or devices associated therewith which are well-known in art per se will not be described in detail for the sake of brevity and so that the description of the fundamental aspects of the present invention is not obscured.
Referring now to FIG. 1 , a wafer stage 100 installed inside a vacuum chamber of an exposure apparatus, according to the present invention, includes a base 110 , Y-directional members 120 symmetrically disposed at ends of an upper part of the base 110 , an X-directional member 130 spanning the Y-directional movable members 120 , a first driving motor 122 engaged with one of the Y-directional movable members 120 and to which the X-directional member 130 is attached, a second driving motor 132 engaged with the X-directional member 130 , and a table 140 for supporting a wafer 150 in a magnetically levitated state. The table 140 is disposed on the X-directional movable member 130 so as to move therewith in a Y direction and so as to be movable therealong in an X direction as will be described in more detail below. The wafer 150 may be set atop the table 140 by a transfer robot (not shown).
Referring also to FIGS. 2 , 3 a and 3 b , the top surface of the table 140 is constituted by a first coating 142 including a magnetic substance of positive polarity. Also, a second coating 152 including a magnetic substance of positive polarity is formed on the bottom surface of the wafer 150 . The first and second coatings 142 and 152 may be formed at the top surface of the table 140 and the bottom surface of the wafer 150 , respectively. Alternatively, the first and second coatings 142 and 152 may be respective films, each including a magnetic substance, and adhered to the upper surface of a body of the table 140 and the bottom surface of the wafer 150 .
The wafer 150 is levitated above the table 140 by a force of repulsion between the first coating 142 of the table 140 and the second coating 152 of the wafer 150 . The force of repulsion is created because the first coating 142 of the table 140 and the second coating 152 of the wafer 150 both have positive polarities.
Also, the first driving motor 122 can drive itself along the Y-directional movable member 120 with which it is engaged so as to move in a Y direction parallel to the Y-directional members 120 . Thus, the first driving motor 122 drives the X-directional member 130 and the table 140 in the Y direction. On the other hand, the second driving motor 132 can drive itself along the X-directional member 130 so as to move in an X direction parallel to the X-directional member 130 . Thus, the second driving motor 132 drives the table 140 in the X direction. In this way, the wafer 150 is levitated above the table 140 , and the table 140 is selectively moved in X and Y directions to facilitate an exposure process. In this respect, there is enough drag between the table 140 and the wafer 150 to move the wafer 150 along with the table as the table 140 is moved by the motors.
FIG. 4 illustrates a table 10 of another embodiment of a wafer stage according to the present invention, and a wafer 12 whose bottom surface includes a magnetic substance having a positive polarity. The wafer 12 can be transferred onto the table 10 by a transfer robot (not shown) at which time the table 10 magnetically levitates the wafer 12 . To this end, several electromagnets a 1 -a 10 , b 1 -b 10 . . . j 1 -j 10 are embedded in the upper surface of the wafer table 10 . The electromagnets are arrayed in rows ( 1 - 10 ) and columns (a-j), i.e., in two dimensions. The polarity of each of the electromagnets a 1 -a 10 , b 1 -b 10 . . . j 1 -j 10 depends on the direction of current flowing through the coil of the electromagnet.
Referring to FIG. 5 electronics for driving the electromagnets of the wafer table 10 includes a main control unit 20 , a position controlling unit 22 operatively connected to the main control unit 20 , and an electromagnetic driving circuit 24 operatively connected to the position controlling unit 22 and to the electromagnets a 1 -a 10 , b 1 -b 10 . . . j 1 -j 10 . The main control unit 20 generates a control command to position the wafer 12 at a desired location represented by X and Y coordinates of a Cartesian coordinate system. The position controlling unit 22 receives the control command from the main control unit 20 and, on the basis of the control command, determines a polarity (positive or negative) of each of the electromagnets a 1 -a 10 , b 1 -b 10 . . . j 1 -j 10 that will effect the movement of the wafer 12 to the desired location on the table 10 , and outputs corresponding polarity determinative signals to the electromagnetic driving circuit 24 . The electromagnetic driving circuit 24 receives the polarity determinative signals output by the position controlling unit 22 and, on the basis of such signals, supplies electric current to the electromagnets a 1 -a 10 , b 1 -b 10 . . . j 1 -j 10 in such directions that the electromagnets a 1 -a 10 , b 1 -b 10 . . . j 1 -j 10 keep the wafer 12 magnetically levitated and simultaneously move the wafer 12 to the desired location on the table 10 .
FIG. 6 illustrates how the electromagnets a 1 -a 10 , b 1 -b 10 . . . j 1 -j 10 move the wafer 12 while keeping the wafer 12 magnetically levitated above the table 10 .
Assuming that the magnetic coating of the wafer 12 exhibits a positive polarity at the bottom of the wafer 12 , the electromagnetic driving circuit 24 initially supplies electric current to all of the electromagnets a 1 -a 10 , b 1 -b 10 . . . j 1 -j 10 in such directions that the magnetism produced by each of the electromagnets a 1 -a 10 , b 1 -b 10 . . . j 1 -j 10 has a positive polarity above the surface of the table 10 . Accordingly, the wafer 12 is levitated by the force of repulsion between the positive magnetic force produced by the electromagnets a 1 -a 10 , b 1 -b 10 . . . j 1 -j 10 and the positive magnetic force produced by the magnetic coating of the wafer 12 .
To move the wafer 12 levitated above the table 10 to the right, as shown in FIG. 6 , electric current is supplied by the electromagnetic driving circuit 24 to the electromagnets a 10 , b 10 . . . j 10 , namely to the electromagnets arrayed along the right side of the table 10 , for a predetermined time and in such directions through the cores of the electromagnets a 10 , b 10 . . . j 10 that the polarity of the magnetism produced by these electromagnets a 10 , b 10 . . . j 10 above the surface of the table 10 is negative. Accordingly, the wafer 12 is attracted in the direction of the negative magnetic field lines produced by the electromagnets a 10 , b 10 . . . j 10 above the surface of the table 10 such that the wafer 12 is moved towards the right side of the table 10 while it is levitated.
Likewise, to move the wafer 12 towards the end of the table, as shown at the top of FIG. 6 , the electromagnetic driving circuit 24 supplies electric current for a predetermined time to the electromagnets a 1 , a 2 . . . a 10 , namely the electromagnets arrayed on the end of the wafer table 10 , such that these electromagnets a 1 , a 2 . . . a 10 produce magnetism having a negative polarity above the surface of the table 10 . As a result, the wafer 12 is attracted in the direction of the negative magnetic field lines produced by the electromagnets a 1 , a 2 . . . a 10 above the surface of the table 10 such that the wafer 12 is moved towards the end of the table 10 while it is levitated. Similar operations can be used to move the wafer 12 towards the other side of the table 10 (the left side in FIG. 6 ) or towards the other end of the table 10 (the end shown at the bottom of FIG. 6 ). Also, these operations can be used in combination to basically set the wafer 12 at any relative location on the table 10 .
The electromagnets a 1 -a 10 , b 1 -b 10 . . . j 1 -j 10 can be superconducting electromagnets. That is, the coils of the electromagnets a 1 -a 10 , b 1 -b 10 . . . j 1 -j 10 can be of a superconducting metal. For example, the coils of the electromagnets a 1 -a 10 , b 1 -b 10 . . . j 1 -j 10 are formed of a niobium-titanium alloy. Superconductivity is a condition in which certain metal materials exhibit zero electrical resistance at extremely low temperatures close to absolute zero (−237 degrees Celsius). Therefore, for a given voltage, the electric current flowing through the superconducting electromagnets and hence, the strength of the magnetic fields produced by the superconducting electromagnets, is relatively high.
As described above, the wafer stage according to the present invention magnetically levitates a wafer above the wafer table by a magnetic force of repulsion between the wafer and the wafer table. Consequently, the present invention prevents the back of the wafer from being mechanically abraded. Thus, the present invention can prevent defocusing errors when the wafer stage is employed in an exposure apparatus of photolithographic equipment. Also, in the case in which the table has the magnetic substance forming the upper surface thereof, the table can be lightweight. Thus, the table can be moved using a relatively small amount of mechanical power. Accordingly, the motors can be correspondingly small and the mechanical system produces very little abrasion. In the case in which the table is provided with electromagnets, the relatively lightweight wafer can be levitated easily using a relatively small amount of electrical power and the wafer is moved without any abrasion occurring.
Finally, although the present invention has been described in connection with the preferred embodiments thereof, it is to be understood that the scope of the present invention is not so limited. On the contrary, various modifications of and changes to the preferred embodiments will be apparent to those of ordinary skill in the art. For example, although the present invention has been described above in connection with the forming of magnetism having positive polarities at the bottom of the wafer and at the upper surface of the table of the wafer stage, the present invention is not so limited. Rather, the present invention can be carried out by employing magnetism having negative polarities at the bottom of the wafer and at the upper surface of the table of the wafer stage. Thus, changes to and modifications of the preferred embodiments may fall within the true spirit and scope of the invention as defined by the appended claims. | A magnetic levitation wafer stage is used to align a wafer in an exposure apparatus of photolithographic equipment. The wafer stage includes a base, a table supported on the base and whose entire top surface exhibits magnetism of a single polarity, and motors for moving the table in the X and Y directions relative to the base. Alternatively, the wafer stage includes a wafer table having a main body and a number of electromagnets disposed in an upper portion of the main body, and electronics that selectively supply current in either direction through coils of the electromagnets respectively and independently of one another. In the exposure process, the bottom surface of the substrate is provided with a magnetic substance such that the substrate exhibits magnetism of a given polarity. The substrate is delivered to and set on the table of the stage. There, the substrate is levitated by a magnetic force of repulsion between the substrate and the table. The substrate can be moved horizontally while the substrate remains levitated above the table of the stage. | 5 |
FIELD OF THE INVENTION
This invention relates to logic analyzers, and more particularly to a data acquisition circuitry architecture and method of operation that permits the dynamic allocation of the memory space used to hold acquired data in a logic analyzer.
BACKGROUND OF THE INVENTION
Logic analyzers have traditionally had two basic modes of data acquisition: synchronous and asynchronous. Synchronous data acquisition, or state analysis as it is also known, refers to the process of acquiring data at times determined by the active edge of the user's system clock signal. Asynchronous data acquisition, or timing analysis, refers to the process of acquiring data at times determined by the active edge of a clock that is generated by the logic analyzer. Asynchronous data acquisition is typically performed at sampling rates that are faster than the user's system clock in order to provide a closer look at the timing of particular signals.
A third kind of data, known as "glitch" data has also been acquired by logic analyzers. A "glitch" is usually defined as more than one transition across the logic threshold within one data acquisition interval, i.e., within the interval between successive active edges of the acquisition clock. For example, three transitions and a change in logic state, or two transitions and the same logic state, are both defined as glitches. More thorough discussions of glitches and means for detecting them are contained in U.S. Pat. Nos. 4,353,032, 4,843,255, and 4,857,760 for a "Glitch Detector", a "Self-Latching Monostable Circuit", and a "Bipolar Glitch Detector Circuit", respectively, all hereby incorporated by reference.
When glitches are being acquired, keeping track of glitch data requires as much memory as the corresponding data acquisition does. This is because every active clock edge on which data is sampled has associated with it the interval between that edge and the next edge during which a glitch can occur. Therefore, when glitches are being acquired, half of the available memory must be dedicated to storing glitch data. This means that either half of the memory depth or half of the memory width is utilized for this function.
To conserve the amount of memory required for data storage, "transitional" data storage is now frequently employed, especially in conjunction with asynchronous data acquisition. In this approach, rather than storing the logic state of a signal upon the occurrence of every acquisition clock signal, no data is stored for acquisition clock cycles in which no data has changed. When the data does change, the new data is stored along with a timestamp that provides a record of the time when the new data was acquired. Thus, memory is only used in direct proportion to the number of logic state transitions and, even though extra memory is required to store the timestamps, a considerable amount of memory is conserved in most circumstances.
It is frequently desirable to acquire both synchronous and asynchronous data in relationship to the same event. For example, if a hardware problem is suspected in certain circuitry, but it only seems to occur during specific kinds of operations, it might be desirable to use synchronous acquisition to monitor microprocessor operations until the specific kind of operation is occurring, and then trigger asynchronous data acquisition in the vicinity of the certain circuitry to learn more about the suspected problem.
In the past, this sort of cross-triggering of asynchronous acquisition by events detected through synchronous acquisition was accomplished by two logic analyzers, or two distinct portions of a single logic analyzer. However, this requires double probing of the circuitry under analysis. Also, when using two separate logic analyzers, the user must perform a calculation to determine the timing relationship between the synchronous data and the asynchronous data. When using a logic analyzer with integrated synchronous and asynchronous sections, the delay from probe tip to trigger machine and between trigger machines for each section may not be accurately aligned to place the timing data in the desired relationship with a synchronous event of interest.
Even in advanced logic analyzers, such as those in the Philips PM 3580 Family, which eliminate dual probing and provide a single trigger machine for both state and timing analysis, memory is pre-allocated to state, timing, or equally to both in advance. This is an inefficient use of memory when the user's interest in the data does not conform to these pre-allocations.
SUMMARY OF THE INVENTION
Accordingly, the present invention is an apparatus and method for dynamic memory allocation that conserves memory resources while providing efficient and effective interaction between concurrent synchronous and asynchronous acquisition of data for logic analysis.
The apparatus includes means for acquiring synchronous data, means for acquiring asynchronous data, means for generating timestamp values, means for determining when the synchronous data is valid, means for determining when the asynchronous data is valid, and means for packing valid synchronous data and valid asynchronous data into a memory according to the sequence in which it was acquired with sufficient timestamp values included to permit reconstruction of the relative timing between all of the acquired data, with each data and timestamp value being identified with status bits to indicate whether it was synchronous data, asynchronous data, or a timestamp value.
The method of dynamic memory allocation includes the steps of acquiring synchronous data, acquiring asynchronous data, generating timestamp values, determining when the synchronous data is valid, also determining when the asynchronous data is valid, and packing valid synchronous data and valid asynchronous data into a memory according to the sequence in which it was acquired with sufficient timestamp values included to permit reconstruction of the relative timing between all of the acquired data, with each data and timestamp value being identified with status bits to indicate whether it was synchronous data, asynchronous data, or a timestamp value.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a block diagram of a portion of the data acquisition circuitry that implements the method of the present invention.
FIG. 2 is a block diagram of the remainder of the data acquisition circuitry that implements the method of the present invention.
FIG. 3 is a block diagram of the synchronous data log-in circuitry used in the data acquisition circuitry according to the present invention.
FIG. 4 is a schematic diagram of the synchronizer used in the data acquisition circuitry according to the present invention.
FIG. 5 is a schematic diagram of the synchronous sampler used in the data acquisition circuitry according to the present invention.
FIG. 6 is a schematic diagram of the asynchronous sampler used in the data acquisition circuitry according to the present invention.
FIG. 7 is a block diagram of the test, trigger, and storage control circuitry used in the data acquisition circuitry according to the present invention.
FIG. 8 is a block diagram of the memory preparation circuitry used in the data acquisition circuitry according to the present invention.
FIG. 9 is a timing diagram illustrating the operation of the memory preparation circuitry shown in FIG. 8.
FIG. 10 is a memory allocation diagram showing how the data prepared as shown in FIG. 9 is actually stored in RAM.
FIG. 11 is table of time/data relationships reconstructed from the data shown in FIG. 10.
DETAILED DESCRIPTION OF THE INVENTION
Referring to FIG. 1, synchronous data log-in circuitry 20 monitors the user's clock signal, USERCLKS, the USER's QUALIFIERS, and the USER's DATA signals to be monitored. The synchronous data log-in circuitry 20 produces 1/2UCLK and QUDATA. 1/2UCLK is a consolidated version of the user's clocks that runs at half speed. QUDATA is a version of the USER DATA that is synchronized to a full speed version of UCLK and that has been qualified by selected combinations of the USER's QUALIFIERS. Hence, QUDATA is "qualified user data".
The USER's DATA is also applied to A-sampler 60, which asynchronously samples the USER's DATA at times determined by SYSCLK, the data acquisition circuitry's system clock signal. A-sampler 60 produces asynchronous data, A-DATA, as its output. Note that, while this data derived from asynchronous acquisition will be referred to below as "asynchronous" and identified as "A-DATA", it is manipulated synchronously to SYSCLK throughout the rest of the circuitry to be described; i.e., the label "asynchronous" only refers to its origin.
1/2UCLK is monitored by synchronizer 30, which also receives the acquisition system clock, SYSCLK. The synchronizer 30 produces UCDET and SELECT. UCDET (user's clock detected) is a signal that goes active during the system clock signal cycle that immediately follows a valid user's clock active edge. SELECT is a signal that is sent to S-sampler (synchronous sampler) 50 to indicate which half cycle of the system clock the user's clock active edge occurred in. The function of both of these signals will be further described below.
The S-sampler 50 receives QUDATA from the synchronous log-in circuitry 20, SELECT from the synchronizer 30, and SYSCLK, the data acquisition circuitry system clock. The S-sampler produces synchronous data, S-DATA, as its output.
Referring now to FIG. 2, the UCDET, S-DATA, and A-DATA outputs of the circuitry shown in FIG. 1, as well as a RUN signal and PF (post-fill) and HOLDOFF values, are inputs to the remaining portion of the data acquisition circuitry shown in this Figure. (The SYSCLK signal is a "not shown" input to all of the circuitry shown in FIG. 2 except the AND gate 82 and OR gate 93.) The RUN signal is produced by a system controller (200, FIG. 7), and tells the data acquisition circuitry when to commence a new data acquisition. AND gate 82 produces GO signal that enables the test, trigger, and storage control circuitry 70 when RUN is true and HOLDOFF and MEMFULL (memory full) are both false. The PF (post-fill) and HOLDOFF values tell the memory preparation circuitry 100 how long to keep filling memory after a TRIGGER and how long to hold GO off while prefilling the memory, respectively.
The test, trigger, and storage control circuitry 70 receives S-DATA, A-DATA, UCDET, and the ENable signal output of AND gate 82, and produces STORE-A, STORE-S, and TRIGGER signals. The STORE-S and TRIGGER signals are applied directly to memory preparation circuitry 100, while the STORE-A signal is stretched by 19 system clock pulses before being applied to the memory preparation circuitry 100. STORE-A is stretched to be a minimum of 20 system clock pulses in width by the operation of OR gate 93 which monitors STORE-A and the output of the 19 flip-flops 91-92.
The memory preparation circuitry receives delayed signals S-DATA', A-DATA', and UCDET'. UCDET' is a version of UCDET that has been delayed by pipe 89 to compensate for the delay through the test, trigger, and storage control circuitry 70. S-DATA' is a version of S-DATA that has been delayed by passage through S-pipe 84, while A-DATA' is a version of A-DATA that has been delayed by passage through both A-pipe1 85 and A-pipe2 86. S-pipe and A-pipe1 compensate for the delay of test, trigger, and storage control circuitry 70, while A-pipe2 and the pulse stretching circuitry of flip-flops 91-92 and OR gate 93 operate to provide a storage window of asynchronous data centered around a specified event in the synchronous data. The memory preparation circuitry 100 also receives a HOLDOFF VALUE directly from the controller 200.
Change detector 88 detects changes in A-DATA' and produces an active DELTA signal whenever such changes occur. Also, whenever the stretched STORE-A output of OR gate 93 changes state, indicating the beginning or end of an asynchronous acquisition, the change detector 88 responds by asserting DELTA to force the storage of an asynchronous sample. This is to ensure that asynchronous data is stored in memory, even if no data transition occurs.
Time stamp counter 83 starts counting in response to the rising edge of the RUN signal and produces thereafter a TIMESTAMP value that is the final input to the memory preparation circuitry 100. Flip-flop 94 stores a copy of each TIMESTAMP value for one SYSCLK cycle, so that it is able to retain the LASTTIME value at the end of an acquisition, as will be further described below.
The memory preparation circuitry 100 produces/WRITE (not write) and ADDRESS controls for RAM (random access memory) 120. The memory preparation circuitry 100 also supplies data in the form of DATA/TIME and STATUS to be written into RAM 120. In addition, the memory preparation circuitry 100 supplies HOLDOFF and MEMFULL signals to AND gate 82 and to external circuitry, including the controller 200.
Referring now to FIG. 3, the synchronous data log-in circuitry 20 of FIG. 1 can be seen here in relative detail. Multiple USER CLOCKS, typically four, are applied to the input of selectable edge detector 22. The EDGE SELECTION control signals from the system controller (not shown) determine which edges of which USER CLOCKS the selectable edge detector 22 will respond to. According to these instructions, the selectable edge detector produces UCLK, a consolidated version of the user's system clocks, by ORing together pulses produced in response to the selected rising or falling edges of the selected USER CLOCKS.
The UCLK signal clocks USER DATA into flip-flop 23 which holds it until the log-in state machine 24 has had a chance to produce a QUALIFY result, as is further described below. Delay element 25 produces a delayed version of UCLK, UCLK', which is used to clock the output of flip-flop 23, USER DATA', into flip-flop 26 after the log-in state machine 24 has had a chance to produce a valid QUALIFY signal if it is going to.
The UCLK' signal is divided by two at flip-flop 28, whose/Q output is connected to be its D input, to produce 1/2UCLK. The UCLK' signal also clocks USER DATA into flip-flop 26 (which actually represents a number of such flip-flops, as does flip-flop 23). Flip-flops 26 and 28 are both enabled by a QUALIFY signal from the log-in state machine 24. The log-in state machine 24 is programmed to produce the QUALIFY signal based on its present state and the state of its USER QUALIFIERS inputs.
Referring now to FIG. 4, the synchronizer 30 shown in FIG. 1 is shown in greater (schematic) detail in this Figure. 1/2UCLK is applied to the D inputs of flip-flops 31 and 38. Flip-flops 31-34 and 42 are clocked by SYSCLK, while flip-flops 38-41 are clocked by an inverted version of SYSCLK. Each of these strings of flip-flops serve to reduce the likelihood of metastability propagating throughout their length. As is further described in U.S. Pat. No. 4,949,361 to Jackson for a "Digital Data Transfer Synchronization Circuit and Method", hereby incorporated by reference, XOR gate 35 monitors the outputs of the last two flip-flops 33 and 34 in the upper string to detect transitios of the 1/2 UCLK signal. Active outputs of XOR gate 35 are clocked into flip-flop 36 by the next active (hith-goint) edge of SYSCLK. The output of flip-flop 36 is the clock detected signal, UCDET.
Since flip-flops 38-41 are clocked 180° out of phase relative to flip-flops 31-34, they resolve the timing of transitions in 1/2UCLK by an extra factor of two, so that it is less than or equal to the period of the system clock, SYSCLK. This information from flip-flop 41 is delayed one half clock period less and brought into phase with the information in flip-flop 34 as a result of flip-flop 42's being clocked by SYSCLK rather than/SYSCLK (not-SYSCLK). XOR gate 37 detects when the contents of flip-flops 34 and 42 are unequal to produce the SELECT signal. Thus, the SELECT signal indicates when 1/2UCLK edges were in the second half of SYSCLK, from 180°-360° , while/SELECT indicates when the 1/2UCLK edges were in the second half of SYSCLK, from 0°-180°.
Referring now to FIG. 5, the S-sampler (synchronous sampler) shown in FIG. 1 is shown in greater (schematic) detail in this Figure. QUDATA (qualified user data) is clocked into flip-flop 51 by SYSCLK and into flip-flop 54 by/SYSCLK. The output of flip-flop 51 then passes through flip-flop 52 and into flip-flop 53 on the next two active (rising) edges of SYSCLK. The output of flip-flop 54 passes through flip-flop 55 and then into flip-flop 56, where it is brought into time alignment with the data in flip-flop 53. Multiplexer 57 receives the output of flip-flop 53 on its "0" input and the output of flip-flop 56 on its "1" input. The SELECT signal from the synchronizer 30 controls which input to multiplexer 57 is produced as its output, thus ensuring that the resulting synchronous data is accurately associated with the correct user clock edge and closest acquisition system clock. Flip-flop 58 receives the selected output from multiplexer 57 on its input and clocks it in on the next SYSCLK to produce S-DATA as its output. The data that is selected for S-DATA is that which was sampled one half of a SYSCLK period later than the SYSCLK edge that sampled 1/2UCLK.
Referring next to FIG. 6, the A-sampler (asynchronous sampler) 60 shown in FIG. 1 is shown in greater (schematic) detail in this Figure. USER DATA is clocked into flip-flop 61 on the active (rising) edges of/SYSCLK (which occur at the same time as the falling edges of SYSCLK). This data is then clock through flip-flops 62-65 and into flip-flop 68 on the occurrence of an active edge of SYSCLK. The length of the A-sampler path, i.e., the number of flip-flops represented by 65, is chosen to align together S-DATA and A-DATA samples that were taken one half cycle apart, as is further described below.
FIG. 7 shows in relative detail the test, trigger, and storage control block 70 shown in FIG. 2. An S/A (synchronous, not-asynchronous) signal from the controller 200 selects between the S-DATA and A-DATA inputs to multiplexer 80 for application to the inputs of four data recognizers, DR 0 71 through DR 3 74. WORDS, RANGES signals from the controller 200 program the data recognizers 71-74 with word and range recognition values that the selected DATA signals from multiplexer 80 are compared with. The determination as to whether or not the specified conditions are satisfied is determined at the active edge of SYSCLK.
The logic analyzer prior art contains a number of disclosures dealing with word recognition, range recognition, event recognition, etc. Specifically, U.S. Pat. Nos. 4,475,237 to Glasby for "Programmable Range Recognizer", 4,752,928 to Chapman et al. for "Transaction Analyzer", 4,789,789 and 4,801,813 to Kersenbrock et al. for "Event Distribution and Combination System(s)", 4,823,076 to Haines for "Method and Apparatus for Triggering", and 4,849,924 to Providenza et al. for "Event Counting Prescaler", all hereby incorporated by reference, describe a variety of such recognizers, many of which would be suitable for use as data recognizers DR 0 71 through DR 3 74.
The polarity, edge, and combination logic 75 examines the outputs of the data recognizers DR 0 -DR 3 71-74 and determines whether any of four programmable tests, TEST 1 -TEST 3 , are satisfied. Each test can be programmed by CONTROL signals from the controller 80 to include events from the data recognizers or their absence (event not), transitions into or out of events, and sequences or combinations of events.
Most of the polarity, edge and combination logic 75 only operates during times when it is enabled by ENAB', a version of the output of OR gate 81, ENAB, that has been delayed for one cycle of SYSCLK by flip-flop 77. An exception is the timers within the trigger state machine 76 which run once they are started even while ENAB" is inactive. During synchronous triggering operations OR gate 81 is satisfied whenever UCDET (user's clock detected) is active high. During asynchronous triggering operations OR gate 81 is always satisfied by the high output of inverter 79, A/S (asynchronous, not-synchronous).
Upon receiving an active GO signal, the programmable (RAM-based) trigger state machine 76 monitors the test outputs TEST 0 -TEST 3 , and determines the state of its STORE-A, STORE-S, TRIGGER outputs according to BEHAVIOR and COUNT/TIMES signals from the controller 200. To limit its operation to valid cycles, the trigger state machine 76 is enabled by ENAB", a version of ENAB' that has been further delayed one SYSCLK cycle by flip-flop 78.
Referring next to FIG. 8, the memory preparation circuitry 100 shown in FIG. 2 is shown in relative detail in this Figure. Data integrator 104 is clocked by SYSCLK and receives as inputs S-DATA', A-DATA', and TIMESTAMP information, as well as VALID s and VALID A , signals from AND gates 101 and 102, respectively. VALID s is true when both STORE-S and UCDET' are true, while VALID A is true when both STORE-A and DELTA are true.
The dam integrator 104 supplies two multi-bit signals, S-STREAM and A-STREAM, and two single-bit signals, S-VALID and A-VALID, to data packing circuitry 106. The S-VALID signal is a delayed version of the VALID s signal and is active (high) when S-STREAM contains valid synchronous data. The A-VALID signal is a delayed version of the VALID A signal and is active (high) when A-STREAM contains valid asynchronous data.
The data packing circuitry 106 supplies two multi-bit signals, PACK 0 and PACK 1 , four STATUS bits, two of which are associated with each PACK signal, and a single bit signal, PACKFULL, that indicates when the PACK signals contain new data. The pairs of STATUS bits have the following significance: 00=TIMESTAMP, 01=SYNC, and 10=ASYNCH (with 11=unused).
The postfill counter 110 is enabled by the output of AND gate 111, which has TRIGGER' and PACKFULL as its inputs. TRIGGER' is a version of the TRIGGER signal that has been delayed by pipeline 109. The postfill counter 110 counts down from the value PFVALUE (postfill value) upon those occurrences of SYSCLK that occur while PACKFULL is high after TRIGGER' has gone high. When zero is reached, MEMFULL (memory full) is generated.
The format and address generation circuitry 108 is enabled by RUN and clocked by SYSCLK to demultiplex PACK 0 and PACK 1 and their associated STATUS signals into DATA, TIME, and associated STATUS signals at twice the width and half the frequency. It also generates ADDRESS and /WRITE signals to control the RAM 120, and a HOLDOFF signal whose duration is determined by the HOLDOFF VALUE input that it receives from the controller 200 (FIG. 2). The HOLDOFF signal is used to prevent a trigger from occurring before the RAM has had a chance to prefill when the operator wishes to view activity that occurs before the trigger.
Referring now to FIG. 9, as well as FIG. 8, the data integrator 104 produces its outputs S-STREAM, S-VALID, A-STREAM, and A-VALID from its inputs as shown in this Figure. Note that the TIMESTAMP data at the top of FIG. 9 increments by two on each clock, so that the TIMESTAMP values associated with data acquired on rising edges of SYSCLK are all even while the TIMESTAMP values associated with data acquired on falling SYSCLK edges are all odd. (To avoid confusion with numbers associated with circuit blocks, TIMESTAMP values and synchronous and asynchronous data values are shown in italics, such as 100, S1, and A1 throughout the following discussion.)
Note in FIG. 9 that VALID A is not active (high) until the rising edge of the SYSCLK associated with the TIMESTAMP value 110. This could be because the A-DATA' is not changing and therefor the change detector 88 has not caused DELTA to go active, or it could be because STORE-A has not yet been activated by the test, trigger, and storage control circuitry 70. In either event, the A-DATA' is not of interest prior to this interval.
During the SYSCLK cycle while the TIMESTAMP value is 100, VALID s goes active, indicating that S-DATA' is valid at that time. Therefore, the first valid synchronous data in this example is S1. Additional valid synchronous data values S2and S3 are identified by VALID s at the times corresponding to the TIMESTAMP values of 104 and 106. During the interval while the TIMESTAMP value is 102, neither VALID s nor VALID A is active and the data on S-DATA' and A-DATA' are both invalid.
During the interval corresponding to the TIMESTAMP value 102, and in response to the presence of valid S-DATA' during the interval corresponding to the TIMESTAMP value 100, the data integrator 104 produces an active S-VALID signal and places the S1 data on its S-STREAM output. At the same time A-VALID also goes active and TIMESTAMP value 100 is placed on the A-STREAM output. During the next clock cycle, while the current TIMESTAMP value is 104, the S-STREAM and A-STREAM outputs of the data integrator contain TIMESTAMP values 101 and 102, respectively. However, the S-VALID and A-VALID signals remain inactive (low) and these TIMESTAMP values are discarded.
During the interval corresponding to the TIMESTAMP values 104 and 106, VALID s is again active and S2 and S3 appear sequentially on the S-DATA' lines. During the interval corresponding to the TIMESTAMP value 106, the data integrator 104 places S2 on its S-STREAM output, TIMESTAMP value 104 on its A-STREAM output, and makes S-VALID and A-VALID active to notify the data packing circuitry 106 aware that valid data is present on its inputs.
During the interval corresponding to the TIMESTAMP value 108, the data integrator 104 places S3 on its S-STREAM output, TIMESTAMP value 106 on its A-STREAM output, and again makes S-VALID and A-VALID active again to notify the data packing circuitry 106 of the valid data on both of its data inputs.
By the time of the interval corresponding to the TIMESTAMP value 104, the data packing circuitry 106 has received synchronous data value S1 and TIMESTAMP value 100, and placed them on its PACK 0 and PACK 1 outputs, respectively. PACKFULL is asserted during this same interval to notify the format and address generation circuitry 108 of the valid data on its inputs. The STATUS signals at the output of the data packing circuitry 106 are delayed versions of the STATUS signals at its input.
The format and address generation circuitry 108 latches in the PACK 0 and PACK 1 values S1 and 100 at the end of the interval corresponding to the TIMESTAMP value 104 will not make any of its outputs available until they all are ready at the beginning of the interval corresponding to the TIMESTAMP value 110, at which time S1 and 100 will appear on its DATA 0 and DATA 1 outputs, respectively.
During the interval corresponding to the TIMESTAMP value 108, the data packing circuitry 106 causes PACKFULL to go active (high) again and produces S2 at its PACK 0 output and 104 at its PACK 1 output. At the end of the interval corresponding to the TIMESTAMP value 108, the format and address generation circuitry 108 accepts the PACK 0 and PACK 1 data on its inputs, and presents those same values, S2 and 104, on its DATA 2 and DATA 3 outputs, respectively, during the interval corresponding to the next TIMESTAMP value 110.
The DATA 0 -DATA 3 outputs of the format and address generation circuitry 108 all contain valid data, S1, 100, S2, and 104, during the interval corresponding to the TIMESTAMP value 110. In this example, the current ADDRESS being supplied to the RAM 120 is 0, so when /WRITE (not write) goes active-low the DATA 0 through DATA 3 values are written into the RAM 120 at this address.
Returning now to the top of FIG. 9, at the time interval corresponding to TIMESTAMP value 106, S-DATA' goes to the value S3 and VALID s remains active (high). Accordingly, during the next SYSCLK cycle, the time interval corresponding to TIMESTAMP value 108, the outputs of the data integrator, S-STREAM and A-STREAM, carry the values S3 and 106, respectively, and both S-VALID and A-VALID remain active (high).
During the interval corresponding to the next TIMESTAMP value, 110, the PACKFULL output of the data packing circuitry 106 remains active (high) and the PACK 0 and PACK 1 outputs are presenting the values S3 and 106 to the format and address generation circuitry 108, which is presently outputting S1, 100, S2, and 104. The format and address generation circuitry 108 latches in these values and holds them until it has another full set of outputs ready.
Returning again to the top of FIG. 9, at the time interval corresponding to TIMESTAMP value 108, S-DATA' remains at the value S3 and VALID s goes to inactive (low). Since VALID s is low, indicating that the S3 value is no longer valid data, the data integrator 104 places the next TIMESTAMP values, 107 and 108 on S-STREAM and A-STREAM next. ("Next" in this context means the next after the last, 106.) This data is not meaningful, since neither S-VALID nor A-VALID is active while it is present, and it will be discarded.
During the interval corresponding to the TIMESTAMP value 110, VALID s is low but VALID A goes high for the first time. The low (inactive) level of VALID s reflects that fact that S3 is old, invalid data. The active (high) level of VALID A indicates that the asynchronous data A-DATA', with the value A1, is now valid. During the next SYSCLK cycle, the interval corresponding to TIMESTAMP interval 112, the data integrator 104 produces the A1 data on A-STREAM and an active high level on A-VALID to indicate the validity of the value on A-STREAM. Since there wasn't any valid synchronous data, the TIMESTAMP value 109, which does not correctly correspond to the acquisition time of the A1 data, is placed on S-STREAM, but is identified as invalid by the inactive (low) state of S-VALID. The correct TIMESTAMP value for A1 is 111, as will be seen below when the interpretation of the final memory contents is explained. The data packing circuitry 106 stores the valid A1 value and ignores the invalid 109 value.
During the interval corresponding to the TIMESTAMP value 112 VALID A goes low, indicating that A-DATA' is no longer valid, and VALID s goes high, indicating that the value S4 on S-DATA' is valid synchronous data. In response to these inputs, during the next SYSCLK cycle (corresponding to TIMESTAMP value 114) the data integrator 104 places S4 on the S-STREAM and TIMESTAMP value 112 on the A-STREAM and marks them both as valid by causing S-VALID and A-VALID to go (or stay) high.
The data packing circuitry 106 responds to the new valid data values S4 and 112 during interval 114 by latching them in and, during the 116 interval, putting the A1 value which it received earlier and the S4 value which it just received on its PACK 0 and PACK 1 outputs, respectively, and exerts PACKFULL to inform the format and address generation circuitry 108 that the PACK x signals are valid. The 112 value that was present on A-STREAM is held until it can be paired with the next valid data received.
At time 118, when the format and address generation circuitry 108 receives the A1 and S4 values, it immediately places them on its DATA 2 and DATA 3 outputs, respectively. At the same time, also puts the S3 and 106 values that it received back at time 110 on its DATA 0 and DATA 1 outputs, respectively. The ADDRESS output of the format and address generation circuitry 108 had already been changed from 0 to 1 at time 114 after the active /WRITE pulse (low-going) during times 110 and 112, so everything is now ready for the active /WRITE pulse that occurs in times 118 and 120.
Returning to the top of FIG. 9, at time 114 VALID s goes low, indicating that the S4 value on S-DATA' is no longer valid. At the same time, VALID A goes high to indicate that a new, valid value, A2, is present on A-DATA'. At time 116 the data integrator 104 responds to these inputs by putting A2 in the A-STREAM and another invalid time value, 113, on the S-STREAM. The high on A-VALID and low on S-VALID reflect the respective validity and invalidity of the values A2 and 113. At time 118 the data packing circuitry 106 puts the 112 TIMESTAMP value on PACK 0 and the A2 asynchronous data value on PACK 1 and keeps PACKFULL asserted to cause the format and address generation circuitry 108 to accept this data as the next valid data to be written to the RAM 120.
Starting again at the top of FIG. 9, this time at time 116, VALID s goes high to indicate that there is a new valid synchronous data value, S5, present on the S-DATA' lines. At the same time VALID A remains high indicating that A-DATA' also has a new valid data value, A3. At time 118 the data integrator places S5 and A3 on S-STREAM and A-STREAM, respectively, and asserts both S-VALID and A-VALID. At time 120 the data packing circuitry 106 puts these same values, S5 and A3, on the PACK 0 and PACK 1 lines, and asserts PACKFULL, thus making these values available to the format and address generation circuitry 108.
Having previously received two valid pieces of data, 112 and A2, when the format and address generation circuitry receives these two pieces, S5 and S3, it puts all four of them on DATA 0 -DATA 3 , respectively, and changes the ADDRESS from 1 to 2. Half a SYSCLK cycle later /WRITE is asserted (low) and this data is written to the RAM 120.
FIG. 10 shows the data sent to memory in FIG. 9 as it resides in the RAM 120 after acquisition is complete. Memory banks BANK 0 -BANK 3 receive their data from data lines DATA 0 -DATA 3 , respectively. Each item of data in the memory is supplied with a tag derived from the pair of STATUS bits that accompanied it from the format and address generation circuitry 108. These pairs of STATUS bits have the following significance: 00=TIMESTAMP, 01=SYNC, and 10=ASYNCH.
To aid in reconstructing the timing of the acquired data, when an acquisition ends, the absence of both STORE-S and the stretched version of STORE-A (from OR gate 93) disable OR gate 95 and the enable input to flip-flop 94, thereby causing the TIMESTAMP value associated with the last data value in memory to be retained in flip-flop 94. In our example this LASTTIME value is 117. Software then performs post-acquisition processing to recreate the time/data relationship for display.
FIG. 11 is table of time/data relationships reconstructed from the data shown in FIG. 10 and the contents of the LASTTIME flip-flop 94. Referring now to FIGS. 10 and 11, the post-processing software starts at the end of memory which was filled last and associates with it the LASTTIME value 117. Thus, time 117 is associated with asynchronous data value A3. By knowing how the memory preparation circuitry 100 has processed the data for storage, the software knows that the TIMESTAMP values contained in the acquisition memory are those associated with the data stored immediately in front of them in memory. Adjacent data values of the opposite type, such as the synchronous value S5 residing next to the asynchronous value A3, have TIMESTAMP values that are one apart. Thus, S5 has a TIMESTAMP value of 116, and A2 has a TIMESTAMP value of 115. Continuing backward through memory, the next TIMESTAMP value is 112, and it is associated with synchronous data S4. Since asynchronous data value A1 is adjacent to S4, it has the TIMESTAMP value 111. S3, S2, and S1 each have their own TIMESTAMP value stored immediately after them in memory.
The memory preparation circuitry 100 that is shown in FIG. 8 and whose operation is illustrated in FIG. 9 accomplishes a data compaction and labeling function that is unique and distinctly advantageous. Notice, in FIG. 9, how the DATA 0 -DATA 3 lines fill and transfer data more slowly on the left and faster on the fight. The slower rate on the left reflects the fact that only synchronous data is being acquired before TIMESTAMP value 110, while the faster rate on the fight reflects the fact that after time 110 both synchronous and asynchronous data are being acquired at once.
Referring again to FIGS. 10 and 11, as well as FIG. 9, note that when data is changing slowly, the memory preparation circuitry 100 stores a TIMESTAMP value with each piece of data, adopting transitional storage. But that when synchronous and asynchronous data are being acquired rapidly, on every half SYSCLK cycle, the data is packed together without TIMESTAMP values to conserve space. This maximizes the effective bandwidth of the acquisition memory without the need for a separate timestamp memory. Moreover, the transition between these two modes is automatic and dynamic, so that memory allocation is optimized. Note how the system switches rapidly back and forth between these two modes from time 112 to time 115.
It should be noted that the present invention permits windows of detailed asynchronous data to be placed around events of interest in the synchronous data, much like "A delayed by B" provides an expanded view of a portion of a signal of interest in the oscilloscope world. Moreover, these windows can be precisely positioned with respect to those events.
When asynchronous acquisition is enabled, i.e., when STORE-A is high, the circuitry described above operates to capture glitches that have a duration of 10 ns or greater. Moreover, this glitch detection leads to the display of actual data, rather than just an indication that something occurred. And, because asynchronous data acquisition can be turned on and off "on-the-fly" according to preprogrammed criteria, glitch capture can be selectively enabled to conserve memory.
A more traditional glitch capture capability could be realized by replacing UCDET with a periodic signal at the frequency of SYSCLK, or SYSCLK/n for slower operation. This would yield 5 ns glitch capture for a system with SYSCLK running at 100 MHz. 2.5 ns glitch detection can be realized by using a four phase version of the same system clock signal and reducing the number of effective channels by a factor of four to provide the increased bandwidth through the rest of the acquisition hardware.
While a preferred embodiment of the present invention has been shown and described, it will be apparent to those skilled in the art that many changes and modifications may be made without departing from the invention in its broader aspects. The claims that follow are therefore intended to cover all such changes and modifications as fall within the true scope of the invention. | An apparatus and method for dynamic memory allocation conserves memory resources while providing efficient and effective interaction between concurrent synchronous and asynchronous acquisition of data for logic analysis. The apparatus includes circuitry for acquiring synchronous data, circuitry for acquiring asynchronous data, circuitry for generating timestamp values, circuitry for determining when the synchronous data is valid, circuitry for determining when the asynchronous data is valid, and circuitry for packing valid synchronous data and valid asynchronous data into a memory according to the sequence in which it was acquired with sufficient timestamp values included to permit reconstruction of the relative timing between all of the acquired data, with each data and timestamp value being identified with status bits to indicate whether it was synchronous data, asynchronous data, or a timestamp value. The method of dynamic memory allocation includes the steps of acquiring synchronous data, acquiring asynchronous data, generating timestamp values, determining when the synchronous data is valid, also determining when the asynchronous data is valid, and packing valid synchronous data and valid asynchronous data into a memory according to the sequence in which it was acquired with sufficient timestamp values included to permit reconstruction of the relative timing between all of the acquired data, with each data and timestamp value being identified with status bits to indicate whether it was synchronous data, asynchronous data, or a timestamp value. | 6 |
BACKGROUND
The following description relates to information management systems.
An information management system may include an information retrieval system and/or a database management system. An information management system can include a computer system and one or more databases, each of which is a collection of tables representing classes of physical or conceptual objects. Each object is represented by a record. The information contained in a record may be organized by multiple attributes. For example, if a database were used to keep track of employees in a corporation, each record might represent an employee and each record might include attributes such as a first name, last name, home address, and telephone number.
Relational database management systems are commonly employed to manage relational databases. A relational database is a database that includes one or more tables, where each table is organized by columns and rows. In such a database, each column is an attribute and each row is a record.
There are different ways to view the data in a database. One type of view is known as a multidimensional view. In a multidimensional view, each fact table has several dimensions such that each attribute of a table represents a dimension. Relational databases can be used to generate a multidimensional view of data. One use case for accessing data and performing operations on a database, when using a multidimensional view, is known as online analytical processing (OLAP). In accordance with OLAP, there are many database operations that manipulate data in response to a query, and many of these operations may need to aggregate data in order to generate a result. In relational databases, aggregating data is the process of summarizing a table by selecting columns and representing (e.g. by summing, averaging, or finding the maximum or minimum) the key figures for similar attribute values in each of the selected columns to generate a view with a “coarser granularity.” Aggregation may require a table scan. A table scan is the process of reading through a table record by record. Because aggregation may require access to many values in a database, aggregation can be a time and resource consumptive process. Also, because database operations may require a lot of memory, operations tend to have several accesses to a storage device of a computer system while performing the operation, rather than storing a table in a memory of the computer system.
In relational OLAP (ROLAP), the speed of aggregation queries may be increased by having frequently used aggregates precalculated and stored in the database. In multidimensional OLAP (MOLAP), the speed of aggregation queries may be increased by having all the aggregates precalculated and stored in special data structures. Precalculating aggregates tends to reduce response times for any queries that involve the precalculated aggregates; however, the ROLAP solution is advantageous only for those aggregates that are precalculated, and the MOLAP solution is computationally expensive.
SUMMARY
The present disclosure includes systems and techniques relating to an information management system and methods of performing aggregation by table scans. The systems described here, and corresponding techniques for use, may include various combinations of the following features.
In one general aspect, the techniques feature a method of aggregating data in an information management system. The method includes receiving a query for a response to a search on a database, loading data from the database into a memory if the data necessary to generate the response to the query is absent from the memory, filtering the data based on the query to generate a list of results, buffering at least one key figure corresponding to a result in the list of results, buffering at least one dimension value corresponding to each key figure, aggregating the dimension values to generate an aggregate key, aggregating the key figures corresponding to the same aggregate key to generate one or more aggregate key figures, and displaying the response to the search on a display device. In that case, the response to the search includes at least one aggregate key figure.
Implementations may include one or more of the following features. The method may further include generating a hash key based on the aggregate key and storing in a hash table aggregate key figures corresponding to that hash key. Loading data from the database into a memory may include compressing data according to a compression algorithm. In that case, the compression algorithm may be dictionary-based compression. Loading data from the database may include loading data into memory. Loading data from the database into a memory may include organizing the data in the memory as columns of the database. Aggregating the dimension values may include concatenating the dimension values. Filtering the data based on the query may be performed blockwise.
In another aspect, an information management system includes a database and a computer system. In that case the computer system is programmed to load data from the database into a memory, where the data represents a table; filter the data based on a query, which includes generating a list of results, buffer at least one key figure corresponding to a result in the list of results; buffer at least one dimension value corresponding to each key figure; generate an aggregate key based on the dimension values; aggregate key figures with the same aggregate key to generate one or more aggregate key figures; and, display at least one aggregate key figure on a display device.
Implementations may include one or more of the following features. The computer system may be further programmed to generate a hash key based on the aggregate key and store in a hash table aggregate key figures corresponding to the hash key. The operation of loading data from the database into a memory may include compressing data according to a compression algorithm. In that case, the compression algorithm may be dictionary-based compression. The operation of loading data from the database may include loading data into memory. The operation of filtering the data based on the query may be performed blockwise. The operation of loading data from the database into a memory may include organizing the data in the memory as columns of the database. The operation of generating an aggregate key may include concatenating the dimension values.
Implementations of the systems and techniques described here may occur in hardware, firmware, software or a combination of these, and may include instructions for causing a machine to perform the operations described.
The system and method of performing table scans in memory, and related mechanisms and/or techniques described here may provide one or more of the following advantages. Aggregates may be generated each time a query is submitted by performing a table scan. Performing a table scan each time a query is submitted is advantageous because any aggregate can then be generated as required. Performance tends to be increased because data from the database is stored in the memory of at least one computer system when the table scan is performed. The amount of memory required to perform a table scan may be reduced by storing compressed data in the memory.
Details of one or more implementations are set forth in the accompanying drawings and the description below. Other features and advantages may be apparent from the description and drawings, and from the claims.
BRIEF DESCRIPTION OF THE DRAWINGS
These and other aspects will now be described in detail with reference to the following drawings.
FIG. 1 is a flowchart of a method of aggregating data.
FIGS. 2A , 2 B are diagrams of a memory based procedure for extracting aggregate data from an external source.
Like reference numerals and designations in the drawings indicate like elements.
DETAILED DESCRIPTION
The systems and techniques described here relate to an information management system and to a method of performing aggregation by table scans in memory.
FIG. 1 is a flowchart of a method of aggregating data. At 110 , in response to a query, a determination is made of the data required to answer the query. Any data required to answer the query that is not already stored in the memory of the computer system is loaded from a database. If a large volume of data is to be processed, it may be advantageous to distribute the data over multiple computer systems. This tends to speed up the execution of the query and tends to reduce memory consumption in each computer system. Data may need to be loaded into the memories of several computer systems if more data is required to respond to the query than there is memory available on one of the computer systems. The data may be compressed before it is loaded into the memory, which may advantageously reduce the amount of memory necessary to store the data. Any number of compression algorithms may be used. For example, dictionary-based compression may be used. Dictionary-based compression uses a dictionary that maps references to a list of all the values that appear in the database. In any case, the data is logically stored in columns that correspond to the table columns in the database.
At 120 , the data in the memory is filtered based on criteria in the query. Filtering uses criteria in the query to generate a list of records that are relevant. For example, a Structured Query Language (SQL).query may include a “where” condition that is used to select the relevant rows from a table, and filtering may be performed based on the “where” condition, such that results are limited to those records that meet the condition. The filtering may be performed blockwise (i.e. in blocks of N rows).
At 130 , a block of N row identifiers (IDs) is loaded into a temporary memory location for hashing and aggregation. The value of N may be 1, but depending on the technical specification of the caching mechanism, N may advantageously be set to a value greater than 1, such as 128 or more. If the key figures for a row are still at their initial value (i.e. if they have not been maintained), the row need not be loaded into the cache, since it will have no effect on the aggregate key figures that are to be calculated. For example, a database may exist that organizes customer information by the attributes of customer key or customer identification (ID), time (in months), and the number of products purchased. Some customers in the database might not have purchased any products. In that case, the N block may include a list of row identifiers for records with only those customers who have purchased products. The N block may include row identifiers. Key figures are buffered for each record identified in the N block. The key figure columns contain the data values that are to be aggregated. In the prior example, the key figures may be the number of products purchased. Dimension values may be buffered next to each key figure so that a key figure is identifiable by nearby dimension values. The dimension values are keys for attributes or characteristics that belong together, in a record. For example, if a dimension represents customers, a dimension value may represent a particular customer and the attributes or characteristics that belong together may be customer name and address. In a record, a dimension value appears with one or more key figures. Each row identifier in the N block refers to a dimension value that is buffered. If dictionary-based compression is used, the dimension values that are buffered may be the dictionary references corresponding to the dimension values. All of the buffering should be handled in the memory of a computer system. In alternative implementations the data need not be processed blockwise, i.e. in blocks of N rows.
Aggregate keys are generated at 140 . An aggregate key is generated for each combination of dimension values in the buffer. The aggregate keys may be generated by concatenating the dimension values. If dictionary-based compression is used, the aggregate keys may be a concatenation of the dictionary references. For example, if dictionary references 0122 and 06 are used to represent dimension values CompanyA and June, respectively, the aggregate key may be 012206.
At 150 , a hash key is generated for each aggregate key and each hash key is written into a hash table. Generating a hash key involves the use of a hash function. In the case that dictionary-based compression is used, the length of the hash key may be set to n bits, where n is greater than or equal to the number of bits needed to represent the product of the cardinalities (i.e. the total number of different values for a dimension value) of the respective dimensions—i.e. 2 n ≧|D1×D2×. . . DY|, where each D is the cardinality of a dimension value. In any case, a suitable procedure must be available for handling hash key collisions.
For each hash key, key figures are aggregated at 160 during a table scan. A table scan is performed over the buffer where the key figures and respective dimension values are stored. The table scan involves the aggregation of the key figures with dimension values that correspond to the same aggregate key. If the table is divided among several computer systems, aggregate key figures may be aggregated locally and a separate server may merge the locally aggregated key figures. The aggregate key figures are entered into a hash table using the respective hash keys generated at 150 . The hash table may then be used to generate a suitable display, including the results of the aggregation, at a user interface. The processes of 120 - 160 of FIG. 1 may be performed in the memory of one or more computer systems, which advantageously tends to increase performance because operations on memory tend to be quicker than operations that involve disk accesses.
FIGS. 2A , 2 B are diagrams of a memory based procedure for extracting aggregate data from an external source, such as a database. FIG. 2A is a procedure for filling a buffer with selected rows of a table that match the criteria in a query. FIG. 2B is a procedure for aggregating key figures corresponding to the selected rows of the table. Database 205 stores one or more tables. The database may exist in one computer system, or may be spread among multiple computer systems. Memory 210 is the memory of a computer system. The memory 210 includes the data 215 , the filter results 220 , the N block 225 , the dimension values 230 , the key figures 235 , the buffer 240 , the aggregate key 245 , the hash key 250 , and the hash table 255 . The memory 210 stores compressed data loaded from the database 205 . The data 215 is loaded into the memory 210 in response to a query. If the data necessary to respond to the query already exists in the memory 210 , data need not be loaded. Although the data 215 is stored in the memory 210 of one computer system in FIG. 2A , in alternative implementations the data 215 may be loaded and stored in memories of multiple computer systems. The data 215 may be loaded into the memories of multiple computer systems, for example, if there is insufficient memory in one computer system to store the data necessary to respond to a query, or simply to speed up query processing. The data 215 is compressed data and is stored in columns. The data 215 may be compressed based on dictionary-based compression. In accordance with dictionary-based compression, the data 215 may be references that are mapped to a list of possible values. Each column represents a column of the database 205 . Although the data 215 in FIG. 2A is compressed data, in alternative implementations the data 215 need not be compressed.
Filtering the data 215 generates the filter results 220 . The filter results 220 are a list of row IDs referring to rows that are determined to be relevant based on a query. Filtering may use criteria in the query. For example, “where” conditions of a query may be used such that results are limited to those records which meet the filter condition specified.
The N block 225 is a cached part of the memory that stores row identifiers. The row identifiers correspond to the records in the filter results 220 . The N block 225 excludes records that have key figures that are null (i.e. still set at their initial value). Because the N block stores row identifiers that correspond to the filter results 220 , the N block is used as a reference when storing the dimension values 230 and the key figures 235 in the buffer 240 .
The dimension values 230 and the key figures 235 respectively correspond to row IDs in the N block 225 . For each row identifier in the N block, the corresponding key figure and dimension values are stored in the buffer 240 . In FIG. 2A , each key figure and its corresponding dimension values are copied from their temporary locations 225 and 230 , respectively, to adjacent locations in the buffer 240 .
An aggregate key, such as the aggregate key 245 , is generated for each combination of dimension values that exists in the buffer 240 . Thus, two key figures that have the same dimension values would generate the same aggregate key. The aggregate key 245 may be generated by concatenating the corresponding dimension values. If dictionary-based compression is used, references that represent dimension values may be concatenated.
Each aggregate key is used to generate a hash key, such as the hash key 250 . The hash key 250 may be any length and may be generated according to any function for generating hash keys. For example, the hash keys may be at least as long as the aggregate key 245 , or the hash key can be shorter than the aggregate key 245 . In the case that the hash key 250 is smaller than the aggregate key 245 , collisions in the hash table 255 need to be handled. In the case that dictionary-based compression is used, the length of the hash key may be set to n bits, where n is greater than or equal to the number of bits needed to represent the product of the cardinalities (i.e. the total number of different values for a dimension value) of the respective dimensions—i.e. 2n≧|D1×D2×. . . DY|, where each D is the cardinality of a dimension value.
The hash table 255 is configured to be indexed by the hash key 250 . The hash table 255 stores aggregate key figures. The aggregate key figures are generated by scanning the buffer 240 and aggregating all key figures with the same corresponding aggregate keys. The aggregate key figures are then stored in the hash table 255 . From the hash table 255 , the aggregate key figures can be accessed so they may be displayed on a display device. In exceptional scenarios where the aggregate keys are short and the result sets are small, a hashing procedure may not be necessary and the results can be aggregated using a simply array. However, in scenarios where the proposed method can scale to nontrivial use cases, hashing is likely to be required.
Although the method of aggregating data is shown in FIG. 1 as being composed of six different processes, additional and/or different processes and subprocesses can be used instead. Similarly, the processes for aggregating data need not be performed in the order depicted. Thus, although a few embodiments have been described in detail above, other modifications are possible. Other embodiments may be within the scope of the following claims. | Methods and apparatus, including computer systems and program products, relating to an information management system and aggregating data by performing table scans. In general, in one aspect, the technique includes receiving a query for a response to a search on a database, loading data from the database into memory, filtering the data based on the query to generate a list of results, buffering at least one key figure corresponding to a result, buffering at least one dimension value corresponding to each key figure, aggregating the dimension values to generate an aggregate key, aggregating key figures corresponding to the same aggregate key to generate one or more aggregate key figures, and displaying the response to the search on a display device. Loading the data may include compressing the data. Filtering the data may be performed blockwise. | 8 |
RELATED APPLICATION
This application is a continuation of U.S. application Ser. No. 08/472,189, filed Jun. 7, 1995, which is a continuation of U.S. application Ser. No. 08/285,652, filed Aug. 3, 1994, now U.S. Pat. No. 5,478,783.
BACKGROUND OF THE INVENTION
The present invention relates to infrared (IR) and ultraviolet (UV) absorbing soda-lime-silica glass compositions for use in glazing. More particularly, the present invention relates to windows of a neutral tint made from such glasses primarily, but not exclusively, for vehicles such as automobiles.
Special glasses have been developed for use in vehicles which have low levels of direct solar heat transmission (DSHT) and ultraviolet transmission (UVT). These glasses aim to reduce the problems caused by excessive heating within the vehicle on sunny days, and to protect the interior furnishings of the car from the degradation caused by ultraviolet radiation. Glasses having good infrared absorption properties are usually produced by reducing iron present in the glass to the ferrous state or by adding copper. Such materials give glasses a blue color. The materials added to achieve good ultraviolet radiation absorption are Fe 3+ , Ce, Ti or V. The quantities of such materials which are added to provide the desired level of absorption tend to color the glass yellow. Accordingly, if both good UV and good IR absorption are required in the same glass, the color of such glass is, almost inevitably, either green or blue. When the color of the glasses is defined by the CIELAB system, such commercial glasses, in 4 mm thickness and having greater than 60% light transmission, are found to be either very green (-a*>8) or very blue (-b*>7), neither of which are currently desirable from an aesthetic viewpoint.
Attempts have been made to produce grey or bronze-colored vehicle glazing having good protection against both IR and UV radiation, but such glasses still tend to have a greenish yellow tinge.
We have identified a requirement for a range of glasses having a neutral tint and a visible light transmittance (Illuminant A) of at least 70 percent such that, in the CIELAB system, the glasses have color co-ordinates lying in the ranges a* from -7 to +1, b* from -5 to +7.5. The term "neutral tint" is hereinafter used to describe glasses having such color co-ordinates.
We have further identified a requirement for glasses having a neutral tint which have visible light transmissions of at least 70 percent (at a thickness of 4 mm), but which also have a direct solar heat transmission which is at least twelve percentage points (preferably fifteen percentage points and most preferably twenty percentage points) less than the visible light transmission. Basically, glasses are known which do have a low direct solar heat transmission but nearly all of these have a low visible light transmission which tend to make such glasses of limited use in vehicles. Glasses satisfying the above-identified requirements should, we anticipated, be of more general use in vehicles due to the higher light transmission but the lower direct solar heat transmission should keep the interior of the car cool despite the higher light transmission.
Furthermore, we believed that it would be desirable if the glasses had an ultraviolet transmission less than 55% and ideally less than 50% because we felt that such a low transmission would minimize the adverse effects of ultraviolet radiation on plastics material and fabrics, particularly in automotive vehicles.
The field of tinted glasses is one in which relatively small changes can produce major changes in tint. Wide ranges disclosed in prior patents can encompass many possibilities, and it is only the teaching of the specific examples that can be relied on as identifying how particular tints associates with particular ranges of absorption of infrared and ultraviolet radiation can be obtained.
Our invention is based on the surprising discovery that the incorporation of relatively small amounts of certain coloring agents compensates for the green color arising from the presence of infrared and ultraviolet radiation absorbing components.
SUMMARY OF THE INVENTION
According to the present invention, there is provided an IR and UV absorbing soda lime silica glass of a neutral tint (as herein defined) having, in a 4 mm thickness, a visible light transmission of at least 70%, a direct solar heat transmission at least 12 percentage points below the visible light transmission, a UV transmission not greater than 55%, a dominant wavelength less than 560 nm and a color purity not greater than 6, preferably not more than 5 and most preferably no more than 3. Most, preferably the direct solar heat transmission is at least 20 percentage points lower than the visible light transmission. The composition comprises a soda-lime-silica base glass and a total iron content, expressed as Fe 2 O 3 , in the range of from 0.3 to 0.7% by weight. The glass is tinted to a neutral color by the inclusion of 0.5 to 10 parts by million (ppm) of Se, from about 3 to 25 ppm of Co 3 O 4 , and a ferrous iron content to provide a ratio of ferrous iron to total iron in the range of 21 to 34, preferably 25 to 31 (i.e., percent of total iron as ferrous iron (Fe 2+ ) of 21% to 34%, preferably 25% to 31%*). NiO and TiO 2 may be added to the glass, in ranges of 0 to 50 ppm NiO and 0 to 1.5 weight percent TiO 2 . Thus, it has been determined that amounts of NiO and TiO 2 , in the above ranges can produce beneficial affects on color purity and UV absorption, respectively, without deleteriously influencing the unique and highly advantageous properties of our novel glass.
For the purpose of the present specification and claims, references to visible light transmission are to light transmission (LT) measured using CIE Illuminant A; UVT or ultraviolet radiation transmission is an integrated term representing the area under the transmission versus wavelength curve for wavelengths between 300 and 400 nm; and references to direct solar heat transmission (DSHT) are references to solar heat transmission integrated over the wavelength range 350 to 2100 nm according to the relative solar spectral distribution Parry Moon for air mass 2.
Suitable batch materials for producing glasses according to the present invention, which materials are compounded by conventional glass batch ingredient mixing devices, include sand, limestone, dolomite, soda ash, salt cake or gypsum, niter, iron oxide, carbon, selenium and cobalt oxide (Co 3 O 4 ) . In the event TiO 2 and/or NiO are desired in the composition, a titanium compound such as titanium dioxide and a nickel compound such as nickel oxide may be included in the batch. In this connection, and in accordance with an important embodiment of this invention it has surprisingly been discovered that the use of wuestite as the source of iron is particularly advantageous, supplying at least a partial amount or preferably all of the Fe 2 O 3 and substantially eliminating the need for carbon. Thus, carbon is a very deleterious element in neutral tint glasses, e.g., grey and bronze glasses, but is required to raise the ferrous values of the glasses where employing rouge as the batch iron source. The use of wuestite as the iron source instead of rouge greatly increases the ferrous value of a glass. The use of a raw material with a higher natural ferrous value allows better control of higher ferrous values in glasses such as the neutral tint glasses of this invention.
The batch materials are conveniently melted together in a conventional glass making furnace, to form a neutral tinted infrared energy and ultraviolet radiation absorbing glass composition, which thereafter may be continuously cast onto the molten metal bath in a float glass process.
The composition of soda-lime-silica flat glasses suitable for use in accordance with the present invention typically have the following weight percentage constituents:
______________________________________ SiO.sub.2 65-80% Na.sub.2 O 10-20 CaO 5-15 MgO 0-10 Al.sub.2 O.sub.3 0-5 K.sub.2 O 0-5 BaO 0-5 B.sub.2 O.sub.3 0-5______________________________________
Other minor ingredients, including melting and refining aids such as SO 3 , may also appear in the glass composition. The coloring constituents of the present invention set forth above are added to this base glass. The glass is essentially free of colorants other than iron, cobalt, and selenium, and optionally nickel and titanium, other than any trace amounts of oxides that may be present as impurities. Accordingly, the glass of the present invention may be melted and refined in a conventional tank-type melting furnace and formed into flat glass sheets of varying thicknesses by the float method in which the molten glass is supported on a pool of molten metal, usually tin, as it assumes a ribbon shape and is cooled.
The glass compositions of the present invention are particularly suited for the production of infrared energy and ultraviolet radiation absorbing glass for automotive and architectural glazings. Thus, glass sheets of this composition may be heat strengthened or tempered, or alternately annealed and laminated together through an interposed transparent resinous layer, for example composed of polyvinyl butyral, and employed, for example, as a windshield. Generally, the glass sheets for windshield use are of a thickness in the range of from about 1.7 mm to about 2.5 mm, while those tempered and used as sidelights or backlights are in the range of about 3 mm to about 5 mm thick.
Unless otherwise noted, the term percent (%) as used herein and in the appended claims, means percent (%) by weight. Wavelength dispersive X-ray fluorescence was used to determine the weight percents of TiO 2 and total iron expressed as Fe 2 O 3 . Percent reduction of total iron was determined by first measuring the radiant transmission of a sample at a wavelength of 1060 nanometers, using a spectrophotometer. The 1060 nm transmission value was then used to calculate optical density, using the following formula: ##EQU1##
(T o =100 minus estimated loss from reflection=92; T=transmission at 1060 nm).
The optical density was then used to calculate the percent reduction: ##EQU2##
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
The concentrations of each of the three essential colorant constituents depend upon the optical properties desired for the glass and are interrelated to each other. Iron is added, typically as Fe 2 O 3 , and is partially reduced to FeO. The total amount of iron in the batch is critical, and must equal from 0.3 percent to about 0.7 percent by weight, expressed as Fe 2 O 3 . Likewise, the degree of reduction is critical and must equal between 21% and 34%. If the iron is more highly reduced than the critical amount, or if a higher total amount of iron is employed, the glass will become too dark and the Illuminant A visible light transmittance will drop below about 70 percent. Additionally, the glass batch melting process will become increasingly difficult as the increased amount of FeO prevents the penetration of heat to the interior of the melt. If the iron is less reduced than the critical amount, or if a lower total amount of iron is employed, then the direct solar heat transmittance for a desired thickness glass can rise to an unacceptable level, i.e., above about 58%.
From about 3 to about 25 ppm cobalt oxide is added, typically as Co 3 O 4 , along with about 0.5 to about 10 ppm selenium. The proper selenium and cobalt content provides an aesthetically pleasing, neutral tint, somewhat gray color to the glass. Preferred compositions, include a soda-lime-silica base glass and colorants consisting essentially of 0.45 to 0.65 total iron (as Fe 2 O 3 ), with a ratio of ferrous iron to total iron of 25 to 31, 1 to 5 ppm Se, 8 to 20 ppm Co 3 O 4 , 0 to 35 ppm NiO and 0 to 1 weight percent TiO 2 .
The following examples illustrate glass compositions in accordance with the invention that are readily formed into glass articles or glazings such as automobile windshields. The compositions absorb both infrared and ultraviolet rays and have an Illuminant A visible light transmission of at least about 70% and a direct solar heat transmission at least 12 percentage points less than the visible light transmission.
The examples, except examples 1 and 11 which are for comparison purposes only, illustrate but do not limit the invention. In the examples, all parts and percentages are by weight and:
(a) Fe 2 O 3 , FeO, and TiO 2 are expressed in percent; Se, Co 3 O 4 and NiO are expressed in parts per million;
(b) total iron is expressed as if all iron present were present as ferric oxide; and
(c) the FeO content is calculated from the equation ##EQU3## Fe 2 O 3 =percentage total iron, expressed as Fe 2 O 3 , in the glass (143.7 being the molecular weight of 2×FeO and 159.7 being the molecular weight of Fe 2 O 3 ).
The transmittance data in the Table below and throughout are based on a nominal glass thickness of 4 mm.
TABLE 1__________________________________________________________________________Example1 2 3 4 5 6 7 8 9 10 11__________________________________________________________________________Total Iron 0.5 0.55 0.55 0.31 0.61 0.56 0.56 0.54 0.57 0.51 0.53as Fe.sub.2 O.sub.3FeO 0.11 0.14 0.13 0.08 0.14 .13 0.14 0.13 0.16 0.12 0.09% of Total 25 29 27 27.2 26 25 27 27 31 27 19Iron as Fe.sup.2+Se 2 7 9 3 2 2 1 1 <1 2 5Co.sub.3 O.sub.4 10 10 19 20 12 5 13 24 10 12 13TiO.sub.2 1.6 0.33 0.34 -- -- -- -- -- -- 1.0 --NiO -- -- 15 -- -- 23 -- 31 -- -- -- 72 71 71 75 73 76 74 72 74 71 71DSHT 53 50 51 63 51 54 52 53 50 52 57UVT 36 45 47 59 51 51 51 53 53 40 46a* -5.1 -4.8 -5.2 -2.0 -4.7 -4.9 -5.3 -5.0 -6.2 -5.2 -1.9b* 7.5 3.2 2.4 0.2 1.5 1.9 0.3 -1.0 -0.8 5.5 4.1\D 565 546 529 499 512 518 498 499 494 560 569Purity 6.9 2.4 1.7 0.8 1.3 1.3 2.3 3.3 3.6 4.8 4.0__________________________________________________________________________
The base glass composition for example 7, which is essentially the same for all of the examples, was as follows:
______________________________________Component Weight Percent of Total Glass______________________________________SiO.sub.2 73.91Na.sub.2 O 14.04CaO 7.86MgO 3.47SO.sub.3 0.20Al.sub.2 O.sub.3 0.16K.sub.2 O 0.039______________________________________
The batch mixture for example 7, which is likewise similar for all of the examples except for the colorants, was:
______________________________________Constituent Parts by Weight______________________________________Sand 154Soda Ash 50Gypsum 1Limestone 11Dolomite 33Wuestite 1.02C.sub.3 O.sub.3 0.0011Selenium 0.0014Carbon 0.027______________________________________
It is an advantage of the present invention that the composition can be manufactured into flat glass products using commercial manufacturing processes, in particular the float process. A sheet of glass that has been formed by the float process is characterized by measurable amounts of tin oxide that migrated into surface portions of the glass on at least one side. Typically a piece of float-forming glass has an SnO 2 concentration of at least 0.05% by weight in the first few microns below the surface that was in contact with the tin. Glass made by the float process typically ranges from about 2 millimeters to 10 millimeters in thickness.
Another characteristic of most float glass is the presence of traces of melting and refining aids such as sulfur, analyzed in the glass as SO 3 , or fluorine or chlorine. Small amounts of these melting and refining aids (usually less than 0.3% by weight) may be present in the glass compositions of the present invention without effect on the properties.
This description of the invention has been made with reference to specific examples, but it should be understood that variations and modifications as are known to those of skill in the art may be resorted to without departing from the scope of the invention as defined by the claims that follow. | A process and glass batch composition are provided for producing a soda-lime-silica glass containing oxides of iron. The process includes admixing, heating and melting a soda-lime-silica float glass batch mixture comprising sand, soda ash, dolomite, limestone, and a sulfate selected from the group consisting of salt cake and gypsum. In addition, wuestite is included in the batch as at least a partial source of the iron oxides in the resulting glass. | 2 |
BACKGROUND OF THE INVENTION
(1) Field of the Invention
This invention relates to a new fuel for internal combustion engines formed by mixing alcohol with saponified fatty material, which solution can be used as a fuel by itself or in combination with gasoline. The use of the products of this invention will greatly reduce the need for gasoline to run the automobiles and other internal combustion machines in our country.
(2) Desription of the Prior Art
Methods of mixing alcohol with different oils, gas - oil, and some solvents for use as fuels or fuel additives are known, specifically as described in U.S. Pat. Nos. 1,420,622; 1,469,148; 2,646,348; 4,036,604; and 4,177,768. However, none of the formulations disclosed are based on saponified fatty material as an additive.
SUMMARY OF THE INVENTION
The present invention relates to a method of preparing and the products formed by mixing saponified fatty material in alcohol for use as a fuel for internal combustion engines by itself or in combination with gasoline. Commercially available saponified fatty material is dissolved in heated ethanol and a quantity of the saponified fatty material-alcohol solution is added to ethanol. The saponified fatty material dissolves completely in the ethanol and does not separate at low temperatures, thus forming a fuel which is completely stable from low through fuel burning temperatures. It has been found that fatty material products that have not been through the process of saponification will separate from the alcohol at low temperatures, which results in a very defective fuel.
The internal combustion engine in which this new composition of fuel is used does not overheat because the saponified fatty material, having the characteristics of a soap in a liquid state, cleans the engine of any dirt or carbon residue left by previously used fuels. Further, when the saponified fatty material in the alcohol is burned in the engine, it appears to leave a very light lubricating film on the engine parts, thus allowing the engine to work at greater efficiency.
In addition, the alcohol and saponified fatty material solution may be combined with gasoline to provide an efficient fuel while reducing the amount of gasoline necessary to operate the engine.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
The alcohol used in the present invention is completely denatured 199 proof anhydrous ethanol, such as that sold under the Trademark "Corn Power", with the following typical analysis:
______________________________________Apparent proof 199 (min.)Formulation CDA-19(BATF Regulations):Flash Point 60° F.Pounds/Gallon 60° F. 6.60-6.63Specific Gravity 60° F. 0.794Color Colorless______________________________________
The saponified fatty material is of 69% purity, the remaining 31% being chemical components used to saponify a fatty material and water combination. The saponified fatty material used in my tests has the following characteristics:
______________________________________Sodium Chloride (Na Cl) 0.5%Sodium Hydroxide (NaOH) 0.10%Glycerine 0.5%______________________________________
The saponified fatty material for the preparations herein described was obtained from the Colgate-Palmolive Company and was prepared by saponifying rendered meat fat, but it is believed that products formed by the saponification of vegetable oils will work in the same way as described herein.
According to the process of this invention, one part by weight of saponified fatty material is combined with two parts by weight of ethanol in a container which is then placed in a water bath maintained at just below the boiling temperature (100° C.) of water for a period of approximately 2 hours during which time the saponified fatty material dissolves completely in the ethanol. As stated above, the saponified fatty material-alcohol solution thus formed is completely stable at low temperatures. The saponified fatty material-alcohol solution was then added to pure ethanol and ethanol-gasoline mixtures in various proportions and drive tested in both six and eight cylinder automobiles. In all examples the cars ran smoothly during test drives. In addition, after the test drives were completed, the engines were dismantled and were found to be cleaned of all filth and carbon residue and also appeared to be coated with a light film of lubricant which enhanced smooth operation.
EXAMPLE 1
99 parts by volume of 199 proof ethanol were mixed with 1 part by volume of saponified fatty material-alcohol solution at room temperature. The fuel composition formed operated satisfactorily in six and eight cylinder automobile engines.
EXAMPLE 2
99.6 parts of 199 proof ethanol and 0.4 part of saponified fatty material-alcohol solution on a volume basis were mixed at room temperature. The fuel composition formed operated satisfactorily in six and eight cylinder automobile engines.
EXAMPLE 3
94 parts of 199 proof ethanol and 6 parts of saponified fatty material-alcohol solution on a volume basis were mixed at room temperature. The fuel composition formed operated satisfactorily in six and eight cylinder automobile engines.
EXAMPLE 4
80 parts of 199 proof ethanol, 19 parts gasoline and 1 part saponified fatty material-alcohol solution on a volume basis were mixed at room temperature. The fuel composition formed operated satisfactorily in six and eight cylinder automobile engines.
EXAMPLE 5
80.6 parts of 199 proof ethanol, 19 parts gasoline and 0.4 part saponified fatty material-alcohol solution on a volume basis were mixed at room temperature. The fuel composition formed operated satisfactorily in six and eight cylinder automobile engines.
EXAMPLE 6
75 parts of 199 proof ethanol, 19 parts gasoline and 6 parts of saponified fatty material-alcohol solution on a volume basis were mixed at room temperature. The fuel composition formed operated satisfactorily in six and eight cylinder automobile engines.
The amounts of each ingredient in the foregoing compositions can be varied within the limits set forth. Further, all tests in Examples 4 through 6 operated satisfactorily with regular, premium, high octane and no-lead gasolines. The examples set out above may also be expressed in terms of percentages since each example comprises a total of 100 parts. | Internal combustion engine fuels comprising solutions of ethyl alcohol containing dissolved saponified grease and solutions of gasoline and ethyl alcohol containing dissolved saponified grease. The method of preparing the solutions comprises predissolving saponified grease in ethanol and then combining the dissolved saponified grease with ethanol or with a combination of ethanol and gasoline. | 2 |
CROSS REFERENCE TO RELATED APPLICATIONS
[0001] This application claims the benefit of US Provisional Application No. 61/733, 472 filed Dec. 05, 2012. The application is also continuation-in-part of:
1. U.S. patent application Ser. No. 13/482,473 filed on May 29, 2012; 2. U.S. patent application Ser. No. 13/279,673 filed on Oct. 24, 2011; 3. U.S. patent application Ser. No. 13/050,515, filed on Mar. 17, 2011 which claims the benefit of US provisional application No. 61/316,844 filed on Mar. 24, 2010; and 4. U.S. patent application Ser. No. 13/214,588, filed on Aug. 22, 2011. The contents of each of the above-referenced applications are incorporated herein by reference.
TECHNICAL FIELD
[0006] The invention generally relates to a system for managing a campaign, and more specifically to system and methods for monitoring the behavior of an advertisement over the web and providing recommendations respective thereof.
BACKGROUND
[0007] The ubiquity of access availability to information using the Internet and the worldwide web (WWW), within a short period of time, and by means of a variety of access devices, has naturally drawn the focus of advertisers. The advertisers may pay publishers such as search engines, for example, Google® or Yahoo!®, for the placement of their advertisement when a related keyword to said advertisement is submitted by a user for a search. Other publishers may be social networks, such as Facebook®, Google+®, and Linked In® that further allow placement of advertisements for a fee.
[0008] Each of the advertisement publishers provides a unique application programming interface (API) through which a user wishing to place an advertisement, or bidding for a placement respective thereof, is expected to use. As on-line advertising continuously changes and develops, with more publishers becoming available and utilizing many different types of unique APIs, it has become difficult to monitor the performance of a campaign. Furthermore, it has become difficult to predict the efficiency at the starting point of the campaign due to the plurality of variables needed to be considered.
[0009] It would therefore be advantageous to overcome the limitations of the prior art by providing an effective way to monitor the performance of a campaign. It would be further advantageous to overcome the limitations of the prior art by providing an effective way to predict a future performance of a campaign.
SUMMARY
[0010] Certain embodiments disclosed herein include a method for adaptive learning of at least one advertisement behavior. The method comprises receiving electronically at least one advertisement and associated metadata from a client node over a network; continuously monitoring the behavior of the at least one advertisement; analyzing the performance of the at least one advertisement; and determining the future performance of the at least an advertisement respective of the analysis.
[0011] Certain embodiments disclosed herein also include an apparatus for an adaptive learning of at least one advertisement behavior. The apparatus comprises an interface to a network for receiving and sending data over the network; a client node coupled to the network; a database coupled to the network; a processing unit coupled to the network; and a memory coupled to the processing unit that contains therein instructions that when executed by the processing unit configures the apparatus to: receive electronically at least one advertisement and associated metadata from a client node over the network; and, continuously monitor the behavior of the at least one advertisement; analyze the performance of the at least one advertisement; determine the future performance of the at least an advertisement respective of the analysis.
BRIEF DESCRIPTION OF THE DRAWINGS
[0012] The subject matter that 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 objects, features, and advantages of the invention will be apparent from the following detailed description taken in conjunction with the accompanying drawings.
[0013] FIG. 1 —is a schematic diagram of a system in accordance with an embodiment;
[0014] FIG. 2 —is a flowchart describing the operation of the system in accordance with an embodiment; and,
[0015] FIG. 3 —is graph describing the monitoring of an advertisement in accordance with an embodiment.
DETAILED DESCRIPTION
[0016] The embodiments disclosed by the invention are only examples of the many possible advantageous uses and implementations of the innovative teachings presented herein. In general, statements made in the specification of the present application do not necessarily limit any of the various claimed inventions. Moreover, some statements may apply to some inventive features but not to others. In general, unless otherwise indicated, singular elements may be in plural and vice versa with no loss of generality. In the drawings, like numerals refer to like parts through several views.
[0017] A system monitors in real-time the performance of an advertisement over the web. The system analyzes the performance of the advertisement and provides tools for optimal management of an advertisement budget in real-time. In one embodiment the system is capable of predicting the behavior of an advertisement and providing recommendations respective thereof.
[0018] FIG. 1 depicts an exemplary and non-limiting schematic diagram of a system 100 in accordance with an embodiment. A server 110 , such as, but not limited to, a computer comprising of a processing unit 114 which is coupled to an internal memory 112 , where the server 110 is connected to a network 120 . The server 110 is configured to receive requests for placements of advertisements which include the advertisement itself and metadata associated thereto, and responsively after, interfacing with the requested publisher node to place the request advertisement. The network 120 can be wired or wireless, a local area network (LAN), a wide area network (WAN), a metro area network (MAN), the Internet, the worldwide web (WWW), the likes, and any combinations thereof. The memory 112 contains instructions that when executed by the processing unit 114 configure the server 110 to perform the functions described herein below. The server 110 receives a request to publish an advertisement with at least a publisher node from the plurality of publisher nodes 140 - 1 through 140 -N, and associated metadata from a client node, for example, client node 130 . Responsive thereto, the server 110 is configured to monitor in real-time the behavior of the published advertisement and analyze the advertisement's performance.
[0019] According to one embodiment, in order to analyze the performance of a single advertisement, the server 110 monitors the output of the advertising platform, for example, the budget spent and the volume of impressions collected from users that view or responded to the published advertisement. The server 110 is then configured to recalculate and suggest a better input, for example, a better budget split. According to another embodiment the server 110 tracks the non-time-invariant behavior of the published advertisement. The tracking of the non-time invariant behavior of the published advertisement is necessary because the volume of impressions through time is heavily affected by the presence of crowd routine viewing the advertisement through time. As an example, the more people are on Facebook®, the more ad-spaces are available. Furthermore, as the advertisement price is usually determined based on a bid, additional circumstances must be considered in order to achieve an optimal performance. Such circumstances may relate to the common behavior of web advertising, for example, while approaching end of quarter advertisers tends to increase the advertisement. Other example is that most of the advertisers do not work weekends. In order to track the non-time-invariant behavior of the published advertisement, the server 110 identifies the volume of impressions received respective the published advertisement within a specific location considering the local time in that location.
[0020] The behavior of the published advertisement together with the respective analysis is saved in a database 150 for future use. The accumulative data stored in the database 150 may further be used by the server 110 to determine and predict a publisher's behavior. As a non-limiting example, by analyzing the costs for publishing a specific type of advertisements with Facebook® over time, the server 110 may identify that at the end of every quarter, the costs for publishing such type of advertisements is higher. Respective of such identification the server 110 is capable of profiling the behavior of Facebook® and provide recommendations respective thereof.
[0021] The server 110 is then capable of providing one or more recommendations for optimal management of the advertisement. It should be understood that while a single client node 130 is shown in FIG. 1 , this should not be viewed as limiting on the invention, and one of ordinary skill in the art would readily appreciate that additional client nodes can be added without departing from the spirit and/or scope of the invention. In another embodiment of the invention the one or more recommendations are automatically executed by the server 110 without further intervention by a user of the client node 130 .
[0022] FIG. 2 depicts an exemplary and non-limiting flowchart 200 describing the operation of the system in accordance with an embodiment. In S 210 , a server, for example the server 110 , receives a request to publish an advertisement from a client node, for example the client node 130 , and associated metadata respective of the advertisement. Such metadata may be the targeted audience, a multimedia content to be displayed, budget constraints, preferred publishers, preferred advertising platforms, preferred times, etc. In one embodiment the server 110 may further receive from the user of the client node 130 expectations or requirements respective of the advertisement. In S 220 , the server 110 monitors the behavior of the published advertisement in real-time. The behavior may be related to an advertising platform's outputs. Such advertising platform's outputs may be but are not limited to at least one of: audience impression related to the advertisement, amounts of clicks on a multimedia content in the advertisement, conversions from the advertiser's website, etc. The monitoring is continuously performed as the platform's outputs may be unevenly spaced through time. In S 230 , the server 110 analyzes the performance of the published advertisement. The analysis may be made respective of the requirements determined by the user or respective of one or more statistical parameters which are based on experience related to one or more similar advertisements. According to one embodiment, respective of the analysis, the server 110 is configured to determine the future performance of the advertisement. In S 240 , the server 110 is configured to provide a recommendation for optimal management of the advertisement respective of the analysis. The recommendation may comprise the process of: calculating a recommendation, display a recommendation, operating the system 100 respective of a recommendation and a combination thereof. Such recommendation may relate to the split of the budget, the time of the day, the week or the month the advertisement is published, changes in the bidding and/or bidding strategy on the ad space, changes on the budget spent on every variation of the ad, changes in the budget spent on every variation of the targeting parameters of the ad, etc. In S 250 , it is checked whether there are more requests and if so, execution continues with S 210 ; otherwise, execution terminates. It should be understood that the server 110 is further capable of monitoring and analyzing a campaign comprising a plurality of advertisements and provide recommendations respective thereto as further described hereinabove. According to another embodiment, the server 110 is capable of predicting the future behavior of an advertisement respective of data stored in a database, for example the database 150 , and provide recommendations respective thereto.
[0023] FIG. 3 depicts an exemplary and non-limiting graph 300 describing the monitoring of an advertisement in accordance with an embodiment. The horizontal axis 310 uses a predetermined time frame's resolution where the server 110 monitors the amount of clicks on the advertisement. The vertical Axis 320 of the graph 300 shows the amount of clicks on the advertisement over the predetermined time frames (labeled as 310 ). The server 110 , by continuously analyzing of the amount of clicks on the advertisement over time, instantly identifies the changes of the delivery rate respective of the advertisement over the course of a day. Respective thereto the server 110 is capable of recommending when to increase or decrease a bid respective of the advertisement during the course of the day. According to another embodiment, the server 110 can further predict the behavior of an advertisement by comparing the behavior of one or more advertisements which have related metadata. According to another embodiment a publisher, for example, Facebook®, may require a mandatory decrease in a bid respective of an advertisement upon meeting a certain threshold. Such requirement may occur when the provider wishes to optimize the user experience for the targeted audience and prevent users from viewing the same advertisements periodically. In such embodiment the server 110 , is capable of identifying a common pattern related to such mandatory requirement received from a provider and provide a real-time recommendation regarding the allocation of the budget while avoiding reaching such a threshold. The various embodiments of the invention are implemented as hardware, firmware, software, or any combination thereof. Moreover, the software is preferably implemented as an application program tangibly embodied on a program storage unit or computer readable medium consisting of parts, or of certain devices and/or a combination of devices. The application program may be uploaded to, and executed by, a machine comprising any suitable architecture. Preferably, the machine is implemented on a computer platform having hardware such as one or more central processing units (“CPUs”), a memory, and input/output interfaces. The computer platform may also include an operating system and microinstruction code. The various processes and functions described herein may be either part of the microinstruction code or part of the application program, or any combination thereof, which may be executed by a CPU, whether or not such computer or processor is explicitly shown. In addition, various other peripheral units may be connected to the computer platform such as an additional data storage unit and a printing unit. Furthermore, a non-transitory computer readable medium is any computer readable medium except for a transitory propagating signal.
[0024] All examples and conditional language recited herein are intended for pedagogical purposes to aid the reader in understanding the principles of the invention and the concepts contributed by the inventor to furthering the art, and are to be construed as being without limitation to such specifically recited examples and conditions. Moreover, all statements herein reciting principles, aspects, and embodiments of the invention, as well as specific examples thereof, are intended to encompass both structural and functional equivalents thereof. Additionally, it is intended that such equivalents include both currently known equivalents as well as equivalents developed in the future, i.e., any elements developed that perform the same function, regardless of structure. | A system and method for adaptive learning of at least one advertisement behavior. The method comprises receiving electronically at least one advertisement and associated metadata from a client node over a network; continuously monitoring the behavior of the at least one advertisement; analyzing the performance of the at least one advertisement; and determining the future performance of the at least an advertisement respective of the analysis. | 6 |
CROSS-REFERENCE TO RELATED APPLICATIONS
[0001] The present invention is a continuation of U.S. patent application Ser. No. 10/864,359, entitled “Device for manipulation of limited quantities of liquids”, filed on Jun. 10, 2004 and incorporates all of the material therein by reference.
BACKGROUND OF THE INVENTION
[0002] This invention relates to a device for manipulation of liquids and a process for producing and using such a device.
[0003] Document WO 02/085520 A2 discloses a body which has a surface which has first and second surface areas which have different wettability with a liquid. The surface areas can, for example, be hydrophilic on the one hand and hydrophobic on the other hand. It is possible for the surface areas to be lipophilic or lipophobic with respect to oily solutions. In this publication, two processes for producing different surface areas are named. Thus, on the one hand the different wetting properties can be achieved by coatings. These coatings can be attained by lithographic processes with subsequent coating steps. On the other hand, the different wetting properties can be attained by microstructuring, as is the case in the so-called lotus effect which is based on different roughnesses of the surface. These different roughnesses can be obtained by microstructuring of the corresponding surface areas. Within the microstructured areas, capillary forces act which keep the liquids in these surface areas. The publication, as an example for producing a microstructure, names a chemical treatment, or ion irradiation.
[0004] If microstructuring is produced by chemical treatment, etching is possible, or by ion irradiation, an irregularly structured surface is formed in the generic solids. The surface cannot be exactly acquired by computations.
[0005] Therefore, it is difficult to exactly specify the acting capillary forces. But if surface areas with different capillary forces are to be produced, it is advantageous to know exactly the acting capillary forces of each surface area and to produce surface areas with desired capillary forces.
[0006] Another problem with the microstructures produced by the known processes is that the acting capillary forces which keep the liquid in one of the surface areas and which thus also dictate the amounts of liquid which can be stored in the surface area are relatively small. Thus only a relatively small amount of liquid can be deposited in the microstructured surface area.
[0007] The publication, with the publication number U.S. Pat. No. 6,451,264 B1, discloses a device with which liquids are routed through curved capillary channels to different chambers in which the liquid can be tested for certain reactions. In the device, there are dry reagents which are suitable for this purpose. The dry reagents should be located in the chambers in which the liquid is tested.
[0008] In the curved capillary channels, the phenomenon occurs that the liquid on the wall with the smaller radius is conveyed more rapidly than the opposing channel wall with the larger radius. Uniform motion of the liquid through the curved channels is therefore conventionally not possible. In order to remedy this problem, in the indicated publication, it is proposed that microstructured surfaces with regularly arranged structure elements be placed in the curved channel; these elements ensure uniform motion of the liquid in the curved channels. If a liquid reaches such a microstructured surface area in the curved channel, first this microstructured surface area is filled with liquid. Only when the microstructured surface area is completely filled with liquid do the transport forces cause the liquid in the transport direction to emerge again from the microstructured surface area. Transport along the channel wall with the smaller radius which is more rapid than the transport of the liquid along the channel wall with the larger radius is thus prevented. The liquid is transported uniformly through the curved channel.
[0009] The microstructured surface areas in the curved channels of the device, according to the indicated publication, are thus not suited or intended for storing or depositing a liquid. The purpose of the microstructured surface areas is to ensure uniform motion of the liquid in the curved channel. The device, as is known from the publication with the publication number U.S. Pat. No. 6,451,264 B1, is not suited for manipulation of liquids in the sense of this invention, especially not for storage or deposition of defined amounts of liquid.
[0010] The document, with publication number U.S. Pat. No. 6,368,871 B1, discloses a device which has a surface area in which microstructure elements are located. This surface extends in a widened point of a channel from the one channel wall to the opposing channel wall. The structures are used to filter a certain substance out of the liquid flowing through the channel in order to extract or concentrate it (column 7, line 40 to line 57). The microstructure elements of the surface area in the channel are neither suited nor intended to store or deposit defined amounts of liquid. Nor is storage of defined amounts of reagents in the surface areas known.
[0011] A device for manipulation of liquids has a solid. This solid has, as is already known, surface areas in which different capillary forces are acting. One or more first surface areas have a microstructured and/or nanostructured surface which have regularly arranged structure elements. The structure elements are connected in one piece to the remaining solid and consist of the same material as the remaining solid.
[0012] The regularly arranged structure elements in the first surface area, or in the first surface areas, produce capillary forces which provide for the liquid's remaining in the first surface area. The action of the capillary forces is so great that the liquid which touches the edge of the first surface area is sucked into the first surface area by the capillary force. By the choice and the configuration of the structure elements in the first surface area, the capillary force caused by the structure elements can be set. Setting can take place by trying out various geometries or by concerted calculation of the capillary force of the geometries. The defined capillary force of the first surface areas makes it possible to store or deposit a defined amount of liquid in the first surface areas. Thus, for example, defined amounts of one or different reagent liquids can be deposited and immobilized in the surface areas, for example dried up. This ensures that a defined amount of the reagent is located in the first surface area. Later a second amount of liquid, for example, a sample liquid, can be delivered onto the first surface area, this second amount of liquid also being limited, i.e. being defined, by the known capillary force of the first surface area.
[0013] One or more first surface areas can be provided with one or different agents. The reagents can be stored between the structure elements. Furthermore, it is possible for the reagents to be encapsulated in particles, these particles being plastic particles or magnetic particles. Likewise, it is possible for the second surface areas to be provided with reagents.
[0014] The reagent or the reagents can be stored in a resuspendable manner in the first surface area or areas. To do this, the reagents can be moved in liquid form by means of a pipette onto the first surface areas of the device. Then the reagents are dried up. The reagents are not covalently coupled to the surface, but can be resuspended over suitable liquids.
[0015] The reagents can then be resuspended, for example, by a sample (liquid material for analysis). To do this, the sample can be moved directly onto the first surface areas or can be routed via a channel system, especially via a channel system of capillary channels, to the first surface areas from an inlet. The reagents are dissolved and mobilized by contact with the sample. In this way, they can react with the sample. The reagents which have been dried up in the first surface area and which are also called dry chemicals or dry reagents because of this drying up, can be suited to detection of a certain component of the sample. The dry chemicals can be used to make the components of the sample visible. This can take place by simple dyeing or by conventional enzymatic chemoluminometric indicator reactions. The reaction can then be analyzed, for example, by photometric studies or with the naked eye. In addition to the indicated optical processes, electrochemical analysis processes can also be used, for example, by electrodes in the device.
[0016] The reagents can also be permanently stored in the first surface areas of a device as described in the invention. The reagents can then be used as biochemical probes, the substance present in a sample liquid which has been dispensed onto the first surface areas being bound in a concerted manner to these biochemical probes; this enables detection of the substance. The reagents stored permanently in the first surface areas are not resuspended by the sample liquid. The reagents are inserted rather securely in the surface of the first surface areas. The substances which are present in the sample liquid react with these stored reagents. The reaction product cannot be washed out. Rather the reaction product must be examined at the location of the first surface areas, for example, by optical processes.
[0017] A device as claimed in the invention can be produced for example by the following process. First, in the surface of the solid, surface areas are produced by working (for example, metal cutting, laser working or ion beam working) of the solid, in the surface areas at least partially different capillary forces acting. In the first surface areas during working microstructured and/or nanostructured surfaces are produced and are formed by regularly arranged structure elements. Likewise, it is possible to mold the microstructures of the first surface areas in the production of the solid, for example, by injection molding (microinjection molding) into the surface of the solid. A solid then advantageously consist of a plastic. But it is also possible to produce the solid of a device from glass or silicon.
[0018] In the device, there can be second surface areas which are made preferably flat, i.e. without microstructuring or nanostructuring. In the second surface areas preferably compared to the first surface areas in any case low capillary forces are acting so that a liquid is preferably stored in the first surface areas or is preferably taken up by the first surface areas.
[0019] In the first surface areas of a device capillary forces of different size can act.
[0020] The structure elements of a device which are intended for microstructuring and/or nanostructuring of the first surface areas can comprise columns and/or stelae. These columns can have a diameter from 0.1 to 500 microns. The distance from column or stele to column or stele can be 0.1 to 500 microns.
[0021] The columns or stelae can have a circular or polygonal cross section. The diameter of the columns or stelae is advantageously 0.1 to 500 microns.
[0022] The structure elements can furthermore comprise grooves which preferably have a width from 0.1 to 500 microns and a depth from 0.1 to 500 microns. The grooves are preferably arranged in parallel, have a distance from 0.1 to 500 microns from one another and are preferably 0.1 to 500 microns deep. The grooves can be straight or circular. It is possible for the grooves to have a notch-like cross section. The grooves can be joined to one another and form a channel structure, for example, a net-like or meandering channel structure.
[0023] Moreover, it is possible for there to be crosspieces as structure elements in the device. These crosspieces can have a width from 0.1 to 500 microns and a height from 0.1 to 500 microns. Advantageously, the crosspieces have a distance from 0.1 to 500 microns and are arranged in parallel to one another.
[0024] In a lowered first surface area, the structure elements can also be notches which are made in the edge of the lowered surface area. These notches are, for example, known from document U.S. Pat. No. 6,296,126 B1, FIG. 6, reference number 17 as means for overcoming a capillary stop.
[0025] In the device, one or more first surface areas are lowered or elevated relative to the surrounding surface. Such a sudden change of the surface properties and the resulting large capillary force, similarly to a capillary stop, lead to a capillary jump which clearly delimits the elevated or lowered surface areas.
[0026] The first surface areas can be arranged in the form of a matrix, the first surface areas being surrounded in part or preferably completely by the second surface area. The first surface areas can be located especially also in a chamber of the device which has an inlet and an outlet so that a sample liquid can flow through the chamber. The first surface areas can then be located both next to one another and also in succession in one or more rows in the chamber, each first surface area being surrounded by the second surface area.
[0027] The first surface areas of a device can be functionalized before applying the reagents by plasma processes such as, for example, plasma polymerization or wet chemical processes. In this way, the amount of reagent which is to be stored in the first surface area can be increased.
[0028] In one preferred version of a device, one section of the continuous first and/or second surface areas is lowered relative to the surrounding surface. This continuous section can then be closed with a cover, and the cover can be formed by a second solid which can be made like the first solid, and the space located between the section and the cover forming a reaction chamber. If the second solid is made similarly to the first solid, it preferably has first surface areas which are located advantageously opposite to the first surface areas of the first solid.
[0029] Such a device can then have a first inlet. This inlet then advantageously comprises an inlet channel which discharges into the reaction chamber, an inlet chamber and/or an inlet opening in the cover or in the solid. The inlet can also discharge directly into the first surface area.
[0030] Analogously there can also be an outlet in the device. This outlet can comprise an outlet channel which begins in the reaction chamber and which advantageously adjoins an outlet chamber. This outlet chamber can then be connected to the environment via an outlet opening in the cover or in the solid.
[0031] The inlet and the outlet of a device as claimed in the invention are used on the one hand to add and remove the sample liquid. On the other hand the inlet and the outlet are also used for aeration and deaeration during transport processes in a device and especially in its reaction chamber.
[0032] In a device, there can be one or more second inlets. These second inlets, analogously to the first inlets, are equipped advantageously with inlet channels, inlet chambers, and/or inlet openings in the cover or in the solid. The inlet channels are then joined to one first surface area at a time. But it is also conceivable for the inlet channels of the second inlets to be connected to a second surface area.
[0033] In the process, after producing the first surface areas in the solid, a reagent-containing liquid can be dispensed onto the first surface areas. Different liquids can be dispensed onto different first surface areas. These liquids can then be mixed with another liquid, specifically a sample, the sample reacting with the reagents. It is possible for the reagents to be temporarily attached, for example, dried up, to the first surfaces. The reagents are then stored as a solid on the surfaces. By supplying a sample these dried-up reagents can then be dissolved. The sample then reacts with the dissolved reagents in the area of the first surface areas, on a separate reaction chamber of the device or after removal from the device outside the device. Furthermore, it is also possible for the dried-up reagents to be dissolved with a solvent in order then in the area of the first surface areas or in another area of the device to be mixed with a sample liquid in order to initiate the desired reaction.
[0034] It is possible for the reagents to be permanently attached in the first surface areas, i.e. immobilized. The reagents can be attached via a covalent bond. The sample can then be delivered onto the first surface areas for analysis. If then the substance which is to be analyzed should be present in the sample, it binds to the corresponding first surface areas. This binding reaction can be detected via a corresponding indicator reaction.
[0035] The microstructured or nanostructured surfaces of the first surface areas can be shaped in a depression of the solid. If this depression is closed with a cover, the depression forms a reaction chamber. Advantageously, there is a first inlet for this reaction chamber. Furthermore, there can also be a second inlet which is closed when a liquid with reagents is added to the device. The closing of the second inlet has the advantage that in this way the amount of liquid exactly metered with the reagents can be delivered into the device or into the reaction chamber in order to isolate it subsequently from the environment.
BRIEF DESCRIPTION OF THE DRAWINGS
[0036] Embodiments for devices as claimed in the invention are detailed using the drawings.
[0037] FIG. 1 shows an overhead view of a first device as claimed in the invention,
[0038] FIG. 2 shows a section according to line II-II in FIG. 1 ,
[0039] FIG. 3 shows an overhead view of a carrier of a second device as claimed in the invention,
[0040] FIG. 4 shows a section through the second device as claimed in the invention according to line IV-IV in FIG. 3 ,
[0041] FIG. 5 shows an overhead view of a carrier of a third device as claimed in the invention,
[0042] FIG. 6 shows a section through the second device as claimed in the invention according to line VI-VI in FIG. 5 ,
[0043] FIG. 7 shows a section through the third device as claimed in the invention according to line VII-VII in FIG. 5 , and
[0044] FIG. 8 shows a section through the third device as claimed in the invention according to line VIII-VIII in FIG. 5 .
DETAILED DESCRIPTION OF THE INVENTION
[0045] The device which is shown in FIGS. 1 and 2 consists of a solid which is designated the carrier 1 , in the form of a cuboid. On the top of the carrier 1 there are first surface areas 6 a to 6 e and second surface areas 7 . The first surface areas 6 a to 6 e are located spaced apart from one another and each of these first surface areas 6 a to 6 e has a shape which is rectangular in an overhead view. These first surface areas 6 a to 6 e of the carrier 1 have a microstructured surface. The second surface areas 7 which include the first surface areas are conversely made flat. In the areas of the first surface areas 6 a to 6 e greater capillary forces act than in the second surface areas 7 due to the microstructured surface in the first surface areas 6 a to 6 e.
[0046] For the first surface areas 6 a to 6 e the surfaces are microstructured in different ways. But devices for certain applications are feasible in which the surfaces are microstructured in the same way. It is common to all first surfaces 6 a to 6 e that the microstructured surfaces of the first surface areas 6 a to 6 e have regularly arranged structure elements A to E. The first surface areas 6 a to 6 e of the carrier 1 differ in the shape of the selected structure elements. Due to the different structure elements in the first surface areas 6 a to 6 e capillary forces act which are different from one another and which have a certain effect on the storage capacity of the liquids of the respective microstructured surface.
[0047] It is common to the structure elements of the first surface areas 6 a to 6 e that they are advantageously produced solely by mechanical working of the carrier 1 , the carrier 1 consisting of a material and the structure elements not be applied by coatings or the like to the carrier 1 .
[0048] In the carrier 1 as shown in FIGS. 1 and 2 there are the following structure elements A to E in the first surface areas 6 a to 6 e . The first structure area 6 a has notch-like grooves A as the structure elements. These grooves are arranged parallel to one another in the transverse direction of the carrier 1 .
[0049] Spaced apart from the first surface area 6 a and separated by a second surface area 7 is the first surface area 6 b . This first surface area 6 b as structure elements has columns B which are arranged in a grid. These columns B have a circular cross section.
[0050] Spaced apart from this first surface area 6 b and separated by a second surface area 7 is the first surface area 6 c . As structure elements here there are in turn grooves C which are likewise arranged in the transverse direction of the carrier 1 , but which have a rectangular cross section.
[0051] Separated by a second surface area 7 and spaced apart from the first surface area 6 c is the first surface area 6 d . This first surface area 6 d has crosspieces D arranged in the lengthwise direction of the carrier 1 as structure elements.
[0052] Separated by another second surface area is the last first surface area 6 e of the carrier 1 . This first surface area 6 e as structure elements has columns E which however in contrast to columns A of the first surface area 6 b have a square cross section.
[0053] Furthermore, reference is made to FIGS. 3 and 4 which show a second device as claimed in the invention. The second device has a solid which is designated the carrier 1 , and a cover 2 , in FIG. 3 for the sake of better clarity only the carrier 1 being shown in an overhead view. The carrier 1 on its top has several recesses which are connected to one another and which are at least partially closed by the cover 2 . In this way the recess in the top of the carrier 1 forms cavities or channels between the carrier 1 and the cover 2 . One of the cavities in the second device forms a reaction chamber 4 here.
[0054] The reaction chamber 4 is connected to the environment via an inlet 3 , 3 a , 3 b and an outlet 5 , 5 a , 5 b . The inlet comprises an inlet opening 3 b in the cover 2 which is connected to the inlet chamber 3 a which is formed by a recess in the top of the carrier 1 . This inlet chamber 3 a is connected via an inlet channel 3 to the reaction chamber 4 . The reaction chamber 4 is then connected via an outlet channel 5 to the outlet chamber 5 a . From this outlet chamber 5 a there is a connection to the environment via an outlet opening 5 b in the cover 2 .
[0055] The inlet channel 3 , the reaction chamber 4 and the outlet channel 5 are made such that a liquid dispensed into the inlet 3 , 3 a , 3 b as a result of the action of capillary forces or other transport forces such as, for example, pressure can be transported out of the inlet 3 , 3 a , 3 b into the reaction chamber 4 and from there further in the direction of the outlet 5 , 5 a , 5 b . The aeration and deaeration of the reaction chamber 4 which are necessary in this transport process of a liquid by or in the second device takes place via the inlet opening 3 b and the outlet opening 5 b in the cover 2 .
[0056] The bottom of the reaction chamber 4 is formed by a section of the surface of the carrier 1 . This section consists of continuous first surface areas 6 b , 6 d and the second surface areas 7 surrounding them. The first surface areas 6 b , 6 d have a microstructured surface which are formed by regularly arranged structure elements B, D. In these microstructured surfaces 6 b , 6 d larger capillary forces act than in the second surface areas 7 surrounding them. In this way the first surface areas 6 b , 6 d can be more easily wetted (hydrophilic) especially for water or aqueous solutions.
[0057] The first surface area 6 b is lowered compared to the surrounding second surface areas 7 . This has the advantage that a liquid which has collected in the first surface area 6 b must first overcome capillary forces which prevent overflow of the liquid from the first surface area 6 b on the edges of the first surface area b. The edges of the lowered first surface area 6 b thus form a type of capillary stop which prevents liquid transport beyond the edges of the first surface area 6 b.
[0058] There are crosspieces D which are arranged parallel to one another as structure elements in the surface area 6 d of the second device.
[0059] The first surface areas 6 b , 6 d of the second device are otherwise treated with reagents (advantageously different reagents). This means that before the cover 2 is placed on the carrier 1 , reagents are applied to the first surface areas 6 b , 6 d for example with a dispenser. Thereupon the reagents can be dried up in the first surface areas 6 b , 6 d and then the reaction chamber 4 can be closed by placing the cover 2 on the carrier 1 . Via the inlet 3 , 3 a , 3 b now a sample liquid can be delivered into the second device which as a result of capillary forces or other transport forces, for example pressure, is pulled into the reaction chamber 4 and wets the first surface areas 6 b , 6 d there.
[0060] The cover 2 is generally attached to the carrier 1 by welding or the like. Here it can happen especially in welding that heat-sensitive reagents which are stored in the first surface areas 6 b , 6 d can be damaged. A solution to this problem is however offered by the third device as is described using FIGS. 5 to 8 , to which reference is made below.
[0061] The third device which is shown in FIGS. 5 to 8 , like the device as shown in FIGS. 3 and 4 , has a carrier 1 and a cover 2 which borders the reaction space 4 to the top. Furthermore, the third device has an inlet 3 , 3 a , 3 b and an outlet 5 , 5 a , 5 b like the second device, as is shown in FIGS. 3 and 4 . The reaction chamber 4 is formed by a continuous section of the first surface areas 6 d and the second surface areas 7 . The first surface areas 6 d are arranged spaced apart from one another and separated by the second surface areas 7 . The first surface area 6 d which is the left one in FIGS. 5 and 6 is a surface area which is lowered compared to the surrounding surface of the second surface area 7 . Conversely, the first surface area 6 d which is the right one in the figure is raised compared to the surrounding second surface areas 7 . The two first surface areas have crosspieces D as structure elements. The crosspieces D of the left first surface area 6 d are arranged parallel to one another in the lengthwise direction of the reaction chamber 4 , while the crosspieces D of the first surface area which is the right one in the figure are arranged parallel to one another in the transverse direction of the reaction chamber 4 .
[0062] The first surface area 6 d which is the left one in the figure is spaced apart from the side walls of the reaction chamber 4 , while the first surface area 6 d which is the right one in the figure with its structure elements D adjoins the side walls of the reaction chamber 4 which extend in the lengthwise direction.
[0063] Both the left first surface area and the right first surface area are connected to the environment of the third device via second inlets 8 , 8 a , 8 b for reagents. These second inlets have an inlet channel 8 which discharges in the first surface areas 6 d . This inlet channel 8 is connected to the inlet chamber 8 a which adjoins the inlet opening 8 b which leads through the cover 2 .
[0064] The advantage of such a third device as claimed in the invention is that after placing the cover 2 on the carrier 1 , via the inlet openings 8 a of the second inlets 8 , 8 a , 8 b reagents can be dispensed into the third device. They are transported for example as a result of capillary forces to the first surface areas 6 b where they are uniformly distributed and advantageously dry up there. At a later time then a sample liquid can be delivered into the inlet opening 3 b which as a result of active capillary forces is distributed over the inlet channel 3 in the reaction chamber 4 .
[0065] Devices and their applications are described by way of example below:
Example 1
[0066] One preferred embodiment of the invention relates to a microstructured device (microchip) with which a liquid can be studied. The microchip contains a fill area and an examination area with at least one microstructured first surface area which is arranged within the examination area and which is surrounded by a second surface area. The first surface area comprises essentially regularly arranged columns, crosspieces or recesses and allows storage of dry chemicals (for example as indicators) which are used generally as detection reagents by application (spotting) of a liquid with the dissolved reagent (chemical, enzyme, antibody, nucleic acid, particle coated with chemicals and the like) and its subsequent drying.
[0067] In one preferred embodiment of the microchip the surface of the first surface areas is continuously hydrophilic. When a liquid droplet or a defined amount of liquid was applied by means of a pipette or dispenser to an unstructured part of the chip surface, for example the second surface, the liquid droplet ran irregularly and uncontrolled and the reagent was not uniformly dried up and immobilized or absorbed on the surface. This would result in that the following test would be less precise.
[0068] In this embodiment, the liquid droplet or the liquid amount with the reagent dissolved therein however after application by means of a dispenser or a pipette remains within the limits of the structured first surface area. This results in that the reagent is dried up and stored only in the geometrical area which is defined by the surface structuring. Thus the location of any such spot can be accurately predicted; this simplifies the automated readout of the spot which is typically used in array technology by means of an optical scanner.
[0069] By applying a host of chemicals to a host of these structured surface areas a so-called array test chip can be devised in this way. To do this, following the spotting the structured side of the microchip is closed with a cover (adhesive film, plastic plate, glass plate, etc.) except for an inlet and an outlet.
[0070] For analysis of a sample liquid the sample is routed via the inlet into the examination chamber where individual sample components can react with the different spots.
[0071] The microchip is suited for applications and tests of liquids which contain biomolecules such as nucleic acids and proteins.
Example 2
Immobilization of Streptavidin
[0072] To immobilize streptavidin the microstructured first surface areas of the microchip according to example 1 are coated with streptavidin. To do this, by means of a laboratory dispenser (GeSiM) 0.1 μl streptavidin solution (1 μg/ml in 0.1 M phosphate buffer, pH 7.0) is applied to the individual microstructured first surface areas and dried up. Then the excess, unbound streptavidin is removed by washing with 0.1 M phosphate buffer, pH 7.0. In order to increase the amount of streptavidin bound to the surface, the first surface areas before spotting can be functionalized by for example plasma processes such as plasma polymerization or wet-chemical processes.
[0073] For analysis purposes the fluorescein-biotin sample is applied to the entire chip surface in different concentrations (1.0 μM in PBS) and removed by a washing buffer after an incubation time of 30 seconds. The chip can then be optically measured under a fluorescence microscope or fluorescence reader at 485/525 nm (Virtek reader), the fluorescence intensity correlating with the concentration of fluorescein-biotin.
Example 3
Production of an Antibody Microarray
[0074] In an antibody microarray antibodies in high density are applied to the first surface areas of the plastic plate (solid) and immobilized. The plastic plate is connected after immobilization of the antibodies to a second plastic plate with a channel structure (channel plate) so that via its channel structure from the outside liquids can be routed over the first surface areas. For detection of antigens in the sample liquids, to do this the sample (for example, cell lysate) is routed via the inlet and the channel structure into a reaction chamber 4 and its first surface areas. After a defined time interval the sample is removed from the reaction chamber by applying a washing solution. The bound antigen can be detected by supplying a suitable indicator solution.
Example 4
Enzymatic Determination of Infectious Diseases in Urine Samples
[0075] The individual first surface areas (spots) within the reaction chamber contains reagents for enzymatic detection of leukocytes, nitrite, albumin, occult blood and creatinine. In the presence of the corresponding analysis targets in the liquid sample a color change takes place in the test areas and it can be analyzed as in a test strip with the naked eye and color scale or with photometric tests.
Example 5
Determination of Chorion Gonadotropin (hCG) in Urine (Sandwich Immunoassay)
[0076] A defined amount of a urine sample is placed with a pipette in the inlet of the device, from where it flows via capillary action into a central channel and in doing so in a resuspension area of a reaction chamber with a dried up, stain-marked antibody against hCG which is present in the first surface area absorbs and dissolves. hCG present in the urine sample binds to the hCG antibodies which are dissolved in the urine sample.
[0077] The hCG-bound antibodies and unbound antibodies flow by capillary force farther into one test area of the reaction chamber. In the test area there are likewise first surface areas. These first surface areas contain immobilized hCG antibodies of the second type which are specific to another epitope of the hCG hormone and cannot be resuspended. They bind to the possibly present hCG to which the first antibodies have already been bound. This yields a fixed, sandwich-like molecule complex.
[0078] Via a washing stage the unbound antibodies present in the first reaction chamber are removed and the bonding, or the detection of hCG, is ascertained via color formation. The presence of hCG in the sample can be detected for example qualitatively with the naked eye via coloring of the test area.
Example 6
Determination of Glucose in Blood Plasma
[0079] Chemiluminometric determination of glucose in plasma is described below, glucose being enzymatically converted via glucose oxidase catalytically into gluconic acid. The hydrogen peroxide which is formed here among others reacts in the presence of a peroxidase in a light-producing reaction with luminol. In doing so luminol is oxidized to 3-aminophthalate, light in the blue wavelength range (425 nm) being emitted. The intensity of the emitted light is proportional here to the glucose concentration and can be measured via conventional photosensitive sensors such as photomultipliers or photodiodes.
[0080] The reagent or the reagents are present in dried form in the first surface areas in the resuspension area of the device. For this purpose, the first surface areas of the device are pretreated accordingly. Conventionally, via dispenser technology the complex-forming reagent is applied in liquid form to the surface of the resuspension area and then dried. To do this, pipette stations or standard laboratory robots (for example Biomek from Beckman Coulter) can be used which allow pipetting of extremely small volumes in the microliter range. The first surface areas are made such that the applied liquid wets exclusively the first surface areas and does not flow on the surrounding second surface area into the bordering channels or cavities. In this example as the reagent 1 μl of a mixture of glucose oxidase (100 U/μl), microbial peroxidase Arthromyces ramosus (200 U/μl) and luminol (10 mM) in the resuspension area was applied and dried.
[0081] After sealing or covering the resuspension area which comprises the structured first surface area with, for example, an adhesive film the device is serviceable and can be filled with the corresponding sample. It is also possible here to apply the reagent as a solid, for example lyophilizate, powder, pellet, tablet, plastic particle (beads) etc. into the cavities which are provided for this purpose on the chip.
[0082] As a sample 2 μl K 2 EDTA blood or blood plasma were dispensed with a pipette into the inlet of the device from where the blood sample is transported via capillary forces into a transport channel, through the resuspension area and from there into an incubation section. While the sample is flowing through the resuspension area the dry chemical is partially dissolved and mixed with the sample. The incubation section is used to set a reaction time which is predefined in terms of time between the chemical and the sample. The reaction time is the time interval which the sample needs to flow completely through the incubation area. The reaction time can be precisely set over the capillary cross section of the incubation area and its surface properties. The sample which has been pretreated in this way finally flows into a collecting channel where the resulting light signal is measured by a photomultiplier which rests externally on the transparent cover. | Holding device for the arrangement of at least one optical component in front of a laser light source of a laser unit, including a first holding part to which at least one optical component is attached, the holding device furthermore including a second holding part which is attached to one part of the laser unit, and the first holding part being attached to the second holding part. Furthermore this invention relates to an arrangement with such a holding device and a process for producing this arrangement. | 1 |
[0001] This application claims the benefit of U.S. Provisional Application No. 60/795,041, filed on Apr. 25, 2006, which is hereby incorporated by reference.
BACKGROUND OF THE INVENTION
[0002] 1. Field of the Invention
[0003] The present invention relates to a method of transmitting data, and more particularly, to a method of transmitting data by utilizing resources in hybrid automatic request operations.
[0004] 2. Discussion of the Related Art
[0005] In the world of cellular telecommunications, those skilled in the art often use the terms 1G, 2G, and 3G. The terms refer to the generation of the cellular technology used. 1G refers to the first generation, 2G to the second generation, and 3G to the third generation.
[0006] 1G refers to the analog phone system, known as an AMPS (Advanced Mobile Phone Service) phone systems. 2G is commonly used to refer to the digital cellular systems that are prevalent throughout the world, and include CDMAOne, Global System for Mobile communications (GSM), and Time Division Multiple Access (TDMA). 2G systems can support a greater number of users in a dense area than can 1G systems.
[0007] 3G commonly refers to the digital cellular systems currently being deployed. These 3G communication systems are conceptually similar to each other with some significant differences.
[0008] In a wireless communication system, it is important to devise schemes and techniques that increase the information rate and improve the robustness of a communication system under the harsh conditions of the wireless environment. To combat less-than-ideal communication conditions and/or to improve communication, various methods, including reducing transmission of unnecessary data, can be used to free up resources as well as promote more effective and efficient transmission.
SUMMARY OF THE INVENTION
[0009] Accordingly, the present invention is directed to a method of transmitting data by utilizing resources in hybrid automatic request operations that substantially obviates one or more problems due to limitations and disadvantages of the related art.
[0010] An object of the present invention is to provide a method of transmitting at least one sub-packet in a wireless communication system.
[0011] Another object of the present invention is to provide a method of using resources in various domains for sub-packet transmission.
[0012] Additional advantages, objects, and features of the invention will be set forth in part in the description which follows and in part will become apparent to those having ordinary skill in the art upon examination of the following or may be learned from practice of the invention. The objectives and other advantages of the invention may be realized and attained by the structure particularly pointed out in the written description and claims hereof as well as the appended drawings.
[0013] To achieve these objects and other advantages and in accordance with the purpose of the invention, as embodied and broadly described herein, a method of transmitting at least one sub-packet in a wireless communication system includes transmitting at least one sub-packet based on combination of resources from multiple domains, wherein the combination of resources indicate whether to maintain or change the resource arrangement for subsequent transmission.
[0014] In another aspect of the present invention, a method of using resources in various domains for sub-packet transmission includes combining the resources from the various domains, determining whether each of the various domains indicates adaptation or no adaptation, and transmitting the sub-packets based on combination of the indicated adaptation or no adaptation of each resource.
[0015] It is to be understood that both the foregoing general description and the following detailed description of the present invention are exemplary and explanatory and are intended to provide further explanation of the invention as claimed.
BRIEF DESCRIPTION OF THE DRAWINGS
[0016] The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this application, illustrate embodiment(s) of the invention and together with the description serve to explain the principle of the invention. In the drawings;
[0017] FIG. 1 is an exemplary diagram illustrating transmit diversity combined with antenna selection;
[0018] FIG. 2 is another exemplary diagram illustrating transmit diversity combined with antenna selection;
[0019] FIG. 3 is an exemplary diagram illustrating antenna selection and frequency allocation; and
[0020] FIG. 4 is another exemplary diagram illustrating antenna selection and frequency allocation.
DETAILED DESCRIPTION OF THE INVENTION
[0021] Reference will now be made in detail to the preferred embodiments of the present invention, examples of which are illustrated in the accompanying drawings. Wherever possible, the same reference numbers will be used throughout the drawings to refer to the same or like parts.
[0022] A hybrid automatic request (H-ARQ) is a physical layer error control technique providing increased throughput by introducing less interference to the system and compensating inaccuracy presented, for example, in power control. In addition, the increased peak data transmission rate can be achieved by early termination. Encoded packet is divided into multiple sub-packets. Each sub-packet carries incremental redundant information on uncoded packet. H-ARQ can be classified as synchronous and asynchronous ones based on the timing of retransmissions and adaptive and non-adaptive ones based on the change of the parameters, e.g., modulation order, in each transmission.
[0023] In implementing the H-ARQ operations, all of the available resources are not jointly used which in turn limits the system capacity. Hence, discussions are made hereinafter to discuss ways to further increase the system capacity.
[0024] The available resources for the H-ARQ operations can be defined in various domains including time, frequency, space, modulation, power, and code domains. These various domain resources can be used for sub-packet transmission.
[0025] More specifically, transmission time and duration of each sub-packet can be maintained (synchronous) or changed/varied (asynchronous). If the number of retransmissions exceeds the maximum number of allowable retransmissions, the packet can be retransmitted. For example, the maximum number of retransmissions can be set to six (6) times.
[0026] Further, in multi-carrier operation (e.g., orthogonal frequency division multiplexing (OFDM)), the number or set of sub-carriers used for the transmission of each sub-packet can be maintained or changed. Similarly, the number of antenna element involved in the transmission of each sub-packet can be maintained (synchronous) or changed (asynchronous). Moreover, the modulation order used in the transmission of each sub-packet can be maintained or changed.
[0027] In addition, the power allocated to the transmission of each sub-packet can be maintained or changed. Lastly, the number of codes for each sub-packet can be maintained or changed.
[0028] Regarding changes and maintenance of various resources associated with different domains can be described in more detail with respect to Table 1. As discussed, the same resources can be used or different/varied resources can be used with respective to each domain.
[0029] Table 1 illustrates various H-ARQ operations that can be obtained by combining resources in various domains.
Synchronous or Asynchronous Frequency Space Modulation Power Code 0 0 0 0 0 0 0 0 0 1 0 0 0 1 0 0 0 0 1 1 0 0 1 0 0 0 0 1 0 1 0 0 1 1 0 0 0 1 1 1 0 1 0 0 0 0 1 0 0 1 0 1 0 1 0 0 1 0 1 1 0 1 1 0 0 0 1 1 0 1 0 1 1 1 0 0 1 1 1 1 1 0 0 0 0 1 0 0 0 1 1 0 0 1 0 1 0 0 1 1 1 0 1 0 0 1 0 1 0 1 1 0 1 1 0 1 0 1 1 1 1 1 0 0 0 1 1 0 0 1 1 1 0 1 0 1 1 0 1 1 1 1 1 0 0 1 1 1 0 1 1 1 1 1 0 1 1 1 1 1
[0030] Referring to Table 1, ‘0’ and ‘1’ mean ‘no change’ and ‘change,’ respectively, in the transmission of sub-packets. Here, ‘no change’ means that the same resources are used for each sub-packet transmission where as ‘change’ means that different resources are used. More specifically, ‘change’ also means that the resources can be increased or decreased. Furthermore, change and no change can also be referred to as adaptation or variation and no adaptation or no variation.
[0031] Moreover, ‘change’ in various domains can be with respective to time (e.g., synchronous or asynchronous), frequency in which the number of subcarriers in the transmission of subsequent sub-packets can be increased or decreased), space in which the number of antenna elements involved in the transmission of subsequent sub-packets can be increased or decreased, modulation in which the modulation order used in the transmission of subsequent sub-packets can be increased or decreased, power in which the power allocated to the transmission of subsequent sub-packets can be increased or decreased; and code in which the number of codes assigned to the transmission of each sub-packet can be increased or decreased.
[0032] With respect to the frequency domain, ‘0’ denotes that the same frequency resource may be used for all sub-packet transmissions. Alternatively, ‘1’ means that frequency resource used in each or subset of sub-packet transmission(s) may be different. That is, it can be increased or decreased. For example, in OFDM transmission, the first sub-packet may be transmitted using 50 sub-carriers and the second to the last sub-packet may be transmitted using 25 (decreased) sub-carriers or 75 (increased) sub-carriers.
[0033] With respect to the space domain, ‘0’ means that the same space resource may be used for all sub-packet transmissions. Alternatively, ‘1’ means that space resource used in each or subset of sub-packet transmission (s) may be different. That is, it can be increased or decreased. For example, in antenna selection case, the first sub-packet may be transmitted using the antenna(s) selected from four (4) antennas and the second to the last sub-packet may be transmitted using an antenna selected from 2 antennas.
[0034] Further, consider the case where each or subset of sub-packet(s) is transmitted using different set of antennas selected from the same set of antennas. This example can be applicable to beamforming and cyclic delay diversity cases. Each or subset of sub-packet(s) may be transmitted using different beam shape. First sub-packet may be transmitted using narrow beam (beneficial if the 1 st sub-packet carries systematic bits in Turbo Code) and the second to the last sub-packet may be transmitted using wider beam.
[0035] In addition, each or subset of sub-packet(s) may be transmitted using different number of cyclic diversity. First sub-packet may be transmitted using three (3) antenna cyclic diversity and the second to the last sub-packet may be transmitted using two (2) antenna cyclic diversity.
[0036] FIG. 1 is an exemplary diagram illustrating transmit diversity combined with antenna selection. Referring to FIG. 1 , data stream is encoded based on feedback information provided from the receiving side. More specifically, based on the feedback information, the data is processed using an adaptive modulation and coding (AMC) scheme at the transmitting end. The data processed according to the AMC scheme is channel coded, interleaved, and then modulated into symbols (which can also be referred to as coded or modulated data stream).
[0037] The symbols are then demultiplexed to multiple STC encoder blocks. Here, demultiplexing is based on the code rate and modulation that the carrier can support. Each STC encoder block encodes the symbols and outputs to encoded symbols to inverse fast Fourier transform (IFFT) block(s). The IFFT block transforms the encoded symbols. The transformed symbols are then assigned to antennas selected by antenna selector(s) for transmission to the receiving end. The selection as to which antenna to be used for transmission can be based on the feedback information.
[0038] FIG. 2 is another exemplary diagram illustrating transmit diversity combined with antenna selection. Different from FIG. 1 which is designed for a single codeword (SWC) operation, in FIG. 2 , adaptive modulation and coding is performed per carrier basis and is designed for a multiple codeword (MWC) operation.
[0039] According to FIGS. 1 and 2 , the data is processed by the STC encoders before being processed by the IFFT block(s). However, it is possible for the data to be processed by the IFFT block before being processed by the STC encoder blocks. In short, the processing order between the STC encoders and the IFFT blocks can be switched.
[0040] In detail, the feedback information from the receiving end can be used in performing channel coding and modulation (or in executing the AMC scheme) to the data stream. This AMC scheme process is illustrated in a dotted box. The feedback information used in channel coding and modulation can be a data rate control (DRC) or a channel quality indicator (CQI), for example. Further, the feedback information can include various information such as sector identification, carrier/frequency index, antenna index, supportable CQI value, best antenna combination, selected antennas, and a supportable signal-to-interference noise ratio (SINR) for a given assigned multi-carriers.
[0041] The information related to selected antennas as well as its supportable SINR can be transmitted through a channel from the receiving end to the transmitting end (e.g., reverse link) or on a different channel. Such a channel can be a physical channel or a logical channel. Further, the information related to the selected antennas can be transmitted in a form of a bitmap. The position of each bitmap represents the antenna index.
[0042] The DRC or the CQI, for example, can be measured per transmit antenna. As an example of the CQI, a transmitting end can send signal (e.g., pilot) to a receiving end to determine the quality of the channel(s) through which the signal was sent. Each antenna transmits its own pilot for the receiving end to extract the channel information from the antenna element to the receiving end. The transmitting end can also be referred to as an access node, base station, network, or Node B. Moreover, the receiving end can also be referred to as an access terminal, mobile terminal, mobile station, or mobile terminal station. In response to the signal from the transmitting end, the receiving end can send to the transmitting end the CQI to provide the channel status or channel condition of the channel through which the signal was sent.
[0043] Furthermore, the feedback information (e.g., DRC or CQI) can be measured using a pre-detection scheme or a post-detection scheme. The pre-detection scheme includes inserting antenna-specific known pilot sequence before an orthogonal frequency division multiplexing (OFDM) block using a time division multiplexing (TDM). The post-detection scheme involves using antenna-specific known pilot pattern in OFDM transmission.
[0044] Further, the feedback information is based on each bandwidth or put differently, the feedback information includes the channel status information on each of N number of 1.25 MHz, 5 MHz, or a sub-band of OFDM bandwidth.
[0045] As discussed, the symbols processed using the AMC scheme are demultiplexed to multiple STC encoder blocks. The STC encoder blocks can implement various types of coding techniques. For example, the encoder block can be a STC encoder. Each STC encoder can have a basic unit of MHz. In fact, in FIG. 1 , the STC encoder covers 1.25 MHz. Other types of coding techniques include space-time block code (STBC), non-orthogonal STBC (NO-STBC), space-time Trellis coding (STTC), space-frequency block code (SFBC), space-time frequency block code (STFBC), cyclic shift diversity, cyclic delay diversity (CDD), Alamouti, and precoding.
[0046] As discussed, the IFFT transformed symbols are assigned to specific antenna(s) by the antenna selectors based on the feedback information. That is, in FIG. 1 , the antenna selector chooses the pair of antenna corresponding to two outputs from the STC encoder specified in the feedback information.
[0047] The antenna selectors select the antennas for transmitting specific symbols. At the same time, the antenna selector can choose the carrier (or frequency bandwidth) through which the symbols are transmitted. The antenna selection as well as frequency selection is based on the feedback information which is provided per each bandwidth of operation. Furthermore, the wireless system in which antenna and frequency allocation is made can be a multi input, multi output (MIMO) system.
[0048] FIG. 3 is an exemplary diagram illustrating antenna selection and frequency allocation. Referring to FIG. 3 , there are four (4) frequency bandwidths or carriers and three (3) antennas. Here, the symbols processed through Alamouti encoder Block # 0 are assigned to antennas by the antenna selectors. The symbols from Block # 0 are assigned to a first antenna on frequency 0 (f 0 ) from a first of two antenna selectors. At the same time, the other symbols of Block # 0 are assigned to a third antenna on frequency on frequency 0 (f 0 ) from the other antenna selector. Moreover, the symbols from Block # 3 are assigned to a second antenna on frequency 3 (f 3 ) from a first of two antenna selectors. At the same time, the other symbols of Block # 3 are assigned to a third antenna on frequency on frequency 3 (f 3 ) from the other antenna selector. With respect to frequency allocation, frequency allocation is maintained for at least two consecutive OFDM symbol intervals.
[0049] Similarly, FIG. 4 is another exemplary diagram illustrating antenna selection and frequency allocation. In FIGS. 3 and 4 , the data symbols from each block are assigned to different antennas so as to achieve diversity gain.
[0050] In general case, each or subset of sub-packet(s) transmission may utilize different antenna technologies. For example, first sub-packet may be transmitted using beamforming and second to the last sub-packet may be transmitted using space time transmit diversity (STTD), antenna selection, or single input single output (SISO), among others.
[0051] The order of using antenna technologies is arbitrary. For example, antenna selection from increasing number of antenna elements as the sub-packet transmission increases may be used. First sub-packet may be transmitted using an antenna selected from two (2) antennas, and second to the last sub-packet may be transmitted using the antenna(s) selected from four (4) antennas.
[0052] With respect to the modulation domain, ‘0 means that the same modulation scheme is used for all sub-packet transmissions. Alternatively, ‘1’ means that the modulation scheme used in each or subset of sub-packet transmission(s) may be different. That is, modulation order can be increased or decreased. For example, in modulation step-down, first sub-packet is transmitted using 16 quadrature amplitude modulation (16-QAM) scheme and the second to the last sub-packet is transmitted using 8 phase shift keying (PSK), quadrature PSK (QPSK), or binary PSK (BPSK), among others. In modulation step-up, lower order modulation may be used in the 1 st sub-packet transmission and higher order modulation may be used in subsequent sub-packet transmissions.
[0053] With respect to the power domain, ‘0’ means that the same power may be used for all sub-packet transmissions. Alternatively, ‘1’ means that the power used in each or subset of sub-packet transmission(s) is different. That is, it may be increased or decreased, For example, in energy (or power) reduction, first sub-packet may be transmitted using higher energy (or power) and the second to the last sub-packet is transmitted using lower energy (or power). In energy (or power) increase, lower power may be used in the first sub-packet transmission and higher power may be used in subsequent sub-packet transmissions.
[0054] With respect to the code domain, ‘0’ means that the same number and code (spreading) may be used for all sub-packet transmissions. Alternatively, ‘1’ means that the number and code used in each or subset of sub-packet transmission(s) may be different. That is, it may be increased or decreased.
[0055] For example, first sub-packet may be transmitted using larger number of codes and the second to the last sub-packet is transmitted using less number of spreading codes. Here, the number of codes assigned to the transmission of each sub-packet can be one (1) bit for the first transmission, then increased to 10 bits for the second transmission, and then decreased to two (2) bits for the third transmission, and so on. This illustrates how the number of codes used in the transmission can be increased and/or decreased.
[0056] In reverse case, less number of codes may be used in the first sub-packet transmission and larger number of codes may be used in subsequent sub-packet transmissions. This can be applicable to code division multiple access (CDMA) and multi-carrier CDMA (MC-CDMA).
[0057] Referring to Table 1, by way of an example, row # 2 (whose domains are all indicated by ‘0’s except for code domain indicated by ‘1’) would increase or decrease the number of codes used in transmission of each subset or sub-packet. Moreover, the last row indicates that all the domains would need to increase or decrease. In a similar manner, each row can be interpreted.
[0058] The resource allocation in H-ARQ can be maintained or changed throughout the retransmission (e.g., resources in various domains can be adaptively allocated throughout H-ARQ operation). Channel quality feedback from the receiver can be used to select the resource allocation adaptively. Selection of the resources per transmission can be informed to the receiver using control or overhead channel.
[0059] The discussion of above can be used in systems such as an ultra mobile broadband (B) system.
[0060] It will be apparent to those skilled in the art that various modifications and variations can be made in the present invention without departing from the spirit or scope of the inventions. Thus, it is intended that the present invention covers the modifications and variations of this invention provided they come within the scope of the appended claims and their equivalents. | A method of transmitting at least one sub-packet in a wireless communication system is disclosed. More specifically, the method includes transmitting at least one sub-packet based on combination of resources from multiple domains, wherein the combination of resources indicate whether to maintain or change the resource arrangement for subsequent transmission. | 7 |
BACKGROUND OF THE INVENTION
1. Field of the Art
This invention relates to a novel substance, more particularly a novel physiologically active substance, MH435, having antitumor activity and antimicrobial activity.
A considerable number of substances have already been put to practical use as antitumor agents and antimicrobial agents, but they are not always satisfactory in pharmaceutical activity and/or the matter of side effect. Thus, there still remains a need for improved novel antitumor agents and antimicrobial agents.
2. Prior Art
Bishop, J. M. has reported that a product of certain cancer genes has a tyrosine specific protein kinase activity [Ann. Rev. Biochem., 52, 301-354 (1983)]. Cohen et al. have described in their report that the tyrosine specific protein kinase has a role as a signal substance in the processes of cell proliferation owing to many cell growth factors [J. Biol. Chem., 257, 1523-1531 (1982)].
SUMMARY OF THE INVENTION
With these results in view, we have screened a variety of substances in natural occurrence for the purpose of finding inhibitors of the tyrosine specific protein kinase activity. As a result of the screening, we have found that these inhibitors have antitumor activity and antimicrobial activity.
The novel physiologically active substance according to this invention is represented by the formula: ##STR2## wherein R represents either of the following groups A and B A: --CH═CH--NHCHO
B: --CH 2 --CH 2 --NHCHO.
DETAILED DESCRIPTION OF THE INVENTION
Novel Physiologically Active Substance MH435
1. Chemical Structure
The substance MH435 has a chemical structure represented by the formula (I) set forth above.
Depending on the type of the substituent R, the substance MH435 includes two species, viz. MH435-A and MH435-B.
2. Physicochemical Properties
The physical properties of the substance MH435 are set forth in the following Table 1.
TABLE 1__________________________________________________________________________ MH435-A MH435-B__________________________________________________________________________Melting point 78-82° C.Molecular weight 179 181Molecular formula C.sub.9 H.sub.9 O.sub.3 N C.sub.9 H.sub.11 O.sub.3 NElementary analysis C H O C H OFound: 60.3 5.1 26.8 59.7 6.1 26.5Calculated: 60.3 5.1 26.8 59.7 6.1 26.5UV and visible absorption spectrum 330,275,208 295,235(λ.sub.max,nm)IR absorption spectrum 1650, 1540, 1510, 1400, 1320, 1260, 1200, 1650, 1510, 1460, 1380, 1200, 820(K Br tab.; cm.sup.-1) 960, 820, 780NMR spectrum (.sup.1 H-NMR;δ) 6.45(d), 6.50(dd), 6.68(d), 6.72(d), 2.77(t), 3.50(t), 6.58(dd), 6.68(d), 6.80(d), 7.70(s), 8.00(s), 8.15(s), 6.70(s), 7.78(s), 8.00(s), 8.25(s), 9.28(s) 8.40(s)Rf values*.sup.1 0.36(Chloroform:Methanol = 10:2) 0.36(Chloroform:Methanol = 10:2) 0.24(Toluene:Acetone = 1:1) 0.12(Toluene:Acetone = 1:1)Appearance Pale yellow Pale yellow__________________________________________________________________________ *.sup.1 measured with "KIESELGEL 60" manufactured by Merck & Co.
Preparation of MH435
1. Summary
MH435 is currently prepared only by the cultivation of a microorganism (for MH435-A) and by the synthetic chemical modification of the cultivation product of MH435-A (for MH435-B). It may also be prepared by other processes, for example, total synthesis by a chemical method.
As the microbial strain used for the process by the cultivation of a microorganism, strains of the genus Streptomyces having MH435-A-producing capability are used. Specifically, we have shown that the MH435-hF3 strain we have isolated, which will be described in more detail hereinbelow, produces MH435-A. It is possible to isolate other strains which are suitable for producing the substance from natural sources by the conventional method of isolating antibiotic-producing microorganisms. It is also possible to increase the MH435-A-producing capacity by subjecting the MH435-A-producing microorganisms including the MH435-hF3 strain to mutation treatment such as irradiation by a high energy ray such as UV. Furthermore, it may also be possible to derive the MH435-A-producing microorganisms by subjecting the gene DNA which carries genetic informations with respect to the production of MH435-A to recombinant DNA techniques such as transformation and cell fusion.
2. Strain MH435-hF3
The strain MH435-hF3 that we have found as a strain of the genus Streptomyces having the MH435-A-producing capacity will now be described.
(A) Source and accession number
The strain MH435-hF3 is an actinomycete which was isolated from the soil in the grounds of the Institute of Microbiological Chemistry, Japan, in November, 1984. It was deposited with the Fermentation Research Institute, Agency of Industrial Science and Technology, Japan, on May 21, 1985 and was assigned an accession number: FERM P-8246. This strain now bears the accession number FERM BP-1082 under the terms of the Budapest Treaty on the International Recognition of the Deposit of Microorganisms for the Purposes of Patent Procedure. This depository fully complies with the rules of the Budapest Treaty. Specifically, it fully complies with Rule 11.3 of the Budapest Treaty whereby the organism is available to the public on patent grant and with Rule 9 of the Budapest Treaty which requires the maintenance of the organism for a period of at least 30 years after the date of deposit.
(B) Microbiological properties of the strain MH435-hF3
(1) Morphology
The strain MH435-hF3 under microscopic observation extends aerial mycelia having spiral hyphae from branched substrate mycelia with no verticil branch. Chains of 10 or more spores in matured spore chains, wherein the size of the spores is in the range of about 0.6-0.8×1.0-1.2 μ, are observed. The spores have projections in the form of relatively long prickles.
(2) Cultural Characteristics
Information will be given below, in which the description of color in parentheses is carried out in accordance with the Color Harmony Manual of the Container Corporation of America.
(i) Sucrose-nitrate agar (incubated at 27° C.)
On colorless growth, yellowish brown (2 ni, Mustard Brown) to brownish gray (2 li Covert Brown) aerial mycelium develops. No soluble pigment.
(ii) Glucose-asparagine agar (incubated at 27° C.)
On pale yellow growth, light olive gray to olive gray (11/2 ig, Olive Gray--11/2 li Lt Olive Drab--2 li Covert Brown) aerial mycelium develops. No soluble pigment.
(iii) Glycerol-asparagine agar
(ISP medium No. 5, incubated at 27° C.)
On pale yellowish brown (2 le, Mustard--3 pg, Golden Brown) growth, light gray to light olive gray (1 fe, Griege--11/2 ge, Lt Olive Gray) aerial mycelium develops. The soluble pigment is tinged with yellowish brown.
(iv) Starch-inorganic salt agar (ISP medium No. 4, incubated at 27° C.)
On colorless growth, grayish olive (2 ni, Mustard Brown) aerial mycelium develops. The soluble pigment is slightly tinged with brown.
(v) Tyrosine agar (ISP medium No. 7, incubated at 27° C.)
On pale yellowish brown (2 gc, Bamboo--2 le, Mustard) to yellowish brown (3 ng, Yellow Maple) growth, brownish white to light olive gray (1 ge, Citron Gray--11/2 ge, Lt Olive Gray--11/2 ig, Olive Gray) aerial mycelium develops. The soluble pigment is tinged with yellowish brown.
(vi) Nutrient agar (incubated at 27° C.)
Growth is tinged with pale yellowish brown (2 gc, Bamboo) with no aerial mycelium. No soluble pigment.
(vii) Yeast-malt agar (ISP medium No. 2, incubated at 27° C.)
On pale yellowish brown (3 le, Cinnamon--3 pg, Golden Brown) growth, light olive gray (11/2 lg, Golden Olive) to olive gray (11/2 ni, Olive) aerial mycelium develops. The soluble pigment is slightly tinged with brown.
(Viii) Oatmeal agar (ISP medium No. 3, incubated at 27° C.)
On colorless to pale yellow growth, aerial mycelium develops. The soluble pigment is slightly tinged with brown.
(ix) Glycerol-nitrate agar (incubated at 27° C.)
Growth is tinged with pale yellow (2 gc, Bamboo). No aerial mycelium develops or white aerial mycelium develops scantily. The soluble pigment is slightly tinged with brown.
(x) Starch agar (incubated at 27° C.)
On colorless growth, yellowish brown aerial mycelium develops. No soluble pigment.
(xi) Calcium malate agar (incubated at 27° C.)
Growth is tinged with pale yellowish brown (2 ge, Bamboo). No aerial mycelium develops or light olive gray aerial mycelium develops scantily. No soluble pigment.
(xii) Cellulose (incubated at 27° C.)
Growth is colorless, and light olive gray aerial mycelium develops scantily. No soluble pigment.
(xiii) Gelatin stab culture medium
In simple gelatin medium (cultured at 20° C.), growth is colorless or tinged with pale yellow. No aerial mycelium develops, nor is produced soluble pigment. In glucose-peptone-gelatin medium (incubated at 27° C.), growth is tinged with pale yellow. No aerial mycelium develops, nor is produced soluble pigment.
(xiv) Skimmed milk (incubated at 27° C. and 37° C.)
On incubation at 27° C., white aerial mycelium slightly develops on pale yellow growth, and no soluble pigment is produced. On incubation at 37° C., growth is rather poor and tinged with pale yellow. No aerial mycelium develops, nor is produced soluble pigment.
(3) Physiological Properties
(i) Growth temperature range
When tests were carried out at temperatures of 20° C., 24° C., 27° C., 30° C., 37° C. and 50° C. using the starch-inorganic salt agar medium (ISP medium No. 4), growth was observed at all these temperatures, except at 50° C., among which the optimum temperature is presumably around 30° C.
(ii) Liquefaction of gelatin (15% simple gelatin: incubated at 20° C.; and glucose-peptone-gelatin: incubated at 27° C.)
Liquefaction begins after ca. 4 days of incubation on the simple gelatin medium, while it begins after ca. 3 days of incubation on the glucose-peptone-gelatin medium. The liquefactive strength is moderate to strong.
(iii) Hydrolysis of starch (Starch-inorganic salt agar medium and starch agar medium)
Negative on either medium.
(iv) Coagulation and peptonization of skimmed milk (skimmed milk, incubated at 27° C. and 37° C.)
Peptonization begins without coagulation after ca. 10 days of incubation at 27° C., and the strength is moderate to strong. On the other hand, peptonization begins after ca. 14 days of incubation at 37° C. in which growth is rather poor, and the strength is moderate to weak.
(v) Production of melanoid pigment (tryptone-yeast extract broth, ISP medium No. 1: peptone-yeast extract-iron agar, ISP medium No. 6: tyrosine agar, ISP medium No. 7, each incubated at 27° C.)
Negative on any of the media.
(vi) Utilization of carbon sources (Pridham-Gottlieb agar medium, ISP medium No. 9; incubated at 27° C.)
Glucose, raffinose and D-mannitol are utilizable for growth and L-arabinose is probably utilizable, but sucrose and rhamnose are not utilizable. It is questionable whether D-xylose, D-fructose and inositol are utilizable or not.
(vii) Dissolution of calcium malate (calcium malate agar, incubated at 27° C.)
Calcium malate is dissolved around the periphery of growth after ca. 7 days of cultivation. The dissolving action is moderate to strong.
(ix) Nitrate reduction (0.1% potassium nitrate-containing peptone water, ISP medium No. 8; incubated at 27° C.)
Negative or positive depending upon the case in repeated tests.
To sum up the above described properties, no sporangium is observed in the strain MH435-hF3. The aerial mycelium is spiral in configuration with no verticil branch. The surface of the spore is covered with prickles. On various culture media, the growths are colorless to pale yellow or pale yellowish brown, and the aerial mycelia are light olive gray to olive gray or yellowish brown. The soluble pigment is slightly tinged with brown to yellowish brown. Production of a melanoid pigment is negative, and hydrolysis of starch is not observed. The proteolytic ability is moderate to strong.
The 2,6-diaminopimelic acid contained in the whole bacterial cell of the strain is of the LL-type. In view of this feature together with the aforementioned features, it is apparent that the strain MH435-hF3 belongs to the genus Streptomyces.
On searching for known strains similar to the strain MH435-hF3 based on these features, this strain has been found to be close to the following three strains:
Streptomyces viridosporus [lit.: International Journal of Systematic Bacteriology, 22, 371 (1972) (lit. 1), and UKP No. 712,547 (lit. 2)],
Streptomyces viridodiastaticus [lit.: ibid., 19, 500 (1969); ibid., 30, 405 (1980)] and
Streptomyces mitakaensis [lit.: The Journal of Antibiotics, Series A, 11, 14 (1958)].
Streptomyces viridodiastaticus (IMC S-0350 [ISP5249]) and Streptomyces mitakaensis (IMCS-0508 [NIHJ77]) are very close to each other, but these two strains were clearly distinguished from the strain MH435-hF3 by comparison tests with respect to their microscopic observations, particularly aerial mycelium formation and spiral formation at the head thereof, colors of aerial mycelia, peptonization of milk, etc. The results of comparison tests of the strain MH435-hF3 with the remaining Streptomyces viridosporus are shown in Table 2 below.
TABLE 2______________________________________ Streptomyces viridosporus, IMCS-0696 MH435-hF3 (ISP5243)______________________________________Formation of verticil - -branchSpiral formation + +Surface of Spore prickly prickly, prickly to hairy*.sup.2Color of aerial mycelium light olive gray to light olive gray to olive gray olive grayColor of growth colorless to pale pale yellow to yellow, pale pale yellowish yellowish brown brownSoluble pigment -to pale brown -Formation of melanoidpigmentISP medium No. 1 - -ISP medium No. 6 - -ISP medium No. 7 - -Hydrolysis of starch - +Coagulation of milk - -Peptonization of milk + + (+*.sup.3)Liquefaction of gelatin (+*.sup.3)Simple gelatin + +Glucose-peptone-gelatin + + weakNitrate reduction - or + -Utilization of carbon sources*.sup.1Glucose + +L-Arabinose (+) +D-Xylose ± +D-Fructose ± +Sucrose - -Inositol ± +Rhamnose - +Raffinose + -D-Mannitol + +______________________________________ *.sup.1 +: positive utilization; (+): probable utilization; ±: questionable utilization; -: no utilization. *.sup.2 the aforementioned lit. 1. *.sup.3 the aforementioned lit. 2.
As is apparent from Table 2, the strain MH435-hF3 and Streptomyces viridosporus are different in hydrolysis of starch and utilization of carbon sources (raffinose and rhamnose). Furthermore, according to the description in the literature, there is some difference in the surface structures of the spores. However, when the surface structures of the two strains are observed, the projections on the spore surface of Streptomyces viridosporus are thicker at their bases and may be properly defined as being like elongated prickles rather than hair. The strain MH435-hF3 has also projections in the form of elongated prickles. Therefore, these surface structures can hardly be considered distinct from each other. Moreover, the other properties of the two strains are very similar to each other, and coincide with each other, particularly in respect of the microscopic observation that the aerial mycelia are light olive gray to olive gray and of the peptonization of skimmed milk without coagulation.
From these results, the strain MH435-hF3 is of a species closest to Streptomyces viridosporus, but they can hardly be regarded as falling under the same species. Therefore, the strain MH435-hF3 is designated as Streptomyces sp. MH435-hF3.
3. Cultivation/Production of MH435-A
The substance MH435-A can be produced by incubating an MH435-A-producing Streptomyces strain aerobically in a suitable medium and separating the objective substance from the culture.
The culture medium may be one containing any nutrient sources which can be utilized by MH435-A-producing microorganisms. For example, glycerol, glucose, sucrose, maltose, dextrin, starch, fats and oils are useful as carbon sources. As nitrogen sources, organic materials such as soybean meal, cotton seed meal, meat extract, peptone, dry yeast, yeast extract and corn steep liquor, and inorganic materials such as ammonium salts or nitrates, for example, ammonium nitrate, sodium nitrate and ammonium chloride can be used. If necessary, inorganic salts such as sodium chloride, potassium chloride, phosphates, heavy metal salts can also be added. For the purpose of suppressing foaming during fermentation, it is also possible to add an appropriate anti-foaming agent such as silicone or soybean oil in accordance with customary methods.
The most suitable cultivation method is submerged aerobic liquid culture which is employed usually for producing antibiotics. The suitable cultivation temperature is in the range of 20-35° C., preferably 25-30° C. When this method is used, the production output of the substance MH435-A reaches a maximum after 2 to 4 days of either shake culture or aerated stirring culture.
Thus, there can be obtained a cultured broth in which the substance MH435-A is accumulated. In the cultured broth, the substance MH435-A is present partly within the mycelium, but most part thereof is present in the supernatant of the cultured broth.
In order to recover the substance MH435-A from the cultured broth, it is possible to employ any methods suitable for the recovery. One of the methods is based on extraction. For example, the substance MH435-A in the supernatant can be recovered by extraction with a water-immiscible solvent such as ethyl acetate, butyl acetate or chloroform. The substance MH435-A in the mycelium can be recovered by treating the mycelium with ethyl acetate, chloroform, methanol, ethanol, butanol, acetone or methyl ethyl ketone. It is also possible to subject the cultured broth as such without isolating the mycelium to the aforementioned extraction procedure. It is also possible to subject the mycelium to crushing followed by extraction. Counter-current distribution may be included in the extraction methods.
Another method of recovering the substance MH435-A from the cultured broth is based on adsorption. According to this method, the substance MH435-A-containing liquid material, such as cultured broth filtrate or an extract obtained by the aforementioned extraction procedure, is subjected to column chromatography, liquid chromatography or the like using an appropriate adsorbent such as activated carbon, alumina, silica gel or "DIAION HP20" (manufactured by Mitsubishi Chemical Industries, Ltd.). The objective substance MH435-A adsorbed onto the adsorbent is then eluted therefrom. The solution of the substance MH435-A thus obtained is concentrated to dryness under reduced pressure to obtain a crude product of the substance MH435-A as a white powder.
The crude MH435-A product thus obtained can be purified by carrying out the aforementioned extraction and adsorption procedures, if necessary, in combination, over a necessary number of times followed by recrystallization, if desired. For example, it is possible to accomplish purification by a combination of column chromatography using an absorbent such as silica gel, "SEPHADEX LH20" or "DIAION HP20" (manufactured by Mitsubishi Chemical Industries, Ltd.) or a gel filter; liquid chromatography using an appropriate solvent; counter-current distribution; and thin layer chromatography. Specifically, for instance, the crude powder of the substance MH435-A is dissolved in a small amount of chloroform and the solution is applied to a silica gel column which is developed with an appropriate solvent to elute the active components individually. The aimed active fractions are combined together and concentrated under reduced pressure. The concentrate is further subjected to thin layer chromatography, and the desired component is scraped off. Thus the objective substance can be isolated substantially as a single substance. In order to further purify the substance, it is also possible to apply high-performance liquid chromatography or crystallization from an appropriate solvent.
4. Chemical Modification of MH435-A/Production of MH435-B
The substance MH435-B of the present invention can be prepared by adding hydrogen to the substance MH435-A in the presence of a catalyst. The hydrogen addition reaction can be carried out by any methods suitable for the purpose, for example, by dissolving the substance MH435-A in methanol, adding platinum oxide to the solution and then reacting the mixture with hydrogen. The isolation and purification of the substance MH435-B thus obtained can be carried out, for example, by chromatography using silica gel or the like in accordance with the aforementioned procedures for the substance MH435-A.
In the above processes of incubation and purification, MH435 was traced by detecting the inhibition activity thereof by measuring the tyrosine specific protein kinase in test samples in accordance with the following method.
[Measurement of tyrosine specific protein kinase activity]
The measurement of tyrosin specific protein kinase activity was carried out by modifying the method of measuring enzyme activity described by G. Carpenter et al. in The Journal of Biological Chemistry, 254, 4874-4891 (1979) using the membrane fraction of human epithelial carcinoma cells A-431 with respect to the tyrosine specific protein kinase in the epidermal growth factor receptor. That is to say, the pre-incubation was carried out with 50 μl of 20 mM HEPES buffer (pH 7.4) containing 1 mM of MnCl 2 , 100 ng of the epidermal growth factor, 40 μg of the A-431 membrane fraction, 7.5 μg of albumin, 3 μg of histone and the substance MH435-A or MH435-B at 0° C. for 10 min. Then, 10 μl of [Y- 32 P]adenosine triphosphate (0.25 mCi/0.125 ml) was added to the mixture and the reaction was carried out at 0° C. for 30 min. A portion of the reaction product (50 μl) was taken out and adsorbed on Whatman filter paper No. 3 MM. The filter paper was dipped in ice-cooled TCA, left standing for 30 min. and taken out for washing with TCA, ethanol and ether. Then, 32 P adsorbed on the filter paper was measured by counting the radioactivity (a). At the same time, count (b) was measured for the reaction product which was obtained by the same reaction and treated in the same manner as above except that the test sample was excluded, while counts (a') and (b') were measured for the reaction products in which the membrane fractions were further excluded, respectively. The inhibitory ratio with respect to the epidermal growth factor receptor kinase was then calculated from the equation
[(a-a')/(b-b')]×100.
Physiological Activity of MH435
The substance MH435 according to this invention has antitumor activity and antimicrobial activity as shown below and is useful as a drug.
1. Inhibitory activity against tyrosine specific protein kinase
The 50% inhibitory concentrations of the substances MH435-A and MH435-B which were measured by the aforementioned method were respectively 0.55 μg/ml and 6.0 μg/ml.
2. Effects on cultured carcinoma cells
The substance MH435-A according to this invention inhibits at a very low concentration the proliferation of the cultured cells such as L1210 leukemia cells, IMC carcinoma cells, or Ki-NRK, ts Src-NRK and A-431 cells. (See Table 3 below.)
TABLE 3______________________________________ IC.sub.50Cultured carcinoma cells (μg/ml)______________________________________L1210 2.41IMC carcinoma 3.01Ki-NRK 1.70ts Src-NRK (at 33° C.) carcinoma form 2.00ts Src-NRK (at 39° C.) normal form 3.60A-431 3.60______________________________________
IC 50 was measured by inoculating the respective cells in dished (3-5×10 4 cells/dish), incubating the cells for 1 day (at 37° C.; CO 2 concentration, 5%), then adding the substance MH435-A, further incubating the resultant mixture for 3 days under the same conditions and finally counting the number of the cells.
3. Acute toxicity (LD 50 )
The LD 50 value of the substance MH435-A according to this invention after a single intraperitoneal administration into a mouse was 200 mg/kg or more.
4. Antimicrobial activity
Minimum inhibitory concentrations (MIC) of the substance against various bacteria determined by the agar dilution method using Muller-Hinton culture medium are shown in the following Table 4.
TABLE 4______________________________________ MIC (μg/ml)Bacteria tested MH435-A MH435-B______________________________________S. aureus 209 P 50 50S. aureus Smith 25 50S. aureus MS8710 50 50S. aureus MS9610 50 50M. lysodelkticus IFO 333 50 50B. Subtilis PCI 219 100 100B. cereus ATCC 10702 100 100Coryn. bovis 1810 100 100E. coli NIHJ 100 100K. pneumoniae PCI 602 100 100Sal. typhi T-63 100 100Serr. marcessens 100 100Prot. vulgaris OX19 100 50Pseu. aeruginosa A3 25 50______________________________________
EXPERIMENTAL EXAMPLES
EXAMPLE 1
One platinum loopful of a slant culture of the strain MH435-hF3, an MH435-A-producing strain, was inoculated into the culture medium preliminarily sterilized at 120° C. for 20 min. and distributed in an amount of 110 ml in 500-ml Erlenmeyer flasks (the medium containing 3% of glycerol, 2% of fish meal and 0.2% of calcium carbonate, pH 7.4). The inoculated medium was subjected to aerobic shake culture at 180 rpm at 27° C. The production output of the substance MH435-A was checked periodically by measuring the anti-epidermal growth factor receptor kinase activity of the culture broth. As the result thereof, it was observed that the concentration of the MH435-A culture broth quantitatively measured in terms of the inhibitory activity against the epidermal growth factor receptor kinase reached a maximum after 4 days of incubation and kept stable during 2 days of further incubation, decreasing gradually thereafter.
EXAMPLE 2
A seed culture broth obtained by the incubation for 48 hours under the same cultural conditions as in Example 1 was inoculated in an amount of 3 ml into the same culture medium as in Example 1 and incubated for 96 hours as above. Five liters of the culture broth thus obtained was subjected to centrifugation to obtain 4.6 liters of a culture filtrate. 4.6 liters of the culture filtrate obtained was extracted with the equivalent volume of butyl acetate and concentrated to dryness under reduced pressure to obtain 360 mg of a crude powder. The crude powder thus obtained was adsorbed in a column packed with 20 g of silica gel "KIESEL GEL 60" (manufactured by Merck & Co., 70-230 mesh) and eluted stepwise with varying mixing ratios of chloroform-methanol. Fractions containing MH435-A were collected and concentrated to dryness under reduced pressure to obtain 110 mg of a crude powder. The epidermal growth factor receptor kinase inhibitory activity (IC 50 ) of the crude powder was 1.6 μg/ml.
The crude powder was dissolved in methanol, adsorbed in a reversed phase column for preparative high performance liquid chromatography packed with "NUCLEOSIL 5 C 18 " (manufactured by M. Nagel Co.) which had been equilibrated with a 20% aqueous methanol solution, and eluted with a 20% aqueous methanol solution at an elution speed of 8 ml/min. The eluate was fractionated into 10 ml aliquots. The active fractions were combined together and concentrated under reduced pressure, extracted with butyl acetate, concentrated again to dryness, dissolved in a small amount of ethyl acetate and crystallized from chloroform to obtain 60.3 mg of crystalline substance MH435-A. The epidermal growth factor receptor kinase inhibitory activity (IC 50 ) of the crystalline MH435-A was 0.55 μg/ml.
EXAMPLE 3
The crystalline substance MH435-A (23.4 mg) obtained in Example 2 was dissolved in 10 ml of methanol and one spatula of platinum oxide was added to the solution. The resulting solution was subjected to reduction treatment for 2 hours under hydrogen stream and then filtered. The filtrate was concentrated under reduced pressure, adsorbed on a thin layer of silica gel (KIESEL GEL 60F 254 " manufactured by Merck & Co.), developed with a 1:1 solvent mixture of toluene and acetone. The separated MH435-B-containing portion was scraped off and eluted with ethyl acetate. The fraction thus obtained was concentrated and passed through a "SEPHADEX LH-20" column of 1.0×40 cm which had been equilibrated with methanol. The column was developed with the same solvent as was used in the thin layer chromatography. The eluate was concentrated to dryness under reduced pressure to obtain 10.1 mg of the substance MH435-B. The epidermal growth factor receptor kinase inhibitory activity (IC 50 ) of the substance MH435-B was 6.0 μg/ml. | Disclosed is a novel physiologically active substance, MH435, represented by the formula: ##STR1## wherein R represents either of the following groups A and B A: --CH═CH--NHCHO
B: --CH 2 --CH 2 --NHCHO.
The substance MH435 has an inhibitory activity against tyrosine specific protein kinase, and the 50% inhibitory concentrations of the substances MH435-A and MH435-B are respectively 0.55 μg/ml and 6.0 μg/ml. | 2 |
STATEMENT REGARDING FEDERALLY SPONSORED RESEARCH OR DEVELOPMENT
The U.S. Government has rights in this invention pursuant to the terms and conditions of Contract No. W-7405-ENG-36 awarded by the U.S. Department of Energy to Los Alamos National Laboratory.
CROSS-REFERENCE TO RELATED APPLICATIONS
Not Applicable.
BACKGROUND OF THE INVENTION
1. Field of the Invention (Technical Field)
The present invention relates to methods to desensitize metastable intermolecular composite materials.
2. Description of Related Art
Metastable Intermolecular Composites (MICs) are materials comprised of nanoscale composite energetic materials, often a metal and an oxidizer. Similar in composition to classical composites, MICs differ in that the individual particle sizes are on the nanometer scale (10 −9 m) instead of millimeter or sub-millimeter (10 −4 m to 10 −3 m). This significant change in spatial scale significantly changes the chemical and mechanical properties, enabling a new set of behaviors. For example, instead of burning at tens of millimeters per second, MICs are capable of combustion velocities of tens of meters per second up to kilometers per second. These differences make these a new class of materials.
These materials have found a variety of possible applications including as electric and percussion igniters or primers. See, for example, U.S. Pat. No. 5,717,159 for percussion primers. However, a significant practical issue limits their widespread and scaled production. This issue is the sensitivity of these nanoscale materials to electrostatic discharge (ESD) and friction. For applications such as lead-free igniters or primers, the sensitivity is needed for the application to work. Specifically, a small hot spot caused by the heating of the bridgewire must be sufficient to ignite the mixture in an electric igniter. Similarly, the material must be friction sensitive enough to be reliably ignitable by the action in a percussion primer. Ideally what is needed is a material that can be desensitized to friction and ESD so that large amounts of the material can be handled, yet re-sensitized when configured in the final desired application for the particular material.
While other processes may achieve similar results (such as a hydrous process involving modification of nanoscale aluminum to reduce MIC sensitivity), these require more complex processing, especially to produce a MIC material of as high a quality as the starting MIC material. Furthermore, the present invention permits the undisturbed use of organic polymers in conjunction with the MIC material.
BRIEF SUMMARY OF THE INVENTION
The present invention is of a method to substantially desensitize a metastable intermolecular composite material to electrostatic discharge and friction, comprising: mixing the composite material with an organic diluent; and removing enough organic diluent from the mixture to form a mixture with a substantially putty-like consistency. In the preferred embodiment, mixing comprises mixing the composite material with an anhydrous, inflammable solvent, preferably one or more of fluorinated, chlorinated, or bromated, most preferable either one that is fully one or more of fluorinated, chlorinated, or bromated (e.g., a Fluorinert™ fluid) or that is a hydrofluoroether (e.g., a Novec™ fluid). The diluent preferably has a vapor pressure less than approximately 10 torr, most preferably between approximately 1 and 5 torr.
The invention is also of a method to recover a metastable intermolecular composite material substantially desensitized to electrostatic discharge and friction, comprising: receiving a mixture of the composite material and an organic diluent; and removing substantially all of the organic diluent.
The invention is further of a method to substantially desensitize and then recover a metastable intermolecular composite material, comprising: mixing the composite material with an organic diluent; removing enough organic diluent from the mixture to form a mixture with a substantially putty-like consistency; and removing substantially all of the organic diluent. In the preferred embodiment, mixing comprises mixing the composite material with an anhydrous, inflammable solvent, preferably one or more of fluorinated, chlorinated, or bromated, most preferable either one that is fully one or more of fluorinated, chlorinated, or bromated (e.g., a Fluorinert™ fluid) or that is a hydrofluoroether (e.g., a Novec™ fluid). The diluent preferably has a vapor pressure less than approximately 10 torr, most preferably between approximately 1 and 5 torr. Removing preferably comprises drying.
Objects, advantages and novel features, and further scope of applicability of the present invention will be set forth in part in the detailed description to follow, taken in conjunction with the accompanying drawings, and in part will become apparent to those skilled in the art upon examination of the following, or may be learned by practice of the invention. The objects and advantages of the invention may be realized and attained by means of the instrumentalities and combinations particularly pointed out in the appended claims.
BRIEF DESCRIPTION OF THE SEVERAL VIEWS OF THE DRAWINGS
The accompanying drawings, which are incorporated into and form a part of the specification, illustrate one or more embodiments of the present invention and, together with the description, serve to explain the principles of the invention. The drawings are only for the purpose of illustrating one or more preferred embodiments of the invention and are not to be construed as limiting the invention. In the drawings:
FIG. 1 shows pressure test results on MIC primers both treated and recovered according to the invention and untreated; and
FIG. 2 is shows pressure and burn test results on MIC powders both treated and recovered according to the invention and untreated.
DETAILED DESCRIPTION OF THE INVENTION
The present invention describes a method to desensitize a MIC material until it is configured into a final application. By keeping the material wetted with an appropriate solvent the material can be rendered insensitive to friction and ESD. Reaction will not propagate in the wetted material. In addition, one can press this desensitized material into a primer and then remove the solvent by drying to yield a fully functional primer, as good and often better in quality than the starting material.
The solvent can be any organic diluent, preferably with a relatively low boiling point and high volatility. However, many such diluents are flammable. The preferred solvents for use with the invention are anhydrous, inflammable solvents such as fluorinated, chlorinated, and/or bromated solvents, more preferably fully fluorinated, chlorinated, and/or bromated solvents such as the Fluorinert™ fluids available from Minnesota Mining and Manufacturing Corporation (3M), or hydrofluoroethers such as the Novec™ fluids from 3M (which do not have high global warming potentials). Most preferred are such solvents having vapor pressures of less than approximately 10 torr, most preferably approximately 1-5 torr. Solvents with such vapor pressures provide sufficient speed and controllability of evaporation.
One embodiment that demonstrates the desensitization of MIC according to the present invention employs Fluorinert™ FC-40, a perfluorinated liquid having a vapor pressure of 3 torr. Fluorinert FC-40 is useful because of its low flammability in air and acceptable volatility. One can mix, for example, a MIC composite of nano-aluminum and MoO 3 in hexane and FC-40. The hexane is much more volatile than the FC-40 and therefore the hexane can be removed by rough drying while leaving the MIC and FC-40 mixture.
Such a mixture, with sufficient FC-40, will not allow flame propagation. Furthermore, ESD and friction tests show that the resulting mixture is desensitized. Test results are shown in Table 1 and 2. The mixtures considered were: 1) 0.76 cc/g, 2) 0.7 cc/g, and 3) 0.54 cc/g FC-40 to final MIC material. These results demonstrate that acceptable ESD and friction sensitivities can be achieved by the present invention.
TABLE 1
Human Electrostatic Discharge Sensitivity Testing
(Spark gap of 0.085 in. and foil thickness of 0.003 in. at 15.24 kv)
50%
Sample
Energy (J)
No Goes
Goes
% RH
Temp (° C.)
FC-40/MIC #1
0.36
13
0
19.1
21.3
FC-40/MIC #2
0.36
13
0
19.1
21.3
FC-40/MIC #3
0.36
13
0
19.1
21.3
PETN Standard
0.36
13
0
20.5
21.3
(0601-012)
Batch RPS-3518
TABLE 2
Friction Sensitivity Testing
(The 50% load in kg determined using “Bruceton up/down method)
Sample
50% Load in kg
Log Units
% RH
Temp (° C.)
FC-40/MIC #1
7.2
8.04*
22.1
19.0
FC-40/MIC #2
3.1
1.50
22.3
18.5
FC-40/MIC #3
1.2
1.20
22.4
19.0
PETN Standard
6.0
1.37
19.6
22.0
(0601-012)
Batch RPS-3518
*Range varied from 14.4 kg at start of test to 2.4 at end of test.
In addition, performance of the MIC material can be restored by drying the MIC once it is in a primer configuration or in loose powder. FIGS. 1 and 2 show performance of the materials above as determined by close bomb tests and open tray burning rate. The treated material meets or exceeds the standard materials.
In short, one can desensitize and then recover the performance of MIC materials. This allows widescale application of MIC materials because the materials can now be scaled and handled.
Further details on manner of processing are next provided in the context of the example materials described above.
Using Nanotechnologies 80 nm aluminum and Climax MoO 3 and an optimum ratio of 38/62, dry components were weighed and combined with 15 ml of Hexane and 2 ml of Fluorinert FC-40. The material was sonicated with a sonic horn for 30 seconds. The petri dish was weighed and recorded and tared. The slurry was poured into the dish and rough dried on hot plate in a vent hood. When the material showed little sign of wetness, the petri dish was moved to a small vacuum/oven.
The concentration of FC-40/MIC is calculated as follows: An estimate of actual MIC is needed. Through experience it is known that a 1 gram batch processed through standard procedures results in 0.95 g of material. The density of FC-40 is 1.87 g/cc. For this example, the target concentration was 0.6 cc/g of MIC or 1.122 mg of FC/1 gram of MIC. Add the weight of the tare, the MIC and the FC-40. This will be the gross target weight.
A rough vacuum (23″Hg) was pulled and the oven heated to about 40° C. By checking the gross weight every few minutes, one can get a feel on when one is approaching the target weight. Note that heat accelerates the drying time and is the biggest contributor to the drying process and therefore should be regulated very closely. When the target weight is achieved, the semi-dried material can be harvested. A glove box with an open container of FC-40 is recommended to harvest. The more surface area of FC-40 the better. One can use a long tray (as a space saver) and a Kim-Wipe as a wick to get to a saturated state. Previous experience has shown that the uptake of FC-40 will make the FC-40/MIC ratio increase. This is a slow process and should not be an issue if the material is harvested and sealed in the same day.
Harvesting the material is identical to the standard procedure used to harvest regular MIC. The material is brushed through a sieve with more intensity due to the consistency of the material (putty like).
The saturated environment of the glove box is also where the primer cup loading takes place. Loading the desensitized material is the same as with the sensitive material. Pouring an amount of material on top of the die and scrapping it over the holes with a single edged blade. Simply tapping the full die on a hard surface multiple times produces compression much as the vibrators did. Add more material and scrap level, tap again and repeat. For the above concentration, a typical amount of material is 21.8 mg (dried weight) compared to an untreated primer of 23.5 mg. The push rods are started and the assembly is removed to the hydraulic press for final pressing. The rest of the loading procedure is identical to non-treated primer construction and does not require the glove box environment. An amount of FC is squeezed out of the material during pressing and is obvious by the wet spots left on the die base and the “mud” residue left on the pins and die barrel.
To obtain an accurate weight of material in each cup, note the weight of the cup and anvil, the total wet weight before drying and a final dry weight. Having these numbers one can calculate the actual amount/ratio of FC to MIC. The primers made have an average of 0.476 cc/g. The FC-40 has to be removed completely by vacuum/heat as before. This takes approximately 4 hours at 40°-45° C. and can be monitored as before to assure complete drying. Through previous tests, and taking into account the sensitivity of the scale, all the FC-40 can be removed.
Evidence of condensation on the vacuum/ovens glass door indicates that the recovering of the FC-40 should not be a problem.
Although the invention has been described in detail with particular reference to these preferred embodiments, other embodiments can achieve the same results. Variations and modifications of the present invention will be obvious to those skilled in the art and it is intended to cover in the appended claims all such modifications and equivalents. The entire disclosures of all references, applications, patents, and publications cited above are hereby incorporated by reference. | A method to substantially desensitize a metastable intermolecular composite material to electrostatic discharge and friction comprising mixing the composite material with an organic diluent and removing enough organic diluent from the mixture to form a mixture with a substantially putty-like consistency, as well as a concomitant method of recovering the metastable intermolecular composite material. | 2 |
BACKGROUND
This invention relates to a method of keying a pattern into a complimentary sealing ring and reel which are normally mated when assembled at some time during their use. The pattern is such that it will allow the mating of a particular sealing ring with a particular complimentary reel, but will prevent the mating of a particular sealing ring with any other reel.
Various forms of sealing rings and reels are currently available for computer tape. It is general practice to store a particular reel, with its particular sealing ring attached, alongside other particular reels with their particular sealing rings attached. The reels with their attached sealing rings are stored side by side, flat side of a reel along flat side of an adjacent reel. The reels are usually made visually indentifiable by attaching a label. The particular sealing ring associated with a particular reel also has a label attached, the label bearing the same identification as contained on the label of the reel to which the sealing ring is attached. In storage the label of the sealing ring is exposed to view to distinguish one assembly from among its neighbors.
When it is desired to use a particular reel of computer tape on computer related equipment, the particular reel with its attached sealing ring, as identified by the visually exposed label on the sealing ring, is removed from storage. Once the reel and the attached sealing ring are removed from storage, the identity of the reel is verified by the label attached thereto.
When the reel is to be used on computer associated equipment, the attached sealing ring must first be removed. From that point in time, until the sealing ring is reattached, the identity of the reel is dependent upon its attached label. When the use of the reel is no longer required, its particular sealing ring is reattached and the assembly is returned to side by side storage with similar assemblies.
It is not uncommon for many reels of computer tape to be in use in a particular computer associated area at a given point in time. Also, it is not uncommon, when reassembling sealing rings and reels, after use, that the sealing ring reapplied to a particular reel is mistakenly that which came from another reel. Thus, when the assembly is returned to storage, the identity of the particular reel, as indicated by the label on the visually exposed edge of the sealing ring, does not correspond to the reel which the sealing ring encircles. Locating a reel in storage, mistakenly encircled by other than its own particular sealing ring, creates difficulty which this invention seeks to avoid.
BRIEF STATEMENT OF THE INVENTION
The primary object of the present invention is to provide a means of keying a particular sealing ring to a particular reel in a manner such that the particular sealing ring can successfully encircle only the particular reel by virtue of complimentary formations in the sealing ring and reel, and the particular sealing ring can be prevented from successfully encircling any other reel by virtue of encountering a non-complimentary and interfering formation in the other reel.
The sealing ring of the invention comprises a strip of flexible material, preferably plastic, which is configured with a pattern, or formation, which pattern is complimentary to, in a keyed sense, a pattern, or formation, in the flanges of the reel, also preferably plastic, which allows the particular sealing ring to be used only with a particular reel. The manner in which this is accomplished is through the application of combinatorial theory.
Although the invention is not so limited, the sealing ring of the disclosed embodiment is formed in a molding operation, in the manner and with materials normally used, except that the sealing ring has a formation molded into one of its edges. Likewise the reel is formed in a molding operation, in the manner and with materials normally used, except that the reel has a particular formation molded into one of its flanges. Each sealing ring so molded has its own unique pattern, which is complimentary to that which is molded into the reel. In this fashion, each sealing ring is unique and can be mated with only a reel possessing the identical complimentary pattern. At the time of molding, or shortly thereafter, each sealing ring and reel can be impressed or labled with a serial number which is descriptive of the pattern. In this fashion, the sealing ring and its reel are identified until the ultimate user affixes his own lables.
Although molding is mentioned as the particular method of incorporating the unique pattern into the sealing rings and reels, this invention is not intended to limit itself to molding as a method of accomplishment. The same invention could be accomplished by cutting, grinding or equivalent operation following a non-specific molding operation. However, the design impressed on the sealing ring and reel during molding must be such to allow a unique pattern to be constructed during a later operation.
The method developed for the particular keying formation will be apparent from the drawings and from a detailed description of the preferred embodiment.
DESCRIPTION OF THE DRAWINGS
In the drawings:
FIG. 1 is a plan view of a reel and sealing ring assembly embodying the invention;
FIG. 2 is a sectional view taken along line 2--2 of FIG. 1;
FIG. 3 is an exploded fragmentary view of the assembly of FIG. 1 taken on a larger scale;
FIGS. 4 and 5 are exploded views of the upper and lower fragments, respectively, of the assembly of FIG. 2;
FIG. 6 is another exploded fragmentary view of the assembly according to the invention, with the reel positioned as in FIG. 4, but with the sealing ring reversed and therefore in improper position for assembly;
FIG. 7 is a schematic view of an assembly with formations of five slots and five tabs in one possible positional alignment;
FIGS. 8 to 11 are schematic views similar to FIG. 7 but with formations of four slots and four tabs in various positional arrangements;
FIGS. 12 to 17 are additional schematic views similar to FIG. 7 but with formations of three slots and three tabs in various positional arrangements;
FIGS. 18 to 21 are further schematic views similar to FIG. 7, but with formations of two tabs and two slots in various positional arrangements;
FIG. 22 is another schematic view similar to FIG. 7 but with formations of one tab and one slot in a matching position;
FIGS. 23 to 25 are still further schematic views similar to FIG. 7, with formations of various numbers of tabs and slots in a variety of positional arrangements.
The schematic views of FIGS. 7 to 25 are not to scale, and are intended to show positional relationships of tabs and slots, not their relative sizes. The size relationships are shown in FIGS. 1 to 3.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
Referring to the drawings, there is shown in FIG. 1 an assembly 10 comprising a reel 12 and a sealing ring 14. Ordinarially the reel 12 and ring 14 are both made out of plastic which possesses appropriate physical properties.
The reel 12 includes a central spool 16 and, as best seen in FIG. 2, a pair of spaced flanges 18, 20.
The sealing ring 14 comprises a strap 22 of flexible material, formed integrally with a latch 24 for drawing and holding the ends of the ring together and thus forming a ring which sealingly encircles the reel 12. Optionally, there is further provided a hook 26 for hanging the assembly 10 in storage.
Referring to FIG. 4, the sealing ring 14 may be seen in an enlarged cross sectional view having a groove 28 in each of its two edges 30, 32 as shown. Each groove 28 receives one of the flanges 18, 20 in sealing relationship, thus protecting the contents of the assembly 10.
The peripheral edge 30 of the strap 22 is provided with a first formation 34 in the shape of a primary tab 36 for keying or orienting the sealing ring 14 with respect to the reel 12. The first formation 34 is further provided with a plurality of secondary tabs 38, 40 as shown in FIG. 1. The tabs of formation 34 are received in correspondingly positioned matingly sized notches in a circular ridge 41, the latter being part of the second formation 42 in flange 18. The reference numeral 44 is applied to a primary notch associated with primary tab 36. Similarly referenced numerals 46, 48 are applied to the secondary notches associated with the secondary tabs 38, 40 respectively.
The circular ridge 41 is formed in flange 18 coencentrically with the circumference of reel 12 and comprises with the notches 44, 46, 48 a second formation, generally designated 42, which is complimentary to the first formation 34.
As may be seen in FIGS. 4 to 5, the tab 36 is disposed on one edge 30 of the sealing ring 14 and no tab or formation extends inwardly of the edge 32.
A full, unbroken circular or annular ridge 50 is formed in flange 20 of reel 12, such ridge being of diameter, form and dimension like that of annular ridge 41, thereby providing a third formation 52 on the assembly 10. (See FIGS. 2 and 4 to 6). The third formation 52 is complimentary to edge 32 of sealing ring 14 in that there can be no interference with a tab or formation along edge 32 since there are no tabs along edge 32. However, should the ring 14 be reversed during improper assembly to the reel 12, interference between tab 36 and ridge 50 will result as shown in FIG. 6. Stated another way, the third formation 52 is complimentary to the edge 32 and uncomplimentary to the first formation 34.
The pattern of tabs in the first formation 34 of the invention and of the notches in the second formation 42 of the invention must be such that it is necessary and sufficient that mating occur for the complimentary first and second formations of the correctly paired sealing ring and reel, but not allow mating when the particular sealing ring and reel are mispaired with any other non-complimentary sealing rings and reels, respectively.
FIG. 7 depicts, schematically, a sealing ring 14 sealingly encircling a reel 12 with the edge 30 of the sealing ring 14 having five tabs 36, 60, 38, 40, 62 of which one is a primary tab 36 while the remaining four tabs 60, 38, 40, 62 are secondary, and with the circular ridge 41 of the reel 12 having five notches 44, 64, 46, 48, 66 of which one is a primary notch 44 while the remaining four notches 64, 46, 48, 66 are secondary.
The notches and tabs, shown in FIG. 7, are equally spaced about the circumference, but need not necessarily be so.
The primary notch 44 and the primary tab 36, both at the top of FIG. 7, are wider than the remaining secondary notches 64, 46, 48, 62 and secondary tabs 60, 38, 40, 62, respectively. The positions occupied by the notches are termed notch positions while the positions occupied by the tabs are termed tab positions. The primary notch position 44 in the annular ridge 41 of the reel 12 is always nothced and the primary tab position 36 in the lip 30 of the sealing ring 14 is always tabbed. This serves as an orientation mechanism, as later will be illustrated.
The secondary positions may or may not be notched, insofar as the annular ridge 41 is concerned, and may or may not be tabbed, insofar as the lip 30 of the sealing ring is concerned. The number of permutations, with four secondary positions is 2 raised to the 4th power, or 16. All of these permutations, for both the notching of the annular ridge 41, which in this illustration has one primary notch and four secondary notch positions, and the tabbing of the lip 30 of the sealing ring, which in this illustration, likewise, has one primary and four secondary tab positions, are shown in FIGS. 7 through 22. FIG. 7 shows all secondary positions notched and tabbed, FIGS. 8 through 11 show three of the secondary positions notched or tabbed. FIGS. 12 through 17 show two secondary positions notched or tabbed, FIGS. 18 through 21 show one secondary position notched or tabbed and FIG. 22 shows no secondary positions notched or tabbed.
However, all of the permutations shown in FIGS. 7 through 22 are not exclusive of each other in the mating sense. This is illustrated in FIG. 23, where the ring from FIG. 18 can be mispaired and falsely mated with the reel from FIG. 12. Here the primary tab 36 successfully mates with the primary notch 44, the secondary tab 60 successfully mates with the secondary notch 64, and while a secondary notch exists at 46, there is no secondary tab at position 38, and the ring can successfully be closed about the reel.
Close consideration of all the permutations in FIGS. 7 through 22 will disclose that all rings with a given number of secondary tabs can be successfully closed about some reels with a larger number of secondary notches, and, conversely, all reels with a given number of secondary notches can be successfully enclosed by some rings with a lesser number of tabs.
Further consideration of FIGS. 7 through 22 will disclose that a ring with a given number of secondary tabs can only be successfully mated with a reel with the same number of secondary notches, if and only if, the notches occupy the same secondary positions as the tabs on the sealing ring. Mathematically for 2 N+1 positions (where one position is the primary position), the maximum number of mutually exclusive permutations to produce unique non-complimentary non-mating patterns, unless an exact match of tabs and notches occur, is the combination of 2 N things taken N at a time. In the illustration being used in FIGS. 7 through 22, with five positions for notches and tabs, N is equal to 2. The maximum number of mutually exclusive patterns of tabs and notches is secured with all possible combinations of two primary notches and tabs, i.e. FIGS. 12 through 17 inclusive.
Under the two position example cited above, FIG. 24 displays the necessity of the primary notch and tab. FIG. 24 shows the two secondary tab sealing ring of FIG. 17 with the primary tab removed, the former tab position being indicated by 36. Also shown in FIG. 24 is the reel of FIG. 12 with the primary notch position 44 being filled in. Note that by rotating the reel and ring with respect to one another, the sealing ring may be successfully closed about the reel, although it is not desired that this be so. If the primary notch position 44 had not been filled in, and the primary tab position 36 had not had its tab removed, the false match could not have been obtained.
Under the two secondary position example shown above, FIG. 25 displays the necessity of the primary position tab and notch being wider than the secondary position tabs and notches. FIG. 25 shows the two secondary position sealing ring of FIG. 12 with the primary tab 36 narrowed to the width of a secondary tab. Also shown in FIG. 25 is the two secondary position notch reel of FIG. 14, with the primary notch 44 narrowed to the width of a secondary notch. Note that by rotating the reel and sealing ring with respect to each other, the sealing ring may be successfully closed about the reel, although it is not desired that this be so. If the primary notch 44 had not been narrowed, and the primary tab 36 had not been narrowed, the false mating could not have been secured.
As previously stated, for a given number of notch positions, 2 N+1, where 2 N positions are available for secondary formations, and one position is used for a primary formation, the maximum number of mutually exclusive mating patterns are secured among the sealing rings and reels when the number of secondary positions notched or tabbed are N. Under these circumstances the unique number of combinations is the combination of 2 N things taken N at a time. With a standard large tape reel used in the computer industry, which has a circumference of about 33 inches, with secondary positions, say, every one half inch, approximately 60 secondary positions are available, which leads to about 100,000,000,000,000,000 unique combinations of notches and tabs in these secondary positions. | A reel and sealing ring assembly for computer tape is provided with a unique formation on one edge of the sealing ring. Further provided is a complimentary formation on one flange of the reel and an uncomplimentary portion on the other flange of the reel. The uniqueness of these formations guards against mismatching the labeled sealing ring of one assembly with the labeled reel of another assembly. | 6 |
TECHNICAL FIELD
[0001] This patent application relates to an object with a bearing location where the object comes into frictional contact with a counter-part or a counter-piece. Such an object can be a sliding bearing or a friction bearing on which different components of one or more devices, in particular the movable components of a machine or another mechanical device, move against one another under pressure.
BACKGROUND
[0002] The surfaces of the object and the corresponding counter-piece that rub against one another at the bearing location can be made of a metal, a ceramic material, or any other desired solid material. If these materials rub directly against one another, the bearing location can heat up as a consequence of friction. As a result, deformation of the bearing location and increased wear can arise. Even the undisturbed movement of the object and the counter-piece against one another can be impeded as a result of friction and, as a consequence, thermal expansion.
[0003] Objects with bearing locations usually have either a separate sliding bearing or a friction bearing or they are to be provided with a friction-reducing coating at the critical location. It is known, for example, that such solid sliding bearings or friction bearings can be manufactured from Teflon, a silicone, PEEK, PA, PI, PA/PI or a natural or synthetic hard rubber. It is also known that a friction-reducing coating of Teflon, polyimide and/or polyamide can be applied to objects that rub against one another and press against one another under slight pressure. Coatings of a sintered metal are also known for this purpose.
[0004] For objects with a friction-bearing location, although friction at the bearing surface is reduced relative to a bearing location without a coating, wear is still too great, especially that of the friction-reducing insert or the friction-reducing layer. Additionally, the known friction-reducing coatings and inserts have a limited stability with respect to temperature and a limited mechanical strength. Such extensive wear leads to a reduced service life or it requires frequent changing of the friction-reducing inserts or coatings.
[0005] For example, metallic, slippage-promoting coatings are known for high loads in terms of pressure and speed but exhibit poor dry-running properties.
[0006] Synthetic materials in the form of slippage-promoting lacquers or fully synthetic solid bearings, which have good dry-running properties, are known for low loads, but are unsuitable for high loads.
SUMMARY
[0007] Described herein is an object with a sliding or friction bearing location which is improved in regard to friction and/or wear and capable of being used in a versatile manner.
[0008] It has been found in this application that friction and/or wear at the bearing location can be reduced with a thin layer of a coating, which essentially comprises a high-performance thermoplastic. This thermoplastic polymer can be selected from the family comprising the polyaryletherketones (PAEK), such as polyetheretherketone (PEEK), polyetherketone (PEK), polyetherketoneetherketone (PEKEK) and mixtures thereof. The polymer can also comprise a liquid crystalline polymer (LCP). Use can also be made of PPS with slight restrictions to achieve very good results. PEEK and PEK are especially preferred, along with mixtures that comprise PEEK and PEK. These polymers are characterized by having higher mechanical strength with simultaneously high stability with respect to temperature. Surprisingly, it has been found that friction at such a coating can be reduced with these polymers.
[0009] Coatings made exclusively of the thermoplastic polymer show very good wear properties as well. Homogeneous and mechanically highly stressable coatings obtained have significantly lower wear with simultaneously lower friction compared to known coatings that comprise PI, PAI or PDFE.
[0010] The coating can have a layer thickness ranging from 5 μm up to e.g. 50 μm, advantageously from 5-30 μm and, sufficient for the majority of applications, 10-20 μm. It is found that layers starting from approximately 3 μm can be manufactured homogeneously with desired strength and the lubricity and wear properties can reach an optimum starting from even 5 μm.
[0011] An additional advantage of the coating with a small layer thickness is that the dissipation of heat from such thin coatings into the supporting material, which is e.g. metallic and is located under the coating, is improved at the bearing location. This is particularly interesting for applications in which large frictional forces and consequently large amounts of frictional heat are produced. These can be dissipated more rapidly before overheating sets in, which can lead to melting of the coating or, in general, to damage or to the destruction. Thus the stability of the coating or of the object with such a coating is improved relative to known coatings.
[0012] It has also been found that the disadvantageous effects of thermoplastics that arise when the glass transition temperature is exceeded, such as, in particular, reduced mechanical strength, cannot be observed when the thin coating in this application is heated above the glass transition temperature of the thermoplastic. This could be due to a strain effect on the thin coating along with the surface that is located beneath it, which acts positively on the material properties of the thin layer and prevents the glass transition process or at least the negative consequences on the layer properties. This effect may be further amplified as a result of the good adhesion properties of the coating to suitable substrates.
[0013] In addition to the thermoplastic polymers, the coating can also contain finely divided solid fillers in a total proportion of up to 10 wt %, and up to maximally 5 wt %. The fillers are selected in such a way that, on the one hand, they do not reduce the stability of the coating with respect to temperature and, on the other hand, do not increase friction but still have great mechanical strength.
[0014] Suitable fillers can be (nano-) ceramic particles, metallic particles, or silica. Quartz or diamond may also be very suitable. Surprisingly, it has been found that these fillers have practically no effect in terms of increasing the friction of the coating but are capable of further increasing the hardness and wear resistance of the coating.
[0015] Finely divided metallic particles, from e.g. aluminum, bronze, copper, tin, chromium, nickel, antimony, titanium, zirconium, manganese, cobalt, zinc and the oxides thereof, or iron oxide, can also be contained in the coating.
[0016] It is generally true that the particulate fillers may be rounded rather than being sharp-edged or angular. It is also advantageous if the particle size of the fillers is approximately an order of magnitude below the desired layer thickness of the coating. It is also advantageous if the particles are present in only a narrowly regulated size distribution so that a particle size, which is based on e.g. the d 50 value, varies in size over a narrow range. Fibers of the small size required for thin layers are no longer available and are unsuitable as fillers for the coating.
[0017] The high-performance thermoplastic may be present at a level of purity of at least 95 wt % and, in particular, at more than 97 wt %, so that maximally 5 wt % of the polymer matrix comprises other polymers, which may be also hard and stable with respect to high temperatures. The fluorine polymers, which are usually contained in known slippage-promoting layers, such as PTFE, do not result in any advantages for the slippage-promoting layer in this application, so the slippage-promoting layer is free from fluorine polymers.
[0018] Additionally or alternatively to the filler, a friction-reducing coating can also contain a dry lubricant in a proportion of e.g., maximally 10 wt %, wherein the proportion of the fillers and/or the dry lubricant contained in the polymer matrix advantageously do not exceed the aforementioned 10 wt % individually nor in terms of their sum. Such a dry lubricant can be compounds that have a layer structure, such as graphite and molybdenum sulfide.
[0019] For one embodiment, the thermoplastic high performance polymer is present in a proportion of at least 60 wt %. A proportion of up to 20 wt % of molybdenum sulfide and, in addition, up to 20 wt % of graphite may be suitable as a filler or dry lubricant in the coating.
[0020] For example, an advantageous friction-reducing coating of an object comprises the following components:
[0021] A) 90-100 wt % of a thermoplastic polymer that may be PEEK, PEK, LCP, PPS and mixtures comprising PEEK and PEK;
[0022] B) 0-10 wt % of a finely divided filler and/or;
[0023] C) 0-10 wt % of a dry lubricant.
[0024] An advantageous friction-reducing and/or wear-reducing coating for an object with a bearing location can also be obtained with a coating that has a multilayer structure. In particular, the multilayer structure can comprise an adhesion-promoting layer as the lowermost layer, in which 30-90 wt % of finely divided metallic particles are present in addition to the designated high-performance thermoplastic polymer. With such metal-containing adhesion-promoting layers, a stable multilayer structure of the entire coating arises as a result of the thermoplastic component that is common to all the sublayers, this multilayer structure also having significantly improved adhesion to metallic surfaces in particular. It is also advantageous if such an adhesion-promoting layer does not worsen the mechanical properties of the coating. In regard to the metallic particles in the adhesion-promoting layer, the choice of metal is subject to significantly fewer limitations since these particles do not have to contribute to the reduction in friction of the entire coating. Thus iron-containing particles, for example, or those comprising a light metal or a nonferrous metal may be very suitable.
[0025] Objects with a friction-reducing and/or a wear-reducing coating have a coating thickness that has been adapted to the desired type of use in terms of bearing force, ambient temperature, chemical environment and relative speed of the surfaces that slide over or rub against one another. For example, a coating that has been designed for chemical requirements that are not too demanding can even be realized with a layer thickness of up to about 10 μm.
[0026] The coating can be applied, with good adhesion, to surfaces that comprise metal, a ceramic material and synthetic materials as well, provided that the material endures the high temperatures of the layer production process, which are engendered by the manufacturing process.
[0027] If the metal or ceramic surface under the coating has a suitable roughness, it can increase the mechanical strength of the coating and the proportion of filler materials can also be further reduced by these materials serving merely to increase the strength.
[0028] Two processes are available in principle for applying the coating that reduces friction or wear. It is possible, for example, to apply the coating in the dry state in the form of a powder coating, and then to convert the initially applied powder layer into a homogeneous coating in a second thermal step. The powder coating can be assisted electrostatically by providing the powder to be applied with an electric charge while the object to be coated, in contrast, is electrically grounded or connected to an opposing polarity. It is also possible to carry out the coating on a pre-heated surface of the object, to which the particles may be able to adhere as a result of the melting in of the components.
[0029] The powder particles can be sprayed on, sprinkled on or applied in some other way. Compaction of the layer then takes place. In order to do this, the object together with the applied powder layer can be brought in an oven to a certain temperature at least above the melting point of the polymers contained in the powder layer. For this purpose, it is advantageous to subject the object with the powder layer to a temperature program that provides defined holding times at defined temperatures and, accordingly, includes suitable cooling down. It is also possible to carry out the temperature treatment in a tunnel oven with zones that may be thermostatically controlled to different levels, through which the object may be led with appropriate dwell times.
[0030] Another particularly advantageous possibility for the manufacture of a coating is to apply to the object a dispersion that contains all the components of the coating in finely divided and dispersed form in a solvent or a solvent mixture, e.g. aqueous or with water and/or alcohols, and then dry the coating and subsequently subject it to a thermal treatment, as in the case of the powder coating.
[0031] The dispersion can be applied by immersion, brushing, spraying, or in other ways. In order to achieve greater layer thicknesses, it can be advantageous to carry out the coating in several sequential steps. After each step one can, for example, evaporate the solvent from the applied dispersion layer. It is also possible to carry out a temperature treatment after each individual step in order to melt, or at least to pre-compact, the dispersion layer. The number of coating steps to be carried out may be determined by the desired layer thickness and depends on the particle size of the solids (thermoplastic and filler) contained in the dispersion and on the application process that has been selected.
DESCRIPTION OF THE DRAWINGS
[0032] FIG. 1 shows a schematic cross section of an object with an applied dispersion layer;
[0033] FIG. 2 shows an object with a coating;
[0034] FIG. 3 shows a process sequence for a coating using different process steps; and
[0035] FIG. 4 shows a flow diagram for a coating by dispersion processes.
DETAILED DESCRIPTION
[0036] The substrate to be coated SUrepresents the object to be coated, or a region thereof. The surface to be coated can initially be subjected to a chemical and/or mechanical activation treatment. For this, mechanical roughening can be used, e.g. by a sandblasting blower, or via etching with acids or alkalis, or via a plasma treatment. An appropriately pretreated surface has additional chemical/physical bonding sites and it is clean and free from grease and, if roughened, has a larger surface area which leads to better adhesion of the coating to be applied. An advantageous feature may be a degree of roughness of up to 20 μm (RZ value or height), wherein the roughness-engendered height differences on the surfaces to be coated should amount to maximally approximately 50% of the desired layer thickness of the coating. The layer thickness of the finished coating to be selected may be determined by the mean level of the peaks and valleys formed by roughening.
[0037] Optimum roughening can also be effected by an appropriately rough intermediate layer that can be manufactured in a simple manner with the desired surface roughness. Sintered ceramic layers or sintered bronzes may be suitable for this purpose.
[0038] A dispersion layer DS is then applied to this surface, the dispersion containing all the coating components, which may be dispersed in finely divided form in a solvent or mixture of solvents, and have a particle size distribution that is as homogeneous as possible. An application process is selected that may be suitable for the manufacture of the desired layer thickness. FIG. 1 shows a substrate SU coated in this way with an applied dispersion layer DS.
[0039] After carrying out a temperature program—during which the substrate or the object to be provided with the dispersion layer DS is heated to a temperature above the melting point of the thermoplastic contained in the dispersion—a homogeneous coating BS may be obtained that is free of pores and compact and has good mechanical cohesion along with good adhesion to the substrate SU. FIG. 2 shows the finished object.
[0040] It is possible to carry out the coating on only one subregion of the surface. The remaining region that is not to be coated can be shielded, or an application process for the dispersion may be selected that is capable of differentiating between different surface regions, e.g. brushing or printing. This covering procedure can also take place with a shadow mask during the spraying on of the dispersion. This shadow mask can also be constructed in the form of a film that is applied to the surface of the substrate SU and that leaves uncovered the regions of the surface that are to be coated. After the application of the dispersion layer DS, the film can be removed and pulled off, for instance, whereby the regions of the dispersion layer DS that have been applied over it are pulled off at the same time.
[0041] FIG. 3 shows one embodiment of the process with which a greater layer thickness can be achieved despite the smaller particle diameter that has been selected for the solids contained in the dispersion. In order to do this, at least the solvent is removed—as an alternative, the first dispersion layer is additionally pre-compacted to an appropriate extent by a temperature treatment—following the application of the first dispersion layer DS 1 as illustrated in FIG. 3 a. In a second step, the dispersion coating is repeated, and a second dispersion layer DS 2 is applied. If required, this layer can also be pre-compacted and the coating step can be repeated once again. In a final step, as illustrated in FIG. 3 c, the structure, which includes dispersion layers and several sub-layers, is finally brought to a temperature above the melting point of the thermoplastic, whereby one obtains a fully compacted, pore-free sealed coating BS on the substrate SU.
[0042] For example, a composition which may be suitable for application by dispersion processes and may be also friction-reducing, contains solids in the following proportions by weight:
[0043] 97 wt % PEEK;
[0044] 1 wt % nano-particulate Al 2 O 3 ;
[0045] 1 wt % MoS powder; and
[0046] 1 wt % graphite powder.
[0047] The solids may be optionally dispersed with auxiliary agents in a solvent, which may be water or, advantageously, may be miscible with water, or mixed with water, e.g. alcohol and isopropanol. The dispersion mixture then contains approximately 30 wt % of the aforementioned solids.
[0048] The process sequence described above is illustrated in a clearer form in FIG. 4 in a flow diagram. In step 1 , the process comprises the manufacture and preparation of the powder mixture. For this purpose, the ingredients, selected from a thermoplastic polymer, a filler and a dry lubricant, may be either brought to a suitable particle size, for example, by grinding, and/or they are brought, by subsequent sorting, to a grain size that conforms to the desired grain size distribution, which is as narrow as possible.
[0049] In step 2 , in parallel to this, one prepares the solvent, which may be innocuous from environmental and heath-related viewpoints and may be water-based e.g., prepared from a mixture comprising alcohol and water, e.g. isopropanol and water. An advantageous solvent composition contains, for instance, 25-75 wt % isopropanol in water. A solvent with approximately 75 wt % isopropanol in water is especially preferred.
[0050] In step 3 , the dispersion may be manufactured by mixing the prepared powder mixture with the solvent, maintaining a solids content of 30-50 wt %. In order to improve the stability of the dispersion, conventional dispersion aids can be added in small proportions.
[0051] In step 4 , the surface of the object is coated, e.g. by spraying, immersion, brushing, printing or by spin-coating. As homogeneous as possible a thickness of the dispersion layer is sought and surface regions that are not to be coated are left alone.
[0052] In step 5 , the solvent is removed by evaporation, which can optionally be assisted by negative pressure.
[0053] In the subsequent step 6 , the object with the applied and dried dispersion layer may be converted into a homogeneous coating by heating and melting of the thermoplastics, and then the object may be cooled down once again.
[0054] Followed by step 6 , a finished coating can be obtained at point 7 .
[0055] In one embodiment of the process, it is possible to carry out steps 4 through 7 again directly after step 7 .
[0056] In another embodiment V 2 follows on from step 6 , after the melting of the first dispersion layer, a new dispersion layer may be applied (step 4 ) and appropriately compacted (steps 5 through 7 ).
[0057] V 3 In one embodiment of the process, a second sublayer, which is different from the first coating, may be applied following the manufacture of the first coating. In order to do this, a further dispersion may be manufactured in accordance with process steps 1 - 3 , and the object may be coated therewith in accordance with steps 4 - 6 . Here also, the process V 1 V 2 can be modified by repeating individual process steps or individual process step sequences in order to achieve the desired layer thickness.
[0058] A Homogeneous coating can be obtained, in particular when finely divided particles are used for the dispersion, this especially homogenous coating making multiple coating advantageous or essential because of the small particle diameters.
[0059] A wear test was carried out with a coating produced and a comparison was made with a conventional coating that comprises a sintered metal. Whereas wear amounting to a layer thickness reduction of 15 μm arises for a given load and initial layer thickness with the conventional coating after a given time, reduced wear in the form of a layer thickness reduction of only 2 μm is observed with a coating in this application for the same load and the same initial layer thickness. This shows the superiority of the new coating and its improved wear resistance.
[0060] Possible variations result, in particular, from a suitable selection of fillers and, optionally, from mixtures of different fillers. The quantity relationships that are used for the components of the coating may be selected in accordance with the desired load on the coating. The same applies to the layer thicknesses, which are likewise not limited to the examples that have been given. The coating may be advantageously applied to metallic surfaces, but the coating can also take place on other surfaces, such as a ceramic material, glass or suitable synthetic materials.
[0061] This application may be advantageously used for an object whose bearing location is constructed in the form of a sliding bearing. Such a sliding bearing can be suitable for the accommodation of a rotating shaft or to facilitate, e.g., as a result of reduced friction with improved wear characteristics, the translational movements of a device that comprises an object and counter-piece in operation in accordance with regular requirements. Coatings can also reduce rolling friction, and are therefore utilized in roller bearings. Naturally, it is also possible to utilize these coatings in a wide variety of bearings, even if the bearing location may be not subject to friction via the counter-piece. The coating can thus be employed for static and dynamic bearings and machine parts and, in this way, it can also perform simple sealing functions, wherein it always has only low wear. Fields of application are mechanical and electromechanical devices and machines, as well as combustion engines. Concrete, but not exhaustive, examples of additional applications are therefore connecting rod bearings, pistons, piston rods, piston rings and piston seals in combustion engines, pumps and compressors, as well as dynamic seals and wheel suspension units.
[0062] In general terms, this application may be usable for bearing surfaces that are located within the flow of power, e.g. in cylinder head seals, and especially for the stoppers that have to accommodate the greater part of the compressive pressure and hence large forces and are subjected to large frictional forces as well. | An object has bearing location where the object comes into contact with a counter-piece. The bearing location includes a coating to reduce wear and friction. The coating comprises about 90-100 weight percent thermoplastic polymer and about 0-10 weight percent finely divided solid fillers and finely divided dry lubricants. The coating has a thickness of between about 5-50 μm. | 5 |
BACKGROUND OF THE INVENTION
The invention relates to an ink only label, which is removable from a substrate to which it has been applied by washing with water or an aqueous alkaline solution and to a transfer label comprising a backing layer and the ink only label which is releasably attached to the backing layer.
The invention also relates to a container provided with an ink only label according to the invention and to a method of removing the ink only label from such a container.
More in particular the present invention is directed to a label for returnable plastic containers such as crates and more specifically to decorative promotional and/or informational labels suitable for use on plastic crates. Still more particularly, the invention is directed to a label composite which applies only the inks of the graphics to a polymeric substrate, having the ability to be removed from the substrate, without destructive treatment of the substrate surface, so that the substrate can be relabelled.
It is known in the packaging technology art to label containers such as plastic crates by providing a non-removable permanent image by a silk screen method. Such labels offer a highly durable finish with two or three color availability. This technique however offers limited colors, lacks the improved graphics that other labelling techniques offer, is not flexible in its ability to have graphic changes to meet market strategies leading to large inventories of obsolete units, tends to show signs of wear after about four trips (typical crate life expected at 60 return trips and is relatively expensive as compared to other label techniques.
When removable inks are to be applied to re-usable plastic crates by a screen printing or a tampon printing process, the inks have to be applied in the bottling plant, such as a brewery, which may lead to problems with respect to registration. Upon removal from the crates by means of crate washers, the inks will be dissolved in the washing liquid and in this way contaminate the crate washers. Furthermore the speed of application is limited, and curing of the inks requires a lot of space and long storage times prior to delivery.
A second way of labelling containers encompasses gluing printed paper labels to containers such as plastic crates or bottles at the time of filling and sealing. This type of label however offers little resistance to label damage from handling and exposure to moisture (wrinkling). Furthermore, paper labels are difficult to remove from crates, and tend to clog the crate washers available today. Upon removal of paper labels from plastic crates, a glue residue may be left on the crates.
A third technique for labelling containers, in particular glass bottles is based on the principles described in WO 90/05088. This method of labelling bottles provides a durable, highly impact resistant label and yet permits high definition label printing. A transfer label comprising a removable backing layer is provided which backing layer is reverse printed with a vinyl or acrylic ink which is cured and overprinted with adhesive. The label is applied to the container with its adhesive surface in contact therewith. The backing layer is separated from the transfer layer of the label for instance by the application of heat to either the container, the label or to both. The labelled container is then applied with a coating which is subsequently cured. The cured coating provides the required degree of impact resistance and durability. The disadvantage of permanently attached labels, is that when these labels get scratched or otherwise damaged, they cannot be easily removed from the bottles. Further, it is not possible to provide the same containers each time with new and/or different labels, which is desirable for promotional activities.
The need for returnable bottles and crates is a direct result of industry preference and government legislation with regard to returnable (refillable) containers in various parts in the world in lieu of one way packaging. In this type of recycling environment a whole new market has been created for the handling of packaged beverage containers. This is presently true of both refillable PET and glass bottle containers. Certain countries, European in particular, have invested large sums of money in the creation of distribution systems that rely heavily on the returnable crate concept.
Typically the only product presentation in such a recycling (refillable) market is that which can be printed on the exterior of the crate. Due to handling, space and storage considerations the only marketing, name brand, promotional, UPC code or other informational presentation is that which is printed on the exterior of the crate. The reason is that typically the crates are stacked at commercial outlets such as grocery stores with only the side and end panels showing. As such, the presentations on the said panels of the crates are the only distinguishing features from one product to another.
In the use of returnable crates it would be very interesting to be able to use one uniform crate for various different products or brands. However, this is only possible if there exists an easy and inexpensive method of providing an image or imprint on the crate, which is also easily removed after the crate is returned to the bottling line for refilling.
On the other hand, it is important that the label image or imprint on the crate is durable, especially during transport, storage and is durable even when subjected to humid conditions.
Accordingly it is an object of the invention to provide a label for a returnable plastic crate creating an imprint, or image on at least one of its surfaces, which is durable, scratch, wear, weather and moisture resistant during use, but which is easily removable during the crate washing operation upon return to the filler.
It is also an object of the invention that the label on the plastic container shall be impervious to handling contact and ambient storage conditions both outdoor and indoor.
It is also an object of the invention that the label, if desired, be readily and completely removed in the standard crate washer used when the plastic container is returned to the beverage plant for refilling.
It is also an object of the invention that the properties of the label with respect to removing it can be controlled, so that the label will not be removed or damaged in standard crate washing operations, but only under specific, more severe crate washing operations.
It is an object of the present invention that the labels incorporate a full range of graphics, from a simple one color up to a full photographic reproduction.
Finally it is also an object that the method be simple and low cost.
SUMMARY OF THE INVENTION
These and other objects are achieved by the ink-only label according to the present invention, said label at least consisting of an adhesive layer, an ink-only image layer and optionally a protective layer, wherein the label, when applied to a substrate, has a water permeability coefficient, as defined herein, which is sufficient to enable fast removal of the label from the substrate with water or an aqueous alkaline solution, without destructive treatment of the said substrate.
In order to provide the desired removal characteristics it has been found essential to control the water permeability characteristics of the label when applied to the substrate surface, such as a crate surface. On the one hand the water permeability must be sufficiently high to provide a speedy removal of the label through break-up and/or swelling of the material when immersed in or sprayed with water. On the other hand it should not be so high that the label becomes removed when subjected to normal ambient conditions. In effect the water permeability characteristics have been fine-tuned to provide a label that meets the criteria defined herein above.
The water permeability coefficient is defined as the amount of water that the label takes up, as a fraction of the dry weight of the label within a period of three hours immersion at 20° C. The coefficient can be determined using the test method for the water uptake.
As indicated above the value for this coefficient should on the one hand be sufficient to enable removal of the label from the substrate with water, without destructive treatment of the said substrate, and on the other hand be such that during normal outdoor conditions the label remains intact and good-looking.
In general this means that the lower limit for the water permeability coefficient is 0.15, preferably 0.25 and most preferred 0.50. The upper limit for this coefficient is 2.50, preferably 1.35 and most preferred 1.00.
According to a preferred embodiment the label of the invention possesses a water uptake test value which is between 1 and 75 g water/m 2 of label, typically about 5 g/m 2 . The water uptake test value is especially a measure for the resistance of the label against removal by soaking. The test is carried out as defined furtheron.
When the value is not more than 75 g/m 2 , the label is resistant to removal under ambient outdoor conditions, i.e. when the label has been applied to a crate which has been left in rainy conditions, the label will not become damaged or removed, at least to a substantial degree.
On the other hand, when the value is more than 1 g/m 2 , preferably more than 2.5 g/m 2 , the label can be removed sufficiently fast in a standard crate washing equipment.
Likewise the properties of the label can be determined using the pencil scratch test, which is also described in detail later, both under dry and wet conditions. In general test values for pencil hardness of at least 1 N indicate sufficient durability of the label under ambient (dry) conditions. Generally values between 1 and 10 N are acceptable, whereas lower values result in insufficient scratch resistance and values of over 7 N are indicative of labels that are not easily removed. After immersion in water the pencil hardness should drop to below 0.5 N within an acceptable period of time (10 min., preferably 3 min, more preferred 1 min.).
Another property of the label that is important for determining the ease of removal of the label from a substrate is the water vapor transmission rate per m 2 per 24 h. This rate should of course be higher than 0, as otherwise no vapor transmission will occur (and in all likelihood no water uptake). In general, suitable labels have a water vapor transmission rate of at least 50. The upper limit of this rate is about 750, whereas a typical, suitable value is about 600 g/cm 2 /24 h.
The term “ink only label” is used herein to define a label that does not have a paper or plastic backing, but which comprises an image layer of ink, which is directly applied to a surface. Quite often the surface remains at least partly visible through the image layer. An ink only label may conveniently be applied to a surface by image transfer using a reverse printed label.
The label to be used in accordance with the present invention is essentially based on an ink image without a backing material. The ink image will adhered to the surface of the crate by an adhesive, and the surface of the image may be protected by a protective layer.
The present invention provides a distinct improvement over the prior art systems, which were based on paper or plastic labels. In order to remove these labels expensive high pressure equipment was necessary, especially in the case where labels were required on adjacent sides of the crate. Removal of the labels through simple soaking, as in the present invention, is virtually impossible. Further the residues of the labels have a tendency to clog the crate washing equipment.
The system of the present invention is less expensive and environmentally more friendly, as the residues of the ink only label are easily recovered from the water so that the water can be recycled.
The present invention also provides the possibility to use the label for scanning possibilities, for example by including a UPC (bar) code therein, which code may be used to define the recipient, the contents or any other information that is suitable. The system also allows the producer to reduce the stock of crates, as it is no longer necessary to keep stock crates of all brands or types. The system according to the present invention makes it possible for a producer to have only one type of crate for each type of material, for example a bottle, irrespective of the brand of the material. This makes it possible to reduce the stock of crates substantially. Of course the reduction would be even greater if the whole industry in a country or continent would decide to use the system.
In such a case many different producers (bottlers) of beverage containers would share common crates, and yet maintain individual market identification via the present invention. At the same time an improved user friendly and cost effective recycling system would be perfected. Such a system could be utilized on a national of even a multi-national level.
According to a preferred embodiment a transparent protective coating is present on top of the image layer. This coating improves the resistance of the label against environmental influences. Generally the material of the protective coating is compatible with the material of the ink. More preferably all materials, adhesive, ink and protective coating are at least partly based on acrylate polymers. In order to improve the durability of the label further, it may be advantageous that after application of the label (and the coating) one or more treatments are given. These treatments provide a coalescence of the materials of the various layers, resulting in improved service life, without, however, deteriorating the wash-off behaviour.
By careful selection of the composition of the label, the use of a protective coating and the nature of the post treatment, it is possible to steer the properties of the label, especially with respect to the behavior during crate washing. More specifically, it is possible to design the system in such a way, that the label is removed during standard crate washing. This means that after each return to the beverage filling plant, the label is removed and a new, optionally different, label may be applied. On the other hand, the label may be made so durable that it can not be removed or damaged during standard crate washing, but only in the case when a specific, severe washing operation is used. In this way the label is not permanent, however it has all the advantages of a permanent imprint, for example a silk screen, without the disadvantages thereof, such as the high costs thereof in terms of investments and energy requirements, inflexibility and low number of colors.
The selection of the adhesive to be used in adhering the label image to the crate surface will at least partly depend on the intended service life of the label, one-way or multiple trip use. Of course the adhesive must remain removable during crate washing. The adhesive must have been activated prior to or during application of the image to the crate. An easy and generally preferred method of applying the image is through the use of heat activatable adhesives, that have been applied to the image in the form of a reverse printed label. Other methods include the use of adhesives that can be activated through radiation, chemicals, electron-beam, micro-wave, UV and the like. It is also possible to use adhesives that can be activated through photo initiation, humidity, enzymatic action, pressure or ultra-sonic treatment.
It is preferred to use adhesives that are activated either by heat or by pressure. The latter case also encompasses adhesives, which require pressure to remain adhered, although they may have some tackiness without pressure. Preferred heat activatable adhesives have an initial tack temperature of not more than 90° C., preferably between 70 and 87.5° C.
The adhesive is preferably present on the back side of the image before it is applied to the crate surface. However, it is also possible to apply the adhesive to the crate prior to transferring the image. Another possibility is the use of inks in the image that have the adhesive incorporated therein.
The protective layer, if used, may be applied after the image has been transferred to the crate, for example using a conventional roller coater or spray system. In the alternative the protective layer may be part of the image material as it is transferred.
According to a further preferred embodiment the label layer consists of an image layer which is contained within containment layers, as described in the copending application of the same date titled: “Transfer label having ink containment layers. container comprising a transfer layer and method of washing such a container” (attorney reference BO 40707), the contents of which application is incorporated herein by way of reference.
The label of the present invention may be applied to a substrate surface by a method comprising in its broadest form:
providing a surface, preferably moving at a uniform rate of speed,
presenting a reverse printed label according to the invention on a substrate, separable from its substrate, and
transferring the label ink to the polymeric surface.
The label is applied to a polymeric surface which has preferably been surface treated and temperature stabilized. The label is applied by transferring the ink from its film substrate utilizing a roller or a pad. Preferably a heated roller is used under pressure. As indicated previously, the adhesive may either be present on the label or may be on the polymeric surface. The adhesive has to be activated prior to or during transfer. Depending on the type of adhesive, the activation method will differ. The skilled person will be aware which type of activation will be required. In case of a pressure sensitive adhesive, pressure will be applied during transfer. If a heat activatable adhesive is used, it is preferred to preheat the polymeric surface, optionally in combination with a heated transfer system, such as a roller.
In a preferred embodiment a heat activatable adhesive is used, in combination with a heat-pretreatment of the polymeric surface. As the heat activated adhesive printed over the ink becomes tacky, the ink is released from the film substrate and adheres to the plastic surface.
The labels may be supplied on a roll, from which the images are transferred to the substrate, optionally in combination with a cutting operation. It is also possible to provide a stack of separate labels, using a suitable application device, such as a magazine fed labeler.
Depending on the requirements on the image it may be preferred to have a protective coating on top thereof. This coating may have been applied as part of the reverse printed label during image transfer. In a preferred embodiment the protective coating is applied after image transfer, for example by the use of a roller coater.
In that situation, the transfer surface is coated with a thin layer of protective coating, such as an acrylic wax. Subsequently a post treatment, preferably one or more heat treatments are given. With this treatment the label materials coalesce and without being bound thereto, it is assumed that the durable bond obtained thereby is affected through interdiffusion of the adhesive and plastic surface.
A label according to the present invention that combines sufficient durability during storage and use, with quick and economic removal, has preferably been heat treated after application to the container at a temperature of between 40° C. and 100° C., more preferably between 50° C. and 90° C.
In the case where the image has to be more durable, for example for multi-trip use, it is preferred to use either a more durable coating, such as a urethane or a cross-linked urethane, and/or a prolonged, more extensive post treatment.
It is well-known that polymeric materials and especially high density polyethylene in particular, are difficult materials to bond with adhesives. This invention describes a specific method of surface treatment to ensure adhesive bonding that is fast and economically.
An important discovery described in the invention is the coalescing of the label materials and surface coating by exposing the labelled area to very high temperatures for a few seconds to increase durability and resistance to moisture. This process alters the label composite from a series of adhered layers which are easily dissociated with immersion in water for two or more hours to a coalesced matrix of label adhesive, label inks and outer coating. During the heating the adhesive material inter diffuses with the plastic surface. The simultaneous coalescing and inter diffusion of this preferred embodiment of the invention result in a very durable label matrix. Resistance to water immersion can be varied from a few hours to several weeks by varying the time of exposure and the resultant temperature.
It should be noted, that the resistance to water immersion of an untreated label according to the invention may be sufficient as it never completely loses its bonding with the polymeric surface. The bonding only weakens; drying restores the bonding strength to its original value.
Having achieved the required label durability, it is also necessary to remove the label after it has served its purpose of identifying the contents of the container prior to consumption. The empty plastic containers and beverage bottles are returned to the beverage plant for refilling. The plastic containers are washed. During this wash the label must either be completely removed, or remain on the surface undamaged, depending on the situation (one-way or multi-trip).
In the former case, the heat treated adhesive used to bond the ink matrix, while durable in water, breaks down in the washing solution, preferably hot caustic, enabling the label and adhesive to be completely removed. The label residue is filtered out of the caustic solution. In the latter case the label is only removed when the washing conditions are changed to remove the label, for example by using a prolonged soaking and/or a stronger caustic solution, optionally in combination with the use of high pressure jets (liquid or gas).
Alternative methods for removing the images without a destructive treatment of the substrate (polymeric) surface comprise chemical removal (solvents), ultra sonic, sub-cooling, heating, brushing, enzymatic treatment, vacuum treatment, peeling and radiation, such as UV. Combinations of various methods are of course also possible.
The invention is also directed to a method of washing crates in order to remove the ink only label.
It may be desirable that the processing equipment be arranged so that the plastic containers are labelled in-line during the normal progression through the beverage facility, so that the crate label matches the bottle contents.
DESCRIPTION OF THE DRAWINGS
FIG. 1 Heat Transfer Label
FIG. 2 Surface Treatment and Temperature Stabilization
FIG. 3 Label Application and Ink Transfer
FIG. 4 Coating Application
FIG. 5 Post Treatment
FIG. 6 schematically shows a method of applying the image layer according to the present invention, to a returnable crate
FIG. 7 shows a washing device for removal of a transfer layer according to the present invention from a container, in particular from a plastic crate.
FIG. 8 shows a cross-sectional view of the washing device according to FIG. 7 along the line III—III.
DETAILED DESCRIPTION OF THE INVENTION
The preferred embodiment of the label and application according to the present invention will be described first with references to FIG. 1 which shows the plastic container ( 1 ) and the label positioned for application. The label is printed on a film substrate ( 10 ) which may be any thin film, but in the case described is polypropylene of 2 mils thickness. ( 14 ) is an acrylic coating which may or may not be employed, depending on the type and source of the film available. ( 12 ) is a release material which coats the film. In the case of the invention it is silicone which is applied at the time of film manufacture. ( 20 ) represents all. the printed ink material. Depending on the label graphics and opacity requirements the ink materials may be as many as five (5) different colors in one or more layers, some of which many overlay another ( 30 ) and ( 40 ) represent two (2) layers of adhesive to indicate the build up of adhesive from 0.5 to 1.5 pounds per ream, depending on the labelled surface uniformity and rigidity of the container being labelled.
Upon application, all of the printed materials are transferred from the silicone release coated film substrate. The printed ink materials are urethane, vinyl or acrylic resin based, colored with temperature and ultra violet stable pigments. In the case of white ink, titanium dioxide is the pigment of choice. Pigment particle size ranges from three (3) to five (5) μm. The printed adhesive is a waterbased organic .material with an initial tack temperature of 185° F. (85° C.). This initial tack temperature is very important to the plastic labelling process because it determines the required plastic surface temperature at the time of transfer. With the particular plastic container being labelled, there is no support of the inside surface, hence it is desirable to maintain the plastic below 200° F. (93° C.) to avoid distortion of the surface by reaching its point of deformation during the label transfer.
The label application method will now be described on the basis of FIG. 6, the presently developed best mode of application of the invention, whereby the FIGS. 2-5 show the various steps of the process in more detail FIG. 6 shows a schematic view of the application process of a transfer layer from a transfer label according to the invention to a returnable crate 59 .
The label application process will now be described in the order of progression on the basis of this figure. Station 60 shows the step of surface treatment and temperature stabilization by means of a pre-heating treatment using a flame heater or burner 60 ′. For adhesion of two polymeric materials to occur, many factors must be considered such as cleanliness, pressure, temperature, contact time, surface roughness, movement during bonding and adhesive film thickness. An additional important consideration is the critical surface tension. The commonly accepted method of measuring the critical surface tension is with a Dyne solution, which is well known. For most adhesive applications the critical surface tension of polyethylene is 31 g/m 2 . A series of tests were performed which demonstrated for best adhesion of the adhesive previously described to the polyethylene surface, a treatment level of 60 to 70 g/m 2 was necessary. Further testing of commercially available equipment showed that flame treatment optimized both capital cost, operating cost and time required to achieve the required critical surface treatment.
For the adhesive to achieve and maintain tack quickly it is necessary to heat the polyethylene crate 59 at station 61 before the label adhesive is in contact with it. To avoid deforming of the container, it is desirable not to heat the surface over 200° F. (93° C.). As the surface temperature leaving the flame treatment is approximately 125° F. (52° C.), it is necessary to heat the surface approximately 75° F. (24° C.) at station 61 . Here again, many options are available for heating. Hot air, additional flame heaters, gas fired infrared panels and electric ceramic panels were all tested and found to be either too slow or difficult to control. It was found that an electrically heated flat fused quartz emitter plate 61 ′ with zonal band control for localized label transfer would provide maximum free air transmission of infra-red energy without the effects of ambient environmental factors. With an emissivity of 0.9 for polyethylene a desired emitter plate temperature of between 1652° F. (900° C.) to 1725° F. (940° C.) will emit the most efficient wavelength (2.5 to 3.2 μm) of infra-red energy to peak absorption. The unit tested was rated at 60 watts per square inch. The time to heat the polyethylene surface the necessary 75° F. (24° C.) was 4.5 seconds at a distance from the emitter plate of 2.5 centimeters.
Station 62 illustrates the method of label application whereby the printed ink materials are transferred from the polypropylene film substrate to the polyethylene surface utilizing the tactile characteristics of the heat activated adhesive to overcome the bond of the transfer layer to the corona treated silicone coating. The factors that influence transfer are time to contact, temperature during contact, applied pressure and film tension during contact particularly tension of the film after ink release. The diameter of pressure roll 63 is also a factor but not a variable. For this application the roll diameters are 38 mm. The roller 63 was made of silicone rubber over a steel core, with rubber durometer ranging from 50 Shore A to 80 Shore A. It should be noted that distortion (flattening) of the rubber roller is less at a higher durometer, consequently the contact area is less and the transfer pressure is greater. This is important at the higher line speeds where contact time is minimized. Thus a crate moving 18.3 meters per minute (60 feet per minute) past a roller of 38 mm diameter will. have a contact time of 1 millisecond per 1 degree of roller rotation where there is no roller distortion.
Roller pressure is provided by an air cylinder 64 activated by a conventional solenoid valve which in turn is operated by two (2) proximity switches, one to advance the roller and the other to retract. Other means, such as mechanical linkage are obvious and will not be listed here. The pressure is distributed across the length of the cylinder and for this particular ink, transfer ranges from 12 to 17 kilograms per centimeter of roller length are desirable.
Thus the invention results in the film being advanced at exactly the same rate as the crate is moving past the roller by virtue of the heat activated adhesive adhering to the high energy crate surface. The pressure roller 63 , which rotates freely, maintains the same tangential speed as the linear speed of the film and crate. Thus the ink is transferred completely and without distortion.
For purposes of fast and complete adhesion the pressure roller 63 is molded to a hollow core. Suspended within the hollow core is a resistance heater operated through a controller. The heating element, rated at 500 W, will maintain the roller surface at any predetermined temperature. For purposes of the invention, the roller surface temperature range between 250° F. and 370° F. (120° C. and 190° C.).
Many silicone coated polymer films may be used for the printed substrate. High temperature films such as polyester may be operated in continuous contact with the heated roller. Low temperature films such as polypropylene must be prevented from contacting the heated roller during pauses in the labelling operation. To accomplish this, film guides 65 are used to support the film when the roller is retracted. The guides 65 are mounted to maintain a clearance of approximately 13 mm between the guides and the labelled surface. At the same time the roller is retracted approximately 13 mm behind the film. By maintaining these clearances, stretching and distortion of the film such as polypropylene is avoided. High temperature films would not require the guides.
It has also been discovered that film tension, especially on the film exit side of the roller, is important to complete ink transfer. Through trials, it was found a continuous tension of approximately 2.5 kilograms is useful. This is achieved through a spring loaded dancer arm and roller.
Conventional nip rollers and stepping motor are used to advance the film to the next label and position it accurately, using a printed mark to trigger an optical scanning device.
Protection of the ink against scratching by casual handling as well as insuring its weatherability when subjected to outdoor storage is achieved with the application of an acrylic based wax emulsion at station 66 . This is applied by a roll applicator 68 which is supplied from a wet roller with a controlled amount of coating. Control is achieved with a doctor blade. The coating extends well past the edges of the ink pattern and seals the edges from intrusive moisture.
The final processing step is to coalesce the layers of the coating, label ink, and adhesive at station 67 by means of flame heater 67 ′ and also to inter diffuse the adhesive layer with the polyethylene substrate formed by the crate 59 . This discovery was made through extensive trials of many heating systems. As flame treatment was discovered to be the best technique that would provide the required surface energy for label adhesion, so it was discovered that flame treatment of the label and coating composite was the best technique that would develop the required water immersion durability without sacrificing mechanical properties or altering the visual characteristics of the applied label, or distorting the polypropylene crate 59 .
FIG. 2 shows the technique of surface treatment and temperature stabilization.
FIG. 3 illustrates the method of label application whereby the printed ink materials are transferred from the polypropylene film substrate to the polyethylene surface utilizing the tactile characteristics of the heat activated adhesive to overcome the bond of the ink layer 14 to the corona treated silicone coating 12 .
Protection of the ink against scratching by casual handling as well as insuring its weatherability when subjected to outdoor storage is achieved with the system described in FIG. 4 .
The final processing step is to coalesce the layers of the coating, label ink, and adhesive and also to inter diffuse the adhesive layer with the polyethylene substrate as shown in FIG. 5 .
FIG. 7 shows a schematic side view of a crate washing apparatus for removing the transfer layers according to the present invention from crates 112 that are supplied to the crate washer 110 via a transport conveyor 111 . Crates 112 are first transported to pre-rinsing station 113 and sprayed with a pre-rinsing solution which is applied from a number of nozzles 114 located above and below the transport conveyor 111 . The speed of the conveyor 111 is such that the dwell time of the crate 111 in the pre-rinsing station is between 6 and 8 seconds. The temperature of the pre-rinse solution is 60° C. The pre-rinse solution preferably comprises a 0.5% NaOH solution.
After passing through the pre-rinsing station 113 , the crates are transported through a soaking station 115 via a downwardly sloping section 116 of the conveyor 111 . The dwell time of crate in the soaking station is between 40 and 110 seconds. In the soaking station, the crate is completely submerged and a soaking solution is recirculated in the soaking station 115 by means of nozzles 35 to cause turbulent soaking conditions. The turbulent soaking may for instance include recirculating the liquid from the soaking station 115 via the nozzles 35 at a rate of 60 m 3 /h for a total volume of the soaking solution of 5 m 3 . It is important that the labels are completely removed from the crates 112 in the soaking station 115 , without any pieces remaining on the crates. Such remaining pieces would, when dried, adhere firmly to the crates and form an undesirable contamination of the crate surface.
From the soaking station 115 , the crates are transported via the upwardly sloping conveyor track 117 to an after-rinse station 118 . The after-rinse solution may comprise water at a temperature of 30° C. The dwell time of the crates in the after-rinse station 118 is between 6 and 13 seconds.
Connected to each rinsing station 113 , 118 and to the soaking station 115 are sieving sections 120 , 121 and 122 . Each sieving section comprises a rotating belt sieve 123 , 124 , 125 , which are driven by motors 126 , 127 , 128 respectively. Pumps 129 , 130 and 131 draw the rinsing liquid and the soaking liquid from each perspective station through the rotating sieve belts 123 124 , 125 a rate of for instance 60 m 3 /h. The sieved liquids are recirculated back to nozzles 114 and 119 in the pre-rinse and after-rinse stations 113 , 118 respectively and to the soaking station 115 .
FIG. 8 shows a cross-sectional view along the lines III—III of FIG. 7 . It can be seen that the sieve belt 124 is rotated around two rollers 137 , 138 . The top end of the sieve belt 124 extends above the level of the soaking liquid in the soaking station 115 . The sieve belt 124 comprises a dual layer belt-like sieving element with a mesh size of 2 millimeters. During operation it is important to continuously rotate the sieve belt 124 to prevent the label pieces from the transfer layers that break up into pieces in the soaking station 115 , from clogging the sieve belt. A spraying nozzle 139 cleans the surface of the belt-like sieving elements by high pressure water or air jets. The removed label elements are collected in a collection compartment 140 .
It was found that a very efficient removal of labels from crates 112 is achieved by using a 0.1 to 5%, preferably a 0.5% NaOH-solution in the pre-rinsing station 113 and the soaking station 115 . However, it is also possible to apply a pre-treatment material onto the labels, prior to entry into the crate washer 110 , which acts to soften the label prior to entry into the crate washer. For instance. a surface active component can be sprayed onto the crates 112 when travelling to the crate washer 110 . It is also possible to apply a gel-like material of a chemical composition which starts attacking the label prior to entry into the crate washer 10 . In such a case it may be possible to use water only in the crate washer 110 , instead of the alkaline solution.
It is preferred that the properties of the label and the conditions in the crate washer are such, that the label breaks up into at least 4 pieces, which can be sieved from the water in the crate washer within a soaking time of not more than 20 minutes, preferably, within 10 seconds.
To illustrate the various properties which influence the adherence and the washability of the preferred transfer layer according to the present invention, the following tests were carried out, including a washing trial, a pencil scratch test, a water uptake/release test and a water vapour transmission rate test as described hereafter.
Washing Trial
To determine the optimum washing conditions for the labels according to the present invention, a label 50 was applied to a polyethylene crate. The dimensions of the label were about 10 by 10 centimeter and the adhesive layer 54 was a 100% urethane adhesive with a tack temperature of 79° C. The labels were applied to the crate with a temperature of roller 63 in FIG. 6 of 155° C. at a roller pressure of 2.5 bar. The pre-heat temperature of the crate (in stations 60 and 61 of FIG. 6 ), was 75° C. The speed of the crates 59 through the label applicator was 40 crates per minute. To determine the influence of the post-treat temperature with which the crates after label application were heated in station 67 of FIG. 6, post-treat temperatures of 40° C., 65° C. and 90° C. were used. After label application the crates were stored for at least 24 hours at a temperature of 20° C. The crates to which a label was applied, were thereafter soaked in a 0.5% NaOH-solution at temperatures of 20, 50 and 70° C.
The soaking of the crates was carried out in a soaking bath of 20 liters without turbulence, for such a soaking time (10-50 seconds) that after spraying the soaked crate with a showerhead at a rate of 6 liters/minutes, the label was completely removed within 2 seconds.
A second set of crates was prepared wherein after label application, a coating layer of wax was applied, such as at station 66 of FIG. 6 .
The results of the soaking times required for label removal within 2 seconds, versus the water permeability coefficient and the post-treatment temperature. are given in tables I and II. From table I it can be seen that for labels to which no wax layer was applied the soaking time decreases drastically at temperatures of the soaking solution above 20° C. For post-heat temperatures of 90°, the durability of the label increased and the soaking times remain above 5 seconds.
TABLE I
crate washing trial
(no wax layer applied)
0.5% caustic
T
postheat
Time
Time
Time
Average
(° C.)
(° C.)
WPC
(sec)
(sec)
(sec)
(sec)
20
none
—
90
120
105
40
—
180
150
165
65
—
210
240
225
90
—
480
420
450
50
none
—
2
2
2
2
40
—
3
3
3
3
65
—
3
3
4
3.4
90
—
15
14
13
14
70
none
—
1
1
1
1
40
—
1
1
1
1
65
—
1
1
1
1
90
—
6
6
7
6.3
It was found that an optimum post-heat temperature was between 65° C. and 90° C. At a post-heat temperatures below 65° C., too little coalescing of the applied transfer layer was achieved, such that the applied transfer layers had insufficient durability and could be too easily removed during storage and use. At post-heat temperatures higher than 90° C., the durability of the transfer layer became too large, and quick removal times could not be achieved in an economically feasible manner. During the spraying period with the showerhead, it was observed that after soaking, the labels detached from the crate and broke up in several (2 to 4) pieces.
When prior to the flame treatment step at station 67 in FIG. 6 a wax layer is applied at station 66 , the water permeability coefficient is decreased and the durability of the labels is improved, and soaking times are increased. From table II it can be seen that for a 0.5% caustic solution, the wax coating leads to longer soaking times.
TABLE II
crate washing trial
(with wax layer applied)
0.5% caustic
T
postheat
Time
Time
Time
Average
(° C.)
(° C.)
WPC
(sec)
(sec)
(sec)
(sec)
20
none
—
150
150
150
40
—
180
180
180
65
0.7
300
270
285
90
—
<600
600
50
none
—
4
4
5
4.3
40
—
6
6
6
6
65
0.7
7
7
8
37.3
90
—
13
14
16
14.3
70
none
—
2
2
3
2.3
40
—
2
2
2
2
65
0.7
2
2
2
2
90
—
6
6
7
6.3
It was observed that by trying to remove the labels as were tested in the washing trial described above, solely with high pressure water jets at 20° C. and at a pressure of 120 bar, at a conveyor speed of 15 meters per minutes and a spraying angle of 90° at a distance of 10 centimeters, no label removal was achieved. Even for labels without any wax coating and no post-heat treatment, no removal by means of high-pressure water jets was possible.
Pencil Scratch Test
The purpose of the pencil scratch test is to identify the minimum and maximum durability of a label which can be obtained by taking different measures such as the use of a covering wax layer and heat treatment to cause coalescing of the label layers. Crates with labels which were applied with different post-heating temperatures, with and without wax, have been tested.
The labels were the same labels as used in the washing trial described above, and were applied to the crates under the same conditions.
The pencil scratch tests were carried out with a “scare resistance test model 435” supplied by Erichsen (PO Box 720, D-5870 Hemer Germany).
During the scratch test, a pencil with a plastic insert was used to scratch the label at an angle of 90° horizontally in the middle thereof.
After label application, the crates were stored for at least 24 hours at a temperature of 20° C. Prior to scratching, the crates were soaked in a water without turbulence at 20° C. The results of the scratch test are given in tables III and table IV in which the scratch results are given in N.
TABLE III
Pencil scratch test (in N)
label without wax coating
Post-heat
Temperature
soaking time (min)
(° C.)
WPC
0
0.5
1
1.5
2
2.5
3
3.5
none
—
1
0.4
0.2
0.1
1
0.3
0.2
0.1
40
—
1.3
0.9
0.2
0.1
1.1
0.7
0.2
0.1
65
—
1.1
0.7
0.2
0.1
1
0.5
0.1
0.1
90
—
1.5
1.2
0.8
0.6
0.6
0.4
0.2
0.1
1.1
1
0.8
0.6
0.5
0.3
0.2
0.1
TABLE IV
Pencil scratch test (in N)
label with wax coating
Post-
treat
soaking time (min)
(° C.)
0
0.5
1
1.5
2
2.5
3
4
5
6
7
8
9
10
none
5
3
1.4
0.5
0.3
0.2
0.1
5
3
1.5
0.7
0.4
0.2
0.1
40
5
2.8
1.3
0.4
0.3
0.1
5
3
1.4
0.6
0.4
0.2
0.1
65
5
2.5
1.2
0.5
0.3
0.2
0.1
5
2.9
1.3
0.5
0.2
0.1
90
5
4
2.5
1.3
0.7
0.7
0.6
0.4
0.4
0.4
0.3
0.3
0.3
0.3
5
1
2.8
1.5
0.8
0.7
0.5
0.3
0.3
0.3
0.2
0.2
0.2
0.2
From table III and IV it can be seen that the post-heat flame treatment does not seem to influence the scratch resistance of the label significantly. From table IV it appears that application of a wax layer covering the label, decreases the water permeability coefficient and improves the scratch resistance of the dry label significantly. It was found that for high post-heat flame treatment temperatures of 110° C. in combination with a wax coating, a scratch force of 8 Newton was achieved. Labels with a pencil hardness of 8 Newton are considered to be semi-permanent labels which cannot be removed in an economically feasible manner.
Also at post-heat temperatures above 90° C., problems occurred during labelling as at these temperatures the polyethylene crates became brittle after a few applications, the crate pigments were found to discolor and deformations of the softened crates on the conveyor and the pelletizer were found to occur.
At a post-heat temperature below 65° C., the strength of the labels was found to be insufficient for labels which did not have a wax coating. For labels without a wax coating the target pencil hardness in the dry state should be around 1.2 N and the soaking time until the scratch force drops below 0.3 Newton should be below 3 minutes. For a wax coated label, the target scratch force should be about 5 Newton in the dry state and the soaking time until the scratch force drops below 0.3 N should be below 10 minutes. Transfer layers having the above properties were found to have an optimal combination of durability and washability.
Water Uptake Test
The labels according to the present invention can be easily removed from a container, in particular from a plastic crate due to their specific water permeability which allows the soaking solution to penetrate the label, and subsequently break up the label in pieces and detach it from the container. It was found that preferred labels have a water permeability coefficient of about 0.5, corresponding to a water absorption of around 5 g/m 2 after 3 hours, in a water uptake test as described below. Labels according to the invention have a water uptake value higher than 0, preferably higher than 1 and less than 100, preferably less than 75 g/m 2 after 24 hours. The water release of a preferred label was 4.5 g/m 2 within 30 minutes in the water release test as described below. Preferred labels according to the present invention will have a water release value greater than 0 and less than 100 g/m 2 in hours.
Two samples were prepared, each sample containing 2 labels of a thickness of 12.7 μm each at 22.4° C. and 48% relative humidity, each sample having a surface area of 85.8 cm 2 . For each sample, two labels were applied on a single piece of clear glass of 3 inch×9 inch×0.02 inch. Due to the extremely low weight of the labels it was necessary to apply two labels per piece of glass to obtain a weight that would register within the range of a two decimal place electronic gram scale.
The samples were prepared as follows: the glass supports were thoroughly cleaned and placed in a heating oven until an approximate temperature of 130° C. was reached on the glass surface. The glass was then removed from the heating oven and placed on a silicone rubber mat. A label was immediately set on the glass and secured to the surface by the use of a silicone roller. Rolling pressure was continually supplied to the full length of the label until all entrapped air was removed (approximately 5-6 back and forth motions). After the glass had cooled, the carrier film was removed. Thereafter the opposite side of the glass plates were labelled by heating a clean aluminum plate (slightly larger than the glass plate) to approximately 131° C. in a convective oven, then placing the glass on the surface of the aluminum plate (label surface down) which allowed the heating of the glass upper surface. The label was then applied and secured in place by the silicone roller as described above. Once again, when the glass cooled, the carrier film was removed. Next a wax coating having a dry weight of 0.043 grams was applied to the surface of both labels. In the final step, using a propane oxidizing flame, flame treatment was applied to both labels by quickly passing the flame across the entire surface of the label sample. Once the samples were cooled the labels were ready for the Water Uptake test.
A stainless steel immersion tank of a 33.66 centimeter diameter and 24.13 centimeter height was filled with the deionized water. Care was taken that the water level was deep enough to allow total immersion of the sample. The sample was placed with the short dimension set perpendicular to the bottom of the tank. The glass supports were placed on a thin wire frame in the immersion tank. A thermocouple was installed inside the water immersion tank. After each time period, as given in table V, the sample was removed from the tank, excess surface water was blotted dry, the sample was weighted and placed back in the tank. This procedure was continued for the duration of the test. The results are shown in table V. With regard to sample 1, this sample reached it maximum absorption of 0.04 grams at the 3 hour mark and maintained this level to the 5 hour mark. After the 5 hour period the label lost its ability to hold water. We believe this phenomenon was caused because of label structure degradation. For sample 2, this sample also reached its maximum absorption of 0.04 grams at a 3 hour mark. At the 5 hour mark this sample was terminated from further testing in preparation for the water release test described below.
From the water uptake test, at can be deduced that a preferred label of a thickness of 12.7 microns has a water uptake value of 0.04 g/85.8 cm 2 or about 5 g/m 2 after 3 hours at room temperature.
TABLE V
Water Uptake Test
Sample 1
Sample 2
Tank
Weight
Weight
Water
in
in
Tempera-
Time
grams
grams
ture (° F.)
8:00
59.77 g
59.77 g
71
a.m.
8:10
59.80 g
59.80 g
71
a.m.
9:00
59.81 g
59.81 g
71
a.m.
10:00
59.83 g
59.83
71
a.m.
11:00
59.85 g
59.85 g
72
a.m.
12:00
59.85 g
59.85 g
72
p.m.
1:00
59.85
72
p.m.
2:00
59.84 g
72
p.m.
3:00
59.81
72
p.m.
Water Release Test
Immediately after the conclusion of the above Water Uptake Test the sample 2 as prepared above was subjected to the water release test. The sample was blotted to remove access water, weighted and the data were recorded. The sample was first exposed to ambient temperature for one half hour and weighed. Half an hour after weighing the sample, it was placed in a prewarmed (53° C.) test oven (small electrically heated oven, Quieny Lab Inc., Model 20 Lab oven or equivalent). The sample was left in the prewarmed oven for more than one hour and weighted. Thereafter the sample was placed back in the test oven and remained there for 3.5 hours.
From table VI it can be concluded that the water absorbed by sample 2 was released within 30 minutes exposure to ambient room temperature and humidity (48%). In fact, the sample registered a weight loss of 0.01 grains from its original weight which could seem to indicate that the label was not thoroughly dried at installation. So a preferred label of 85.8 cm 2 size and 12.7 μm thickness has water release greater than 0 and less than 0.10 g/24 hours with a mean release of 0.045 g within 30 minutes given these parameters.
TABLE VI
Water Release Test
Sample 2
Room
Oven
Weight in
Temperature
Relative
Temperature
Time
Grams
(° F.)
Humidity
(° C.)
12:00
59.85 g
72.6
48
53.5
p.m.
12:30
59.76 g
72.6
45
53.7
p.m.
1:30
59.76 g
52.3
p.m.
Next
59.76 g
53.0
Reading
5:00
a.m.
Water Vapor Transmission Rate Test
The optimum combination of durability and washability of the labels according to the invention is at least partly due to the permeability of the label for the soaking solution. A sample of the transfer layer of the sane type as tested in the water uptake/release test of a thickness of 12.7 μm (microns) was tested for water vapour transmission. A 25 milliliter glass container with a 15.9 milliliter orifice was cleaned with acetone and filled with approximately 10 milliliters of deionized water. The orifice area of the container was heated to approximately 47.8 (118° F.) and a circle segment of the transfer layer was firmly applied using a small piece of silicone rubber as a pressure pad. After the container/label had cooled, the backing film was gently removed. The sample preparation was completed by adding a wax coating (0.001 g across the 1.99 cm 2 surface) and let air dry. A second glass container of the same dimensions as described above was cleaned thoroughly with acetone and filled with 10 ml of deionized water. The orifice area of the sample was heated as well. This sample was used as the control sample. The completed samples were then weighted various intervals over a 26.6 hour time period. The water vapour transmission rate over the total time of the experiment equated to 568.75 g/m 2 in a 24 hour time period at 22.2° C. at 46% relative humidity. It was found that a “steady state” water vapour transmission rate was not achieved until approximately 28 minutes from time 0. when using the “steady state” data after 28 minutes from time 0, the water vapour transmission rate was found to be about 525 g/m 2 in 24 hours.
For the control sample without a label, a water vapour transmission rate over the total time of the experiment of 1085.7 g/m 2 in 24 hours was found. The water vapour transmission rate of the preferred label according to the present invention will lay between 50 and 750 g/m 2 after 24 hours (22.2° C., 44% relative humidity), preferably around 500 g/m 2 after 24 hours.
It will Le appreciated that further modifications could be made to the embodiment disclosed above, while still obtaining many of the advantages and without departing from the scope of the invention as defined in the appended claims. | The invention is directed to an ink-only label at least consisting of an adhesive layer, an ink-only image layer and optionally a protective layer, wherein the label, when applied to a substrate, has a water permeability coefficient, as defined herein, which is sufficient to enable fast removal of the label from the substrate with water or an aqueous alkaline solution, without destructive treatment of the said substrate. | 8 |
CROSS-REFERENCE TO RELATED APPLICATIONS
[0001] This patent application claims the benefit of co pending U.S. Provisional Patent Application Nos. 61/573,900, 61/573,957, 61/573,958, 61/573,956, 61/573,955, 61/573,954, 61/573,953 and 61/573,952, all filed on Sep. 14, 2011, the disclosures of which are hereby incorporated by reference in their entireties.
FIELD OF THE INVENTION
[0002] The present invention is generally directed toward the treatment of water and, more particularly, toward the treatment of water containing large amounts of dissolved solids as may result, for example, from use of the water as a fracking fluid used in drilling gas wells. However, the embodiment proposed herein may be used in any situation where impurities to be removed from water exist.
BACKGROUND OF THE INVENTION
[0003] Ensuring a supply of potable water has been a frequent concern in many locations. Further concerns arise about the environmental impact of the disposal of contaminated water.
[0004] Conventional water treatment techniques for such purposes as, for example, municipal water treatment and/or obtaining potable water from sea water are known and are successful in many instances. However, some current activities show those techniques to have limited cost effectiveness.
[0005] For example, mining with water used to fracture rock or shale formations to recover natural gas (e.g., in the shale regions in the United States and western Canada including, but not limited to, Pennsylvania, Maryland, New York, Texas, Oklahoma, West Virginia and Ohio) requires a very large amount of water input and a significant amount of return (flowback) water that contains a great deal of contaminants and impurities. In order for this flowback water to be used in an environmentally responsible manner, it needs to be relatively free of contaminants/impurities. Water used, for example, in natural gas well drilling and production may contain organic materials, volatile and semi-volatile compounds, oils, metals, salts, etc. that have made economical treatment of the water to make it potable or reusable, or even readily and safely disposable, more difficult. It is desirable to remove or reduce the amount of such contaminants/impurities in the water to be re-used, and also to remove or reduce the amount of such contaminants/impurities in water that is disposed of.
[0006] The present invention is directed toward overcoming one or more of the above-identified problems.
SUMMARY OF THE INVENTION
[0007] The present invention can take numerous forms among which are those in which waste water containing a large amount of solids, including, for example, dissolved salts, is pressurized to allow considerable heat to be applied before the water evaporates, and is then subjected to separation and recovery apparatus to recover relatively clean water for reuse and to separate solids that include the afore-mentioned dissolved salts. In some instances, the concentrated solids may be disposed of as is, e.g., in a landfill. Where that is not acceptable (e.g., for reasons of leaching of contaminants), the concentrated solids may be supplied to a thermal, pyrolytic, reactor (referred to herein as a “crystallizer”) for transforming them into a vitrified mass which can be placed anywhere glass is acceptable.
[0008] Particular apparatus for systems and processes in accordance with the present invention can be adapted from apparatus that may be presently currently available, but which has not been previously applied in the same manner. As an example, conventional forms of flash evaporation equipment, such as are used for treating sea water, in one or in multiple stages, may be applied herein as a salts concentration apparatus. Likewise, conventional forms of gasification/vitrification reactors, such as are used for municipal solid waste (“MSW”) processing including, but not limited, to plasma gasification/vitrification reactors, may be applied for final separation of the contaminants from the water and for initial heating of the waste water.
[0009] The present disclosure presents examples of such systems and processes in which, in one or more successive concentration stages, steam output of a flash evaporator used to concentrate salts is raised in pressure by mechanical vapor compressors from a low level (e.g., 5 psia) to a substantially higher level (e.g., 150 psia), accompanied by elevation of the steam temperature. The steam is applied to heat incoming waste water for treatment and permits use of a smaller and less expensive heat exchanger than would be needed without such pressurization.
[0010] Additionally, in some examples, steam from one or more stages of salts concentration is pressurized (e.g., from 5 psia up to 150 psia) before applying the steam to a stripper to remove, for example, volatile organic compounds (“VOCs”), and making the water available for reuse in a prior or subsequent stage and the VOCs available for reaction in a pyrolytic (e.g., plasma) reactor or crystallizer.
[0011] In addition, examples can include use of a turbine to expand steam (e.g., having an input of steam exiting a reactor or crystallizer at 150 psia and an output of steam at 15 psia) which goes then to a VOC stripper for use as described above. A turbine, or the like, for steam pressure reduction generates power or mechanical energy that reduces overall energy consumption.
[0012] Such uses of compressors and turbines, while adding some additional initial costs, can save significant operating costs.
[0013] The present disclosure, among other things, also presents examples of such systems and processes in which, in one or more successive concentration stages, steam output from a flash evaporator used to concentrate salts is reduced in pressure from, for example, 150 psia input pressure to 25 psia output pressure, and the output steam is then sent to the stripper. The steam from the crystallizer (e.g., at 180 psia) is sent back to heat the pressurized waste water in each stage. A portion of the steam from the crystallizer is sent to the stripper after expanding in a turbine (e.g., a mechanical vapor turbine). A turbine is used to expand this steam before sending it to a stripper of volatile organic compounds (“VOCs”).
[0014] The system and process of the present invention also includes, for example, applying saturated steam from the crystallizer to a condenser prior to flash evaporation of waste water and, therefore, a heater stage can be avoided. A preheater is used to heat incoming waste water (e.g., from 60° F. to 134° F.) by use of the condensate from the condenser.
[0015] The present disclosure, among other things, further presents examples of such systems and processes in which, in one or more successive concentration stages, steam output of a flash evaporator used to concentrate salts is reduced in pressure from, for example, 150 psia input to 5 psia downstream. The output steam is then repressurized to, e.g., 180 psia, prior to being applied to a crystallizer.
[0016] The system and process of the present invention further includes, for example, that saturated steam from the reactor/crystallizer is applied to a condenser prior to flash evaporation of waste water and, therefore, an extra heater stage can be avoided. A preheater, provided before the condenser, is used to heat incoming waste water (e.g., from 60° F. to 134° F.) by use of the condensate from the condenser.
[0017] The present disclosure, among other things, further presents examples of such systems and processes in which, in one or more successive concentration stages, waste water with dissolved solids (salts) is pressurized (e.g., from 15 psia to 400 psia) and heated (e.g., to 445° F.) before flash evaporation to a significantly lower flash pressure and temperature (e.g., 15 psia and 212° F.) and brine water with more concentrated salts.
[0018] Steam output from the concentration stages is, at least in part, supplied to a stripper to remove volatile organic compounds (“VOCs”). Additional steam from the concentration stages is pressurized (e.g., to 665 psia) prior to recycling back to the concentration stages as a heating fluid for incoming waste water.
[0019] Brine water from the concentration stages may be disposed of as is, with a significant amount of clean water recovered (e.g., as distilled water from heat exchangers of the concentration stages). Brine water may alternatively be treated in a thermal (e.g., plasma) reactor or crystallizer in order to separate the salts and recover water included in the brine water from the concentration stages.
[0020] Present examples described herein include operation of a crystallizer at a significantly higher pressure (e.g., 665 psia) than in many other thermal reactor systems in order to achieve a large temperature difference in heat exchangers of the concentration stages.
[0021] Examples described herein also include supplying saturated steam from the crystallizer directly to condensers of the concentration stages, from each of which it is then applied as a heating fluid of a preheater for the waste water. Such a system will not normally require any additional heating of the waste water prior to flash evaporation.
[0022] The present disclosure, among other things, presents examples of such systems and processes in which, in one or more concentration stages, waste water with dissolved solids (salts) is pressurized (e.g., to 400 psia) and heated (e.g., to 445° F.) before flash evaporation in a single flash evaporator to which multiple concentration stages supply waste water in parallel. For example, the waste water is split into three equal flows that are individually pressurized and heated prior to being subjected to flash evaporation together.
[0023] The flash evaporator produces steam that is then usable as a heating medium and brine water with more concentrated salts than the original waste water.
[0024] The resulting combined brine water from the concentration stages may be disposed of as is, with a significant amount of clean water recovered (e.g., as distilled water from heat exchangers of the concentration stages). Brine water may alternatively be treated in a pyrolytic (e.g., plasma) reactor or crystallizer in order to separate the salts and recover water included in the brine water from the concentration stages.
[0025] Where a crystallizer is used, it can provide superheated steam (developed from steam from the single, or plural, flash evaporator(s)) that is applied directly to condensers of the concentration stages, from each of which it is then applied as a heating fluid of a preheater for the waste water. Such a system will not normally require additional heating of the waste water prior to flash evaporation.
[0026] While the another embodiment of the present invention is described with respect to FIGS. 17-20 as including stages operating in parallel, it should be understand that any of the stages of the other embodiments may also be operated in parallel without departing from the spirit and scope of the present invention. Additionally, the embodiment of FIGS. 17-20 may also be operated in series.
[0027] A system for treating waste water is disclosed, the system including: a pump receiving waste water at a first pressure and a first temperature and pressurizing the received waste water to a second pressure greater than the first pressure, the waste water comprising dissolved solids, volatile organic compounds and other components generally and collectively called impurities; first and second preheaters receiving the pressurized waste water from the pump and preheating the pressurized waste water in successive stages to a second temperature greater than the first temperature to produce pressurized/preheated waste water, each of the first and second preheaters producing distilled water without boiling of the waste water across heat transfer surfaces; a condenser receiving the pressurized/preheated waste water and further heating the pressurized/preheated waste water to a third temperature greater than the second temperature to produce a pressurized/further heated waste water without boiling of the waste water across heat transfer surfaces; a heater receiving the pressurized/further heated waste water and still further heating the pressurized/further heated waste water to a fourth temperature greater than the third temperature to produce pressurized/heated waste water without boiling of the waste water across heat transfer surfaces; and an evaporator, operated at a third pressure less than the second pressure, removing dissolved solids from the pressurized/heated waste water by evaporation caused by depressurization of the waste water to produce steam and brine water, wherein the brine water has a total dissolved solids content greater than a total dissolved solids content of the received waste water, wherein steam from the evaporator is superheated to a fifth temperature greater than the fourth temperature and is used as a heat source by at least one of the heater, condenser and second preheater without boiling of the waste water across heat transfer surfaces.
[0028] The second pressure may be approximately 120-180 psia, and the third pressure may be approximately 4-6 psia.
[0029] The fourth temperature may be approximately 286-430° F., and the firth temperature may be approximately 400-600° F.
[0030] In one form, the pump, first and second preheaters, condenser, heater and evaporator comprise a stage, and wherein the system comprises multiple stages with the brine water output by one stage used as the received waste water of a next stage. The brine water output by each stage has a total dissolved solids content that is higher than that of a previous stage.
[0031] In another form, the system further includes a crystallizer crystallizing the brine water to produce a solid mass of waste product and steam, which may be a vitrified glass. The steam from the crystallizer may be mixed with steam from the evaporator and superheated to the fifth temperature, wherein the mixed and superheated steam may be used as a heat source by at least one of the heater, condenser and second preheater without boiling of the waste water across heat transfer surfaces.
[0032] In a further form, the crystallizer includes a plasma crystallizer and includes a plasma torch for vaporizing the water from the brine water and producing the solid mass of waste product and steam. The system further includes a stripper initially receiving the waste water and removing volatile organic compounds from the waste water prior to the waste water being pressurized by the pump, wherein the removed volatile organic compounds are used as a heat source by the plasma torch to crystallize the brine water. The steam produced by the evaporator, when cooled, produces distilled water. Additionally, the steam produced by the evaporator may be used as a heat source by the stripper without boiling of the waste water across heat transfer surfaces. The steam produced by the evaporator may also be used as a heat source by the first preheater without boiling of the waste water across heat transfer surfaces.
[0033] In yet a further form, the pump, first and second preheaters, condenser, heater and evaporator comprise a stage, and wherein the system comprises multiple stages operating in parallel with each receiving a portion of the waste water. The brine water output by each stage has a total dissolved solids content that is higher than that of the received waste water. The brine water from each stage is combined and supplied to the crystallizer which crystallizes the brine water to produce a solid mass of waste product and steam.
[0034] In still a further form, the pump, first and second preheaters, condenser, heater and evaporator comprise a stage, wherein the system comprises multiple stages with the brine water output by one stage used as the received waste water of a next stage, and wherein the received waste water at stages subsequent to a first stage is at a third pressure less than the first pressure.
[0035] A system for treating waste water is also disclosed, the system including: a pump receiving waste water at a first pressure and a first temperature and pressurizing the received waste water to a second pressure greater than the first pressure, the waste water comprising dissolved solids, volatile organic compounds and other components generally and collectively called impurities; a preheater receiving the pressurized waste water from the pump and preheating the pressurized waste water to a second temperature greater than the first temperature to produce pressurized/preheated waste water without boiling of the waste water across heat transfer surfaces; a condenser receiving the pressurized/preheated waste water and further heating the pressurized/preheated waste water to a third temperature greater than the second temperature to produce a pressurized/heated waste water without boiling of the waste water across heat transfer surfaces; an evaporator, operated at a third pressure less than the second pressure, removing dissolved solids from the pressurized/heated waste water by evaporation caused by depressurization of the waste water to produce steam and brine water, wherein the brine water has a total dissolved solids content greater than a total dissolved solids content of the received waste water; and a crystallizer, operated at a fourth pressure greater than the second pressure, receiving the brine water and crystallizing the brine water to produce a solid mass of waste product and steam, wherein steam from the crystallizer, at the fourth pressure and a fourth temperature greater than the third temperature, is used as a heat source by at least one of the condenser and preheater without boiling of the waste water across heat transfer surfaces, and wherein steam from the evaporator is used as a heat source by the crystallizer without boiling of the waste water across heat transfer surfaces.
[0036] In one form, the first pressure may be approximately 11.8-17.6 psia, and the first temperature may be approximately 480-72° F.
[0037] In one form, the second pressure may be approximately 120-180 psia, and the third temperature may be approximately 288-432° F.
[0038] In one form, the second pressure may be approximately 320-480 psia, and the third temperature may be approximately 356-534° F.
[0039] In one form, the third pressure may be approximately 20-30 psia, the fourth pressure may be approximately 144-216 psia, and the fourth temperature may be approximately 298-448° F.
[0040] In one form, the third pressure may be approximately 4-6 psia, the fourth pressure may be approximately 144-216 psia, and the fourth temperature may be approximately 298-448° F.
[0041] In one form, the third pressure may be approximately 12-18 psia, the fourth pressure may be approximately 532-798 psia, and the fourth temperature may be approximately 400-600° F.
[0042] In another form, the crystallizer includes a plasma crystallizer and includes a plasma torch for vaporizing the water from the brine water and producing the solid mass of waste product and steam. The system further includes a stripper initially receiving the waste water and removing volatile organic compounds from the waste water prior to the waste water being pressurized by the pump, wherein the removed volatile organic compounds are used as a heat source by the plasma torch to crystallize the brine water without boiling of the waste water across heat transfer surfaces.
[0043] In a further form, the system further included a mechanical vapor turbine receiving the steam from the crystallizer and reducing its pressure to the third pressure, wherein the reduced pressure steam is combined with the steam from the evaporator and used as a heat source by the stripper.
[0044] In yet a further form, the system further includes a mechanical vapor compressor receiving the steam from the evaporator and increasing its pressure to the fourth pressure, wherein the increased pressure steam is combined with the steam from the crystallizer and used as a heat source by at least one of the condenser and preheater without boiling of the waste water across heat transfer surfaces.
[0045] In still a further form, the pump, preheater, condenser and evaporator comprise a stage, and wherein the system comprises multiple stages with the brine water output by one stage used as the received waste water of a next stage, and wherein the brine water output by a last stage is input to the crystallizer. The brine water output by each stage has a total dissolved solids content that is higher than that of a previous stage.
[0046] In an additional form, the pump, preheater, condenser and evaporator comprise a stage, and wherein the system comprises multiple stages operating in parallel with each stage receiving a portion of the waste water, and wherein the brine water from each stage is combined and supplied to the crystallizer. The brine water output by each stage has a total dissolved solids content that is higher than that of the received waste water.
[0047] In yet and additional form, the pump, preheater, condenser and evaporator comprise a stage, wherein the system comprises multiple stages with the brine water output by one stage used as the received waste water of a next stage, and wherein the received waste water at stages subsequent to a first stage is at the third pressure.
[0048] A method of treating waste water is also disclosed, the method including the steps of: (a) receiving waste water at a first pressure and a first temperature, the waste water comprising dissolved solids, volatile organic compounds and other components generally and collectively called impurities; (b) pressurizing the received waste water to a second pressure greater than the first pressure; (c) preheating the pressurized waste water to a second temperature greater than the first temperature, wherein said preheating step is performed by first and second preheaters in successive stages to produce pressurized/preheated waste water, each of the first and second preheaters producing distilled water without boiling of the waste water across heat transfer surfaces; (d) heating the pressurized/preheated waste water to a third temperature greater than the second temperature to produce a pressurized/heated waste water without boiling of the waste water across heat transfer surfaces; (e) further heating the pressurized/heated waste water to a fourth temperature greater than the third temperature to produce pressurized/further heated waste water without boiling of the waste water across heat transfer surfaces; and (f) removing, by evaporation caused by depressurization of the waste water, dissolved solids from the pressurized/further heated waste water by an evaporator operated at a third pressure less than the second pressure to produce steam and brine water, wherein the brine water has a total dissolved solids content greater than a total dissolved solids content of the received waste water, wherein steam from the evaporator is superheated to a fifth temperature greater than the fourth temperature and is used as a heat source in at least one of steps (c)—by the second preheater, (d) and (e) without boiling of the waste water across heat transfer surfaces.
[0049] The second pressure may be approximately 120-180 psia, and the third pressure may be approximately 4-6 psia.
[0050] The fourth temperature may be approximately 286-430° F., and the firth temperature may be approximately 400-600° F.
[0051] In one form, steps (a)-(f) comprise a stage, and wherein the method is performed in multiple stages with the brine water output by step (f) in one stage used as the received waste water in step (a) of a next stage. The brine water output in step (f) of each stage has a total dissolved solids content that is higher than that of a previous stage.
[0052] In another form, the method further includes the steps of: (g) crystallizing the brine water to produce a solid mass of waste product and steam. The steam produced by step (g) is mixed with steam produced by step (f) and superheated to the fifth temperature, wherein the mixed and superheated steam may be used as a heat source in at least one of steps (c)—by the second preheater, (d) and (e) without boiling of the waste water across heat transfer surfaces. A plasma crystallizer using a plasma torch may be used to crystallize the brine water. The solid mass may include a vitrified glass of the salts in the brine water.
[0053] In a further form, the method further includes the steps of: (b′) prior to step (b), removing the volatile organic compounds from the received waste water, wherein the removed volatile organic compounds are used as a heat source by the plasma torch to crystallize the brine water. The steam produced by step (f) may be used as a heat source in step (b′). The steam produced by step (f) may be used as a heat source in step (c)—by the first preheater.
[0054] In yet a further form, steps (a)-(f) comprise a stage, and wherein the method is performed in multiple stages operating in parallel with each stage receiving a portion of the waste water. The brine water output in step (f) of each stage has a total dissolved solids content that is higher than that of the received waste water. The brine water output in step (f) of each stage is combined and supplied to a crystallizer which crystallizes the combined brine water to produce a solid mass of waste product and steam.
[0055] In still a further form, steps (a)-(f) comprise a stage, and wherein the method is performed in multiple stages with the brine water output by step (f) in one stage used as the received waste water in step (a) of a next stage, and wherein the received waste water at step (a) in stages subsequent to a first stage is at a third pressure less than the first pressure.
[0056] A method of treating waste water is also disclosed, the method including the steps of: (a) receiving waste water at a first pressure and a first temperature, the waste water comprising dissolved solids, volatile organic compounds and other components generally and collectively called impurities; (b) pressurizing the received waste water to a second pressure greater than the first pressure; (c) preheating the pressurized waste water to a second temperature greater than the first temperature to produce distilled water and pressurized/preheated waste water without boiling of the waste water across heat transfer surfaces; (d) heating the pressurized/preheated to a third temperature greater than the second temperature to produce pressurized/heated waste water without boiling of the waste water across heat transfer surfaces; (e) removing, by evaporation caused by depressurization of the waste water, dissolved solids from the pressurized/heated water, by an evaporator operated at a third pressure less than the second pressure, to produce steam and brine water, wherein the brine water has a total dissolved solids content greater than a total dissolved solids content of the received waste water; and (f) crystallizing the brine water, by a crystallizer operated at a fourth pressure greater than the second pressure, to produce a solid mass of waste product and steam, wherein steam produced by step (f), at the fourth pressure and a fourth temperature greater than the third temperature, is used as a heat source in at least one of steps (c) and (d), and wherein steam produced by step (e) is used as a heat source in step (g).
[0057] In one form, the first pressure may be approximately 11.8-17.6 psia, and the first temperature may be approximately 480-72° F.
[0058] In one form, the second pressure may be approximately 120-180 psia, and the third temperature may be approximately 288-432° F.
[0059] In one form, the second pressure may be approximately 320-480 psia, and the third temperature may be approximately 356-534° F.
[0060] In one form, the third pressure may be approximately 20-30 psia, the fourth pressure may be approximately 144-216 psia, and the fourth temperature may be approximately 298-448° F.
[0061] In one form, the third pressure may be approximately 4-6 psia, the fourth pressure may be approximately 144-216 psia, and the fourth temperature may be approximately 298-448° F.
[0062] In one form, the third pressure may be approximately 12-18 psia, the fourth pressure may be approximately 532-798 psia, and the fourth temperature may be approximately 400-600° F.
[0063] In another form, step (f) uses a plasma torch to crystallize the brine water, and wherein the method further includes the steps of: (b′) prior to step (b), removing the volatile organic compounds from the received waste water, wherein the removed volatile organic compounds are used as a heat source by the plasma torch to crystallize the brine water.
[0064] In a further form, the steam produced by step (f) is reduced in pressure to the third pressure, and wherein the reduced pressure steam is combined with steam produced in step (e) and used as a heat source in step (b′).
[0065] In yet a further form, the steam produced in step (e) in increased in pressure to the fourth pressure, and wherein the increased pressure steam is combined with steam produced in step (f) and used as a heat source in at least one of steps (c) and (d).
[0066] In still a further form, steps (a)-(e) comprise a stage, and wherein the method is performed in multiple stages with the brine water output by step (e) in one stage used as the received waste water in step (a) of a next stage, and wherein the brine water output by step (e) in a last stage is input to the crystallizer at step (f). The brine water output by step (e) of each stage has a total dissolved solids content that is higher than that of a previous stage.
[0067] In yet another form, steps (a)-(e) comprise a stage, and wherein the method is performed in multiple stages operating in parallel with each stage receiving a portion of the waste water, and wherein the brine water output by step (e) in each stage is combined and supplied to the crystallizer at step (f). The brine water output by step (e) of each stage has a total dissolved solids content that is higher than that of the waste water received at that particular stage.
[0068] In still another form, steps (a)-(e) comprise a stage, and wherein the method is performed in multiple stages operating in parallel with each stage receiving a portion of the waste water, wherein the brine water output by step (e) in each stage is combined and supplied to the crystallizer at step (f), and wherein the received waste water at stages subsequent to a first stage is at the third pressure.
[0069] Further explanations and examples of various aspects of the present invention are presented in the following disclosure.
[0070] It is an object of the present invention to provide a system and method for the economic and environmental treatment of waste water.
[0071] Various other objects, aspects and advantages of the present invention can be obtained from a study of the specification, the drawings, and the appended claims.
BRIEF DESCRIPTION OF THE DRAWINGS
[0072] Further possible embodiments are shown in the drawings. The present invention is explained in the following in greater detail as an example, with reference to exemplary embodiments depicted in drawings. In the drawings:
[0073] FIGS. 1 , 2 and 3 are schematic flow diagrams of particular examples of stages of a treatment system in accordance with the present invention;
[0074] FIG. 4 is a schematic flow diagram of an exemplary thermal reactor for use in a water treatment system in conjunction with elements such as those shown in FIGS. 1-3 in accordance with the present invention;
[0075] FIGS. 5 , 6 and 7 are schematic flow diagrams of stages of a treatment system in accordance with a further embodiment of the present invention;
[0076] FIG. 8 is a schematic flow diagram of an exemplary thermal reactor configured for use with water treatment stages such as those shown in FIGS. 5-7 in accordance with the further embodiment of the present invention;
[0077] FIGS. 9 , 10 and 11 are schematic flow diagrams of particular examples of stages of a treatment system in accordance with yet a further embodiment of the present invention;
[0078] FIG. 12 is a schematic flow diagram of an exemplary thermal reactor configured for use in a water treatment system in conjunction with treatment stages and elements such as those shown in FIGS. 9-11 in accordance with yet a further embodiment of the present invention;
[0079] FIGS. 13 , 14 and 15 are schematic flow diagrams of particular examples of stages of a treatment system in accordance with still a further embodiment of the present invention; and
[0080] FIG. 16 is a schematic flow diagram of an exemplary thermal reactor configured for use in a water treatment system in conjunction with treatment stages and elements such as those shown in FIGS. 13-15 in accordance with still a further embodiment of the present invention;
[0081] FIGS. 17 , 18 and 19 are schematic flow diagrams of particular examples of stages of a treatment system in accordance with another embodiment of the present invention; and
[0082] FIG. 20 is a schematic flow diagram of an exemplary thermal reactor configured for use in a water treatment system in conjunction with treatment stages and elements such as those shown in FIGS. 17-19 in accordance with another embodiment of the present invention.
DETAILED DESCRIPTION OF THE INVENTION
[0083] FIGS. 1 , 2 and 3 will be individually discussed, but first their general relation to each other in an exemplary multi-stage system will be described. FIG. 1 shows Stage # 1 . This first stage takes in waste water at an inlet 20 , processes it and produces first stage brine water at an outlet 30 of the first stage. The first stage brine water from the outlet 30 is input to the second stage shown in FIG. 2 (Stage # 2 ) for additional processing, and a resulting second stage brine water is produced as an output at outlet 50 . Similarly, the brine water from outlet 50 of the second stage is supplied as an input to the third stage shown in FIG. 3 (Stage # 3 ) that has additional processing, resulting in a third stage output of brine water at an outlet 70 .
[0084] It will be seen and appreciated by one skilled in the art how the successive stages of FIGS. 1 , 2 and 3 increase the concentration of salts in the brine water (e.g., Total Dissolved Solids—“TDS”). It will also be appreciated how the number of stages is a variable that can be chosen according to various factors including, but not limited to, the salts content of the original waste water and the desired salt content after concentration. In general, a system in accordance with these exemplary embodiments may include any one or more stages such as are shown, for example, in FIGS. 1-3 . The examples presented herein are merely illustrative of systems and methods that may be chosen not merely for good technical performance but also for reasons relating to economic factors, such as, for example, initial capital cost and operating cost, as well as convenience factors, such as, for example, space requirements and portability. While three stages are shown and described herein, one skilled in the art will appreciate that any number of stages may be utilized depending on the particular application without departing from the spirit and scope of the present invention.
[0085] Each of the FIGS. 1-4 , merely by way of further example and without limitation, are described in this specification, and include legends, including numerical values (all of which are merely representative approximations and are not necessarily exact technical values and/or calculations). Further, these legends are not necessarily the only suitable values that represent the nature and characteristics of materials as applied to, affected by, and resulting from the operations of the exemplary system(s). Not all such legends will be repeated in this text, although all form a part of this disclosure and are believed understandable to persons of ordinary skill in water treatment and thermal processes. As appreciated by one skilled in the art, such data are sometimes referred to as heat and material balances. It is specifically to be understood and will be appreciated by one skilled in the art that the various values indicated in the legends may have a tolerance of ±20%, as they are representative approximations and not exact technical values.
[0086] Referring to FIG. 1 , which shows Stage # 1 , the waste water progresses from the input 20 to the output 30 successively through a pump 11 , preheaters 12 a and 12 , a condenser 13 , an additional heater 14 , and a flash evaporator 15 . In the preheater 12 a, the heating medium is the excess steam available from a crystallizer 90 (see FIG. 4 ), while for the preheater 12 , the heating medium is the hot water available from the condenser 13 .
[0087] The pump 11 elevates the waste water pressure from approximately 14.7 psia (1 atm) to approximately 150 psia. The level of pressurization of waste water in all stages is such that there is no boiling of the waste water inside and across the heat exchanger surfaces of all heat exchangers used in this system. This is done to prevent formation of deposits (scales, fouling etc.) on the heat exchanger surfaces. The temperature is also raised by the successive preheaters 12 a and 12 , the condenser 13 and the heater 14 , so the input waste water to the flash evaporator 15 at inlet 15 a is at 150 psia and 358° F.
[0088] The elevation in temperature is the effect of steam from one steam output 80 of the crystallizer subsystem 90 of FIG. 4 . That steam is mixed in a mixer 16 of FIG. 1 with part of the steam from the flash evaporator 15 at line 15 b that goes through a compressor 17 before it reaches the mixer 16 at input 16 a. Some of the steam from the evaporator 15 at line 15 b is also fed to the stripper 130 (see FIG. 4 ). The output 16 b of the mixer 16 is a superheated steam at approximately 500° F. and 150 psia which, following its use as a heating fluid in the heater 14 , continues to the condenser 13 and the preheater 12 until it exits the preheater 12 at outlet 12 b as distilled water. Additionally, as shown in FIG. 1 , the output of preheater 12 a at outlet 12 c is also distilled water. Under certain operating conditions, the steam addition from the crystallizer 90 may be negative, i.e., steam is sent as excess to the crystallizer 90 for other uses (e.g., as a heat source for the stripper 130 ).
[0089] The Stage # 1 output 30 has the volume of waste water reduced from the input 10 with the salts more concentrated to 25% TDS, which is increased from the initial approximately 20% TDS in the exemplary waste water at the input 20 .
[0090] Stage # 2 of the system as shown in FIG. 2 has elements substantially like those of Stage # 1 in FIG. 1 , but with some different operating parameters as shown in the legends in FIG. 2 . Referring to FIG. 2 , which shows Stage # 2 , the waste water progresses from the input 30 to the output 50 successively through a pump 31 , preheaters 32 a and 32 , a condenser 33 , an additional heater 34 , and a flash evaporator 35 . In the preheater 32 a, the heating medium is the excess steam available from a crystallizer 90 (see FIG. 4 ), while for the preheater 32 , the heating medium is the hot water available from the condenser 33 .
[0091] The pump 31 elevates the waste water pressure from approximately 5 psia at its input to approximately 150 psia. The temperature is also raised by the successive preheaters 32 a and 32 , the condenser 33 and the heater 34 , so the input waste water to the flash evaporator 35 at inlet 35 a is at 150 psia and 358° F.
[0092] The elevation in temperature is the effect of steam from one steam output 80 of the crystallizer subsystem 90 of FIG. 4 . That steam is mixed in a mixer 36 of FIG. 2 with part of the steam from the flash evaporator 35 at line 35 b that goes through a compressor 37 before it reaches the mixer 36 at input 36 a. Some of the steam from the evaporator 35 at line 35 b is also fed to the stripper 130 (see FIG. 4 ). The output 36 b of the mixer 36 is a superheated steam at approximately 500° F. and 150 psia which, following its use as a heating fluid in the heater 34 , continues to the condenser 33 and the preheater 32 until it exits the preheater 32 at outlet 32 b as distilled water. Additionally, as shown in FIG. 2 , the output of preheater 32 a at outlet 32 c is also distilled water. Under certain operating conditions, the steam addition from the crystallizer 90 may be negative, i.e., steam is sent as excess to the crystallizer 90 for other uses (e.g., as a heat source for the stripper 130 ).
[0093] The Stage # 2 output 50 has the volume of waste water reduced from the input 30 with the salts more concentrated to 31% TDS, which is increased from the initial approximately 25% TDS in the exemplary brine water at the input 30 .
[0094] Similarly, Stage # 3 of FIG. 3 has elements substantially like those of FIG. 2 , but with still some differences in operating parameters as shown in the legends in FIG. 3 . Referring to FIG. 3 , which shows Stage # 3 , the waste water progresses from the input 50 to the output 70 successively through a pump 51 , preheaters 52 a and 52 , a condenser 53 , an additional heater 54 , and a flash evaporator 55 . In the preheater 52 a, the heating medium is the excess steam available from a crystallizer 90 (see FIG. 4 ), while for the preheater 52 , the heating medium is the hot water available from the condenser 53 .
[0095] The pump 51 elevates the waste water pressure from approximately 5 psia at its input to approximately 150 psia. The temperature is also raised by the successive preheaters 52 a and 52 , the condenser 53 and the heater 54 , so the input waste water to the flash evaporator 55 at inlet 55 a is at 150 psia and 358° F.
[0096] The elevation in temperature is the effect of steam from one steam output 80 of the crystallizer subsystem 90 of FIG. 4 . That steam is mixed in a mixer 56 of FIG. 3 with part of the steam from the flash evaporator 55 at line 55 b that goes through a compressor 57 before it reaches the mixer 56 at input 56 a. Some of the steam from the evaporator 55 at line 55 b is also fed to the stripper 130 (see FIG. 4 ). The output 56 b of the mixer 56 is a superheated steam at approximately 500° F. and 150 psia which, following its use as a heating fluid in the heater 54 , continues to the condenser 53 and the preheater 52 until it exits the preheater 52 at outlet 52 b as distilled water. Additionally, as shown in FIG. 2 , the output of preheater 52 a at outlet 52 c is also distilled water. Under certain operating conditions, the steam addition from the crystallizer 90 may be negative, i.e., steam is sent as excess to the crystallizer 90 for other uses (e.g., as a heat source for the stripper 130 ).
[0097] The Stage # 3 output 70 has the volume of waste water reduced from the input 50 with the salts more concentrated to 39% TDS, which is increased from the initial approximately 31% TDS in the exemplary brine water at the input 50 .
[0098] The exemplary system includes multiple (three) concentration stages ( FIGS. 1-3 ) that are substantially alike in the combination of equipment used. However, other exemplary systems with multiple concentration stages may have individual stages of more viewed combinations of equipment without departing from the spirit and scope of the present invention.
[0099] The level of pressurization of waste water in all stages is such that there is no boiling (nucleate or other type) of the waste water inside and across the heat exchanger surfaces of the condensers, heaters and preheaters of each stage. This prevents the formation of deposits (scales, fouling etc.) on the heat exchanger surfaces and reduces the requirement for cleaning of the heat exchangers. This results in the reduction of the operating cost.
[0100] FIG. 4 represents an exemplary embodiment of applying the output brine water (line 70 ) of the Stage # 3 treatment ( FIG. 3 ) to a plasma crystallizer 90 . The plasma crystallizer 90 is an example of a known pyrolytic reactor that can be used to finish separation of water from salts dissolved therein. One skilled in the art will appreciate, however, that other thermal reactors may also be used without departing from the spirit and scope of the present invention. The example of a plasma reactor, which can be consistent with known plasma gasification/vitrification reactors, operated with one or more plasma torches 92 , as is well-known in published literature, is believed to provide opportunity for a favorable cost-benefit ratio.
[0101] In general, for multistage operation, the plasma crystallizer 90 (or other reactor) is utilized after the final concentration stage when the output brine water has been concentrated to a desired level, as described in the above example. It can also be suitable to have a multistage system not only for salts concentration (as in FIGS. 1-3 ), but also a separation subsystem with a reactor (e.g., plasma crystallizer 90 ) after any individual one of the early concentration stages (e.g., after either, or both, of Stages # 1 and # 2 ). However, it is generally more cost effective to have a single separation subsystem after the last of a determined number of concentration stages for the desired separation.
[0102] In general, any thermal reactor may be used to separate the salts and the water. A reactor operated to produce disposable salts (referred to herein as a “crystallizer”) is generally suitable. Where the salts have toxicity, it may be desirable to operate the reactor in a manner so they are vitrified or made into glass. Accordingly, any reference to a crystallizer herein can also include a vitrifier.
[0103] As shown in FIG. 4 , the crystallizer 90 has a salts output at an outlet 95 that is generally equivalent to the total salts content of the original waste water. The water output of the total system is recovered as clean distilled water from the preheaters 12 a, 12 , 32 a, 32 , 52 a, 52 of the respective stages of FIGS. 1-3 , and/or may be recovered directly from excess steam exiting the crystallizer system 90 at line 80 and/or the excess steam exiting the respective flash evaporators 15 , 35 , 55 at line 99 (the excess steam is condensed to form distilled water). The pressure of the steam in line 99 is first increased by a compressor 100 from approximately 5 psia to 15 psia at line 110 . This excess steam 110 is then utilized to heat air in the heater 120 and then condensed in condenser 125 to produce distilled water at line 125 a. The condenser 125 can be cooled by air or by plant cooling tower water.
[0104] FIG. 4 shows the brine water 70 entering the crystallizer 90 via a pump 91 that raises the pressure to 150 psia. FIG. 4 also shows how steam from the crystallizer 90 can be redirected back to the respective earlier Stages of FIGS. 1-3 . The steam output from the crystallizer 90 at line 80 may be provided back to the various Stages # 1 , # 2 and # 3 and used for heating by the respective heaters and condensers therein. Heated air at line 115 from the heater 120 is used in the stripper 130 which is utilized to remove, for example, volatile organic compounds (“VOCs”) from the waste water. Some excess steam may also be used for other purposes, e.g., to preheat the waste water in a preheater or a condenser.
[0105] Before treatment in the Stages shown in FIGS. 1-3 , the incoming waste water 10 can be, for example, sent to the stripper 130 where steam 115 is used to remove VOCs from the waste water 10 . FIG. 4 shows steam from the concentration Stages # 1 , # 2 and # 3 at an input 99 of the compressor 100 that is elevated to a temperature of 213° F. for use in the stripper 130 . The excess steam can be used directly in the stripper 130 , as shown in FIG. 4 , or used to heat air in a separate heat exchanger where the heated air is then used in the stripper to remove the VOCs. Additionally, the steam from the compressor 100 can be applied to another compressor 101 to increase its temperature and pressure to that of the steam in line 80 , and then combined with the steam in line 80 .
[0106] The stripped wastewater is sent as feed to the input 20 to Stage # 1 of FIG. 1 . The VOCs which are removed from the waste water 10 exit the stripper 130 through a conduit 135 which is sent to a condenser 140 , in which the VOCs are condensed to form liquid by using, for example, cooling water or air. The VOCs exit the condenser 140 at outlet 136 which connects to the plasma crystallizer 90 . The VOCs are fed in front of the plasma torch 92 (e.g., along with brine water 70 from the pump 91 ) such that they intensely mix with the high temperature gases exiting from the plasma torch 92 . The plasma torch 92 is operated using appropriate gas (e.g., air, oxygen, hydrogen, etc.) that will aid in, or result in, the complete destruction of the VOCs. The VOCs are substantially converted to carbon dioxide and steam. The heat generated by this conversion of VOCs to carbon dioxide and steam is utilized in the plasma crystallizer 90 , along with heat inputted through the plasma torch 92 , to vaporize the water from the brine water 70 . This reduces the amount of heat and the corresponding amount of electricity utilized in the plasma crystallizer 90 , thus increasing its cost effectiveness.
[0107] The steam exiting the plasma crystallizer 90 can be periodically vented to the atmosphere (not shown) to keep the levels of non-condensable gases low enough such that they do not degrade the performance of the heat exchangers used in the inventive system and process.
[0108] It is therefore seen that systems and processes in accordance with the present invention can make use of known and available components (such as, for example, flash evaporators for concentration of salts and plasma (or other) gasifier reactors for crystallization (or vitrification) of the salts) in particular innovative ways with insight as to both the capital cost and the operating cost. A need for such cost effective water treatment has been heightened by practices such as, for example, the use of large amounts of water in natural gas drilling. However, the present invention may be used in any situation where impurities to be removed exist.
[0109] In general summary, but without limitation, an embodiment of the present invention can be characterized in the following ways, for example: A system, and a corresponding method, in which waste water is supplied to one or more stages of equipment including a pump for pressurizing the water (e.g., to at least about 10 times atmospheric pressure), a heater that heats the pressurized waste water well above normal boiling temperature, a flash evaporator, or other device, that receives the heated, pressurized water and results in fluid evaporation and concentration of solids that were in the waste water. In for example, instances in which the waste (brine) water with concentrated solids cannot be otherwise readily and safely disposed of, a thermal or pyrolytic reactor is provided to crystallize or otherwise yield a form of the solids that can be readily and safely disposed of. In one form, such a reactor may also be applied as a heater for the original incoming waste water. Also, or alternatively, such a reactor may be used to form a vitrified glass of the salts output of any water treatment system that produces a brine water.
[0110] Furthermore, the examples of FIGS. 1-4 show how use can be made of flash evaporators operated at a low downstream pressure (e.g., 5 psia or only about one-third of 1 atm) along with compressors, as well as with a mixer for steam from a flash evaporator (after compression in a compressor) added with steam returned from a reactor. All of which is believed to contribute significantly to reduced operating costs which can be very beneficial, even though initial capital costs may be increased.
[0111] FIGS. 5-8 illustrate a further embodiment of the present invention. FIGS. 5 , 6 and 7 will be individually discussed, but first their general relation to each other in an exemplary multi-stage system will be described. FIG. 5 shows Stage # 1 . This first stage takes in waste water at an inlet 200 , processes it and produces first stage brine water at an outlet 220 of the first stage. The first stage brine water from the outlet 220 is input to the second stage shown in FIG. 6 (Stage # 2 ) for additional processing, and a resulting second stage brine water is produced as an output at outlet 240 . Similarly, the brine water from outlet 240 of the second stage is supplied as an input to the third stage shown in FIG. 7 (Stage # 3 ) that has additional processing, resulting in a third stage output of brine water at an outlet 260 .
[0112] It will be seen and appreciated by one skilled in the art how the successive stages of FIGS. 5 , 6 and 7 increase the concentration of salts in the brine water (e.g., Total Dissolved Solids—“TDS”). It will also be appreciated how the number of stages is a variable that can be chosen according to various factors including, but not limited to, the salts content of the original waste water and the desired salt content after concentration. In general, a system in accordance with these exemplary embodiments may include any one or more stages such as are shown, for example, in FIGS. 5-7 . The examples presented herein are merely illustrative of systems and methods that may be chosen not merely for good technical performance but also for reasons relating to economic factors, such as, for example, initial capital cost and operating cost, as well as convenience factors, such as, for example, space requirements and portability. While three stages are shown and described herein, one skilled in the art will appreciate that any number of stages may be utilized depending on the particular application without departing from the spirit and scope of the present invention.
[0113] Each of the FIGS. 5-8 , merely by way of further example and without limitation, are described in this specification, and include legends, including numerical values (all of which are merely representative approximations and are not necessarily exact technical values and/or calculations). Further, these legends are not necessarily the only suitable values that represent the nature and characteristics of materials as applied to, affected by, and resulting from the operations of the exemplary system(s). Not all such legends will be repeated in this text, although all form a part of this disclosure and are believed understandable to persons of ordinary skill in water treatment and thermal processes. As appreciated by one skilled in the art, such data are sometimes referred to as heat and material balances. It is specifically to be understood and will be appreciated by one skilled in the art that the various values indicated in the legends may have a tolerance of ±20%, as they are representative approximations and not exact technical values.
[0114] Referring to FIG. 5 , the waste water progresses from the input 200 to the output 240 successively through a pump 201 , a preheater 202 , a condenser 203 , and a flash evaporator 205 . One alternative is to have, in place of a single preheater 202 , a series of preheaters or heat exchangers. The heating medium for the preheater 202 can be excess steam available from a crystallizer 265 (see FIG. 8 ) and/or hot water from the condenser 203 .
[0115] In this example, the pump 201 , preheater 202 , and condenser 203 elevate the waste water pressure to 150 psia and the temperature to 360° F. at the inlet 206 to the flash evaporator 205 without use of any heater elements between the condenser 203 and flash evaporator 205 . The pump 201 elevates the pressure from 14.7 psia (1 atm) to 150 psia. The level of pressurization of waste water in all stages is such that there is no boiling of the waste water inside and across the heat exchanger surfaces of all heat exchangers used in this system. This is done to prevent the formation of deposits (scales, fouling etc.) on the heat exchanger surfaces. The preheater 202 elevates the temperature from 60° F. to 134° F., while the condenser 202 further elevates the temperature to 360° F. Additionally, the preheater 202 produces distilled water at outlet 207 .
[0116] For drawing convenience, each concentration Stage ( FIGS. 5-7 ) shows a heater (e.g., heater 204 in FIG. 5 , heater 224 in FIG. 6 , heater 244 in FIG. 7 ) which may be omitted entirely or, if present, not supplied with any heating fluid. As shown in FIGS. 5-7 , that heater 204 , 224 , 244 has zero input and zero output of heating fluid (e.g., DowTherm™). For system equipment economy, heater 204 , 224 , 244 is preferably omitted. However, systems may be arranged as shown and provide the option to operate or to not operate such a heater 204 , 224 , 244 . Further explanation of what enables avoiding use of a heater 204 , 224 , 244 is given below.
[0117] One aspect of Stage # 1 of FIG. 5 is, as shown in the legend to the right of the flash evaporator 205 , that it is operated so the flash pressure, i.e., the downstream or output pressure of the flash evaporator 205 , is approximately 25 psia, contrasting with the input or upstream pressure of 150 psia. The effect of this change in the pressure is that a portion of the water component of the waste water is separated from the dissolved solids in the form of steam. The remaining waste water becomes more concentrated in dissolved solids and exits the flash evaporator at outlet 220 .
[0118] The condenser 203 receives some saturated steam directly from the crystallizer 265 of FIG. 8 at line 266 which, with the preheater 202 elevating the waste water temperature from 60° F. to 134° F. before the condenser 203 , provides waste water at 360° F. from the condenser 203 and, favorably, there no need for the presence or operation of the heater 204 . Under certain operating conditions, the steam addition from the crystallizer 265 may be negative, i.e., steam is sent as excess to the crystallizer 265 for other uses (e.g., as a heat source for the stripper 270 ).
[0119] The Stage # 1 output 220 has the volume of waste water reduced from the input 200 with the salts more concentrated to approximately 23% TDS, which is increased from the initial approximately 20% TDS in the exemplary waste water at the input 200 .
[0120] Stages # 2 and # 3 in FIGS. 6 and 7 , respectively, have essentially the same equipment as shown in FIG. 5 for Stage # 1 but with some different operating parameters as shown in the legends of FIGS. 6-7 . Each of Stages # 2 and # 3 may also omit, or not operate, a heater between the condenser and flash evaporator of that stage.
[0121] Referring to FIG. 6 (Stage # 2 ), the brine water progresses from the input 200 to the output 240 successively through a pump 221 , a preheater 222 , a condenser 223 , and a flash evaporator 225 . One alternative is to have, in place of a single preheater 222 , a series of preheaters or heat exchangers. The heating medium for the preheater 222 can be excess steam available from a crystallizer 265 (see FIG. 8 ) and/or hot water from the condenser 223 .
[0122] In this example, the pump 221 , preheater 222 , and condenser 223 elevate the waste water pressure to 150 psia and the temperature to 360° F. at the inlet 226 to the flash evaporator 225 without use of any heater elements between the condenser 223 and flash evaporator 225 . The pump 221 elevates the pressure from 25 psia to 150 psia. The preheater 222 elevates the temperature from 239° F. to 253° F., while the condenser 222 further elevates the temperature to 360° F. Additionally, the preheater 222 produces distilled water at outlet 227 .
[0123] One aspect of Stage # 2 of FIG. 6 is, as shown in the legend to the right of the flash evaporator 225 , that it is operated so the flash pressure, i.e., the downstream or output pressure of the flash evaporator 225 , is approximately 25 psia, contrasting with the input or upstream pressure of 150 psia. The effect of this change in the pressure is that a portion of the water component of the waste water is separated from the dissolved solids in the form of steam. The remaining waste water becomes more concentrated in dissolved solids and exits the flash evaporator at outlet 240 .
[0124] The condenser 223 receives some saturated steam directly from the crystallizer 265 of FIG. 8 at line 266 which, with the preheater 222 elevating the waste water temperature from 239° F. to 253° F. before the condenser 223 , provides waste water at 360° F. from the condenser 223 and, favorably, there no need for the presence or operation of the heater 224 . Under certain operating conditions, the steam addition from the crystallizer 265 may be negative, i.e., steam is sent as excess to the crystallizer 265 for other uses (e.g., as a heat source for the stripper 270 ).
[0125] The Stage # 2 output 240 has the volume of waste water reduced from the input 220 with the salts more concentrated to approximately 26% TDS, which is increased from the initial approximately 23% TDS in the exemplary waste water at the input 220 .
[0126] Referring to FIG. 7 (Stage # 3 ), the brine water progresses from the input 240 to the output 260 successively through a pump 241 , a preheater 242 , a condenser 243 , and a flash evaporator 245 . One alternative is to have, in place of a single preheater 242 , a series of preheaters or heat exchangers. The heating medium for the preheater 242 can be excess steam available from a crystallizer 265 (see FIG. 8 ) and/or hot water from the condenser 243 .
[0127] In this example, the pump 241 , preheater 242 , and condenser 243 elevate the waste water pressure to 150 psia and the temperature to 360° F. at the inlet 246 to the flash evaporator 245 without use of any heater elements between the condenser 243 and flash evaporator 245 . The pump 241 elevates the pressure from 25 psia to 150 psia. The preheater 242 elevates the temperature from 239° F. to 254° F., while the condenser 242 further elevates the temperature to 360° F. Additionally, the preheater 242 produces distilled water at outlet 247 .
[0128] One aspect of Stage # 3 of FIG. 7 is, as shown in the legend to the right of the flash evaporator 245 , that it is operated so the flash pressure, i.e., the downstream or output pressure of the flash evaporator 245 , is approximately 25 psia, contrasting with the input or upstream pressure of 150 psia. The effect of this change in the pressure is that a portion of the water component of the waste water is separated from the dissolved solids in the form of steam. The remaining waste water becomes more concentrated in dissolved solids and exits the flash evaporator at outlet 260 .
[0129] The condenser 243 receives some saturated steam directly from the crystallizer 265 of FIG. 8 at line 266 which, with the preheater 242 elevating the waste water temperature from 239° F. to 254° F. before the condenser 243 , provides waste water at 360° F. from the condenser 243 and, favorably, there no need for the presence or operation of the heater 244 . Under certain operating conditions, the steam addition from the crystallizer 265 may be negative, i.e., steam is sent as excess to the crystallizer 265 for other uses (e.g., as a heat source for the stripper 270 ).
[0130] The Stage # 3 output 260 has the volume of waste water reduced from the input 240 with the salts more concentrated to approximately 30% TDS, which is increased from the initial approximately 26% TDS in the exemplary waste water at the input 220 .
[0131] The exemplary system includes multiple (three) concentration stages ( FIGS. 5-7 ) that are substantially alike in the combination of equipment used. However, other exemplary systems with multiple concentration stages may have individual stages of more varied combinations of equipment without departing from the spirit and scope of the present invention.
[0132] The level of pressurization of waste water in all stages is such that there is no boiling (nucleate or other type) of the waste water inside and across the heat exchanger surfaces of the condensers and preheaters of each stage. This prevents the formation of deposits (scales, fouling etc.) on the heat exchanger surfaces and reduces the requirement for cleaning of the heat exchangers. This results in the reduction of the operating cost.
[0133] FIG. 8 represents an example of applying the output brine water (line 260 ) of the Stage # 3 treatment ( FIG. 7 ) to a plasma crystallizer 265 . The plasma crystallizer 265 is an example of a known pyrolytic reactor that can be used to finish separation of water from salts dissolved in it. One skilled in the relevant art will appreciate, however, that other thermal reactors may also be used without departing from the spirit and scope of the present invention. The example of a plasma reactor, which can be consistent with known plasma gasification/vitrification reactors, operated with one or more plasma torches 267 , as is well-known in published literature, is believed to provide opportunity for a favorable cost-benefit ratio.
[0134] In general, for multistage operation, the plasma crystallizer 265 (or other reactor) is utilized at the final concentration stage when the output brine water has been concentrated to a desired level, as described in the above example. It can also be suitable to have a multistage system not only for salts concentration (as in FIGS. 5-7 ), but also a separation subsystem with a reactor after any individual one of the early concentration stages (e.g., after either, or both, of Stages # 1 and # 2 ). However, it is generally more cost effective to have a single separation subsystem after the last of a determined number of concentration stages for the desired separation.
[0135] In general, any thermal reactor may be used to separate the salts and the water. A reactor operated to produce disposable salts (referred to herein as a “crystallizer”) is generally suitable. Where the salts have toxicity, it may be desirable to operate the reactor in a manner so they are vitrified or made into glass. Accordingly, any reference to a crystallizer herein can also include a vitrifier.
[0136] As shown in FIG. 8 , the crystallizer 265 has a salts output at an outlet 268 equivalent to the total salts content of the original wastewater. The water output of the total system is now recovered as clean distilled water from the preheaters 202 , 222 , 242 of the respective Stages of FIGS. 5-7 , and/or may also be recovered directly from steam exiting the crystallizer 265 .
[0137] FIG. 8 shows brine water 260 entering the crystallizer 265 via a pump 280 that raises the pressure to 180 psia. FIG. 8 also shows how steam from the crystallizer 265 can be redirected back to the respective earlier Stages of FIGS. 5-7 . The steam output from the crystallizer 265 at line 266 may be provided back to the various Stages # 1 , # 2 and # 3 and used for heating by the respective preheaters and condensers therein. Also, FIG. 8 shows an “Excess Steam to Stripper” of a certain amount at line 269 . This steam 269 is used in a stripper 270 which is utilized to remove volatile organic compounds (“VOCs”) from the waste water before processing. Some excess steam from the crystallizer 265 may also be used for other purposes, e.g., to preheat the input waste water in a preheater or condenser.
[0138] Before treatment in the Stages shown in FIGS. 5-7 , the incoming waste water 10 can be, for example, sent to the stripper 270 where the steam 269 is used to remove VOCs from the waste water 10 . FIG. 8 shows steam from concentration Stages # 1 , # 2 and # 3 at an input 272 joined at a junction 273 with exiting steam from the crystallizer 265 that has been reduced in pressure by expansion in a mechanical vapor turbine 275 to recover energy and reduce the total amount of energy used in the process. The excess steam 269 can be used directly in the stripper 270 , as shown in FIG. 8 , or used to heat air in a separate heat exchanger where the heated air is then used in the stripper to remove the VOCs. The stripped waste water is sent as feed to the input 200 to Stage # 1 of FIG. 5 . The VOCs which are removed from the waste water 10 exit the stripper through a conduit 277 which connects to the plasma crystallizer 265 . Additionally or alternatively, a condenser with a knock-out pot (not shown) can be used between the plasma crystallizer 265 and the stripper 270 with the condensed VOCs (as well as any stripped VOCs) fed directly to the plasma crystallizer 265 . The VOCs are fed in front of the plasma torch 267 (e.g., along with brine water 260 from Stage # 3 from the pump 280 ) such that they intensely mix with the high temperature gases exiting from the plasma torch 267 . The plasma torch 267 is operated using appropriate gas (e.g., air, oxygen, hydrogen, etc.) that will aid in, or result in, the complete destruction of the VOCs. The VOCs are substantially converted to carbon dioxide and steam. The heat generated by this conversion of VOCs to carbon dioxide and steam is utilized in the plasma crystallizer 265 , along with heat inputted through the plasma torch 267 , to vaporize the water from the brine water 260 . This reduces the amount of heat and the corresponding amount of electricity utilized in the plasma crystallizer 265 , thus increasing its cost effectiveness.
[0139] The steam exiting the plasma crystallizer 265 can be periodically vented to the atmosphere (not shown) to keep the levels of non-condensable gases low enough such that they do not degrade the performance of the heat exchangers used in the inventive system and process.
[0140] It is therefore seen that systems and processes in accordance with the further embodiment of the present invention can make use of known and available components, such as, for example, flash evaporators for concentration of salts and plasma (or other) gasifier reactors for crystallization (or vitrification) of the salts, in particular innovative ways with insight as to both the capital cost and the operating cost. A need for such cost effective water treatment has been heightened by practices such as the use of large amounts of water in natural gas drilling However, the present invention may be used in any situation where impurities to be removed exist.
[0141] In general summary, but without limitation, the further embodiment of the present invention can be characterized in the following ways, for example: A system, and a corresponding method, in which waste water is supplied to one or more stages of equipment including a pump for pressurizing the water (e.g., to at least about 10 times atmospheric pressure), a heater that heats the pressurized water well above normal boiling temperature, a flash evaporator, or other device, that receives the heated, pressurized water and results in fluid evaporation and concentration of solids that were in the wastewater, and, for instances in which the brine water with concentrated solids cannot be otherwise readily and safely disposed of, a thermal or pyrolytic reactor to crystallize or otherwise yield a form of the solids that can be readily and safely disposed of, such a reactor may also be applied as a heater for the original incoming waste water. Also, or alternatively, such a reactor may be used to form a vitrified glass of the salts output of any water treatment system that produces a brine water.
[0142] Furthermore, the examples provided herein show how use can be made of flash evaporators operated at reduced downstream pressure (e.g., 25 psia compared to 150 psia upstream pressure) along with an expander (e.g., turbine), for energy recovery from the steam output of a crystallizer. All of which is believed to contribute significantly to reduced operating costs which can be very beneficial, even though initial capital costs may be increased.
[0143] FIGS. 9-12 illustrate yet a further embodiment of the present invention. FIGS. 9 , 10 and 11 will be individually discussed, but first their general relation to each other in an exemplary multi-stage system will be described. FIG. 9 shows Stage # 1 . This first stage takes in waste water at an inlet 300 , processes it and produces first stage brine water at an outlet 320 of the first stage. The first stage brine water from the outlet 320 is input to the second stage shown in FIG. 10 (Stage # 2 ) for additional processing, and a resulting second stage brine water is produced as an output at outlet 340 . Similarly, the brine water from outlet 340 of the second stage is supplied as an input to the third stage shown in FIG. 11 (Stage # 3 ) that has additional processing, resulting in a third stage output of brine water at an outlet 360 .
[0144] It will be seen and appreciated by one skilled in the art how the successive stages of FIGS. 9 , 10 and 11 increase the concentration of salts in the brine water (e.g., Total Dissolved Solids—“TDS”). It will also be appreciated how the number of stages is a variable that can be chosen according to various factors including, but not limited to, the salts content of the original waste water and the desired salt content after concentration. In general, a system in accordance with these exemplary embodiments may include any one or more stages such as are shown, for example, in FIGS. 9-11 . The examples presented herein are merely illustrative of systems and methods that may be chosen not merely for good technical performance but also for reasons relating to economic factors, such as, for example, initial capital cost and operating cost, as well as convenience factors, such as, for example, space requirements and portability. While three stages are shown and described herein, one skilled in the art will appreciate that any number of stages may be utilized depending on the particular application without departing from the spirit and scope of the present invention.
[0145] Each of the FIGS. 9-12 , merely by way of further example and without limitation, are described in this specification, and include legends, including numerical values (all of which are merely representative approximations and are not necessarily exact technical values and/or calculations). Further, these legends are not necessarily the only suitable values that represent the nature and characteristics of materials as applied to, affected by, and resulting from the operations of the exemplary system(s). Not all such legends will be repeated in this text, although all form a part of this disclosure and are believed understandable to persons of ordinary skill in water treatment and thermal processes. As appreciated by one skilled in the art, such data are sometimes referred to as heat and material balances. It is specifically to be understood and will be appreciated by one skilled in the art that the various values indicated in the legends may have a tolerance of ±20%, as they are representative approximations and not exact technical values.
[0146] Referring to FIG. 9 , the waste water progresses from the input 300 to the output 340 successively through a pump 301 , a preheater 302 , a condenser 303 , and a flash evaporator 305 . One alternative is to have, in place of a single preheater 302 , a series of preheaters or heat exchangers. The heating medium for the preheater 302 can be excess steam available from a crystallizer 365 (see FIG. 12 ) and/or hot water from the condenser 303 .
[0147] In this example, the pump 301 , preheater 302 , and condenser 303 elevate the waste water pressure to 150 psia and the temperature to 360° F. at the inlet 306 to the flash evaporator 305 without use of any heater elements between the condenser 303 and flash evaporator 305 . The pump 301 elevates the pressure from 14.7 psia (1 atm) to 150 psia. The level of pressurization of waste water in all stages is such that there is no boiling of the waste water inside and across the heat exchanger surfaces of all heat exchangers used in this system. This is done to prevent the formation of deposits (scales, fouling, etc.) on the heat exchanger surfaces. The preheater 302 elevates the temperature from 60° F. to 134° F., while the condenser 302 further elevates the temperature to 360° F. Additionally, the preheater 302 produces distilled water at outlet 307 .
[0148] For drawing convenience, each concentration Stage ( FIGS. 9-11 ) shows a heater (e.g., heater 304 in FIG. 9 , heater 324 in FIG. 10 , heater 344 in FIG. 11 ) between the condenser and flash evaporator, which may be omitted entirely or, if present, not supplied with any heating fluid. As shown in FIGS. 9-11 , that heater 304 , 324 , 344 has zero input and zero output of heating fluid (e.g., DowTherm™). For system equipment economy, heater 304 , 324 , 344 is preferably omitted. However, systems may be arranged as shown and provide the option to operate or to not operate such a heater 304 , 324 , 344 . Further explanation of what enables avoiding use of a heater 304 , 324 , 344 is given below.
[0149] One aspect of Stage # 1 of FIG. 9 is, as shown in the legend to the right of the flash evaporator 305 , that it is operated so the flash pressure, i.e., the downstream or output pressure of the flash evaporator 305 , is approximately 5 psia, contrasting with the input or upstream pressure of 150 psia and the flash pressure of 25 psia in FIGS. 5-8 . The effect of this change in the pressure is that a larger portion of the water component of the waste water is separated from the dissolved solids in the form of steam. The remaining waste water becomes more concentrated in dissolved solids and exits the flash evaporator at outlet 320 .
[0150] The condenser 303 receives some saturated steam directly from the crystallizer 365 of FIG. 12 at line 366 which, with the preheater 302 elevating the waste water temperature from 60° F. to 134° F. before the condenser 303 , provides waste water at 360° F. from the condenser 303 and, favorably, there no need for the presence or operation of the additional heater 304 . Under certain operating conditions, the steam addition from the crystallizer 365 may be negative, i.e., steam is sent as excess to the crystallizer 365 for other uses (e.g., as a heat source for the stripper 370 ).
[0151] The Stage # 1 output 320 has the volume of waste water reduced from the input 300 with the salts more concentrated to approximately 25% TDS, which is increased from the initial approximately 20% TDS in the exemplary waste water at the input 300 .
[0152] Stages # 2 and # 3 in FIGS. 10 and 11 , respectively, have essentially the same equipment as shown in FIG. 9 for Stage # 1 but with some different operating parameters as shown in the legends of FIGS. 10-11 . Each of Stages # 2 and # 3 may also omit, or not operate, a heater between the condenser and flash evaporator of that stage.
[0153] Referring to FIG. 10 (Stage # 2 ), the brine water progresses from the input 300 to the output 340 successively through a pump 321 , a preheater 322 , a condenser 323 , and a flash evaporator 325 . One alternative is to have, in place of a single preheater 322 , a series of preheaters or heat exchangers. The heating medium for the preheater 322 can be excess steam available from a crystallizer 365 (see FIG. 12 ) and/or hot water from the condenser 323 .
[0154] In this example, the pump 321 , preheater 322 , and condenser 323 elevate the waste water pressure to 150 psia and the temperature to 360° F. at the inlet 326 to the flash evaporator 325 without use of any heater elements between the condenser 323 and flash evaporator 325 . The pump 321 elevates the pressure from 5 psia to 150 psia. The preheater 322 elevates the temperature from 162° F. to 197° F., while the condenser 322 further elevates the temperature to 360° F. Additionally, the preheater 322 produces distilled water at outlet 327 .
[0155] One aspect of Stage # 2 of FIG. 10 is, as shown in the legend to the right of the flash evaporator 325 , that it is operated so the flash pressure, i.e., the downstream or output pressure of the flash evaporator 325 , is approximately 5 psia, contrasting with the input or upstream pressure of 150 psia and the flash pressure of 25 psia in FIGS. 5-8 . The effect of this change in the pressure is that a larger portion of the water component of the waste water is separated from the dissolved solids in the form of steam. The remaining waste water becomes more concentrated in dissolved solids and exits the flash evaporator at outlet 340 .
[0156] The condenser 323 receives some saturated steam directly from the crystallizer 365 of FIG. 12 at line 366 which, with the preheater 322 elevating the waste water temperature from 162° F. to 197° F. before the condenser 323 , provides waste water at 360° F. from the condenser 323 and, favorably, there no need for the presence or operation of the heater 324 . Under certain operating conditions, the steam addition from the crystallizer 365 may be negative, i.e., steam is sent as excess to the crystallizer 365 for other uses (e.g., as a heat source for the stripper 370 ).
[0157] The Stage # 2 output 340 has the volume of waste water reduced from the input 320 with the salts more concentrated to approximately 31% TDS, which is increased from the initial approximately 25% TDS in the exemplary waste water at the input 320 .
[0158] Referring to FIG. 11 (Stage # 3 ), the brine water progresses from the input 340 to the output 360 successively through a pump 341 , a preheater 342 , a condenser 343 , and a flash evaporator 345 . One alternative is to have, in place of a single preheater 342 , a series of preheaters or heat exchangers. The heating medium for the preheater 342 can be excess steam available from a crystallizer 365 (see FIG. 12 ) and/or hot water from the condenser 343 .
[0159] In this example, the pump 341 , preheater 342 , and condenser 343 elevate the waste water pressure to 150 psia and the temperature to 360° F. at the inlet 346 to the flash evaporator 345 without use of any heater elements between the condenser 343 and flash evaporator 345 . The pump 341 elevates the pressure from 5 psia to 150 psia. The preheater 342 elevates the temperature from 162° F. to 197° F., while the condenser 342 further elevates the temperature to 360° F. Additionally, the preheater 342 produces distilled water at outlet 347 .
[0160] One aspect of Stage # 3 of FIG. 11 is, as shown in the legend to the right of the flash evaporator 345 , that it is operated so the flash pressure, i.e., the downstream or output pressure of the flash evaporator 345 , is approximately 5 psia, contrasting with the input or upstream pressure of 150 psia and the flash pressure of 25 psia in FIGS. 5-8 . The effect of this change in the pressure is that a larger portion of the water component of the waste water is separated from the dissolved solids in the form of steam. The remaining waste water becomes more concentrated in dissolved solids and exits the flash evaporator at outlet 360 .
[0161] The condenser 343 receives some saturated steam directly from the crystallizer 365 of FIG. 12 at line 366 which, with the preheater 342 elevating the waste water temperature from 162° F. to 197° F. before the condenser 343 , provides waste water at 360° F. from the condenser 343 and, favorably, there no need for the presence or operation of the heater 344 . Under certain operating conditions, the steam addition from the crystallizer 365 may be negative, i.e., steam is sent as excess to the crystallizer 365 for other uses (e.g., as a heat source for the stripper 370 ).
[0162] The Stage # 3 output 360 has the volume of waste water reduced from the input 340 with the salts more concentrated to approximately 39% TDS, which is increased from the initial approximately 31% TDS in the exemplary waste water at the input 320 .
[0163] The exemplary system includes multiple (three) concentration stages ( FIGS. 9-11 ) that are substantially alike in the combination of equipment used. However, other exemplary systems with multiple concentration stages may have individual stages of more varied combinations of equipment without departing from the spirit and scope of the present invention.
[0164] The level of pressurization of waste water in all stages is such that there is no boiling (nucleate or other type) of the waste water inside and across the heat exchanger surfaces of the condensers and preheaters of each stage. This prevents the formation of deposits (scales, fouling, etc.) on the heat exchanger surfaces and reduces the requirement for cleaning of the heat exchangers. This results in the reduction of the operating cost.
[0165] FIG. 12 represents an example of applying the output brine water (line 360 ) of the Stage # 3 treatment ( FIG. 11 ) to a plasma crystallizer 365 . The plasma crystallizer 365 is an example of a known pyrolytic reactor that can be used to finish separation of water from salts dissolved in it. One skilled in the relevant art will appreciate, however, that other thermal reactors may also be used without departing from the spirit and scope of the present invention. The example of a plasma reactor, which can be consistent with known plasma gasification/vitrification reactors, operated with one or more plasma torches 367 , as is well-known in published literature, is believed to provide opportunity for a favorable cost-benefit ratio.
[0166] In general, for multistage operation, the plasma crystallizer 365 (or other reactor) is utilized at the final concentration stage when the output brine water has been concentrated to a desired level, as described in the above example. It can also be suitable to have a multistage system not only for salts concentration (as in FIGS. 9-11 ), but also a separation subsystem with a reactor after any individual one of the early concentration stages (e.g., after either, or both, of Stages # 1 and # 2 ). However, it is generally more cost effective to have a single separation subsystem after the last of a determined number of concentration stages for the desired separation.
[0167] In general, any thermal reactor may be used to separate the salts and the water. A reactor operated to produce disposable salts (referred to herein as a “crystallizer”) is generally suitable. Where the salts have toxicity, it may be desirable to operate the reactor in a manner so they are vitrified or made into glass. Accordingly, any reference to a crystallizer herein can also include a vitrifier.
[0168] As shown in FIG. 12 , the crystallizer 365 has a salts output at an outlet 368 equivalent to the total salts content of the original wastewater. The water output of the total system is now recovered as clean distilled water from the preheaters 302 , 322 , 342 of the respective Stages of FIGS. 9-11 , and/or may also be recovered directly from steam exiting the crystallizer 365 .
[0169] FIG. 12 shows brine water 360 entering the crystallizer 365 via a pump 380 that raises the pressure to 180 psia. FIG. 12 also shows how steam from the crystallizer 365 can be redirected back to the respective earlier Stages of FIGS. 9-11 . The steam output from the crystallizer 365 at line 366 may be provided back to the various Stages # 1 , # 2 and # 3 and used for heating by the respective preheaters and condensers therein. Also, FIG. 12 shows an “Excess Steam to Stripper” of a certain amount at line 369 . This steam 369 is used in a stripper 370 which is utilized to remove volatile organic compounds (“VOCs”) from the waste water before processing. Some excess steam from the crystallizer 365 may also be used for other purposes, e.g., to preheat the input waste water in a preheater or condenser.
[0170] Before treatment in the Stages shown in FIGS. 9-11 , the incoming waste water 10 can be, for example, sent to the stripper 370 where the steam 369 is used to remove VOCs from the waste water 10 . The excess steam 369 can be used directly in the stripper 370 , as shown in FIG. 12 , or used to heat air in a separate heat exchanger where the heated air is then used in the stripper to remove the VOCs. The stripped waste water is sent as feed to the input 300 to Stage # 1 of FIG. 9 . The VOCs which are removed from the waste water 10 exit the stripper through a conduit 377 which connects to the plasma crystallizer 365 . Additionally or alternatively, a condenser with a knock-out pot (not shown) can be used between the plasma crystallizer 365 and the stripper 370 with the condensed VOCs (as well as any stripped VOCs) fed directly to the plasma crystallizer 365 . The VOCs are fed in front of the plasma torch 367 (e.g., along with brine water 360 from Stage # 3 from the pump 380 ) such that they intensely mix with the high temperature gases exiting from the plasma torch 367 . The plasma torch is operated using appropriate gas (e.g., air, oxygen, hydrogen, etc.) that will aid in, or result in, the complete destruction of the VOCs. The VOCs are substantially converted to carbon dioxide and steam. The heat generated by this conversion of VOCs to carbon dioxide and steam is utilized in the plasma crystallizer 365 , along with heat inputted through the plasma torch 367 , to vaporize the water from the brine water 360 . This reduces the amount of heat and the corresponding amount of electricity utilized in the plasma crystallizer 365 , thus increasing its cost effectiveness.
[0171] The steam exiting the plasma crystallizer 365 can be periodically vented to the atmosphere (not shown) to keep the levels of non-condensable gases low enough such that they do not degrade the performance of the heat exchangers used in the inventive system and process.
[0172] FIG. 12 also shows some steam (e.g., about 36% of the input, in lbs/hr) from the flash evaporators 305 , 325 , 345 of concentration Stages # 1 , # 2 and # 3 at an input 372 goes to a compressor 375 that is elevated to 180 psia and a temperature of 373° F. for part of the steam that goes back to the treatment Stages of FIGS. 9-11 .
[0173] It is therefore seen that systems and processes in accordance with the yet further embodiment of the present invention can make use of known and available components, such as, for example, flash evaporators for concentration of salts and plasma (or other) gasifier reactors for crystallization (or vitrification) of the salts, in particular innovative ways with insight as to both the capital cost and the operating cost. A need for such cost effective water treatment has been heightened by practices such as the use of large amounts of water in natural gas drilling However, the present invention may be used in any situation where impurities to be removed exist.
[0174] In general summary, but without limitation, the yet further embodiment of the present invention can be characterized in the following ways, for example: A system, and a corresponding method, in which waste water is supplied to one or more stages of equipment including a pump for pressurizing the water (e.g., to at least about 10 times atmospheric pressure), a heater that heats the pressurized water well above normal boiling temperature, a flash evaporator, or other device, that receives the heated, pressurized water and results in fluid evaporation and concentration of solids that were in the wastewater, and, for instances in which the brine water with concentrated solids cannot be otherwise readily and safely disposed of, a thermal or pyrolytic reactor to crystallize or otherwise yield a form of the solids that can be readily and safely disposed of, such a reactor may also be applied as a heater for the original incoming waste water. Also, or alternatively, such a reactor may be used to form a vitrified glass of the salts output of any water treatment system that produces a brine water.
[0175] Furthermore, the examples provided herein show how use can be made of flash evaporators operated at low downstream pressure (e.g., 5 psia or only about one-third of 1 atm) along with a compressor elevating the pressure of some steam from the flash evaporators to, e.g., 180 psia, before being added with steam from the reactor that goes back to the earlier concentrations Stages. All of which is believed to contribute significantly to reduced operating costs which can be very beneficial, even though initial capital costs may be increased.
[0176] FIGS. 13-15 illustrate still a further embodiment of the present invention. FIGS. 13 , 14 and 15 will be individually discussed, but first their general relation to each other in an exemplary multi-stage system will be described. FIG. 13 shows Stage # 1 . This first stage takes in waste water at an inlet 400 , processes it and produces first stage brine water at an outlet 420 of the first stage. The first stage brine water from the outlet 420 is input to the second stage shown in FIG. 14 (Stage # 2 ) for additional processing, and a resulting second stage brine water is produced as an output at outlet 440 . Similarly, the brine water from outlet 440 of the second stage is supplied as an input to the third stage shown in FIG. 15 (Stage # 3 ) that has additional processing, resulting in a third stage output of brine water at an outlet 460 .
[0177] It will be seen and appreciated by one skilled in the art how the successive stages of FIGS. 13 , 14 and 15 increase the concentration of salts in the brine water (e.g., Total Dissolved Solids—“TDS”). It will also be appreciated how the number of stages is a variable that can be chosen according to various factors including, but not limited to, the salts content of the original waste water and the desired salt content after concentration. In general, a system in accordance with these exemplary embodiments may include any one or more stages such as are shown, for example, in FIGS. 13-15 . The examples presented herein are merely illustrative of systems and methods that may be chosen not merely for good technical performance but also for reasons relating to economic factors, such as, for example, initial capital cost and operating cost, as well as convenience factors, such as, for example, space requirements and portability. While three stages are shown and described herein, one skilled in the art will appreciate that any number of stages may be utilized depending on the particular application without departing from the spirit and scope of the present invention.
[0178] Each of the FIGS. 13-16 , merely by way of further example and without limitation, are described in this specification, and include legends, including numerical values (all of which are merely representative approximations and are not necessarily exact technical values and/or calculations). Further, these legends are not necessarily the only suitable values that represent the nature and characteristics of materials as applied to, affected by, and resulting from the operations of the exemplary system(s). Not all such legends will be repeated in this text, although all form a part of this disclosure and are believed understandable to persons of ordinary skill in water treatment and thermal processes. As appreciated by one skilled in the art, such data are sometimes referred to as heat and material balances. It is specifically to be understood and will be appreciated by one skilled in the art that the various values indicated in the legends may have a tolerance of ±20%, as they are representative approximations and not exact technical values.
[0179] Referring to FIG. 13 (Stage # 1 ), the waste water progresses from the input 400 to the output 440 successively through a pump 401 , a preheater 402 , a condenser 403 , and a flash evaporator 405 . One alternative is to have, in place of a single preheater 402 , a series of preheaters or heat exchangers. The heating medium for the preheater 402 can be excess steam available from a crystallizer 465 (see FIG. 16 ) and/or hot water from the condenser 403 .
[0180] In this example, the pump 401 , preheater 402 , and condenser 403 elevate the waste water pressure to 400 psia and the temperature to 445° F. at the inlet 406 to the flash evaporator 405 without use of any heater elements between the condenser 403 and flash evaporator 405 . The pump 401 elevates the pressure from 14.7 psia (1 atm) to 400 psia. The level of pressurization of waste water in all stages is such that there is no boiling of the waste water inside and across the heat exchanger surfaces of all heat exchangers used in this system. This is done to prevent the formation of deposits (scales, fouling, etc.) on the heat exchanger surfaces. The preheater 402 elevates the temperature from 60° F. to 254° F., while the condenser 402 further elevates the temperature to 445° F. Additionally, the preheater 402 produces distilled water at outlet 407 .
[0181] For drawing convenience, each concentration Stage ( FIGS. 13-15 ) shows a heater (e.g., heater 404 in FIG. 13 , heater 424 in FIG. 14 , heater 444 in FIG. 15 ) between the condenser and flash evaporator, which may be omitted entirely or, if present, not supplied with any heating fluid. As shown in FIGS. 13-15 , that heater 404 , 424 , 444 has zero input and zero output of heating fluid (e.g., DowTherm™). For system equipment economy, heater 404 , 424 , 444 is preferably omitted. However, systems may be arranged as shown and provide the option to operate or to not operate such a heater 404 , 424 , 444 . Further explanation of what enables avoiding use of a heater 404 , 424 , 444 is given below.
[0182] One aspect of Stage # 1 of FIG. 13 is, as shown in the legend to the right of the flash evaporator 405 , that it is operated so the flash pressure, i.e., the downstream or output pressure of the flash evaporator 405 , is approximately 15 psia, contrasting with the input or upstream pressure of 400 psia. The effect of this change in the pressure is that a larger portion of the water component of the waste water is separated from the dissolved solids in the form of steam. The remaining waste water becomes more concentrated in dissolved solids and exits the flash evaporator at outlet 420 .
[0183] The condenser 403 receives some saturated steam directly from the crystallizer 465 of FIG. 16 at line 466 which, with the preheater 402 elevating the waste water temperature from 60° F. to 254° F. before the condenser 403 , provides waste water at 445° F. from the condenser 403 and, favorably, there no need for the presence or operation of the additional heater 404 . In the exemplary system, the elevation in temperature is the effect of steam from the steam output 466 of the crystallizer subsystem 465 of FIG. 16 . That steam continues to the condenser 403 and the preheater 402 until it exits the preheater 402 at line 407 as distilled water. Under certain operating conditions, the steam addition from the crystallizer 465 may be negative, i.e., steam is sent as excess to the crystallizer 465 for other uses (e.g., as a heat source for the stripper 470 ).
[0184] The Stage # 1 output 420 has the volume of waste water reduced from the input 400 with the salts more concentrated to approximately 27% TDS, which is increased from the initial approximately 20% TDS in the exemplary waste water at the input 400 .
[0185] Stages # 2 and # 3 in FIGS. 14 and 15 , respectively, have essentially the same equipment as shown in FIG. 13 for Stage # 1 but with some different operating parameters as shown in the legends of FIGS. 14-15 . Each of Stages # 2 and # 3 may also omit, or not operate, a heater between the condenser and flash evaporator of that stage.
[0186] Referring to FIG. 14 (Stage # 2 ), the brine water progresses from the input 400 to the output 440 successively through a pump 421 , a preheater 422 , a condenser 423 , and a flash evaporator 425 . One alternative is to have, in place of a single preheater 422 , a series of preheaters or heat exchangers. The heating medium for the preheater 422 can be excess steam available from a crystallizer 465 (see FIG. 16 ) and/or hot water from the condenser 423 .
[0187] In this example, the pump 421 , preheater 422 , and condenser 423 elevate the waste water pressure to 400 psia and the temperature to 445° F. at the inlet 426 to the flash evaporator 425 without use of any heater elements between the condenser 423 and flash evaporator 425 . The pump 421 elevates the pressure from 15 psia to 400 psia. The preheater 422 elevates the temperature from 212° F. to 272° F., while the condenser 422 further elevates the temperature to 445° F. Additionally, the preheater 422 produces distilled water at outlet 427 .
[0188] One aspect of Stage # 2 of FIG. 14 is, as shown in the legend to the right of the flash evaporator 425 , that it is operated so the flash pressure, i.e., the downstream or output pressure of the flash evaporator 425 , is approximately 15 psia, contrasting with the input or upstream pressure of 400. The effect of this change in the pressure is that a larger portion of the water component of the waste water is separated from the dissolved solids in the form of steam. The remaining waste water becomes more concentrated in dissolved solids and exits the flash evaporator at outlet 440 .
[0189] The condenser 423 receives some saturated steam directly from the crystallizer 465 of FIG. 16 at line 466 which, with the preheater 422 elevating the waste water temperature from 212° F. to 272° F. before the condenser 423 , provides waste water at 445° F. from the condenser 423 and, favorably, there no need for the presence or operation of the heater 424 . In the exemplary system, the elevation in temperature is the effect of steam from the steam output 466 of the crystallizer subsystem 465 of FIG. 16 . That steam continues to the condenser 423 and the preheater 422 until it exits the preheater 422 at line 427 as distilled water. Under certain operating conditions, the steam addition from the crystallizer 465 may be negative, i.e., steam is sent as excess to the crystallizer 465 for other uses (e.g., as a heat source for the stripper 470 ).
[0190] The Stage # 2 output 440 has the volume of waste water reduced from the input 420 with the salts more concentrated to approximately 36% TDS, which is increased from the initial approximately 27% TDS in the exemplary waste water at the input 420 .
[0191] Referring to FIG. 15 (Stage # 3 ), the brine water progresses from the input 440 to the output 460 successively through a pump 441 , a preheater 442 , a condenser 443 , and a flash evaporator 445 . One alternative is to have, in place of a single preheater 442 , a series of preheaters or heat exchangers. The heating medium for the preheater 442 can be excess steam available from a crystallizer 465 (see FIG. 16 ) and/or hot water from the condenser 443 .
[0192] In this example, the pump 441 , preheater 442 , and condenser 443 elevate the waste water pressure to 400 psia and the temperature to 445° F. at the inlet 446 to the flash evaporator 445 without use of any heater elements between the condenser 443 and flash evaporator 445 . The pump 441 elevates the pressure from 15 psia to 400 psia. The preheater 442 elevates the temperature from 212° F. to 273° F., while the condenser 442 further elevates the temperature to 445° F. Additionally, the preheater 442 produces distilled water at outlet 447 .
[0193] One aspect of Stage # 3 of FIG. 15 is, as shown in the legend to the right of the flash evaporator 445 , that it is operated so the flash pressure, i.e., the downstream or output pressure of the flash evaporator 445 , is approximately 15 psia, contrasting with the input or upstream pressure of 400. The effect of this change in the pressure is that a larger portion of the water component of the waste water is separated from the dissolved solids in the form of steam. The remaining waste water becomes more concentrated in dissolved solids and exits the flash evaporator at outlet 460 .
[0194] The condenser 443 receives some saturated steam directly from the crystallizer 465 of FIG. 16 at line 466 which, with the preheater 442 elevating the waste water temperature from 212° F. to 273° F. before the condenser 443 , provides waste water at 445° F. from the condenser 443 and, favorably, there no need for the presence or operation of the heater 444 . In the exemplary system, the elevation in temperature is the effect of steam from the steam output 466 of the crystallizer subsystem 465 of FIG. 16 . That steam continues to the condenser 443 and the preheater 442 until it exits the preheater 442 at line 447 as distilled water. Under certain operating conditions, the steam addition from the crystallizer 465 may be negative, i.e., steam is sent as excess to the crystallizer 465 for other uses (e.g., as a heat source for the stripper 470 ).
[0195] The Stage # 3 output 340 has the volume of waste water reduced from the input 440 with the salts more concentrated to approximately 48% TDS, which is increased from the initial approximately 36% TDS in the exemplary waste water at the input 420 .
[0196] The exemplary system includes multiple (three) concentration stages ( FIGS. 13-15 ) that are substantially alike in the combination of equipment used. However, other exemplary systems with multiple concentration stages may have individual stages of more varied combinations of equipment without departing from the spirit and scope of the present invention.
[0197] The level of pressurization of waste water in all stages is such that there is no boiling (nucleate or other type) of the waste water inside and across the heat exchanger surfaces of the condensers and preheaters of each stage. This prevents the formation of deposits (scales, fouling, etc.) on the heat exchanger surfaces and reduces the requirement for cleaning of the heat exchangers. This results in the reduction of the operating cost.
[0198] FIG. 16 represents an example of applying the output brine water (line 460 ) of the Stage # 3 treatment ( FIG. 15 ) to a plasma crystallizer 465 . The plasma crystallizer 465 is an example of a known pyrolytic reactor that can be used to finish separation of water from salts dissolved in it. One skilled in the relevant art will appreciate, however, that other thermal reactors may also be used without departing from the spirit and scope of the present invention. The example of a plasma reactor, which can be consistent with known plasma gasification/vitrification reactors, operated with one or more plasma torches 467 , as is well-known in published literature, is believed to provide opportunity for a favorable cost-benefit ratio.
[0199] In general, for multistage operation, the plasma crystallizer 465 (or other reactor) is utilized at the final concentration stage when the output brine water has been concentrated to a desired level, as described in the above example. It can also be suitable to have a multistage system not only for salts concentration (as in FIGS. 13-15 ), but also a separation subsystem with a reactor after any individual one of the early concentration stages (e.g., after either, or both, of Stages # 1 and # 2 ). However, it is generally more cost effective to have a single separation subsystem after the last of a determined number of concentration stages for the desired separation.
[0200] In general, any thermal reactor may be used to separate the salts and the water. A reactor operated to produce disposable salts (referred to herein as a “crystallizer”) is generally suitable. Where the salts have toxicity, it may be desirable to operate the reactor in a manner so they are vitrified or made into glass. Accordingly, any reference to a crystallizer herein can also include a vitrifier.
[0201] As shown in FIG. 16 , the crystallizer 465 has a salts output at an outlet 468 equivalent to the total salts content of the original wastewater. The water output of the total system is now recovered as clean distilled water from the preheaters 402 , 422 , 442 of the respective Stages of FIGS. 13-15 , and/or may also be recovered directly from steam exiting the crystallizer 465 .
[0202] FIG. 16 shows brine water 460 entering the crystallizer 465 via a pump 480 that raises the pressure to 665 psia. FIG. 16 also shows how steam from the crystallizer 465 can be redirected back to the respective earlier Stages of FIGS. 13-15 . The steam output from the crystallizer 465 at line 466 may be provided back to the various Stages # 1 , # 2 and # 3 and used for heating by the respective preheaters and condensers therein. Also, FIG. 16 shows an “Excess Steam to Stripper” of a certain amount at line 469 . This steam 469 is used in a stripper 470 which is utilized to remove volatile organic compounds (“VOCs”) from the waste water before processing. Some excess steam from the crystallizer 465 may also be used for other purposes, e.g., to preheat the input waste water in a preheater or condenser.
[0203] Before treatment in the Stages shown in FIGS. 13-15 , the incoming waste water 10 can be, for example, sent to the stripper 470 where the steam 469 is used to remove VOCs from the waste water 10 . The excess steam 469 can be used directly in the stripper 470 , as shown in FIG. 16 , or used to heat air in a separate heat exchanger where the heated air is then used in the stripper to remove the VOCs. The stripped waste water is sent as feed to the input 400 to Stage # 1 of FIG. 13 . The VOCs which are removed from the waste water 10 exit the stripper through a conduit 477 which connects to the plasma crystallizer 465 . Additionally or alternatively, a condenser with a knock-out pot (not shown) can be used between the plasma crystallizer 465 and the stripper 470 with the condensed VOCs (as well as any stripped VOCs) fed directly to the plasma crystallizer 465 . The VOCs are fed in front of the plasma torch 467 (e.g., along with brine water 460 from Stage # 3 from the pump 480 ) such that they intensely mix with the high temperature gases exiting from the plasma torch 467 . The plasma torch 467 is operated using appropriate gas (e.g., air, oxygen, hydrogen, etc.) that will aid in, or result in, the complete destruction of the VOCs. The VOCs are substantially converted to carbon dioxide and steam. The heat generated by this conversion of VOCs to carbon dioxide and steam is utilized in the plasma crystallizer 465 , along with heat inputted through the plasma torch 467 , to vaporize the water from the brine water 460 . This reduces the amount of heat and the corresponding amount of electricity utilized in the plasma crystallizer 465 , thus increasing its cost effectiveness.
[0204] The steam exiting the plasma crystallizer 465 can be periodically vented to the atmosphere (not shown) to keep the levels of non-condensable gases low enough such that they do not degrade the performance of the heat exchangers used in the inventive system and process.
[0205] FIG. 16 also shows some steam from the flash evaporators 405 , 425 , 445 of concentration Stages # 1 , # 2 and # 3 at an input 472 goes to a compressor 475 that elevates the steam to a pressure of 665 psia and a temperature of 500° F. to be recycled as part of the steam that goes back to the treatment Stages of FIGS. 13-15 .
[0206] It is therefore seen that systems and processes in accordance with the still further embodiment of the present invention can make use of known and available components, such as, for example, flash evaporators for concentration of salts and plasma (or other) gasifier reactors for crystallization (or vitrification) of the salts, in particular innovative ways with insight as to both the capital cost and the operating cost. A need for such cost effective water treatment has been heightened by practices such as the use of large amounts of water in natural gas drilling However, the present invention may be used in any situation where impurities to be removed exist.
[0207] In general summary, but without limitation, the still further embodiment of the present invention can be characterized in the following ways, for example: A system, and a corresponding method, in which waste water is supplied to one or more stages of equipment including a pump for pressurizing the water (e.g., to about 400 psia), a preheater that heats the pressurized waste water well above normal boiling temperature, a condenser that effects further heating of the pressurized waste water, a flash evaporator, or other device, that receives the heated, pressurized waste water and results in fluid evaporation and concentration of solids that were in the waste water. In for example, instances in which the waste (brine) water with concentrated solids cannot be otherwise readily and safely disposed of, a thermal or pyrolytic reactor is provided to crystallize or otherwise yield a form of the solids that can be readily and safely disposed of. In one form, such a reactor may also be applied as a heater for the original incoming waste water. Also, or alternatively, such a reactor may be used to form a vitrified glass of the salts output of any water treatment system that .produces a brine water.
[0208] Furthermore, the examples described herein show how use can be made of flash evaporators operated at a considerable difference of upstream pressure (e.g., 400 psia) and downstream pressure (e.g., 15 psia). To do so, the pyrolytic reactor of the inventive system is operated at a significantly higher pressure than is usual for such equipment (e.g., a plasma crystallizer operated at a pressure of 665 psia and steam developed in the reactor is supplied directly to the condensers of the earlier salts concentration Stages). All of which is believed to contribute significantly to reduced operating costs which can be very beneficial, even though initial capital costs may be increased.
[0209] FIGS. 17-20 illustrate another embodiment of the present invention. FIGS. 17 , 18 and 19 will be individually discussed, but first their general relation to each other in an exemplary multi-stage system (here with three stages) will be described.
[0210] Each of the FIGS. 17-20 , merely by way of further example and without limitation, are described in this specification, and include legends, including numerical values (all of which are merely representative approximations and are not necessarily exact technical values and/or calculations). Further, these legends are not necessarily the only suitable values that represent the nature and characteristics of materials as applied to, affected by, and resulting from the operations of the exemplary system(s). Not all such legends will be repeated in this text, although all form a part of this disclosure and are believed understandable to persons of ordinary skill in water treatment and thermal processes. As appreciated by one skilled in the art, such data are sometimes referred to as heat and material balances. It is specifically to be understood and will be appreciated by one skilled in the art that the various values indicated in the legends may have a tolerance of ±20%, as they are representative approximations and not exact technical values.
[0211] A separate batch of wastewater 500 is supplied to each of the inlets 510 a, 510 b, and 510 c of FIGS. 17-19 , respectively. Each Stage heats and pressurizes the waste water that is then supplied to a single flash evaporator 515 a, 515 b and 515 c, respectively. The flash evaporators 515 a, 515 b and 515 c have brine water outputs, at an outlet 530 a, 530 b and 530 c, respectively, that is combined into a single output 530 from wastewater to each of the inputs 510 a, 510 b and 510 c.
[0212] Referring to FIGS. 17 , 18 and 19 , which represent Stages # 1 A, # 1 B and # 1 C, respectively, each batch of waste water progresses from the input 510 a, 510 b, 510 c to the output 530 a, 530 b , 530 c successively through a pump 511 a, 511 b, 511 c, a preheater 512 a, 512 b, 512 c, a condenser 513 a, 513 b, 513 c, and a flash evaporator 515 a, 515 b, 515 c. One alternative is to have, in place of a single preheater 512 a, 512 b, 512 c , a series of preheaters or heat exchangers. The heating medium for the preheater 512 a, 512 b, 512 c can be excess steam available from a crystallizer 565 (see FIG. 20 ) and/or hot water from the condenser 513 a, 513 b, 513 c.
[0213] For convenience, when referring to the same element in the various Stages, the reference letters a-c will be omitted and only the reference number will be used. It is to be understood that the element referred to is the same element in all three Stages.
[0214] Referring to FIGS. 17-19 , the pump 511 , preheater 512 , and condenser 513 elevate the waste water pressure to 400 psia and the temperature to 445° F. at the inlet 506 to the flash evaporator 515 without use of any heater elements between the condenser 513 and flash evaporator 515 . The pump 511 elevates the pressure from 14.7 psia (1 atm) to 400 psia. The level of pressurization of waste water in all stages is such that there is no boiling of the waste water inside and across the heat exchanger surfaces of all heat exchangers used in this system. This is done to prevent the formation of deposits (scales, fouling, etc.) on the heat exchanger surfaces. The preheater 512 elevates the temperature from 60° F. to 199° F., while the condenser 513 further elevates the temperature to 445° F. Additionally, the preheater 512 produces distilled water at outlet 507 .
[0215] For drawing convenience, each concentration Stage ( FIGS. 17-19 ) shows a heater 514 (e.g., heater 514 a in FIG. 17 , heater 514 b in FIG. 18 , heater 514 c in FIG. 19 ) between the condenser and flash evaporator, which may be omitted entirely or, if present, not supplied with any heating fluid. As shown in FIGS. 17-19 , the heater 514 has zero input and zero output of heating fluid (e.g., DowTherm™). For system equipment economy, the heater 514 is preferably omitted. However, systems may be arranged as shown and provide the option to operate or to not operate such a heater 514 . Further explanation of what enables avoiding use of a heater 514 is given below.
[0216] One aspect of Stages # 1 A, # 1 B and # 1 C of FIGS. 17 , 18 and 19 is, as shown in the legend to the right of the flash evaporator 515 , that it is operated so the flash pressure, i.e., the downstream or output pressure of the flash evaporator 515 , is approximately 15 psia, contrasting with the input or upstream pressure of 400 psia. The effect of this change in the pressure is that a larger portion of the water component of the waste water is separated from the dissolved solids in the form of steam. The remaining waste water becomes more concentrated in dissolved solids and exits the flash evaporator at outlet 530 .
[0217] The condenser 513 receives some saturated steam directly from the crystallizer 565 of FIG. 20 at line 566 which, with the preheater 512 elevating the waste water temperature from 60° F. to 199° F. before the condenser 513 , provides waste water at 445° F. from the condenser 513 and, favorably, there no need for the presence or operation of the additional heater 514 . In the exemplary system, the elevation in temperature is the effect of steam from the steam output 566 of the crystallizer subsystem 565 of FIG. 20 . That steam continues to the condenser 513 and the preheater 512 until it exits the preheater 512 at line 507 as distilled water. Under certain operating conditions, the steam addition from the crystallizer 565 may be negative, i.e., steam is sent as excess to the crystallizer 565 for other uses (e.g., as a heat source for the stripper 570 ).
[0218] The output 530 of the various parallel Stages has the volume of waste water reduced from the input 510 with the salts more concentrated to a brine water to approximately 27% TDS, which is increased from the initial approximately 20% TDS in the exemplary waste water at the input 510 .
[0219] In each of FIGS. 17-19 , it is shown the individual stages outputs 530 a, 530 b, 530 c of the system's single flash evaporator 515 a, 515 b, 515 c, respectively, are equal. The combined inputs 510 a, 510 b, 510 c to the treatment stages make up 6000 lbs/hr, including salts of 1200 lbs/hr. The brine water outputs 530 a, 530 b, 530 c of the single flash evaporators 515 a, 515 b, 515 c , respectively, include each stage's output which are combined (as shown in FIG. 20 as conduit 530 ), equals a total of 4491 lbs/hr, which includes the 1200 lbs/hr of salts in the three inputs 510 a, 510 b, 510 c. The salts are now 27% of each Stage and of the total outputs in Total Dissolved Solids (“TDS”), compared to just 20% at the inputs.
[0220] The exemplary system includes multiple (three) concentration stages ( FIGS. 17-19 ) that are substantially alike in the combination of equipment used. However, other exemplary systems with multiple concentration stages may have individual stages of more varied combinations of equipment without departing from the spirit and scope of the present invention.
[0221] The level of pressurization of waste water in all stages is such that there is no boiling (nucleate or other type) of the waste water inside and across the heat exchanger surfaces of the condensers and preheaters of each stage. This prevents the formation of deposits (scales, fouling, etc.) on the heat exchanger surfaces and reduces the requirement for cleaning of the heat exchangers. This results in the reduction of the operating cost.
[0222] FIG. 20 represents an example of applying the output brine water (line 530 with the combined individual outputs 530 a, 530 b, 530 c ) of the single flash evaporators 515 a, 515 b, 515 c , respectively, of the concentration Stages # 1 A, # 1 B, # 1 C to a plasma crystallizer 565 . The plasma crystallizer 565 is an example of a known pyrolytic reactor that can be used to finish separation of water from salts dissolved in it. One skilled in the relevant art will appreciate, however, that other thermal reactors may also be used without departing from the spirit and scope of the present invention. The example of a plasma reactor, which can be consistent with known plasma gasification/vitrification reactors, operated with one or more plasma torches 567 , as is well-known in published literature, is believed to provide opportunity for a favorable cost-benefit ratio.
[0223] The exemplary arrangement shown in FIGS. 17-20 uses a single plasma crystallizer 565 , as well as a multiple flash evaporators 515 a, 515 b, 515 c, for any number of parallel waste water flows (which are of equal volume and content in the illustrated example, but can vary from each other). Alternatively the multiple flash evaporators 515 a, 515 b, 515 c may be replaced by a single flash evaporator. The size and cost of equipment can, at least in some instances, be favorable for use of a combination of multiple pressurizing and heating elements and a single concentration element.
[0224] In general, any thermal reactor may be used to separate the salts and the water. A reactor operated to produce disposable salts (referred to herein as a “crystallizer”) is generally suitable. Where the salts have toxicity, it may be desirable to operate the reactor in a manner so they are vitrified or made into glass. Accordingly, any reference to a crystallizer herein can also include a vitrifier.
[0225] As shown in FIG. 20 , the crystallizer 565 has a salts output at an outlet 568 equivalent to the total salts content of the original wastewater. The water output of the total system is now recovered as clean distilled water from the preheaters 512 a, 512 b, 512 c of the respective parallel Stages of FIGS. 17-19 , and/or may also be recovered directly from steam exiting the crystallizer 565 .
[0226] FIG. 20 shows brine water 530 entering the crystallizer 565 via a pump 580 that raises the pressure to 665 psia. FIG. 20 also shows how steam from the crystallizer 565 can be redirected back to the respective earlier Stages of FIGS. 17-19 . The steam output from the crystallizer 565 at line 566 may be provided back to the various Stages # 1 A, # 1 B, # 1 C and used for heating by the respective preheaters and condensers therein. Also, FIG. 20 shows an “Excess Steam to Stripper” of a certain amount at line 569 . This steam 569 is used in a stripper 570 which is utilized to remove volatile organic compounds (“VOCs”) from the waste water before processing. Some excess steam from the crystallizer 565 may also be used for other purposes, e.g., to preheat the input waste water in a preheater or condenser.
[0227] Before treatment in the Stages shown in FIGS. 17-19 , the incoming waste water 10 can be, for example, sent to the stripper 570 where the steam 569 is used to remove VOCs from the waste water 10 . FIG. 20 shows steam 569 developed from concentration Stages # 1 A, # 1 B, # 1 C at an input 572 joined at a junction 573 with exiting steam from the crystallizer 565 that has been reduced in pressure by expansion in a mechanical vapor turbine 575 to recover energy and reduce the total amount of energy used in the process. The excess steam 569 can be used directly in the stripper 570 , as shown in FIG. 20 , or used to heat air in a separate heat exchanger where the heated air is then used in the stripper to remove the VOCs. The stripped waste water 500 is sent as feed to the inputs 510 a, 510 b, 510 c of Stages # 1 A, # 1 B, # 1 C, respectively, as shown in FIGS. 17-19 . The VOCs which are removed from the waste water 10 exit the stripper through a conduit 577 which connects to the plasma crystallizer 565 . Additionally or alternatively, a condenser with a knock-out pot (not shown) can be used between the plasma crystallizer 565 and the stripper 570 with the condensed VOCs (as well as any stripped VOCs) fed directly to the plasma crystallizer 565 . The VOCs are fed in front of the plasma torch 567 (e.g., along with brine water 530 from the pump 580 ) such that they intensely mix with the high temperature gases exiting from the plasma torch 567 . The plasma torch 567 is operated using appropriate gas (e.g., air, oxygen, hydrogen, etc.) that will aid in, or result in, the complete destruction of the VOCs. The VOCs are substantially converted to carbon dioxide and steam. The heat generated by this conversion of VOCs to carbon dioxide and steam is utilized in the plasma crystallizer 565 , along with heat inputted through the plasma torch 567 , to vaporize the water from the brine water 560 . This reduces the amount of heat and the corresponding amount of electricity utilized in the plasma crystallizer 465 , thus increasing its cost effectiveness.
[0228] The steam exiting the plasma crystallizer 565 can be periodically vented to the atmosphere (not shown) to keep the levels of non-condensable gases low enough such that they do not degrade the performance of the heat exchangers used in the inventive system and process.
[0229] It is therefore seen that systems and processes in accordance with the another embodiment of the present invention can make use of known and available components, such as, for example, flash evaporators for concentration of salts and plasma (or other) gasifier reactors for crystallization (or vitrification) of the salts, in particular innovative ways with insight as to both the capital cost and the operating cost. A need for such cost effective water treatment has been heightened by practices such as the use of large amounts of water in natural gas drilling However, the present invention may be used in any situation where impurities to be removed exist.
[0230] In general summary, but without limitation, the another embodiment of the present invention can be characterized in the following ways, for example: A system, and a corresponding method, in which waste water is supplied to one or more stages of equipment including a pump for pressurizing the water (e.g., about 400 psia), a preheater that heats the pressurized waste water well above normal boiling temperature, a condenser that effects further heating of the pressurized waste water, a single, or plural, flash evaporator(s), or other concentration device(s), that receives the heated, pressurized water flows from multiple parallel stages of pressurizing and heating elements and results in fluid evaporation and concentration of solids that were in the waste water. In, for example, instances in which the waste (brine) water with concentrated solids cannot be otherwise readily and safely disposed of, a thermal or pyrolytic reactor is provided to crystallize or otherwise yield a form of the solids that can be readily and safely disposed of. In one form, such a reactor may also be applied as a heater for the original incoming wastewater. Also, or alternatively, such a reactor may be used to form a vitrified glass of the salts output of any water treatment system that produces a brine water.
[0231] The examples described herein show how use can be made of a single flash evaporator receiving multiple heated and pressurized flows of waste water with the concentrated output of the flash evaporator subjected to final separation of salts and water in a single reactor.
[0232] It will be apparent to those skilled in the art that numerous modifications and variations of the described examples and embodiments are possible in light of the above teachings of the disclosure. The disclosed examples and embodiments are presented for purposes of illustration only. Other alternate embodiments may include some or all of the features disclosed herein. Therefore, it is the intent to cover all such modifications and alternate embodiments as may come within the true scope of this invention, which is to be given the full breadth thereof. Additionally, the disclosure of a range of values is a disclosure of every numerical value within that range. | System and method of treating waste water includes: receiving waste water at a first pressure and a first temperature, the waste water comprising dissolved solids and VOCs; pressurizing the waste water to a second pressure; preheating the pressurized waste water to a second temperature to produce distilled water and pressurized/preheated water; heating the pressurized/preheated to a third temperature to produce pressurized/heated water; removing dissolved solids from the pressurized/heated water, by an evaporator operated at a third pressure less than the second pressure, to produce steam and brine water; and crystallizing the brine water, by a crystallizer operated at a fourth pressure greater than the second pressure, to produce a solid mass waste product and steam. Steam produced by the crystallizer, at the fourth pressure and a fourth temperature, is a heat source for the preheater and/or heater, and steam produced by the evaporator is a heat source for the crystallizer. | 1 |
CROSS-REFERENCES TO RELATED APPLICATIONS
This application is related to U.S. Pat. No. 4,714,339, entitled “Three and Five Axis Laser Tracking Systems” and issued Dec. 22, 1987; U.S. Pat. No. 6,049,377, entitled “Five-Axis/Six-Axis Laser Measuring System” and issued Apr. 11, 2000; U.S. Pat. App. Pub. No. U.S. 2003/0043362 A1, entitled “Six Dimensional Laser Tracking System and Method” and published Mar. 6, 2003; U.S. Pat. App. Pub. No. U.S. 2003/020685 A1, entitled “Nine Dimensional Laser Tracking System and Method” and published Nov. 6, 2003. The present application claims the benefit of Provisional Application No. 60/601,831, entitled “System and Method for Three-Dimensional Measurement” and filed Aug. 16, 2004. The present application hereby incorporates by reference all above-referenced patents and patent applications in their entirety.
BACKGROUND
Rapid, precise measurement of the position and orientation of a tool or workpiece is critical to many automated manufacturing processes. Although a variety of different measurement systems have been developed, optical measuring systems have proven precise, adaptable, reliable, and relatively inexpensive.
Most optical measuring systems exploit various effects obtained by manipulating the output of low-intensity lasers. For example, highly accurate linear distance measurements can be obtained by counting interference fringes that shift position as a laser beam reflects from a shifting target. Such a system may be initially calibrated by measuring the time of flight of a laser pulse that strikes a target and returns to a source.
Orientation measurements have posed more of a challenge, since, for example, a light beam parallel to a rotational axis of a target may register no distance variation. One solution to this problem utilizes the polarizing effects of a Glan-Thompson prism, which resolves an incoming laser beam into two orthogonal vector components that vary in intensity according to the rotational orientation of the prism with respect to the beam. Once such a system is calibrated, a target's angle of rotation about an axis may be calculated from the measured intensity differential between output vector components.
However, obtaining complete positional data for a target using the simplest forms of such measurement techniques may require a separate distance-measuring system for each translational axis and a separate rotation-measuring system for each rotational axis. As the setup and operation of simple multi-dimensional measurement systems may become cumbersome and expensive, it is highly desirable to make as many different but simultaneous measurements as possible with a single light beam.
SUMMARY
The present invention increases the number of translational and angular measurements made with a single laser beam by combining an optical interferometer with an optical autocollimator. This system and method provides both a precise linear distance measurement on one translational axis and simultaneous yaw and pitch measurements. Utilizing a single laser beam, a translational measurement is made with an optical interferometer and angular measurements are made with an autocollimator. In a preferred embodiment, angular deviations in the reflected measuring beam are minimized with a reverse telescopic lens assembly, allowing a wider range of angular measurements without significant degradation of interferometer accuracy. All of these features and advantages of the present invention, and more, are illustrated below in the drawings and detailed description that follow.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 shows the present invention's axes of measurement.
FIG. 2 shows a diagram of a typical optical interferometer.
FIG. 3 shows a simplified diagram of an autocollimator.
FIG. 4 shows a schematic view of a preferred embodiment of the present invention, including an optical interferometer, an autocollimator, and a reverse telescopic lens assembly.
FIG. 5 shows a typical measurement setup utilizing two modules of the present invention.
DETAILED DESCRIPTION
The present invention combines an optical interferometer with an optical autocollimator to measure a target's linear translation in one dimension and rotational orientation in two dimensions with a single low-intensity laser beam. As shown in FIG. 1 , linear translation of an object 130 along the y-axis may be measured by an optical interferometer 110 that directs a light beam 100 against a reflective surface 140 .
FIG. 2 shows a diagram of a typical optical interferometer. A stable light source 200 emits a coherent light beam 210 that impinges upon a beam splitter 260 as is known in the art. A reference portion 220 of the light beam 210 is directed to a fixed reference reflector 230 and returned to the beam splitter 260 . A target portion 240 of the light beam 210 passes through the beam splitter 260 to impinge upon a target reflector 250 . The target reflector 250 may be a flat reflector, retroreflector, or other suitable reflector affixed directly or indirectly to a surface or object having its linear translation measured. The target portion 240 of the light beam is returned from the target reflector 250 to the beam splitter 260 to be recombined with the reference portion 220 of the light beam 210 .
The position of the reference reflector 230 is fixed with respect to the beam splitter 260 , so linear translation of the target reflector 250 along the axis of the beam causes a phase shift between the target beam 240 and the reference beam 220 . Resulting interference within the recombined beam 270 produces minima and maxima that are sensed by a fringe counter 280 as the target reflector 250 translates on the axis of measurement. The positional change of the target reflector 250 may be calculated from the number of fringes sensed by the fringe counter 280 .
FIG. 3 depicts the operation of a generalized autocollimation device utilizing light from a point source. Light rays 310 from a light source 300 are refracted by a lens 320 into a collimated beam 330 comprising parallel rays. The collimated beam 330 is reflected by a flat reflector 340 back through the lens 320 , which focuses the collimated beam 330 to a receiving point 350 on the plane of the light source 300 . If the collimated beam 330 is orthogonal to the flat reflector 340 , the receiving point 350 will coincide with the light source 300 . However, if the flat reflector 340 is angled with respect to the collimated beam 330 , the receiving point 350 will shift with respect to the light source 300 a distance d. For small angles (where tan(2a) is approximately equal to 2a), the slant angle a in radians of the flat reflector 340 may be calculated as a=d/2f where f is the focal length of the lens 320 .
The present invention places both an interferometer and an autocollimator in the same beam path, allowing measurement of pitch, yaw, and linear translation with a single beam. FIG. 4 shows a schematic view of a preferred embodiment of the present invention that combines an interferometer and an autocollimator. An HeNe or other laser 400 as is known in the art emits a beam containing at least two orthogonally polarized components. Output from the laser 400 is conducted by a Polarization Maintaining (PM) fiber 402 to a lens 404 that directs the beam into an interferometer 406 . The PM fiber allows isolation of the laser 400 from the measuring apparatus, reducing extraneous heat and vibration that may degrade measurement accuracy. The preferred interferometer of the present invention comprises a polarizing beam splitter 420 , quarter-wave retardation plates 421 , 422 , a fixed retroreflector 424 , and a fringe counter 426 , as are all known in the art. The preferred embodiment may also comprise a reverse telescopic lens assembly 428 .
As previously described, a light beam directed into the interferometer is divided by the polarizing beam splitter 420 into a reference beam 405 and an outgoing target beam 407 . The outgoing target beam 407 passes through a quarter-wave retardation plate 422 and an autocollimator 408 comprising a beam splitter 430 , a lens 432 , and a detector 434 . The outgoing target beam 407 initially passes through the beam splitter 430 and strikes a flat reflective target surface 410 , from which a return target beam 409 is reflected back through the beam splitter 430 . The target 410 is typically a flat mirror, although corner reflectors and other known specular reflectors may be used.
Although FIG. 4 depicts outgoing and return target beams as traveling separate paths for clarity, both travel the same path when the target surface 410 is orthogonal to the outgoing target beam 407 . The beam splitter 430 directs an autocollimator portion 436 of the return target beam 409 through a lens 432 that focuses the autocollimator portion 436 of the beam onto a detector 434 . The detector 434 generates an output signal corresponding to the location of the focused beam on the detector surface that is communicated via a serial connector 440 or other data connector known in the art to a computer (not shown). A typical detector 434 would utilize a lateral effect photodiode. An alternate embodiment of the present invention may utilize a dual-axis lateral effect photodiode such as an SC/10 from United Detector Technology. A dual-axis photodiode provides two output signals which together measure in two lateral dimensions where on the photodiode focused beam strikes.
Since the autocollimator portion 436 of the beam enters the autocollimator 408 as an undiffused laser beam, the preferred autocollimator 408 of FIG. 4 is simplified in comparison with the generalized autocollimation device of FIG. 3 . No return reflection path is required within the autocollimator 408 to collimate the autocollimator portion 436 of the beam. No point source is needed to establish a zero-deviation point. Instead, any point on the detector 434 may be arbitrarily designated as a zero-deviation point.
When the reflective target surface 410 is orthogonal to the outgoing target beam 407 , the autocollimator portion 436 of the beam is orthogonal to the outgoing target beam 407 and focused on a zero-deviation point on the detector 434 . Reorientations of the reflective target surface 410 corresponding to changes in the pitch or yaw of the surface cause the focal point of the autocollimator portion 436 of the reflected beam to shift across the surface of the detector 434 , allowing measurement of the amount of shift and calculation of the pitch and yaw angles. The output voltage signal from the detector 434 is converted to digital form by an A/D converter for transmission to a computer.
The remainder of the return target beam 409 returns to the interferometer beam splitter 420 to be recombined with the reference beam 405 and directed into the fringe counter 426 for measurement of linear translation of the reflective target surface 410 . Fringe counters known in the art typically generate an averaged output signal from an array of detectors (not shown) corresponding to movement of minima and maxima across the detectors. The present invention may utilize any suitable fringe counter known in the art. The fringe counter output signal is communicated via a serial connector 442 or other data connector known in the art to a computer (not shown). The present invention may additionally be equipped with time-of-flight detectors as are known in the art to initially establish the absolute distance between the present invention and the target reflector.
Changes in the pitch or yaw of the reflective target surface 410 cause the return target beam 409 to shift across the fringe counter detector arrays, introducing measurement errors and, with a sufficient shift, directing the return target beam 409 away from the array altogether. A preferred embodiment of the present invention introduces a reverse telescopic lens assembly 428 into the return target beam 409 path between the polarizing beam splitter 420 and the fringe counter 426 . The reverse telescopic lens assembly 428 , which is essentially a reversed telescope as is known in the art, reduces the angle of deviation of the return target beam 409 by the reciprocal of assembly's magnification, so that a 10× telescopic array would reduce a 10 second deviation to a 1 second deviation. This reduction advantageously allows measurement of significantly larger changes in pitch and yaw while still allowing accurate linear translation measurements. Placement of the reverse telescopic lens assembly 428 between the polarizing beam splitter 420 and the fringe counter 426 advantageously allows the reduction of interferometric error without affecting autocollimator 408 operation.
FIG. 5 depicts an application of the present invention. A platform 502 with mirrored surfaces 504 A, 504 B moves upon a base 500 . The position of an object (not shown) mounted upon the platform 502 may be measured and calculated as the platform 502 moves. A laser 508 supplies light through PM fibers 510 A, 510 B to measuring devices 506 A, 506 B embodying the present invention. The measuring devices 506 A, 506 B may be mounted on the base 500 or on fixtures within line-of-sight of the platform 502 . Preferentially, the laser beams 512 A, 512 B projected by the measuring devices 506 A, 506 B are mutually orthogonal. Data cables 522 A, 522 B transmit the outputs of both the fringe counters and the autocollimator detectors in each measuring device 506 A, 506 B device to a computer 520 .
As the platform 502 moves upon the base 500 , the interferometric components of each measuring device respond to translational movement on the x and y axes, with one measuring device 506 A measuring translation along the x-axis while the other measuring device 506 B measuring translation along the y-axis. Rotation of the platform 502 about the z-axis (yaw) causes the reflected laser beams 512 A, 512 B to shift direction, in turn causing the autocollimator portions of these beams to shift across the autocollimator detector surface within each measuring device 506 A, 506 B. The resulting output signals are processed within a computer 520 utilizing hardware and software disclosed in the applicant's previous patents and patent applications and/or well-known in the art to calculate, store, display, and/or output changes in platform 502 position and orientation. Both measuring devices can measure yaw, although autocollimator detector output from one would ordinarily be selected. If the platform 502 is rotated out of the plane of the base 500 , one measuring device 506 A can measure roll while the other measuring device 506 B can measure pitch.
An additional interferometer (not shown) with a beam parallel to the z-axis could be added to measure translation along the z-axis. With suitable components, the present invention can measure translational movement of one nanometer and angular changes of 1/100 of a second of arc.
The principles, embodiments, and modes of operation of the present invention have been set forth in the foregoing specification. The embodiments disclosed herein should be interpreted as illustrating the present invention and not as restricting it. The foregoing disclosure is not intended to limit the range of equivalent structure available to a person of ordinary skill in the art in any way, but rather to expand the range of equivalent structures in ways not previously contemplated. Numerous variations and changes can be made to the foregoing illustrative embodiments without departing from the scope and spirit of the present invention. | An optical measurement system increases the number of translational and angular measurements made with a single laser beam by combining an optical interferometer with an optical autocollimator. Translational measurements are made with an optical interferometer and yaw and pitch measurements are made with an autocollimator. In a preferred embodiment, angular deviations in the reflected measuring beam are minimized with a reverse telescopic lens assembly, allowing a wider range of angular measurements without significant degradation of interferometer accuracy. | 6 |
CROSS-REFERENCE TO RELATED APPLICATIONS
The present Application is a Continuation-in-Part of my co-pending Application, Ser. No. 07/105,660, filed on Oct. 7, 1987, and now U.S. Pat. No. 4,843,661.
BACKGROUND OF THE INVENTION
1. Field of the Invention
The invention relates to devices that assist people as they rise up from a seated position in a chair, more particularly to assists which are removably separate from the chair structure.
2. Description of the Prior Art
Many persons have difficulty rising from a seated position, because of an infirmity due to illness, advanced age, or other debilitation. This becomes of especial concern when chairs and couches are used, as the individual may be deeply seated in the cushioning, aggravating any difficulty in getting up.
Devices for assisting persons rising from a seated position are generally of two types. One type utilizes a mechanism within the seat itself which actually lifts up as the person rises from a seated position, thereby assisting him or her. These devices are expensive and only help people when they sit in those particular pieces of furniture that include the lifting mechanism. The other type, which encompasses the class of inventions to which the present invention appertains, utilizes a handle means to permit the seated person to grab hold of and pull on while rising. These devices have the advantage that they are not connected to any particular piece of furniture, and so may be employed wherever the individual may be seated.
Prior assist devices, such as U.S. Pat. Nos. 3,041,636 to Twedt, 3,272,530 to Klasses, and 4,157,593 to Kristensson, are rather complicated and are more particularly directed to infirm persons who are generally non-ambulatory, in that a retaining structure is provided to prevent the user from falling out of the device and dolly wheels are provided for locomotion.
It is an object of the present invention to provide an assist for seated persons to aid in helping them rise in the form of an inexpensive, portable, foldable, simple device provided with easily reachable handles for the user to grab hold of while rising.
It is an additional object of the present invention to provide an assist to seated persons having handles to grab hold of enabling them to more easily rise, while maintaining simultaneously an unobstructed pathway through which users may walk while entering or leaving the immediate vicinity of the seat.
It is another object of the present invention to provide an assist to seated persons so that they may more easily rise that works efficiently with any type of seating, be that a chair, sofa, bed, or other structure on which a person may sit.
It is a further object of the invention to provide an assist for seated persons to aid them while rising which includes means to stabilize it against pitching up while the user pulls on the handles.
It is still a further object of the present invention to provide an assist for seated persons to aid them while rising by providing handles which allow them to push downwardly thereonto, thereby allowing them to lift themselves up from the seat.
These and additional objects, advantages, features, and benefits of the invention will become apparent from the following specification.
SUMMARY OF THE INVENTION
The present invention is a portable, adjustable assist device for seated persons that aids in enabling them to rise to a standing position. The invention consists broadly of a platform having two handles which are rotatably attached thereto and stabilizers which are extendably attached to the platform, being extensible outward in the plane of the platform. The handles are separated from each other to allow a user to walk between them.
In operation, the user places the assist in front of a seat, rotates the handles into a raised position which is generally perpendicular to the platform surface, extends the stabilizers, positions the assist adjacent the seat, and sits down. To get up, the user grabs the handles, one in each hand, and pulls or pushes downwardly, as needed, while rising up. The user can then walk directly across the platform and away from the seat in a normal fashion. The invention may then be removed in a manner opposite in sequence to the manner in which it was deployed.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a perspective view showing the invention configured for deployment.
FIG. 2 is a side view of the invention as shown in FIG. 1, along lines 2--2.
FIG. 3 is a plan view of the invention as shown in FIG. 1.
FIG. 4 is a front detail view of the handle attachment to the platform according to the invention, along lines 4--4 in FIG. 3.
FIG. 5 is a plan view as in FIG. 3, showing the folded configuration of the present invention for transportation.
FIG. 6 is a detail view of the spring pin members as indicated by circle 6 in FIG. 2.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
Referring now to the drawings, FIG. 1 shows the invention generally as it would be configured for deployment in front of a seat. A rigid, generally rectangular platform 10 is provided from which depends a set of stabilizers 12 and 14 as well as a set of handles 16 and 18. Each of the handles are rotatably attached to the platform by a part cylindrically shaped bracket member 20 and 22 respectively, which traps a portion, 24 and 26 respectively, of the handles rotatably in relation to the platform. Additionally, spring pins 28 are provided on the trapped portion of the handles which are spring biased outwardly from the handles. The spring pins 28 are receivable into apertures 30 provided on the bracket members for holding the handles in a generally perpendicular orientation relative to the platform 10. It is preferred that the spring pins be attached to the handles by use of a strip of spring steel 27, as shown in FIG. 6. The orientation for deployment of the invention relative to the seat to which it is to be used in conjunction with, is such as to permit the stabilizers to extend under the seat; that is, the stabilizers are directed toward the seat. The stabilizers ensure that the torque generated by a person in the act of rising, who is pulling on the handles, will not cause the platform to pitch up.
FIG. 2 shows generally the relative orientation between the platform, handles and stabilizers along line 2--2 in FIG. 1. It will be seen from in spection of the figures that the handles are designed to have a generally "U" shape. This is to ensure that the torque generated by the user in the act of rising does not bend or in any other way distort the handles. The handles are rotatably deployed into a generally perpendicular orientation relative to the platform when the spring pins insert into the apertures provided on the bracket members. In this way, a person seated in a customary manner can easily reach the handles by simply stretching his or her arms straight outward. It will be seen by reference to the figures, that the preferred shape of the handles include a portion angled with respect to the platform at an angle other than ninety degrees. This aids in stabilizing the invention when the user pulls on the handles, as well as provides a section of the handle, respectively 32 and 34, that is preferred to be slightly angled off from the vertical, making it a bit easier and more efficient for the user to grab hold of and pull on when attempting to rise from a seated position. Each of the handles further has an additional section 33 and 35 which is oriented substantially horizontally and which is intended for the user to push downwardly on when rising up from a seated position.
FIG. 3 is a top view of the invention. The stabilizers 12 and 14 are, respectively, provided with slots 36 and 38 running longitudinally along their axial length into which a pin or rivet 40 and 42 respectively insert. The pins 40 and 42 are fixedly attached to the platform and act as slidable fastening means for the attachment of the stabilizers to the platform. The length of the slots determine the maximum extendable length of the stabilizers. This length is determined by practical considerations of the torques generated by anticipated users, which recommends a length on the order of one to two feet, where the platform is on the order of two feet square. The stabilizers are designed to be of a "U" shape structure that enables the stabilizer to mate with the platform edge on three sides, as shown more particularly as D, E, and F in FIG. 4. This feature ensures that the stabilizers will be slidably stable by cooperative action of the surfaces of the platform and stabilizer at surfaces D, E and F, in conjunction with that of the stabilizer slot and platform pin 42. A frictional coefficient of moderate value between the platform and the stabilizer surfaces is sufficient to retain the stabilizer at a selected extended or retracted position relative to the platform.
The platform 10 is composed of plywood, plastic, aluminum, or other hard, durable, stiff material can be used for its composition. While the figures depict a substantially rectangular platform having four edges, platforms having other numbers of edges are possible, the least being three. The handle rotation feature is accomplished by use of two bracket members 22 and 24, for each handle respectively. A portion 43 of each bracket member is fixedly attached to one side of the platform 10 by means of common fasteners 44, such as rivets; however, other means, such as welding or gluing, are possible. The remaining portion 45 of the bracket members has a part cylindrical shape which covers the trapped portion 24, 26 of the handles so that they are held in proximity with the platform, while yet being free to rotate relative to the platform. Guide pins 46 are provided on the handles which outwardly extend from the surface of the handles and interferingly engage the edge of the bracket members to prevent the handles from sliding translatably relative to the bracket members.
FIG. 5 shows the invention in the fully folded position, ready for easy transportation or storage. In this configuration, the stabilizers are preferably in a fully retracted position relative to the platform and the handles are rotated into a storage position characterized by being substantially in a plane parallel with that of the platform. In order that the handles may be rotated to a position as close as possible to the plane of the platform, it is necessary to translate one of the handles out of the way of the other. This is made possible by placing one guide pin 48 of the guide pins 46 a distance from the end of the bracket member equal to at least one diameter of the handles, as particularly shown in FIG. 5. To unfold the invention for use, first the handles are rotated to a deployed position characterized by being substantially perpendicular to the plane of the platform, wherein the spring pins engage the apertures in the bracket members to fixedly retain the handles in this position. Next the stabilizers are extended.
In operation, the user would carry the invention in the above indicated folded configuration to a location in front of the planned seating location. The hanldes are first rotated out to the locked position. The stabilizers are then extended. The invention is thereupon positioned directly in front of the perspective seat, oriented so that the stabilizers face toward the seat. The width of the stabilizer spacing is such as to allow for insertion under the seat, avoiding interference with legs or other obstructions. The assist platform according to the invention is then positioned so that the stabilizers slide under the seat and the handles touch the front of the seat.
The user thereupon walks across the platform and sits down normally. To get up, the user grabs the handles, one in each hand, and thereupon: (a) pulls on the handle sections 32 and 34 toward him or her as needed to rise, and/or (b) pushes downwardly on the handle sections 33 and 35 as needed to rise. It should be noted that the user in the act of rising to a standing position would have his or her feet firmly on the platform, this will serve as an additional aid against the tendency of the platform to pitch up. Once standing, the user walks across the platform freely.
Because the platform is not in any way connected to the seat, it may be folded up at any time by pressing inwardly on the spring pins and then rotating the handles, followed by retracting of the stabilizers by pushing on them.
The preferred embodiment of the invention has incorporated on the underside of the platform a plurality of anti-skid strips 50.
To those skilled in the art to which this invention appertains, the above described preferred embodiment may be subject to change or modification. For instance, the invention may be practiced without foldable handles. Further, the handles may be interconnected with a frame structure, the frame structure providing connection of the handles with respect to the platform. Still further, the frame structure itself may be designated as the platform, and either the frame structure is shaped so that it can serve as its own stabilizer or the stabilizers are connected with it in the manner described above. Such changes or modifications can be carried out without departing from the scope of the invention, which is intended to be limited only by the scope of the appended claims. | A portable assist to aid persons who have difficulty rising from a seated position including a platform having connected therewith two handles and an adjustable stabilizer which prevents the platform from pitching while the user pulls on the handles while in the act of getting up. The handles may be rotatably connected with respect to the platform. A section of the handles may be horizontally oriented so that the user may push downwardly thereupon in order to rise. | 8 |
FIELD OF THE INVENTION
[0001] The present invention is directed to an earth-working vehicle, such as a backhoe loader, having an implement, such as a backhoe, in which the implement is capable of being shifted transversely of the vehicle.
BACKGROUND OF THE INVENTION
[0002] For many years, it has been common to mount the backhoe support structure or swing tower on a frame and utilize a pair of hydraulic cylinders to pivot the tower with respect to the frame. In such a unit, the hydraulic cylinders are usually connected to the boom support or swing tower on opposite sides of the vertical pivot axis between the swing tower and the frame. For example, in one type disclosed in Long U.S. Pat. No. 3,047,171, the free ends of the piston rods of the hydraulic cylinders are connected to the frame structure at spaced locations while the cylinder barrels are connected at transversely spaced points to the swing tower or mast.
[0003] In more recent years, an earth-working vehicle of the type disclosed in the Long patent has also been mounted in a manner that the entire unit can be shifted transversely with respect to the vehicle. The frame supporting the mast or tower is supported on transversely extending rails that are secured to the rear end of the vehicle. This allows the operator to position the frame in any one of an infinite number of positions with respect to the fixed rails and readily lock the unit with respect to the rails.
[0004] A side-shift backhoe incorporates a frame which supports the backhoe mechanism and which is mounted for lateral, transverse movement with respect to the tractor or the like on which the backhoe is mounted. This type of backhoe was developed primarily for trenching in confined spaces, such as in close proximity to a house or other obstruction and enables operation closer to the obstructions than if the backhoe were mounted centrally of the rear of the tractor.
[0005] Traditionally, an implement bucket has been repositioned by uncontrolled movement of the backhoe while supporting the backhoe bucket teeth on the ground to one side and pushing the slide carrying the backhoe out on the other side using hydraulic cylinders. Some of the side-shift backhoes required complex components including hydraulically or manually operated clamps or pins.
SUMMARY OF THE INVENTION
[0006] In one preferred embodiment, an earth-working vehicle, such as a backhoe loader, has an elongated main frame and an implement support slidingly mounted to the main frame. The implement support is mounted at one end of the main frame and is capable of sliding transversely with respect to the elongated main frame. The vehicle also includes a motive means to slide the implement support with respect to the elongated main frame. The motive means includes a hydraulic motor mounted to one of the main frame and the implement support and either a chain having both ends secured to the other of the main frame and the implement support or the rack of a rack and pinion secured to the other of the main frame and the implement support. The hydraulic motor has a driving sprocket to drive the chain or a pinion to drive the rack and slide the implement support.
[0007] Other features and advantages of the present invention will be apparent from the following more detailed description of the preferred embodiment, taken in conjunction with the accompanying drawings which illustrate, by way of example, the principles of the invention.
BRIEF DESCRIPTION OF THE DRAWINGS
[0008] FIG. 1 is a fragmentary perspective view of a vehicle having an earth-working implement attached to the rear end thereof;
[0009] FIG. 2 is an enlarged fragmentary sectional view, as viewed along line 2 - 2 of FIG. 1 ;
[0010] FIG. 3 is an enlarged fragmentary sectional view, as viewed along line 3 - 3 of FIG. 2 ; and
[0011] FIG. 4 is a schematic illustration, as viewed along line 4 - 4 of FIG. 3 , showing structural support components.
[0012] FIG. 5 is a schematic illustration, similar to FIG. 4 , showing a second embodiment of the slidable implement support.
[0013] FIG. 6 is a schematic illustration, similar to FIG. 4 , showing a third embodiment of the slidable implement support.
[0014] FIG. 7 is a schematic illustration, similar to FIG. 4 , showing a fourth embodiment of the slidable implement support.
DETAILED DESCRIPTION OF THE INVENTION
[0015] FIG. 1 of the drawings generally shows an earth-working vehicle 10 including rear wheels 13 with an earth-working implement 14 secured to the rear end of the vehicle 10 . The vehicle 10 has a pair of horizontally oriented, vertically spaced rails 16 secured to the rear end of the vehicle 10 . Each of the rails 16 is substantially rectangular in cross section (see FIG. 3 ) and includes a rear vertical implement support plate 18 , with the rails releasably connected to vehicle 10 through quick release frame 17 . However, other rail and plate arrangements may be used. As most clearly shown in FIG. 3 , tower frame 20 consists of upper and lower plates 22 and 24 that are interconnected by a pair of vertical beams 26 . The transversely spaced vertical columns or beams 26 each have a pair of lock members or means 28 supported thereon for securely locking the tower frame 20 in any one of a plurality of adjusted positions with respect to rails 16 . These lock members or means may be of the type disclosed in Magee U.S. Pat. No. 3,494,636 or may be hydraulically actuated assemblies well known in the art.
[0016] Upper and lower plates 22 and 24 each have a pair of transversely spaced abutments 27 secured thereto by bolts and the abutments engage the forward surfaces of plates 18 while the lower surface of upper plate 22 is supported on the edge of upper plate 18 . Thus, the entire tower frame 20 may be laterally shifted with respect to rails 16 and locked in adjusted positions by lock means 28 .
[0017] Mobile tower frame 20 supports a swing tower 40 that has a substantial C-shaped configuration with upper and lower portions 42 and 44 respectively pivotally supported on upper and lower plates 22 and 24 by pivot pins 46 . Pivot pins 46 define a vertical tower pivot axis for supporting swing tower 40 for pivotal movement on tower frame 20 . Swing tower 40 supports an implement, such as backhoe 48 for pivotal movement about a horizontal pivot 49 . The backhoe 48 is well known in the art.
[0018] The swing tower 40 is pivoted with respect to the tower frame 20 by a pair of hydraulic cylinders that are mounted in order to allow the tower frame 20 to be moved along the sliding rails 16 while still having the center of gravity for the backhoe 48 as close as possible to the rear axle for the vehicle 10 . As most clearly shown in FIGS. 2 and 3 , the tower frame 20 has a support portion consisting of three plates 50 extending between rails 16 and the plates 50 terminating forwardly of the rails 16 . The two hydraulic cylinders, which define the swing mechanism for swing tower 40 , each include a cylinder barrel 52 and a piston rod 54 that extends from one end of the cylinder barrel 52 . Each of the cylinder barrels 52 has a trunnion mounting bracket 56 secured to the cylinder barrel 52 intermediate opposite ends with a pair of trunnions 58 carried by the bracket 56 . The trunnions 58 are received in openings 60 in the plates 50 so that the two cylinder barrels 52 are mounted in vertically spaced relation to each other and are located between an adjacent pair of plates 50 . Also, the openings 60 are positioned so that both cylinder barrels 52 are supported on a common vertical pivot axis at the forward ends of the plates 50 . It will be noted in FIG. 2 that the common pivot axis defined by openings 60 and trunnions 58 are located on a plane P, which extends through the pivot axis defined by pins 46 and this plane is generally parallel to the longitudinal axis of the vehicle 10 and the pivot axis may be located forward of rails 16 and between the rear edges of wheels 13 .
[0019] Piston rods 54 of the hydraulic cylinders are connected to an intermediate portion of the swing tower 40 . This connection consists of brackets 66 extending from the body of the swing tower 40 with pins 68 extending through the apertures in the brackets and apertures in the end of piston rods 54 . As shown in FIGS. 2 and 3 , the piston rods 54 are connected to the intermediate portion of the swing tower 40 at laterally and vertically spaced points, both of which are spaced from the vertical pivot axis defined by pins 46 .
[0020] As shown in FIG. 4 , a hydraulic motor 72 is supported on mounting bracket 73 that is securely mounted on the rear end of the vehicle main frame 74 . The hydraulic motor 72 provides the motive power to slide the implement support plate 18 and the attached backhoe 48 transversely of the vehicle 10 . The hydraulic motor 72 may be a low speed high torque hydraulic motor (LSHT motor). A driving sprocket 76 is mounted on the shaft of the hydraulic motor 72 .
[0021] The ends of a roller chain 79 are secured to a pair of yoke end connectors 80 that are mounted on the implement support plate 18 . See FIG. 4 . One end of the roller chain 79 is secured to one of the yoke end connectors 80 . The roller chain 79 passes around a chain sprocket 82 mounted to one side of the quick release frame 17 at one end of the rails 16 , around the driving sprocket 76 , around tensioner sprocket 84 mounted to the mounting bracket 73 , around a second chain sprocket 82 mounted to the other side of the quick release frame 17 at the opposite end of the rails 16 , and is secured to the second yoke end connector 80 . The tensioner sprocket 84 deters the roller chain 79 from jumping out from the sprockets.
[0022] The LSHT motor 72 rotates under applied hydraulic pressure from the vehicle hydraulic circuit at very low speeds without need for an intermediate speed reducer, and directly moves the roller chain 79 , which moves the backhoe 48 . The mechanism is simple with very few parts. Hence, frictional losses are minimal and the system is easy to maintain. The steel roller chain 79 is designed to operate without an enclosure. Due to the short duration and extent of movement, as well as the low speed of operation, the roller chain 79 runs efficiently without lubrication.
[0023] By using the present system, movement of the backhoe 48 is controlled. Safety is improved since the controlled movement is without jerking that is prevalent in the prior systems. The present system is compact and improves vehicle maneuverability.
[0024] A second embodiment of the slidable implement support is shown in FIG. 5 . In this embodiment, the mounting bracket 73 , on which the hydraulic motor 72 is secured, is mounted on the implement support plate 18 and the yoke end connectors 80 are secured to the main frame 74 . One end of the roller chain 79 is secured to one of the yoke end connectors 80 and passes around a chain sprocket 82 mounted to one side of the quick release frame 17 at one end of the rails 16 , around the driving sprocket 76 , around tensioner sprocket 84 mounted to the mounting bracket 73 , around a second chain sprocket 82 mounted to the other side of the quick release frame 17 at the opposite end of the rails 16 , and secured to the second yoke end connector 80 . A third chain sprocket may be mounted on the mounting bracket 73 opposite the tensioner sprocket 84 to guide the roller chain 79 more parallel to the movement of the implement support plate 18 .
[0025] In FIG. 6 , the mounting bracket 73 and hydraulic motor 72 are mounted on the implement support plate 18 and the roller chain 79 is replaced with a rack 86 . The hydraulic motor 72 drives the pinion 88 moving the implement support plate 18 transversely with respect to the vehicle main frame 74 .
[0026] The mounting bracket 73 , hydraulic motor 72 and pinion 88 may be mounted on the rails 16 , as shown in FIG. 7 . In that case, the rack 86 is mounted on the implement support plate 18 .
[0027] While the invention has been described with reference to a number of preferred embodiments, it will be understood by those skilled in the art that various changes may be made and equivalents may be substituted for elements thereof without departing from the scope of the invention. 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 embodiments 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. | An earth-working vehicle, such as a backhoe loader, has an implement, such as a backhoe, mounted in a manner that the implement can be shifted transversely with respect to the vehicle. A hydraulic motor and roller cable or rack are secured to the vehicle main frame and implement supporting plate to position the implement transversely of the vehicle without the jerky movements of prior backhoe loaders. | 4 |
RELATED APPLICATION
This patent application is a continuation of U.S. patent application Ser. No. 13/749,603, filed Jan. 24, 2013, which is a continuation of U.S. patent application Ser. No. 13/137,064, filed Jul. 19, 2011 and now abandoned, which is a divisional of U.S. patent application Ser. No. 12/379,461, filed Feb. 23, 2009 and now U.S. Pat. No. 7,980,916, which was a continuation-in-part of U.S. patent application Ser. No. 11/177,428, filed Jul. 11, 2005 and now U.S. Pat. No. 7,753,755, which claims priority to U.S. Provisional Application Ser. No. 60/640,041, filed Dec. 30, 2004. The U.S. patent application Ser. No. 12/379,461, filed Feb. 23, 2009 and now U.S. Pat. No. 7,980,916, also claims priority from U.S. Design patent application Ser. No. 29/312,447, filed Oct. 21, 2008.
FIELD OF THE INVENTION
This invention relates to radio-controlled motorized toy vehicles capable of operation on surfaces of all orientations, e.g., walls and ceilings as well as floors.
BACKGROUND OF THE INVENTION
Radio-controlled motorized toy vehicles, that is, vehicles driven by motors and steered responsive to commands transmitted remotely, are of course well-known. Toy vehicles that are very sophisticated in terms of their suspension and steering systems are available and are very popular. A toy vehicle that operated other than on essentially horizontal surfaces, e.g., which could operate on a vertical wall, or inverted on a ceiling, and which could be made and sold at a competitive price, would be very desirable.
U.S. Pat. No. 5,014,803 to Urakami shows a device for “suction-adhering” to a wall and moving along the wall, e.g. for cleaning the interiors of tanks and the like. The Urakami device relies on a relative vacuum; that is, air is drawn by a vacuum pump out from a sealed volume formed between the interior of the device and the wall, so that air pressure on the outer surface of the device forces it against the wall. This necessitates that an essentially air-tight seal be formed around the periphery of the device. Forming an air-tight seal between a moving device and a fixed surface is not a simple problem, and the Urakami patent is directed primarily to such seals. The obvious problems to be overcome are friction between the sealing member and the wall, which impedes motion of the device and causes wear of the sealing members, loss of vacuum at irregularities in the surface, and the large amount of power required to form an effective vacuum. This approach is not satisfactory for a toy vehicle that must be durable when operated by children and be able to be operated for a sufficiently long time with a limited amount of battery capacity to not frustrate the user.
SUMMARY OF THE INVENTION
The present invention provides a motorized toy vehicle that is capable of operating on vertical and inverted horizontal surfaces such as walls and ceilings, while being manufacturable at reasonable cost and operable on batteries having sufficient lifetime as to be enjoyable. The vehicle of the invention, referred to hereinafter as the Wall Racer, employs a freely-flowing stream of air between the surface-abutting periphery of the interior volume of the vehicle to create a pressure differential with respect to the surrounding air, so that the pressure of the surrounding air urges the Wall Racer against the surface.
More specifically, one or more battery-powered fans draw air from around all or defined portions of the periphery of the chassis of the Wall Racer through a carefully-shaped duct formed between the undersurface of the chassis and a juxtaposed surface, so that the air in the portion of the duct immediately adjacent the surface flows at high velocity. According to Bernouilli's Principle, this high-velocity air stream is of low pressure; the differential between this low-pressure air stream and the relatively greater pressure of the surrounding air urges the vehicle against the surface, allowing it to adhere to vertical surfaces, such as walls, or be operated inverted on horizontal surfaces, such as ceilings. The differential pressure thus urging the vehicle against the surface is referred to hereinafter, as in the automotive industry, as “downforce”. Because the air stream must be freely flowing to attain high velocity, seals such as required for wall-climbing vehicles employing a vacuum (and which make it very difficult to provide workable vehicles, as above) are unnecessary. Indeed, entry of the air into the duct formed between the undersurface of the chassis and the juxtaposed surface is essential, and is controlled carefully to ensure stable, and insofar as possible non-turbulent flow.
It would be of self-evident amusement interest, or “toy value”, to provide a radio-controlled vehicle capable of making the transition between operation on a floor to climbing a wall, and the Wall Racer in certain embodiments can do so. In order that the vehicle can make the transition, the fan(s) driving the air stream are actuated only when the vehicle begins to climb the wall.
Other inventive aspects of the Wall Racer will appear as the discussion below proceeds.
BRIEF DESCRIPTION OF THE DRAWINGS
The invention will be better understood if reference is made to the accompanying drawings, in which:
FIG. 1 and FIG. 2 show respectively a perspective view and an elevation in partial cross-section of a first embodiment of the Wall Racer;
FIG. 3 and FIG. 4 show respectively a perspective view and an elevation in partial cross-section of a second embodiment of the Wall Racer;
FIGS. 5, 6, and 7 show views of a gear train employed in the embodiment of FIGS. 3 and 4 ;
FIG. 8 and FIG. 9 show respectively a perspective view and an elevation in partial cross-section of a third embodiment of the Wall Racer;
FIG. 10 and FIG. 11 show respectively a perspective view and an elevation in partial cross-section of a fourth embodiment of the Wall Racer;
FIG. 12 shows a detailed diagram of one successful shape for the duct employed to form the high-velocity air stream, e.g., as employed in the second embodiment of FIGS. 3 and 4 ;
FIG. 13 shows a cross-sectional view of a switch employed to actuate the fans when the Wall Racer transitions from floor to wall operation, and which prevents its operation inverted on a ceiling, for safety reasons, while FIG. 13A shows a typical circuit in which it may be used;
FIGS. 14, 15, and 16 show respectively a perspective view, an elevation in partial cross-section, and an enlarged cross-section of a caster used in several of the embodiments of the Wall Racer, while FIG. 14A shows a partial view corresponding to FIG. 14 , illustrating a optional variation; and
FIGS. 17, 18, and 19 show a further embodiment of the invention, wherein FIG. 17 is a schematic plan view, FIG. 18 a partial cross-section taken along the line 18 - 18 in FIG. 17 , with certain components shown in dotted lines, and FIG. 19 is a partial cross-section taken along the line 19 - 19 in FIG. 17 .
DESCRIPTION OF THE PREFERRED EMBODIMENTS
It will be apparent that one type of Wall Racer toy vehicle that would be desirably offered is one resembling an automobile, for example a race car, while other sorts of vehicles, such as trucks or military vehicles, e.g., armored tanks, might also be of interest. The first, second, fourth and fifth embodiments of the Wall Racer discussed herein are of generally elongated shape, so as to be fitted with model automobile bodies not otherwise contributing to the operation of the Wall Racer, while the third embodiment is circular and might be made to resemble a “flying saucer” type of space vehicle. All of these embodiments operate similarly, with differences as occasioned by the differing body shapes.
For example, FIGS. 1 and 2 show respectively a perspective and an elevation in partial cross-section of a first embodiment of the Wall Racer, which as noted is generally elongated and could readily be fitted with a model race car or other vehicle body (not shown). As mentioned above, in order that downforce urging the Wall Racer against an abutting surface W (hereinafter simply “the wall”) can be developed, a high velocity stream of air is induced to flow in an underbody venturi duct formed between the undersurface of the chassis of the Wall Racer and the wall W. According to Bernouilli's Principle, as above, such a high velocity stream of air will be of reduced pressure with respect to the ambient air. The differential between this reduced pressure and the surrounding atmospheric pressure generates a resultant force D, termed “downforce” where, as here, its direction is such as to urge the vehicle “downwardly” toward the wall W. The amount of downforce D developed is proportional to the area over which the low pressure is created, and to the differential in pressure per unit area, so this area and the differential pressure must be adequate for the purpose.
Thus, as illustrated in FIGS. 1 and 2 , a fan 10 is mounted in a fan duct extending through the chassis 12 , and is driven by a battery-powered motor 11 so as to draw a high-velocity stream of air in from around at least a portion of the periphery of chassis 12 . The stream of air flows through an underbody venturi duct 15 formed between the underside of chassis 12 and the juxtaposed surface of wall W, and is exhausted on the “upper” side of chassis 12 , that is, on the side away from the abutting wall W. Downforce D is created as noted due to the differential in pressure between the low pressure of the high-velocity air stream in the underbody venturi duct and the ambient air; as noted, the total amount of downforce is proportional to the area over which the low pressure is developed, and to the differential in pressure at each point.
To maximize the area of low pressure by avoiding air being drawn in along the edges 12 a of the chassis 12 , that is, to ensure that the air stream is principally drawn in at the ends 12 b of the chassis 12 , flexible “skirts” 14 extend from the chassis 12 toward wall W and form a partial seal therebetween, limiting “short-cutting” of air from the sides of the chassis juxtaposed to the fan duct. The skirts thus define one or more, in this case two, sections of the periphery of the underbody of the chassis at which air is drawn into an entry portion of the underbody venturi duct, which directs airflow into the fan duct. Accordingly, air is drawn in primarily at the ends 12 b , which are provided with a broad radius to ensure smooth and insofar as possible non-turbulent airflow; for similar reasons, the undersurface 12 c of the chassis 12 is smooth. Thus the high-velocity air stream extends for a substantial portion of the overall length of the chassis, ensuring that adequate downforce is developed. In the absence of the skirts 14 , air would tend to be drawn in along the sides of the chassis, limiting the area over which the reduced pressure is developed, and thus limiting downforce; there would likely also be considerable turbulence, further interfering airflow and reducing downforce.
In some circumstances, a further increase in downforce can be realized by limiting the clearance between the ends of the undersurface of the chassis and the wall surface, e.g., by providing downwardly extending baffles, akin to the side skirts 14 but extending only to the wall surface, that is, not intended to be drawn against the wall surface as are the side skirts 14 . The reduction in intake area causes a further acceleration of the air flowing under these baffles, further reducing the pressure and increasing the downforce.
By comparison, in the generally circular third embodiment of the Wall Racer shown in FIGS. 8 and 9 (discussed further below) a substantial distance exists between all points on the outer periphery of the undersurface of its chassis and the centrally-located exhaust duct, so that the airflow in this embodiment is radially inwardly from all directions, the downforce is developed uniformly around the chassis, and no skirts need to be fitted.
As noted, the differential in pressure and thus the downforce developed is a function of the air velocity, which up to a point can be increased by reducing the cross-sectional area of the duct formed between the underside of the chassis and the wall W, that is, by reducing the ground clearance of the Wall Racer. However, if the cross-sectional area is reduced too much, turbulence will impede flow and reduce the desired effect; reducing the ground clearance would also increase the Wall Racer's sensitivity to surface irregularities and the like. No detailed theoretical calculations have as yet been carried out which would allow optimization of the effect sought. For example, by optimizing the duct design the current draw of the motor powering the fan inducing the flow could perhaps be reduced, increasing operating time per battery charge. Detailed specifications of the duct and other components employed in a successfully-tested embodiment of the Wall Racer are provided below.
Returning to discussion of the first embodiment of FIGS. 1 and 2 , as illustrated the chassis 12 is supported by two opposed drive wheels 16 and 18 , spaced transversely from one another on either side of the chassis near the midpoint thereof, and by opposed casters 20 (that is, devices comprising freely-rotating wheels mounted for pivoting about an axis perpendicular to their axis of rotation) at either end of the chassis 12 . As indicated schematically by belt drives 22 , the opposed drive wheels 16 and 18 are separately powered by motors 24 that are supplied with current by a battery pack 28 in response to control signals provided by radio-controlled receiver 26 . The overall construction and operation of these components is conventional except as noted and will not be discussed in detail herein. Thus, if both motors are controlled to drive wheels 16 and 18 in the same direction, the Wall Racer moves in that direction, while turning is accomplished by driving the wheels 16 and 18 in differing directions or at differing rates. Casters 20 are unpowered, mounted on the longitudinal centerline of chassis 12 , and simply serve to maintain the correct spacing between undersurface 12 c of chassis 12 and wall W; preferred locations and design of casters 20 are discussed below.
The “differential” drive scheme shown is preferred over, for example, a conventional four-wheel chassis, with one pair of wheels powered and one pair steering, for the following reasons. In order that a vehicle can climb a vertical wall, sufficient downforce must be exerted, urging the vehicle toward the wall, not only to support the vehicle against the force of gravity but also to provide sufficient traction to propel the vehicle vertically against gravity. (By comparison, providing a vehicle that operates inverted on a ceiling is simplified, since it need only support itself and need not also climb vertically.) Ensuring good traction thus becomes paramount. So as to maximize the traction provided by the downforce available, the drive wheels are located centrally, at the center of the pressure exerted by the downforce, so that essentially all of the downforce is transmitted directly to the drive wheels, maximizing traction.
The casters 20 are preferably mounted so that both do not simultaneously touch a flat surface, so that a three-point support is always available, with the drive wheels 16 and 18 forming two of the three contact points. The motion thus provided, whereby the vehicle can rock slightly back and forth about the axis of the drive wheels 16 and 18 , as one or the other of casters 20 touches the wall W, is referred to as “teeter” herein. Thus the downforce is balanced over the central drive axle, which maximizes traction, while allowing the vehicle to be steered by differential driving of the opposed drive wheels 16 and 18 .
FIGS. 3 and 4 show a second embodiment of the Wall Racer; this embodiment appears likely to correspond to the earliest production version of the Wall Racer. FIG. 12 provides detailed dimensional information concerning this embodiment, and preproduction specifications are provided below as well.
As shown by FIG. 3 , in this embodiment two exhaust fans 38 are provided, spaced laterally from another on the transverse centerline of the chassis 40 , and each fan being driven by a motor 39 with the fan mounted directly on the motor shaft. Six drive wheels 42 are provided, three on either side of the chassis 40 , with the three wheels 42 on either side of the chassis being geared (or belt-driven) to one another so as to be driven in common by two separately radio-controlled motors. The radio control receiver and battery are not shown, as being generally within the skill of the art. FIGS. 5, 6, and 7 (discussed below) show a preferred gear train and motor arrangement. Thus, as in the FIG. 1 embodiment, steering is accomplished by differentially driving the wheels on either side of the chassis 40 . As shown, skirts 44 are again provided, so as to ensure that the airflow is primarily from the ends of the chassis to the fan exhaust duct 46 , in turn to ensure that an adequate area of high-velocity, low-pressure air flow is provided to generate adequate downforce. As illustrated by FIG. 4 , the center pair of wheels are slightly lower in the chassis than the end pairs, so as to provide “teeter” and ensure that the center pair of drive wheels are always in good contact with the wall W.
The pairs of wheels 42 at each end of the chassis are slightly proud of (i.e., extend slightly beyond) the respective ends of the chassis, so that as the vehicle approaches a wall while operating on a floor, the wheels contact the wall first. Thus providing the six-wheel arrangement of this embodiment allows the Wall Racer to make the transition from floor to wall in either direction. So that downforce urging the Wall Racer toward the floor does not prevent the Wall Racer from initially climbing the wall, the fans 38 are only energized when the chassis 40 reaches a predetermined inclination with respect to the horizontal. FIG. 13 shows a preferred switch, and FIG. 13A a circuit, for controlling the fans accordingly.
As indicated above, FIGS. 5, 6, and 7 show a preferred arrangement of the two drive motors and corresponding gear trains for differentially driving the six wheels of the Wall Racer in its FIGS. 3 and 4 embodiment. FIG. 5 shows a plan view, and FIGS. 6 and 7 cross-sectional views along lines 6 - 6 and 7 - 7 respectively. Thus, assuming the Wall Racer is traveling toward the right in FIG. 5 , so that the upper side of the drawing is the “left”, and the lower the “right”, there are provided left-side and right-side drive motors 150 and 152 respectively. Motors 150 and 152 each drive reduction gear trains, 154 and 156 respectively; the gears of each are idlers, that is, spin freely on shafts 158 , so that gears from both trains can be supported on the same shafts 158 while turning independently of one another. The output gears of train 154 and 156 drive gears 160 , 162 respectively, which are fixed with respect to sleeve axles 164 , 166 respectively, riding on a fixed axle 168 , and thence to gears 170 , 172 respectively. Gears 170 , 172 are fixed to corresponding drive wheels 174 , 176 , and also drive further gear trains 178 , 180 , which drive central drive gears 182 , 184 , which are fixed to central drive wheels 186 , 188 . Central drive gears 182 , 184 also drive further gear trains 190 , 192 ; these in turn drive gears 194 , 196 , to which are fixed wheels 198 , 200 . Implementation of this drive arrangement is within the skill of the art; while the gear trains and axles are shown as mounted on a metallic frame 202 , in production this chassis will typically comprise molded components.
It is also within the scope of the invention to employ a generally comparable arrangement to provide a four-wheel drive version of the vehicle of the invention, with differential steering as above. In this case one of the wheels might be mounted so as to spaced very slightly away from a plane contacted by the other three wheels; consequently the vehicle would “teeter” about an axis connecting the contact patches of the two of the wheels not diagonally opposite the wheel so spaced from the plane, so that either that wheel or the one diagonally opposite it would contact the plane. For example, if the left front (“LF”) wheel were slightly spaced from a plane contacted by the RF, LR, and RR wheels, the vehicle would teeter about an axis connecting the points at which the RF and LR wheels contact the plane, and the teeter would be limited by contact of either the LF or RR wheels with the plane. By comparison, if the wheels were located so as to simultaneously contact a flat plane, the vehicle would tend to be much more sensitive to any irregularities in the surface.
Implementation of differential steering of a four-wheel drive vehicle would not be unduly complex. By comparison, if steering were to be accomplished by pivoting of one or both pairs of wheels, this would involve additional complexity.
It is to be noted that a differential steering arrangement in a four-wheel drive vehicle with all four wheels in good contact with the surface would involve substantial resistance to steering due to “tire scrub”, that is, frictional resistance caused by the different effective turning radii of the “contact patch” of the tires on opposite sides of the vehicle. In general, to limit tire scrub within a given tire, relatively narrow tires are fitted to the drive wheels of the vehicles of the invention. Tire scrub becomes less significant as the overall size of the vehicle is reduced. To improve appearance, and to allow operation on thick carpets and the like, wider supplemental tires of slightly lesser diameter and formed of a lightweight foam or the like (not shown) can be assembled to the outer surfaces of the drive wheels.
As mentioned, FIG. 12 shows a detailed view of the underbody venturi duct 50 formed between the undersurface of chassis 40 and a juxtaposed surface, such as a wall W. This embodiment of the underbody was employed in one successfully-tested version of the second embodiment of the Wall Racer of the invention, as shown in FIGS. 3 and 4 . FIG. 12 further provides reference to dimensional details of the chassis 40 . In this version, the overall chassis length H is 11.828″, with six wheels of 2.524″ diameter; the wheelbase F of the outer pairs of wheels is 9.50″, so that the wheels are proud of the chassis, i.e., extend slightly beyond the end of the chassis 40 , in order to engage a vertical surface and thus enable the Wall Racer to climb a wall from the floor. The center axle is 0.050″ closer to the wall W than the end pairs of wheels, so that the desired “teeter” is provided.
The underbody venturi duct 50 is longitudinally symmetric about a centerline J, with one end only shown in detail by FIG. 12 . As shown in detail by FIG. 12 , each “half” of the underbody duct 50 formed between the undersurface of the chassis 40 and the wall W comprises an entry portion 50 a , a transition portion 50 b , and an exit portion 50 c , which makes a smooth transition into a fan duct 46 , also of venturi shape, in which the fan(s) are located. Air enters each half of the underbody venturi duct at an inlet opening at the periphery of the chassis 40 , defined by the entry portion 50 a of underbody venturi duct 50 . Entry portion 50 a is defined by a radius R formed on the end of the chassis; in the version shown, this radius is 1.164″. The axles of the front and rear pairs of wheels lie on the center of this radius, and are slightly larger in radius, so that each tire's rolling surface is somewhat proud of the chassis end, as noted. Entry portion 50 a is faired into and connects smoothly with an extended flat transition portion 50 b formed by a flat surface on the underside of the chassis; since the duct 50 formed between the underside of chassis 40 and the wall is of minimum cross-sectional area in this region, the maximum air flow velocity, and accordingly the maximum downforce per unit area, are developed here.
The goal in designing the underbody venturi duct 50 is to maximize the extent of the region of minimum cross-sectional area, while optimizing its cross-sectional dimension, so as to provide smooth, preferably non-turbulent flow into and out of this region, all in order to maximize flow velocity. To ensure smooth flow, the section of the undersurface of chassis 40 defining the upper bound of entry portion 50 a is radiused, and the corresponding section defining the upper bound of exit portion 50 c describes a portion of an ellipse. In the successfully-tested version depicted, this elliptical contour was drawn using a 2″×4″ ellipse as found on a draftsman's “30-degree” template; that is, dimensions D and C are 1″ and 2″, respectively. As illustrated, then, the extent E of flat portion 50 b is 2.25″ long, forming a “tunnel flat”. With the vehicle balanced on the center pair of wheels, so that the flat portion 50 b is parallel to the wall, the ground clearance G therebetween is 0.098″. Flat portion 50 b makes a smooth transition to exit portion 50 c , which as noted is 2.00″ long and elliptical in longitudinal cross-section. Exit portion 50 c in turn makes a smooth transition to a central venturi section 46 a of fan duct 46 , in which the fan(s) are located. In the two-fan embodiment of FIGS. 3 and 4 and detailed in FIG. 12 , the longitudinal dimension B of the narrowest portion of this venturi section 46 a is 1.00″; section 46 a extends across the chassis 50 so as to form a transverse “mail slot”. As it extends away from the wall, the mail slot section 46 a then broadens out gradually in the longitudinal direction and is divided along the longitudinal centerline to form two circular-section ducts 46 b in which the fans 38 are located; their diameter, dimension A, is 1.625″.
The following are the principal specifications of a successfully-tested version of the Wall Racer, as shown in FIGS. 3 and 4 and dimensioned as in FIG. 12 :
Wheelbase (dimension F) 9.5″ (front to rear axle) Track width 5.8″ (centerline to centerline, at contact points) Underbody duct width 4.9″ (between skirts) Chassis weight 584 g. Body weight 29 g. Total weight 613 g. Weight distribution (without body, center axle unsupported):
Front axle 260 g (44.5%) Rear axle 324 g (55.5%)
Ground clearance (dimension G) 0.098″ Motor voltage 6 v. nominal (five 1.2 v. 1000 mah NiMH cells) Downforce fans current draw 4 amperes total Ducted fans (two)—1.625″ diameter, 3 blades Total net downforce 1280 g. Teeter (center axle offset) 0.050″ Fan RPM 30,000
The chassis itself can be molded of a lightweight foam material, having its undersurface shaped to define the venturi duct 50 in cooperation with the surface of the wall W. It is convenient to mount the components, such as bearings for the axles carrying the wheels, drive motors and gear or belt drive components, radio control receiver, batteries, and motor and fan assemblies, in recesses molded into the foam of the chassis. In particular, the fan assemblies may alternatively comprise hard plastic molded ducts within which the fan and drive motor are retained; the exit portion of the underbody venturi duct is then shaped to mate smoothly therewith.
In a successfully-tested prototype, the skirts 44 ( FIG. 3 ) were formed of “Tyvek” spunbonded nonwoven olefin envelope material sized and located so as to curve outwardly at a nominal 45 degrees when in contact with the wall; a stiffening strip of plastic glued to the lower edge of the skirts, but spaced slightly therefrom, may be desirable to prevent local buckling.
Given the above detailed disclosure of the invention, those of skill in the art would have no difficulty in its practice. In particular, it will be appreciated that batteries (exemplary specifications being provided above) must be provided to power the fans and the drive wheels, that the drive wheels, three on each side in the embodiment of FIGS. 3 and 4 , must be linked to one another and to the respective drive motor by gears, as illustrated in FIGS. 5, 6 , and 7 , or by belts or other means, and that the motors must be individually controllable by signals provided by an operator by way of a radio or infrared transmitter and receiver pair. These aspects of the implementation of the invention are within the skill of the art. It is also within the scope of the invention to drive each of the six wheels individually, that is, to eliminate the gear or belt arrangement in favor of separate motors for each wheel, but this alternative is considered undesirable as it would involve a weight penalty.
FIGS. 8 and 9 show as mentioned a third version of the Wall Racer, in this case with a circular chassis 60 to provide a “flying saucer” appearance. In this version, two drive wheels 62 and 64 are provided on diametrically opposed points on the chassis 60 , with casters 66 on opposite sides, along a line perpendicular to the axis of the drive wheels 62 and 64 . The casters may be raised slightly from a plane including both drive wheels and the casters, to provide “teeter” as above. (It will be apparent that this version of the Wall Racer cannot negotiate the transition between floor and wall.) Downforce is provided by a centrally-located fan 68 disposed in a venturi duct 70 and driven by a motor 72 . Drive wheels 62 and 64 are individually driven by motors 74 and 76 responsive to control signals from a radio-control receiver 78 and powered by battery 80 .
In this version, as mentioned above, the exhaust duct 70 is equidistant from all points on the periphery of chassis 60 , so that the inward air flow path is of equal length at all points around the chassis 60 . Hence there is no need for skirts, and the air flow is radially inward all around the periphery. Again, a radius is provided around the periphery of the lower edge of chassis 60 , as illustrated at 60 b , so that the inlet opening of the underbody venturi duct extends circumferentially around the chassis, and a large-radius or elliptical transition portion 60 c is provided where the underbody duct 82 meets the exhaust duct 70 , to ensure smooth and substantially non-turbulent airflow. The transition portion of the underbody duct 82 formed between the underside 60 a of chassis 60 and the wall is preferably shallow and substantially conical in section, as illustrated, so that the cross-sectional area of the duct 82 stays constant as its radius from the center of exhaust duct 70 varies; in this way the velocity of the inward-flowing air stream and the differential pressure exerted thereby are both substantially constant, so that the downforce is exerted evenly at substantially all points on the chassis 60 , that is, outside of duct 70 .
FIGS. 10 and 11 show a further version of the Wall Racer, again having an elongated chassis 90 suitable for mounting of a model race car body or the like. In this embodiment, a single fan 92 is located centrally on the chassis, is driven by a motor 94 , and is disposed within an exhaust duct 96 communicating with an underbody venturi duct 98 formed between the underside of chassis 90 and the wall W. The underbody duct 98 is designed generally as discussed above with respect to FIG. 12 .
In this embodiment, a single drive wheel 100 driven by a motor powered by a battery and responsive to control signals provided by a radio control receiver (none of the unnumbered components being shown) is located on the vehicle's longitudinal centerline, near the center of effort of the downforce, but disposed toward one end of the chassis so as not to interfere with the exhaust duct 96 . Two casters 102 and 104 are mounted at the opposite end of the chassis 90 . Caster 102 is free to pivot about an axis perpendicular to wall W, while caster 104 is also pivoted about a similarly perpendicular axis, but only between angular limits (see FIG. 14A , below).
Thus, chassis 90 rests on a tripod comprising drive wheel 100 and casters 102 and 104 . If drive wheel 100 is driven so as to propel the vehicle toward the direction of the end of the chassis on which drive wheel 100 is disposed, that is, rightwardly in FIG. 11 , the casters trail behind, and the vehicle travels in a straight line; if drive wheel 100 is driven in the opposite direction (counterclockwise in FIG. 11 ), the caster 104 provided with angular stops rotates about the axis perpendicular to wall W until its pivoting is stopped at one or the other of its angular limits, so the vehicle turns in one direction until the direction of travel is reversed. Hence directional control of the Wall Racer in this embodiment is substantially constrained; being greatly simplified, this embodiment might be best suited to a low-cost version of the invention.
As mentioned, FIGS. 14-16 show respectively a perspective view, a cross-section, and an enlarged partial cross-section of a caster 102 used in several of the embodiments of the Wall Racer, while FIG. 14A shows a partial view corresponding to FIG. 14 , illustrating a optional variation. In these views, the caster 102 is shown inverted, that is, with its face which would be juxtaposed to wall W oriented “up” in the drawings. A roller 110 , which contacts wall W, is carried by an axle 112 that is mounted for rotation in a rotating plate 114 ; plate 114 rotates about an axis A perpendicular to but offset from that defined by axle 112 . In the embodiment shown, rotating plate 114 in turn rides on a number of balls 116 , which bear against a closure ring 118 ; closure ring 118 is secured to a frame 120 , which can be mounted to the chassis. Thus, roller 110 engages the wall, and rotates about axle 112 as the vehicle is maneuvered; the assembly of roller 110 , axle 122 and plate 114 can rotate with respect to frame 120 and thus with respect to the vehicle chassis, as the latter is steered. The axle 112 is offset with respect to the axis A about which plate 114 rotates, so that as the vehicle is steered, plate 114 rotates and roller 110 trails the axis A of rotation of plate 114 .
If it is desired to restrict the rotation of plate 114 , e.g., as discussed above with respect to the version of the Wall Racer shown in FIGS. 7 and 8 , so as to provide some turning, albeit not precisely controlled, this can be accomplished as shown, for example, in FIG. 14A . As illustrated, a pin 122 extends through and is retained in the upper flange of frame 120 and fits within an angular recess 114 a formed in the upper surface of rotating plate 114 , limiting the degree of rotation about axis A that is permitted to plate 114 .
As mentioned, in the embodiments of the Wall Racer in which it is capable of operation on a floor and climbing onto a wall (that is, the embodiment of FIGS. 3-7 ), it is desired to provide a switch that actuates the exhaust fan(s) only when the Wall Racer reaches a desired angle, typically between 30 and 60 degrees with respect to the horizontal, so that downforce does not prevent the vehicle from beginning to climb the wall as the wheels engage the wall's surface. FIG. 13 shows a switch 128 for so doing, and which also de-energizes the fan if the Wall Racer is placed upside-down, against a ceiling; this may be preferred for safety reasons, so that the Wall Racer cannot fall on anyone. FIG. 13A shows a typical circuit in which switch 128 may be used.
Switch 128 comprises an electrically conductive metal ball 130 disposed within a hollow nonconductive switch body 132 . Body 132 is symmetrical about a vertical axis, and defines a generally frusto-conical lower portion 132 a , in which ball 130 rests when the vehicle is on the floor, as shown in full, a disc-shaped central portion 132 b , into which the ball falls, as indicated in dotted lines, when the vehicle begins to be oriented vertically, as when it begins to climb a wall, and a generally frusto-conical upper portion 132 c , in which ball 130 falls if the Wall Racer is placed inverted against a ceiling. Conductive contacts 134 are disposed on the inner surfaces of lower portion 132 a and upper portion 132 c , so that when ball 130 is disposed in either the upper or the lower portions, it connects the contacts 134 .
As shown in FIG. 13A , contacts 134 (two of which are connected in common) are wired in series with a normally-open relay 140 and battery 28 , which controls a circuit including battery 28 and fan motor 39 . Thus, with switch 128 closed, that is, with the Wall Racer essentially horizontal, and ball 130 making the connection between contacts 134 , relay 140 is closed, as shown; when the Wall Racer leaves the horizontal sufficiently that ball 130 falls out of lower section 132 a , into upper section 132 b , relay 140 opens, closing the motor circuit and energizing motor 39 , so as to drive fan 38 . In this embodiment, if the Wall Racer is placed inverted against a ceiling, ball 130 falls into upper portion 132 c , similarly connecting contacts 134 , and preventing operation of fan motor 39 .
As mentioned, FIGS. 17-19 show a further embodiment of the invention. The principal improvements provided by this embodiment with respect to those discussed above are the provision of a radial-flow fan rather than the axial-flow fan(s) shown in the previous embodiments, provision of two drive wheels offset longitudinally from one another, principally for reasons of packaging convenience, and elimination of the casters or other wheels in favor of allowing the undersurface of the chassis to touch the wall.
Thus, as shown in FIGS. 17-19 , a fan motor 150 drives a radial-flow fan 152 , that is, comprising a circular end plate 152 b and vanes 152 a that are generally perpendicular to the end plate and angled with respect to the axis of rotation. Air is drawn in along the axis, that is, flowing upwardly around motor 150 , and is exhausted radially outwardly. The radially outward ends of vanes 152 a are curved so as to be closely juxtaposed to a diffuser or fan duct 160 defining a generally bell-shaped interior surface, for efficiency in use. Motor 150 is received in a recess 154 in a transverse member 156 . Member 156 extends transversely across chassis 158 , filling the central portion of a transverse “mail slot” 158 d in chassis 158 .
Generally as discussed above in connection with FIG. 12 , and as shown by FIG. 18 , chassis 158 is radiused at 158 a to define entry portions of the underbody venturi duct, is flat at 158 b to provide the transition portions thereof, and defines a smooth duct at 158 c to define the exit portions thereof. Skirts 159 are again provided to prevent air entry along the long sides of the chassis 158 . On either side of the motor-receiving recess 154 , member 156 is shaped as indicated by dashed lines 156 a , in order to provide a fair flow path for air drawn in at the ends of chassis 158 . The exit portions of the venturi duct as formed by chassis 158 at 158 c mate with diffuser duct 160 , the inside surface of which is generally bell-shaped so as to be closely juxtaposed to vanes 152 a of fan 152 , as noted above. As also shown, assembly is simplified by formation of transversely-extending ears 160 a on diffuser duct 160 . Ears 160 a mate with posts 156 b formed on transverse member 156 , as shown in FIG. 19 ; fasteners passing therethrough also secure gearboxes 162 , which are discussed further below.
Propulsion for the vehicle is provided by two motors 164 , which drive two drive wheels 166 through reduction gearboxes 162 , as mentioned above. As previously, motors 164 are controlled responsive to radio, or preferably, infrared signals transmitted by a remote transmitter (not shown) and received by a receiver 168 . Power for motors 164 as well as for fan motor 150 is provided by a battery 170 . Electrical connection between these components, provision for battery charging, on-off switching, mechanical details such as the construction of gearboxes 162 , selection and operation of receiver 168 , and the control of motors 164 responsive to the received signals are within the skill of the art and need not be detailed here.
As illustrated, drive wheels 166 are offset longitudinally with respect to one another, and no casters are provided. The axes of drive wheels 166 are located with respect to the bottom surface of chassis 158 such that the flat central portion 158 b of the chassis is spaced on the order of 0.020″ from the wall surface W. Consequently, the chassis 158 “teeters”, that is, pivots very slightly about a diagonal axis extending between the points at which drive wheels 166 contact the wall surface W, such that in use the teeter or pivoting is limited by undersurface of the chassis 158 contacting the wall surface W at one or the other diagonal corner. The undersurface of chassis 158 is made smooth to reduce friction between it and the wall surface W as the vehicle is propelled. Slight “bumps” might also be formed at the diagonal corners of the chassis, to localize the contact between the chassis and wall surface W. It is found that the friction experienced in use of the toy of the invention with walls and other surfaces of typical smoothness—e.g., conventionally painted interior walls—is sufficiently small as to present no difficulty, and likewise that the slight asymmetry in the airflow path under the chassis presents no difficulty.
Thus, in use, the fan 152 is energized and the vehicle is placed against a surface W. Air drawn by fan 152 passes inwardly from the ends of the chassis 158 , up through the venturi tunnel collectively formed by the mail slot 158 d in the chassis 158 , transverse member 158 , and diffuser duct 160 , and exits fan 152 in the radially-outward direction. Downforce is thereby created, pulling the vehicle toward the wall surface W. Motors 164 can then be differentially activated to propel the vehicle in any desired direction.
While several preferred embodiments of the invention have been disclosed herein in detail, the invention is not to be limited by the disclosed embodiments, which are exemplary only. | A motorized toy vehicle or Wall Racer that is capable of operating on vertical and inverted horizontal surfaces such as walls and ceilings, while being manufacturable at reasonable cost and operable on batteries having sufficient lifetime as to be enjoyable. One or more battery-powered fans draw air from around all or defined portions of the periphery of the chassis of the Wall Racer through a carefully-shaped duct, so that the air in the portion of the duct immediately adjacent the surface flows at high velocity and low pressure; the relatively greater pressure of the surrounding air urges the vehicle against the surface, allowing it to operate on vertical surfaces, such as walls, or inverted on horizontal surfaces, such as ceilings. | 1 |
CROSS-REFERENCE TO RELATED APPLICATION
[0001] This application claims priority to German Patent Application No. 102008020087.5, filed Apr. 22, 2008, which is incorporated herein by reference in its entirety.
TECHNICAL FIELD
[0002] The present invention relates to a pyrotechnic actuator for an active hood of a motor vehicle.
BACKGROUND
[0003] A pyrotechnic actuator is known from DE 10 2006 008 900 A1, for example. The object of such an actuator is to lift the front hood of a motor vehicle involved in an accident in the shortest time possible by igniting a propellant charge to increase the distance between the hood and underlying parts of the engine block or other non-deformable components of the vehicle, thereby creating as expansive a delay zone as possible for any impacted pedestrian to lower the danger of serious injury.
[0004] In practice, it turns out that the compressed gas supplied by the propellant charge is significantly encumbered with solid particles that get into the cylinder of the actuator upon its activation. As a result, the actuator can only be used a second time, if at all, if the particles are removed from the cylinder. This requires that the actuator go through a costly stay at the workshop each time it is triggered.
[0005] In view of the foregoing, at least one object of the present invention is to provide a pyrotechnic actuator that can be reused with the lowest outlay. In addition, other objects, desirable features, and characteristics will become apparent from the subsequent summary and detailed description, and the appended claims, taken in conjunction with the accompanying drawings and this background.
SUMMARY
[0006] The at least one object, and other objects, desirable features, and characteristics, is achieved in a pyrotechnic actuator for an active hood with a gas generator, a cylinder incorporating a moving piston and a compressed gas line, which links the gas generator with the cylinder, and a filter body is arranged on the compressed gas line to trap particles contained in the compressed gas of the gas generator.
[0007] Surprisingly, it was shown that a good filtering effect can be achieved with a filter body that covers a wall of the compressed gas line.
[0008] It makes sense in particular to align an upstream section of the compressed gas line in such a way as to form a gas jet aimed against the covered wall. Because of their mass inertia, the particles contained in the gas jet penetrate more deeply into the material of the filter body than the gas, so that the gas can no longer entrain them once they come to rest in the filter body.
[0009] In order to achieve this effect, it is not necessary for the gas stream to traverse the filter body; rather a downstream section of the compressed gas line preferably proceeds from a surface of the filter body receiving the stream.
[0010] To efficiently separate out the particles, it is advantageous if the upstream and downstream section of the compressed gas line be aligned at a right angle to each other.
[0011] A filter body that crosses the compressed gas line can also be provided. The design of the actuator is simplified by having the filter body covering the wall and the filter body crossing the compressed gas line in sections of one and the same filter body.
[0012] Such an arrangement can be easily realized by designing the filter body as a hollow item, and having an inner cavity of the filter belong to the downstream section of the compressed gas line.
[0013] In particular, the filter body can be tubular, and a first peripheral section of the tubular filter body covers the wall, and a peripheral section lying opposite the first peripheral section is adapted to cross the upstream line section.
[0014] This filter body can be enveloped by an annular or sectoral cavity, which belongs to the upstream section of the compressed gas line.
[0015] Several upstream line sections each originating with various gas generators advantageously hit various sections of the filter body. Since the cylinder is protected against particles by the preceding filter body, and can hence be used multiple times, the several gas generators for repeated use of the cylinder can already be integrated into the actuator from the start. This minimizes the repair outlay after an accident, since parts of the pyrotechnic actuator need only be replaced or enhanced once all gas generators have been expended. Because the line sections are aligned toward respectively different sections of the filter body, a different section of the filter body is used to filter out the particles each time the actuator is activated, so that the efficiency and permeability of the filter remains essentially unchanged over several activations.
[0016] The actuator can be given an especially compact design by arranging the sections of the filter body crossing the compressed gas lines on a first half of the circumference of the filter body, and the sections covering the wall on a second half.
[0017] Another configuration makes it possible to accommodate the filter body in a blind cavity that faces the upstream section.
[0018] The piston can preferably be locked in the cylinder, and unlocked by the supply of compressed gas.
BRIEF DESCRIPTION OF THE DRAWINGS
[0019] The present invention will hereinafter be described in conjunction with the following drawing figures, wherein like numerals denote like elements, and:
[0020] FIG. 1 is a partial longitudinal view through the socket area of a pyrotechnic actuator according to a first embodiment of the invention;
[0021] FIG. 2 is an axial view through the socket area of an actuator according to a second embodiment of the invention;
[0022] FIG. 3 is a radial section along the III-III plane from FIG. 2 ;
[0023] FIG. 4 is a section analogous to FIG. 3 according to a third embodiment of the invention;
[0024] FIG. 5 is an axial section according to a fourth embodiment of the invention;
[0025] FIG. 6 is a section along the VI-VI plane from FIG. 5 ;
[0026] FIG. 7 is a radial section analogous to FIG. 6 according to a fifth embodiment of the invention;
[0027] FIG. 8 is a partial longitudinal section through the socket area of a pyrotechnic actuator according to a sixth embodiment of the invention;
[0028] FIG. 9 is a section along the IX-IX plane from FIG. 8 ; and
[0029] FIG. 10 is a section along the X-X-plane from FIG. 8 .
DETAILED DESCRIPTION
[0030] The following detailed description is merely exemplary in nature and is not intended to limit application and uses. Furthermore, there is no intention to be bound by any theory presented in the preceding background and summary or the following detailed description.
[0031] FIG. 1 shows a section through an actuator according to an embodiment of the invention along the longitudinal axis of its cylinder 1 only partially depicted on the figure. A sliding piston 2 inside the cylinder 1 is secured to an engine hood of a motor vehicle to be lifted by the actuator (not shown on the figure) by a piston rod 3 exiting at the upper end of the cylinder 1 . The entire actuator is mounted under the engine hood in the body structure of a motor vehicle.
[0032] The piston 2 encompasses a hollow cylindrical piston sheath 4 rigidly connected with the piston rod 3 and open toward the bottom, and a slider 5 with an essentially cylindrical shape, the bottom side of which is enlarged by a continuous collar 6 , so that it fills out the free cross section of the cylinder 1 to the exclusion of a slight clearance. In the configuration shown, a top section 7 of the slider 5 holds a plurality of latching balls 8 securely in a position where some are accommodated in boreholes 28 in the jacket sheath 4 , and others engage a groove 9 on the inside of the cylinder 1 . The latching balls 8 keep the piston 2 locked firmly in place, so that the engine hood on the motor vehicle body remains securely anchored by the actuator.
[0033] A compressed gas line 10 links the bottom side of the slider 5 with a plurality of gas generators 11 . When one of these gas generators 11 is fired, the compressed gas it supplies first streams against the bottom side of the slider 5 , forcing it upwards. As a result, a continuous groove 12 of the slider 5 moves to the level of the latching balls 8 , while the slider 5 simultaneously hits the jacket sheath 4 , and conveys the pressure of the gas to it. This causes the latching balls 8 to slip out of the groove 9 of the cylinder 1 and into the groove 12 of the slider 5 , releasing the lock of the piston 2 . The piston can now yield to the pressure of the gas and lift the hood.
[0034] The compressed gas line 10 encompasses a plurality of boreholes incorporated into the massive metal socket of the cylinder 1 . Three parallel boreholes each form chambers, which incorporate gas generators 11 . They are interconnected by a collective borehole 13 , which is introduced from the bottom side of the socket and tightly sealed by a cover 14 . One of the three boreholes marked 15 that accommodates the gas generators 11 is lengthened up to the longitudinal axis of the cylinder 1 and a bit further beyond that. It crosses a borehole 16 that axially lengthens the chamber of the cylinder 1 . A filter body 17 comprised of a porous material is housed in a sack-like end section of the borehole 15 lying opposite the gas generator 11 on the other side of the borehole 16 .
[0035] When one of the gas generators 11 is fired, the compressed gas ejected by it first shoots along the borehole 15 until deflected in the crossing zone of the boreholes 15 , 16 . Particles entrained by the compressed gas cannot catch up with the directional change of the gas fast enough, are carried through the crossing area, and hit the opposing filter body 17 , where they remain stuck. The compressed gas that finally reaches the chamber of cylinder 1 is essentially free of particles. As a result, the actuator can be activated several times without having to be taken apart and cleaned after each time activated.
[0036] A borehole 44 running through the piston 2 allows the compressed gas to seep out after the piston 2 has been released and lifted. As a result, after keeping the hood lifted for the time necessary for cushioning the pedestrian, the piston 2 can be pressed backs into the position shown on FIG. 1 without exerting a lot of force, and be locked into that position once again.
[0037] FIG. 2 shows an axial section through the socket area of a pyrotechnic actuator according to a second embodiment of the invention. The cylinder of the actuator itself and the piston accommodated therein are not shown; their structural design can be the same as described above with reference to FIG. 1 . The collective borehole 13 is omitted in this embodiment; in its place, each of a total of three gas generators 11 is incorporated in a separate upstream borehole 15 , which runs in a radial direction toward the downstream axial borehole 16 and is lengthened a bit beyond the latter to form a receiving pocket for a filter body 17 . As readily evident in the radial section on FIG. 3 , each gas generator 11 lies opposite a filter body 17 , which is flanked on both sides by the boreholes 15 of other gas generators 11 , and traps particles of the gas generator 11 opposite it.
[0038] In a radial section along the same plane on FIG. 3 , FIG. 4 shows a third embodiment of the actuator. In order to reduce the diameter of the actuator socket, the gas generators 11 are here accommodated in boreholes parallel to the piston axis, and hence visible in a top view on the figure. Upstream boreholes 15 into which the gas generators 11 release their respective compressed gas are oriented radially, perpendicular to the longitudinal axis of the cylinder 1 , and end in a shared axial parallel, downstream borehole 16 via nozzles 18 . The nozzles 18 bundle the ejected compressed gas on the filter body 17 lying respectively diametrically opposite the nozzle 18 . The respective filter body 17 is accommodated in a borehole 29 diametrically opposite the upstream borehole 15 of the allocated gas generator 11 , and both boreholes 15 , 29 are each sealed to the outside by screwed-in stoppers 19 .
[0039] FIG. 5 in turn shows an axial section through the socket area of an actuator according to a fourth embodiment of the invention. The arrangement of gas generators 11 is the same as described in reference to FIG. 1 . The structural design of the cylinder 1 and the piston 2 is also identical to the one shown on FIG. 1 , and hence not shown separately on FIG. 5 .
[0040] A hollow cylindrical or tubular filter body 17 is incorporated in a chamber in the crossing area of a radially oriented upstream borehole 15 and a downstream borehole 16 running on the cylindrical axis. In the present case, the chamber 20 is formed by a borehole with a large diameter, which is advanced from the bottom side of the socket and oriented coaxially to the borehole 16 , just as a collective borehole 13 that joins the gas generators 11 with the borehole 15 . The collective borehole 13 and chamber 20 are here sealed by a shared cover 21 .
[0041] If required by the structure of the material comprising the filter body 17 , the filter body 17 can be stabilized against the pressure of the gas released by one of the gas generators 11 by having the journal 22 of the cover 21 extend a bit inside the cavity of the filter body 17 and/or an upper edge of the filter body 17 extend into a groove on the cover of the chamber 20 .
[0042] As evident from the section on FIG. 6 , the filter body 17 has two areas 23 , 24 that act in respectively different ways on the gas stream of the gas generator 11 . The gas stream passes by the area 23 facing the gas generator 11 , catching a portion of the particles contained therein. Since the area 23 does not have to catch all particles, it can be highly porous, so that the pressure drop at area 23 can be kept low enough not to notably delay the raising motion of the hood, and not to load the filter material beyond its load-bearing limit. The convex bulging of the surface of the filter body 17 facing the gas generator 11 increases its load-bearing capacity further.
[0043] Particles that were not trapped in the traversed area 23 of the filter body 17 pass through the inner cavity of the filter body 17 , and head to the area 24 on the opposite side, where they remain stuck.
[0044] FIG. 7 shows an axial section through a fifth embodiment of the actuator, which combines the features of the second and fourth embodiment. Three radial boreholes 15 respectively fitted with a gas generator 11 empty via nozzles 18 into a cylindrical chamber 20 , which is equipped with a tubular filter body 17 . The filter body 17 has three sections 23 , 24 that alternate in the peripheral direction. The sections 23 lying in front of a respective nozzle 25 carry the compressed gas from one of the gas generators 11 when fired; adjacent sections 24 trap the respective particles of another of the gas generators 11 that have passed the respectively diametrically opposing area 23 without being caught. Since separate areas 23 or 24 are allocated to each gas generator 11 in this embodiment, the gas from each gas generator 11 that is fired hits fresh sections of the filter body 17 not yet encumbered with the particles of other gas generators. For this reason, the efficiency of the filter body 17 remains essentially just as good when activating the third gas generator 11 as it was when generating the first.
[0045] The sections 24 of the filter body do not have to completely abut a wall area of the chamber 20 that they cover. As denoted by a dashed line on FIG. 7 , a well chamber 26 for particles can be recessed diametrically opposite to a respective borehole 15 . However, areas 27 of the wall should contact the filter body 17 between such a well chamber 26 and adjacent nozzles 24 to prevent an area 24 already loaded with particles from being flushed in the opposite direction when another gas generator 11 is activated, entraining particles trapped therein.
[0046] A preferred embodiment of the pyrotechnic actuator according to an embodiment of the invention is described based on the axial section on FIG. 8 and the two cross sections on FIG. 9 and FIG. 10 , which each show sections along the IX-IX or X-X planes on FIG. 8 . Elements of this actuator that were already described with respect to the preceding embodiments are marked with the same reference numbers, and will only be elucidated below to the extent that there are differences relative to the other embodiments.
[0047] The cylinder 1 of this actuator consists of at least two elements joined together, a long stretched-out pipe section 30 and a footing 31 . The footing 31 has a base plate 32 and a pipe fitting 33 projecting from the base plate 32 , into which the pipe section 30 is screwed. The groove 9 forms a border between the pipe section 30 and the footing 31 , so that both parts 30 , 31 can be easily fabricated without back cuts.
[0048] The footing 31 is housed in a pot-shaped casing 34 . The base plate 32 and a floor area of the casing 34 border a cavity 35 , which incorporates a molding 36 and, in a flat chamber 20 of the latter, an annular or tubular filter body 17 . A large opening 37 in the floor plate 33 joins the chamber of the cylinder 1 with the interior cavity of the filter body 17 . Three smaller openings 38 of the base plate 32 are joined with the outside of the filter body 17 by ditches 39 which are recessed in the molding 36 .
[0049] Three sleeves 40 parallel to the axis of the cylinder 1 are embedded in a second molding 41 above the base plate 32 . A ring 42 screwed onto the upper edge of the casing 34 keeps a cover plate 43 pressed against the molding 41 . The respective gas generators 11 are positively secured to openings of the cover plate and in the sleeves 40 .
[0050] The compressed gas ejected by one of the gas generators 11 passes through an opening in the floor of the sleeve 40 accommodating the generator, one of the openings 38 in the floor plate 33 and one of the ditches 39 and on to the filter body 17 . The sections 23 of the filter body 17 carrying gas from the three gas generators 11 extend roughly over half its periphery; the sections 24 where the compressed gas passing through the sections 23 is diverted and the residual particles of the compressed gas are trapped in the process form another half of the periphery of the filter body 17 . As evident, the fact that the gas generators 11 are oriented parallel to the cylindrical axis 1 and placed on the same half of the periphery of the filter 17 enables an especially compact design of the actuator.
[0051] While at least one exemplary embodiment has been presented in the foregoing summary and detailed description, 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 in any way. Rather, the foregoing summary and detailed description will provide those skilled in the art with a convenient road map for implementing an exemplary embodiment, 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 as set forth in the appended claims and their legal equivalents. | A pyrotechnic actuator is provided for an active hood that encompasses an installation site for a gas generator, a cylinder incorporating a moving piston and a compressed gas line that joins the installation site with the cylinder. A filter body for trapping particles from the gas stream of the gas generator is arranged on the compressed gas line. | 5 |
[0001] The work leading to this invention was supported in part by Grant No. RO1 CA 54404 from the National Institutes of Health. The U.S. Government retains certain rights in this invention.
BACKGROUND
[0002] 1. File of the Invention
[0003] This invention is directed to various members of a gene family with transformation modulating activity, and to diagnostic and gene therapy techniques based on the variants.
[0004] 2. Review of Related Art
[0005] Prostatic adenocarcinoma is the most frequent malignancy in adult men with approximately 317,000 new cases diagnosed each year (Parker, et al., CA, 46:8-27, 1996). In spite of the capabilities for early diagnosis and treatment (Potosky, et al., JAMA, 273:548-552, 1995), it represents the second leading cause of cancer death in men following lung cancer.
[0006] To date, the study of alterations in specific genes has not been particularly rewarding in primary prostate cancer. Most alterations in the widely studied oncogenes and tumor suppressor genes occur in only 20-30% of primary prostate carcinomas, except for the myc gene, where overexpression has been observed in as many as 50-60% of such cases (Fleming, et al., Cancer Res., 46:1535-1538, 1986). Up to 40% of primary prostate cancers studied by comparative genomic hybridization display chromosomal aberrations (Visakorpi, et al., Cancer Res., 55:342-347, 1995), although such alterations occur more frequently as tumors recur and become refractory to hormonal therapy. Characterization of candidate proto-oncogenes or tumor suppressor genes at such altered loci may eventually shed light on tumor progression in the prostate.
[0007] pp32 (GenBank HSU73477) is a highly conserved nuclear phosphoprotein. Increased expression of pp32 or closely related species is a frequent feature of clinical cancers. For example, in human prostate cancer, high-level expression of RNA hybridizing with pp32 probes occurs in nearly 90% of clinically significant prostate cancers, in contrast to the substantially lower frequencies of alterations of other oncogenes and tumor suppressors (See U.S. Pat. No. 5,726,018, incorporated herein by reference). Molecular Features and Activities of pp 32.
[0008] pp32 is a nuclear phosphoprotein that is differentiation-regulated during differentiation of adult prostatic epithelium (Walensky, et al., Cancer Res. 53:4720-4726, 1993). The human pp32 cDNA sequence (Gen-Bank U73477) is 1052 bp in length and encodes a protein of 249 amino acids. The protein is composed of two domains: an amino terminal amphipathic α-helical region containing a leucine zipper, and a highly acidic carboxyl terminal region. The murine and human forms of pp32 are highly conserved with over 90% nucleic acid homology and over 95% protein-level homology.
[0009] Human pp32 has been isolated independently by a number of groups. Vaesen et al. (“Purification and characterization of two putative HLA class II associated proteins: PHAPI and PHAPII.” Biol. Chem. Hoppe - Seyler., 375:113-126, 1994) cloned an essentially equivalent molecule, termed PHAPI, from an EBV-transformed human B-lymphoblastoid cell line; PHAPII, cloned by the same strategy, is unrelated to pp32. This study identified PHAPI through its association in solution with human HLA class II protein, noting membrane and cytoplasmic localization as well as nuclear; the gene has putatively been localized to chromosome 15q22.3-q23 by fluorescent in situ hybridization (Fink, et al., “Localization of the gene encoding the putative human HLA class II-associated protein (PHAPI) to chromosome 15q22.3-q23 by fluorescence in situ hybridization.” Genomics, 29:309-310, 1995). More recently, a group studying inhibitors of protein phosphatases identified pp32 as IIPP2a, an inhibitor of protein phosphatase 2a (Li, et al., “Molecular Identification of II PP2A, a novel potent-heat-stable inhibitor protein of protein phosphatase 2A.” Biochemistry 35:6998-7002, 1996); another phosphatase inhibitor, I2PP2a, is unrelated to pp32. Interestingly, another recent report (Ulitzur, et al., “Biochemical characterization of mapmodulin, a protein that binds microtubule-associated proteins.” Journal of Biological Chemistry 272:30577-30582, 1997) identified pp32 as a cytoskeletally-associated cytosolic protein in CHO cells. It is not clear whether this finding stems from a difference in system, or whether pp32 can localize to the cytoplasm under certain circumstances. pp32 has also been identified as LANP, a leucine rich nuclear protein in the central nervous system (Matsuoka, et al., “A nuclear factor containing the leucine-rich repeats expressed in murine cerebellar neurons. Proc Natl Acad Sci USA 91:9670-9674, 1994).
[0010] There are also a number of reports of gene products bearing lesser degrees of homology to pp32. The Vaesen group has identified a series of unpublished sequences, termed PHAPI2a (EMBL Locus HSPHAPI2A) and PHAPI2b (EMBL Locus HSPHAPI2B), also cloned from an EBV-transformed human B-lymphoblastoid cell line. These variant pp32 sequences are distinct from the sequences reported herein, representing the April protein instead. April, cloned from human pancreas, is shorter than PHAPI2a by two N-terminal amino acids (Mencinger, et al., “Expression analysis and chromosomal mapping of a novel human gene, APRIL, encoding an acidic protein rich in leucines.” Biochimica et Biophysica Acta, 1395:176-180, 1998, see EMBL Locus HSAPRIL); PHAPI2b is identical to a subset of APRIL. Silver-stainable protein SSP29 (unpublished GenBank Locus HSU70439) was cloned from HeLa cells and is identical to PHAPI2a.
[0011] The nuclear phosphoprotein pp32 has been linked to proliferation. Malek and associates reported that various neoplastic cell lines showed markedly elevated expression levels and that bacterial polysaccharide induced expression of pp32 epitopes by B lymphocytes upon polyclonal expansion (Malek, et al., J. Biol. Chem., 265:13400-13409, 1990). Walensky and associates reported that levels of pp32 expression, measured by in situ hybridization, increased in direct relation to increasing Gleason grade of human prostatic cancers.
[0012] pp32 cDNA probes hybridize strongly with prostatic adenocarcinoma, whereas the hybridization signal in normal prostate is confined to basal cells. Polyclonal anti-pp32 antibodies react strongly with sections of human prostatic adenocarcinoma. The antibodies and riboprobes used by the investigators in previous studies are consistent with cross-reactivities of the reagents with all reported members of the pp32 nuclear phosphoprotein family, therefore, while previous descriptions focused upon pp32, it cannot be excluded that homologous proteins were detected.
SUMMARY OF THE INVENTION
[0013] In one aspect, this invention provides a DNA molecule containing at least a portion of the sequence consisting of base pairs 4894-4942 of the sequence shown in FIG. 2 or its complement. Alternatively, the DNA molecule may contain at least a portion consisting of base pairs 4879-4927, or base pairs 4858-4927. Alternatively, this invention provides a DNA molecule that contains at least a portion of a nucleotide sequence encoding amino acid residues 146-163 of tumor-derived pp32r1 sequence; preferably the DNA encodes all of that segment. In one mode, the DNA molecule is an expression vector which expresses said amino acid sequence, and the invention also includes a recombinant cell containing the expression vector. In another mode, the DNA molecule has the particular sequence operatively linked to a promoter in antisense orientation. In another alternative, this invention provides a DNA probe which specifically hybridizes on Northern blot with nucleic acid encoding the amino acids from residue 146-163 of the tumor-derived pp32r1 sequence, a preferred probe would have a sequence of at least 8 contiguous nucleotides “unique” to the nucleotide sequence of the pp32r1 variant as described herein. In yet another alternative, the invention provides a pair of nucleic acid primers each of which comprises at least 10 contiguous nucleotides, at least one of the primers binding specifically to the pp32r1 sequence, where if the primers are used in nucleic acid amplification of a suitable source of human nucleic acid, the amplification will produce an amplified nucleic acid encoding at least residues 146-163 of the pp32r1 sequence.
[0014] In still another aspect, this invention provides antibodies that specifically bind the tumor derived pp32, but do not bind to normal pp32. Preferably, these antibodies are monoclonal antibodies. The invention also provides polypeptides containing epitopes that bind these antibodies.
[0015] In yet another aspect, this invention provides diagnostic methods for predicting malignant potential of neuroendocrine, neural, mesenchymal, lymphoid, epithelial or germ cell derived tumors by determining, in a sample of human neuroendocrine, neural, mesenchymal, lymphoid, epithelial or germ cell derived tissue, the level of, or the intracellular sites of expression of, a gene product expressed from a gene sequence which encodes, inter alia, residues 146-163 of tumor derived pp32r1. Where the gene product is mRNA, the mRNA is extracted from the sample and quantitated, optionally by PCR, or the level of mRNA may be determined by in situ hybridization to a section of the tissue sample. Where the gene product is protein, the determination may include reacting the sample with an antibody that specifically binds to tumor derived pp32, but not to normal pp32. Preferably, the tissue sample is carcinoma tissue. e.g., carcinoma or sarcoma of a tissue selected from the group consisting of epithelial, lymphoid, hematopoietic, mesenchymal, central nervous system and peripheral nervous system tissues, including colon carcinoma, prostate carcinoma and non-Hodgkin's lymphoma.
[0016] In still another aspect, this invention provides an androgen-activated transcriptional promoter which may be inserted into recombinant DNA molecules. The minimal promoter is made up of a transcription initiation site and at least one binding site for a steroid hormone receptor protein. Typically the consensus sequence for the steroid hormone receptor protein binding site is positioned within 5000 nucleotide base pairs (bp), more preferably within 3000 bp, or even fewer bp of the transcription initiation site: In a preferred mode, a number of binding sites for steroid hormone receptor proteins are positioned within that distance of the transcription initiation site, the promoter may contain five, ten or even 25 steroid hormone receptor protein binding sites. Preferably, the binding site(s) for steroid hormone receptor protein binding are selected from the consensus sequences listed on Table 1. In a preferred mode of the invention, the androgen-activated transcriptional promoter is operatively linked to an open reading frame comprising at least one exon of a protein coding sequence, operative linking of the open reading frame thereby providing an expression vector in which expression of the open reading frame is regulated by steroids.
[0017] In another aspect, this invention provides a method for screening candidate compounds for pharmacological activity by (1) culturing a cell transfected with the DNA molecule containing the androgen-activated transcriptional promoter which is operatively linked to an open reading frame comprising at least one exon of a protein coding sequence, and (2) determining expression of the open reading frame in the presence and absence of the compound. In a preferred mode the androgen-activated promoter may be all or an operative portion of the sequence in FIG. 2 which is up-stream of the translation initiation site, or alternatively the androgen-activated promoter may be the 2700 bp of the sequence in FIG. 2 which is upstream from the translation initiation site.
[0018] pp32 is a member of a highly conserved family of differentiation-regulated nuclear proteins that is highly expressed in nearly all human prostatic adenocarcinomas of Gleason Grade ≧5. This contrasts with the low percentage of prostate tumors that express molecular alterations in proto-oncogenes or demonstrate tumor suppressor mutation or loss of heterozygosity. By analysis of specimens of human prostatic adenocarcinoma and paired adjacent normal prostate from three individual patients, the inventors have shown that normal prostate continues to express normal pp32, whereas three of three sets of RT-PCR-amplified transcripts from prostatic adenocarcinomas display multiple cancer-associated coding sequence changes. The cancer-associated sequence changes appear to be functionally significant. Normal pp32 exerts antineoplastic effects through suppression of transformation. In contrast, cancer-associated pp32 variants augment, rather than inhibit, transformation.
BRIEF DESCRIPTION OF THE DRAWINGS
[0019] [0019]FIG. 1A shows detection of pp32-related mRNA in benign prostate and prostate cancer tissue sections by in situ hybridization.
[0020] [0020]FIG. 1B shows immunohistochemical stain of prostate cancer sections with anti-pp32 antibodies.
[0021] [0021]FIG. 2 shows the genomic sequence of variant pp32r1 isolated from human placenta.
[0022] [0022]FIG. 3 provides a base-by-base comparison of the sequence of pp32r1 (top) with normal human pp32 (bottom). The numbering system for pp32r1 corresponds to FIG. 1, and the numbering system for normal pp32 is taken from Chen, et al. Nucleotide base differences are underlined in the pp32r1 sequence. Sequences within the normal pp32 sequence missing in pp32r1 are represented by dashes. The open reading frame for pp32r1 is indicated by overlining.
[0023] [0023]FIG. 4 shows the alignment of the pp32r1 amino acid sequence (top) with normal human pp32 (bottom). Residue changes are underlined in the pp32r1 sequence. Amino acids missing in the pp32r1 sequence compared to normal pp32 are represented by dashes.
[0024] [0024]FIG. 5 shows the genomic sequence of variant pp32r2.
[0025] [0025]FIG. 6A shows RT-PCR amplification of pp32 and pp32 variants from human prostate cancer and prostate cancer cell line.
[0026] [0026]FIG. 6B shows cleavase fragment length polymorphism analysis of pp32 detects variant pp32 transcripts in human prostate cancer.
[0027] [0027]FIG. 7 shows the alignment of nucleic acid (A) and amino acid (B) sequences from human prostatic adenocarcinoma and prostatic adenocarcinoma cell lines with pp32.
[0028] [0028]FIG. 8 is a bar graph showing ras+myc induced transformed focus formation. Co-transfection with a pp32 expression vector reduces transformation, while co-transfection with a pp32r1 expression vector stimulates transformation.
[0029] [0029]FIG. 9 is a bar graph showing pp32r1 stimulation of ras+myc induced transformed focus formation. Co-transfection with a pp32 expression vector reduces transformation, while co-transfection with expression vectors for pp32r1 sequences from prostate cancer cell lines stimulate transformation.
[0030] [0030]FIG. 10 is a graph of transformation assay results for cells transfected with variant pp32 species, which are shown to stimulate transformation with variable potency.
DETAILED DESCRIPTION OF THE INVENTION
[0031] The inventors have discovered that phenotypic changes in pp32 are a common feature of human prostate cancer. Previous data show that 87% of prostate cancers of Gleason Score 5 and above express pp32 or closely-related transcripts (U.S. Pat. No. 5,734,022, incorporated herein by reference). This is striking in comparison to the frequency of molecular alterations in other widely studied oncogenes and tumor suppressor genes in primary prostatic adenocarcinoma, which occur in a substantially smaller proportion of cases. For example, myc overexpression (Fleming, et al.) occurs in around 60% of cases, and p53 is abnormal in only around 25% of primary tumors (Isaacs, et al., in “Genetic Alterations in Prostate Cancer.” Cold Spring Harbor Symposia on Quantitative Biology, 59:653-659, 1994).
[0032] Several lines of evidence suggest that pp32 may act as a tumor suppressor. Functionally, pp32 inhibits transformation in vitro by oncogene pairs such as ras with myc, mutant p53, Ela, or jun, or human papilloma virus E6 and E7 (Chen, et al., “Structure of pp32, an acidic nuclear protein which inhibits oncogene-induced formation of transformed foci.” Molecular Biology of the Cell, 7:2045-2056, 1996). pp32 also inhibits growth of transformed cells in soft agar (Chen, et al.). In another system, ras-transfected NIH3T3 cells previously transfected to overexpress normal human pp32 do not form foci in vitro or, preliminarily, do not form tumors in nude mice, unlike control cells. In contrast, knockout of endogenous pp32 in the same system by an antisense pp32 expression construct markedly augments tumorigenesis (Example 12 below).
[0033] In clinical prostate cancer, the situation at first appears counterintuitive. Most human prostate cancers seem to express high levels of pp32 by in situ hybridization (see Example 1 below) and stain intensely with anti-pp32 antibodies. Because pp32 inhibits oncogene-mediated transformation (Chen, et al.), its paradoxical expression in cancer was investigated at the sequence level. The paradoxical question of why prostate cancers seem to express high-levels of an anti-oncogenic protein was addressed by comparing the sequence and function of pp32 species from paired normal prostate and adjacent prostatic carcinoma from three patients as well as from four prostate cancer cell lines. It is demonstrated herein that pp32 is a member of a closely-related gene family, and that alternate expression of these closely-related genes located on different chromosomes modulates oncogenic potential in human prostate cancer. The variant pp32 species expressed in prostate cancer are closely related to pp32.
[0034] The present data indicate that prostate cancers express variant pp32 transcripts, whereas adjacent normal prostate expresses normal pp32. Two instances clearly show that expression of alternate genes on different chromosomes can lead to the phenotypic switch, rather than mutation or alternate splicing. This switch in molecular phenotype is accompanied by a switch in functional pp32 phenotype. Normal pp32 is anti-oncogenic in character, in contrast to the pro-oncogenic variant transcripts that foster oncogene-mediated transformation. The high frequency of this abnormality suggests that expression of variant pp32 species may play an etiologic role in the development of human prostate cancer. In addition, these findings have significant diagnostic and prognostic implications.
[0035] Definitions
[0036] In describing the present invention, the following terminology is used in accordance with the definitions set out below.
[0037] Nucleic Acids
[0038] In discussing the structure of particular double-stranded DNA molecules, sequences may be described herein according to the normal convention of giving only the sequence in the 5′ to 3′ direction along the nontranscribed stand of DNA (i.e., the-strand having a sequence homologous to the mRNA).
[0039] A DNA sequence “corresponds” to an amino acid sequence if translation of the DNA sequence in accordance with the genetic code yields the amino acid sequence (i.e., the DNA sequence “encodes” the amino acid sequence): one DNA sequence “corresponds” to another DNA sequence if the two sequences encode the same amino acid sequence.
[0040] Two DNA sequences are “substantially similar” when at least about 90% (preferably at least about 94%, and most preferably at least about 96%) of the nucleotides match over the defined length of the DNA sequences. Sequences that are substantially similar can be identified by the assay procedures described below or by isolating and sequencing the DNA molecules. See e.g., Maniatis et al., infra, DNA Cloning, vols. 1 and II infra: Nucleic Acid Hybridization, infra.
[0041] A “heterologous” region or domain of a DNA construct is an identifiable segment of DNA within a larger DNA molecule that is not found in association with the larger molecule in nature. Thus, when the heterologous region encodes a mammalian gene, the gene will usually be flanked by DNA that does not flank the mammalian genomic DNA in the genome of the source organism. Another example of a heterologous region is a construct where the coding sequence itself is not found in nature (e.g., a cDNA where the genomic coding sequence contains introns, or synthetic sequences having codons different than the native gene). Allelic variations or naturally-occurring mutational events do not give rise to a heterologous region of DNA as defined herein.
[0042] A “coding sequence” or “open reading frame” is an in-frame sequence of codons that (in view of the genetic code) correspond to or encode a protein or peptide sequence. Two coding sequences correspond to each other if the sequences or their complementary sequences encode the same amino acid sequences. A coding sequence in association with appropriate regulatory sequences may be transcribed and translated into a polypeptide in vivo. A polydenylation signal and transcription termination sequence will usually be located 3′ to the coding sequence. A “promoter sequence” is a DNA regulatory region capable of binding RNA polymerase in a cell and initiating transcription of a downstream (3′ direction) coding sequence. Promoter sequences typically contain additional sites for binding of regulatory molecules (e.g., transcription factors) which affect the transcription of the coding sequence. A coding sequence is “under the control” of the promoter sequence or “operatively linked” to the promoter when RNA polymerase binds the promoter sequence in a cell and transcribes the coding sequence into mRNA, which is then in turn translated into the protein encoded by the coding sequence.
[0043] Vectors are used to introduce a foreign substance, such as DNA, RNA or protein, into an organism. Typical vectors include recombinant viruses (for DNA) and liposomes (for protein). A “DNA vector” is a replicon, such as plasmid, phase or cosmid, to which another DNA segment may be attached so as to bring about the replication of the attached segment. An “expression vector” is a DNA vector which contains regulatory sequences which will direct protein synthesis by an appropriate host cell. This usually means a promoter to bind RNA polymerase and initiate transcription of mRNA, as well as ribosome binding sites and initiation signals to direct translation of the mRNA into a polypeptide. Incorporation of a DNA sequence into an expression vector at the proper site and in correct reading frame, followed by transformation of an appropriate host cell by the vector, enables the production of a protein encoded by said DNA sequence.
[0044] An expression vector may alternatively contain an antisense sequence, where a small DNA fragment, corresponding to all or part of an mRNA sequence, is inserted in opposite orientation into the vector after a promoter. As a result, the inserted DNA will be transcribed to produce an RNA which is complementary to and capable of binding or hybridizing with the mRNA. Upon binding to the mRNA, translation of the mRNA is prevented, and consequently the protein coded for by the mRNA is not produced. Production and use of antisense expression vectors is described in more detail in U.S. Pat. No. 5,107,065 (describing and exemplifying antisense regulation of genes in plants) and U.S. Pat. No. 5,190,931 (describing antisense regulation of genes in both prokaryotes and eukarvotes and exemplifying prokaryotes), both of which are incorporated herein by reference.
[0045] “Amplification” of nucleic acid sequences is the in vitro production of multiple copies of a particular nucleic acid sequence. The amplified sequence is usually in the form of DNA. A variety of techniques for carrying out such amplification are described in a review article by Van Brunt (1990, Bio/Technol., 8(4):291-294). Polymerase chain reaction or PCR is a prototype of nucleic acid amplification and use of PCR herein should be considered exemplary of other suitable amplification techniques.
[0046] Polypeptides
[0047] For the purposes of defining the present invention, two proteins are homologous if 80% of the amino acids in their respective amino acid sequences are the same; for proteins of differing length, the sequences will be at least 80% identical over the sequence which is in common (i.e., the length of the shorter protein).
[0048] Two amino acid sequences are “substantially similar” when at least about 87% of the amino acids match over the defined length of the amino acid sequences, preferably a match of at least about 89%, more preferably a match of at least about 95%. Typically, two amino acid sequences which are similar will differ by only conservative substitutions.
[0049] “Conservative amino acid substitutions” are the substitution of one amino acid residue in a sequence by another residue of similar properties, such that the secondary and tertiary structure of the resultant peptides are substantially the same. Conservative amino acid substitutions occur when an amino acid has substantially the same charge or hydrophobicity as the amino acid for which it is substituted and the substitution has no significant effect on the local conformation of the protein. Amino acid pairs which may be conservatively substituted for one another are well-known to those of ordinary skill in the art.
[0050] The polypeptides of this invention encompass pp32r1 and pp32r1 analogs, pp32r2 and pp32r2 analogs, along with other variants of pp32 and their analogs. pp32r1 and pp32r2 are naturally occurring, mature proteins, and further encompass all precursors and allelic variations of pp32r1 and pp32r2, as well as including forms of heterogeneous molecular weight that may result from inconsistent processing in vivo. An example of the pp32r1 sequence is shown in FIG. 3, top line. “pp32r1 analogs” are a class of peptides which includes:
[0051] 1) “Allelic variations of pp32r1,” which are polypeptides which are substantially similar to pp32r1. Preferably the amino acid sequence of the allelic variation is encoded by a nucleic acid sequence that differs from the sequence of pp32r1 by one nucleotide in 300;
[0052] [0052] 2 ) “Truncated pp32r1 peptides,” which include fragments of either pp32 or allelic variations of pp32r1 that preferably retain either (i) an amino acid sequence unique to pp32r1, (ii) an epitope unique to pp32r1 or (iii) pp32r1 activity;
[0053] 3) “pp32r1 fusion proteins,” which include heterologous polypeptides which are made up of one of the above polypeptides (pp32r1, allelic variations of pp32r1 or truncated pp32r1 peptides) fused to any heterologous amino acid sequence.
[0054] “Unique” sequences of the pp32r1 variant according to this invention, either amino acid sequences or nucleic acid sequences which encode them, are sequences which are identical to a sequence of a pp32r1 polypeptide, but which differ in at least one amino acid or nucleotide residue from the sequences of human pp32 (Genbank Locus HSU73477), murine pp32 (Genbank Locus MMU73478), human cerebellar leucine rich acidic nuclear protein (LANP) (Genbank Locus AF025684), murine LANP (Genbank Locus AF022957). IIPP2a or human potent heat-stable protein phospatase 2a inhibitor (Genbank Locus HSU60823), SSP29 (Genbank Locus HSU70439), HLA-DR associated protein 1 (Genbank Locus HSPPHAPI, Accession No. X75090), PHAPI2a (EMBL Locus HSPHAPI2A, Genbank Accession No. Y07569), PHAPI2b (EMBL Locus HSPHAPI2B, Genbank Accession No. Y07570), and April (EMBL Locus HSAPRIL), and preferably, are not found elsewhere in the human genome. (A list of these sequences is provided in Table 3A.) Similarly, an epitope is “unique” to pp32r1 polypeptides if it is found on pp32r1 polypeptides but not found on any members of the set of proteins listed above. Analogs of pp32r2 and unique pp32r2 sequences are defined similarly. Of course, unique sequences of pp32r1 are not found in pp32r2 and vice versa.
[0055] “Variants of pp32” are homologous proteins which differ from pp32 by at least 2 amino acids. In particular, sequence comparison between pp32 and a variant will demonstrate at least one segment of 10 amino acids in which the sequence differs by at least two (2) amino acids. More typically a variant will exhibit at least two such 10 amino acid segments. Preferably, variants of pp32 in accordance with this invention will exhibit differences in functional activity from pp32. In particular, pp32r1 and pp32r2 are variants of pp32 whose activity includes stimulation of transformation in the rat fibroblast transformation assay described herein.
[0056] A composition comprising a selected component A is “substantially free” of another component B when component A makes up at least about 75% by weight of the combined weight of components A and B. Preferably, selected component A comprises at least about 90% by weight of the combined weight, most preferably at least about 99% by weight of the combined weight. In the case of a composition comprising a selected biologically active protein, which is substantially free of contaminating proteins, it is sometimes preferred that the composition having the activity of the protein of interest contain species with only a single molecular weight (i.e.. a “homogeneous” composition).
[0057] As used herein, a “biological sample” refers to a sample of tissue or fluid isolated from a individual, including but not limited to, for example, plasma, serum, spinal fluid, lymph fluid, the external sections of the skin, respiratory, intestinal, and genitourinary tracts, tears, saliva, milk, blood cells, tumors, organs, and also samples of in vivo cell culture constituents (including but not limited to conditioned medium resulting from the growth of cells in cell culture medium, putatively virally infected cells, recombinant cells, and cell components).
[0058] “Human tissue” is an aggregate of human cells which may constitute a solid mass. This term also encompasses a suspension of human cells, such as blood cells, or a human cell line.
[0059] The term “immunoglobulin molecule” encompasses whole antibodies made up of four immunoglobulin peptide chains, two heavy chains and two light chains, as well as immunoglobulin fragments. “Immunoglobulin fragments” are protein molecules related to antibodies, which are known to retain the epitopic binding specificity of the original antibody such as Fab, F(ab)′ 2 , Fv, etc. Two polypeptides are “immunologically cross-reactive” when both polypeptides react with the same polyclonal antiserum.
[0060] General Methods
[0061] The practice of the present invention employs, unless otherwise indicated, conventional molecular biology, microbiology, and recombinant DNA techniques within the skill of the art. Such techniques are well known to the skilled worker and are explained fully in the literature. See, e.g., Maniatis, Fritsch & Sambrook, “Molecular Cloning: A Laboratory Manual” (1982); “DNA Cloning: A Practical Approach,” Volumes I and II (D. N. Glover, ed., 1985); “Oligonucleotide Synthesis” (M. J. Gait. ed., 1984); “Nucleic Acid Hybridization” (B. D. Hames & S. J. Higgins, eds., 1985): “Transcription and Translation” (B. D. Hames & S. J. Higgins, eds., 1984): “Animal Cell Culture” (R. I. Freshney, ed., 1986); “Immobilized Cells and Enzymes” (IRL Press, 1986); B. Perbal, “A Practical Guide to Molecular Cloning” (1984), and Sambrook, et al., “Molecular Cloning: a Laboratory Manual” (1989).
[0062] pp32 Related Genomic DNA
[0063] Screening a human genomic library in bacteriophages with probes generated from human pp32 cDNA yielded a new sequence that contained an open reading frame encoding a protein homologous with pp32 (see Example 2; pp32 sequence, reported in Chen, et al., Mol. Biol. Cell, 7:2045-2056, 1996). While the pp32r1 and pp32r2 sequences (see FIGS. 2 and 5) are substantially homologous to pp32, multiple single nucleotide base changes and short deletions suggest that they are encoded by gene distinct from pp32 gene. The pp32 family also includes substantially homologous polypeptides reported by others: HLA-DR associated protein 1 (Vaesen, 1994), leucine-rich acidic nuclear protein (Matsuoka, 1994), and protein phosphatase 2A inhibitor (Li, 1996).
[0064] DNA segments or oligonucleotides having specific sequences can be synthesized chemically or isolated by one of several approaches. The basic strategies for identifying, amplifying and isolating desired DNA sequences as well as assembling them into larger DNA molecules containing the desired sequence domains in the desired order, are well known to those of ordinary skill in the art. See. e.g., Sambrook, et al., (1989); B. Perbal, (1984). Preferably, DNA segments corresponding to all or a part of the cDNA or genomic sequence of pp32r1 may be isolated individually using the polymerase chain reaction (M. A. Innis, et al., “PCR Protocols: A Guide To Methods and Applications.” Academic Press, 1990). A complete sequence may be assembled from overlapping oligonucleotides prepared by standard methods and assembled into a complete coding sequence. See, e.g., Edge (1981) Nature 292:756: Nambair, et al. (1984) Science 223:1299: Jay, et al. (1984) J. Biol. Chem., 259:6311.
[0065] The assembled sequence can be cloned into any suitable vector or replicon and maintained there in a composition which is substantially free of vectors that do not contain the assembled sequence. This provides a reservoir of the assembled sequence, and segments or the entire sequence can be extracted from the reservoir by excising from DNA in the reservoir material with restriction enzymes or by PCR amplification. Numerous cloning vectors are known to those of skill in the art, and the selection of an appropriate cloning vector is a matter of choice (see, e.g., Sambrook, et al., incorporated herein by reference). The construction of vectors containing desired DNA segments linked by appropriate DNA sequences is accomplished by techniques similar to those used to construct the segments. These vectors may be constructed to contain additional DNA segments, such as bacterial origins of replication to make shuttle vectors (for shuttling between prokaryotic hosts and mammalian hosts), etc.
[0066] Procedures for construction and expression of proteins of defined sequence are well known in the art. A DNA sequence encoding pp32r1, pp32r2, or an analog of either pp31R1 or pp32r2, can be synthesized chemically or prepared from the wild-type sequence by one of several approaches, including primer extension, linker insertion and PCR (see, e.g., Sambrook, et al.). Mutants can be prepared by these techniques having additions, deletions and substitutions in the wild-type sequence. It is preferable to test the mutants to confirm that they are the desired sequence by sequence analysis and/or the assays described below. Mutant protein for testing may be prepared by placing the coding sequence for the polypeptide in a vector under the control of a promoter, so that the DNA sequence is transcribed into RNA and translated into protein in a host cell transformed by this (expression) vector. The mutant protein may be produced by growing host cells transfected by an expression vector containing the coding sequence for the mutant under conditions whereby the polypeptide is expressed. The selection of the appropriate growth conditions is within the skill of the art.
[0067] The assembled sequence can be cloned into any suitable vector or replicon and maintained there in a composition which is substantially free of vectors that do not contain the assembled sequence. This provides a reservoir of the assembled sequence, and segments or the entire sequence can be extracted from the reservoir by excising from DNA in the reservoir material with restriction enzymes or by PCR amplification. Numerous cloning vectors are known to those of skill in the art, and the selection of an appropriate cloning vector is a matter of choice (see, e.g., Sambrook, et al., incorporated herein by reference). The construction of vectors containing desired DNA segments linked by appropriate DNA sequences is accomplished by techniques similar to those used to construct the segments. These vectors may be constructed to contain additional DNA segments, such as bacterial origins of replication to make shuttle vectors (for shuttling between prokaryotic hosts and mammalian hosts), etc.
[0068] Producing the Recombinant Peptide
[0069] Preferably, DNA from the selected clones should be subcloned into an expression vector, and the protein expressed by cells transformed with the vector should be tested for immunoreactivity with antibodies against the recombinant protein of this invention prepared as described below. Such subcloning is easily within the skill of the ordinary worker in the art in view of the present disclosure. The amino acid coding region of the DNA sequence of this invention may be longer or shorter than the coding region of the disclosed sequence, so long as the recombinant peptide expressed by the DNA sequence retains at least one epitope cross-reactive with antibodies which are specifically immunoreactive with pp32r1, pp32r2; or other pp32 variant as desired. The preparation of selected clones which contain DNA sequences corresponding to all or part of the sequence of pp32r1 or pp32r2 may be accomplished by those of ordinary skill in the art using conventional molecular biology techniques along with the information provided in this specification.
[0070] It is possible to purify a pp32 variant protein such as pp32r1, which is cross-reactive with antibodies specific for pp32, from an appropriate tissue/fluid source; however, a cross-reactive pp32 variant, or analog thereof, may also be produced by recombinant methods from a DNA sequence encoding such a protein or polypeptide. Polypeptides corresponding to the recombinant protein of this invention may be obtained by transforming cells with an expression vector containing DNA from a clone selected from an mammalian (preferably human) library as described herein. Suitable expression vector and host cell systems are well known to those of ordinary skill in the art, and are taught, for instance, in Sambrook, et al., 1989. The peptide may be obtained by growing the transformed cells in culture under conditions wherein the cloned DNA is expressed. Of course, the peptide expressed by the clone may be longer or shorter than pp32r1 or pp32r2, so long as the peptides are immunologically cross-reactive. Depending on the expression vector chosen, the peptide may be expressed as a fusion protein or a mature protein which is secreted or retained intracellularly, or as an inclusion protein. The desired polypeptides can be recovered from the culture by well-known procedures, such as centrifugation, filtration, extraction, and the like, with or without cell rupture, depending on how the peptide was expressed. The crude aqueous solution or suspension may be enriched for the desired peptide by protein purification techniques well known to those skilled in the art. Preparation of the polypeptides may include biosynthesis of a protein including extraneous sequence which may be removed by post-culture processing.
[0071] Using the nucleotide sequences disclosed herein and the polypeptides expressed from them, antibodies can be obtained which have high binding affinity for pp32r1 or pp32r2, but much lower affinity for pp32 and/or other variants of pp32. Such antibodies, whether monoclonal or purified polyclonal antibodies can be used to specifically detect pp32r1 or pp32r2. Techniques for preparing polypeptides, antibodies and nucleic acid probes for use in diagnostic assays, as well as diagnostic procedures suitable for detection of pp32 are described in U.S. Pat. Nos. 5,726,018 and 5,734,022, incorporated herein by reference, and these techniques may be applied to pp32r1 or pp32r2 by substitution of the nucleic acid sequences disclosed herein. Similar substitution may be applied to other variants of pp32.
[0072] pp32r1 Promoter Sequence
[0073] Multiple consensus sequences for binding active steroid receptors found in genomic sequences upstream from the pp32r1 coding region are consistent with hormone regulation of gene expression. The consensus sequences were associated with the both induction and repression of expression by steroid hormones. The combination of both positively and negatively acting elements suggests complex regulation of pp32r1 expression.
[0074] Possible steroid hormone regulation of pp32r1 expression is important in regard to prostate cancer. While about one-half of treated patients initially respond to androgen ablation, subsequent hormone refraction and continued aggressive tumor growth is common (Garnick, M. B., “Prostate Cancer,” in Scientific American Medicine , Dale, D. C. and Federman, D. D. Eds., Scientific American Inc., New York. 1995). Many different steroid hormones regulate the growth of prostate cancer cells (Huggins, et al., “Studies on prostate cancer: I. The effect of castration, of estrogen, and of androgen injection on serum phosphatases in metastatic carcinoma of the prostate,” Cancer Res., 1:293, 1941). These findings established a basis for androgen ablation therapy for the treatment of metastatic prostate cancer.
[0075] The present invention provides androgen-activated promoters based on the upstream portion of the genomic sequence in FIG. 2. The promoter sequence provided by this invention is bounded at its 3′ terminus by the translation start codon of a coding sequence and extends upstream (5′ direction) to include at least the number of bases or elements necessary to initiate transcription at levels above background. Within the promoter sequence will be found a transcription initiation site (conveniently defined by mapping with nuclease S1), a protein binding domain (consensus sequence) within about 100 bases upstream of the transcription initiation site generally designated the TATA box (a binding site for TATA box binding proteins and RNA polymerase), and various other protein binding domains (consensus sequences) upstream of the TATA box that modulate the basic transcriptional activity of the transcription initiation site and the TATA box. The various other protein binding domains preferably contain recognition sequences shown in Table 1 for binding (1) androgen receptors, estrogen receptors, glucocorticoid receptors, and progesterone receptors; (2) transcription factors containing the leucine zipper motif including, but not limited to Fos, Jun, JunB, and Myc; and, (3) certain tissue specific transcription factors including, but not limited to GATA-1 and GATA-2. The various other protein binding domains upstream of the TATA box may contribute to specificity (tissue specific expression), accuracy (proper initiation), and strength (transcription frequency) of the promoter. The promoter elements may serve overlapping functions so that the promoter may function in the absence of subsets of these elements.
[0076] Therapy
[0077] Inhibition of function of protransforming variants of pp32 by any means would be expected to be an avenue of therapy.
[0078] U.S. Pat. No. 5,726,018, incorporated herein by reference, describes various therapeutic avenues which may be applied by the skilled worker based on the nucleotides and protein sequences disclosed herein. In a particular embodiment, all or a portion of the sequence of pp32r1 or pp32r2 may be supplied in the antisense orientation to block expression of the variants found in carcinomas particularly prostate cancer. Suitable methods for preparation of antisense expression vectors and administration of antisense therapy may be found in U.S. Pat. No. 5,756,676, incorporated herein by reference. Prescreening of the patient population using the diagnostic methods described herein to identify patients having tumors expressing the particular pp32 variant is preferred.
[0079] Screening for compounds having therapeutic effects in prostate cancer may also be facilitated by the present invention. Studies which may be used to screen candidate compounds are described in U.S. Pat. No. 5,756,676, incorporated herein by reference, modified by the use of cell lines which express particular variants of pp32 (see, e.g., Examples below). Compounds which affect steroid dependent protein expression may also be detected according to this invention by similar screening studies using an androgen-activated promoter as provided herein operatively coupled to a DNA sequence whose expression may be detected. (Marker sequences are well known in the art, see, e.g., Sambrook, et al., and selection of an appropriate detectable expression marker is a routine matter for the skilled worker.) Screening by testing the effect of candidate compounds on recombinant cells containing an expression vector having an androgen-activated promoter operatively coupled to an expression marker, with appropriate controls, is within the skill of the art, in view of the promoter sequences provided herein. In one aspect, this invention provides a method for screening candidate compounds for pharmacological activity by (1) culturing a cell transfected with the DNA molecule containing an androgen-activated transcriptional promoter which is operatively linked to an open reading frame comprising at least one exon of a protein coding sequence, and (2) determining expression of the open reading frame in the presence and absence of the compound. In a preferred mode the androgen activated promoter may be the portion of the sequence in FIG. 2 which is up-stream of the translation initiation site, or alternatively the androgen activated promoter may be the 2700 bp upstream from the translation initiation site.
[0080] Diagnostic Methods Based on the pp32 Gene Family
[0081] In one aspect, this invention provides methods for detecting and distinguishing among members of the pp32 gene family. As explained herein, the presence of one or more members of the gene family may be detected using assays based on common structures among the members resulting from common or similar sequences. For example, polyclonal antibodies elicited by pp32 will cross-react with pp32r1 and pp32r2, including various alleles of these pp32 variants. Similarly, the full coding region of the pp32 cDNA will hybridize under suitable conditions with nucleic acid encoding any of the variants, as shown by the in situ detection of the variants in tumor sections which were subsequently shown to contain either pp32r1 or pp32r2 allelic forms (Example 1). Selection of conditions that promote the immune cross-reactivity or cross-hybridization necessary for such detection is within the skill of the art, in view of the examples provided herein. For example, by using large nucleotide probes in hybridization experiments, the effects of one or a few differences in sequence may be overcome, i.e., larger probes will bind to more dissimilar target sequences, in contrast to shorter probes for which each nucleotide makes a larger percentage contribution to the affinity, and a single nucleotide alteration will cause a greater relative reduction in hybridization efficiency. Typically probes of 50 or more nucleotides are used to find homologues to a given sequence, and the studies reported in Example 1 used the entire sequence of pp32 as a probe to find cells expressing homologous members of the gene family other than pp32. Likewise, polyclonal antisera elicited to an antigen having multiple epitopes is more likely to cross-react with a second antigen that has a few of the same epitopes along with many different epitopes, while a monoclonal antibody or even a purified polyclonal antiserum might not bind to the second antigen.
[0082] In addition to determining the presence of one or more members of the pp32 gene family, this invention also provides methods for distinguishing among members. Determining which pp32 variant may be useful, for instance, to determine whether a transfomation promoting or suppressing variant is present in a tissue sample. Suitable methods for distinguishing include both immunoassay and nucleic acid binding assays. Preferred are methods which can detect a 10-fold difference in the affinity of the detecting ligand (e.g., antibody or oligonucleotide) for the target analyte. Such methods are well documented for other systems, and may be adopted to distnguish between pp32 variants by routine modification of such methods in view of the guidance provided herein.
[0083] Protein level assays may rely on monoclonal or purified polyclonal antibodies of relatively greater affinity for one variant compared to another (see, e.g., Smith, et al. (“Kinetics in interactions between antibodies and haptens,” Biochemistry, 14(7):1496-1502, 1975, which shows that the major kinetic variable governing antibody-hapten interactions is the rate of dissociation of the complex, and that the strength of antibody-hapten association is determined principally by the activation energy for dissociation), and Pontarotti, et al.(“Monoclonal antibodies to antitumor Vinca alkaloids: thermodynamics and kinetics,” Molecular Immunology, 22(3):277-84, 1985, which describes a set of monoclonal antibodies that bind various dimeric alkaloids and can distinguish among the alkaloid haptens due to different relative affinities of the various monoclonal antibodies for particular dimeric alkaloids), each of which is incorporated herein by reference). Suitable modifications of the conditions for immunoassays to emphasize the relative affinity of monoclonal antibodies with different affinity are also discussed in U.S. Pat. No. 5,759,791, incorporated herein by reference.
[0084] A number of methods are available which are capable of distinguishing between nucleic acid sequences which differ in sequence by as little as one nucleotide. For example, the ligase chain reaction has been used to detect point mutations in various genes (see. e.g., Abravaya, et al., “Detection of point mutations with a modified ligase chain reaction (Gap-LCR).” Nucleic Acids Research, 23(4):675-82, 1995, or Pfeffer, et al., “A lipase chain reaction targeting two adjacent nucleotides allows the differentiation of cowpox virus from other Orthopoxvirus species,” Journal of Virological Methods, 49(3):353-60, 1994, each of which is incorporated herein by reference). Amplification of a sequence by PCR also may be used to distinguish sequences by selection of suitable primers, for example, short primers, preferably 10-15 matching nucleotides, where at least one of the primers has on the 3′ end a unique base that matches one variant but not other variants, and using annealing conditions under which the primer having the unique base has at least a ten-fold difference in dissociation rate between the fully matching variants and variants which do not fully match. Similar differentiation may be achieved in other methods dependent on hybridization by using short probes (typically under 50 bp, preferably 25 bp or less more preferably less than 20 bp or even 10-12 bp) by adjusting conditions in hybridization reactions to achieve at least a ten-fold difference in dissociation rate for the probes between the fully matching variants and variants which do not fully match. Cleavase fragment length polymorphism may also be used, and a specific example below provides guidance from which the skilled worker will be able to design similar studies by routine selection of other cleavase enzymes in view of the sequences provided herein.
[0085] The diagnostic methods of this invention may be used for prognostic purposes and patient differentiation as described herein. In particular, the methods of this invention allow differentiation between products expressed from the various sequences disclosed in FIG. 7. Preferred methods are those that detect and/or differentiate, between pp32, pp32r1, and/or pp32r2. Situations in which differentiation between pp32 variants will be of benefit will be readily apparent to the skilled clinician, in view of the present disclosure. Selection among the diagnostic methods provided by this invention of a suitable technique to achieve the desired benefit is a routine matter for the skilled clinician.
EXAMPLES
[0086] In order to facilitate a more complete understanding of the invention, a number of Examples are provided below. However, the scope of the invention is not limited to specific embodiments disclosed in these Examples, which are for purposes of illustration only.
Example 1
[0087] Cellular Location of pp32 Expression
[0088] pp32 mRNA can be detected by in situ hybridization with a pp32 probe under stringent conditions.
[0089] In situ hybridization. Bases 1-298 of the pp32 cDNA sequence (GenBank HSU73477) were subcloned into the Bluescript vector by standard techniques. Digoxigenin labeled anti-sense and sense RNA probes were generated using a commercially available kit (Boehringer Mannheim). Vector DNA linearized with BamHI and Xhol served as template for antisense and sense probe generation respectively. In vitro transcription was performed for 2 hours at 37° in a final volume of 20 μl which contained 1 μg of template DNA, 2 U/μl of either T3 or T7 RNA polymerase. 1 U/μl ribonuclease inhibitor, 1 mM each of ATP, CTP, GTP, 0.65 mM UTP, 0.35 mM digoxigenin-11-UTP, 40 mM Tris-HCl pH 8.0, 10 mM NaCl, 10 mM DTT, 6 mM MgCl 2 and 2 mM spermidine. The reaction was stopped by adding 2 μl of 0.2M EDTA, pH 8. 0 and the synthesized transcripts were precipitated for 30 min at −70° with 2.2 μl of 4 M LiCl and 75 μl of pre-chilled ethanol. RNA was pelleted by centrifugation, washed with 80% ethanol, mildly dried and dissolved in 100 μl of DEPC treated water. Yields of labeled probe were determined by an enzyme linked irrimunoassay using a commercially available kit (Boehringer Mannheim). Non-radioactive in situ hybridization was performed with anti-sense and sense pp32 RNA probes generated by in vitro transcription (see U.S. Pat. No. 5,726,018, incorporated herein by reference). FIG. 1A shows that normal prostatic basal cells are positive, whereas the clear, differentiated glandular cells are negative. In contrast, prostatic adenocarcinoma, shown at left, is strikingly positive. Note that the signal is cytoplasmic since it is mRNA and not the protein that is detected in this assay.
[0090] pp32 displays a distinctive pattern of expression in vivo (Chen, et al.; Malek. et al., “Identification and preliminary characterization of two related proliferation-associated nuclear phosphoproteins.” Journal of Biological Chemistry, 265:13400-13409, 1990; Walensky, et al., “A novel M(r) 32,000 nuclear phosphoprotein is selectively expressed in cells competent for self-renewal.” Cancer Research 53:4720-4716, 1993). In normal peripheral tissues, expression is restricted to stem-like cell populations such as crypt epithelial cells in the gut and basal epithelium in the skin: in the adult central nervous system, cerebral cortical neurons and Purkinje cells also express pp32. In normal prostate, basal cells express pp32, whereas pp32 mRNA is not detectable by in situ hybridization in differentiated glandular cells (FIG. 1A). In contrast, strong in situ hybridization to pp32 probes is found in nearly all clinically significant human prostatic adenocarcinomas. 87% of human prostatic adenocarcinomas of Gleason Score 5 and above express mRNA that hybridizes strongly with probes to pp32 in contrast to only 11% of prostate cancers of Gleason Score 4 and below in a study of 55 patients.
[0091] Immunohistochemistry. Formalin-fixed, paraffin-embedded tissue was sectioned at 4 μM, deparaffinized, hydrated, processed for heat-induced antigen retrieval at 95° in 0.01 M citrate buffer, pH 6.0, for 20 min (Cattoretti, et al., “Antigen unmasking on formalin-fixed, paraffin-embedded tissue sections,” Journal of Pathology 171:83-98, 1993), then incubated overnight at room temperature with a {fraction (1/20)} dilution of anti-pp32 antibody. Following washing, the slide was sequentially developed with biotinylated swine-anti-rabbit IgG at {fraction (1/100)} (Dako), strepavidin peroxidase (Dako), and diaminobenzidine. FIG. 1B shows a representative high-grade human prostate cancer stained with affinity-purified rabbit polyclonal anti-pp32 antibody (Gusev, et al., “pp32 overexpression induces nuclear pleomorphism in rat prostatic carcinoma cells.” Cell Proliferation 29:643-653, 1996). The left-hand panel shows a representative field at 250x: the rectangle indicates the area shown in computer venerated detail in the right-hand panel. Strongly hybridizing tumors show intense immunopositivity with antibodies to pp32, indicating that they express pp32 or immunologically related proteins (FIGS. 1A and 1B).
Example 2
[0092] ESTs Corresponding to pp32
[0093] Several potential variant pp32 species have been identified in the prostate cancer expressed sequence tag libraries of the NCI's Cancer Genome Anatomy Project. Clone 588488 encodes a protein that is 96% identical to APRIL, although absent retrieval and sequencing of the full clone, it is impossible to tell whether the entire EST clone encodes a pp32 related sequence; neither is it possible to assess the biologic function of this molecule at this time. Nevertheless, it is apparent that the sequenced portion encodes a protein bearing great similarity to pp32. This EST does not appear in the database for normal prostate. As with the variant pp32 species recovered from prostate cancer, generation of this molecule by mutation would require a complex mechanism.
[0094] pp32-related genes are present in other organisms. The existence of a pp32 gene family in rodent would be consistent with the existence of a comparably sized family in human. A murine pp32 (GenBank U73478) has 89% amino acid identity to pp32, but less identity to pp32r1 and APRIL. (The murine cerebellar leucine rich acidic nuclear protein has a single amino acid substitution relative to murine pp32.) We additionally identified a murine EST, GenBank AA066733, with closest identity to APRIL protein at 85% identity over 148 amino acids of a predicted open reading frame. Several other murine EST's. AA212094 and W82526, are closely related to the pp32 family but are not significantly more related to either pp32, pp32r1, or APRIL. A human homologue of such a gene would be expected to encode a fourth member of this gene family. We identified EST's predicted to encode pp32-related proteins in C. elegans , schistosomes, zebrafish, and Drosophila (data not shown). However, these sequences may not represent the complete extent of the pp32 gene family in these organisms, and thus are not informative for the likely size of the mammalian pp32 gene family.
Example 3
[0095] The Structure of a Gene Encoding a Relative of the pp32 Family
[0096] Screening a human genomic library in bacteriophages with probes generated from human pp32 cDNA yielded a new sequence that contained an open reading frame encoding a protein homologous with pp32.
[0097] Screening a Human Genomic Library in Bacteriophages for pp32 cDNA.
[0098] A genomic library from human placenta in the Lambda Fix II vector was expressed in E. coli strain XL-1 Blue MRA (Stratagene #946206). Screening for bacteriophage clones containing DNA inserts homologous with pp32 cDNA followed routine procedures (Sambrook, et al.). Briefly, nitrocellulose filters that had overlain bacteriophage plaques were hybridized with P-32 labeled probes for pp32 cDNA. The probes were prepared by the random primer method (Stratagene #300385) using pp32 cDNA as a template (Chen, et al., Molec. Biol. Cell, 7:2045-2056,1996.). Reactive bacteriophage plaques were plugged and the bacteriophages were eluted, reexpressed, and rescreened with pp32 cDNA probes until pure. Bacteriophage DNA was prepared by the plate lysate method (Sambrook, et al.).
[0099] Identifying Restriction Fragments within Bacteriophage DNA Containing Sequences Homologous with pp32 cDNA.
[0100] DNA from a bacteriophage clone containing pp32 cDNA sequences was digested with HindIII. Using routine methods, the restriction fragments were separated by agarose gel electrophoresis, transferred in alkaline buffer to positively charged nylon filters, and hybridized with probes that were selective for the 5′ and 3′ ends of the pp32 cDNA (Sambrook, et al.). The 5′ and 3′ probes were prepared as described above except that the products of polymerase chain reactions (PCR) were used as templates for the labeling reactions (Sailki, et al., Science, 239:487-491, 1988.). One PCR product was a 249 base pair segment of pp32 cDNA containing nucleotides 32 through 279. It was the result of a reaction using a pp32cDNA template and the primers
[0101] 5′-TATGCTAGCGGGTTCGGGGTTTATTG-3′ and
[0102] 5′-GATTCTAGATGGTAAGTTTGCGATTGAGG-3′ (primer set A).
[0103] The other product was a 263 base pair segment of pp32 cDNA including nucleotides 677 through 938. It was the result of a reaction using a pp32 cDNA template and the primers
[0104] 5′-GAATCTAGAAGGAGGAGGAAGGTGAAGAG-3′ and
[0105] 5′-CTATCTAGATTCAGGGGGCAGGATTAGAG-3′ (primer set B).
[0106] The PCR reactions included 35 cycles of one minute denaturations at 95° C., one minute primer annealings at 50° C., and one minute extensions at 72° C. (cycling program A). A 4.7 kb HindIII restriction fragment that hybridized with the 5′ probe, but not with the 3′ probe and a 0.9 kb HindIII fragment that hybridized with the 3′ probe, but not with the 5′ probe were subcloned into pBluescript (Gibco) by routine methods (Sambrook, et al.). The nucleotide sequences of both strands of purified plasmid DNA containing the inserts were determined by automated procedures (DNA Analysis Facility, Johns Hopkins University School of Medicine).
[0107] Completion of Sequencing by Direct Sequencing of PCR Products. Alignment of the sequences of the 4.7 and 0.9 kb HindIII restriction fragments with pp32 cDNA showed about 90% homologies between the 3′ end of the 4.7 kb fragment and the 5′ region of pp32 cDNA and the 5′ end of the 0.9 kb fragment and the 3′ region of the pp32 cDNA. There was an unaligned 199 base pair gap of pp32 cDNA sequence between the ends of the restriction fragments. Primers were designed to specifically anneal to relative pp32 sequences on both sides of the sequence gap. The primer sequences were
[0108] 5′-GAGGTTTATTGATTGAATTCGGCT-3′ and
[0109] 5′-CCCCAGTACACTTTTCCCGTCTCA-3′ (primer set C).
[0110] Polymerase chain reactions followed cycling program A with primer set C and pure bacteriophage DNA as a template. The 943 base pair products were shown by ethidium bromide staining agarose gels, extracted from excised fragments of low melt agarose (NuSieve) electrophoresis gels, and sequenced by automated procedures as described above.
[0111] A sequence of 5,785 bases was obtained from the human placental genomic library bacteriophage clone containing segments homologous with pp32 cDNA (FIG. 2). This sequence was deposited in Genbank under Accession No. U71084, Locus HSU71084. The sequence has an open reading frame extending from nucleotides 4,453 to 5,154. Analysis of the nucleotide sequence upstream of the open reading frame revealed consensus sequences for active steroid hormone receptors at over twenty positions (Table 1).
[0112] Sequence analysis of the open reading frame showed 94% sequence homology to pp32 (FIG. 3). Alignment of the-open reading frame sequence to pp32 cDNA revealed 33 scattered, solitary base differences and clustered differences of two and seven bases. There were two internal deletions of three and nine bases. The open reading frame encoded a polypeptide containing 234 amino acid residues with 88% protein-level homology to pp32 (FIG. 4). Alignment of the translated sequence to the pp32 amino acid sequence revealed 18 scattered, solitary amino acid residue differences, three differences in clusters of two residues, and one difference in a clusters of four residues. There were two internal deletions of one and three residues and a terminal deletion of eleven residues. The translated sequence contained 69 acidic residues, 26 fewer than pp32.
Example 4
[0113] Chromosome Mapping of pp32r1
[0114] The pp32r1 gene maps to chromosome 4 as determined by PCR of the NIGMS monochromosomal panel 2 (Drwinga, et al., “NIGMS human/rodent somatic cell hybrid mapping panels 1 and 2,” Genomics 16:311314, 1993) followed by sequencing of the PCR product. Interestingly, the full sequence of pp32r1 including 4364 nucleotides of sequence 5′ to the start ATG contained over 400 matches in a blastn search of the non-redundant GenBank database. These matches were to two short regions of about 278 and 252 base pairs (nucleotides 674-952 and 2542-2794) that represent repeats in opposite orientations. The repeats are significantly related to elements on many chromosomes.
[0115] The human pp32 gene has been mapped to chromosome 15q22.3-q23 by fluorescence in situ hybridization (Fink, et al.). A Unigene entry for pp32 (Hs. 76689; HLA-DR associated protein 1) lists 93 EST sequences corresponding to this gene, 12 of which contain a mapped sequence-tagged site (STS). These STS sites are all reported to map to chromosome 15, as are many of the pp32 EST's analyzed by electronic PCR (http://www.ncbi.nlm.nih.gov). APRIL protein was also mapped to chromosome 15q25 (Mencinger, et al.; GenBank Y07969).
Example 5
[0116] Sequence Analysis of pp32r2
[0117] A pp32-related sequence (designated pp32r2) has been identified on chromosome 12 by methods analogous to those described in Example 2 for isolation of the unique intronless pp32-related gene pp32r1, found on chromosome 4. It was initially thought that the chromosome 12 sequence, encoding a truncated protein, might represent a pseudogene; however that interpretation has been reassessed in view of the present findings. The sequence has been designated pp32r2, and is recorded in Genbank as locus AF008216: the sequence of pp32r2 is shown in FIG. 5. By BESTFIT analysis (Genetics Computer Group. Inc., Wisconsin Package, version 9.1, Madison, Wis., 1997), pp32r2 is 99.5% identical to FT1.11, FT2.4 and T1, showing four nucleotide differences over the 875 nucleotide overlap of the sequences: this level of variation is consistent with a polymorphism. Similarly, BESTFIT analysis shows that PP32R1 is 99.6 % identical to FT3.3 and 99.4% identical to FT2.2, displaying four and five nucleotide differences, respectively (see FIG. 7 below).
Example 6
[0118] Sequence Comparison of Multiple Clones
[0119] Screening of a human placental genomic library in Lambda Fix II vector (Stratagene #946206) with P-32 labeled probes for pp32 cDNA yielded a clone of approximately 23 kb. 4.7 kb and 0.9 kb HindIII restriction fragments of this clone hybridized with probes for pp32 cDNA. The 4.7 kb clone aligned with the 5′ portion of the pp32 cDNA sequence, and the 0.9 kb fragment aligned with the 3′ end. A small discontinuity of 0.2 kb was sequenced from a bridging PCR product. No introns were identified.
[0120] Cultured cells including the whole human embryonic line FSH173WE and the prostatic cancer cell lines PC-3 and LNCaP (American Type Culture Collection) were grown under recommended tissue culture conditions. Poly A+RNA was prepared by oligo dT adsorption (MicroFasTrack, Invitrogen) and used as a template for the, generation of cDNA through reactions with reverse transcriptase and random hexamers (GeneAmp RNA PCR Kit, Perkin Elmer). The cDNA sequences encoding the open reading frame were amplified by nested PCR using primers specifically selective for the genomic sequence over pp32 sequences. The final 298 base pair products were seen by ethidium bromide staining agarose electrophoretic gels.
[0121] Using procedures similar to those described in Example 3, except without the need for nested primers in most cases, transcripts from DU-145 cells and from numerous patients were sequenced for comparison to the transcripts from the above samples. The results are shown in Table 2. A summary of the degree of identity between various transcripts is provided in Table 3.
Example 7
[0122] Sequence Variation for Individual Isolates of Different Cell Lines and Tumor Tissue
[0123] The explanation for the apparent discordant expression of p32 in cancer is that prostate tumors do not generally express pp32, but rather express variant pp32 species that promote transformation, instead of inhibiting it.
[0124] RT-PCR and CFLP. Sequences were reverse-transcribed and amplified using bases 32 to 52 of HSU73477 as a forward primer and 9 19 to 938 of the same sequence as a reverse primer in conjunction with the Titan One-Tube RT-PCR kit (Boehringer). Reverse transcription was carried out at 50° for 45 min followed by incubation at 94° for 2 min; the subsequent PCR utilized 45 cycles of 92° for 45, 55° for 45 sec. and 68° for 1 min with a final extension at 68° for 10 min in a PTC 100 thermocycler (MJ Research). Template RNA was isolated from cell lines or frozen tumor samples using RNAzol B (Tel-Test) according to the manufacturer's instructions, then digested with RNAse-free DNAse 1 (Boehringer). pCMV32 was used as a positive control without reverse transcription. The cleavage assay was performed according to the manufacturer's specifications (Life Technologies) with digestion at 55° for 10 min at 0.2 mM MnCl 2 and electrophoresed on a 6% denaturing polyacrylamide sequencing gel.
[0125] At the level of RTPCR, paired normal prostate and prostatic adenocarcinoma from three patients yielded amplification products (FIG. 6A) ranging from 889 to 909 bp. The reaction employed consensus primers capable of ampliring the full-length coding sequence from pp32 and the two closely-related intronless genomic sequences pp32r1 and pp32r2. The sole difference noted was a diminished amplicon yield from normal tissue as compared to neoplastic. Four human prostatic adenocarcinoma cell lines, DU-145, LNCaP, PC-3, and TSUPR-1, also yielded similar products.
[0126] [0126]FIG. 6A shows RT-PCR amplified DNA from human prostate and prostate cancer cell lines. Lane a is an undigested control whose band migrated substantially slower than the digestion produces; samples in all other lanes were digested with cleavage as described. The lanes show: 1 kb ladder (Lifé Technologies), A; pCMV32, B; DU-145, C; LNCaP, D; PC-3, E; TSUPr-1, F; a representative sample, FT-1, without reverse transcription, G; FN-1 H; FT-1, I; FN-2, J; FT-2, K; FN-3, L; FT3, M; negative control with template omitted. FN indicates frozen benign prostate and the number indicates the patient: FT indicates frozen prostatic adenocarcinoma and the number indicates the patient. Numbers on the left-hand side of the figure indicate the size in kb of a reference 1 kb DNA ladder (Life Technologies).
[0127] Qualitative differences between normal and neoplastic tissue began to emerge when the RT-PCR products were subcloned and analyzed by cleavage fragment length polymorphism analysis (CFLP) and sequence analysis. FIG. 6B shows a cleavase fragment length polymorphism analysis of cloned cDNA amplified by RT-PCR from human prostatic adenocarcinoma, adjacent normal prostate, and human prostatic adenocarcinoma cell lines using primers derived from the normal pp32 cDNA sequence. The lanes show individual RT-PCR-derived clones from the DU-145, LNCaP, PC-3 and TSUPr1 cell lines, from frozen prostate cancer (FT), and from frozen normal prostate (FN): a, undigested normal pp32 cDNA, be normal pp32cDNA: c, DU-145-1; d, DU-145-3; e, DU-145-5; f, LNCaP-3; g, PC3-3; h, PC3-8; i, TSUPr1, -I; j, TSUPr1-3; k, TSUPr1-6; 1, FT1.11; m, FT1.7; n, FT2.2; o, FT2.4; p, FT3.18; q, FT3.3; r, FN3.17; s, FN2.1. LNCaP expresses normal pp32. The band shifts correspond to sequence differences. All clones of RT-PCR product from normal prostate tissue displayed a normal CFLP pattern that corresponded precisely to that obtained from cloned pp32 cDNA template (GenBank HSU73477, FIG. 6B). Prostatic adenocarcinomas yielded four distinct CFLP patterns upon similar analysis, of which three were unique and one mimicked the normal pp32 pattern. Examination of DU-145, PC-3, and TSUPR-1 cell lines yielded substantially similar results whereas LnCaP yielded only a normal pp32 CFLP pattern. Further analysis at the sequence level confirmed that normal prostate and LnCaP contained solely normal pp32 transcripts.
[0128] Transcripts obtained from prostatic adenocarcinomas and from most cell lines represented closely-related variant species of pp32, summarized in Table 1. These transcripts varied from 92.4% to 95.9% nucleotide identity to normal pp32 cDNA (Genetics Computer Group, Inc., Wisconsin Package, version 9.1, Madison, Wis., 1997). Of the sixteen variant transcripts obtained, fifteen had open reading frames encoding proteins ranging from 89.3% to 99.6% identity to normal pp32. The table summarizes data obtained for variant pp32 transcripts obtained from human prostatic adenocarcinoma and prostate cancer cell lines. Sequences falling into closely related groups are indicated by the group letters (A,B,C); U indicates unassigned sequences not clearly falling into a group. The origin of each sequence is: FT, frozen tumor followed by patient number, decimal point, and clone number; D, DU-145 followed by clone number (as are all cell line sequences); P, PC3; and T, TSUPr1. Nucleotide identity, gaps in the nucleotide sequence alignment, and protein identity were determined from BESTFIT alignments with the normal pp32 cDNA and protein sequences. The effect on transformation is described as: stimulates, more foci obtained when transfected with ras+myc than with ras-myc+vector control: inactive, equivalent foci obtained as with ras+myc+vector control; and suppresses, fewer foci obtained as with ras+myc+vector control.
[0129] The predicted protein sequences fell into three discrete groups: [1] truncated sequences spanning the N-terminal 131 amino acids of pp32, of which one such sequence substantially equivalent to pp32r2 was obtained identically from two of three patients and from the TSUPR-1 cell line; [2] sequences more closely homologous to a distinct pp32-related gene, pp32r1 than to pp32, and [3] heterogeneous pp32-related sequences. Tumors from two of the three patients analyzed contained no detectable normal pp32 transcripts. Two of twelve cloned transcripts from the third patient tumor were normal by CFLP pattern, with sequence confirmation of normality on one clone. Two clones from cell lines were normal by CFLP screening, but were later shown to represent variant-sequences.
[0130] [0130]FIGS. 7A and 7B show a multiple pairwise alignment of nucleotide and predicted protein sequences for all transcripts (Smith, et al., “Identification of common molecular subsequences,” J. Mol. Biol., 147:195-197 1981). The figures were compiled with the GCG Pileup and Pretty programs (Smith, et al.). Differences from the consensus sequences are shown as indicated, agreement with the consensus sequence is shown as a blank. Normal human pp32 is designated hpp32. Sequences from the TSUPr1, PC3, and DU-145 cell lines are as indicated. The designation FT indicates sequence derived from a frozen human prostatic adenocarcinoma. Only the normal pp32 sequence. hpp32, was obtained from normal prostate adjacent to tumor tissue. FIG. 8A shows alignment of the amplicon nucleotide sequences with pp32 and the predicted amplicon from pp32r1: FIG. 8B shows alignment of the predicted protein sequences. One sequence (FT 1.11), independently obtained three times from two separate patients and the TSUPR-1 cell line, is shown only once in the diagram. The pileup and pairwise alignments illustrate several important points: [1] there is a high degree of sequence conservation at both the nucleotide and predicted amino acid levels; [2] the sequence differences are distributed throughout the length of the sequence without obvious hotspots; [3] there is no obvious clustering or segmentation of sequence differences: and [4] the variant sequences fall into the previously described groups. These points are detailed in FIGS. 8A and 8B.
Example 8
[0131] Diagnostic Method to Distinguish Among Family Members
[0132] The three members of the pp32 family which are expressed in human prostate cancer are pp32, pp32r1 and pp32r2. Whereas pp32 suppresses in vitro transformation and in vivo tumorigenesis in model systems, pp32r1 and pp32r2 are pro-transforming and are tumorigenic in the same systems. It is possible to determine which of the three members is expressed in a tissue sample by using a protocol similar to that described in Example 7.
[0133] Analysis from freshly frozen human tissue and cell lines. Total RNA is extracted from freshly frozen human tissues or human cancer cell lines and subjected to reverse transcription and polymerase chain reaction amplification with single set of primers capable of amplifying the entire coding region of the cDNA of all the three genes. A suitable set of primers is:
[0134] Upper: 5′GGGTTCGGGGTTTATTG3′—This corresponds to bp32 to bp48 of the pp32 cDNA sequence (Genbank U73477)
[0135] Lower: 5′CTCTAATCCTGCCCCCTGAA3′—This corresponds to bp919 to bp938 of the pp32 cDNA sequence (Genbank U73477)
[0136] The observed amplicon sizes with this primer set are pp32-907 bp, pp32r1-889 bp and pp32r2-900 bp. The three cDNAs are distinguished from each other by restriction enzyme digestion with the following enzymes—EcoR I, Hind III and Xho I. The resultant digest is run on a 2.5% agarose gel to positively identify the three different cDNAs. The table below lists the sizes of the bands observed The bolded numbers indicate the band sizes useful for identification of the three cDNAs.
TABLE 4A Expected band sizes upon restriction digestion of the RT-PCR product from fresh tissue and cell lines EcoR I/Hind III EcoR I/Xho I Undigested EcoR I Double digest Double digest hpp32 907 21,177,709 21,177,69,640 21,177,709 pp32r1 889 21,177,691 21,19,66,198,427 21,177,691 pp32r2 900 21,879 21,244,635 21,385,494
[0137] Analysis from formalin fixed and paraffin embedded tissue. A similar approach is followed for identification of pp32, pp32r1 and pp32r2 transcripts from formalin fixed and paraffin embedded tissues. Total RNA is extracted and subjected to reverse transcription and PCR amplification with a single set of primers capable of amplifying a stretch of 200 bp from all the three cDNAs. A suitable set of primers is:
[0138] Upper primer—from bp394 to bp414 of the pp32 cDNA sequence (Genbank U73477)
[0139] Lower primer—from bp609 to bp629 of the pp32 cDNA sequence (Genbank U73477)
[0140] The three cDNAs are distinguished from each other by restriction enzyme digestion with the following enzymes—Hind III, Xho I and BseR 1. The resultant digest is run on a 3% agarose gel to positively identify the three different cDNAs. The table below lists the sizes of the bands observed. The bolded numbers indicate the band sizes useful for identification of the three cDNAs.
TABLE 5A Expected band sizes upon restriction digestion of the RT-PCR product from formalin fixed and paraffin embedded tissues Undigested Hind III Xho I BseR I hpp32 200 200 200 80,120 pp32r1 200 100,100 200 200 pp32r2 200 200 44,156 80,120
Example 9
[0141] pp32r1 Augments Oncogene-Mediated Transformation of Rat Embryo Fibroblasts.
[0142] pp32r1 was subcloned into a eukaryotic expression vector under the CMV promoter and analyzed for its effect on ras+myc-mediated formation of transformed foci in rat embryo fibroblasts. Genomic sequences including the entire coding region for pp32r1 were amplified by PCR and subcloned into the eukaryotic TA cloning and expression vector pCR3.1 vector (Invitrogen) which contains a CMV promoter. The assay was performed as described (Chen et al. Mol Biol Cell, 7:2045-56, 1996) with each T75 flask receiving 5 micrograms of pEJ-ras, and/or 10 micrograms of pMLV-c-myc, pCMV32, pp32r1 in PCR3.1, or PCR 3.1 alone. After 14 days, transformed colonies were enumerated. FIG. 8 shows the results. The data represent the average of seven replicates from two separate experiments in duplicate and one in triplicate. The error bars indicate standard error of the mean. In contrast to pp32, which consistently suppresses focus formation induced by ras+myc and other oncogene pairs, pp32r1 caused a statistically significant stimulation of focus formation with p=0.004 by an unpaired t-test.
Example 10
[0143] Effect of Transcripts from Various Cell Lines on Rat Fibroblast Transformation Assays
[0144] Expression constructs prepared as described above from PC-3 and DU-145 cells were tested in the rat embryo fibroblast transformation assay described by Chen, et al., Mol Biol Cell., 7:2045-56, 1996, incorporated herein by reference. The results are shown in FIG. 9. Transcripts from the two cell lines stimulated ras+myc induction of transformed rat embryo fibroblast foci, in contrast to normal pp32, which suppressed transformation. The figure shows the mean±the standard deviation, except for DU-145, which represents a single determination.
Example 11
[0145] Transformation Activity of Various Isolates from Patient Tumors
[0146] The variant transcripts isolated from prostate cancer patients differ significantly from pp32 in sequence. The isolated transcripts were found to stimulate transformation. Transformation assay. Rat embryo fibroblasts were transfected with the indicated constructs as described (Chen, et al.) and transformed foci enumerated. For each experiment, approximately 1×10 6 cells were plated per T75 flask and incubated for 2 to 3 d prior to transfection to achieve approximately 40% confluency. For each flask of primary rat embryo fibroblasts, the plasmids indicated in each experiment were added in the following amounts: pEJ-ras, 5 μg; and pMLV-c-myc, pCMV32, pCMVneo, or variant pp32 constructs in pCR3.1 (Invitrogen), 10 μg. Plasmids were prepared in two volumes Lipofectin (2 μl lipofectin per μg DNA) then gently mixed by inversion in 1.5 ml OPTIMEM in sterile 15 ml polystyrene tubes and allowed to incubate at room temperature for >15 min. For experiments with more than one flask, mixtures of all reagents were increased in proportion to the numbers of flasks required for each transfection. Cells were washed once with OPTIMEM (Gibco-BRL), and then fed with 6 ml of OPTIMEM and 1.5 ml of the DNA/Lipofectin mix. After overnight incubation, the cells were grown in standard media and refed with fresh media twice weekly. Foci were counted fourteen days post-transfection. FIG. 10 summarizes four separate experiments. Each data point represents the results from an individual flask expressed as the percent foci obtained in the contemporaneous control of ras+myc+vector.
[0147] [0147]FIG. 10 shows that expressed variant transcripts from prostate cancer cell lines and from human prostatic adenocarcinoma generally produce increased numbers of transformed foci when co-transfected with ras and myc as compared to the number of foci obtained when ras and myc are transfected with blank vector. Variant pp32 transcripts from DU-145 (D3), and from three prostate cancers (FT 1.7, FT 2.2 and FT3.18) yield increased numbers of transformed foci over those produced by ras and myc alone with blank vector. This stands in marked contrast to normal pp32, which consistently suppresses transformation. These activities are also summarized in Table 1.
Example 12
[0148] Effect of pp32 Variants on Tumorigenesis in Vivo
[0149] Experiments testing the effect of transfection of NIH3T3 cells on tumorigenesis in vivo are consistent with in vitro results in rat embryo fibroblasts. NIH3T3 cells were stably transfected by lipofection with the pp32 species indicated in Table 6A carried in the pCR3.1-Uni CMV-driven mammalian expression vector (Invitrogen). The G418-resistant clones employed in these experiments were all shown by genomic PCR to carry the indicated pp32 species. For analysis of tumorigenesis, 5×10 6 cells in 100 microliters of unsupplemented Dulbecco's modified Eagle's medium without phenol red were injected into the flanks of female athymic nude mice on an outbred background of greater than six weeks in age (Harlan). For logistical reasons, inoculations of the various groups were staggered over a seven day period. Each group of mice was euthanized precisely seven weeks after inoculation. Where a mouse had a tumor, the tumor was dissected, measured, and weighed, and Table 6A reports the average weight of tumors in mice injected with cells carrying various vectors. One tumor from each group was examined histologically. All tumors were fibrosarcomas without noteworthy inflammation present. Data obtained with NIH3T3 cells indicate that NIH3T3 cells stably transfected with the variant pp32 species P3, P8, FT1.7, FT2.2, and FT2.4 form tumors when inoculated into nude mice. In contrast, NIH3T3 cells stably transfected to express human pp32 fail to form tumors in vivo even when further transfected with ras. Lines of NIH3T3 cells were also established that were stably transfected with expression constructs encoding pp32 or pp32-antisense. Basal expression of pp32 is essential for maintenance of contact inhibition and serum-dependent cell growth: antisense ablation of endogenous pp32 synthesis permitted cells to grow normally following serum withdrawal. Constitutive over-expression of pp32 potently suppressed ras-mediated transformation of NIH3T3 cells in vitro and tumorigenesis in vivo. In contrast, antisense ablation of endogenous pp32 dramatically increased the number and size of ras-transformed foci; in vivo, tumors obtained from ras-transformed antisense pp32 cells were approximately 50-fold greater in mass than tumors obtained from ras-transformed control cells.
[0150] For purposes of clarity of understanding, the foregoing invention has been described in some detail by way of illustration and example in conjunction with specific embodiments, although other aspects, advantages and modifications will be apparent to those skilled in the art to which the invention pertains. The foregoing description and examples are intended to illustrate, but not limit the scope of the invention. Modifications of the above-described modes for carrying out the invention that are apparent to persons of skill in medicine, immunology, hybridoma technology, pharmacology, pathology, and/or related fields are intended to be within the scope of the invention, which is limited only by the appended claims.
[0151] All publications and patent applications mentioned in this specification are indicative of the level of skill of those skilled in the art to which this invention pertains. All publications and patent applications are herein incorporate reference to the same extent as if each individual publication or patent application was specifically and individually indicated to be incorporated by reference.
TABLE 1 Consensus Position Strand Sequence Factor 4 C TTTCCT PEA3 21 N CAAGGTCA ELP 23 N AGGTCA PPAR 32 C CCCTAA TBF1 41 N CTTGGC NF-1 (-like proteins) 81 N TAAACAC Pit-1 82 N AAACACA HiNF-A 113 C CTTCCC c-Ets-2 118 N CTATCA GATA-1 122 N CAGTTG c-Myc 212 C AATAAATA TFIID 213 N ATAAATA ETF 247 N TATCTA NIT2 261 C AAGGAA c-Ets-2 262 N AGGAAA PEA3 283 C TTTTTCTTTTTC Hb 320 C TTATAT GAL4 333 N TAAAAAA TBP 349 N TTATACATT TBP 363 C AAGGAA c-Ets-2 394 C TTTCTATA TBP 398 N TATAAA TBP 398 N TATAAA TFIID 411 C CTGAATT Pit-1 420 N TGTCCC GR 423 C CCCTAA TBF1 434 N TTCCTT c-Ets-2 447 C CTTCCC c-Ets-2 514 N TTATCTCT GATA-1 514 C TTATCT GATA-2 515 N TATCTC NIT2 537 N TATGCA EFII 553 N AAGTCA GCN4 608 N TGACTA GCN4 628 N CCTCCCAAC LyF-1 640 N TGTCCT GR 648 N TTAAAATTCA 1-Oct 648 N TTAAAATTCA 4-Oct 649 N TAAAAT F2F 649 N TAAAAT Pit-1 661 N TAAAAAA TBP 673 N CTTGGC NF-1 (-like proteins) 725 N AGGCGG Sp1 729 N GGGCGG ETF 729 N GGGCGG Sp1 729 C GGGCGG Sp1 741 N AGGTCA PPAR 793 N TATAAATA B factor 793 N TATAAA TBP 793 N TATAAATA TFIID 793 N TATAAAT TMF 794 N ATAAATA ETF 809 N TTATCT GATA-1 809 C TTATCT GATA-2 815 N GGGTGTGG TEF-2 826 C CACATG muEBP-C2 826 C CACATG TFE3-S 826 N CACATG USF 978 N ATGTAAAACA 1-Oct 978 N ATGTAAAACA 2-Oct 978 N ATGTAAAACA NF-IL-2A 1000 N ATGTCAGA CSBP-1 1006 N GATTTC H4TF-1 1034 C TTTTCAT Pit-1 1047 N AAGATAAAACC RVF 1048 C AGATAA GATA-1 1048 N AGATAA GATA-2 1049 N GATAAA TFIID 1083 C GCCAAG NF-1 (-like proteins) 1124 N CGCCAT UCRF-L 1163 C GACCTG TGT3 1307 N CAGTCA GCN4 1347 C TGCATA EFII 1373 C AGAACA AR 1373 N AGAACAT GR 1373 N AGAACA GR 1373 C AGAACA GR 1373 N AGAACA PR 1373 C AGAACA PR 1373 N AGAACA PR A 1373 C AGAACA PR A 1393 C TCACTT IRF-1 1393 C TCACTT IRF-2 1395 C ACTTCCT E1A-F 1423 N TTATCT GATA-1 1423 C TTATCT GATA-2 1424 N TATCTA NIT2 1452 N TTACTC GCN4 1471 N TGGGTCA c-Fos 1471 N TGGGTCA c-Jun 1471 N TGGGTCA ER 1496 N TCTCTTA c-Myc 1511 N TATAAA TBP 1511 N TATAAA TFIID 1549 C TTTGAA TFIID 1568 C AATGTATAA TBP 1581 C TTTGAA TFIID 1590 C AGATAA GATA-1 1590 N AGATAA GATA-2 1591 C GATAATTG Dfd 1657 C AGGACA GR 1670 C ATTTTA F2F 1670 C ATTTTA Pit-1 1671 C TTTTATA B factor 1671 C TTTTATA Dr1 1671 C TTTTATA En 1671 C TTTTATA TBP 1671 C TTTTATA TBP-1 1671 C TTTTATA TFIIA 1671 C TTTTATA TFIIB 1671 C TTTTATA TFIID 1671 C TTTTATA TFIIE 1671 C TTTTATA TFIIF 1671 C TTTTATA TRF 1672 C TTTATA TBP 1694 C AATAAATA TFIID 1695 N ATAAATA ETF 1733 N AGGAAA PEA3 1749 C TTATAT GAL4 1783 N TAACTCA AP-1 1829 C TAGATA NIT2 1857 N CGCCAT UCRF-L 1875 N TTCTGGGAA IL-6 RE-BP 1895 N TGACTA GCN4 1899 N TATTTAA TBP 1942 N ATATAA GAL4 1985 C TTTATA TBP 1985 C TTTATA TFIID 2010 C AATAAATA TFIID 2011 N ATAAATA ETF 2058 C TGCATA EFII 2095 N CAGTCA GCN4 2146 C AAGGAA c-Ets-2 2147 N AGGAAA PEA3 2190 N AGGAAA PEA3 2220 C GGCACA GR 2252 N CCAATAG gammaCAAT 2286 N TGTGCC GR 2292 N ATGGGA PTF1-beta 2314 N TATGCA EFII 2328 C GGCACA GR 2350 C ATGATAAG GATA-1 2351 N TGATAAG GATA-1 2363 N GGGAAG c-Ets-2 2367 N AGCCACT CP2 2369 C CCACTGGGGA AP-2 2404 N TAAAAT F2F 2404 N TAAAAT F2F 2404 N TAAAAT Pit-1 2409 N TTGTCATA 77 + 82K protein 2409 N TTGTCATA VETF 2415 N TATCTA NIT2 2451 C TTTATC TFIID 2452 N TTATCT GATA-1 2452 C TTATCT GATA-2 2486 N CTCTCTCTCTCTC GAGA factor 2644 N AGGCGG Sp1 2658 N ACAGCTG GT-IIBalpha 2658 N ACAGCTG GT-IIBbeta 2709 C GGCCAGGC AP-2 2723 N TGAACT GR 2731 C TGACCT PPAR 2731 C TGACCTCA URTF 2753 N CTTGGC NF-1 (-like proteins) 2818 C TGATGTCA AP-1 2818 C TGATGTCA c-Fos 2818 C TGATGTCA c-Jun 2818 C TGATGTCA CREB 2845 N GGGAAG c-Ets-2 2858 N AGATAG GATA-1 2858 C AGATAG GATA-1 2864 C AGTTCA GR 2899 N ATATAA GAL4 2900 N TATAAAA B factor 2900 N TATAAAA Dr1 2900 N TATAAAA En 2900 N TATAAAA TBP 2900 N TATAAA TBP 2900 N TATAAAA TBP-1 2900 N TATAAAA TFIIA 2900 N TATAAAA TFIIB 2900 N TATAAAA TFIID 2900 N TATAAAA TFIIE 2900 N TATAAAA TFIIF 2900 N TATAAAA TRF 2921 C TTTGAA TFIID 2924 C GAAATC H4TF-1 2930 C CATTAG Is1-1 2948 C TGTACA GR 2948 C TGTACA PR 2948 C TGTACA PR A 2964 C ATTTGAGAA VITF 3030 N AGTGTTCT GR 3032 N TGTTCT AR 3032 N TGTTCT GR 3032 C TGTTCT GR 3032 N TGTTCT PR 3032 C TGTTCT PR 3032 N TGTTCT PR A 3032 C TGTTCT PR A 3104 C GGATTATT T11 3106 C ATTATTAA AFP1 3111 N TAAAAT F2F 3111 N TAAAAT Pit-1 3125 C ATTTTA F2F 3125 C ATTTTA Pit-1 3142 N TGTGAT GR 3169 N GTTTTATT HOXD10 3169 N GTTTTATT HOXD8 3169 N GTTTTATT HOXD9 3175 C TTTGAA TFIID 3185 N TTGCTCA Zta 3206 N GATTTC H4TF-1 3212 N AGGAAA PEA3 3238 C ATTTTA F2F 3238 C ATTTTA Pit-1 3256 C TTTGAA TFIID 3266 N TTGCTCA Zta 3320 C ATTTTA F2F 3320 C ATTTTA Pit-1 3358 N ATGGGA PTF1-beta 3360 C GGGACA GR 3440 C CACTCA GCN4 3460 C TTTCCT PEA3 3483 N GACACA GR 3491 C TTTCCT PEA3 3495 N CTAATG Is1-l 3523 C AGAACA AR 3523 N AGAACA GR 3523 C AGAACACT GR 3523 C AGAACA GR 3523 N AGAACA PR 3523 C AGAACA PR 3523 N AGAACA PR A 3523 C AGAACA PR A 3538 C TTTATC TFIID 3539 N TTATCT GATA-1 3539 C TTATCT GATA-2 3551 N TGAGTG GCN4 3569 C TCCCAT PTF1-beta 3594 N TTAGGG TBF1 3653 C CCTGCTGAA LyF-1 3668 N CTCATGA 1-Oct 3668 N CTCATGA 2-Oct 3668 N CTCATGA Oct-2B 3668 N CTCATGA Oct-2B 3668 N CTCATGA Oct-2C 3679 C TGTGTAA Zta 3685 C AGAACT GR 3712 C TTTCCT PEA3 3713 N TTCCTT c-Ets-2 3717 N TTGCTCA Zta 3727 C AAAACATAAAT ssARS-T 3749 N TAAAAAA TBP 3784 C CACTCA GCN4 3791 C ATTTTA F2F 3791 C ATTTTA Pit-1 3815 N TATCTA NIT2 3829 C TAGATA NIT2 3859 C AGAACA AR 3859 N AGAACAG GR 3859 N AGAACA GR 3859 C AGAACA GR 3859 N AGAACA PR 3859 C AGAACA PR 3859 N AGAACA PR A 3859 C AGAACA PR A 3860 N GAACAG LVa 3877 C ATCACA GR 3886 N TGAGTCA AP-1 3886 C TGAGTCA AP-1 3886 C TGAGTCA c-Fos 3886 C TGAGTCA c-Jun 3886 C TGAGTCA FraI 3886 C TGAGTCA NF-E2 3887 C GAGTCA GCN4 3931 N AGATAG GATA-1 3931 C AGATAG GATA-1 3960 N TTGGCA NF-1/L 3965 C ATTTTA F2F 3965 C ATTTTA Pit-1 4026 N TATTTAA TBP 4037 N TGTGAT GR 4040 N GATGCAT Pit-1 4Q42 C TGCATA EFII 4079 N TTCAAAG SRY 4079 N TTCAAAG TCF-1A 4079 N TTCAAA TFIID 4097 N CAGGTC TGT3 4140 N TGATTCA AP-1 4140 C TGATTCA AP-1 4140 N TGATTC GCN4 4164 N GGGAGTG p300 4205 C AGATAA GATA-1 4205 N AGATAA GATA-2 4219 C TTAGTCAC AP-1 4219 C TTAGTCA AP-1 4219 C TTAGTCAC c-Fos 4219 C TTAGTCAC c-Jun 4219 C TTAGTCA c-Jun 4219 C TTAGTCA Jun-D 4220 C TAGTCA GCN4 4271 N TGTTCT AR 4271 N TGTTCT GR 4271 C TGTTCT GR 4271 N TGTTCT PR 4271 C TGTTCT PR 4271 N TGTTCT PR A 4271 C TGTTCT PR A 4280 C TGACCCA c-Fos 4280 C TGACCCA c-Jun 4280 C TGACCCA ER 4292 C CTTATCAG GATA-1 4292 C CTTATCA GATA-1 4361 N TTCAAAG SRY 4361 N TTCAAAG TCF-1A 4361 N TTCAAA TFIID
[0152] [0152] TABLE 2 COMPARISON OF ALL PROTEIN SEQUENCES 1 15 16 30 31 45 46 60 61 75 TSU6 MEMGRRIHLELRNGT PSDVKELVLDNSRSN EGKLEGLTDEFEELE FLSTINVGLTSIANL PKLNKLKKLELSSNR D3 MEMGRRIHLELRNRT PSDVKELVLDNSRSN EGKLEGLTDEFEELE FLSTINVGLTSIANL PKLNKLKKLELSDNR PG MEMGKWIHLELRNRT PSDVKELFLDNSQSN EGKLEGLADEFEELE LLNTINIGLSSIANL AKLNKLKKLELSSNR FT1.11 MEMGKWIHLELRNRT PSDVKELFLDNSQSN EGKLEGLTDEFEELE LLNTINIGLTSIANL PKLNKLKKLELSSNR TSU1 MEMGKWIHLELRNRT PSDVKELFLDNSQSN EGKLEGLTDEFEELE LLNTINIGLTSIANL PKLNKLKKLELSSNR FT3.18 MEMGKWIHLELRNRT PSDVKELFLDNSQSN EGKLEGLTDEFEELE LLNTINIGLTSIANL PKLNKLKKLELSSNR FT2.4 MEMGKWIHLELRNRT PSDVKELFLDNSQSN EGKLEGLTDEFEELE LLNTINIGLTSIANL PKLNKLKKLELSSNR FT2.2 MEMGRRIHSELRNRA PSDVKELVLDNSRSN EGKLEALTDEFEELE FLSKINGGLTSISDL PKL-KLRKLEL---K KG MEMGRRIHSELRNRA PSDVKELALDNSRSN EGKLEALTDEFEELE FLSKINGGLTSISDL PKL-KLRKLEL---R FT1.7 MEMGRRIHLELRNRT PSDVKELVLDNSRSN EGKLEGLTDEFEELE FLSTINVGLTSIANL PKL-KLRKLEL---R P3 MEMGKWIHLELRNRT PSDVKELFLDNSQSN EGKLEGLTDEFEELE LLNTINIGLTSIANL PKLNKLKKLELSSNR L3 MEMGRRIHLELRNRT PSDVKELVLDNSRSN EGKLEGLTDEFEELE FLSTINVGLTSIANL PKLNKLKKLELSDNR pp32 MEMGRRIHLELRNRT PSDVKELVLDNSRSN EGKLEGLTDEFEELE FLSTINVGLTSIANL PKLNKLKKLELSDNR P8 MEMGRRIHLELRNRT PSDVKELVLDNSRSN EGKLEGLTDEFEELE FLSTINVGLTSIANL PKLNKLKKLELSSNR 76 90 91 105 106 120 121 135 136 150 TSU6 ASVGLEVLAEKCPNL 90 IHLNLSGNKIKDLST IEPLKKLENLESLDL FTCEVTNLNNY---- --------------- D3 VSGGLEVLAEKCPNL 90 IHLNLSGNKIKDLST IEPLKKLENLESLDL FTCEVTNLNNY---- --------------- PG ASVGLEVLAEKCPNL 90 IHLNLSGNKIKDLST IEPLKKLENLESLDL FTCEVTNLNNY---- --------------- FT1.11 ASVGLEVLAEKCPNL 90 IHLNLSGNKIKDLST IEPLKKLENLESLDL FTCEVTNLNNY---- --------------- TSU1 ASVGLEVLAEKCPNL 90 IHLNLSGNKIKDLST IEPLKKLENLESLDL FTCEVTNLNNY---- --------------- FT3.18 ASVGLEVLAEKCPNL 90 IHLNLSGNKIKDLST IEPLKKLENLESLDL FTCEVTNLNNY---- --------------- FT2.4 ASVGLEVLAEKCPNL 90 IHLNLSGNKIKDLST IEPLKKLENLESLDL FTCEVTNLNNY---- --------------- FT2.2 VSGGLEVLAEKCPNL 86 THLYLSGNKIKDLST IEPLKQLENLKSLDL FNCEVTNLNDYGENV FKLLLQLTYLDSCYW KG VSGGLEVLAEKCPNL 86 THLYLSGNKIKDLST IEPLKQLENLKSLDL FNCEVTNLNDYGENV FKLLLQLTYLDSCYW FT1.7 VSGGLEVLAEKCPNL 86 THLYLSGNKIKDLST IEPLKQLENLKSLDL FNCEVTNLNDYGENV FKLLLQLTYLDSCYW P3 ASVGLEVLAEKCPNL 90 IHLNLSGNKIKDLST IEPLKKLENLESLDL FTCEVTNLNNYRENV FKLLPQLTYLDGYDR L3 VSGGLEVLAEKCPNL 90 THLNLSGNKIKDLST IEPLKKLENLESLDL FNCEVTNLNDYRENV FKLLPQLTYLDGYDR pp32 VSGGLEVLAEKCPNL 90 THLNLSGNKIKDLST IEPLKKLENLESLDL FNCEVTNLNDYRENV FKLLPQLTYLDGYDR P8 ASVGLEVLAEKCPNL 90 IHLNLSGNKIKDLST IEPLKKLENLESLDL SNCEVTNLNDYRENV FKLLPQLTYLDGYDR 151 165 166 180 181 195 196 210 TSU6 --------------- --------------- 131 --------------- --------------- D3 --------------- --------------- 131 --------------- --------------- PG --------------- --------------- 131 --------------- --------------- FT1.11 --------------- --------------- 131 --------------- --------------- TSU1 --------------- --------------- 131 --------------- --------------- FT3.18 --------------- --------------- 131 --------------- --------------- FT2.4 --------------- --------------- 131 --------------- --------------- FT2.2 DHKEAPYSDIEDHVE GLDDEEEGEHEEEYD 176 EDAQVVEDEEGEEEE EEGEEEDVSGGDEED KG DHKEAPYSDIEDHVE GLDDEEEGEHEEEYD 176 EDAQVVEDEEGEEEE EEGEEEDVSGGDEED FT1.7 DHKEAPYSDIEDHVE GLDDEEEGEHEEEYD 176 EDAQVVEDEEGEEGE EEGEEEDVSGGDEED P3 DDKEAPDSDAEGYVE GLDDEEEDEDEEEYD 180 EDAQVVEDEEDEDEE EEGEEEDVSGEEEED L3 DDKEAPDSDAEGYVE GLDDEEEDEDEEEYD 180 EDAQVVEDEEDEDEE EEGEEEDVSGEEEED pp32 DDKEAPDSDAEGYVE GLDDEEEDEDEEEYD 180 EDAQVVEDEEDEDEE EEGEEEDVSGEEEED P8 DDKEAPDSDAEGYVE GLDDEEEDEDEEEYD 180 EDAQVVEDEEDEDEE EEGEEEDVSGEEEED 211 225 226 240 241 TSU6 --------------- --------------- --------- 131 D3 --------------- --------------- --------- 131 PG --------------- --------------- --------- 131 FT1.11 --------------- --------------- --------- 131 TSU1 --------------- --------------- --------- 131 FT3.18 --------------- --------------- --------- 131 FT2.4 --------------- --------------- --------- 131 FT2.2 EEGYNDGEVDGEEDE EELGEEERGQKRK-- --------- 234 KG EEGYNDGEVDGEEDE EELGEEERGQKRK-- --------- 234 FT1.7 EEGYNDGEVDDEEDE EELGEEERGQKRKRE PEDEGEDDD 245 P3 EEGYNDGEVDDEEDE EELGEEERGQKRKRE PEDEGEDDD 249 L3 EEGYNDGEVDDEEDE EELGEEERGQKRKRE PEDEGEDDD 249 pp32 EEGYNDGEVDDEEDE EELGEEERGQKRKRE PEDEGEDDD 249 P8 EEGYNDGEVDDEEDE EELGEEERGQKRKRE PEDEGEDDD 249
[0153] [0153] TABLE 3 Comparison to pp32 Sequences % Identity % Similarity CLONE cDNA Protein Protein D3, DU-145 cells 95 90 95 P3, PC-3 86 94 96 P8, PC-3 98 97 97 FT1.11 97 86 92 FT1.7 95 95 95 FT2.2 94 85 88 FT2.4 99 86 92 FT3.18 99 90 94
[0154] [0154] TABLE 1A Effect on Oncogene- Sequence Nucleotide Protein Identity Mediated Sequence Group Identity with pp32 Gaps with pp32 Transformation Comment FT1.3 A 99.8 100 Not Tested Identical to pp32 D1 A 99.9 100 Not tested identical to pp32 with 2 silent nt changes L3 A 99.9 100 Not Tested D3 U 95.8 0 96.9 Generally Encodes truncated variant Stimulatory pp32 D5 U 99.6 0 99.6 Not Tested FT1.2 U 92.9 1 Not tested No ORF P3 U 96.5 1 94.4 Slightly Stimulatory P8 U 98.7 0 98.0 Variable FT1.11 B 92.4 2 89.3 Not Tested All sequences identical, appears to be product of pp32r2 FT2.4 B 92.4 2 89.3 Variable T1 B 92.4 2 89.3 T6 U 94.2 1 93.9 Not Tested Encodes truncated variant pp32 FT3.18 U 94.7 2 89.3 Stimulatory Encodes truncated variant pp32 FT2.2 C 94.4 3 87.6 Stimulatory Sequences differ by 1 nt appears to be product of pp32r1 FT3.3 C 94.4 3 87.6 not tested FT1.7 U 95.9 2 91.4 Stimulatory
[0155] [0155] TABLE 2A Genbank Protein Accession Length Human pp32 Human pp32r1 Human pp32r2 Human April Murine pp32 Human pp32 HSU73477 249 100% 88% Identity 84% Identity 0 71% Identity 89% Identity 2 gaps; Z = 77 gaps; Z = 73 3 gaps; Z = 58 1 gap; Z = 87 Human pp32r1 AF008216 234 100% Identity 785 Identity 2 61% Identity 90% identity 3 gaps; Z = 65 5 gaps; Z = 15 gaps; Z = 64 Human pp32r2 HSU71084 131 100% Identity 61% Identity 77% Identity 3 gaps; Z = 52 1 gap; Z = 80 Human April Y07969 249 100% 71% Identity 4 gaps; Z = 68 Murine pp32 U734778 247 100% Identity
[0156] [0156] TABLE 3A pp32 Homologs human pp32 (Genbank Locus HSU73477) murine pp32 (Genbank Locus MMU73478) human cerebellar leucine rich acidic nuclear protein (LANP) (Genbank Locus AF025684) murine LANP (Genbank Locus AF022957) murine RFC1 (Genbank Locus MUSMRFC, Accession NO. L23755) HPP2a or human potent heat-stable protein phospatase 2a inhibitor (Genbank Locus HSU60823) SSP29 (Genbank Locus HSU70439) HLA-DR associated protein I (Genbank Locus HSPPHAPI, Accession No. X75090) PHAPI2a (EMBL Locus HSPHAPI2A, Genbank Accession No. Y07569) PHAPI2b (EMBL Locus HSPHAPI2B, Genbank Accession No. Y07570) April (EMBL Locus HSAPRIL)
[0157] [0157] TABLE 6A Tumorigenicity in Nude Mice of NIH3T3 Cells Transfected with pp32 and pp32 Variants pp32 Species Clone Tumors/ Average Tumor Weight FT1.7 1 3/3 14.9 ± 2.1 2 1 3/3 13.3 ± 3.7 FT2.2 1 3/3 10.5 ± 2.8 2 3/3 3.8 ± 2.1 FT2.4 1 3/3 6 1.3 ± 0.9 2 3/3 13.8 ± 3.3 D3 5 2 0/3 6 2 0/3 P3 11 3/3 5.7 ± 0.5 14 3 3/3 2.1 ± 1.2 P8 1 4 3/3 6.4 ± 5.3 2 3/3 11.3 ± 3.9 4 5 3/3 10.1 ± 4.8 L3 (pp32) 5 5 0/3 6 4 0/3 Vector Control 2 3 0/3 3 1 0/3
[0158] [0158]
1
51
1
5785
DNA
Homo sapiens
CDS
(4453)..(5154)
1
aagctttcct gatctctaaa tcaaggtcag ctccctaagc tcttggctcc cgtactgaaa 60
ctttttctta tgtaactctc ataaacacat agcataatgt tttgcatgtt tttcttccct 120
atcagttgca agttccagca gagctgatat attttcattt cattcgctac tatagcccta 180
gagcctgaca tagtttctgg ctgtgaatgc tcaataaata tttgtttaat tgagtagaaa 240
cataaagtat ctatttcatt gaaggaaaga ataattagct acatttttct ttttcttgcc 300
ttaatatttg aggaatttgc ttatatgtca taataaaaaa gttaaagcct tatacattat 360
actaaggaat ttggacatta aattcaagct agcctttcta taaacaaaat actgaatttc 420
tgtccctaaa tttgttcctt ccctattctt ccccattgag atgacaccaa atccctctag 480
ctgctcaaac caagtacccg tatgttattc ttaattatct ctttaccttg cttctcatat 540
gcaatttgtt aacaagtcat cttcagtctg tatccattat tctccctttc cagaccacca 600
acatgtcttg actatactgc tacaatagcc tcccaactct tgtcctactt aaaattcatt 660
gtaaaaaatc agtcttggcc gggcacggtg gctcacacct ataatcccag cactttggga 720
gtcccaggcg ggcgggtcac gaggtcaaga gatggagacc atcatggcca acatggtgaa 780
accctgtctc tactataaat acaaaaaaat tatctgggtg tggtggcaca tgcctgtaat 840
cccaactact agggaggctg aggcaggaga atcgcttgaa cctgggaggc ggaggttgca 900
gtgagccgag atcgcaccat tgcactccag cctggcaaca gagcgagact ccatcccaaa 960
acaaaacaaa acaaaaccat gtaaaacatg tctgtaaaac atgtcagatt tcgtgttcag 1020
aagtcttaca tgtcttttca ttatgctaag ataaaaccca aatgcatttt cttggtttct 1080
aaagccaaga aaataagagt tgctttcagc aaccttgttt cttccgccat gcttttccct 1140
agctcactct ttttaggcaa gtcgacctga ttttctttct gttagtctgt ttctgcctcg 1200
tggtctggct ttctttctgt tagtctgttt ccacctcgtg gtcttggtcc tggctcttca 1260
ttctgcctgg aatgctctcc actccagatc cttactagat cttagctcag tcatcaccct 1320
cgcaggaaga tcttccaacc attcacctgc atacacctat ggctgctccc tagagaacat 1380
cattctgttt tcttcacttc ctagcactta ctgctttctg aaattatcta ctttgattgt 1440
ttatttcttt ctttactctt actaggatac ctgggtcatt aaaggaggga tatttctctc 1500
ttatttactg ttataaactt aatgcttagg ctgtagaagt tatacaatat ttgaagaata 1560
aatcgttaaa tgtataacat ttttgaagaa agataattgt gggatccatt tagtttgcaa 1620
acatttgatc tgtgtgttag acagaaggcc atggtaaagg acaaagacat attttatagg 1680
actgtaccct gaaaaataaa taaacttgaa ccagttatac aagacttatg tgcaggaaac 1740
aggtaccagt tatatttaga aatggtaaat caccttctaa gcataactca gagcacaata 1800
tattagaggg tagagagaga agtgcgtctt agatattggt aatcatatta ggactgacgc 1860
catccttgat ttttcttctg ggaaacagct caaaatgact atttaatgtt tacaatgata 1920
tcttgcatct tgccagtaaa taatataata gacactagga atccaaattg taagatgaac 1980
aagtctttat agagggagag ccaaatacac aataaataac acaaggtggt aaatgcagta 2040
atacaaacat acataccatg cataggagtg cagagaaggt gtgcttctcc gaatgcagtc 2100
acccagaaag tccttctgta gaaagggata tcttaaatgg tgcttaaagg aaaagtaacc 2160
aaaggcaact aaagattgca aggaggtccc aggaaaaagc aaaagaacca aaggtacata 2220
ggcacaaaag tagcctgcct tcctgggaac ttccaatagt ttgctggagc acacagttag 2280
aagtactgtg ccatgggagc aaagactgaa gacatatgca ggttcaaggg cacagagccc 2340
catatatgtc atgataagat attgggaagc cactggggag ctactgaaac tttaagcagg 2400
gaaataaaat tgtcatatct acaccttaga aatttgattt ttttctcttc ttttatcttc 2460
tcttctcctc tcttctctct ctctctctct ctctctctct gtgtgtgtgt gtgtgtgtgt 2520
gtgtgtgtgt gacagagtcc tgctctgtca cccaggctgg agtgtagtgg agtgatctcc 2580
gcttactgca gtctctgcct ctcaagcgat tccctgcctc agcctcccga gtagctggga 2640
ttacaggcgg gctctacaac agctggctaa cttttgtatt ttttggtaac aaccaggttt 2700
taccatgttg gccaggctgg tcttgaactc ctgacctcag gtgatctgcc tgccttggct 2760
ttccaaagtg ctgggattac aggcgtgagc caccctgcct ggtgtagaag tttgattttg 2820
atgtcagtgt ggtagatgaa tttgtgggaa gcaaaacaag atagagttca atgacagtga 2880
aaagtttatt gtataagcta tataaaagaa aatgttgaag gtttgaaatc cattagtggc 2940
agtaagggtg tacagaacga aactatttga gaagtacaca aggcaagtct tactttcaag 3000
gcagtttatg taagctcatt caattgtctc agtgttcttg ctatgtgtgg gttataggat 3060
ttggaacata tgatcaatct gagcacacat cagtaaactg aataggatta ttaaaatcca 3120
caagcatttt actagtggaa tctgtgatat tttctagcta ctcttgcttg ttttatttga 3180
atcttttgct catatcctat agtaaagatt tcaggaaata tatttttatt tgcctagaat 3240
tttagccttt tagttttttg aatctattgc tcatattctt atagtaagag tttcagggaa 3300
tgtatttcta tttgtctgga attttagcct ttcaggtttt tgagcccctc ttttgcttat 3360
gggacatagt atgagacaag atgaaatgat acttctattc ccaattcact gatggggaaa 3420
atgaagcaaa aaatgttatt cactcaaggc ttctgccatg tttcctggtg gaattacggc 3480
tcagacacaa atttcctaat gcctgtgctg ctaacttctc aatagaacac tatattaatt 3540
tatcttcttc ctgagtgttt ttccacaaat cccatagcct gtgaaaagat tgttttaggg 3600
aaatattatt tttaatatag catattttgt caatgtggga cataggacta gtacctgctg 3660
aaaaccatct catgatcctt gtgtaagaac taattcacac tagaaatact attttccttg 3720
ctcattaaaa acataaatgt ctcagaaagt aaaaaattat tcctctctaa ataaacatac 3780
atgccactca aattttattc ctctaccact tgccgtatct aaacctagtt agatactttg 3840
gttttaggta taatctgaca gaacagatac aaccaagatc acattgtgag tcagaagtgg 3900
aaaattcata attcatgatg ataccaataa aagatagatt tagcttttta caggatgttt 3960
ttggcatttt attctttcat ttgaggggag atctcaccaa aatatgtctt tcatggttca 4020
ttgtgttatt taatttctgt gatgcatatt ctcaggttac tttaaaccta gtctatagat 4080
tcaaagatat cccgtgtcag gtctctaaaa gtaaaaagaa aaatgggtac ttgtgaaggc 4140
tgattcacag taagtagtgt agaggggagt gccttgtgta ttcacaaatt atcaacgtga 4200
gcatcagata agattttctt tagtcacaca cacctacctt cttactagga agatccatat 4260
acttgaataa ttgttctgct tgacccaggt tacttatcag tccctttatt ataatatttg 4320
taaatattgg ggctcgagaa ccgagcggag ctggttgagt cttcaaagtc ctaaaacgtg 4380
cggccgtggg ttcgaggttt attgattgaa ttcggctggc acgagagcct ctgcagacag 4440
agagcgcgag ag atg gag atg ggc aga cgg att cat tca gag ctg cgg aac 4491
Met Glu Met Gly Arg Arg Ile His Ser Glu Leu Arg Asn
1 5 10
agg gcg ccc tct gat gtg aaa gaa ctt gcc ctg gac aac agt cgg tcg 4539
Arg Ala Pro Ser Asp Val Lys Glu Leu Ala Leu Asp Asn Ser Arg Ser
15 20 25
aat gaa ggc aaa ctc gaa gcc ctc aca gat gaa ttt gaa gaa ctg gaa 4587
Asn Glu Gly Lys Leu Glu Ala Leu Thr Asp Glu Phe Glu Glu Leu Glu
30 35 40 45
ttc tta agt aaa atc aac gga ggc ctc acc tca atc tca gac tta cca 4635
Phe Leu Ser Lys Ile Asn Gly Gly Leu Thr Ser Ile Ser Asp Leu Pro
50 55 60
aag tta aag ttg aga aag ctt gaa cta aga gtc tca ggg ggc ctg gaa 4683
Lys Leu Lys Leu Arg Lys Leu Glu Leu Arg Val Ser Gly Gly Leu Glu
65 70 75
gta ttg gca gaa aag tgt cca aac ctc acg cat cta tat tta agt ggc 4731
Val Leu Ala Glu Lys Cys Pro Asn Leu Thr His Leu Tyr Leu Ser Gly
80 85 90
aac aaa att aaa gac ctc agc aca ata gag cca ctg aaa cag tta gaa 4779
Asn Lys Ile Lys Asp Leu Ser Thr Ile Glu Pro Leu Lys Gln Leu Glu
95 100 105
aac ctc aag agc tta gac ctt ttc aat tgc gag gta acc aac ctg aac 4827
Asn Leu Lys Ser Leu Asp Leu Phe Asn Cys Glu Val Thr Asn Leu Asn
110 115 120 125
gac tac gga gaa aac gtg ttc aag ctt ctc ctg caa ctc aca tat ctc 4875
Asp Tyr Gly Glu Asn Val Phe Lys Leu Leu Leu Gln Leu Thr Tyr Leu
130 135 140
gac agc tgt tac tgg gac cac aag gag gcc cct tac tca gat att gag 4923
Asp Ser Cys Tyr Trp Asp His Lys Glu Ala Pro Tyr Ser Asp Ile Glu
145 150 155
gac cac gtg gag ggc ctg gat gac gag gag gag ggt gag cat gag gag 4971
Asp His Val Glu Gly Leu Asp Asp Glu Glu Glu Gly Glu His Glu Glu
160 165 170
gag tat gat gaa gat gct cag gta gtg gaa gat gag gag ggc gag gag 5019
Glu Tyr Asp Glu Asp Ala Gln Val Val Glu Asp Glu Glu Gly Glu Glu
175 180 185
gag gag gag gaa ggt gaa gag gag gac gtg agt gga ggg gac gag gag 5067
Glu Glu Glu Glu Gly Glu Glu Glu Asp Val Ser Gly Gly Asp Glu Glu
190 195 200 205
gat gaa gaa ggt tat aac gat gga gag gta gat ggc gag gaa gat gaa 5115
Asp Glu Glu Gly Tyr Asn Asp Gly Glu Val Asp Gly Glu Glu Asp Glu
210 215 220
gaa gag ctt ggt gaa gaa gaa agg ggt cag aag cga aaa tgagaacctg 5164
Glu Glu Leu Gly Glu Glu Glu Arg Gly Gln Lys Arg Lys
225 230
aagatgaggg agaagatgat gactaagtag aataacctat tttgaaaaat tcctattgtg 5224
atttgactgt ttttacccat atcccctccc ccctccaatc ctgccccctg aaacttactt 5284
ttttctgatt gtaacattgc tgtgggaatg agacgggaaa agtgtactgg gggttgtgga 5344
gggagggagg gcaggaggcg gtggactaaa atactatttt tactgccaaa taaaataata 5404
tttgtaaata ttaactggga tactagcttt gtagaatgat tactattaat tattctctct 5464
ctctttttat ttttttacac attctattct tttaagtata gtccttttag tccaaggaaa 5524
aggcactaca atccacttat taatgcttgc tactgtgttc aagtaaaata agctccagga 5584
tttaacaaaa agaggaaaga aaatatttac aatgaaaatg ttgctaaaaa tttaaaacaa 5644
attacagtaa atgtattgtt aaagcaaatt ctatttttaa aatttattaa taaggaaata 5704
atttgctaaa gcaaattttt ggaaaaataa taatgcactt tatacttgat tttatttatt 5764
aaaacaatga tttataagct t 5785
2
234
PRT
Homo sapiens
2
Met Glu Met Gly Arg Arg Ile His Ser Glu Leu Arg Asn Arg Ala Pro
1 5 10 15
Ser Asp Val Lys Glu Leu Ala Leu Asp Asn Ser Arg Ser Asn Glu Gly
20 25 30
Lys Leu Glu Ala Leu Thr Asp Glu Phe Glu Glu Leu Glu Phe Leu Ser
35 40 45
Lys Ile Asn Gly Gly Leu Thr Ser Ile Ser Asp Leu Pro Lys Leu Lys
50 55 60
Leu Arg Lys Leu Glu Leu Arg Val Ser Gly Gly Leu Glu Val Leu Ala
65 70 75 80
Glu Lys Cys Pro Asn Leu Thr His Leu Tyr Leu Ser Gly Asn Lys Ile
85 90 95
Lys Asp Leu Ser Thr Ile Glu Pro Leu Lys Gln Leu Glu Asn Leu Lys
100 105 110
Ser Leu Asp Leu Phe Asn Cys Glu Val Thr Asn Leu Asn Asp Tyr Gly
115 120 125
Glu Asn Val Phe Lys Leu Leu Leu Gln Leu Thr Tyr Leu Asp Ser Cys
130 135 140
Tyr Trp Asp His Lys Glu Ala Pro Tyr Ser Asp Ile Glu Asp His Val
145 150 155 160
Glu Gly Leu Asp Asp Glu Glu Glu Gly Glu His Glu Glu Glu Tyr Asp
165 170 175
Glu Asp Ala Gln Val Val Glu Asp Glu Glu Gly Glu Glu Glu Glu Glu
180 185 190
Glu Gly Glu Glu Glu Asp Val Ser Gly Gly Asp Glu Glu Asp Glu Glu
195 200 205
Gly Tyr Asn Asp Gly Glu Val Asp Gly Glu Glu Asp Glu Glu Glu Leu
210 215 220
Gly Glu Glu Glu Arg Gly Gln Lys Arg Lys
225 230
3
889
DNA
Homo sapiens
3
gggttcgagg tttattgatt gaattcggct ggcacgagag cctctgcaga cagagagcgc 60
gagagatgga gatgggcaga cggattcatt cagagctgcg gaacagggcg ccctctgatg 120
tgaaagaact tgccctggac aacagtcggt cgaatgaagg caaactcgaa gccctcacag 180
atgaatttga agaactggaa ttcttaagta aaatcaacgg aggcctcacc tcaatctcag 240
acttaccaaa gttaaagttg agaaagcttg aactaagagt ctcagggggc ctggaagtat 300
tggcagaaaa gtgtccaaac ctcacgcatc tatatttaag tggcaacaaa attaaagacc 360
tcagcacaat agagccactg aaacagttag aaaacctcaa gagcttagac cttttcaatt 420
gcgaggtaac caacctgaac gactacggag aaaacgtgtt caagcttctc ctgcaactca 480
catatctcga cagctgttac tgggaccaca aggaggcccc ttactcagat attgaggacc 540
acgtggaggg cctggatgac gaggaggagg gtgagcatga ggaggagtat gatgaagatg 600
ctcaggtagt ggaagatgag gagggcgagg aggaggagga ggaaggtgaa gaggaggacg 660
tgagtggagg ggacgaggag gatgaagaag gttataacga tggagaggta gatggcgagg 720
aagatgaaga agagcttggt gaagaagaaa ggggtcagaa gcgaaaatga gaacctgaag 780
atgagggaga agatgatgac taagtagaat aacctatttt gaaaaattcc tattgtgatt 840
tgactgtttt tacccatatc ccctcccccc tccaatcctg ccccctgaa 889
4
907
DNA
Homo sapiens
4
gggttcgggg tttattgatt gaattcggct ggcgcgggag cctctgcaga gagagagcgc 60
gagagatgga gatgggcaga cggattcatt tagagctgcg gaacgggacg ccctctgatg 120
tgaaagaact tgtcctggac aacagtcggt cgaatgaagg caaactcgaa ggcctcacag 180
atgaatttga agaactggaa ttcttaagta caatcaacgt aggcctcacc tcaatcgcaa 240
acttaccaaa gttaaacaaa cttaagaagc ttgaactaag cagtaacaga gcctcagtgg 300
gcctagaagt attggcagaa aagtgtccaa acctcataca tctaaattta agtggcaaca 360
aaattaaaga cctcagcaca atagagcccc tgaaaaagtt agaaaacctc gagagcttag 420
accttttcac ttgcgaggta accaacctga acaactactg agagaagatg ttcaagctcc 480
tcctgcaact cacatatctc aacggctgtg acccggatga caaggaggcc cctaactcgg 540
atggtgaggg ctttgtggag tgcctggatg acaaggagga ggatgaggat gaggaggagt 600
atgatgaaga tgctcaggta atggaagatg aggaggacga ggatgaggag gaggaacgtg 660
aagaggagga cgtgagtgga gacgaggagg agaaggatga aggttataac aatggagagg 720
tagatgatga ggaagatgaa gaagagcttg gtgaagaaga aaggggtcag aagcgaaaat 780
aagaaactga agatgaggga gaagacgatg cctaagtgga ataatctatt ttgaaaaatt 840
ccttttgtga ttttactgtt tttagccgta ccccctctcc ccccccactc taatcctgcc 900
ccctgaa 907
5
130
PRT
Homo sapiens
5
Met Glu Met Gly Arg Arg Ile His Leu Glu Leu Arg Asn Gly Thr Pro
1 5 10 15
Ser Asp Val Lys Glu Leu Val Leu Asp Asn Ser Arg Ser Asn Glu Gly
20 25 30
Lys Leu Glu Gly Leu Thr Asp Glu Phe Glu Glu Leu Glu Phe Leu Ser
35 40 45
Thr Ile Asn Val Gly Leu Thr Ser Ile Ala Asn Leu Pro Lys Leu Asn
50 55 60
Lys Leu Lys Lys Leu Glu Leu Ser Ser Asn Arg Ala Ser Val Gly Leu
65 70 75 80
Glu Val Leu Ala Glu Lys Cys Pro Asn Leu Ile His Leu Asn Leu Ser
85 90 95
Gly Asn Lys Ile Lys Asp Leu Ser Thr Ile Glu Pro Leu Lys Lys Leu
100 105 110
Glu Asn Leu Glu Ser Leu Asp Leu Phe Thr Cys Glu Val Thr Asn Leu
115 120 125
Asn Asn
130
6
907
DNA
Homo sapiens
6
gggttcgggg tttattgatt gaattcggct ggcacgagag cctctgcaga cagagagcgc 60
gagagacgga gatgggcaga cggattcatc tagagctgcg gaacagggcg ccctctgatg 120
tgaaagaact tgccctggac aacagtcggt cgaatgaagg caaactcgaa gccctcacag 180
atgaatttga agaactggaa ttcttaagta aaatcaacgg aggcctcacc tcaatctcag 240
acttaccaaa gttaaacaag ttgagaaagc ttgaactaag cagtaacaga gtctcagggg 300
gcctggaagt attggcagaa aagtgtccaa acctcacgca tctatattta agtggcaaca 360
aaattaaaga cctcagcaca atagagccac tgaaacagtt agaaaacctc aagagcttag 420
accttttcaa ttgcgaggta accaacctga acgactacgg agaaaacgtg ttcaagcttc 480
tcctgcaact cacatatctc gacagctgtt actgggacca caaggaggcc ccttactcag 540
atattgaggc ccacgtggag ggcctggatg acgaggagga gggtgagcat gaggaggagt 600
atgatgaaga tgctcaggta gtggaagatg aggagggcga ggaggaggag gaggaaggtg 660
aagaggagga cgtgagtgga ggggacgagg aggatgaaga aggttataac gatggagagg 720
tagatggcga ggaagatgaa gaagagcttg gtgaagaaga aaggggtcag aagcgaaaat 780
gagaacctga agatgaggga gaagatgatg actaagtaga ataacctatt ttgaaaaatt 840
cctattgtga tttgactgtt tttacccata tcccctctcc cccccccctc taatcctgcc 900
ccctgaa 907
7
905
DNA
Homo sapiens
CDS
(64)..(453)
7
gggttcgggg tttattggtt gaattccgct ggctcaggag cctctgcaga gaaagcgtga 60
gag atg gag atg ggc aaa tgg att cat tta gag ctg cgg aac agg acg 108
Met Glu Met Gly Lys Trp Ile His Leu Glu Leu Arg Asn Arg Thr
1 5 10 15
ccc tcc gat gtg aaa gaa ctt ttc ctg gac aac agt cag tca aat gaa 156
Pro Ser Asp Val Lys Glu Leu Phe Leu Asp Asn Ser Gln Ser Asn Glu
20 25 30
ggc aaa ttg gaa ggc ctc aca gat gaa ttt gaa gaa ctg gaa tta tta 204
Gly Lys Leu Glu Gly Leu Thr Asp Glu Phe Glu Glu Leu Glu Leu Leu
35 40 45
aat aca atc aac ata ggc ctc acc tca att gca aac ttg cca aag tta 252
Asn Thr Ile Asn Ile Gly Leu Thr Ser Ile Ala Asn Leu Pro Lys Leu
50 55 60
aac aaa ctt aag aag ctt gaa cta agc agt aac aga gcc tca gtg ggc 300
Asn Lys Leu Lys Lys Leu Glu Leu Ser Ser Asn Arg Ala Ser Val Gly
65 70 75
cta gaa gta ttg gca gaa aag tgt cca aac ctc ata cat cta aat tta 348
Leu Glu Val Leu Ala Glu Lys Cys Pro Asn Leu Ile His Leu Asn Leu
80 85 90 95
agt ggc aac aaa att aaa gac ctc agc aca ata gag ccc ctg aaa aag 396
Ser Gly Asn Lys Ile Lys Asp Leu Ser Thr Ile Glu Pro Leu Lys Lys
100 105 110
tta gaa aac ctc gag agc tta gac ctt ttc act tgc gag gta acc aac 444
Leu Glu Asn Leu Glu Ser Leu Asp Leu Phe Thr Cys Glu Val Thr Asn
115 120 125
ctg aac aac tactgagaaa agatgttcaa gctcctcctg caactcacat 493
Leu Asn Asn
130
atctcaacgg ctgtgacccg gatgacaagg aggcccctaa ctcggatggt gagggctatg 553
tggagtgcct ggatgacaag gaggaggatg aggatgagga ggagtatgat gaagatgctc 613
aggtaatgga agatgaggag gacgaggatg aggaggagga acgtgaagag gaggacgtga 673
gtggagacga ggaggagaag gatgaaggtt ataacaatgg agaggtagat gatgaggaag 733
atgaagaaga gcttggtgaa gaagaaaggg gtcagaagcg aaaataagaa actgaagatg 793
agggagaaga cgatgcctaa gtggaataat ctattttgaa aaattccttt tgtgatttta 853
ctgtttttag ccgtatcccc tctccccccc cactctaatc ctgccccctg aa 905
8
130
PRT
Homo sapiens
8
Met Glu Met Gly Lys Trp Ile His Leu Glu Leu Arg Asn Arg Thr Pro
1 5 10 15
Ser Asp Val Lys Glu Leu Phe Leu Asp Asn Ser Gln Ser Asn Glu Gly
20 25 30
Lys Leu Glu Gly Leu Thr Asp Glu Phe Glu Glu Leu Glu Leu Leu Asn
35 40 45
Thr Ile Asn Ile Gly Leu Thr Ser Ile Ala Asn Leu Pro Lys Leu Asn
50 55 60
Lys Leu Lys Lys Leu Glu Leu Ser Ser Asn Arg Ala Ser Val Gly Leu
65 70 75 80
Glu Val Leu Ala Glu Lys Cys Pro Asn Leu Ile His Leu Asn Leu Ser
85 90 95
Gly Asn Lys Ile Lys Asp Leu Ser Thr Ile Glu Pro Leu Lys Lys Leu
100 105 110
Glu Asn Leu Glu Ser Leu Asp Leu Phe Thr Cys Glu Val Thr Asn Leu
115 120 125
Asn Asn
130
9
907
DNA
Homo sapiens
CDS
(66)..(812)
9
gggttcgggg tttattgatt gaattccgcc ggcgcgggag cctctgcaga gagagagcgc 60
gagag atg gag atg ggc aga cgg att cat tta gag ctg cgg aac agg acg 110
Met Glu Met Gly Arg Arg Ile His Leu Glu Leu Arg Asn Arg Thr
1 5 10 15
ccc tct gat gtg aaa gaa ctt gtc ctg gac aac agt cgg tcg aat gaa 158
Pro Ser Asp Val Lys Glu Leu Val Leu Asp Asn Ser Arg Ser Asn Glu
20 25 30
ggc aaa ctc gaa ggc ctc aca gat gaa ttt gaa gaa ctg gaa ttc tta 206
Gly Lys Leu Glu Gly Leu Thr Asp Glu Phe Glu Glu Leu Glu Phe Leu
35 40 45
agt aca atc aac gta ggc ctc acc tca atc gca aac ttg cca aag tta 254
Ser Thr Ile Asn Val Gly Leu Thr Ser Ile Ala Asn Leu Pro Lys Leu
50 55 60
aac aaa ctt aag aag ctt gaa cta agc agt aac aga gcc tca gtg ggc 302
Asn Lys Leu Lys Lys Leu Glu Leu Ser Ser Asn Arg Ala Ser Val Gly
65 70 75
cta gaa gta ttg gca gaa aag tgt cca aac ctc ata cat cta aat tta 350
Leu Glu Val Leu Ala Glu Lys Cys Pro Asn Leu Ile His Leu Asn Leu
80 85 90 95
agt ggc aac aaa att aaa gac ctc agc aca ata gag cca ctg aaa aag 398
Ser Gly Asn Lys Ile Lys Asp Leu Ser Thr Ile Glu Pro Leu Lys Lys
100 105 110
tta gaa aac ctc aag agc tta gac ctt tcc aat tgc gag gta acc aac 446
Leu Glu Asn Leu Lys Ser Leu Asp Leu Ser Asn Cys Glu Val Thr Asn
115 120 125
ctg aac gac tac cga gaa aat gtg ttc aag ctc ctc ccg caa ctc aca 494
Leu Asn Asp Tyr Arg Glu Asn Val Phe Lys Leu Leu Pro Gln Leu Thr
130 135 140
tat ctc gac ggc tat gac cgg gac gac aag gag gcc cct gac tcg gat 542
Tyr Leu Asp Gly Tyr Asp Arg Asp Asp Lys Glu Ala Pro Asp Ser Asp
145 150 155
gct gag ggc tac gtg gag ggc ctg gat gat gag gag gag gat gag gat 590
Ala Glu Gly Tyr Val Glu Gly Leu Asp Asp Glu Glu Glu Asp Glu Asp
160 165 170 175
gag gag gag tat gat gaa gat gct cag gta gta gaa gat gag gag gac 638
Glu Glu Glu Tyr Asp Glu Asp Ala Gln Val Val Glu Asp Glu Glu Asp
180 185 190
gag gat gag gag gag gaa ggt gaa gag gag gac gtg agt gga gag gag 686
Glu Asp Glu Glu Glu Glu Gly Glu Glu Glu Asp Val Ser Gly Glu Glu
195 200 205
gag gag gat gaa gaa ggt tat aac gat gga gag gta gat gac gag gaa 734
Glu Glu Asp Glu Glu Gly Tyr Asn Asp Gly Glu Val Asp Asp Glu Glu
210 215 220
gat gaa gaa gag ctt ggt gaa gaa gaa agg ggt cag aag cga aaa cga 782
Asp Glu Glu Glu Leu Gly Glu Glu Glu Arg Gly Gln Lys Arg Lys Arg
225 230 235
gaa cct gaa gat gag gga gaa gat gat gac taagtggaat aacctatttt 832
Glu Pro Glu Asp Glu Gly Glu Asp Asp Asp
240 245
gaaaaattcc tattgtgatt tgactgtttt tacccatatc ccctctcccc cccccctcta 892
atcctgcccc ctgaa 907
10
249
PRT
Homo sapiens
10
Met Glu Met Gly Arg Arg Ile His Leu Glu Leu Arg Asn Arg Thr Pro
1 5 10 15
Ser Asp Val Lys Glu Leu Val Leu Asp Asn Ser Arg Ser Asn Glu Gly
20 25 30
Lys Leu Glu Gly Leu Thr Asp Glu Phe Glu Glu Leu Glu Phe Leu Ser
35 40 45
Thr Ile Asn Val Gly Leu Thr Ser Ile Ala Asn Leu Pro Lys Leu Asn
50 55 60
Lys Leu Lys Lys Leu Glu Leu Ser Ser Asn Arg Ala Ser Val Gly Leu
65 70 75 80
Glu Val Leu Ala Glu Lys Cys Pro Asn Leu Ile His Leu Asn Leu Ser
85 90 95
Gly Asn Lys Ile Lys Asp Leu Ser Thr Ile Glu Pro Leu Lys Lys Leu
100 105 110
Glu Asn Leu Lys Ser Leu Asp Leu Ser Asn Cys Glu Val Thr Asn Leu
115 120 125
Asn Asp Tyr Arg Glu Asn Val Phe Lys Leu Leu Pro Gln Leu Thr Tyr
130 135 140
Leu Asp Gly Tyr Asp Arg Asp Asp Lys Glu Ala Pro Asp Ser Asp Ala
145 150 155 160
Glu Gly Tyr Val Glu Gly Leu Asp Asp Glu Glu Glu Asp Glu Asp Glu
165 170 175
Glu Glu Tyr Asp Glu Asp Ala Gln Val Val Glu Asp Glu Glu Asp Glu
180 185 190
Asp Glu Glu Glu Glu Gly Glu Glu Glu Asp Val Ser Gly Glu Glu Glu
195 200 205
Glu Asp Glu Glu Gly Tyr Asn Asp Gly Glu Val Asp Asp Glu Glu Asp
210 215 220
Glu Glu Glu Leu Gly Glu Glu Glu Arg Gly Gln Lys Arg Lys Arg Glu
225 230 235 240
Pro Glu Asp Glu Gly Glu Asp Asp Asp
245
11
905
DNA
Homo sapiens
CDS
(64)..(810)
11
gggttcgggg tttattggtt gaattccgct ggctcaggag cctctgcaga gaaagcgtga 60
gag atg gag atg ggc aaa tgg att cat tta gag ctg cgg aac agg acg 108
Met Glu Met Gly Lys Trp Ile His Leu Glu Leu Arg Asn Arg Thr
1 5 10 15
ccc tcc gat gtg aaa gaa ctt ttc ctg gac aac agt cag tca aat gaa 156
Pro Ser Asp Val Lys Glu Leu Phe Leu Asp Asn Ser Gln Ser Asn Glu
20 25 30
ggc aaa ttg gaa ggc ctc aca gat gaa ttt gaa gaa ctg gaa tta tta 204
Gly Lys Leu Glu Gly Leu Thr Asp Glu Phe Glu Glu Leu Glu Leu Leu
35 40 45
aat aca atc aac ata ggc ctc acc tca att gca aac ttg cca aag tta 252
Asn Thr Ile Asn Ile Gly Leu Thr Ser Ile Ala Asn Leu Pro Lys Leu
50 55 60
aac aaa ctt aag aag ctt gaa cta agc agt aac aga gcc tca gtg ggc 300
Asn Lys Leu Lys Lys Leu Glu Leu Ser Ser Asn Arg Ala Ser Val Gly
65 70 75
cta gaa gta ttg gca gaa aag tgt cca aac ctc ata cat cta aat tta 348
Leu Glu Val Leu Ala Glu Lys Cys Pro Asn Leu Ile His Leu Asn Leu
80 85 90 95
agt ggc aac aaa att aaa gac ctc agc aca ata gag ccc ctg aaa aag 396
Ser Gly Asn Lys Ile Lys Asp Leu Ser Thr Ile Glu Pro Leu Lys Lys
100 105 110
tta gaa aac ctc gag agc tta gac ctt ttc act tgc gag gta acc aac 444
Leu Glu Asn Leu Glu Ser Leu Asp Leu Phe Thr Cys Glu Val Thr Asn
115 120 125
ctg aac aac tac cga gaa aat gtg ttc aag ctc ctc ccg caa ctc aca 492
Leu Asn Asn Tyr Arg Glu Asn Val Phe Lys Leu Leu Pro Gln Leu Thr
130 135 140
tat ctc gac ggc tat gac cgg gac gac aag gag gcc cct gac tcg gat 540
Tyr Leu Asp Gly Tyr Asp Arg Asp Asp Lys Glu Ala Pro Asp Ser Asp
145 150 155
gct gag ggc tac gtg gag ggc ctg gat gat gag gag gag gat gag gat 588
Ala Glu Gly Tyr Val Glu Gly Leu Asp Asp Glu Glu Glu Asp Glu Asp
160 165 170 175
gag gag gag tat gat gaa gat gct cag gta gtg gaa gac gag gag gac 636
Glu Glu Glu Tyr Asp Glu Asp Ala Gln Val Val Glu Asp Glu Glu Asp
180 185 190
gag gat gag gag gag gaa ggt gaa gag gag gac gtg agt gga gag gag 684
Glu Asp Glu Glu Glu Glu Gly Glu Glu Glu Asp Val Ser Gly Glu Glu
195 200 205
gag gag gat gaa gaa ggt tat aac gat gga gag gta gat gac gag gaa 732
Glu Glu Asp Glu Glu Gly Tyr Asn Asp Gly Glu Val Asp Asp Glu Glu
210 215 220
gat gaa gaa gag ctt ggt gaa gaa gaa agg ggt cag aag cga aaa cga 780
Asp Glu Glu Glu Leu Gly Glu Glu Glu Arg Gly Gln Lys Arg Lys Arg
225 230 235
gaa cct gaa gat gag gga gaa gat gat gac taagtggaat aacctatttt 830
Glu Pro Glu Asp Glu Gly Glu Asp Asp Asp
240 245
gaaaaattcc tattgtgatt tgactgtttt tacccatatc ccctctcccc cccccctcta 890
atcctgcccc ctgaa 905
12
249
PRT
Homo sapiens
12
Met Glu Met Gly Lys Trp Ile His Leu Glu Leu Arg Asn Arg Thr Pro
1 5 10 15
Ser Asp Val Lys Glu Leu Phe Leu Asp Asn Ser Gln Ser Asn Glu Gly
20 25 30
Lys Leu Glu Gly Leu Thr Asp Glu Phe Glu Glu Leu Glu Leu Leu Asn
35 40 45
Thr Ile Asn Ile Gly Leu Thr Ser Ile Ala Asn Leu Pro Lys Leu Asn
50 55 60
Lys Leu Lys Lys Leu Glu Leu Ser Ser Asn Arg Ala Ser Val Gly Leu
65 70 75 80
Glu Val Leu Ala Glu Lys Cys Pro Asn Leu Ile His Leu Asn Leu Ser
85 90 95
Gly Asn Lys Ile Lys Asp Leu Ser Thr Ile Glu Pro Leu Lys Lys Leu
100 105 110
Glu Asn Leu Glu Ser Leu Asp Leu Phe Thr Cys Glu Val Thr Asn Leu
115 120 125
Asn Asn Tyr Arg Glu Asn Val Phe Lys Leu Leu Pro Gln Leu Thr Tyr
130 135 140
Leu Asp Gly Tyr Asp Arg Asp Asp Lys Glu Ala Pro Asp Ser Asp Ala
145 150 155 160
Glu Gly Tyr Val Glu Gly Leu Asp Asp Glu Glu Glu Asp Glu Asp Glu
165 170 175
Glu Glu Tyr Asp Glu Asp Ala Gln Val Val Glu Asp Glu Glu Asp Glu
180 185 190
Asp Glu Glu Glu Glu Gly Glu Glu Glu Asp Val Ser Gly Glu Glu Glu
195 200 205
Glu Asp Glu Glu Gly Tyr Asn Asp Gly Glu Val Asp Asp Glu Glu Asp
210 215 220
Glu Glu Glu Leu Gly Glu Glu Glu Arg Gly Gln Lys Arg Lys Arg Glu
225 230 235 240
Pro Glu Asp Glu Gly Glu Asp Asp Asp
245
13
907
DNA
Homo sapiens
CDS
(66)..(812)
13
gggttcgggg tttattgatt gaattccgcc ggcgcgggag cctctgcaga gagagagcgc 60
gagag atg gag atg ggc aga cgg att cat tta gag ctg cgg aac agg acg 110
Met Glu Met Gly Arg Arg Ile His Leu Glu Leu Arg Asn Arg Thr
1 5 10 15
ccc tct gat gtg aaa gaa ctt gtc ctg gac aac agt cgg tcg aat gaa 158
Pro Ser Asp Val Lys Glu Leu Val Leu Asp Asn Ser Arg Ser Asn Glu
20 25 30
ggc aaa ctc gaa ggc ctc aca gat gaa ttt gaa gaa ctg gaa ttc tta 206
Gly Lys Leu Glu Gly Leu Thr Asp Glu Phe Glu Glu Leu Glu Phe Leu
35 40 45
agt aca atc aac gta ggc ctc acc tca atc gca aac tta cca aag tta 254
Ser Thr Ile Asn Val Gly Leu Thr Ser Ile Ala Asn Leu Pro Lys Leu
50 55 60
aac aaa ctt aag aag ctt gaa cta agc gat aac aga gtc tca ggg ggc 302
Asn Lys Leu Lys Lys Leu Glu Leu Ser Asp Asn Arg Val Ser Gly Gly
65 70 75
ctg gaa gta ttg gca gaa aag tgt ccg aac ctc acg cat cta aat tta 350
Leu Glu Val Leu Ala Glu Lys Cys Pro Asn Leu Thr His Leu Asn Leu
80 85 90 95
agt ggc aac aaa att aaa gac ctc agc aca ata gag cca ctg aaa aag 398
Ser Gly Asn Lys Ile Lys Asp Leu Ser Thr Ile Glu Pro Leu Lys Lys
100 105 110
tta gaa aac ctc aag agc tta gac ctt ttc aat tgc gag gta acc aac 446
Leu Glu Asn Leu Lys Ser Leu Asp Leu Phe Asn Cys Glu Val Thr Asn
115 120 125
ctg aac gac tac cga gaa aat gtg ttc aag ctc ctc ccg caa ctc aca 494
Leu Asn Asp Tyr Arg Glu Asn Val Phe Lys Leu Leu Pro Gln Leu Thr
130 135 140
tat ctc gac ggc tat gac cgg gac gac aag gag gcc cct gac tcg gat 542
Tyr Leu Asp Gly Tyr Asp Arg Asp Asp Lys Glu Ala Pro Asp Ser Asp
145 150 155
gct gag ggc tac gtg gag ggc ctg gat gat gag gag gag gat gag gat 590
Ala Glu Gly Tyr Val Glu Gly Leu Asp Asp Glu Glu Glu Asp Glu Asp
160 165 170 175
gag gag gag tat gat gaa gat gct cag gta gtg gaa gac gag gag gac 638
Glu Glu Glu Tyr Asp Glu Asp Ala Gln Val Val Glu Asp Glu Glu Asp
180 185 190
gag gat gag gag gag gaa ggt gaa gag gag gac gtg agt gga gag gag 686
Glu Asp Glu Glu Glu Glu Gly Glu Glu Glu Asp Val Ser Gly Glu Glu
195 200 205
gag gag gat gaa gaa ggt tat aac gat gga gag gta gat gac gag gaa 734
Glu Glu Asp Glu Glu Gly Tyr Asn Asp Gly Glu Val Asp Asp Glu Glu
210 215 220
gat gaa gaa gag ctt ggt gaa gaa gaa agg ggt cag aag cga aaa cga 782
Asp Glu Glu Glu Leu Gly Glu Glu Glu Arg Gly Gln Lys Arg Lys Arg
225 230 235
gaa cct gaa gat gag gga gaa gat gat gac taagtggaat aacctatttt 832
Glu Pro Glu Asp Glu Gly Glu Asp Asp Asp
240 245
gaaaaattcc tattgtgatt tgactgtttt tacccatatc ccctctcccc cccccctcta 892
atcctgcccc ctgaa 907
14
249
PRT
Homo sapiens
14
Met Glu Met Gly Arg Arg Ile His Leu Glu Leu Arg Asn Arg Thr Pro
1 5 10 15
Ser Asp Val Lys Glu Leu Val Leu Asp Asn Ser Arg Ser Asn Glu Gly
20 25 30
Lys Leu Glu Gly Leu Thr Asp Glu Phe Glu Glu Leu Glu Phe Leu Ser
35 40 45
Thr Ile Asn Val Gly Leu Thr Ser Ile Ala Asn Leu Pro Lys Leu Asn
50 55 60
Lys Leu Lys Lys Leu Glu Leu Ser Asp Asn Arg Val Ser Gly Gly Leu
65 70 75 80
Glu Val Leu Ala Glu Lys Cys Pro Asn Leu Thr His Leu Asn Leu Ser
85 90 95
Gly Asn Lys Ile Lys Asp Leu Ser Thr Ile Glu Pro Leu Lys Lys Leu
100 105 110
Glu Asn Leu Lys Ser Leu Asp Leu Phe Asn Cys Glu Val Thr Asn Leu
115 120 125
Asn Asp Tyr Arg Glu Asn Val Phe Lys Leu Leu Pro Gln Leu Thr Tyr
130 135 140
Leu Asp Gly Tyr Asp Arg Asp Asp Lys Glu Ala Pro Asp Ser Asp Ala
145 150 155 160
Glu Gly Tyr Val Glu Gly Leu Asp Asp Glu Glu Glu Asp Glu Asp Glu
165 170 175
Glu Glu Tyr Asp Glu Asp Ala Gln Val Val Glu Asp Glu Glu Asp Glu
180 185 190
Asp Glu Glu Glu Glu Gly Glu Glu Glu Asp Val Ser Gly Glu Glu Glu
195 200 205
Glu Asp Glu Glu Gly Tyr Asn Asp Gly Glu Val Asp Asp Glu Glu Asp
210 215 220
Glu Glu Glu Leu Gly Glu Glu Glu Arg Gly Gln Lys Arg Lys Arg Glu
225 230 235 240
Pro Glu Asp Glu Gly Glu Asp Asp Asp
245
15
895
DNA
Homo sapiens
CDS
(66)..(767)
15
gggttcgggg tttattgatt gaattcggct ggcacgagag cctctgcaga cagagagcgc 60
gagag atg gag atg ggc aga cgg att cat tca gag ctg cgg aac agg gcg 110
Met Glu Met Gly Arg Arg Ile His Ser Glu Leu Arg Asn Arg Ala
1 5 10 15
ccc tct gat gtg aaa gaa ctt gcc ctg gac aac agt cgg tcg aat gaa 158
Pro Ser Asp Val Lys Glu Leu Ala Leu Asp Asn Ser Arg Ser Asn Glu
20 25 30
ggc aaa ctc gaa gcc ctc aca gat gaa ttt gaa gaa ctg gaa ttc tta 206
Gly Lys Leu Glu Ala Leu Thr Asp Glu Phe Glu Glu Leu Glu Phe Leu
35 40 45
agt aaa atc aac gga ggc ctc acc tca atc tca gac tta cca aag tta 254
Ser Lys Ile Asn Gly Gly Leu Thr Ser Ile Ser Asp Leu Pro Lys Leu
50 55 60
aag ttg aga aag ctt gaa cta aga gtc tca ggg ggc ctg gaa gta ttg 302
Lys Leu Arg Lys Leu Glu Leu Arg Val Ser Gly Gly Leu Glu Val Leu
65 70 75
gca gaa aag tgt cca aac ctc acg cat cta tat tta agt ggc aac aaa 350
Ala Glu Lys Cys Pro Asn Leu Thr His Leu Tyr Leu Ser Gly Asn Lys
80 85 90 95
att aaa gac ctc agc aca ata gag cca ctg aaa cag tta gaa aac ctc 398
Ile Lys Asp Leu Ser Thr Ile Glu Pro Leu Lys Gln Leu Glu Asn Leu
100 105 110
aag agc tta gac ctt ttc aat tgc gag gta acc aac ctg aac gac tac 446
Lys Ser Leu Asp Leu Phe Asn Cys Glu Val Thr Asn Leu Asn Asp Tyr
115 120 125
gga gaa aac gtg ttc aag ctt ctc ctg caa ctc aca tat ctc gac agc 494
Gly Glu Asn Val Phe Lys Leu Leu Leu Gln Leu Thr Tyr Leu Asp Ser
130 135 140
tgt tac tgg gac cac aag gag gcc cct tac tca gat att gag gac cac 542
Cys Tyr Trp Asp His Lys Glu Ala Pro Tyr Ser Asp Ile Glu Asp His
145 150 155
gtg gag ggc ctg gat gac gag gag gag ggt gag cat gag gag gag tat 590
Val Glu Gly Leu Asp Asp Glu Glu Glu Gly Glu His Glu Glu Glu Tyr
160 165 170 175
gat gaa gat gct cag gta gtg gaa gat gag gag ggc gag gag gag gag 638
Asp Glu Asp Ala Gln Val Val Glu Asp Glu Glu Gly Glu Glu Glu Glu
180 185 190
gag gaa ggt gaa gag gag gac gtg agt gga ggg gac ggg gag gat gaa 686
Glu Glu Gly Glu Glu Glu Asp Val Ser Gly Gly Asp Gly Glu Asp Glu
195 200 205
gaa ggt tat aac gat gga gag gta gat ggc gag gaa gat gaa gaa gag 734
Glu Gly Tyr Asn Asp Gly Glu Val Asp Gly Glu Glu Asp Glu Glu Glu
210 215 220
ctt ggt gaa gaa gaa agg ggt cag aag cga aaa tgagaacctg aagatgaggg 787
Leu Gly Glu Glu Glu Arg Gly Gln Lys Arg Lys
225 230
agaagatgat gactaagtag aataacctat tttgaaaaat tcctattgtg atttgactgt 847
ttttacccat atcccatctc ccccccccct ctaatcctgc cccctgaa 895
16
234
PRT
Homo sapiens
16
Met Glu Met Gly Arg Arg Ile His Ser Glu Leu Arg Asn Arg Ala Pro
1 5 10 15
Ser Asp Val Lys Glu Leu Ala Leu Asp Asn Ser Arg Ser Asn Glu Gly
20 25 30
Lys Leu Glu Ala Leu Thr Asp Glu Phe Glu Glu Leu Glu Phe Leu Ser
35 40 45
Lys Ile Asn Gly Gly Leu Thr Ser Ile Ser Asp Leu Pro Lys Leu Lys
50 55 60
Leu Arg Lys Leu Glu Leu Arg Val Ser Gly Gly Leu Glu Val Leu Ala
65 70 75 80
Glu Lys Cys Pro Asn Leu Thr His Leu Tyr Leu Ser Gly Asn Lys Ile
85 90 95
Lys Asp Leu Ser Thr Ile Glu Pro Leu Lys Gln Leu Glu Asn Leu Lys
100 105 110
Ser Leu Asp Leu Phe Asn Cys Glu Val Thr Asn Leu Asn Asp Tyr Gly
115 120 125
Glu Asn Val Phe Lys Leu Leu Leu Gln Leu Thr Tyr Leu Asp Ser Cys
130 135 140
Tyr Trp Asp His Lys Glu Ala Pro Tyr Ser Asp Ile Glu Asp His Val
145 150 155 160
Glu Gly Leu Asp Asp Glu Glu Glu Gly Glu His Glu Glu Glu Tyr Asp
165 170 175
Glu Asp Ala Gln Val Val Glu Asp Glu Glu Gly Glu Glu Glu Glu Glu
180 185 190
Glu Gly Glu Glu Glu Asp Val Ser Gly Gly Asp Gly Glu Asp Glu Glu
195 200 205
Gly Tyr Asn Asp Gly Glu Val Asp Gly Glu Glu Asp Glu Glu Glu Leu
210 215 220
Gly Glu Glu Glu Arg Gly Gln Lys Arg Lys
225 230
17
905
DNA
Homo sapiens
CDS
(64)..(453)
17
gggttcgggg tttattggtt gaattccgct ggctcgagag cctctggaga gaaagcgtga 60
gag atg gag atg ggc aaa tgg att cat tta gag ctg cgg aac agg acg 108
Met Glu Met Gly Lys Trp Ile His Leu Glu Leu Arg Asn Arg Thr
1 5 10 15
ccc tcc gat gtg aaa gaa ctt ttc ctg gac aac agt cag tca aat gaa 156
Pro Ser Asp Val Lys Glu Leu Phe Leu Asp Asn Ser Gln Ser Asn Glu
20 25 30
ggc aaa ttg gaa ggc ctc aca gat gaa ttt gag gaa ctg gaa tta tta 204
Gly Lys Leu Glu Gly Leu Thr Asp Glu Phe Glu Glu Leu Glu Leu Leu
35 40 45
aat aca atc aac ata ggc ctc acc tca att gca aac ttg cca aag tta 252
Asn Thr Ile Asn Ile Gly Leu Thr Ser Ile Ala Asn Leu Pro Lys Leu
50 55 60
aac aaa ctt aag aag ctt gaa cta agc agt aac aga gcc tca gtg ggc 300
Asn Lys Leu Lys Lys Leu Glu Leu Ser Ser Asn Arg Ala Ser Val Gly
65 70 75
cta gaa gta ttg gca gaa aag tgt cca aac ctc ata cat cta aat tta 348
Leu Glu Val Leu Ala Glu Lys Cys Pro Asn Leu Ile His Leu Asn Leu
80 85 90 95
agt ggc aac aaa att aaa gac ctc agc aca ata gag ccc ctg aaa aag 396
Ser Gly Asn Lys Ile Lys Asp Leu Ser Thr Ile Glu Pro Leu Lys Lys
100 105 110
tta gaa aac ctt gag agc tta gac ctt ttc act tgc gag gta acc aac 444
Leu Glu Asn Leu Glu Ser Leu Asp Leu Phe Thr Cys Glu Val Thr Asn
115 120 125
ctg aac aac tactgagaaa agatgttcaa gctcctcctg caactcacat 493
Leu Asn Asn
130
atctcaacgg ctgtgacccg gatgacaagg aggcccctaa ctcggatggt gagggctacg 553
tggagggcct ggacgatgag gaggaggatg aggatgagga ggagtatgat gaagatgctc 613
aggtagtgga agacgaggag gacgaggatg aggaggagga aggtgaagag gaggacgtga 673
gtggagagga ggaggaggat gaagaaggtt ataacgatgg agaggtagat gacgaggaag 733
atgaagaaga gcttggtgaa gaagaaaggg gtcagaagcg aaaacgagaa cctgaagatg 793
agggagaaga tgatgactaa gtggaataac ctattttgaa aaattcctat tgtgatttga 853
ctgtttttag ccgtatcccc tctccccccc cactctaatc ctgccccctg aa 905
18
130
PRT
Homo sapiens
18
Met Glu Met Gly Lys Trp Ile His Leu Glu Leu Arg Asn Arg Thr Pro
1 5 10 15
Ser Asp Val Lys Glu Leu Phe Leu Asp Asn Ser Gln Ser Asn Glu Gly
20 25 30
Lys Leu Glu Gly Leu Thr Asp Glu Phe Glu Glu Leu Glu Leu Leu Asn
35 40 45
Thr Ile Asn Ile Gly Leu Thr Ser Ile Ala Asn Leu Pro Lys Leu Asn
50 55 60
Lys Leu Lys Lys Leu Glu Leu Ser Ser Asn Arg Ala Ser Val Gly Leu
65 70 75 80
Glu Val Leu Ala Glu Lys Cys Pro Asn Leu Ile His Leu Asn Leu Ser
85 90 95
Gly Asn Lys Ile Lys Asp Leu Ser Thr Ile Glu Pro Leu Lys Lys Leu
100 105 110
Glu Asn Leu Glu Ser Leu Asp Leu Phe Thr Cys Glu Val Thr Asn Leu
115 120 125
Asn Asn
130
19
905
DNA
Homo sapiens
CDS
(64)..(453)
19
gggttcgggg tttattggtt gaattccgct ggctcaggag cctctgcaga gaaagcgtga 60
gag atg gag atg ggc aaa tgg att cat tta gag ctg cgg aac agg acg 108
Met Glu Met Gly Lys Trp Ile His Leu Glu Leu Arg Asn Arg Thr
1 5 10 15
ccc tcc gat gtg aaa gaa ctt ttc ctg gac aac agt cag tca aat gaa 156
Pro Ser Asp Val Lys Glu Leu Phe Leu Asp Asn Ser Gln Ser Asn Glu
20 25 30
ggc aaa ttg gaa ggc ctc aca gat gaa ttt gaa gaa ctg gaa tta tta 204
Gly Lys Leu Glu Gly Leu Thr Asp Glu Phe Glu Glu Leu Glu Leu Leu
35 40 45
aat aca atc aac ata ggc ctc acc tca att gca aac ttg cca aag tta 252
Asn Thr Ile Asn Ile Gly Leu Thr Ser Ile Ala Asn Leu Pro Lys Leu
50 55 60
aac aaa ctt aag aag ctt gaa cta agc agt aac aga gcc tca gtg ggc 300
Asn Lys Leu Lys Lys Leu Glu Leu Ser Ser Asn Arg Ala Ser Val Gly
65 70 75
cta gaa gta ttg gca gaa aag tgt cca aac ctc ata cat cta aat tta 348
Leu Glu Val Leu Ala Glu Lys Cys Pro Asn Leu Ile His Leu Asn Leu
80 85 90 95
agt ggc aac aaa att aaa gac ctc agc aca ata gag ccc ctg aaa aag 396
Ser Gly Asn Lys Ile Lys Asp Leu Ser Thr Ile Glu Pro Leu Lys Lys
100 105 110
tta gaa aac ctc gag agc tta gac ctt ttc act tgc gag gta acc aac 444
Leu Glu Asn Leu Glu Ser Leu Asp Leu Phe Thr Cys Glu Val Thr Asn
115 120 125
ctg aac aac tactgagaaa agatgttcaa gctcctcctg caactcacat 493
Leu Asn Asn
130
atctcaacgg ctgtgacccg gatgacaagg aggcccctaa ctcggatggt gagggctttg 553
tggagtgcct ggatgacaag gaggaggatg aggatgagga ggagtatgat gaagatgctc 613
aggtaatgga agatgaggag gacgaggatg aggaggagga acgtgaagag gaggacgtga 673
gtggagacga ggaggagaag gatgaaggtt ataacaatgg agaggtagat gatgaggaag 733
atgaagaaga gcttggtgaa gaagaaaggg gtcagaagcg aaaataagaa actgaagatg 793
agggagaaga cgatgcctaa gtggaataat ctattttgaa aaattccttt tgtgatttta 853
ctgtttttag ccgtatcccc tctccccccc cactctaatc ctgccccctg aa 905
20
130
PRT
Homo sapiens
20
Met Glu Met Gly Lys Trp Ile His Leu Glu Leu Arg Asn Arg Thr Pro
1 5 10 15
Ser Asp Val Lys Glu Leu Phe Leu Asp Asn Ser Gln Ser Asn Glu Gly
20 25 30
Lys Leu Glu Gly Leu Thr Asp Glu Phe Glu Glu Leu Glu Leu Leu Asn
35 40 45
Thr Ile Asn Ile Gly Leu Thr Ser Ile Ala Asn Leu Pro Lys Leu Asn
50 55 60
Lys Leu Lys Lys Leu Glu Leu Ser Ser Asn Arg Ala Ser Val Gly Leu
65 70 75 80
Glu Val Leu Ala Glu Lys Cys Pro Asn Leu Ile His Leu Asn Leu Ser
85 90 95
Gly Asn Lys Ile Lys Asp Leu Ser Thr Ile Glu Pro Leu Lys Lys Leu
100 105 110
Glu Asn Leu Glu Ser Leu Asp Leu Phe Thr Cys Glu Val Thr Asn Leu
115 120 125
Asn Asn
130
21
895
DNA
Homo sapiens
CDS
(66)..(767)
21
gggttcgggg tttattgatt gaattcggct ggcacgagag cctctgcaga cagagagcgc 60
gagag atg gag atg ggc aga cgg att cat tca gag ctg cgg aac agg gcg 110
Met Glu Met Gly Arg Arg Ile His Ser Glu Leu Arg Asn Arg Ala
1 5 10 15
ccc tct gat gtg aaa gaa ctt gtc ctg gac aac agt cgg tcg aat gaa 158
Pro Ser Asp Val Lys Glu Leu Val Leu Asp Asn Ser Arg Ser Asn Glu
20 25 30
ggc aaa ctc gaa gcc ctc aca gat gaa ttt gaa gaa ctg gaa ttc tta 206
Gly Lys Leu Glu Ala Leu Thr Asp Glu Phe Glu Glu Leu Glu Phe Leu
35 40 45
agt aaa atc aac gga ggc ctc acc tca atc tca gac tta cca aag tta 254
Ser Lys Ile Asn Gly Gly Leu Thr Ser Ile Ser Asp Leu Pro Lys Leu
50 55 60
aag ttg aga aag ctt gaa cta aaa gtc tca ggg ggc ctg gaa gta ttg 302
Lys Leu Arg Lys Leu Glu Leu Lys Val Ser Gly Gly Leu Glu Val Leu
65 70 75
gca gaa aag tgt cca aac ctc acg cat cta tat tta agt ggc aac aaa 350
Ala Glu Lys Cys Pro Asn Leu Thr His Leu Tyr Leu Ser Gly Asn Lys
80 85 90 95
att aaa gac ctc agc aca ata gag cca ctg aaa cag tta gaa aac ctc 398
Ile Lys Asp Leu Ser Thr Ile Glu Pro Leu Lys Gln Leu Glu Asn Leu
100 105 110
aag agc tta gac ctt ttc aat tgc gag gta acc aac ctg aac gac tac 446
Lys Ser Leu Asp Leu Phe Asn Cys Glu Val Thr Asn Leu Asn Asp Tyr
115 120 125
gga gaa aac gtg ttc aag ctt ctc ctg caa ctc aca tat ctc gac agc 494
Gly Glu Asn Val Phe Lys Leu Leu Leu Gln Leu Thr Tyr Leu Asp Ser
130 135 140
tgt tac tgg gac cac aag gag gcc cct tac tca gat att gag gac cac 542
Cys Tyr Trp Asp His Lys Glu Ala Pro Tyr Ser Asp Ile Glu Asp His
145 150 155
gtg gag ggc ctg gat gac gag gag gag ggt gag cat gag gag gag tat 590
Val Glu Gly Leu Asp Asp Glu Glu Glu Gly Glu His Glu Glu Glu Tyr
160 165 170 175
gat gaa gat gct cag gta gtg gaa gat gag gag ggc gag gag gag gag 638
Asp Glu Asp Ala Gln Val Val Glu Asp Glu Glu Gly Glu Glu Glu Glu
180 185 190
gag gaa ggt gaa gag gag gac gtg agt gga ggg gac gag gag gat gaa 686
Glu Glu Gly Glu Glu Glu Asp Val Ser Gly Gly Asp Glu Glu Asp Glu
195 200 205
gaa ggt tat aac gat gga gag gta gat ggc gag gaa gat gaa gaa gag 734
Glu Gly Tyr Asn Asp Gly Glu Val Asp Gly Glu Glu Asp Glu Glu Glu
210 215 220
ctt ggt gaa gaa gaa agg ggt cag aag cga aaa tgagaacctg aagatgaggg 787
Leu Gly Glu Glu Glu Arg Gly Gln Lys Arg Lys
225 230
agaagatgat gactaagtag aataacctat tttgaaaaat tcctattgtg atttgactgt 847
ttttacccat atcccccctc ccccccccct ctaatcctgc cccctgaa 895
22
234
PRT
Homo sapiens
22
Met Glu Met Gly Arg Arg Ile His Ser Glu Leu Arg Asn Arg Ala Pro
1 5 10 15
Ser Asp Val Lys Glu Leu Val Leu Asp Asn Ser Arg Ser Asn Glu Gly
20 25 30
Lys Leu Glu Ala Leu Thr Asp Glu Phe Glu Glu Leu Glu Phe Leu Ser
35 40 45
Lys Ile Asn Gly Gly Leu Thr Ser Ile Ser Asp Leu Pro Lys Leu Lys
50 55 60
Leu Arg Lys Leu Glu Leu Lys Val Ser Gly Gly Leu Glu Val Leu Ala
65 70 75 80
Glu Lys Cys Pro Asn Leu Thr His Leu Tyr Leu Ser Gly Asn Lys Ile
85 90 95
Lys Asp Leu Ser Thr Ile Glu Pro Leu Lys Gln Leu Glu Asn Leu Lys
100 105 110
Ser Leu Asp Leu Phe Asn Cys Glu Val Thr Asn Leu Asn Asp Tyr Gly
115 120 125
Glu Asn Val Phe Lys Leu Leu Leu Gln Leu Thr Tyr Leu Asp Ser Cys
130 135 140
Tyr Trp Asp His Lys Glu Ala Pro Tyr Ser Asp Ile Glu Asp His Val
145 150 155 160
Glu Gly Leu Asp Asp Glu Glu Glu Gly Glu His Glu Glu Glu Tyr Asp
165 170 175
Glu Asp Ala Gln Val Val Glu Asp Glu Glu Gly Glu Glu Glu Glu Glu
180 185 190
Glu Gly Glu Glu Glu Asp Val Ser Gly Gly Asp Glu Glu Asp Glu Glu
195 200 205
Gly Tyr Asn Asp Gly Glu Val Asp Gly Glu Glu Asp Glu Glu Glu Leu
210 215 220
Gly Glu Glu Glu Arg Gly Gln Lys Arg Lys
225 230
23
895
DNA
Homo sapiens
CDS
(66)..(767)
23
gggttcgggg tttattgatt gaattccgcc ggcgcgggag cctctgcaga gagggagcgc 60
gagag atg gag atg ggc aga cgg att cat tta gag ctg cgg aac agg acg 110
Met Glu Met Gly Arg Arg Ile His Leu Glu Leu Arg Asn Arg Thr
1 5 10 15
ccc tct gat gtg aaa gaa ctt gtc ctg gac aac agt cgg tcg aat gaa 158
Pro Ser Asp Val Lys Glu Leu Val Leu Asp Asn Ser Arg Ser Asn Glu
20 25 30
ggc aaa ctc gaa ggc ctc aca gat gaa ttt gaa gaa ctg gaa ttc tta 206
Gly Lys Leu Glu Gly Leu Thr Asp Glu Phe Glu Glu Leu Glu Phe Leu
35 40 45
agt aca atc aac gta ggc ctc acc tca atc gca aac tta cca aag tta 254
Ser Thr Ile Asn Val Gly Leu Thr Ser Ile Ala Asn Leu Pro Lys Leu
50 55 60
aag ttg aga aag ctt gaa cta aga gtc tca ggg ggc ctg gaa gta ttg 302
Lys Leu Arg Lys Leu Glu Leu Arg Val Ser Gly Gly Leu Glu Val Leu
65 70 75
gca gaa aag tgt cca aac ctc acg cac cta tat tta agt ggc aac aaa 350
Ala Glu Lys Cys Pro Asn Leu Thr His Leu Tyr Leu Ser Gly Asn Lys
80 85 90 95
att aaa gac ctc agc aca ata gag cca ctg aaa cag tta gaa aac ctc 398
Ile Lys Asp Leu Ser Thr Ile Glu Pro Leu Lys Gln Leu Glu Asn Leu
100 105 110
aag agc tta gac ctt ttc aat tgc gag gta acc aac ctg aac gac tac 446
Lys Ser Leu Asp Leu Phe Asn Cys Glu Val Thr Asn Leu Asn Asp Tyr
115 120 125
gga gaa aac gtg ttc aag ctt ctc ctg caa ctc aca tat ctc gac agc 494
Gly Glu Asn Val Phe Lys Leu Leu Leu Gln Leu Thr Tyr Leu Asp Ser
130 135 140
tgt tac tgg gac cac aag gag gcc cct tac tca gat att gag gac cac 542
Cys Tyr Trp Asp His Lys Glu Ala Pro Tyr Ser Asp Ile Glu Asp His
145 150 155
gtg gag ggc ctg gat gac gag gag gag ggt gag cat gag gag gag tat 590
Val Glu Gly Leu Asp Asp Glu Glu Glu Gly Glu His Glu Glu Glu Tyr
160 165 170 175
gat gaa gat gct cag gta gtg gaa gat gag gag ggc gag gag ggg gag 638
Asp Glu Asp Ala Gln Val Val Glu Asp Glu Glu Gly Glu Glu Gly Glu
180 185 190
gag gaa ggt gaa gag gag gac gtg agt gga ggg gac gag gag gat gaa 686
Glu Glu Gly Glu Glu Glu Asp Val Ser Gly Gly Asp Glu Glu Asp Glu
195 200 205
gaa ggt tat aac gat gga gag gta gat gac gag gaa gat gaa gaa gag 734
Glu Gly Tyr Asn Asp Gly Glu Val Asp Asp Glu Glu Asp Glu Glu Glu
210 215 220
ctt ggt gaa gaa gaa agg ggt cag aag cga aaa cgagaacctg aagatgaggg 787
Leu Gly Glu Glu Glu Arg Gly Gln Lys Arg Lys
225 230
agaagatgat gactaagtgg aataacctat tttgaaaaat tcctattgtg atttgactgt 847
ttttacccat atcccctctc ccccccccct ctaatcctgc cccctgaa 895
24
234
PRT
Homo sapiens
24
Met Glu Met Gly Arg Arg Ile His Leu Glu Leu Arg Asn Arg Thr Pro
1 5 10 15
Ser Asp Val Lys Glu Leu Val Leu Asp Asn Ser Arg Ser Asn Glu Gly
20 25 30
Lys Leu Glu Gly Leu Thr Asp Glu Phe Glu Glu Leu Glu Phe Leu Ser
35 40 45
Thr Ile Asn Val Gly Leu Thr Ser Ile Ala Asn Leu Pro Lys Leu Lys
50 55 60
Leu Arg Lys Leu Glu Leu Arg Val Ser Gly Gly Leu Glu Val Leu Ala
65 70 75 80
Glu Lys Cys Pro Asn Leu Thr His Leu Tyr Leu Ser Gly Asn Lys Ile
85 90 95
Lys Asp Leu Ser Thr Ile Glu Pro Leu Lys Gln Leu Glu Asn Leu Lys
100 105 110
Ser Leu Asp Leu Phe Asn Cys Glu Val Thr Asn Leu Asn Asp Tyr Gly
115 120 125
Glu Asn Val Phe Lys Leu Leu Leu Gln Leu Thr Tyr Leu Asp Ser Cys
130 135 140
Tyr Trp Asp His Lys Glu Ala Pro Tyr Ser Asp Ile Glu Asp His Val
145 150 155 160
Glu Gly Leu Asp Asp Glu Glu Glu Gly Glu His Glu Glu Glu Tyr Asp
165 170 175
Glu Asp Ala Gln Val Val Glu Asp Glu Glu Gly Glu Glu Gly Glu Glu
180 185 190
Glu Gly Glu Glu Glu Asp Val Ser Gly Gly Asp Glu Glu Asp Glu Glu
195 200 205
Gly Tyr Asn Asp Gly Glu Val Asp Asp Glu Glu Asp Glu Glu Glu Leu
210 215 220
Gly Glu Glu Glu Arg Gly Gln Lys Arg Lys
225 230
25
907
DNA
Homo sapiens
25
gggttcgggg tttattgatt gaattccgcc ggcgcgggag cctctgcaga gagagagcgc 60
gagagatgga gatgggcaga cggattcatt tagagctgcg gaacaggacg ccctctgatg 120
tgaaagaact tgtcctggac aacagtcggt cgaatgaagg caaactcgag ggcctcacag 180
atgaatttga agaactggaa ttcttaagta caatcaacgt aggcctcacc tcaatcgcaa 240
acttaccaaa gttaaacaaa cttaagaagc ttgaactaag cgataacaga gtctcagggg 300
gcctggaagt attggcagaa aagtgtccga acctcacgca tctaaattta agtggcaaca 360
aaattaaaga cctcagcaca atagagccac tgaaaaagtt agaaaacctc aagagcttag 420
accttttcaa ttgcgaggta accaacctga acgactaccg agaaaatgtg ttcaagctcc 480
tcccgcaact cacatatctc gacggctatg accgggacga caaggaggcc cctgactcgg 540
atgctgaggg ctacgtggag ggcctggatg atgaggagga ggatgaggat gaggaggagt 600
atgatgaaga tgctcaggta gtggaagacg aggaggacga ggatgaggag gaggaaggtg 660
aagaggagga cgtgagtgga gaggaggagg aggatgaaga aggttataac gatggagagg 720
tagatgacga ggaagatgaa gaagagcttg gtgaagaaga aaggggtcag aagcgaaaac 780
gagaacctga agatgaggga gaagatgatg actaagtgga ataacctatt ttgaaaaatt 840
cctattgtga tttgactgtt tttacccata tcccctctcc cccccccctc taatcctgcc 900
ccctgaa 907
26
905
DNA
Homo sapiens
CDS
(64)..(453)
26
gggttcgggg tttattggtt gaattccgct ggctcaggag cctctgcaga gaaagcgtga 60
gag atg gag atg ggc aaa tgg att cat tta gag ctg cgg aac agg acg 108
Met Glu Met Gly Lys Trp Ile His Leu Glu Leu Arg Asn Arg Thr
1 5 10 15
ccc tcc gat gtg aaa gaa ctt ttc ctg gac aac agt cag tca aat gaa 156
Pro Ser Asp Val Lys Glu Leu Phe Leu Asp Asn Ser Gln Ser Asn Glu
20 25 30
ggc aaa ttg gaa ggc ctc aca gat gaa ttt gaa gaa ctg gaa tta tta 204
Gly Lys Leu Glu Gly Leu Thr Asp Glu Phe Glu Glu Leu Glu Leu Leu
35 40 45
aat aca atc aac ata ggc ctc acc tca att gca aac ttg cca aag tta 252
Asn Thr Ile Asn Ile Gly Leu Thr Ser Ile Ala Asn Leu Pro Lys Leu
50 55 60
aac aaa ctt aag aag ctt gaa cta agc agt aac aga gcc tca gtg ggc 300
Asn Lys Leu Lys Lys Leu Glu Leu Ser Ser Asn Arg Ala Ser Val Gly
65 70 75
cta gaa gta ttg gca gaa aag tgt cca aac ctc ata cat cta aat tta 348
Leu Glu Val Leu Ala Glu Lys Cys Pro Asn Leu Ile His Leu Asn Leu
80 85 90 95
agt ggc aac aaa att aaa gac ctc agc aca ata gag ccc ctg aaa aag 396
Ser Gly Asn Lys Ile Lys Asp Leu Ser Thr Ile Glu Pro Leu Lys Lys
100 105 110
tta gaa aac ctc gag agc tta gac ctt ttc act tgc gag gta acc aac 444
Leu Glu Asn Leu Glu Ser Leu Asp Leu Phe Thr Cys Glu Val Thr Asn
115 120 125
ctg aac aac tactgagaaa agatgttcaa gctcctcctg caactcacat 493
Leu Asn Asn
130
atctcaacgg ctgtgacccg gatgacaagg aggcccctaa ctcggatggt gagggctttg 553
tggagtgcct ggatgacaag gaggaggatg aggatgagga ggagtatgat gaagatgctc 613
aggtaatgga agatgaggag gacgaggatg aggaggagga acgtgaagag gaggacgtga 673
gtggagacga ggaggagaag gatgaaggtt ataacaatgg agaggtagat gatgaggaag 733
atgaagaaga gcttggtgaa gaagaaaggg gtcagaagcg aaaataagaa actgaagatg 793
agggagaaga cgatgcctaa gtggaataat ctattttgaa aaattccttt tgtgatttta 853
ctgtttttag ccgtatcccc tctccccccc cactctaatc ctgccccctg aa 905
27
130
PRT
Homo sapiens
27
Met Glu Met Gly Lys Trp Ile His Leu Glu Leu Arg Asn Arg Thr Pro
1 5 10 15
Ser Asp Val Lys Glu Leu Phe Leu Asp Asn Ser Gln Ser Asn Glu Gly
20 25 30
Lys Leu Glu Gly Leu Thr Asp Glu Phe Glu Glu Leu Glu Leu Leu Asn
35 40 45
Thr Ile Asn Ile Gly Leu Thr Ser Ile Ala Asn Leu Pro Lys Leu Asn
50 55 60
Lys Leu Lys Lys Leu Glu Leu Ser Ser Asn Arg Ala Ser Val Gly Leu
65 70 75 80
Glu Val Leu Ala Glu Lys Cys Pro Asn Leu Ile His Leu Asn Leu Ser
85 90 95
Gly Asn Lys Ile Lys Asp Leu Ser Thr Ile Glu Pro Leu Lys Lys Leu
100 105 110
Glu Asn Leu Glu Ser Leu Asp Leu Phe Thr Cys Glu Val Thr Asn Leu
115 120 125
Asn Asn
130
28
907
DNA
Homo sapiens
CDS
(66)..(812)
28
gggttcgggg tttattgatt gaattccgcc ggcgcgggag cctctgcaga gagagagcgc 60
gagag atg gag atg ggc aga cgg att cat cta gag ctg cgg aac agg acg 110
Met Glu Met Gly Arg Arg Ile His Leu Glu Leu Arg Asn Arg Thr
1 5 10 15
ccc tct gat gtg aaa gaa ctt gtc ctg gtc aac agt cgg tcg aat gaa 158
Pro Ser Asp Val Lys Glu Leu Val Leu Val Asn Ser Arg Ser Asn Glu
20 25 30
ggc aaa ctc gaa ggc ctc aca gat gaa ttt gaa gaa ctg gaa ttc tta 206
Gly Lys Leu Glu Gly Leu Thr Asp Glu Phe Glu Glu Leu Glu Phe Leu
35 40 45
agt aca atc aac gta ggc ctc acc tca atc gca aac tta cca aag tta 254
Ser Thr Ile Asn Val Gly Leu Thr Ser Ile Ala Asn Leu Pro Lys Leu
50 55 60
aac aaa ctt aag aag ctt gaa cta agc gat aac aga gtc tca ggg ggc 302
Asn Lys Leu Lys Lys Leu Glu Leu Ser Asp Asn Arg Val Ser Gly Gly
65 70 75
cta gaa gta ttg gca gaa aag tgt ccg aac ctc acg cat cta aat tta 350
Leu Glu Val Leu Ala Glu Lys Cys Pro Asn Leu Thr His Leu Asn Leu
80 85 90 95
agt ggc aac aaa att aaa gac ctc agc aca ata gag cca ctg aaa aag 398
Ser Gly Asn Lys Ile Lys Asp Leu Ser Thr Ile Glu Pro Leu Lys Lys
100 105 110
tta gaa aac ctc aag agc tta gac ctt ttc aat tgc gag gta acc aac 446
Leu Glu Asn Leu Lys Ser Leu Asp Leu Phe Asn Cys Glu Val Thr Asn
115 120 125
ctg aac gac tac cga gaa aat gtg ttc aag ctc ctc ccg caa ctc aca 494
Leu Asn Asp Tyr Arg Glu Asn Val Phe Lys Leu Leu Pro Gln Leu Thr
130 135 140
tat ctc gac ggc tat gac cgg gac gac aag gag gcc cct gac tcg gat 542
Tyr Leu Asp Gly Tyr Asp Arg Asp Asp Lys Glu Ala Pro Asp Ser Asp
145 150 155
gct gag ggc tac gtg gag ggc ctg gat gat gag gag gag gat gag gat 590
Ala Glu Gly Tyr Val Glu Gly Leu Asp Asp Glu Glu Glu Asp Glu Asp
160 165 170 175
gag gag gag tat gat gaa gat gct cag gta gtg gaa gac gag gag gac 638
Glu Glu Glu Tyr Asp Glu Asp Ala Gln Val Val Glu Asp Glu Glu Asp
180 185 190
gag gat gag gag gag gaa ggt gaa gag gag gac gtg agt gga gag gag 686
Glu Asp Glu Glu Glu Glu Gly Glu Glu Glu Asp Val Ser Gly Glu Glu
195 200 205
gag gag gat gaa gaa ggt tat aac gat gga gag gta gat gac gag gaa 734
Glu Glu Asp Glu Glu Gly Tyr Asn Asp Gly Glu Val Asp Asp Glu Glu
210 215 220
gat gaa gaa gag ctt ggt gaa gaa gaa agg ggt cag aag cga aaa cga 782
Asp Glu Glu Glu Leu Gly Glu Glu Glu Arg Gly Gln Lys Arg Lys Arg
225 230 235
gaa cct gaa gat gag gga gaa gat gat gac taagtggaat aacctatttt 832
Glu Pro Glu Asp Glu Gly Glu Asp Asp Asp
240 245
gaaaaattcc tattgtgatt tgactgtttt tacccatatc ccctctcccc cccccctcta 892
atcctgcccc ctgaa 907
29
249
PRT
Homo sapiens
29
Met Glu Met Gly Arg Arg Ile His Leu Glu Leu Arg Asn Arg Thr Pro
1 5 10 15
Ser Asp Val Lys Glu Leu Val Leu Val Asn Ser Arg Ser Asn Glu Gly
20 25 30
Lys Leu Glu Gly Leu Thr Asp Glu Phe Glu Glu Leu Glu Phe Leu Ser
35 40 45
Thr Ile Asn Val Gly Leu Thr Ser Ile Ala Asn Leu Pro Lys Leu Asn
50 55 60
Lys Leu Lys Lys Leu Glu Leu Ser Asp Asn Arg Val Ser Gly Gly Leu
65 70 75 80
Glu Val Leu Ala Glu Lys Cys Pro Asn Leu Thr His Leu Asn Leu Ser
85 90 95
Gly Asn Lys Ile Lys Asp Leu Ser Thr Ile Glu Pro Leu Lys Lys Leu
100 105 110
Glu Asn Leu Lys Ser Leu Asp Leu Phe Asn Cys Glu Val Thr Asn Leu
115 120 125
Asn Asp Tyr Arg Glu Asn Val Phe Lys Leu Leu Pro Gln Leu Thr Tyr
130 135 140
Leu Asp Gly Tyr Asp Arg Asp Asp Lys Glu Ala Pro Asp Ser Asp Ala
145 150 155 160
Glu Gly Tyr Val Glu Gly Leu Asp Asp Glu Glu Glu Asp Glu Asp Glu
165 170 175
Glu Glu Tyr Asp Glu Asp Ala Gln Val Val Glu Asp Glu Glu Asp Glu
180 185 190
Asp Glu Glu Glu Glu Gly Glu Glu Glu Asp Val Ser Gly Glu Glu Glu
195 200 205
Glu Asp Glu Glu Gly Tyr Asn Asp Gly Glu Val Asp Asp Glu Glu Asp
210 215 220
Glu Glu Glu Leu Gly Glu Glu Glu Arg Gly Gln Lys Arg Lys Arg Glu
225 230 235 240
Pro Glu Asp Glu Gly Glu Asp Asp Asp
245
30
907
DNA
Homo sapiens
CDS
(66)..(455)
30
gggttcgggg tttattgatt gaattccgcc ggcgcgggag cctctgcaga gagagagcgc 60
gagag atg gag atg ggc aga cgg att cat tta gag ctg cgg aac agg acg 110
Met Glu Met Gly Arg Arg Ile His Leu Glu Leu Arg Asn Arg Thr
1 5 10 15
ccc tct gat gtg aaa gaa ctt gtc ctg gac aac agt cgg tcg aat gaa 158
Pro Ser Asp Val Lys Glu Leu Val Leu Asp Asn Ser Arg Ser Asn Glu
20 25 30
ggc aaa ctc gaa ggc ctc aca gat gaa ttt gaa gaa ctg gaa ttc tta 206
Gly Lys Leu Glu Gly Leu Thr Asp Glu Phe Glu Glu Leu Glu Phe Leu
35 40 45
agt aca atc aac gta ggc ctc acc tca atc gca aac tta cca aag tta 254
Ser Thr Ile Asn Val Gly Leu Thr Ser Ile Ala Asn Leu Pro Lys Leu
50 55 60
aac aaa ctt aag aag ctt gaa cta agc gat aac aga gtc tca ggg ggc 302
Asn Lys Leu Lys Lys Leu Glu Leu Ser Asp Asn Arg Val Ser Gly Gly
65 70 75
cta gaa gta ttg gca gaa aag tgt cca aac ctc ata cat cta aat tta 350
Leu Glu Val Leu Ala Glu Lys Cys Pro Asn Leu Ile His Leu Asn Leu
80 85 90 95
agt ggc aac aaa att aaa gac ctc agc aca ata gag ccc ctg aaa aag 398
Ser Gly Asn Lys Ile Lys Asp Leu Ser Thr Ile Glu Pro Leu Lys Lys
100 105 110
tta gaa aac ctc gag agc tta gac ctt ttc act tgc gag gta acc aac 446
Leu Glu Asn Leu Glu Ser Leu Asp Leu Phe Thr Cys Glu Val Thr Asn
115 120 125
ctg aac aac tactgagaaa agatgttcaa gctcctcctg caactcacat 495
Leu Asn Asn
130
atctcaacgg ctgtgacccg gatgacaagg aggcccctaa ctcggatggt gagggctttg 555
tggagtgcct ggatgacaag gaggaggatg aggatgagga ggagtatgat gaagatgctc 615
aggtaatgga agatgaggag gacgaggatg aggaggagga acgtgaagag gaggacgtga 675
gtggagacga ggaggagaag gatgaaggtt ataacaatgg agaggtagat gatgaggaag 735
atgaagaaga gcttggtgaa gaagaaaggg gtcagaagcg aaaataagaa actgaagatg 795
agggagaaga cgatgcctaa gtggaataat ctattttgaa aaattcctat tgtgatttga 855
ctgtttttac ccatatcccc tctccccccc ccctctaatc ctgccccctg aa 907
31
130
PRT
Homo sapiens
31
Met Glu Met Gly Arg Arg Ile His Leu Glu Leu Arg Asn Arg Thr Pro
1 5 10 15
Ser Asp Val Lys Glu Leu Val Leu Asp Asn Ser Arg Ser Asn Glu Gly
20 25 30
Lys Leu Glu Gly Leu Thr Asp Glu Phe Glu Glu Leu Glu Phe Leu Ser
35 40 45
Thr Ile Asn Val Gly Leu Thr Ser Ile Ala Asn Leu Pro Lys Leu Asn
50 55 60
Lys Leu Lys Lys Leu Glu Leu Ser Asp Asn Arg Val Ser Gly Gly Leu
65 70 75 80
Glu Val Leu Ala Glu Lys Cys Pro Asn Leu Ile His Leu Asn Leu Ser
85 90 95
Gly Asn Lys Ile Lys Asp Leu Ser Thr Ile Glu Pro Leu Lys Lys Leu
100 105 110
Glu Asn Leu Glu Ser Leu Asp Leu Phe Thr Cys Glu Val Thr Asn Leu
115 120 125
Asn Asn
130
32
908
DNA
Homo sapiens
32
gggttcgggg tttattgatt gaattccgcc ggcgcgggag cctctgcaga gagagagcgc 60
ggagagatgg agatgggcag acggattcat ttagagctgc ggaacaggac gccctctgat 120
gtgaaagaac ttgtcctgga caacagtcgg tcgaatgaag gcaaactcga aggcctcaca 180
gatgaatttg aagaactgga attcttaagt acaatcaacg taggcctcac ctcaatcgca 240
aacttaccaa agttaaacaa acttaagaag cttgaactaa gcgataacag agtctcaggg 300
ggcctggaag tattggcaga aaagtgtccg aacctcacgc atctaaattt aagtggcaac 360
aaaattaaag acctcagcac aatagagcca ctgaaaaagt tagaaaacct caagagctta 420
gaccttttca attgcgaggt aaccaacctg aacgactacc gagaaaatgt gttcaagctc 480
ctcccgcaac tcacatatct cgacggctat gaccgggacg acaaggaggc ccctgactcg 540
gatgctgagg gctacgtgga gggcctggat gatgaggagg aggatgagga tgaggaggag 600
tatgatgaag atgctcaggt agtggaagac gaggaggacg aggatgagga ggaggaaggt 660
gaagaggagg acgtgagtgg agaggaggag gaggatgaag aaggttataa cgatggagag 720
gtagatgacg aggaagatga agaagagctt ggtgaagaag aaaggggtca gaagcgaaaa 780
cgagaacctg aagatgaggg agaagatgat gactaagtgg aataacctat tttgaaaaat 840
tcctattgtg atttgactgt ttttacccat atcccctctc ccccccccct ctaatcctgc 900
cccctgaa 908
33
906
DNA
Homo sapiens
CDS
(66)..(812)
33
gggttcgggg tttattgatt gaattccgct ggcgcgggag cctctgcaga gagagagcgc 60
gagag atg gag atg ggc aga cgg att cat tta gag ctg cgg aac agg acg 110
Met Glu Met Gly Arg Arg Ile His Leu Glu Leu Arg Asn Arg Thr
1 5 10 15
ccc tct gat gtg aaa gaa ctt gtc ctg gac aac agt cgg tcg aat gaa 158
Pro Ser Asp Val Lys Glu Leu Val Leu Asp Asn Ser Arg Ser Asn Glu
20 25 30
ggc aaa ctc gaa ggc ctc aca gat gaa ttt gaa gaa ctg gaa ttc tta 206
Gly Lys Leu Glu Gly Leu Thr Asp Glu Phe Glu Glu Leu Glu Phe Leu
35 40 45
agt aca atc aac gta ggc ctc acc tca atc gca aac tta cca aag tta 254
Ser Thr Ile Asn Val Gly Leu Thr Ser Ile Ala Asn Leu Pro Lys Leu
50 55 60
aac aaa ctt aag aag ctt gaa cta agc agt aac aga gtc tca ggg ggc 302
Asn Lys Leu Lys Lys Leu Glu Leu Ser Ser Asn Arg Val Ser Gly Gly
65 70 75
cta gaa gta ttg gca gaa aag tgt cca aac ctc acg cat cta aat tta 350
Leu Glu Val Leu Ala Glu Lys Cys Pro Asn Leu Thr His Leu Asn Leu
80 85 90 95
agt ggc aac aaa att aaa gac ctc agc aca ata gag cca ctg aaa aag 398
Ser Gly Asn Lys Ile Lys Asp Leu Ser Thr Ile Glu Pro Leu Lys Lys
100 105 110
tta gaa aac ctc aag agc tta gac ctt ttc aat tgc gag gta acc aac 446
Leu Glu Asn Leu Lys Ser Leu Asp Leu Phe Asn Cys Glu Val Thr Asn
115 120 125
ctg aac gac tac cga gaa aat gtg ttc aag ctc ctc ctg caa ctc aca 494
Leu Asn Asp Tyr Arg Glu Asn Val Phe Lys Leu Leu Leu Gln Leu Thr
130 135 140
tat ctc gac ggc tgt gac cgg gac gac aag gag gcc cct gac tcg gat 542
Tyr Leu Asp Gly Cys Asp Arg Asp Asp Lys Glu Ala Pro Asp Ser Asp
145 150 155
gct gag ggc tac gtg gag ggc ctg gat gac gag gag gag gat gag gat 590
Ala Glu Gly Tyr Val Glu Gly Leu Asp Asp Glu Glu Glu Asp Glu Asp
160 165 170 175
gag gag gag tat gat gaa gat gct cag gta gtg gaa gat gag gag gac 638
Glu Glu Glu Tyr Asp Glu Asp Ala Gln Val Val Glu Asp Glu Glu Asp
180 185 190
gag gat gag gag gag gaa ggt gaa gag gag gac gtg agt gga gag gag 686
Glu Asp Glu Glu Glu Glu Gly Glu Glu Glu Asp Val Ser Gly Glu Glu
195 200 205
gag gag gat gaa gaa ggt tat aac gat gga gag gta gat gac gag gaa 734
Glu Glu Asp Glu Glu Gly Tyr Asn Asp Gly Glu Val Asp Asp Glu Glu
210 215 220
gat gaa gaa gag ctt ggt gaa gaa gaa agg ggt cag aag cga aaa gag 782
Asp Glu Glu Glu Leu Gly Glu Glu Glu Arg Gly Gln Lys Arg Lys Glu
225 230 235
aac ctg aag atg agg gag aag atg atg act aagtggaata acctattttg 832
Asn Leu Lys Met Arg Glu Lys Met Met Thr
240 245
aaaaattcct attgtgattt gactgttttt acccatatcc cctctccccc ccccctctaa 892
tcctgccccc tgaa 906
34
249
PRT
Homo sapiens
34
Met Glu Met Gly Arg Arg Ile His Leu Glu Leu Arg Asn Arg Thr Pro
1 5 10 15
Ser Asp Val Lys Glu Leu Val Leu Asp Asn Ser Arg Ser Asn Glu Gly
20 25 30
Lys Leu Glu Gly Leu Thr Asp Glu Phe Glu Glu Leu Glu Phe Leu Ser
35 40 45
Thr Ile Asn Val Gly Leu Thr Ser Ile Ala Asn Leu Pro Lys Leu Asn
50 55 60
Lys Leu Lys Lys Leu Glu Leu Ser Ser Asn Arg Val Ser Gly Gly Leu
65 70 75 80
Glu Val Leu Ala Glu Lys Cys Pro Asn Leu Thr His Leu Asn Leu Ser
85 90 95
Gly Asn Lys Ile Lys Asp Leu Ser Thr Ile Glu Pro Leu Lys Lys Leu
100 105 110
Glu Asn Leu Lys Ser Leu Asp Leu Phe Asn Cys Glu Val Thr Asn Leu
115 120 125
Asn Asp Tyr Arg Glu Asn Val Phe Lys Leu Leu Leu Gln Leu Thr Tyr
130 135 140
Leu Asp Gly Cys Asp Arg Asp Asp Lys Glu Ala Pro Asp Ser Asp Ala
145 150 155 160
Glu Gly Tyr Val Glu Gly Leu Asp Asp Glu Glu Glu Asp Glu Asp Glu
165 170 175
Glu Glu Tyr Asp Glu Asp Ala Gln Val Val Glu Asp Glu Glu Asp Glu
180 185 190
Asp Glu Glu Glu Glu Gly Glu Glu Glu Asp Val Ser Gly Glu Glu Glu
195 200 205
Glu Asp Glu Glu Gly Tyr Asn Asp Gly Glu Val Asp Asp Glu Glu Asp
210 215 220
Glu Glu Glu Leu Gly Glu Glu Glu Arg Gly Gln Lys Arg Lys Glu Asn
225 230 235 240
Leu Lys Met Arg Glu Lys Met Met Thr
245
35
26
DNA
Homo sapiens
35
tatgctagcg ggttcggggt ttattg 26
36
29
DNA
Homo sapiens
36
gattctagat ggtaagtttg cgattgagg 29
37
29
DNA
Homo sapiens
37
gaatctagaa ggaggaggaa ggtgaagag 29
38
29
DNA
Homo sapiens
38
ctatctagat tcagggggca ggattagag 29
39
24
DNA
Homo sapiens
39
gaggtttatt gattgaattc ggct 24
40
24
DNA
Homo sapiens
40
ccccagtaca cttttcccgt ctca 24
41
12
DNA
Artificial Sequence
recognition sequence
41
tttttctttt tc 12
42
10
DNA
Artificial Sequence
recognition sequence
42
ttaaaattca 10
43
10
DNA
Artificial Sequence
recognition sequence
43
atgtaaaaca 10
44
11
DNA
Artificial Sequence
recognition sequence
44
aagataaaac c 11
45
10
DNA
Artificial Sequence
recognition sequence
45
ccactgggga 10
46
13
DNA
Artificial Sequence
recognition sequence
46
ctctctctct ctc 13
47
11
DNA
Artificial Sequence
recognition sequence
47
aaaacataaa t 11
48
131
PRT
Homo sapiens
48
Met Glu Met Gly Lys Trp Ile His Leu Glu Leu Arg Asn Arg Thr Pro
1 5 10 15
Ser Asp Val Lys Glu Leu Phe Leu Asp Asn Ser Gln Ser Asn Glu Gly
20 25 30
Lys Leu Glu Gly Leu Ala Asp Glu Phe Glu Glu Leu Glu Leu Leu Asn
35 40 45
Thr Ile Asn Ile Gly Leu Ser Ser Ile Ala Asn Leu Ala Lys Leu Asn
50 55 60
Lys Leu Lys Lys Leu Glu Leu Ser Ser Asn Arg Ala Ser Val Gly Leu
65 70 75 80
Glu Val Leu Ala Glu Lys Cys Pro Asn Leu Ile His Leu Asn Leu Ser
85 90 95
Gly Asn Lys Ile Lys Asp Leu Ser Thr Ile Glu Pro Leu Lys Lys Leu
100 105 110
Glu Asn Leu Glu Ser Leu Asp Leu Phe Thr Cys Glu Val Thr Asn Leu
115 120 125
Asn Asn Tyr
130
49
234
PRT
Homo sapiens
49
Met Glu Met Gly Arg Arg Ile His Ser Glu Leu Arg Asn Arg Ala Pro
1 5 10 15
Ser Asp Val Lys Glu Leu Ala Leu Asp Asn Ser Arg Ser Asn Glu Gly
20 25 30
Lys Leu Glu Ala Leu Thr Asp Glu Phe Glu Glu Leu Glu Phe Leu Ser
35 40 45
Lys Ile Asn Gly Gly Leu Thr Ser Ile Ser Asp Leu Pro Lys Leu Lys
50 55 60
Leu Arg Lys Leu Glu Leu Arg Val Ser Gly Gly Leu Glu Val Leu Ala
65 70 75 80
Glu Lys Cys Pro Asn Leu Thr His Leu Tyr Leu Ser Gly Asn Lys Ile
85 90 95
Lys Asp Leu Ser Thr Ile Glu Pro Leu Lys Gln Leu Glu Asn Leu Lys
100 105 110
Ser Leu Asp Leu Phe Asn Cys Glu Val Thr Asn Leu Asn Asp Tyr Gly
115 120 125
Glu Asn Val Phe Lys Leu Leu Leu Gln Leu Thr Tyr Leu Asp Ser Cys
130 135 140
Tyr Trp Asp His Lys Glu Ala Pro Tyr Ser Asp Ile Glu Asp His Val
145 150 155 160
Glu Gly Leu Asp Asp Glu Glu Glu Gly Glu His Glu Glu Glu Tyr Asp
165 170 175
Glu Asp Ala Gln Val Val Glu Asp Glu Glu Gly Glu Glu Glu Glu Glu
180 185 190
Glu Gly Glu Glu Glu Asp Val Ser Gly Gly Asp Glu Glu Asp Glu Glu
195 200 205
Gly Tyr Asn Asp Gly Glu Val Asp Gly Glu Glu Asp Glu Glu Glu Leu
210 215 220
Gly Glu Glu Glu Arg Gly Gln Lys Arg Lys
225 230
50
17
DNA
Homo sapiens
50
gggttcgggg tttattg 17
51
20
DNA
Homo sapiens
51
ctctaatcct gccccctgaa 20 | pp32 is a member of a highly conserved family of differentiation-regulated nuclear proteins that is highly expressed in nearly all human prostatic adenocarcinomas of Gleason Grade ≧5. This contrasts with the low percentage of prostate tumors that express molecular alterations in proto-oncogens or demonstrate tumor suppressor mutation or loss of heterozygosity. By analysis of specimens of human prostatic adenocarcinoma and paired adjacent normal prostate from three individual patients, the inventors have shown that normal prostate continues to express normal pp32, whereas three of three sets of RT-PCR-amplified transcripts from prostatic adenocarcinomas display multiple cancer-associated coding sequence changes. The cancer-associated sequence changes appear to be functionally significant. Normal pp32 exerts antineoplastic effects through suppression of transformation. In contrast, cancer-associated pp32 variants augment, rather than inhibit, transformation. | 2 |
BACKGROUND OF THE INVENTION
[0001] This invention relates to polycarbonates suitable for use in optical articles, and methods for making such polycarbonates. This invention further relates to optical articles, and methods for making optical articles from the polycarbonates.
[0002] Polycarbonates and other polymer materials are utilized in optical data storage media, such as compact disks. In optical data storage media, it is critical that polycarbonate resins have good performance characteristics such as transparency, low water affinity, good processibility, good heat resistance and low birefringence. High water affinity is particularly undesirable in high density optical data storage media as it results in warpage of the recording layer and poor data fidelity
[0003] Improvements in optical data storage media, including increased data storage density, are highly desirable, and achievement of such improvements is expected to improve well established and new computer technology such as read only, write once, rewritable, digital versatile and magneto-optical (MO) disks.
[0004] In the case of CD-ROM technology, the information to be read is imprinted directly into a moldable, transparent plastic material, such as bisphenol A (BPA) polycarbonate. The information is stored in the form of shallow pits embossed in a polymer surface. The surface is coated with a reflective metallic film, and the digital information, represented by the position and length of the pits, is read optically with a focused low power (5 mW) laser beam. The user can only extract information (digital data) from the disk without changing or adding any data. Thus, it is possible to “read” but not to “write” or “erase” information.
[0005] The operating principle in a WORM drive is to use a focused laser beam (20-40 mW) to make a permanent mark on a thin film on a disk. The information is then read out as a change in the optical properties of the disk, e.g., reflectivity or absorbance. These changes can take various forms: “hole burning” is the removal of material, typically a thin film of tellurium, by evaporation, melting or spalling (sometimes referred to as laser ablation); bubble or pit formation involves deformation of the surface, usually of a polymer overcoat of a metal reflector.
[0006] Although the CD-ROM and WORM formats have been successfully developed and are well suited for particular applications, the computer industry is focusing on erasable media for optical storage (EODs). There are two types of EODs: phase change (PC) and magneto-optic (MO). In MO storage, a bit of information is stored as a ˜1 μm diameter magnetic domain, which has its magnetization either up or down. The information can be read by monitoring the rotation of the plane polarization of light reflected from the surface of the magnetic film. This rotation, called the Magneto-Optic Kerr Effect (MOKE) is typically less than 0.5 degrees. The materials for MO storage are generally amorphous alloys of the rare earth and transition metals.
[0007] Amorphous materials have a distinct advantage in MO storage as they do not suffer from “grain noise”, spurious variations in the plane of polarization of reflected light caused by randomness in the orientation of grains in a polycrystalline film. Bits are written by heating above the Curie point, T c , and cooling in the presence of a magnetic field, a process known as thermomagnetic writing. In the phase-change material, information is stored in regions that are different phases, typically amorphous and crystalline. These films are usually alloys or compounds of tellurium which can be quenched into the amorphous state by melting and rapidly cooling. The film is initially crystallized by heating it above the crystallization temperature. In most of these materials, the crystallization temperature is close to the glass transition temperature. When the film is heated with a short, high power focused laser pulse, the film can be melted and quenched to the amorphous state. The amorphized spot can represent a digital “1” or a bit of information. The information is read by scanning it with the same laser, set at a lower power, and monitoring the reflectivity.
[0008] In the case of WORM and EOD technology, the recording layer is separated from the environment by a transparent, non-interfering shielding layer. Materials selected for such “read through” optical data storage applications must have outstanding physical properties, such as moldability, ductility, a level of robustness compatible with popular use, resistance to deformation when exposed to high heat or high humidity, either alone or in combination. The materials should also interfere minimally with the passage of laser light through the medium when information is being retrieved from or added to the storage device.
[0009] As data storage densities are increased in optical data storage media to accommodate newer technologies, such as digital versatile disks (DVD), recordable and rewritable digital versatile disks (DVD-R and DVD-RW), high density digital versatile disks (HD-DVD), digital video recorders (DVR), and higher density data disks for short or long term data archives, the design requirements for the transparent plastic component of the optical data storage devices have become increasingly stringent. In many of these applications, previously employed polycarbonate materials, such as BPA polycarbonate materials, are inadequate. Materials displaying lower birefringence at current, and in the future progressively shorter “reading and writing” wavelengths have been the object of intense efforts in the field of optical data storage devices.
[0010] Low birefringence alone will not satisfy all of the design requirements for the use of a material in optical data storage media; high transparency, heat resistance, low water absorption, ductility, high purity and few inhomogeneities or particulates are also required. Currently employed materials are found to be lacking in one or more of these characteristics, and new materials are required in order to achieve higher data storage densities in optical data storage media. In addition, new materials possessing improved optical properties are anticipated to be of general utility in the production of other optical articles, such as lenses, gratings, beam splitters and the like.
[0011] Birefringence in an article molded from polymeric material is related to orientation and deformation of its constituent polymer chains. Birefringence has several sources, including the structure and physical properties of the polymer material, the degree of molecular orientation in the polymer material and thermal stresses in the processed polymer material. For example, the birefringence of a molded optical article is determined, in part, by the molecular structure of its constituent polymer and the processing conditions, such as the forces applied during mold filling and cooling, used in its fabrication which can create thermal stresses and orientation of the polymer chains.
[0012] The observed birefringence of a disk is therefore determined by the molecular structure, which determines the intrinsic birefringence, and the processing conditions, which can create thermal stresses and orientation of the polymer chains. Specifically, the observed birefringence is typically a function of the intrinsic birefringence and the birefringence introduced upon molding articles, such as optical disks. The observed birefringence of an optical disk is typically quantified using a measurement termed “vertical birefringence” or VBR, which is described more fully below.
[0013] Two useful gauges of the suitability of a material for use as a molded optical article, such as a molded optical data storage disk, are the material's stress optical coefficient in the melt (C m ) and its stress optical coefficient in the glassy state (C g ), respectively. The relationship between C m , C g and birefringence may be expressed as follows:
Δ n=C m ×Δσ m (1)
Δ n=C g ×Δσ g (2)
[0014] where Δn is the measured birefringence and Δσ m and Δσ g are the applied stresses in the melt and glassy states, respectively. The stress optical coefficients C m and C g are a measure of the susceptibility of a material to birefringence induced as a result of orientation and deformation occurring during mold filling and stresses generated as the molded article cools.
[0015] The stress optical coefficients C m and C g are useful as general material screening tools and may also be used to predict the vertical birefringence (VBR) of a molded article, a quantity critical to the successful use of a given material in a molded optical article. For a molded optical disk, the VBR is defined as:
VBR =( n r −n z )=Δ n rz (3)
[0016] where n r and n z are the refractive indices along the r an z cylindrical axes of the disk; n r is the index of refraction seen by a light beam polarized along the radial direction, and n z is the index of refraction for light polarized perpendicular to the plane of the disk. The VBR governs the defocusing margin, and reduction of VBR will lead to alleviation of problems which are not correctable mechanically.
[0017] In the search for improved materials for use in optical articles, C m and C g are especially useful since they require minimal amounts of material and are relatively insensitive to uncontrolled measurement parameters or sample preparation methods, whereas measurement of VBR requires significantly larger amounts of material and is dependent upon the molding conditions. In general, it has been found that materials possessing low values of C g and C m show enhanced performance characteristics, for example VBR, in optical data storage applications relative to materials having higher values of C g and C m . Therefore, in efforts aimed at developing improved optical quality, widespread use of C g and C m measurements is made in order to rank potential candidates for such applications and to compare them with previously discovered materials.
[0018] In applications requiring higher storage density, the properties of low birefringence and low water absorption in the polymer material from which the optical article is fabricated become even more critical. In order to achieve higher data storage density, low birefringence is necessary so as to minimally interfere with the laser beam as it passes through the optical article, for example a compact disk.
[0019] Another critical property needed for high data storage density applications is disk flatness. It is known that excessive moisture absorption results in disk skewing which in turn leads to reduced reliability. Since the bulk of the disk is comprised of the polymer material, the flatness of the disk depends on the low water absorption of the polymeric material. In order to produce high quality disks through injection molding, the polymer, such as polycarbonate should be easily processed.
[0020] There exists a need for compositions having good optical properties and good processibility and which are suitable for use in high density optical recording media. Polycarbonates manufactured by copolymerizing aromatic dihydroxy compounds, such as bisphenol A, with other monomers, such as SBI, may produce acceptable birefringence; however the glass transition temperature is often too high, resulting in poor processing characteristics. Consequently, the obtained moldings have low impact resistance. Further, the water absorption of such polycarbonates is unacceptable for higher density applications.
BRIEF SUMMARY OF THE INVENTION
[0021] The present invention solves these problems, and provides compositions for storage media having unexpected and advantageous properties. These and further objects of the present invention will be more readily appreciated by considering the following disclosure and appended claims.
[0022] The present invention, in one aspect, relates to the blending of polymers to produce miscible blend compositions. In a further aspect, the applicants were surprised to discover that the miscible blend compositions of the present invention possess suitable properties for use in optical articles, in particular for use in optical data storage media.
[0023] This invention provides certain polycarbonates and polycarbonate blends useful in optical article applications. In a preferred embodiment, the present invention provides copolymers of, for example, certain ortho substituted bisphenol A-based polycarbonates and bisphenol A, optionally further comprising polycarbonate residues derived from ortho subsitituted spirobiindane compounds and alkylene or cycloalkylene diacid moieties. In a further embodiment, the present invention provides copolymers of certain ortho-substituted bisphenol A moieties and ortho-substituted spirobiindane moieties. Also provided are optical articles comprised of the copolymers and blends of the present invention. We have found that such copolymers and blends exhibit superior dimensional stability when exposed to water or moisture.
BRIEF DESCRIPTION OF THE DRAWINGS
[0024] [0024]FIG. 1 is a functional bar graph illustrating the effect of substitution on water uptake of polycarbonates.
[0025] [0025]FIG. 2 is a plot illustrating water absorption in BCC:BPA copolymers.
[0026] [0026]FIG. 3 is a plot illustrating radial deviation versus aging time.
[0027] [0027]FIG. 4 is a plot illustrating radial deviation normalized by subtracting initial radial deviation.
[0028] [0028]FIG. 5 is a plot illustrating vertical deviation at outer radius (normalized by initial deviation).
[0029] [0029]FIG. 6 is a plot illustrating the performance of BCC and BCC-BPA PCs relative to BPA-PC vertical deviation at outer radius (normalized by initial deviation).
[0030] [0030]FIG. 7 is a plot illustrating the nonlinear dependence of water diffusivity on percent of BCC in BCC/BPA-PC blends.
[0031] [0031]FIG. 8 is a plot illustrating water uptake in BCC/BPA-PC blends indicating initial slow diffusion of water into CDs.
[0032] [0032]FIG. 9 is a plot illustrating dimensional stability of CDs from BCC-PC/Lexan blends.
[0033] [0033]FIG. 10 is a plot illustrating a correlation of maximum change in vertical deviation to percent of BCC in the blend.
[0034] [0034]FIG. 11 is a plot illustrating a correlation of maximum change in vertical deviation to percent equilibrium water uptake.
DETAILED DESCRIPTION OF THE INVENTION
[0035] The present invention may be understood more readily by reference to the following detailed description of preferred embodiments of the invention and the Examples included therein.
[0036] Before the present compositions of matter and methods are disclosed, it is to be understood that this invention is not limited to specific synthetic methods or to particular formulations, as such may, of course, vary. It is also to be understood that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting.
[0037] In this specification and in the claims which follow, reference will be made to a number of terms which shall be defined to have the following meanings.
[0038] The singular forms “a,” “an” and “the” include plural referents unless the context clearly dictates otherwise.
[0039] “Optional” or “optionally” means that the subsequently described event or circumstances may or may not occur, and that description includes instances where the event or circumstance occurs and instances where it does not.
[0040] “BPA” is herein defined as bisphenol A or 2,2-bis(4-hydroxyphenyl)propane.
[0041] “SBI” is herein defined as 6,6′-dihydroxy-3,3,3′,3′-tetramethylspirobiindane.
[0042] “BCC” is herein defined as 1,1-bis(4-hydroxy-3-methyl phenyl) cyclohexane.
[0043] “CD-1” is herein defined as 6-hydroxy-1-(4′-hydroxyphenyl)-1,3,3-trimethylindane.
[0044] “BPM” is herein defined as 4,4′-(1,3-phenylenediisopropylidene)bisphenol.
[0045] “BPZ” is herein defined as 1,1-bis(4-hydroxyphenyl)cyclohexane.
[0046] “BPI” is herein defined as 1,1-bis(4-hydroxyphenyl)3,3,5-trimethylcyclohexane.
[0047] “bisAP” is herein defined as 4,4′-(1-phenylethylidene)bisphenol.
[0048] “C g ” is the stress optical coefficient of a polymeric material in the glassy state, measured in Brewsters (10 −13 cm 2 /dyne).
[0049] “C m ” is the stress optical coefficient in the melt phase, measured in Brewsters (10 −13 cm 2 /dyne).
[0050] “TMBPA” is 2,2-bis(4-hydroxy-3,5-dimethyl)propane.
[0051] “DMBPA” is 2,2-bis(4-hydroxy-3-methyl)propane.
[0052] “MTBA” is methyltributylammonium chloride
[0053] “DCHBPA” is 2,2-bis(4-hydroxy-3-cyclohexylphenyl)propane
[0054] “Polycarbonate” or “polycarbonates” as used herein includes copolycarbonates, homopolycarbonates and (co)polyester carbonates.
[0055] “Optical articles” as used herein includes optical disks and optical data storage media, for example a compact disk (CD audio or CD-ROM), a digital versatile disk, also known as DVD (ROM,RAM, rewritable), a recordable digital versatile disk (DVD-R), a digital video recording (DVR), a magneto optical (MO) disk and the like; optical lenses, such as contact lenses, lenses for glasses, lenses for telescopes, and prisms; optical fibers; information recording media; information transferring media; high density data storage media, disks for video cameras, disks for still cameras and the like; as well as the substrate onto which optical recording material is applied. In addition to use as a material to prepare optical articles, the polycarbonate may be used as a raw material for films or sheets.
[0056] Unless otherwise stated, “mol %” in reference to the composition of a polycarbonate in this specification is based upon 100 mol % of the repeating units of the polycarbonate. For instance, “a polycarbonate comprising 90 mol % of BCC” refers to a polycarbonate in which 90 mol % of the repeating units are residues derived from BCC diphenol or its corresponding derivative(s). Corresponding derivatives include but are not limited to, corresponding oligomers of the diphenols; corresponding esters of the diphenol and their oligomers; and the corresponding chloroformates of the diphenol and their oligomers.
[0057] The terms “residues” and “structural units”, used in reference to the constituents of the polycarbonate, are synonymous throughout the specification.
[0058] In a first aspect, the present invention provides a polycarbonate comprising
[0059] (a) about 99.9 to 0.1 mole percent of carbonate structural units corresponding to
[0060] wherein R 16 and R 17 are independently selected from hydrogen, C 1 -C 12 alkyl, or phenyl, or R 16 and R 17 are taken together to form a C 3 -C 12 cycloalkyl; R 18 and R 19 and are independently selected from C 1 -C 6 alkyl, C 3 -C 6 cycloalkyl, or phenyl
[0061] (b) about 0.1 to 99.9 mole percent of carbonate structural units corresponding to
[0062] and optionally
[0063] (c) further comprising one or more carbonate structural units corresponding to units selected from the group consisting of
[0064] wherein each R 20 is independently selected from a group consisting of a hydrogen, C 1 -C 6 alkyl, C 3 -C 6 cycloalkyl, or phenyl; and
[0065] wherein Z is a C 1 -C 40 branched or straight chain alkyl group or a C 3 -C 8 cycloalkyl group, and n denotes the number of said structural units;
[0066] wherein the polycarbonate has a glass transition temperature of from about 100° C. to about 185° C. and a water absorption of below about 0.33%, the total of (a), (b), and (c) being 100 mole percent.
[0067] In the above polycarbonates, it is preferred that the glass transition temperature be from about 120° C. to about 165° C., more preferably from about 130° C. to about 150° C.
[0068] In this aspect of the present invention, it is further preferred in component (a), that R 18 and R 19 be selected from methyl, phenyl, n-butyl, sec-butyl, t-butyl, ethyl, cyclohexyl, and isopropyl.
[0069] It is further preferred that R 20 be selected from, methyl, ethyl, and hydrogen.
[0070] Preferred groups -Z- include groups of the formula.
—CH 2 —CH 2 —CH 2 —CH 2 —;
—CH 2 —CH 2 —CH 2 —CH 2 —CH 2 —CH 2 —;
—CH 2 —CH 2 —CH 2 —CH 2 —CH 2 —CH 2 —CH 2 —CH 2 —; and
—CH 2 —CH 2 —CH 2 —CH 2 —CH 2 —CH 2 —CH 2 —CH 2 —CH 2 —CH 2 — and the like.
[0071] In a further preferred embodiment, polycarbonate units (a), (b), and (c) (i) are present in proportions of 20 to 50:20 to 50: and 30 to 50 mole percent, respectively.
[0072] In a further preferred embodiment, polycarbonate units (a), (b), and (c) (ii) are present in proportions of 20 to 50:20 to 50: and 1 to 15 mole percent, respectively.
[0073] In a further preferred embodiment, polycarbonate units (a), (b), (c) (i), and (c) (ii), are present in proportions of 20 to 50:20 to 50:20 to 50 and :1 to 20 mole percent, respectively.
[0074] In each of the above preferred embodiments, it will be understood that the above proportions such that the total will always equal 100 mole percent.
[0075] In a second aspect, the present invention provides a polycarbonate comprising:
[0076] (a) about 0.1 to 99.1 mole percent of carbonate structural units corresponding to
[0077] wherein R 16 and R 17 are independently selected from hydrogen, C 1 -C 6 alkyl, or phenyl, or R 16 and R 17 are taken together to form a C 3 -C 8 cycloalkyl; R 18 and R 19 and are independently selected from C 1 -C 6 alkyl, C 3 -C 8 cycloalkyl, or phenyl
[0078] (b) about 99.1 to 0.1 mole percent of structural units corresponding to
[0079] wherein each R 20 is independently selected from a group consisting of a C 1 -C 6 alkyl, C 3 -C 6 cycloalkyl, or phenyl;
[0080] wherein the polycarbonate has a glass transition temperature of from about 120° C. to about 185° C. and a water absorption of below about 0.33%.
[0081] In this aspect of the present invention, it is further preferred in component (a), that R 18 and R 19 be selected from methyl, ethyl, isopropyl, sec-butyl, tert-butyl and R 18 /R 19 in cyclohexyl ring.
[0082] It is further preferred that R 16 and R 17 be selected from methyl, ethyl, and propyl.
[0083] It is further preferred that R 20 be selected from ethyl and methyl.
[0084] In this aspect, it is further preferred that structural units (a) are present in a range of 35 to 65 mole percent, most preferably about 45 to 55 mole percent, and structural units (b) are present in a range of 65 to 35 mole percent, most preferably about 55 to 45 mole percent.
[0085] In a further embodiment of this second aspect, the polycarbonate may be further comprised of up to about 50 mole percent of residues of bisphenol A.
[0086] The polycarbonates and blends of the present invention are useful in the manufacture of optical articles. Accordingly, in a third aspect, the present invention provides an optical article comprising
[0087] (I) from 90 to 99.99 percent by weight of a polycarbonate comprising
[0088] (a) about 99.9 to 0.1 mole percent of carbonate structural units corresponding to
[0089] wherein R 16 and R 17 are independently selected from hydrogen, C 1 -C 6 alkyl, or phenyl, or R 16 and R 17 are taken together to form a C 3 -C 8 cycloalkyl; R 18 , and R 19 and are independently selected from C 1 -C 6 alkyl, C 3 -C 8 cycloalkyl, or phenyl
[0090] (b) about 0.1 to 99.9 mole percent of carbonate structural units corresponding to
[0091] and optionally
[0092] (c) further comprising one or more carbonate structural units corresponding to units selected from the group consisting of
[0093] wherein each R 20 is independently selected from a group consisting of a C 1 -C 6 alkyl, C 3 -C 6 cycloalkyl, or phenyl; and
[0094] wherein Z is a C 1 -C 40 branched or straight chain alkyl group or a C 3 -C 8 cycloalkyl group group, and n denotes the number of said structural units;
[0095] wherein the polycarbonate blend has a glass transition temperature of from about 120° C. to about 185° C. and a water absorption of below about 0.33%; the total of (a), (b), and (c) being 100 mole percent, and
[0096] (II) from 0.01 to 10 weight percent of further additives.
[0097] Preferred R 20 groups include methyl, ethyl, n-propyl, isopropyl, n-butyl, sec-butyl, and t-butyl.
[0098] Preferred groups -Z- include groups of the formula.
—CH 2 —CH 2 —CH 2 —CH 2 —CH 2 —CH 2 —CH 2 —CH 2 —;
—C 2 —CH 2 —CH 2 —CH 2 —CH 2 —C 2 —CH 2 —CH 2 —CH 2 —;
—CH 2 —CH 2 —CH 2 —CH 2 —CH 2 —CH 2 —CH 2 —CH 2 —CH 2 —CH 2 —; and
—CH 2 —CH 2 —CH 2 —CH 2 —CH 2 —CH 2 —CH 2 —CH 2 —CH 2 —CH 2 —CH 2 — and the like.
[0099] Similarly, in a fourth aspect, the present invention provides an optical article comprising
[0100] (I) from 90 to 99.99 percent by weight of a polycarbonate comprising:
[0101] (a) about 0.1 to 99.9 mole percent of carbonate structural units corresponding to
[0102] wherein R 16 and R 17 are independently selected from hydrogen, C 1 -C 6 alkyl, or phenyl, or R 16 and R 17 are taken together to form a C 3 -C 8 cycloalkyl; R 18 , and R 19 and are independently selected from C 1 -C 6 alkyl, or phenyl
[0103] (b) about 99.1 to 0.1 mole percent of structural units corresponding to
[0104] wherein each R 20 is independently selected from a group consisting of a C 1 -C 6 alkyl, C 3 -C 6 cycloalkyl, or phenyl;
[0105] wherein the polycarbonate has a glass transition temperature of from about 120° C. to about 185° C. and a water absorption of below about 0.33%; and
[0106] (II) from 0.01 to 10 weight percent of further additives.
[0107] We have also discovered that certain polycarbonates form miscible blends which are useful in optical recording applications. Thus, in a fifth aspect, the present invention provides a miscible polycarbonate blend comprising:
[0108] (A) a polycarbonate comprising structural units corresponding to
[0109] wherein R 16 and R 17 are independently selected from hydrogen, C 1 -C 6 alkyl, or phenyl, or R 16 and R 17 are taken together to form a C 3 -C 8 cycloalkyl; R 18 , and R 19 and are independently selected from C 1 -C 6 alkyl, C 3 -C 8 cycloalkyl, or phenyl;
[0110] (B) a polycarbonate comprising structural units corresponding to
[0111] wherein R 16 and R 17 are independently selected from C 1 -C 6 alkyl.
[0112] As noted in the fifth aspect, the miscible blends described therein are useful as optical articles. Accordingly, in a sixth aspect, the present invention provides an optical article comprising
[0113] (I) from 90 to 99.99 percent by weight of a miscible polycarbonate blend comprising
[0114] (A) a polycarbonate comprising structural units corresponding to
[0115] wherein R 16 and R 17 are independently selected from hydrogen, C 1 -C 6 alkyl, or phenyl, or R 16 and R 17 are taken together to form a C 3 -C 8 cycloalkyl; R 18 , and R 19 and are independently selected from C 1 -C 6 alkyl, C 3 -C 8 cycloalkyl, or phenyl
[0116] (B) a polycarbonate comprising structural units corresponding to
[0117] wherein R 16 and R 17 are independently selected from C 1 -C 6 alkyl;
[0118] wherein the polycarbonate has a glass transition temperature of from about 120° C. to about 185° C. and a water absorption of below about 0.33%; and
[0119] (II) from 0.01 to 10 weight percent of further additives.
[0120] Especially preferred blends include those wherein dimethyl bisphenol A polycarbonate and bisphenol A polycarbonate are blended in a proportion of about 25-75 weight percent: 75-25 weight percent, respectively.
[0121] Especially preferred blends include those wherein BCC polycarbonate and bisphenol A polycarbonate are blended in a proportion of about 25-75 weight percent: 75-25 weight percent, respectively.
[0122] In the present invention it is further desirable that the polycarbonates possess other suitable properties for use in optical media. The polycarbonates of the present invention preferably have glass transition temperatures in the range of from about 120° C. to about 185° C., more preferably from about 125° C. to about 165° C., even more preferably from about 130° C. to about 150° C. The water absorption of the polycarbonates is preferably below 0.33%, even more preferably less than about 0.25%.
[0123] The weight average molecular weight (M W ), as determined by gel permeation chromotagraphy relative to polystyrene, of the polycarbonates is preferably from about 10,000 to about 100,000, more preferably between about 10,000 to about 50,000, even more preferably between about 25,000 to about 40,000.
[0124] The polycarbonate should have light transmittance of at least about 85%, more preferably at least about 90% and a C g of less than about 60 Brewsters, more preferably less than 55 Brewsters, even more preferably less than 50 Brewsters. The polycarbonate preferably has a C m of below about 3,000 Brewsters, more preferably below about 2,500 Brewsters, even more preferably less than about 2,450 Brewsters.
[0125] The compositions of a particular polycarbonate may be varied within certain ranges to achieve the suitable property profile. The ranges set forth herein are illustrative ranges for the desired embodiments.
[0126] The polycarbonates of the invention may be prepared by the interfacial, melt, or solid state processes. If the interfacial process is used, the addition of various phase transfer catalysts is optional. Phase transfer catalysts which are suitable include, but are not limited to tertiary amines, such as triethylamine; ammonium salts, such as tetrabutylammonium bromide; or hexaethylguanidium chloride. Monofunctional phenols, such as p-cumylphenol and 4-butylphenol; long chain alkylphenols, such as cardanol and nonyl phenol; and difunctional phenols may be used as chain stopping agents. Optionally 0.1 to 10 mole %, more preferably 1 to 5 mole % of chainstopping agent may be incorporated into the polycarbonate, based on the total moles of the repeating units.
[0127] In some instances, the phosgenation conditions must be adjusted. In particular, the phosgenation conditions should be adjusted in cases where the formation of undesired cyclic oligomers is favored by the characteristic reactivity of the monomer, which is related to monomer solubility in the reaction medium and monomer structure. In the case of BCC, for example, cyclic oligomer formation occurs to a greater extent under standard interfacial polymerization conditions than in the case of, for example, BPA. In polycarbonates containing substantially more than about 20 mol % of BCC, it is advantageous to use an excess of phosgene to promote the formation of linear bischloroformate oligomers which are converted to high molecular weight polymers by partial hydrolysis and polycondensation. Preferably from about 20 to 200 mol % of excess phosgene is used.
[0128] The polycarbonates of the present invention may also be prepared by the melt or transesterification process. This process does not require the use of phosgene or a solvent and minimizes the formation of low molecular weight contaminants, such as cyclic and linear low molecular weight oligomers in the final polymer. The monomers are mixed with a carbonate source, such as a diarylcarbonate, and a small amount of catalyst, such as an alkali metal hydroxide or ammonium hydroxide and heated under a vacuum according to a protocol in which the temperature is raised through a series of stages while the pressure in the headspace over the reaction mixture is lowered from ambient pressure to about 1 torr.
[0129] Suitable carbonate sources, catalysts and reaction conditions are found in U.S. Pat. No. 5,880,248, and Kirk - Othmer Encyclopedia of Chemical Technology, Fourth Edition, Volume 19, pp. 585-600, herein incorporated by reference. The time of the stages and the temperature are such that mechanical losses of material through foaming and the like are avoided. Phenol and excess diphenyl carbonate are removed overhead to complete the polymerization process. The product high polymer is then isolated as a melt which may be compounded with other additives, such as stabilizers and mold release agents prior to pelletization. The products produced by the melt process have reduced numbers of undissolved particles and reduced content of low molecular weight contaminants, such as cyclic oligomers, relative to the interfacially produced product.
[0130] The polycarbonates of the present invention may optionally be blended with any conventional additives used in optical applications, including but not limited to dyestuffs, UV stabilizers, antioxidants, heat stabilizers, and mold release agents, to form an optical article. In particular, it is preferable to form a blend of the polycarbonate and additives which aid in processing the blend to form the desired optical article. The blend may optionally comprise from 0.0001 to 10% by weight of the desired additives, more preferably from 0.0001 to 1.0% by weight of the desired additives.
[0131] Substances or additives which may be added to the polycarbonates of this invention, include, but are not limited to, heat-resistant stabilizer, UV absorber, mold-release agent, antistatic agent, slip agent, antiblocking agent, lubricant, anticlouding agent, coloring agent, natural oil, synthetic oil, wax, organic filler, inorganic filler and mixtures thereof.
[0132] Examples of the aforementioned heat-resistant stabilizers, include, but are not limited to, phenol stabilizers, organic thioether stabilizers, organic phosphite stabilizers, hindered amine stabilizers, epoxy stabilizers and mixtures thereof. The heat-resistant stabilizer may be added in the form of a solid or liquid.
[0133] Examples of UV absorbers include, but are not limited to, salicylic acid UV absorbers, benzophenone UV absorbers, benzotriazole UV absorbers, cyanoacrylate UV absorbers and mixtures thereof.
[0134] Examples of the mold-release agents include, but are not limited to natural and synthetic paraffins, polyethylene waxes, fluorocarbons, and other hydrocarbon mold-release agents; stearic acid, hydroxystearic acid, and other higher fatty acids, hydroxyfatty acids, and other fatty acid mold-release agents; stearic acid amide, ethylenebisstearoamide, and other fatty acid amides, alkylenebisfatty acid amides, and other fatty acid amide mold-release agents; stearyl alcohol, cetyl alcohol, and other aliphatic alcohols, polyhydric alcohols, polyglycols, polyglycerols and other alcoholic mold release agents; butyl stearate, pentaerythritol tetrastearate, and other lower alcohol esters of fatty acid, polyhydric alcohol esters of fatty acid, polyglycol esters of fatty acid, and other fatty acid ester mold release agents; silicone oil and other silicone mold release agents, and mixtures of any of the aforementioned.
[0135] The coloring agent may be either pigments or dyes. Inorganic coloring agents and organic coloring agents may be used separately or in combination in the present invention. Insofar as one desired utility for the polycarbonates and polycarbonate blends of this case is in optical articles, it is most preferred that the polycarbonates and polycarbonate blends be transparent.
[0136] The polycarbonates may be random copolymers, block copolymers or graft copolymers. When graft copolymers and other branched polymers are prepared a suitable branching agent is used during production.
[0137] The desired optical article may be obtained by molding the polycarbonate or polycarbonate blend by injection molding, compression molding, extrusion methods and solution casting methods. Injection molding is the more preferred method of forming the article.
[0138] Because the polycarbonates of the present invention possess advantageous properties such as low water absorption, good processibility and low birefringence, they can be advantageously utilized to produce optical articles. End-use applications for the optical article of the invention include, but are not limited to, a compact disk, a digital audio disk, a digital versatile disk, an magneto-optical disk, an ASMO device and the like; optical lenses, such as contact lenses, lenses for glasses, lenses for telescopes, and prisms; optical fibers; photonics devices such as waveguides and the like; information recording media; information transferring media; disks for video cameras, disks for still cameras and the like.
[0139] The polycarbonate may function as the medium for data storage, i.e. the data may be fixed onto or into the polycarbonate. The polycarbonate may also function as the substrate onto which a data storage medium is applied. An example being a plastic substrate for a first-surface data storage format such as a DVR disk and the like. Further, some combination of both functions may be employed in a single device, as for instance when the polycarbonate is imprinted with tracking to aid in reading a data storage medium which is applied to the polycarbonate.
[0140] In the present invention it is further critical that the polycarbonates possess suitable properties for use in optical articles. The polycarbonates of the further aspect of the present invention preferably have glass transition temperatures in the range of from about 120° C. to about 185° C., more preferably from about 125° C. to about 165° C., even more preferably from about 130° C. to about 150° C. The water absorption of the polycarbonates is preferably below about 0.33%, even more preferably less than about 0.20%.
[0141] The weight average molecular weight (M W ), as determined by gel permeation chromotagraphy relative to polystyrene, of the polycarbonates is preferably from about 10,000 to about 100,000, more preferably between about 10,000 to about 50,000, even more preferably between about 25,000 to about 40,000.
[0142] The polycarbonates should have light transmittance of at least about 85%, more preferably at least about 90% and a C g of less than about 60 Brewsters, more preferably less than 50 Brewsters. The polycarbonates preferably have a C m of below about 3,000 Brewsters, even more preferably below about 2,500 Brewsters.
[0143] The desired optical article may be obtained by molding the polycarbonate or polycarbonate blend by injection molding, compression molding, extrusion methods and solution casting methods. Injection molding is the more preferred method of forming the article.
[0144] The methods of making the polycarbonates, end use applications, and additives that may be blended with the polycarbonates are the same as those described in section I of this specification, in reference to the polycarbonate suitable for use in an optical article.
[0145] As mentioned in reference to the polycarbonates in section I of this specification, the polycarbonate of the further aspect of the invention as defined in section II, and the optical articles made therefrom, may function as the medium for data storage, as in CD audio, CD ROM and DVD, i.e. the data may be fixed onto or into the polycarbonate. The polycarbonate may also function as the substrate onto which a data storage medium is applied. Further, some combination of both functions may be employed in a single device, as for instance when the polycarbonate is imprinted with tracking to aid in reading a data storage medium which is applied to the polycarbonate.
[0146] Experimental Section
[0147] The following examples are put forth so as to provide those of ordinary skill in the art with a complete disclosure and description of how the compositions of matter and methods claimed herein are made and evaluated, and not intended to limit the scope of what the inventors regard as their invention. Efforts have been made to insure accuracy with respect to numbers (e.g., amounts, temperatures, etc.) but some error and deviations should be accounted for. Unless indicated otherwise, parts are by weight, temperature is in ° C. or is at room temperature and pressure is at or near atmospheric.
[0148] The materials and testing procedures used for the results shown herein are as follows:
[0149] Molecular weights are reported as number average (Mn) and weight average (Mw) in units of grams per mol (g/mol). Molecular weights were determined by gel permeation chromatography using an HP 1090 HPLC with two Polymer Labs Mixed Bed C columns at 40° C., a flowrate of 1 milliliter per minute (ml/min), using chloroform as solvent and a calibration based on polystyrene standards.
[0150] T g values were determined by differential scanning calorimetry using a Perkin Elmer DSC7. The T g was calculated based on the ½Cp method using a heating ramp of 20° C./min.
[0151] C g values were determined as follows. The polycarbonate (7.0 grams) was charged to a heated mold having dimensions 5.0×0.5 inches and compression molded at 120° C. above its glass transition temperature while being subjected to applied pressure starting at 0 and ending at 2000 pounds using a standard compression molding device. After the required amount of time under these conditions the mold was allowed to cool and the molded test bar removed with the aid of a Carver press. The molded test bar was then inspected under a polaroscope and an observation area on the test bar located. Selection of the observation area was based on lack of birefringence observed and sufficient distance from the ends or sides of the test bar. The sample was then mounted in a device designed to apply a known amount of force vertically along the bar while the observation area of the bar was irradiated with appropriately polarized light. The bar was then subjected to six levels of applied stress and the birefringence at each level measured with the aid of a Babinet compensator. Plotting birefringence versus stress affords a line whose slope is equal to the stress optical coefficient C g .
[0152] Water absorption (% H 2 O) was determined by the following method which is similar to ASTM D570, but modified to account for the variable thickness of the parts described in these examples. The plastic part (typically a compression-molded bar used for a C g measurement) or injection-molded compact disk was dried in a vacuum for over 1 week. The sample was removed periodically and weighed to determine if it was dry (i.e. stopped loosing mass). The sample was removed from the oven, allowed to equilibrate to room temperature in a desiccator, and the dry weight was recorded. The sample was immersed in a water bath at room temperature. The sample was removed periodically from the bath, the surface was blotted dry, and the weight recorded. The sample was repeatedly immersed and the weight measured until the sample became substantially saturated. The sample was considered substantially saturated or at “Equilibrium” when the increase in weight in a 2 week period averaged less than 1% of the total increase in weight (as described in ASTM method D570-98 section 7.4). Diffusion coefficients were obtained by plotting the mass of water absorbed, M uptake , versus time, t, in units of seconds and fitting this curve to the following equation (expanded to the first 10 terms):
M u p t a k e / M e q = 1 - ∑ n = 0 ∞ { 8 / ( 2 n + 1 ) 2 π 2 exp ( - D ( 2 n + 1 ) 2 π 2 t / ( 4 L 2 ) ) }
[0153] where M eq is the mass of water absorbed at equilibrium in units of grams, D is the diffusivity in units of cm 2 /s and L is the part thickness in units of cm.
[0154] The dimensional stability (the sensitivity of polycarbonate disks to warpage through water absorption) was obtained by measuring radial tilt and vertical deviation as a function of disk radius using a Dr. Shenk Prometeus MT136E optical disk tester. Polycarbonate substrates (120 mm diameter, 1.2 mm thickness) were molded using a CD stamper, metalized with aluminum, and lacquered (on top of the metal layer) with a UV-cured acrylate. Disks were then dried in a vacuum for over 1 week. The sample was removed from the oven, allowed to equilibrate to room temperature in a desiccator, and the initial values of radial tilt and vertical deviation were recorded. The sample was then immersed in a water bath at room temperature. The sample was removed periodically from the bath, the surface was blotted dry, and the radial tilt and vertical deviation recorded. The sample was repeatedly immersed in water and the radial tilt and vertical deviation measured until the sample reached equilibrium—usually about 2 days. Due to the part-to-part variability in initial values of tilt and vertical deviation due to molding variability, it was useful to normalize the data by either dividing or subtracting the vertical deviation data by the initial value at time 0. By mathematically correcting or “normalizing” the variability in the molding process, the dimensional stability performance of the new materials could be more readily assessed.
[0155] Descriptions of Polymer Synthesis:
[0156] Preparation of BCC Homopolycarbonate (LF1 Process):
[0157] Into a 500 mL Morton flask was placed BCC (29.6 g, 100 mmol), 125 mL methylene chloride and 90 mL of water. The pH was adjusted to 12.5 with 50 wt % sodium hydroxide (NaOH). Phosgene was added at 0.6 g/min, at 10.0 g (100 mmol), p-cumylphenol (1.06 g, 5 mol %) was added and phosgene was continued until 12.3 g (20 mol % excess) added. The pH was lowered to 10.5 (with phosgene) at which point 25 uL of triethylamine (TEA) added followed 5 min later with 25 uL more TEA. The chloroformates lasted about 8 min from the original TEA addition. An additional 75 uL of TEA added (125 uL total, about 1 mol %) followed by 4.5 g more phosgene. The reaction mixture is tested for chloroformates. If present they are hydrolyzed by addition of DMBA (5 uL) (dimethylbutylamine). The polymer solution was separated from the brine, washed with aqueous hydrochloric acid (HCl), washed with water and steam crumbed in a blender. T g =140° C., Mw=35,900 (Polystyrene standards).
[0158] Preparation of BCC/BPA (50/50) Copolycarbonate (LF2 Process):
[0159] Into a 500 mL Morton flask was placed BCC (14.8 g, 50 mmol), BPA (11.4 g, 50 mmol), 125 mL methylene chloride and 90 mL of water. The pH was adjusted to 11 with 50 wt % NaOH. Phosgene was added at 0.6 g/min, at 10.0 g (100 mmol), p-cumylphenol (1.48 g, 7 mol %) was added and phosgene was continued until 12.3 g (20 mol % excess) added. The pH was lowered to 10.5 (with phosgene) at which point 25 uL of TEA added followed 5 min later with 25 uL more TEA. The chloroformates lasted about 18 min from the original TEA addition. An additional 75 uL of TEA added (125 uL total, about 1 mol %) followed by 4.5 g more phosgene. The reaction mixture was tested for chloroformates. If present they were hydrolyzed by addition of DMBA (5 uL) (dimethylbutylamine). The polymer solution was separated from the brine, washed with aqueous HCl, washed with water and steam crumbed in a blender. T g =140° C., Mw=27,700 (Polystyrene standards).
[0160] Preparation of TMBPA Homopolycarbonate (LF3 Process):
[0161] Into a 500 mL Morton flask was placed TMBPA (28.6 g, 100 mmol), 120 mL methylene chloride, 90 mL of water and MTBA (0.5 mL of a 75 wt % aqueous solution). The pH was adjusted to 12.0 with 50 wt % NaOH. Phosgene was added at 0.6 g/min, at 11.2 g (112 mmol, 10 mol % excess), p-cumylphenol (1.06 g, 5 mol %) was added and reaction stirred for 3 min. 100 uL of DMBA was added and the chloroformates lasted about 15 min. The polymer solution was separated from the brine, washed with aqueous HCl, washed with water and steam crumbed in a blender. T g ==200° C., Mw=32,400 (Polystyrene standards).
[0162] The following polymers listed in Table 1 were prepared by the LF1 process:
[0163] DMBPA Homopolycarbonate
[0164] BPI Homopolycarbonate
[0165] DEBPA Homopolycarbonate
[0166] BisAP Homopolycarbonate
[0167] DmbisAP Homopolycarbonate
[0168] DMBPI Homopolycarbonate
[0169] DsBBPA Homopolycarbonate
[0170] DIPPBPA Homopolycarbonate
[0171] BPZ Homopolycarbonate
[0172] SBI/BPM Copolycarbonate at 50 mol % SBI
[0173] DESBI/BPM Copolycarbonate at 50 mol % DESBI
[0174] BCC/BPA Copolycarbonates at 80, 60 and 40 mol % BCC
[0175] BCC/DsBBPA Copolycarbonate at 10 mol % DsB-BPA
[0176] The following polymers listed in Table 1 were prepared by the LF2 process:
[0177] BPA Homopolycarbonate
[0178] BCC/BPA Copolycarbonate at 50 mol % BCC
[0179] DMBPA/BPA Copolycarbonate at 50 mol % DMBPA
[0180] BPA/DsBBPA Copolycarbonate at 10 mol % DsB-BPA
[0181] Preparation of di-t-butyl BPA Polycarbonate (LX1 Process):
[0182] A 250 mL glass melt polymerization reactor, which had been previously passivated by acid washing, rinsing and drying overnight at 120° C., was loaded with 46.46 g (0.14 mol) of di-t-butyl BPA and 32.15 g (0.15 mol) of diphenyl carbonate. A 316 stainless steel helixing stirrer was suspended in the powder and 102 microliters of tetramethylammonium hydroxide in the form of a 1.0 M aqueous solution and 1023 microliters of sodium hydroxide in the form of a 0.001 M aqueous solution were added. The vessel was then evacuated and purged with nitrogen three times and heated to 180° C., whereupon the reaction mixture melted. Upon complete melting, the mixture was allowed to thermally equilibrate for 15 minutes after which stirring at 50 rpm was begun. The temperature was raised to 230° C. and the pressure reduced to 170 millibar, whereupon phenol began to distill from the reactor. After 60 minutes, polymerization was continued further with the following temperature/pressure profile: 270° C./20 millibar (30 minutes); 290° C./3.5 millibar (30 minutes); 310° C./0.3 millibar (230 minutes). At the completion of polymerization, the reactor was restored to ambient pressure with nitrogen and the polymer pulled from the reactor. GPC results (based on polycarbonate standards): Mw 54700, Mn 18034.
[0183] Preparation of DMBPA-co-BCC (50/50) Polycarbonate (LX1 Process):
[0184] A 1-liter glass melt polymerization reactor equipped with a mechanical stirrer, heating mantle, vacuum and nitrogen inlets, and a heat-jacketed overhead condenser with a phenol receiving flask, and which had been previously passivated by acid washing, rinsing and drying overnight at 70° C., was loaded with 110.53 g (516 mmol) of diphenyl carbonate, 63.58 g (248 mmol) of DMBPA, and 73.52 g (248 mmol) of BCC. A 316 stainless steel helixing stirrer was suspended in the powder and 372 microliters of tetramethylammonium hydroxide in the form of a 1.0 M aqueous solution and 744 microliters of sodium hydroxide in the form of a 0.001 M aqueous solution were added. The vessel was then evacuated and purged with nitrogen three times, then heated to 180° C. whereupon the reaction mixture melted and was allowed to thermally equilibrate for 10 minutes. The temperature was then raised to 230° C., the pressure reduced to 170 millibar, and the mixture stirred at 50 rpm for 60 minutes. Polymerization was continued further with the following temperature/pressure profile: 27 0 ° C./20 millibar (30 minutes); 300° C./3.4 millibar (30 minutes); 310° C./0.3 millibar (30 minutes). The polymer was then dropped from the reactor and cooled to give 104 g of transparent material (Mn=20400, Mw=50000, T g =134° C.).
[0185] Preparation of Substituted Bisphenol A Based Polycarbonates (LX2 Process):
[0186] Melt phase polycondensation reactions were carried out with 5 and 10 mole % of co-monomer with bisphenol A (BPA) and diphenyl carbonate (DPC). Mole % is defined as 100×(mole co-monomer/(mole BPA+mole co-monomer)). The co-monomers that were used were 2,2-(bis-3-methyl-4-hydroxyphenyl)propane, 2,2-(bis-3-ethyl-4-hydroxyphenyl) propane, 2,2-(bis-3-isopropyl-4-hydroxyphenyl)propane, 2,2-(bis-3-sec.butyl-4-hydroxyphenyl)propane, 2,2-(bis-3-tert.butyl-4-hydroxyphenyl)propane, 2,2-(bis-3-cyclohexyl-4-hydroxyphenyl)propane, and 2,2-(bis-3-phenyl-4-hydroxyphenyl)propane. The total amount (moles) of DPC equaled 1.08×(BPA+co-monomer (in moles)). As catalysts, tetramethylammonium hydroxide (TMAH) (2.5×10 −4 mole/mole (BPA+co-monomer)) and NaOH (7.5×10 −6 mole/mole(BPA+co-monomer)) were added as an aqueous solution. Thus for a typical polymerization, BPA (22.20 g), 2,2-(bis-3-isopropyl-4-hydroxyphenyl)propane (3.38 g), and DPC (25.00 g) were weighed into a glass tube that was previously conditioned in 1 N HCl overnight and rinsed excessively with Milli-Q water and acetone and dried with air. After addition of the monomers, 100 ml of catalyst solution was added (8.2 mM NaOH and 274 mM TMAH). The vessel was then evacuated and purged with nitrogen three times and heated to 180° C., whereupon the reaction mixture melted. Upon complete melting, the mixture was allowed to thermally equilibrate for 10 minutes after which stirring was begun. The pressure was reduced to 130 mbar, whereupon phenol began to distill from the reactor. After 30 minutes, polymerization was continued further with the following temperature/pressure profile: 180° C./65 mbar (30 min.); 220° C./65 mbar (30 min); 220° C./13 mbar (30 min); 270° C./13 mbar (30 min); 270° C./8 mbar (30 min); 270° C./8 mbar (30 min); 300° C./1 mbar (60 min). At the end of the reaction, the reactor was brought back to atmospheric pressure with a gentle nitrogen flow and the polymer was harvested as a colorless to slightly colored, transparent material. To purify, the copolymer was dissolved in chloroform and reprecipitated in methanol. Finally, the polymer was isolated by filtration and dried overnight under vacuum at 50° C.
[0187] Preparation of DMBPA/BPA (50/50) Copolycarbonate (LX3):
[0188] A 250 mL glass melt polymerization reactor, which had been previously passivated by acid washing, rinsing and drying overnight at 120° C., was loaded with 71.08 g (0.28 mol) of Polycarbonate oligomer with Mw=4000 g/mole, 71.66 g (0.28 mol) of dimethyl-bisphenol A (DMBPA), and 62.28 g (0.29 mol) of diphenyl carbonate. A 316 stainless steel helixing stirrer was suspended in the powder and 419 microliters of tetramethylammonium hydroxide in the form of a 1.0 M aqueous solution and 419 microliters of sodium hydroxide in the form of a 0.001 M aqueous solution were added. The vessel was then evacuated and purged with nitrogen three times and heated to 180° C., whereupon the reaction mixture melted. Upon complete melting, the mixture was allowed to thermally equilibrate for 15 minutes after which stirring at 50 rpm was begun. The temperature was raised to 230° C. and the pressure reduced to 170 millibar, whereupon phenol began to distill from the reactor. After 60 minutes, polymerization was continued further with the following temperature/pressure profile: 270° C./20 millibar (30 minutes); 290° C./3.5 millibar (30 minutes); 310° C./0.3 millibar (60 minutes). At the completion of polymerization, the reactor was restored to ambient pressure with nitrogen and the polymer pulled from the reactor. GPC results (based on polycarbonate standards): 84700 Mw, 24700 Mn.
[0189] Preparation of Blends and Optical Articles of DMBPA or BCC Polycarbonate with BPA Polycarbonate (Examples 46-48)
[0190] BPA polycarbonate (LEXAN OQ1050C obtained from General Electric) and DMBPA polymer and/or BCC polymer were premixed in a HENSCHEL high intensity mixer and fed into a 28 mm WP extruder equipped with a mild screw design and extruded at barrel temperatures of from about 260° C. to about 280° C. at a screw speed of 300 rpm and a throughput of from about 10 to 20 lbs/hr. For example 46 (50:50 BCC:OQ1050), 425 g BCC polycarbonate (7 mole % chainstopper, Mw of 28,000 grams/mole) and 425 g BPA polycarbonate (LEXAN OQ 1050C, made by GENERAL ELECTRIC) were premixed and extruded. For example 47 (53:47 DMBPA:OQ1050), 447 g DMBPA polycarbonate and 403 g OQ1050C were premixed and extruded. For example 48 (49:28:22 DMBPA:BCC:OQ1050C), 420 g DMBPA polycarbonate, 241 g BCC polycarbonate, and 190 g OQ1050C were premixed and extruded. The resulting pellets were then injection molded into compact disks using an Engel 275 ton injection molding machine. The optical transmission for all the disks was greater than 84% at 630 nm using an HP UV-visible spectrophotomer. The high transmittance of these examples supports the conclusion that the polymers are miscible.
[0191] Preparation of 5,5′diethylspirobiindane (DESBI)
[0192] 5,5′diethyl SBI was prepared via the double Fries rearrangement of SBI diacetate followed by reduction of 5,5′-diacety SBI.
[0193] SBI-diacetate (10.0 g, 25.5 mmol) and aluminum chloride (20 g, 150 mmol) were mixed well and heated to 170° C. for four minutes. The resulting reddish foam was then cooled to 0° C. and carefully diluted with cold water. The crude product was extracted with ethyl acetate, washed with brine, and dried with sodium sulfate to recover a dark foam. Upon trituration with acetonitrile, the product was recovered as an off-white solid (4 g, 40% yield). Melting Point=212-214° C. Nuclear Magnetic Resonance Spectroscopy (NMR) was consistent with desired 5,5′-diacetyl SBI. At 0° C., ethylchloroformate (5.87 ml, 61.4 mmol) dissolved in 35 ml of tetrahydrofuran (THF) was added to a solution of 5,5′-diacetyl SBI (10 g, 25.5 mmol), triethylamine (8.53 ml, 61.2 mmol), and 85 ml of THF. The mixture was stirred for an additional 30 minutes at 0° C. and then filtered. At 0° C., the filtrate was added dropwise to a mixture of sodium borohydride (7.7 g, 203 mmol) and 100 mL of water. The reaction was stirred at room temperature for one hour, poured into water, neutralized with 10% hydrochloric acid, and extracted with ethyl acetate. The organics were washed with brine, and dried with sodium sulfate to recover a white solid. The crude product was dissolved in ethyl acetate and toluene. Ethyl acetate was removed in vacuo. The remaining mixture was filtered, and the filtercake was washed with hexane to recover a white solid (6.9 g, 74% yield). MP=236-239° C. NMR is consistent with desired 5,5′-diethyl SBI.
[0194] Polymer characteristics of the various materials of the present invention are listed in Tables 1 and 2. The polymers in Table 1 were synthesized using the interfacial polymerization process, while those in Table 2 were synthesized using the melt process. Of critical interest to the performance of optical disks are the resin molecular weight and glass transition temperature (T g ), water uptake and diffusivity, and stress-optical coefficient (C g ). The T g data indicate that the o-substituted bisphenol polycarbonates generally have lower T g 's than their respective non-substituted analogues. For example, the T g 's of the DMBPA- and BCC-based polycarbonates are about 20-30° C. lower than those from BPA and BPZ. Copolymers from these monomers have utility as optical disk substrates due to the lower T g and reduced melt viscosity of the resin during molding, which in turn improves optical birefringence and pit-groove replication. For this reason, the copolycarbonates of Examples 7, 8 and 15 are preferable in that the T g is reduced compared to BPA-PC.
[0195] Stress-optical coefficients of the substituted polycarbonates are also reduced compared to BPA-PC (81 Brewsters). The homopolymers of BCC, DsBBPA, DIPPBPA, DEBPA, and DTBBPA (C g =24 for Example 25) all have substantially better C g values which results in lower optical birefringence in the optical disk when the resins are molded under conditions that result in similar residual stress.
TABLE 1 Polymer characteristics of BPA and alkylated BPA based copolycarbonates (interfacial process) H2O Uptake Tg Mw Mn (% at Diffusivity Ex. # Process Composition (° C.) (Kg/mol) equilibrium) (×10{circumflex over ( )}8 cm2/s) Cg Comparative Examples C1 LF2 OQ1030L (BPA-PC 142 28.3 11.8 0.33 4.6 81 with PCP endcap) C2 LF2 BPZ 169 32.2 12.8 0.28 2.5 C3 LF1 BisAP 179 45.81 8.5 0.43 4.9 C4 LF1 BPI 224 37.21 1.9 0.35 8.3 C5 LF3 TMBPA 200 32.41 2.6 0.79 6.9 60 C6 LF1 BPM:SBI (50:50) 143 45.6 8.2 0.26 Substituted bisphenol polycarbonate samples 1 LF1 BCC 140 35.9 13.1 0.22 0.4 47 2 LF1 BCC:BPA (80:20) 138 34.80 14.7 0.27 0.87 3 LF1 BCC:BPA (60:40) 139 33.30 14.7 0.28 4 LF2 BCC:BPA (50:50) 140 27.7 11.7 0.28 2.3 61 5 LF1 BCC:BPA (40:60) 140 33.2 14.5 0.30 6 LF1 DsBBPA 63 44.6 13.6 0.11 5.5 32 7 LF2 DsBBPA:BPA (10:90) 127 30.5 10.3 8 LF1 DsBBPA:BCC (10:90) 127 31.7 11.0 9 LF1 DIPPBPA 80 42.9 14.2 0.10 4.4 35 10 LF1 DEBPA 72 38.5 13.1 0.17 4.5 50 11 LF1 DMBisAP 155 43.9 17.3 0.34 2.2 12 LF1 DMBPI 196 46.1 15.1 0.34 4.3 13 LF1 BPM:DESBI (50:50) 129 33.8 6.6 0.16 14 LF1 DMBPA 118 31.0 12.1 0.24 1.9 66 15 LF2 BPA:DMBPA (50:50) 129 31.1 12.2 0.29 2.3
[0196] Table 1 also illustrates the superior water absorption properties of the copolycarbonates of the present invention relative to analogous polycarbonate materials. The substituted polycarbonate materials display both a low water absorption (water uptake at 1 week and at equilibrium) and a low kinetic water affinity (diffusivity, related to permeability). The water absorption and diffusivity are thought to be important parameters for determining a material's suitability for use in the manufacture of optical devices such as digital versatile disks (DVD's) and substrates for DVR disks. For these optical disk formats, performance is related to disk flatness, and disk flatness is in turn dependent upon the initial flatness of the polycarbonate substate out of the mold and its sensitivity (rate of water uptake) to atmospheric temperature and humidity conditions. Comparison of the water diffusivity, and the weight percent water absorption at 1 week and at equilibrium among molded parts from different materials permits evaluation of this key material property.
[0197] For the DVR optical disk format, in which a 100 micron plastic film is bonded to a 1.1 to 1.2 mm plastic substrate, disk tilt (or warpage) results when the substrate and film absorb water. The rate of water uptake is not as important as the equilibrium concentration of water in the substrate and the mismatch in water uptake between the substrate and film. Thus, for the DVR format, it is desirable to have resin materials with low equilibrium water uptake. The equilibrium water absorption for a series of modified polycarbonates is shown in FIG. 1. The water absorption trends lower as the length of the alkyl substituent is increased. The effect is shown to be general for a number of bisphenols including BPA, BPZ, BisAP, BPI and SBI. Of particular interest are dimethyl-BPA, dibutyl-BPA, and dimethyl-BPZ (BCC) due to their lower C g , T g 's that are within an acceptable range, and lower water uptake. The equilibrium water uptake can be adjusted through copolymerization of mixtures of BPA with the substituted bisphenols. For example, copolymers of BCC with BPA (Examples 2-5) demonstrate that the equilibrium water uptake varies linearly with composition as shown in FIG. 2.
[0198] For DVD-recordable and rewriteable (DVDR and DVD-RW) and high density DVD (HD-DVD) optical disk formats where tilt specifications are also tighter than they are for CD and DVD, a material with low equilibrium water uptake is also desireable to improve the dimensional stability. In addition, the rate of water uptake, as expressed by the diffusivity, is also important as it can affect the concentration of water, and therefore tilt that occurs in a molded and metalized DVD half-substrates (0.6 mm thickness) prior to bonding. With BPA-PC, it is a common practice in the industry to equilibrate DVD half-substrates for several days in a controlled atmosphere prior to bonding in order to reduce the effect of water-induced tilt. This practice can be eliminated if the entire molding and bonding process were either performed very quickly or in a controlled atmosphere in order to reduce the amount of water allowed to absorb into the substrate. In practice, this is either very difficult or very expensive. The materials of the present invention, with their lower water diffusivity have utility in these applications because the amount of water that is absorbed in the first few hours of exposure to water is very much reduced compared to BPA-PC. Upon exposure to water, the polymers in Examples 1-4 initially have very slow water sorption kinetics, a characteristic that is described by the water diffusion coefficient. The polycarbonates from BCC (Example 1) are especially desirable for these applications because it has a diffusivity that is nearly 10 times lower (0.4×10^ 8 cm 2 /s) than for BPA-PC (4.6×10^ 8 cm 2 /s).
[0199] Several of the copolycarbonates from Table 1 as well as some others which were difficult to polymerize interfacially were also polymerized by the melt process. Properties of these polymers are shown in Table 2. Molecular weights and glass transition temperatures of the melt-polymerized materials were comparable to their interfacially polymerized analogues. Of particular interest are several copolymers that were polymerized by the melt that were not easily polymerized interfacially. Example 25, DtBBPA-PC was difficult to polymerize interfacially, yet high molecular weight was achieved via the melt process.
[0200] It was also surprising to find that the glass transition of DtBBPA-PC is 120° C., closer to the T g of DMBPA-PC than to its isomer, DsBBPA, Example 6, which has a T g nearly 60° C. lower. Given its relatively high T g , within the preferred range of T g 's for optical disk substrates, copolymers of DtBBPA with BPA would find utility in optical disk formats requiring low water uptake and low birefringence. The C g of Example 25 is 24 Brewsters, the lowest of any of the substituted polycarbonates of this invention.
TABLE 2 Characteristics of copolycarbonates (melt process) Tg Mw Mn Example Process Composition (° C.) (Kg/mol) Comparative Examples C7 LX OQ1020C (BPA-PC with 142 30.1 12.8 82% phenyl endcap) C8 *LX3 BPA 150 54.0 22.7 Substituted bisphenol polycarbonate samples 16 LX1 BCC 134 26.1 12.0 17 LX2 DEBPA:BPA (5:95) 141 44.9 21.2 18 LX2 DEBPA:BPA (9.4:90.6) 134 39.7 21.4 19 LX2 DiPPBPA:BPA (4.8:95.2) 149 30.2 13.8 20 LX2 DiPPBPA:BPA (9.7:90.3) 134 45.0 21.7 21 LX2 DsBBPA:BPA (1.7:98.3) 144 70.8 34.1 22 LX2 DsBBPA:BPA (10:90) 138 89.4 39.7 23 LX1 DsBBPA:BPA (10:90) 130 29.4 12.9 24 LX BCC:DsBBPA (90:10) 130 35.1 14.4 25 LX1 DtBBPA 120 55.0 21.5 26 LX2 DtBBPA:BPA (4.6:95.4) 141 31.1 15.2 27 LX2 DtBBPA:BPA (8.6:91.4) 144 68.6 30.5 28 LX2 DCHBPA:BPA (4.6:95.4) 143 44.5 21.0 29 LX2 DCHBPA:BPA (9.3:90.7) 140 37.0 19.3 30 LX2 DPBPA:BPA (5.2:94.8) 145 48.6 20.6 31 LX2 DPBPA:BPA (10:90) 141 43.1 18.1 32 LX2 BPZ:BPA (5.8:94.2) 130 13.1 7.6 33 LX2 BPZ:BPA (11.8:88.2) 156 101.6 40.8 34 LX2 BCC:BPA (5.7:94.3) 160 60.0 24.0 35 LX2 BCC:BPA (11.8:88.2) 154 46.5 18.0 36 LX1 DMBPA 122 46.3 18.9 37 LX2 DMBPA:BPA (4.7:95.3) 132 33.7 15.8 38 LX2 DMBPA:BPA (9.7:90.3) 144 46.3 18.4 39 *LX3 BPA:DMBPA (25:75) 128 55.5 21.0 40 *LX3 BPA:DMBPA (50:50) 132 48.6 20.4 41 *LX3 BPA:DMBPA (75:25) 137 33.8 15.8 42 LX1 BCC:DMBPA (50:50) 134 50.0 20.4 43 LX1 BCC:DMBPA (75:25) 137 49.5 20.1 44 LX1 BPA:BCC:DMBPA 137 42.3 21.1 (25:50:25) 45 LX1 BPA:BCC:DMBPA 138.9 47.7 19.8 (50:25:25)
[0201] Several DMBPA:BPA and DMBPA:BCC copolymers were synthesized (Examples 14 and 15 interfacially, and Examples 36-45 via the melt process); the formulations and resulting molecular weights and measured T g 's are given in Tables 1 and 2. Examples 14, 15 and 42 were compression molded and water uptake was measured as a function of water soak time at 25° C. to obtain the percent water uptake at equilibrium (0.24%, 0.29% and 0.24%, respectively). The water absorption values were very similar to those for the BCC-PC homopolymer (Example 1). In addition, DMBPA-PC (Example 36) has a substantially lower T g (122° C.) than BPA-PC (142-150° C) and BPA:BCC copolymers (138-140° C.). The lower T g of DMBPA homopolymer and BPA copolymers allows for a lower melt viscosity and hence improved birefringence and pit-groove replication. It was found (RD28144 filed USPTO May 31, 2000) that incorporation of a softblock, DDDA (dodecanedioic acid), into BCC:BPA:DDDA copolymers improves the birefringence and replication properties of optical disks. The DMBPA:BCC:BPA copolymers in this invention would have enhanced flow relative to BPA-PC due to the lower T g resulting in lower birefringence, and in addition, would have a lower equilibrium water uptake. DMBPA is both a softblock and a water absorption-lowering agent. Thus, a new composition is invented that has a more optimal combination of cost, T g , flow, and water absorption than BCC:BPA copolymers and BCC:BPA:DDDA terpolymers, allowing for the manufacture of optical disks with improved pit-replication, birefringence and dimensional stability performance.
[0202] Several compositions incorporating BCC, DMBPA, and DsBBPA were molded into substrates in order to assess their utility in the DVR and recordable and rewriteable DVD formats.
TABLE 3 Performance of Compact Disks molded from DMBPA and BCC blends and copolymers Tg Mw % T at IBR VBR Ex. # Process Composition (° C.) (Kg/Mol) Mn 630 nm Min. Max. Disk Avg C1 OQ1050 (BPA-PC with 142 28.3 11.8 15 65 492.4 PCP endcap) 4 LF2 BCC:BPA (50:50) 140 27.7 11.7 −23 50 257 15 LF DMBPA:BPA (50:50) 129 31.1 12.2 −30 71 384.7 7 LF2 DsBBPA:BPA (10:90) 127 30.5 10.3 86.1 −66 24 582 46 **Blend BCC:OQ1050 (50:50) 141 26.7 12.5 84.5 47 **Blend DMBPA:OQ1050 127 41.7 17.1 84.4 (50:50) 48 **Blend BCC:DMBPA:OQ1050 129 39.0 16.4 85.1 (25:50:25)
[0203] Copolymers of dimethyl-BPA-co-BPA (DMBPA:BPA) 50:50 copolymer and di-s-butyl-BPA-co-BPA (DsBBPA:BPA) 10/90 were polymerized interfacially (examples 15 and 7, respectively). The powder was extruded using a 28 mm WP extruder and molded into compact disks using a 275 ton Engel injection molder with a CD stamper. The disks were metalized and lacquered and then dried in a vacuum desicator at room temperature for 1 week and then placed in a humidity chamber at 25° C./90% r.h. The disks were removed periodically (every 1-2 hrs for 50 hrs) from the humidity chamber and tilt was measured using a Dr. Shenk optical disk test. Dimensional stability (tilt) data on the CDs are shown in FIGS. 3 - 5 . The data are averages from 3 replicates of DMBPA:BPA copolymer and OQ1050 BPA-PC. FIG. 3, which shows radial deviation at 40 mm (near the CD center) indicates that DMBPA:BPA CDs generally have a higher radial deviation than the OQ1050 CDs. Presumably, the high initial tilt of the DMBPA:BPA disks, due to residual stresses molded into the parts, might be improved with molding process optimization. However, while most of the tilt for the copolymer CDs is present at the beginning of the test, the OQ1050 CDs showed a tremendous increase in radial deviation (from 0.5 to 2.0) in the first 10 hrs of the test and then recovered with time. FIG. 4, which shows the radial tilt at 40 mm normalized by substracting the initial radial deviation at time 0, more clearly illustrates that the DMBPA:BPA copolymer has a more stable radial tilt than OQ1050. The effect of a lower radial deviation was shown even more clearly when disk curvature data were plotted. Vertical deviation data at the outer radius (at 55 mm) of the CDs (also normalized by subtracting the value at time 0) are shown in FIG. 5. The change in vertical deviation at the outer radius of the CDs during the course of the humidity test is almost 400 microns for the OQ1050 CDs, but less than 100 microns for the DMBPA:BPA disks. This indicates that metalized and lacquered CDs molded from DMBPA:BPA, as with CDs from other low water absorbing PCs such as BCC-PC, can have better dimensional stability during humidity exposure than BPA-PC.
[0204] [0204]FIG. 6 indicates that CDs molded from BCC homopolymers produced by the melt (LX) or interfacial process (LF) have much improved dimensional stability upon exposure to water at 25° C. The vertical deviation at 55 mm for a disk molded from BPA-PC increased by over 100 microns during the water immersion test compared to only about 20 microns for the BCC homopolymer. FIG. 6 also shows that the 50:50 BCC:BPA copolymer also has improved dimensional stability compared to BPA-PC, though not as good as the BCC homopolymers.
[0205] Table 3 also indicates that the 50:50 BCC:BPA and DMBPA:BPA copolymers (Examples 4 and 15, respectively) have an improved (decreased) vertical birefringence (VBR) relative to BPA-PC (Example C1). Also notable are the decreased T g 's of the DMBPA and DsBBPA copolymers and blends (Examples 15, 7, 47 and 48) which is expected to improve the replication of features (pits, grooves or bumps) in plastic substrates molded from these materials.
[0206] Examples 46-48 also demonstrate that blends of BCC polycarbonate and/or DMBPA polycarbonate with BPA polycarbonate possess single T g 's and good (>84%) transparency.
[0207] Optical discs molded from BCC-PC/BPA-PC blends also possess low water absorption and good dimensional stability. Water diffusivity measurements performed on this system also show that the water equilibrium uptake and diffusivity improve (decrease) as the concentration of BCC-PC increases in the blend as listed in Table 4. Surprisingly, this improvement is better than expected, ie. the concentration dependence of the water diffusion coefficient is nonlinear as shown in FIG. 7. At 50 wt % BCC-PC, the diffusion coefficient is 3±0.3×10 −8 cm2/s which is surprisingly lower than the weighted average diffusivity of both homopolymers (1.2+0.2)/2×10 −9 cm 2 /s=7×10 −8 cm 2 /s. Data on BCC-BPA copolymers also show that the concentration dependence of the water absorption is nonlinear. As shown in FIG. 8, the rate of water absorption into CDs molded from BCC-PC/Lexan blends is slow. At times as long as 10 hours, BCC-PC absorbed less than 0.05% water, compared to 0.15% for BPA-PC. This indicates that copolymers containing BCC would perform well in high density recordable and rewriteable DVD formats where in-process (between the molding and bonding steps) dimensional stability is critical.
TABLE 4 Performance of Compact Disks Molded from BCC/BPA-PC Blends H2O Uptake % Change in Vertical Mw % at Diffusivity Deviation Ex. # Process Composition (Kg/mol) equilibrium) (×10{circumflex over ( )}8 cm2/s Maximum 49 LX BPA-PC (OQ1050) 27.4 0.38 8.65 72 50 **Blend BCC-OQ1050 26.7 0.33 3.20 62 (50:50) 51 **Blend BCC-OQ1050 26.2 0.3 1.80 18 (75:25) 52 LX BCC 30.1 0.25 0.84 25 53 LF BPA-PC (PC120) 33.1 0.36 9.00 58 54 **Blend BCC-PC120 32.3 0.34 5.10 59 (25:75) 55 **Blend BCC-PC120 32.1 0.32 2.70 21 (50:50) 56 **Blend BCC-PC120 30.9 0.29 1.10 17 (75:25) 57 LF BCC 28.3 0.22 1.36 6
[0208] As shown in FIG. 9, the dimensional stability of BCC-PC/BPA-PC blends are also very good. The stability of BCC-PC homopolymer is shown to be substantially better than Lexan; blends of the two polymers are shown to have intermediate dimensional stability.
[0209] For each of the molded disks immersed in water, the percent change in vertical deviation (VD) at 55 mm was calculated as follows:
[0210] % change in VD=100×(VD at any time−VD at time 0)/VD at time 0. As indicated in Table 4, the maximum percent increase in vertical deviation during the water immersion test is 72 and 58 percent for BPA-PC (Examples 49 and 53, respectively) compared to only 25 and 6 percent for BCC-PC (Examples 52 and 57). The maximum percent change in vertical deviation is plotted versus polymer blend composition (% BCC-PC) in FIG. 10. There is a clear trend towards improved dimensional stability (lower maximum change in vertical deviation) as the percentage of BCC-PC in the blend is increased. Finally, FIG. 11 indicates that a strong correlation exists between dimensional stability (change in vertical deviation) to equilibrium water uptake. This correlation suggests that BCC copolymers and blends, as well as the other compositions of the present invention with reduced equilibrium water uptake will have improved dimensional stability performance as compared to BPA-PC.
[0211] Particularly preferred ortho substituted dihydric compounds include the following.
[0212] This invention has been described in detail with particular reference to preferred embodiments thereof, but it will be understood that variations and modifications can be effected within the spirit and scope of the invention. | This invention provides certain polycarbonates and polycarbonate blends useful in optical article applications. In a preferred embodiment, copolymers of, for example, certain ortho substituted bisphenol A-based polycarbonates and bisphenol A, optionally further comprising polycarbonate residues derived from ortho subsitituted spirobiindane compounds and alkylene or cycloalkylene diacid moieties. In a further embodiment, the invention provides copolymers of certain ortho-substituted bisphenol A moieties and ortho-substituted spirobiindane moieties. Also provided are optical articles comprised of the copolymers and blends of the invention. We have found that such copolymers and blends exhibit superior dimensional stability when exposed to water or moisture. | 2 |
FIELD OF THE INVENTION
The present invention relates generally to directional drilling applications. More particularly, this invention relates to a control system and method for controlling the direction of drilling.
BACKGROUND OF THE INVENTION
In oil and gas exploration, it is common for drilling operations to include drilling deviated (non vertical) and even horizontal boreholes. Such boreholes may include relatively complex profiles, including, for example, vertical, tangential, and horizontal sections as well as one or more builds, turns, and/or doglegs between such sections. Recent applications often utilize steering tools including a plurality of independently operable force application members (also referred to as blades or ribs) to apply force on the borehole wall during drilling to maintain the drill bit along a prescribed path and to alter the drilling direction. Such force application members are typically disposed on the outer periphery of the drilling assembly body or on a non-rotating sleeve disposed around a rotating drive shaft. Exemplary steering tools are disclosed by Webster in U.S. Pat. No. 5,603,386 and Krueger et al. in U.S. Pat. No. 6,427,783.
In order to control the drilling along a predetermined profile, such steering tools are typically controlled from the surface and/or by a downhole controller. For example, in known systems, the direction of drilling (inclination and azimuth) may be determined downhole using conventional MWD surveying techniques (e.g., using accelerometers, magnetometers, and/or gyroscopes). The measured direction may be transmitted (e.g., via mud pulse telemetry) to a drilling operator who then compares the measured direction to a desired direction and transmits appropriate control signals back to the steering tool. Alternatively, the measured direction may be compared with a desired direction and appropriate control signals determined, for example, using a downhole computer. In curved sections of the borehole (e.g., builds, turns, or doglegs) the rate of penetration and/or the total vertical depth of the borehole is required to determine the desired direction. Such parameters are typically determined at the surface and transmitted downhole.
While such procedures have been utilized successfully in various drilling operations, both tend to be limited by the typically scarce downhole communication bandwidth (e.g., mud pulse telemetry bandwidth) available in drilling operations. Telemetry bandwidth constraints tend to reduce the frequency of survey data available for control of the steering tool. For example, in a typical drilling application utilizing conventional mud pulse telemetry, several minutes may be required to record each survey point and communicate with the surface. Such time delays render sustained control difficult at best and may lead to more tortuous borehole profiles that sometimes require costly and time consuming reaming operations.
Barr et al., in U.S. Patent Application Publication 2003/0037963, discloses a method for measuring the curvature of a borehole utilizing a downhole structure including at least three longitudinally spaced distance sensors. The distance sensors are utilized to measure a distance between the structure and the borehole wall. The downhole structure typically further includes strain gauges deployed thereon to determine the curvature of the downhole structure when deployed in the borehole. The curvature of the borehole is then calculated from the curvature of the downhole structure and the distances between the structure and the borehole wall. The curvature of the borehole may then be used as an input component of a bias signal for controlling operation of a downhole bias unit in a directional drilling assembly.
The approach disclosed by Barr et al., while potentially serviceable in some drilling applications, suggests several drawbacks. First, as described above, Barr et al., disclose a complex apparatus for determining borehole curvature, the apparatus including at least three distance sensors and multiple strain gauges mounted on a structure, which is further mounted in a drill collar. Such complexity tends to increase both fabrication and maintenance costs and inherently reduces reliability (especially in the demanding downhole environment). Furthermore, the magnitude of the curvature is inadequate to fully define a change in the longitudinal direction of a borehole. As such, Barr et al. disclose a device having even greater complexity, including a roll stabilized platform suspended in the structure and a plurality of magnets for determining its orientation relative to the structure. Such additional structure is intended to enable the tool to determine both the curvature and tool face of the borehole.
Moreover, since the method disclosed by Barr et al. depends on distance measurements between the borehole wall and a downhole tool, the accuracy of the curvature measurements may be significantly compromised in boreholes having a rough surface (e.g., in formations in which there is appreciable washout during drilling). Another potential source of error is related to the length of the structure to which the distance sensors are mounted. If the structure is relatively short, then the curvature of the borehole is measured along an equally short section thereof and hence subject to error (e.g., via local borehole washout or turtuosity). On the other hand, if the structure is relatively long, then measurement of its curvature becomes complex (e.g., possibly requiring numerous strain gauges) and hence prone to error.
Therefore, there exists a need for an improved method and system for controlling downhole steering tools that address one or more of the shortcomings described above.
SUMMARY OF THE INVENTION
Exemplary embodiments of the present invention are intended to address the above described need for an improved system and method for controlling downhole steering tools. Referring briefly to the accompanying figures, aspects of this invention include a system and method for determining a rate of change of the longitudinal direction (RCLD) of a borehole. Such a rate of change of direction may be determined, for example, by acquiring survey readings at first and second longitudinal positions in the borehole. In one embodiment, a downhole tool includes first and second survey sensor sets deployed at corresponding first and second longitudinal positions thereon. Such a downhole tool may further include a controller that utilizes the measured RCLD of the borehole to steer subsequent drilling of the borehole along a predetermined path.
Exemplary embodiments of the present invention may advantageously provide several technical advantages. For example, exemplary methods according to this invention enable the RCLD of the borehole to be determined independent of the rate of penetration or total vertical depth of the borehole. As such, embodiments of this invention tend to minimize the need for communication between a drilling operator and the bottom hole assembly, thereby advantageously preserving downhole communication bandwidth. Furthermore, embodiments of this invention enable control data to be acquired at significantly increased frequency, thereby improving the control of the drilling process. Such improved control may reduce tortuosity of the borehole and may therefore tend to minimize (or even eliminate) the need for expensive reaming operations.
In one aspect the present invention includes a method for determining a rate of change of longitudinal direction of a subterranean borehole. The method includes (1) providing a downhole tool including first and second surveying devices disposed at corresponding first and second longitudinal positions in the borehole, (2) causing the first and second surveying devices to measure a longitudinal direction of the borehole at the corresponding first and second positions, and (3) processing the longitudinal directions of the borehole at the first and second positions to determine the rate of change of longitudinal direction of the borehole between the first and second positions. One alternative variation of this aspect further includes, by way of example, processing the measured rate of change of longitudinal direction of the borehole and a predetermined rate of change of longitudinal direction to control the direction of drilling of the subterranean borehole.
The foregoing has outlined rather broadly the features and technical advantages of the present invention in order that the detailed description of the invention that follows may be better understood. Additional features and advantages of the invention will be described hereinafter, which form the subject of the claims of the invention. It should be appreciated by those skilled in the art that the conception and the specific embodiment disclosed may be readily utilized as a basis for modifying or designing other structures for carrying out the same purposes of the present invention. It should also be realized by those skilled in the art that such equivalent constructions do not depart from the spirit and scope of the invention as set forth in the appended claims.
BRIEF DESCRIPTION OF THE DRAWINGS
For a more complete understanding of the present invention, and the advantages thereof, reference is now made to the following descriptions taken in conjunction with the accompanying drawings, in which:
FIG. 1 depicts an exemplary embodiment of a downhole tool according to the present invention including both upper and lower sensor sets and a steering tool.
FIG. 2 depicts the downhole tool of FIG. 1 deployed in a deviated borehole.
FIG. 3 depicts a control loop diagram illustrating an exemplary method of this invention.
FIG. 4 is a diagrammatic representation of a portion of the downhole tool of FIG. 1 showing unit magnetic field and gravity vectors.
FIG. 5 is another diagrammatic representation of a portion of the downhole tool of FIG. 1 showing a change in azimuth between the upper and lower sensor sets.
FIG. 6 depicts another control loop diagram illustrating an exemplary method of this invention.
DETAILED DESCRIPTION
It will be appreciated that aspects of this invention enable the rate of change of the longitudinal direction (RCLD) of a borehole to be measured. It will be understood by those of ordinary skill in the art that the RCLD of a borehole is typically fully defined in one of two ways (although numerous others are possible). First, the RCLD of a borehole may be quantified by specifying the build rate and the turn rate of the borehole. Where used in this disclosure the term “build rate” is used to refer to the vertical component of the curvature of the borehole (i.e., a change in the inclination of the borehole). The term “turn rate” is used to refer to the horizontal component of the curvature of the borehole (i.e., a change in the azimuth of the borehole). The RCLD of a borehole may also be quantified by specifying the dogleg severity and the tool face of the borehole. Where used in this disclosure the term “dogleg severity” refers to the curvature of the borehole (i.e., the severity or degree of the curve of the borehole) and the term “tool face” refers to the angular direction to which the borehole is turning (e.g., relative to the high side when looking down the borehole). For example, a tool face of 0 degrees indicates a borehole that is turning upwards (i.e., building), while a tool face of 90 degrees indicates a borehole that is turning to the right. A tool face of 45 degrees indicates a borehole that is turning upwards and to the right (i.e., simultaneously building and turning to the right).
Referring now to FIGS. 1 and 2 , one exemplary embodiment of a downhole tool 100 according to the present invention is illustrated. In FIG. 1 , downhole tool 100 is illustrated as a directional drilling tool including upper 110 and lower 120 sensor sets, a downhole steering tool 130 , and a drill bit assembly 150 . In the embodiment shown, steering tool 130 includes a plurality of stabilizer blades 132 (e.g., three) for engaging the wall of a borehole. The radial positions of each of the individual stabilizer blades 132 (or alternatively the force or pressure applied to the blades 132 ) may be individually controlled by a suitable controller (not shown). One or more of the force application members 132 may be moved in a radial direction, e.g., using electrical or mechanical devices (not shown), to apply force on the borehole wall in order to steer the drill bit 150 outward from the longitudinal axis of the borehole. It will be appreciated that this invention is not limited to any particular type of steering tool. Suitable steering tools may include substantially any known control scheme to control the direction of drilling, for example, by controlling the radial position of (or alternatively the force or pressure applied to) various stabilizer blades 132 . Further, embodiments of this invention may utilize both two-dimensional and three-dimensional rotary steerable tools. FIG. 1 illustrates that the upper 110 and lower 120 sensor sets are disposed at a known longitudinal spacing ‘d’ in the downhole tool 100 . The spacing ‘d’ may be, for example, in a range of from about 2 to about 30 meters (i.e., from about 6 to about 100 feet) or more, but the invention is not limited in this regard. Each sensor set ( 110 and 120 ) includes one or more surveying devices such as accelerometers, magnetometers, or gyroscopes. In one preferred embodiment, each sensor set ( 110 and 120 ) includes three mutually perpendicular accelerometers, with at least one accelerometer in each set having a known orientation with respect to the borehole.
With continued reference to FIGS. 1 and 2 , sensor sets 110 and 120 are connected by a structure 140 that permits bending along its longitudinal axis 50 (as shown in FIG. 2 in which the downhole tool 100 is shown deployed in a deviated borehole 162 ). In certain embodiments, structure 140 may substantially resist rotation along the longitudinal axis 50 between the upper 110 and lower 120 sensor sets, however, the invention is not limited in this regard as described in more detail below. Structure 140 may include substantially any suitable deflectable tube, such as a portion of a drill string. Structure 140 may also include one or more MWD or LWD tools, such as acoustic logging tools, neutron density tools, resistivity tools, formation sampling tools, and the like. It will also be appreciated that while sensor set 120 is shown distinct from steering tool 130 , it may be incorporated into the steering tool 130 , e.g., in a non-rotating sleeve portion thereof.
With reference now to FIG. 3 , and continued reference to FIG. 2 , an exemplary control method 200 according to this invention may be utilized to control the direction of drilling. As shown at 225 of FIG. 3 , sensor sets 110 and 120 may be utilized to determine the local longitudinal directions of the borehole (e.g., the inclination and/or the azimuth values). As described in more detail below, and as shown at 230 , such local directions may be processed downhole to determine the RCLD of the borehole (e.g., the build and turn rates of the borehole or the dogleg severity and tool face of the borehole). At 210 a controller (not shown) compares the measured RCLD determined at 230 with a desired RCLD 205 (e.g., preprogrammed into the controller or received via communication with the surface). The comparison may, for example, include subtracting the measured build and turn rate values from the desired build and turn rate values (or alternatively subtracting the measured dogleg severity and tool face values from the desired values). The output may then be utilized to calculate new blade 132 positions (if necessary) at 215 . The blades 132 may then be reset to such new positions (also if necessary) at 220 prior to acquiring new survey readings at 225 and repeating the loop. It will be appreciated that control method 200 provides for (but does not require) closed loop control of the drilling direction. It will be seen from FIG. 3 that control over the drilling direction, as described above, relies only on the measured and required RCLD values (e.g., turn and build rates or dogleg severity and tool face).
Referring now to FIG. 4 , a diagrammatic representation of a portion of one exemplary embodiment of the downhole tool of FIG. 1 is illustrated. In the particular embodiment shown on FIG. 4 , each sensor set includes three mutually perpendicular gravity sensors, one of which is oriented substantially parallel with a longitudinal axis of the borehole and measures gravity vectors denoted as Gz 1 and Gz 2 for the upper and lower sensor sets, respectively. Likewise, each sensor set also includes three mutually perpendicular magnetic field sensors, one of which is oriented substantially parallel with a longitudinal axis of the borehole and measures magnetic field vectors denoted as Bz 1 and Bz 2 for the upper and lower sensor sets, respectively. Each set of gravity and magnetic field sensors may be considered as determining a plane (Gx, Bx and Gy, By) and pole (Gz, Bz) as shown.
The borehole inclination values (Inc 1 and Inc 2 ) may be determined at the upper 110 and lower 120 sensor sets, respectively, for example, as follows:
Inc1 = arctan ( Gx1 2 + Gy1 2 Gz1 ) Equation 1 Inc2 = arctan ( Gx2 2 + Gy2 2 Gz2 ) Equation 2
where G represents a gravity sensor measurement (such as, for example, a gravity vector measurement), x, y, and z refer to alignment along the x, y, and z axes, respectively, and 1 and 2 refer to the upper 110 and lower 120 sensor sets, respectively. Thus, for example, Gx 1 is a gravity sensor measurement aligned along the x-axis taken with the upper sensor set 110 .
Borehole azimuth values (Azi 1 and Azi 2 ) may be determined at the upper 110 and lower 120 sensor sets, respectively, for example, as follows:
Azi1 = arctan ( ( Gx1 * By1 - Gy1 * Bx1 ) * Gx1 2 + Gy1 2 + Gz1 2 Bz1 * ( Gx1 2 + Gy1 2 ) - Gz1 * ( Gx1 * Bx1 - Gy1 * By1 ) ) Equation 3 Azi2 = arctan ( ( Gx2 * By2 - Gy2 * Bx2 ) * Gx2 2 + Gy2 2 + Gz2 2 Bz2 * ( Gx2 2 + Gy2 2 ) - Gz2 * ( Gx2 * Bx2 - Gy2 * By2 ) ) Equation 4
where G represents a gravity sensor measurement, B represents a magnetic field sensor measurement, x, y, and z refer to alignment along the x, y, and z axes, respectively, and 1 and 2 refer to the upper 110 and lower 120 sensor sets, respectively. Thus, for example, Gx 1 and Bx 1 represent gravity and magnetic field sensor measurements aligned along the x-axis taken with the upper sensor set 110 . The artisan of ordinary skill will readily recognize that the gravity and magnetic field measurements may be represented in unit vector form, and hence, Gx 1 , Bx 1 , Gy 1 , By 1 , etc., represent directional components thereof.
The build and turn rates for the borehole may be determined from inclination and azimuth values, respectively, at the first and second sensor sets. Such inclination and azimuth values may be utilized in conjunction with substantially any known approach, such as minimum curvature, constant curvature, radius of curvature, average angle, and balanced tangential techniques, to determine the build and turn rates. Using one such technique, the build and turn rates may be expressed mathematically, for example, as follows:
BuildRate = Inc2 - Inc1 d Equation 5 TurnRate = Azi2 - Azi1 d Equation 6
where Inc 1 and Inc 2 represent the inclination values determined at the first and second sensor sets 110 , 120 , respectively (for example as determined according to Equations 1 and 2), Azi 1 and Azi 2 represent the azimuth values determined at the first and second sensor sets 110 , 120 , respectively (for example as determined according to Equations 3 and 4), and d represents the longitudinal distance between the first and second sensor sets 110 , 120 (as shown in FIG. 1 ).
Alternatively (as described above), the RCLD may be expressed in terms of dogleg severity and tool face. For example, using known minimum curvature techniques, dogleg severity and tool face may be expressed as follows:
ToolFace = arccos [ cos ( Inc1 ) cos ( D ) - cos ( Inc2 ) sin ( Inc1 ) sin ( D ) ] Equation 7 DogLeg = D d Equation 8
where:
D =arccos[cos(Azi2−Azi1)sin(Inc1)sin(Inc2)+cos(Inc1)cos(Inc2)] Equation 9
and where DogLeg represents the dogleg severity, ToolFace represents the tool face, Inc 1 and Inc 2 represent the inclination values determined at the first and second sensor sets 110 , 120 , respectively, Azi 1 and Azi 2 represent the azimuth values determined at the first and second sensor sets 110 , 120 , respectively, and d represents the longitudinal distance between the first and second sensor sets 110 , 120 .
As shown above in Equations 5 through 9, embodiments of this invention advantageously enable the build and turn rates (and therefore the RCLD) of the borehole to be determined directly, independent of the rate of penetration, total vertical depth, or other parameters that require communication with the surface. For example, if Inc 1 and Inc 2 are 57 and 56 degrees, respectively, and the distance between the first and second sensor sets is 33 feet, then Equation 5 gives a build rate of about 0.03 degrees per foot (also referred to as 3 degrees per 100 feet). Likewise, Equations 7 through 9 give a dogleg severity of about 0.03 degrees per foot at a tool face of zero degrees. It will be further appreciated by those of ordinary skill in the art that embodiments of this invention may be utilized in combination with substantially any known sag correction routines, in order to correct the RCLD values for sag of the downhole tool and/or portions of the drill string in the borehole.
With reference now to FIG. 5 , the RCLD of the borehole may alternatively be determined independent of direct azimuthal measurements, such as via magnetic field sensors (magnetometers). In such alternative embodiments, the RCLD may be determined using only gravity sensors. The difference in the azimuth values between the first and second sensor sets 110 , 120 may be determined from the gravity sensors, for example, as follows:
DeltaAzi = - Beta [ 1 + Inc1 Inc2 ] Equation 10
where DeltaAzi represents the difference in azimuth values between the first and second sensor sets 110 , 120 , Inc 1 and Inc 2 represent inclination values at the first and second sensor sets 110 , 120 , respectively (e.g., as given in Equations 1 and 2), and Beta is given as follows:
Beta = arctan ( ( Gx2 * Gy1 - Gy2 * Gx1 ) * Gx1 2 + Gy1 2 + Gz1 2 Gz2 * ( Gx1 2 + Gy1 2 ) +
Gz1 * ( Gx2 * Gx1 + Gy2 * Gy1 ) ) Equation 11
where Gx 1 , Gy 1 , Gz 1 , Gx 2 , Gy 2 , and Gz 2 represent the gravity sensor measurements as described above. The turn rate may then be determined, for example, as follows:
TurnRate = DeltaAzi d Equation 12
where DeltaAzi is determined in Equation 10 and d represents the longitudinal distance between the first and second sensor sets 110 , 120 , as shown in FIG. 1 . Alternatively, combining Equations 8 and 9, the dogleg severity may be expressed as follows:
DogLeg = arccos [ cos ( DeltaAzi ) sin ( Inc1 ) sin ( Inc2 ) +
cos ( Inc1 ) cos ( Inc2 ) ] d Equation 10
where DeltaAzi, Inc 1 , Inc 2 , and d are as defined above.
As described above with respect to FIGS. 1 and 2 , exemplary embodiments of this invention include a downhole tool having first and second sensor sets 110 , 120 deployed at a known longitudinal spacing thereon. However, it will be appreciated that other embodiments of this invention may include substantially any number of sensor sets. For example, downhole tools including three or more sensor sets deployed at a known longitudinal spacing may also be advantageously utilized. In such embodiments the RCLD of a borehole may be determined in a manner similar to that described above. It will also be appreciated that downhole tools including three or more sensor sets may be advantageous for certain applications in that they generally provide increased accuracy and reliability (although with a trade off being increased costs).
With reference now to FIG. 6 , an alternative embodiment of the control aspect of this invention is illustrated. Control method 300 on FIG. 6 is analogous to control method 200 on FIG. 3 in that it provides for (but does not require) closed loop control of the direction of drilling. As described above, the direction of drilling may be directly controlled by comparing measured and predetermined dogleg severity and tool face values. On FIG. 6 , dogleg severity and tool face values are determined at 380 and 345 , respectively, and compared to predetermined values at 310 and 350 , respectively. Such comparisons may be utilized to determine new blade positions 325 for the steering tool and thus to control the direction of drilling.
With continued reference to FIG. 6 , one exemplary embodiment of control method 300 is now described in more detail. At 310 a controller compares a measured dogleg severity (determined at 380 as described in more detail below) with a required dogleg severity 305 (e.g., preprogrammed into the controller or communicated to the controller from the surface). As also described above with respect to FIG. 3 , the comparison may, for example, include subtracting the measured dogleg severity from the required dogleg severity. The difference between the measured 380 and required 305 dogleg severity values may be utilized to determine a new offset value for the steering tool at 320 . In one exemplary embodiment, an offset value in 320 is determined such that the average dogleg severity calculated in 315 (e.g., along a predetermined section of the borehole) equals the required dogleg severity 305 . In one embodiment, the offset determined in 320 is the radial distance between the longitudinal axis of the steering tool and the longitudinal axis of the borehole. Such an offset is related (e.g., proportionally) to the dogleg severity and may be utilized to calculate new blade positions as shown at 325 . The blade positions may then be adjusted (if necessary) to the newly calculated positions at 330 .
In the exemplary embodiment shown, the lower sensor set may be deployed in the substantially non-rotating outer sleeve of a steering tool. As such, the upper and lower sensor sets may rotate relative to one another about the longitudinal axis of the downhole tool (e.g., axis 50 in FIG. 1 ). In such configurations it may be advantageous to determine one of the two control parameters (e.g., tool face) independent of the upper sensor set (e.g., sensor set 110 in FIG. 1 ) as shown in the exemplary embodiment of control method 300 on FIG. 6 . The position (e.g., displacement from the reset position) of the blades may be determined at 335 and utilized to determine a local borehole diameter and the relative position of the steering tool in the borehole. Accelerometer inputs from the lower sensor set may then be received at 340 and utilized to determine the tool face of the steering tool 345 (and therefore the borehole).
With continued reference to FIG. 6 , a controller compares 350 the measured tool face (determined at 345 ) with a required tool face 355 (e.g., preprogrammed into the controller or received via communication with the surface). The difference between the measured 345 and required 355 tool face values may be utilized to determine a new tool face value for the steering tool at 365 . In one exemplary embodiment, the new tool face value at 365 is determined such that the average tool face calculated at 360 (e.g., along a predetermined section of the borehole) equals the required dogleg severity 355 . At 370 an inclination value may be determined at the steering tool from the accelerometer readings received at 340 . An inclination value may also be received from an upper sensor set (e.g., from an MWD tool) at 375 . Such inclination values and the tool face calculated at 345 may be utilized to determine a dogleg severity at 380 . For example, in one embodiment, the tool face and inclination values may be substituted into Equation 7, which may then, along with Equation 8, be solved for the dogleg severity of the borehole. Returning to 310 the controller may then compare the measured dogleg severity 380 to the required value 305 and repeat the loop.
It will be appreciated that embodiments of this invention may be utilized to control the direction of drilling over multiple sections of a well (or even, for example, along an entire well plan). This may be accomplished, for example, by dividing a well plan into two or more sections, each having a distinct RCLD. Such a well plan would typically further include predetermined inflection points (also referred to as targets) between each section. The targets may be defined by substantially any method known in the art, such as, for example, by predetermined inclination, azimuth, and/or measured depth values. In one exemplary embodiment, a substantially J-shaped well plan may be separated into three sections with a first target between the first and second sections and a second target between the second and third sections. For example, a substantially straight first section (e.g., with an inclination of about 30 degrees) may be followed by a second section that simultaneously builds and turns (e.g., at a tool face angle of about 45 degrees and dogleg severity of about 5 degrees per 100 feet) to a substantially horizontal third section (e.g., having an inclination of about 90 degrees). Such a J-shaped well plan is disclosed by way of illustration only. It will be appreciated that this invention is not limited to any number of well sections and/or intermediary targets.
During drilling of a multi-section borehole, the drilling direction may be controlled in each section, for example, as described above with respect to FIG. 6 . Upon reaching a target, the controller may be reprogrammed to steer subsequent drilling in another direction (e.g., a predetermined direction required to reach the next target). The controller may be reprogrammed in substantially any manner. For example, a new RCLD (e.g., tool face and dogleg severity) may be transmitted from the surface to the controller. Alternatively, the controller may be preprogrammed to include a predetermined RCLD for each section of the well plan. In such an alternative embodiment the controller may be instructed to increment to the next RCLD. Subsequent drilling may proceed in this manner through substantially any number of sections until, if so desired, the borehole is complete. It will also be appreciated that the controller may be programmed to automatically increment to another RCLD upon reaching a predetermined target. For example, upon achieving certain predetermined inclination and/or azimuth values, the controller may automatically increment to the next RCLD. In this manner, an entire borehole may potentially be drilled according to a predetermined well plan without intervention from the surface. Surface monitoring may then be by way of supervision of the downhole-controlled drilling. Alternatively, directional drilling can be undertaken, if desired, without communication with the surface.
It will be understood that the aspects and features of the present invention may be embodied as logic that may be processed by, for example, a computer, a microprocessor, hardware, firmware, programmable circuitry, or any other processing device well known in the art. Similarly the logic may be embodied on software suitable to be executed by a processor, as is also well known in the art. The invention is not limited in this regard. The software, firmware, and/or processing device may be included, for example, on a downhole assembly in the form of a circuit board, on board a sensor sub, or MWD/LWD sub. Alternatively the processing system may be at the surface and configured to process data sent to the surface by sensor sets via a telemetry or data link system also well known in the art. Electronic information such as logic, software, or measured or processed data may be stored in memory (volatile or non-volatile), or on conventional electronic data storage devices such as are well known in the art.
Although the present invention and its advantages have been described in detail, it should be understood that various changes, substitutions and alternations can be made herein without departing from the spirit and scope of the invention as defined by the appended claims. | A method for determining a rate of change of longitudinal direction of a subterranean borehole is provided. The method includes positioning a downhole tool in a borehole, the tool including first and second surveying devices disposed thereon. The method further includes causing the surveying devices to measure a longitudinal direction of the borehole at first and second longitudinal positions and processing the longitudinal directions of the borehole at the first and second positions to determine the rate of change of longitudinal direction of the borehole between the first and second positions. The method may further include processing the measured rate of change of longitudinal direction of the borehole and a predetermined rate of change of longitudinal direction to control the direction of drilling of the subterranean borehole. Exemplary embodiments of this invention tend to minimize the need for communication between a drilling operator and the bottom hole assembly, thereby advantageously preserving downhole communication bandwidth. | 4 |
CROSS-REFERENCE TO RELATED APPLICATIONS
[0001] This application claims the priority right of our prior co-pending provisional application Ser. No. 60/703,125 filed Jul. 27, 2005.
BACKGROUND OF THE INVENTION
[0002] I. Field of the Invention
[0003] This invention relates to the production of metal sheet articles (and particularly foils) having a hydrophilic surface (i.e. a surface that is wettable by a polar liquid, e.g. water). More particularly, the invention relates to methods of imparting wettability to surfaces of sheet articles made of aluminum and aluminum alloys.
[0004] II. Background Art
[0005] Aluminum sheet articles, and particularly aluminum foils (flexible sheets having a thickness in the range of 0.0002 to 0.004 inch), are often required to have fully wettable surfaces for compatibility with various user applications. For example, finstock sheet (which normally has a thickness of 0.004 inch or more) must have a fully wettable surface to allow for proper water drainage in condensers. Sheets having a thickness of 0.002 inch or more are often required to have wettable surfaces to avoid staining in water. Furthermore, metal foils are often intended to be directly printed with inks or directly painted, and this requires wettable surfaces.
[0006] Even more importantly, metal foils may used with other materials to form the basis of multi-layer sheets by direct application of coating materials or by lamination (e.g. lamination with paper, polyester, vinyl or other plastics). Foils of this type are often referred to as “converter foils” because they are destined to be “converted” by customers to a multi-layer sheet or composite (e.g. after passing through a laminator where the foil is sandwiched with another supporting material). The main applications for converter foils are as flexible packaging and sheets required in industrial applications. Converter foils are often made from 1000-series aluminum alloys, e.g. AA1145 and AA1100, and are usually supplied in gauges from 0.0002 to 0.005 inches, so they are consequently quite thin and easy to damage. The surfaces of converter foils should be wettable by aqueous and polar materials, and should be of good appearance, especially when the foils are to be used for packaging purposes. The wettability of the surfaces determines the peel strength of the composites and is therefore a characteristic that requires strict control. The users of the foil normally require full wettability of the surface (so-called “A-wettable” surface quality). However, this is difficult to achieve. Surface wettability is adversely affected by the presence of lubricating oils that are always present on the surfaces of the foils in the condition in which they are obtained from the rolling mill (oils are used in the metal rolling process). To improve adhesion, it is necessary to remove oils from the surface before the foils are supplied to customers of the metal fabricator for coating or lamination procedures.
[0007] A conventional way of removing surface oils and improving surface wettability is to subject sheet article to a prolonged heat treatment (heat anneal) in a furnace at a temperature above 280° for a period of 24-48 hours. Such extended annealing cycles are needed to fully evaporate the oil, but they cause recrystallization of the metal and necessarily convert them to the O-temper (alloys such as AA1145 and AA1100 are completely recrystallized at these temperatures). Foils in the O-temper are quite soft, and are therefore unsuitable, or less desirable, in some applications. Lesser degrees of crystallization require lower temperatures and/or shorter treatment times, but then complete removal of the oil cannot be assured. Thus, the practical result is that the requirement for wettability has limited the application of converter foils, for example, predominantly to O-temper material. It has also resulted in anneal cycles that are significantly longer than those used in other applications, such as the production of plate, fins or containers. If stronger foils or sheets were available, it would reduce damage, and open up the possibility of reducing gauges for many converter applications.
[0008] Chemical cleaning methods are also available to remove surface oil and thereby render the foil or sheet water-wettable. Such methods can be very expensive as they require the use of cleaning towers through which the foil or sheet is processed. Foil, being very thin, can be easily damaged while being processed through this kind of equipment, so maximum speed of travel and other restrictions are strictly enforced, with a consequent reduction of efficiency. Additionally, the chemical pre-treatments may contain chromates, phosphates and other chemicals that can cause the brightness of the foil or sheet to diminish, which is extremely detrimental in converter applications.
[0009] U.S. Pat. No. 2,197,405, issued on Apr. 16, 1940 to Junius D. Edwards, discloses a method of treating aluminum surfaces prior to joining other materials thereto by means of adhesives. This involves the treatment of aluminum surfaces with phosphoric acid or a solution of phosphoric acid in water.
[0010] However, there is a need for improved ways of making the surfaces of aluminum foils wettable without involving prolonged heating cycles.
SUMMARY OF THE INVENTION
[0011] An exemplary form of the invention provides a method of treating a surface of a sheet of aluminum or an aluminum alloy to make the surface wettable, the method comprising: applying a solution of phosphoric acid in a solvent to the surface, the solvent being selected from the group consisting of (a) a polar, non-aqueous, water-free solvent, and (b) a mixture of a polar, non-aqueous, water-free solvent and a volatile polar hydrocarbon solvent; and removing the solvent by drying the surface at ambient temperature or by heating the surface at an elevated temperature above ambient, with the proviso that the elevated temperature does not fall in the range of 130 to 240° C.
[0012] The phosphoric acid is preferably contained in the solution at a concentration such that the phosphoric acid contacts the surface in an amount of 0.5 to 2.0 mg/ft 2 , and is preferably applied to the surface in an amount of at least 10 mg/ft 2 .
[0013] The invention also relates to a metal foil treated by the method above.
BRIEF DESCRIPTION OF THE DRAWINGS
[0014] FIG. 1 is a schematic diagram showing steps in a preferred method according to the present invention.
DETAILED DESCRIPTION OF THE INVENTION
[0015] It will be appreciated that the term “aluminum” as used in the following is intended to include alloys of aluminum, particularly those used for the formation of converter foil, as well as pure aluminum itself.
[0016] In the following description, reference is made to aluminum foil for the sake of convenience, but the description applies to other sheet articles made of aluminum (except where foil alone is clearly intended by the context).
[0017] In the present invention, use is made of a solution containing phosphoric acid to impart substantially complete wettability to the surfaces of aluminum foils. The foils are generally not pre-treated or pre-cleaned before the application of the solution, and consequently they are treated in the form in which they are received directly from the rolling operation or rolling mill. The treatment solution consists of phosphoric acid dissolved in a water-free polar solvent, preferably isopropanol, and the concentration of phosphoric acid is made quite low. Ideally, the concentration of the solution is such that the amount of phosphoric acid applied to the surface (referred to as the “loading” of phosphoric acid on the surface) is within the range of 0.5 to 2.0 mg per square foot of treated surface, and more preferably 0.5 to 21.5 mg/ft 2 . If the loading is less than 0.5 mg/ft 2 , then uniform wettability over the entire surface of the foil cannot be guaranteed in all cases. If the loading is more than 2.0 mg/ft 2 , the resulting surface quality is poor in many cases. While the loading is, of course, dependent on the amount of solution applied to a surface, as well as to the concentration of the solution, the amount applied is normally constant because excess liquid drains from the surface, so the loading tends to be dependent mainly on concentration.
[0018] The solution may be applied to the foil surfaces by any means, but is preferably applied by means that are compatible with high-speed processing and that leave the foil surface with an undamaged, high-quality finish. Ideally, the method employed is one that avoids direct mechanical contact of a solid article with the foil surface. The method may thus comprise dipping, spraying or coating. The most preferred method is spraying, ideally aerated spraying or ultrasonic spraying (i.e. ultrasonic liquid atomization in which high-frequency sound waves are used to produce a spray of atomized liquid). Ultrasonic spraying has the advantages that it can produce a soft (i.e. small droplet), low-velocity spray that virtually eliminates overspray and cannot damage the foil surface. Ultrasonic spraying also has the advantage that it employs a pressureless operation, and provides freedom from clogging of the spray jets.
[0019] While the application of the solution is not intended to “wash-away” the oil present on a surface (e.g. by producing a significant run-off), the solution must be applied in an amount (and pattern of application) sufficient to ensure 100% coverage of the surface to be treated. This generally means that the rate of application of the solution must be at least 10 mg/ft 2 of treated surface. If it is less than this, full wettability cannot be guaranteed in all cases. However, the solution is preferably applied in an amount of no more than 30 mg/ft 2 to avoid run-off and over-utilization of materials.
[0020] The preferred minimum and maximum loading of phosphoric acid and the preferred minimum and maximum application of the solution define the concentration of phosphoric acid required in the solution employed. For example, if the phosphoric acid loading is to be the minimum of 0.5 mg/ft 2 and the solution application is to be a maximum of 30 mg/ft 2 , the concentration of phosphoric acid in the solution should be 1.66 wt %. If the phosphoric acid loading is to be the maximum of 2.0 mg/ft 2 and the solution is applied at the minimum of 10 mg/ft 2 , the concentration should be 20 wt %. An effective range of concentrations is therefore 1.66 to 20% (w/w), more preferably 1.66 to 5% (w/w).
[0021] The solution is preferably applied at ambient temperature and the foil or sheet itself should preferably be held at low temperature (ambient to at most 50° C.). The solution should preferably be kept in contact with the foil surface at ambient temperature for a holding period of at least 30 seconds before a heating or drying step, described below, is carried out. During this time period, the foil may be coiled. There is no particular maximum time during which the solution may be left in this way in contact with the foil surface, but the heating or drying step is preferably commenced as quickly as possible, so the process should preferably be continued as soon as possible after the 30 second holding period.
[0022] Without wishing to be bound by a particular theory of operation, it is believed that the surface is made wettable by this method for the following reasons. Phosphoric acid is soluble in polar solvents such as alcohols, ketones and a few other organic solvents. The solvents are able to penetrate through the layer of oil on the foil surface and reach the bare surface of aluminum where the phosphoric acid can then act to improve wettability. The acid reacts with the aluminum surface, particularly when the solvent escapes by evaporation (see later) leaving a concentrated layer of phosphoric acid, thereby producing a wettable phosphate layer that renders the surface hydrophilic. A similar effect is not present in water-based or water-containing solutions, as such solutions do not penetrate the oil layer and wet the foil surface. Further, if such solutions were made to wet the surface, e.g. by adding surfactants, they would not dry quickly enough to concentrate the acid in the available time. Water can also undesirably stain the surface of aluminum. While the method of the invention may leave residual oil on the foil surface, it is found that the residual oil is generally incorporated into any coating materials (particularly organic polymers) that are subsequently applied. Moreover, as the oil has been rendered less adherent to the foil surface by the polar solvent, it will evaporate at a lower temperature than otherwise required.
[0023] The preferred polar solvents for use in the present invention are isopropanol, ethanol and methyl ethyl ketone (MEK) as they have suitable ability to penetrate the oil layer and a good rate of evaporation. As noted, the solutions employed are always water-free. Methanol and acetone are also effective, but they are toxic, so if they are used, special precautions have to be taken to avoid contamination of the environment, and this reduces the economic desirability of using these solvents in the process.
[0024] It is also possible to replace part of the polar solvent with a non-polar solvent of low volatility that is totally miscible with the acid polar solvent mixture, such as, for example, a solvent sold under the trademark NORPAR® 13 (a carbon-hydrogen saturated hydrocarbon with an average of 13 carbon atoms and having an initial boiling point of about 222° C. and a dry point of 242° C.) marketed by ExxonMobil Chemical Company. In such a case, the polar solvent may be substituted with the non-polar solvent in the range of 0% to 80% by volume, more preferably 0 to 20% by volume. This increases the volatility of the solution, which is beneficial when applying the mixture onto the metal sheet. However, a disadvantage is greater solvent removal during annealing, so this alternative may not be desirable for all cases.
[0025] Following the application of the solution and coiling (if coiling is desired), the foil is subjected to a heating or drying step. This may take one of two forms, or a combination of both. One form is a low temperature treatment that involves drying the foil at ambient temperature or heating the foil at a temperature above ambient but no higher than 130° C. Drying or heating at such a temperature causes evaporation of any residual polar solvent, but does not cause any annealing of the metal of the sheet or foil. A fully-hardened sheet or foil (i.e. one having a cold-rolled temper) may therefore be obtained by this form of heating or drying. The heating or drying time may be the minimum required to achieve full evaporation of the solution (which may be several hours if the foil is in coil form). Longer heating times are not required, but would not be harmful as the structure of the metal is not changed by the applied temperature. As an example, the sheet or foil may be kept at 100° C. for 4 to 5 hours, which is just adequate to evaporate all of the isopropanol when this material is used as the polar solvent and the foil is treated in the form of a coil having a weight of 2000 pounds.
[0026] Alternatively, in a second form of the heating or drying procedure, which may be referred to as a high temperature treatment, the heating may be carried out at a temperature of 240° C. or above). At this temperature, not only is the polar solvent evaporated fully, but the metal may be partially or fully annealed. If a “fully hard” foil is still required, the heating time should be maintained for just long enough to remove the polar solvent but not long enough to influence the properties of the foil. This may require, for example, 3 to 4 hours at 240° C. Alternatively, if the foil is to be “fully soft”, then heating periods of 8 to 16 hours may be employed at temperatures above 240° C. This period of heating is more than adequate to evaporate the solvent, but is required to achieve the desired metallurgical properties.
[0027] Unless a full O-temper is required, the treatment temperature should normally be kept below about 280° C. and the treatment time adjusted accordingly. The treatment time must again be the minimum time required to achieve full evaporation of the solvent, but more time may be required to achieve a desired metal temper. This makes it possible to obtain partially annealed tempers that can yield significantly stronger foil than the totally recrystallized metal.
[0028] In the case of the high temperature treatment, the maximum temperature should generally not exceed 400° C. as this may cause deterioration of the shape of the coil and other damage to the foil itself.
[0029] If desired, both the low temperature form of heating (drying) and the high temperature form may be carried out sequentially. In other words, heating at a temperature of 130° C. or less may be carried out to fully evaporate the polar solvent and to allow the phosphoric acid to work on the surface to make it wettable. The foil may then be heated at a temperature of 240° C. or more to produce a desired transformation of the metal temper. If appropriate, the foil may be stored for an indefinite period of time, ideally in the coiled condition, between these two forms of heating.
[0030] Heating at a temperature in the intervening range of 130-240° C., i.e. between the temperatures employed in the low and high temperature forms, is to be avoided (except for the brief time the foil takes to heat up to 240° C.) because foil heated at temperatures within this range become hydrophobic and the use of such temperatures is thus counter-productive. Heating rates normally employed to raise the temperature to the range employed in the second form do not result in harmful residence times in the intervening range, so no special concern about heating rates is required, provided the temperature is allowed to rise without interruption through the intervening range.
[0031] FIG. 1 of the accompanying drawings sets out the steps of the method in more graphic form. The FIGURE is believed to be self-explanatory, except that “ALTERNATIVE A” shows the option of heating (drying) at 130° C. or less, and “ALTERNATIVE B” shows the option of heating at 240° C. or above.
[0032] The invention is further illustrated by the following Examples, which are not intended to be limiting.
COMPARATIVE EXAMPLE 1
[0033] H19 aluminum foil of 0.002 inch gauge was immersed in isopropanol and the excess was removed by shaking. After one minute at ambient temperature in air, the foil was rendered dry. The wettability of the foil was tested by placing a drop of water on the surface. It was completely non-wettable.
COMPARATIVE EXAMPLE 2
[0034] H19 aluminum foil was placed in an oven at 100° C. and was heated for 40 seconds. It was completely non-wettable.
EXAMPLE 1
[0035] H19 foil was treated with 0.05% (w/w) solution of phosphoric acid in isopropanol. The aluminum sample was immersed in this solution, removed and the excess was then removed by shaking. The foil was then air-dried. The foil became A-wettable. The application of the solution to the surface was about 2 g per square foot. This means that about 0.4 mg per square foot of acid was left on the foil surface after evaporation of the solvent.
EXAMPLE 2
[0036] The foil produced in Example 3 was heated at 100° C. for periods of 40 seconds to 2 hours. It remained wettable.
COMPARATIVE EXAMPLE 3
[0037] The foil produced in Example 3 was heated at 200° C. The sample then became non-wettable.
EXAMPLE 3
[0038] A solution of 44 vol % NORPAR®, 54 vol % water and 2 vol % phosphoric acid solution was sprayed onto a non-wettable aluminum foil. The foil became hydrophilic after one minute. | A method of treating a surface of a metal foil or sheet to make the surface wettable. The method comprises obtaining a metal foil or sheet having an oil-coated surface to be treated, applying a solution of phosphoric acid in a polar, non-aqueous, water-free solvent evenly to the surface at a rate of application in a range of at least 10 mg/ft 2 , the phosphoric acid being contained in the solution at a concentration such that the phosphoric acid contacts the surface in an amount of 0.5 to 2.0 mg/ft 2 ; and removing the solvent by either drying the surface or heating the foil or sheet at an elevated temperature above ambient to evaporate the oil from the surface to be treated with the proviso that the elevated temperature does not fall in the range between 130 to 240° C. The resulting foil has a wettable surface and can be used, for example, for coating with a layer of another material (e.g. polymer or adhesive) and achieve high peel strength. | 2 |
FIELD OF THE INVENTION
[0001] The present invention is directed to methods of treating hepatic fibrosis in humans.
BACKGROUND OF THE INVENTION
[0002] Progressive fibrosis of liver often results in organ failure leading to death or the need for transplantation. These diseases affect hundreds of millions in the United States and worldwide [1]. For example, hepatic fibrosis is the leading non-malignant gastrointestinal cause of death in the United States. Moreover, it has been increasingly recognized that progression of fibrosis is the single most important determinant of morbidity and mortality in patients with chronic liver disease [2].
[0003] There has been remarkable progress in elucidating the cellular basis of fibrosis in liver, kidney and lung. In liver, activation of resident mesenchymal cells known as “stellate cells” is a key event [3]. Activation represents a transformation to a myofibroblast-like cell that is proliferative, fibrogenic and contractile. The extent of fibrosis is directly related to the numbers of these fibrogenic activated stellate cells.
[0004] It has been previously demonstrated that activation and proliferation of hepatic stellate cells (HSC) in liver injury is associated with de novo expression of many cytokine receptors, including beta platelet-derived growth factor receptor (β-PDGFR) [4]. β-PDGF receptor expression in injured liver is largely confined to these activated mesenchymal cells; the rare large arteries within the parenchyma are the only other site within the organ. Thus, the extent of P-PDGF receptor expression parallels the mass of activated stellate cells, which in turn reflects the extent of fibrosis. Moreover, reduction in fibrosis is accompanied by diminished numbers of such activated cells [5].
[0005] Recent advances in anti-inflammatory arid-anti-fibrotic therapies offers the prospect of delaying these outcomes, but to date there are no approved antifibrotic therapies, leaving hundreds of millions of patients worldwide who have chronic liver disease with no therapeutic options apart from the possibility of liver transplantation. Currently only a single trial of antifibrotic therapy is underway (gamma interferon), and the hepatology community and pharmaceutical sector anxiously await results from this trial, as several other putative antifibrotics agents are in development by a number of companies. There has been growing recognition and enthusiasm for the prospect of treating hepatic fibrosis [6]. Thus, there is a large untapped market that is highly receptive to this new approach to treating liver fibrosis.
[0006] The development of imatinib mesylate (GLEEVE™) represented an important milestone in the treatment of chronic myelogenous leukemia (CML), since this small molecular inhibitor of the BCR-ABL oncogene product, the key molecular abnormality in this cancer, is remarkably safe and effective [7-9]. The drug is also effective in CML associated with rearrangements of the β-PDGF receptor [10]. Thus, thousands of patients have been safely treated with modest drug resistance reported. More recently, the drug has been approved for the treatment of GI Stromal tumors, mesenchymal cell neoplasms of the intestinal tract [11]. Of importance, this agent not only blocks the BCR-ABL receptor tyrosine kinase protein, but it has inhibitory activity across a number of related receptor tyrosine kinases, including β-PDGF receptor, a key mediator of stellate cell activation in hepatic fibrosis[12]. Indeed, a recent report has begun to examine the potential impact of GLEEVEC™ on hepatic fibrosis in a rodent model of bile duct obstruction, a standard model used in the field[13].
SUMMARY OF THE INVENTION
[0007] It has now been unexpectedly discovered that GLEEVEC™ can be used as a treatment for patients suffering from hepatic fibrosis based on its ability to downregulate stellate cell activation in culture and in vivo. This includes but is not limited to patients with chronic Hepatitis B, Hepatitis C, non-alcoholic steatophepatitis (NASH), alcoholic liver disease, metabolic liver diseases (Wilson's disease, hemochromatosis), biliary obstruction (congenital or acquired) or liver diseases associated with fibrosis of unknown cause.
[0008] In one aspect, the present invention provides a method for treating hepatic fibrosis comprising administering to a patient in need of such treatment an amount effective to treat hepatic fibrosis of imatinib mesylate.
[0009] This and other aspects of the present invention will be apparent to those of ordinary skill in the art in light of the present specification and appended claims.
DETAILED DESCRIPTION OF THE INVENTION
[0010] In the discussions below, the term “about” or “approximately” means within an acceptable error range for the particular value as determined by one of ordinary skill in the art, which will depend in part on how the value is measured or determined, i.e., the limitations of the measurement system, i.e., the degree of precision required for a particular purpose, such as a pharmaceutical formulation. For example, “about” can mean within 1 or more than 1 standard deviations, per the practice in the art. Alternatively, “about” can mean a range of up to 20%, preferably up to 10%, more preferably up to 5%, and more preferably still up to 1% of a given value. Alternatively, particularly with respect to biological systems or processes, the term can mean within an order of magnitude, preferably within 5-fold, and more preferably within 2-fold, of a value. Where particular values are described in the application and claims, unless otherwise stated the term “about” meaning within an acceptable error range for the particular value should be assumed.
[0011] Presented below is an overview of the pathogenesis of hepatic fibrosis and the role of the activated hepatic stellate cell.
[0012] The hepatic scar consists of a broad accumulation of extracellular matrix (ECM), which includes the macromolecules that comprise the scaffolding of normal and fibrotic liver. These macromolecules consist of three main families: collagens, glycoproteins, and proteoglycans. As the normal liver becomes fibrotic, significant qualitative and quantitative changes occur in the ECM. The content of collagens and noncollagenous components increases three- to fivefold in cirrhotic compared with normal liver. Moreover, the type of subendothelial ECM shifts from low-density basement membrane-like matrix to an interstitial type, which is rich in type I, or fibrillar collagen.
[0013] HSCs and their related cell types (e.g., “myofibroblasts”) are the major cellular source of hepatic ECM in the injured liver. HSCs are located in the subendothelial space of Disse between sinusoidal endothelium and hepatocytes (14). They represent a pericytic cell type with the potential for conversion to a “myofibroblast,” similar to mesangial cells in the kidney, pulmonary mesenchymal cells, and stellate cells in the pancreas [17].
[0014] In liver injury of any type, HSCs undergo activation, which connotes the transition from a quiescent vitamin A-rich cell to a proliferative, highly fibrogenic, and contractile cell with reduced vitamin A content. HSC activation begins almost immediately after the onset of liver injury and progresses through a continuum of cellular and molecular events that can lead to sustained scar accumulation. Alternatively, resolution of fibrosis and loss of activated HSCs through reversion or apoptosis may occur if the injury is self-limited [18].
[0015] A conceptual framework of HSC activation delineates the response of the cell into two discrete phases: initiation and perpetuation (15) [14]. Initiation refers to early changes in gene expression and phenotype that enable the cells to respond to other cytokines and stimuli. Factors provoking initiation are largely derived from neighboring cells and include reactive oxygen species and specific matrix proteins (e.g., cellular fibronectin) derived from sinusoidal endothelium. Perpetuation results from the effects of these stimuli on maintaining the activated phenotype to generate scar. Perpetuation can be further subdivided into several discrete changes in cell behavior that include proliferation, contractility, fibrogenesis, matrix degradation, chemotaxis, retinoid loss, and leukocyte chemoattraction. As noted previously, it is important to recognize that the HSC is continuously evolving during progressive liver injured and fibrosis. Finally, resolution of HSC activation is increasingly appreciated and represents an essential step toward reversibility of fibrosis.
[0000] Proliferation
[0016] β-platelet-derived growth factor (β-PDGF) is the most potent and first stellate cell mito-en identified. Induction of β-PDGF receptors early in HSC activation confers responsiveness to this mitogen, which is minimally active toward quiescent stellate cells [19]. A host of other mitogens are also active toward stellate cells, including thrombin, vascular endothelial cell growth factor (VEGF), and fibroblast growth factor (FGF), among others [16].
[0000] Contractility
[0017] Contractility of HSCs may be a major determinant of increased portal resistance during liver fibrosis, though a role for HSC contracatility has not been established in normal liver blood flow regulation [20]. The major contractile stimulus toward HSCs is endothelin-1. Endothelin receptors are expressed on both quiescent and activated HSCs, but their subtype distribution changes from predominantly “A” to “B” isoform as cells activate, leading to altered cellular responses to this growth factor. Additionally, increased activation of proendothelin by endothelin-converting enzyme yields more active cytokine [21].
[0000] Fibrogenesis
[0018] Increased matrix production by activated HSCs occurs in response to fibrogenic mediators released during liver injury. The most potent stimulus to matrix production is transforming growth factor (TGF)-β1, which is derived from both paracrine and autocrine sources and has a complex and tightly regulated mechanism of activation to control availability of the active cytokine. A fibrogenic role has also been uncovered for connective tissue growth factor (CTGF), a TGF-β1-stimulated gene that stimulates matrix production by HSCs [22]. Additionally, leptin, a 16-kD hormone initially identified in adipose tissue, appears to be necessary for fibrogenesis because leptin-deficient animals lack the ability to accumulate scar following toxic liver injury [29, 24]. Interestingly, HSCs generate their own leptin and express signaling receptors for the hormone as they activate, providing the components of an autocrine loop. Fibrogenic actions of leptin may be particularly important in patients who are obese, because circulating leptin levels correlate closely with adipose mass and are significantly elevated in these individuals. Thus, elevated leptin levels may contribute to the fibrosis increasingly associated with fatty liver and NASH in obese patients.
[0000] Matrix Degradation
[0019] Quantitative and qualitative changes in matrix protease activity play an important role in ECM remodeling accompanying fibrosing liver injury and are largely orchestrated by HSCs [12]. In progressive fibrosis, the balance between matrix production and matrix degradation clearly favors production, through both increased fibrogenesis and inhibition of matrix degradation. A large family of matrix-metalloproteinases (MMP) has been characterized that specifically degrade collagens and noncollagenous substrates. In particular, HSCs are a key source of MMP-2, as well as stromelysin/MMP-3, both of which degrade constitutents of the normal subendothelial matrix and hasten its replacement by fibrillar collagen. Importantly, through the activation of tissue inhibitor of metalloproteinases-1 and -2 (TIMP-1 and -2), activated HSCs can also inhibit the activity of interstitial collagenases that degrade fibrillar collagen, thus favoring the accumulation of fibrillar matrix [26].
[0000] Chemotaxis
[0020] HSCs can migrate toward cytokine chemoattractants, an action that is characteristic of wound-infiltrating mesenchymal cells in other tissues as well. Chemotactic mediators include PDGF and monocyte chemoattractant protein-1 (MCP-1) [27, 28].
[0000] Retinoid Loss
[0021] As HSCs activate, they lose their characteristic perinuclear retinoid (vitamin A) droplets and acquire a more fibroblastic appearance. This pathway remains a somewhat mysterious aspect of HSC activation because it is unclear whether retinoid loss is required for HSC activation to proceed. If so, inhibitors of retinoid loss, once identified, might be used to antagonize HSC activation.
[0000] Leukocyte Chemoattractant and Cytokine Release
[0022] Increased production or activity of cytokines may be critical for both autocrine and paracrine perpetuation of HSC activation. Increasingly, it appears that all key cytokines acting upon activated HSCs are autocrine, suggesting that therapeutic efforts that antagonize HSC activation must reach the subendothelial milieu to be active. Additionally, HSCs can amplify the inflammatory response by inducing infiltration of mono- and polymorphonuclear leukocytes through release of chemoattractants.
[0000] Imatinib Mesylate
[0023] GLEEVEC™ is available in capsule or film coated tablet form and each form (capsule or tablet) contains imatinib mesylate equivalent to 100 mg or 400 mg of imatinib free base. Imatinib mesylate is designated chemically as 4-[(-phenyl)benzamide methanesulfonate and its structural formula is 4-Methyl-1-piperazinyl)methyl[-N-[4-methyl-3-[[4-(3-pyridinyl)-2-pyrimidinyl]amino]-phenyl]benzamide methanesulfonate.
[0024] Imatinib mesylate is a protein-tyrosine kinase inhibitor that inhibits the Bcr-Abl tyrosine kinase, the constitutive abnormal tyrosine kinase created by the Philadelphia chromosome abnormality in chronic myeloid leukemia (CML). It inhibits proliferation and induces apoptosis in Bcr-Abl positive cell lines as well as fresh leukemic cells from Philadelphia chromosome positive chronic myeloid leukemia. In colony formation assays using ex vivo peripheral blood and bone marrow samples, imatinib shows inhibition of Bcr-Abl positive colonies from CML patients.
[0025] In vivo, it inhibits tumor growth of Bcr-Abl transfected murine myeloid cells as well as Bcr-Abl positive leukemia lines derived from CML patients in blast crisis.
[0026] Imatinib is also an inhibitor of the receptor tyrosine kinases for platelet-derived growth factor (PDGF) and stem cell factor (SCF), c-kit, and inhibits PDGF- and SCF-mediated cellular events. In vitro, imatinib inhibits proliferation and induces apoptosis in gastrointestinal stromal tumor (GIST) cells, which express and activating c-kit mutation.
[0027] Amounts of GLEEVEC™ effective to treat hepatic fibrosis would broadly range between about 50 mg and about 600 mg per day and preferably between about 50 mg and about 200 mg per day administered orally. The rationale for this preferred dose range is based on FDA-approved GLEEVEC™ dosing for CML and gastrointestinal stromal tumors (GIST), which are 400 mg and 600 mg per day, respectively. Whereas treatment of CML and GIST require high doses of GLEEVEC™ in order for the drug to reach its targets (bone marrow and the tumor), the liver should be effectively targeted with lower doses because of relatively high concentrations of drug in liver following its oral administration and absorption in the intestine. These lower GLEEVEC™ doses should minimize the risk of toxicity both in liver and other organs. Since liver fibrosis is a disease resulting from chronic liver injury, treatment with GLEEVEC™ over a person's lifetime is envisioned, either alone or in conjunction with therapies aimed at eradicating or reducing the cause of chronic liver injury, for example with antiviral medications such as alpha interferon (Hoffman LaRoche, Nutley, N.J., Schering-Plough, Kenilswirth, N.J.).
[0028] There is a huge potential economic impact of establishing a treatment for hepatic fibrosis. Currently there are over 4 million patients with chronic HCV infection in the United States (up to 1-2% of the population) and all are at risk for fibrosis and cirrhosis. Conservative estimates indicate that up to 100 million people may be infected worldwide. Moreover, chronic Hepatitis B, schistosomiasis, and immune diseases affect hundreds of millions more, particularly in the Far East and Africa. With steady advances in the understanding of hepatic fibrosis, the medical and patient communities are now anxiously awaiting progress in its treatment and are quite receptive to the prospect.
[0029] Currently there are no approved treatments for hepatic fibrosis in patients with chronic liver disease despite the rapidly accelerating worldwide morbidity from this disease. GLEEVEC™ has the unique advantages of a large amount of safety data already generated with excellent safety profile, and oral availability making delivery to the liver highly efficient and allowing the use of decreased doses that minimize toxicity. Moreover, a vast amount of pharmacokinetic and clinical information has been amassed for this drug.
[0030] The present invention is described below in examples which are intended to further describe the invention without limiting its scope.
EXAMPLES
Use of GLEEVEC™ as an Antifibrotic Therapy
[0031] Patients will be treated with GLEEVEC™ (imatinib mesylate) who have evidence of liver fibrosis (scarring) as seen on liver biopsy. Typically, these are patients with chronic Hepatitis C, Hepatitis B, autoimmune hepatitis, metabolic diseases or fatty liver and scarring seen with obesity, but any chronic liver disease associated with fibrosis will be an indication. Doses will range from 50 mg to 200 mg per day, with 100 mg per day as the median dose, administered orally. The efficacy of GLEEVEC™ treatment will be assessed using both non-invasive serologic testing of fibrosis markers in conjunction with liver biopsy at defined intervals (every 1-2 years) during therapy.
[0032] The present invention is not to be limited in scope by the specific embodiments described herein. Indeed, various modifications of the invention in addition to those described herein will become apparent to those skilled in the art from the foregoing description and the accompanying figures. Such modifications are intended to fall within the scope of the appended claims.
[0033] It is further to be understood that all values are approximate, and are provided for description.
[0034] Patents, patent applications, publications, product descriptions, and protocols are cited throughout this application, the disclosures of which are incorporated herein by reference in their entireties for all purposes.
[0000] References
[0035] 1. Friedman, S. L.: Liver Fibrosis—From Bench to Bedside, J. Hepatol. 2003, 38 Supp. 1:38-53.
[0036] 2. Kim, W. R.; Brown, R. S.; Jr., Terrault; N. A.; El-Serag, H.: Burden of Liver Disease in the United States: Summary of A Workshop. Hepatology 2002, 36:227-242.
[0037] 3. Friedman, S. L.: Molecular Regulation of Hepatic Fibrosis, an Integrated Cellular Response to Tissue Injury. J. Biol. Chem., 2000, 275:2247-2250.
[0038] 4. Wong, L.; Yamasaki, G.; Johnson, R. J.; Friedman, S. L.: Induction of Beta-Platelet-Derived Growth Factor Receptor in Rat Hepatic Lipocytes During Cellular Activation In Vivo and In Culture; J. Clin. Invest., 1994, 94:1563-1569.
[0039] 5. Iredale, J. P.; Benyon, R. C.; Pikering, J.; McCullen, M.; Northrop, M.; Pawley, S.; Hovell, C. A; Arthur, M. J.: Mechanisms of Spontaneous Resolution of Rat Liver Fibrosis. Hepatic Stellate Cell Apoptosis and Reduced Hepatic Expression of Metalloproteinase Inhibitors, J. Clin. Invest., 1998, 102:538-549.
[0040] 6. Bonia, P. A.; Friedman, S. L.; Kaplan, M. M.: Is Liver Fibrosis Reversible? N. Engl. J. Med., 2001, 344:452-454.
[0041] 7. Druker, B. J.; Sawyers, C. L.; Kantarijian, H.; Resta, D. J.; Reese, S. F.; Ford, J. M.; Capdeville, R.; Talpaz, M.: Activity of A Specific Inhibitor of The BCR-ABL Tyrosine Kinase in The Blast Crisis of Chronic Myeloid Leukemia and Acute Lymphoblastic Leukemia with The Philadelphia Chromosome. N. Engl. J. Med., 2001, 344:1038-1042.
[0042] 8. Kantaijian, H.; Sawyers, C.; Hochhaus, A.; Guilhot, F.; Schiffer, C.; Gambacorti-Passerini, C.; Niederwieser, D.; Resta, D.; Capdeville, R.; Zoellner, U. et al.: Hematologic and Cytogenetic Responses to Imatinib Mesylate in Chronic Myelogenous Leukemia, N. Engl. J. Med., 2002, 346:645-652.
[0043] 9. Druker, B. J.; Talpaz, M.; Resta, D. J.; Peng, B.; Buchdunger, E.; Ford, J. M.; Lydon, N. B.; Kantaijian, H.; Capdeville, R.; Ohno-Jones, S. et al.: Efficacy and Safety of A Specific Inhibitor of The BCR-ABL Tyrosine Kinase in Chronic Myeloid Leukemia, N. Engl. J. Med., 2001, 344:1031-1037.
[0044] 10. Apperley, J. F.; Gardembas, M.; Melo, J. V.; Russell-Jones, R.; Bain, B. J.; Baxter, E. J.; Chase, A.; Chessells, J. M.; Colombat, M.; Dearden, C. E. et al.: Response to Imatinib Mesylate in Patients with Chronic Myeloproliferative Diseases with Rearrangements of The Platelet-Derived Growth Factor Receptor Beta, N. Engl. J. Med., 2002, 347:481-487.
[0045] 11. Demetri, G. D.; von Mehren; M., Blanke; C. D., Van den Abeele, A. D.; Eisenberg, B., Roberts; P. J., Heinrich; M. C., Tuveson, D. A.; Singer, S.; Janicek, M. et al.: Efficacy and Safety of Imatinib Mesylate in Advanced Gastrointestinal Stromal Tumors, N. Engl. J. Med., 2002, 347:472-480.
[0046] 12. Manley, P. W.; Cowan-Jacob, S.W .; Buchdunger, E.; Fabbro, D.; Fendrich, G.; Furet, P.; Meyer, T.; Zimmermann, J.: Imatinib: A Selective Tyrosine Kinase Inhibitor, Eur. J. Cancer, 2002, 38 Suppl. 5:S19-27.
[0047] 13. Kinnman, N., Francoz, C.; Barbu, V.; Wendum, D.; Rey, C.; Hultcrantz, R.; Poupon, R.; Housset, C.: The Myofibroblastic Conversion of Peribiliary Fibrogenic Cells Distinct from Hepatic Stellate Cells is Stimulated by Platelet-Derived Growth Factor During Liver Fibrogenesis. Lab. Invest., 2003, 83:163-173.
[0048] 14. Friedman, S. L.: Molecular Regulation of Hepatic Fibrosis: An Integrated Cellular Response to Tissue Injury, J. Biol. Chem 2000, 275:2247-2250.
[0049] 15. Friedman, S. L.; Maher, J. J.; Bissell, D. M.: Mechanisms and Therapy of Hepatic Fibrosis: Report of The AASLD Single Topic Basic Research Conference.
[0050] 16. Pinzani, M.; Marra, F.: Cytokine Receptors and Signaling During Stellar Cell Activation, Semin. Liver Dis. 2001, 21:397-416.
[0051] 17. Bachem, M. G.; Schneider; E.; Gross, H.: Identification, Culture, and Characterization of Pancreatic Stellate Cells in Rats and Humans, Gastroenterology 1998, 115:421-432.
[0052] 18. Iredale, J. P.: Stellate Cell Behavior During Resolution of Liver Injury, Semin. Liver Dis. 2001, 21:427-436.
[0053] 19. Wong, L.; Yamasaki, G.; Johnson, R. J.; Friedman, S. L.: Induction of Beta-Platelet-Derived Growth Factor Receptor in Rat Hepatic Lipocytes During Cellular Activation In Vivo and in Culture, J. Clin. Invest. 1994, 94:1563-1569.
[0054] 20. Rockey, D. C.: Hepatic Blood Flow Regulation by Stellate Cells in Normal and Injured Liver, Semin. Liver Dis. 2001, 21:337-350.
[0055] 21. Shao, R.; Rockey, D. C.: Effects of Endothelins on Hepatic Stellate Cell Synthesis of Endothelin-1 During Hepatic Would Healing, J. Cell Physiol. 2002, 191:342-350.
[0056] 22. Paradis, V.; Dargere, D.; Bonvoust, F.: Effects and Regulation of Connective Tissue Growth Factor on Hepatic Stellate Cells, Lab Invest. 2002, 82:767-774.
[0057] 23. Saxena, N. K.; Ideda, K.; Rockey, D. C.: Leptin in Hepatic Fibrosis: Evidence for Increased Collagen Production in Stellate Cells and Lean Littermates of OB/OB/mice, Hepatology 2002, 35:762-771.
[0058] 24. Ikejima, K.; Honda, H.; Yoshikawa, M.: Leptin Augments Inflammatory and Profibrogenic Responses in the Murine Liver Induced by Hepatotoxic Chemicals, Hepatology 2001, 34:288-297.
[0059] 25. Benyon, D.; Arthur, M. J. P.: Extracellular Matrix Degradation and The Role of Stellate Cells, Semin. Liver. Dis. 2001, 21:373-384.
[0060] 26. Iredale, J. P.: Tissue Inhibitors of Metalloproteinases in Liver Fibrosis, Int. J. Biochem. Cell Biol. 1997, 29:43-54.
[0061] 27. Marra, F.; Romanelli, R. G.; Pastacaldi, S.: Monocyte Chemotactic Protein-1 as a Chemoattractant for Human Hepatic Stellate Cells, Hepatology 1999, 29:140-148.
[0062] 28. Ikeda, K.; Wakahara, T.; Wang, Y. Q.: In Vitro Migratory Potential of Rat Quiescent Hepatic Stellate Cells and Its Augmentation by Cell Activation, Hepatology 1999, 29:1760-1767. | Disclosed herein is a method for treating hepatic fibrosis comprising administering to a patient in need of such treatment an amount effective to treat hepatic fibrosis of imatinib mesylate. This is based on the ability of imatinib mesylate to down regulate stellate cell activation in culture and in vivo. Hepatic fibrosis is not limited to patients with chronic Hepatitis B, Hepatitis C, non-alcoholic steatophepatitis (NASH), alcoholic liver disease, metabolic liver diseases (Wilson's disease, hemochromatosis), biliary obstruction (congenital or acquired) or liver diseases associated with fibrosis of unknown cause. | 0 |
Priority is claimed from U.S. Provisional Application Ser. No. 60/432,614, filed Dec. 12, 2002, entitled WELLHEAD DRIVE UNIT listing Ed MATTHEWS, Gregg LACUSTA and Jim ANAKA as inventors.
FIELD OF THE INVENTION
The present invention relates to a drive mechanism associated with artificial lift systems used in the production of oil and other fluids contained within underground formations. More specifically, this invention relates to a wellhead hydraulic drive unit that is installed as an integral part of a wellhead.
BACKGROUND OF THE INVENTION
Fluid production wells having insufficient pressure are unable to flow liquids to the surface by natural means. Such wells require some form of energy or lift to transfer fluids to the surface.
Several artificial lift systems exist to extract the liquids from liquid-bearing reservoirs. In the case of lifting oil from wells, conventional lifting units include the beam pump and the surface hydraulic piston drive. Both of these lift units are situated at the surface of the well and lift fluid to the surface by “stroking” production tubing or rods inside production casing and/or well casing. The production tubing or rods is connected to a wellbore pump configuration, comprising a chamber and a check valve, which allows fluid to enter on the down-stroke and to be lifted to the surface on the up-stroke. These conventional lift units are supplied power from combustion engines or electric drives.
Beam pumps and surface hydraulic piston drives come in many sizes and are used extensively worldwide. U.S. Pat. Nos. 3,376,826; 3,051,237 and 4,296.678 are all examples of the use of a beam drive for a sucker string actuated pump. U.S. Pat. No. 4,403,919 is an example of a surface powered hydraulic pumping unit.
There are many drawbacks associated with the use of conventional beam pumps and surface hydraulic piston drives. These units are large, obtrusive and unsightly in many sensitive regions. Further, the tubing and/or rods from within the wellbore must extend outside the well through a stuffing box to connect the drive units to same. The stuffing box prevents the wellbore fluids from escaping to the surrounding surface environment, however, rarely is this 100% successful thereby resulting in hydrocarbon contamination of the ground surrounding the wellhead.
Additional drawbacks to the use of conventional beam pumps and surface hydraulic piston drives are as follows. These units present a hazard to workers in the surrounding area as a result of exposure to surface moving parts. Further, beam pumps often experience alignment problems resulting in stress on the rods, undue wear and eventual failure. Finally, there are numerous dangers to personnel associated with assembly, transportation, installation, operation and maintenance due to the size of the units and their many moving parts.
U.S. Pat. No. 4,745,969 provides for a hydraulic/mechanical system for pumping oil wells that has a surface unit that can be hung inside of the well casing, so that there are no mechanical working parts outside of the well casing, except for surface pipeline connections. However, the '969 in-casing hydraulic jack system must be suspended from 20 to 40 feet below the surface of the ground, depending upon the required stroke. Further, the hydraulic jack unit is sealed within the well casing resulting in a casing interior space for collecting reservoir fluid above the sealing means. This could result in leakage from the casing interior space to the environment, especially when lifting the hydraulic jack from the casing.
SUMMARY OF INVENTION
The present invention provides a wellhead hydraulic drive unit to operate various styles of downhole pumps. The drive unit is installed as an integral part of the wellhead thereby eliminating the need for a stuffing box. Thus, hydrocarbon leakage from the wellhead drive unit is eliminated. Further, alignment issues through the wellhead and stuffing box associated with beam pumps and surface hydraulic drives are also eliminated.
The wellhead hydraulic drive unit of the present invention is easier and safer to assemble, transport, install, operate and maintain due to its compact size and minimal moving parts. This results in lower installation and retrieval costs. Installation can be completed using a conventional service rig or a location specific small mast unit.
It is important to note that well control is maintained throughout installation. There are no moving parts at the surface or above the wellhead. Once installed, the wellhead hydraulic drive unit of the present invention will have an extremely low profile. The wellhead hydraulic drive unit of the present invention can be easily installed in slant wells as well as horizontal or vertical wells.
The wellhead hydraulic drive unit can be used in a variety of production applications; for example, heavy oil wells, high viscosity and low inflow wells, light oil high production wells, gas well dewatering, steam-assisted gravity drainage (SAGD) wells, slant wells, stroking production tubing or rods, water injection applications, sand disposal applications and pulse wells to stimulate production.
In accordance with the present invention, an in-casing wellhead hydraulic drive unit for operating a downhole production pump via pump connecting means is provided, which hydraulic drive unit comprises:
a hydraulic cylinder having top and bottom ends, an inner wall and a piston positioned within the inner wall for reciprocation within the hydraulic cylinder; hydraulic fluid supply means attached to the hydraulic cylinder for producing reciprocation of the piston within the hydraulic cylinder; ram means having a top and bottom end and an annulus therethrough, slideably received within the inner wall of the hydraulic cylinder and connected to the piston for reciprocation in response to the piston; and production tube means inserted through the annulus of the ram means and connected to the hydraulic cylinder for enabling well fluid to be discharged from the well.
In a preferred embodiment, the in-casing wellhead hydraulic drive unit further comprises a means for mounting the hydraulic drive unit to the wellhead, said mounting means further comprising a hanger means attached to the hydraulic cylinder for landing the hydraulic cylinder within the wellhead. The hydraulic cylinder can be landed in the wellhead such that the top end of the hydraulic cylinder is positioned below the wellhead, within the wellhead or above the wellhead. The bottom end of the hydraulic cylinder is always contained within the well casing.
In another preferred embodiment, the bottom end of the ram means is threaded and the pump connecting means threadably receives the bottom end of the ram means. In the alternative, a coupling means, which couples the ram means to the pump connecting means, is used.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a cross-sectional view of the wellhead hydraulic drive unit in accordance with a preferred embodiment of the invention.
FIG. 2 is a cross-sectional view of the top end of the wellhead hydraulic drive unit inserted in a wellhead and well casing, in accordance with the present invention.
DETAILED DESCRIPTION
With reference to FIG. 1 , the wellhead hydraulic drive unit according to the present invention is shown designated generally by the reference numeral 1 . The various parts which make up the drive unit 1 are for the most part housed within hydraulic cylinder 2 . Hydraulic cylinder 2 is comprised of cylinder outer wall 4 , cylinder inner wall 6 , cylinder top end 8 and cylinder bottom end 10 .
At cylinder top end 8 is situated top gland 12 . Hanger 14 is threaded onto cylinder top end 8 of the hydraulic cylinder 2 to retain top gland 12 to hydraulic cylinder 2 . Top gland seal 16 seals top gland 12 to cylinder inner wall 6 and hanger seal 18 seals hanger 14 to cylinder outer wall 4 .
It should be noted that hanger 14 profiles vary with different wellheads and are manufactured accordingly. Where applications restrict the use of hanger 14 in the wellhead itself, a landing spool (not shown) can be used. The landing spool is bolted on to the wellhead and the hanger 14 of the wellhead hydraulic drive unit 1 will then be landed within the landing spool.
The wellhead hydraulic drive unit 1 can also be directly bolted to the wellhead by means of a flange (not shown), where well control precautions are not an issue. The flange means would be directly threaded onto the wellhead hydraulic drive unit 1 and then bolted directly onto the wellhead.
The wellhead hydraulic drive unit 1 is operated by hydraulic power supplied from an outside source, capable of delivering and operating from 500 psi to 4,000 psi. Hydraulic fluid 32 is delivered to the wellhead hydraulic drive unit 1 via top gland 12 . Hydraulic fluid enters in through hydraulic fluid port 34 and flows down through internal porting (not shown) in top gland 12 . The hydraulic fluid 32 is then routed through the top gland porting down through a plurality of feed tubes 36 attached to top gland 12 and out feed tube ports 38 into lower annular area 40 .
Hydraulic pressure in lower annular area 40 delivers force to main piston 42 for the upstroke or retraction movement. Down stroke movement or extension is normally achieved by tubing or rod weight from below (not shown). In applications where the tubing or rod weight is insufficient, hydraulic fluid can also be delivered to the top side of the main piston 42 through another hydraulic fluid port/vent 44 to actuate downward force.
A plurality of piston seals 46 provides sealing between main piston 42 and cylinder inner wall 6 . A plurality of feed tube seals 48 provides sealing between main piston 42 and feed tubes 36 . Wear rings 50 help provide main piston 42 alignment to cylinder inner wall 6 of hydraulic cylinder 2 .
Main piston 42 is threaded onto cylindrical ram 52 and has a non-rotational lock ring 82 . This allows for the wellhead hydraulic drive unit to provide torque to down hole tools where applicable. The torque is applied to hydraulic cylinder 2 and transmitted out to cylindrical ram 52 via main piston 42 and feed tubes 36 . It is designed to deliver either right or left hand torque in the fully open or fully closed positions only.
Cylindrical ram 52 has ram outer wall 54 and ram inner wall 66 . Cylindrical ram 52 moves up and down within hydraulic cylinder 2 relative to main piston 42 . Cylindrical ram 52 extends the length of hydraulic cylinder 2 from main piston 42 through cylinder bottom end 10 of hydraulic cylinder 2 .
Cylindrical ram bottom 64 is threaded to allow for connecting to a downhole pump via pump connecting means (not shown). Pump connecting means such as tubing joints, continuous tubing, sucker rods and continuous rods can either threadably receive threaded cylindrical ram bottom 64 or various crossover adapter designs can be used to couple the ram bottom 64 with pump connecting means. The design and type of pump will determine crossover design of the coupling adapter.
At cylinder bottom end 10 , end gland 56 is welded in place to cylinder inner wall 4 . A plurality of end gland seals 58 provides sealing between cylindrical ram 52 and end gland 56 . Wiper 60 wipes cylindrical ram 52 clean to keep contaminants from entering end gland seals 58 . Wear rings 62 help provide cylindrical ram 52 alignment inside end gland 56 .
Housed within cylindrical ram 52 is production tube 68 . Production tube 68 is threaded into top gland 12 to create a positive pressure seal. Attached to production tube 68 is production tube piston 70 . A plurality of production tube seals 72 provides sealing between production tube piston 70 and ram inner wall 66 . An additional production tube seal 74 also provides sealing between production tube piston 70 and cylindrical ram 52 , but functions to further seal out hydraulic fluid only from the top side in upper annular area 76 .
As production fluid 78 is pumped from the bottom of the well to surface, it enters into the inner diameter of cylindrical ram 52 as shown by the arrow. As production fluid enters into cylindrical ram 52 , it is produced up through the wellhead hydraulic drive unit 1 by means of the production tube piston 70 and through production tube 68 . Production fluid 78 , after passing through production tube 68 then enters top gland 12 and exits out to the surface via a flow line (not shown) which is connected to top gland 12 by threading into top gland thread 80 .
FIG. 2 shows the wellhead hydraulic drive unit 1 installed in a well casing. The installation of the wellhead hydraulic drive unit 1 is unique in that it is installed as an integral part of the wellhead. As a result of this, the well control features associated with the wellhead are optimized.
With reference now to FIG. 2 , wellhead 84 is shown attached to well casing 86 . The wellhead hydraulic unit 1 is lowered into the wellhead 84 and well casing 86 until hanger 14 is landed in place in wellhead 84 . The lower portion of the well hydraulic drive unit 1 now hangs inside well casing annulus 88 leaving sufficient space between the cylinder outer wall 4 of hydraulic cylinder 2 and the casing inner wall 90 to allow venting of casing annular gas to the surface through wellhead port 92 . A build up of gas pressure inhibits the flow of production fluids from the formation. Thus it is important to have the means for alleviating gas pressure.
It is further important to have sufficient space between cylinder outer wall 4 and casing inner wall 90 in order to determine fluid levels in the well bore to maximize fluid production.
Hanger 14 is secured in wellhead 84 by four equally spaced lag screws 20 and sealed to the wellhead 84 by a plurality of wellhead seals 22 . Once hanger 14 is landed in the wellhead 84 , top cover flange 24 is then installed on wellhead 84 by a plurality of flange bolts 26 and secured down with flange nuts 28 . Top cover flange 24 is sealed to the wellhead 84 by API seal ring 30 . Cylinder top end 8 of hydraulic cylinder 2 is sealed to top cover flange 24 by top cover flange seal 94 .
In practice, hydraulic fluid 32 is supplied at top gland 12 and fed through one or more feed tubes 36 having hydraulic fluid ports 34 at the bottom for hydraulic flow. This hydraulic fluid path provides for main piston 42 upstroke or hydraulic cylinder retraction. Hydraulic fluid can also be supplied directly through the top gland 12 to the top side of the main piston 42 via a second hydraulic fluid port/vent 44 for piston downstroke or hydraulic cylinder extension.
The up and down stroking movement actuates the downhole pump allowing for production fluid 78 to surface. The production fluid 78 passes up through the downhole production tubing, through the cylindrical ram 52 , through the production tube piston 70 and production tube 68 , and finally through the top gland 12 to exit at the surface via a vent or flow line (not shown) attached to the wellhead hydraulic drive unit 1 .
Hydraulic pressure to the main piston 42 is supplied from a surface pump via a control line connected to the cylinder top end 8 of the hydraulic cylinder (not shown). The power for the hydraulic pump can either be electric and/or internal combustion motor.
While various embodiments in accordance with the present invention have been shown and described, it is understood that the same is not limited thereto, but is susceptible of numerous changes and modifications as known to those skilled in the art, and therefore the present invention is not to be limited to the details shown and described herein, but intend to cover all such changes and modifications as are encompassed by the scope of the appended claims. | The present invention provides a wellhead hydraulic drive unit to operate various styles of downhole pumps, which is installed as an integral part of a wellhead thereby eliminating the need for a stuffing box. The wellhead hydraulic drive unit comprises a hollow hydraulic cylinder having a piston positioned therein, a hydraulic fluid supply attached to the hydraulic cylinder for raising the piston within the hydraulic cylinder, a hollow ram slideably received within the inner wall of the hydraulic cylinder and connected to the piston for reciprocation in response to the piston; and a production tube inserted through the ram for enabling well fluid to be discharged from the well. | 4 |
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to a method and an arrangement for transfer between a cordless telecommunication system, such as DECT, and a background cellular mobile telecommunication system such as GSM. The invention is in particular conceived to be used when different operators operate the two systems. In a case where both systems are operated by the same operator and the DECT system is connected directly to the background GSM network, transfer can be effected in a more effective manner.
Generally, the present invention reduces the transfer time between the different systems by among other things transmitting transfer parameters to the portable terminal and setting up a preparatory three-party connection.
2. Discussion of the Background
A user requirement of transfer is that the process is to be on the whole imperceptible for the user. That is to say, the transfer is to take place rapidly and without inconvenient background noise so that the transition which the transfer inevitably implies does not become annoying. It should therefore be possible to carry out the transfer in approximately 1 second, preferably even more rapidly. Within the field, there is a number of documents which describe different solutions to this problem.
U.S. Pat. No. 5,260,988, WO 93/16549, U.S. Pat. No. 5,127,042 and U.S. Pat. No. 4,989,230 describe communication systems which consist of both cordless telephony and a cellular mobile telephone system. The system includes portable cordless units which can initiate and receive calls in both the cordless and the cellular system. Calls can be connected automatically to the system in which the subscriber is located. There is also the possibility of automatically connecting a call in progress between the different systems if the subscriber moves between systems. It is possible for the user to select manually a given system by a button procedure, either permanently or at a given time. On transfer between the two systems, a three-party call is utilized.
U.S. Pat. No. 5,235,632 describes a mobile telephone system which consists of an external system which consists of base stations, divided into cells, with high transmitting power connected to a mobile telephone exchange and an indoor system consisting of base stations with low transmitting power connected to a mobile telephone exchange. According to the document, the possibility exists of connecting a call between the internal and the external system by, for example, measuring signal strength from each system.
U.S. Pat. No. 5,309,502 relates to a radio telephone which combines the function of a cordless telephone and a cellular mobile telephone. The possibility exists, on connecting calls, of automatically selecting via which the communication is to take place. Nothing is mentioned about transfer during calls in progress.
U.S. Pat. No. 5,210,785 relates to a cordless communication system and a terminal which combines two different systems such as cordless telephony and cellular mobile telephony. According to the document, selection of the communication method is to take place automatically.
U.S. Pat. No. 5,329,574 describes a method of continuously maintaining telephone communication when a radio communication unit moves between two different communication systems. When the unit discovers that the communication quality is deteriorating in a first system, a connection packet is transmitted via a central control unit to a second system. The communication in the first system is maintained until the second system confirms it has taken over of the communication.
U.S. Pat. No. 5,212,684 relates to a communication system which utilizes portable radio telephones. The system consists of base stations and portable telephone units in accordance with the GSM standard. The portable telephone units can also work in accordance with the DECT standard. The system carries out both internal and external transfer but does not mention transfer between DECT and GSM.
WO91/16772 describes a method of transfer in a mobile radio communication system. According to the document, the mobile measures signal strengths of surrounding base stations. When the transfer is felt to be justified, the signal strength vectors are correlated with stored vectors and, if there is correlation, transfer takes place in a manner which depends on the position.
EP A1 615 392 describes a further example of transfer in a mobile radio system which utilizes the position of the mobile.
U.S. Pat. No. 5,345,499 relates to a method of transfer in a cellular radio system. The system consists of microcells and macrocells. In the system, the possibility exists of making connection and transfer dependent on the speed of the mobile. Thus, a mobile with a high speed can be prevented from connecting itself to a microcell if it exceeds a given threshold speed.
U.S. Pat. No. 5,276,906 shows a cellular radio telephone system which has two threshold levels for transfer. When the signal strength in a first cell falls below a first threshold value, transfer is initiated to a second cell by this cell being selected with the aid of the mobile. When the signal strength in the first cell then falls below a second threshold value, transfer to the second cell is carried out.
SUMMARY OF THE INVENTION
There is a requirement to carry out transfer between cordless systems, in particular DECT, and cellular communication systems, in particular GSM, in a more rapid manner than that which is achieved in the prior art. Three-party calls alone, which form part of the state of the art and this invention, are thus not adequate. According to the invention, the problem is solved by continuously monitoring the position and identity of the terminal and, where appropriate also transferring to be terminal, and relevant time and transfer parameters being. Thus, a three-party connection can be set up and the terminal can register itself in the mobile telephone exchange for rapid connection, after obtaining an acknowledgement from the mobile system.
The present invention provides method of transfer between a cordless telecommunication system which includes a number of cells within a relatively small area and a cellular mobile telecommunication system which includes a number of cells within a relatively larger area which completely or partly overlaps the area of the cordless system. The system comprises at least one portable terminal with the capacity of communicating with both communication systems.
According to the invention, a transfer zone is fixed by the cordless system and the terminal is monitored with regard to its identity and position so that transfer parameters can be transmitted to the terminal when it is located in the transfer zone. The transfer is prepared by setting up a three-party connection between the terminal and the cordless system and between the terminal and the mobile system. The terminal disconnects the connection to the cordless system and transfer to the mobile system takes place.
Preferably, the three-party connection is set up by a mobile telephone exchange in the mobile system and this is kept in waiting state until the terminal has registered itself with the mobile system and received acknowledgement that transfer can take place.
The transfer can be induced by the terminal or a fixed station of the cordless system.
The invention also relates to an arrangement for implementing the method.
BRIEF DESCRIPTION OF THE DRAWINGS
The invention is explained below in detail with reference to accompanying drawings, in which
FIG. 1 is a block diagram of an example of system architecture according to the present invention,
FIG. 2 is a diagram of an alternative use of a terminal in the DECT system or GSM system,
FIG. 3 shows diagrammatically a coverage area in a DECT system,
FIG. 4A-4C show diagrammatically different transfer situations according to the invention,
FIG. 5 is a time diagram of signaling between the terminal and systems of terminal-initiated transfer from a DECT system to GSM system, and
FIG. 6 is a time diagram corresponding to FIG. 5 which shows transfer initiated by the fixed side in the DECT system.
DETAILED DESCRIPTION OF PREFERRED EMBODIMENTS
As an aid to clearer understanding of the invention, a brief description is first given of the cordless communication system in which the present invention is first and foremost conceived for use.
Digital European Cordless Telecommunications, DECT, is a system which has been specified within ETSI for cordless telecommunication with a number of application areas, for public applications, for private use within e.g. company systems or for home use, and for radio-based connection to the local network. Although DECT has great similarities with the traditional mobile telephony systems, the basic standard lacks a description of the functionality of the network. For this purpose, special access profiles are instead specified, which describe the connection to and the interaction with the background network elements.
For interaction with GSM (Global System for Mobile communication), work is going on with such a profile, DECT/GSM Interworking Profile. The standards in this profile describe how functions and messages in GSM are to be capable of being transmitted over a DECT radio system. Handover or transfer between DECT and GSM is as yet not described in any of the standards which form part of the profile.
DECT is a very flexible standard which combines (1) high system capacity within traffic-intensive areas (2) good quality for both speech and data services. The limited radio coverage of the system, however, results in the DECT system being very local and DECT will hardly be extended to cover as large an area as a mobile telephony network does. DECT systems will probably come to be connected directly to GSM networks, but also to exist as free-standing systems, e.g., in direct connection with subscriber exchanges.
Handover within DECT is normally initiated by the terminal, either because the radio channel is subject to interference, or for reasons of coverage. Such internal handover within a DECT cluster is conducted entirely within the framework of the local DECT system and requires no interaction with background network elements. Transfer to another cluster or to another access system, e.g. to GSM, is called external handover and can be decided either by the terminal or by the central unit of the cluster.
In FIG. 1, an example of a system architecture according to the invention is shown. The fixed side of DECT can be divided into one or more radio units (Radio Fixed Parts) RFP and a central unit (Central Fixed Part) CFP. Together, they form a fixed unit (Fixed Part) FP. Radio units RFP connected to a common central unit constitute a so-called "cluster" and serve all the portables, PP, within a coverage area via the radio interface CI of the DECT system. CFP can for example be a part integrated in a PABX subscriber exchange, or constitute a part of the local station. The DECT system can thus be owned and/or managed either by a public telecommunications operator or a private operator.
The mobile cellular side, that is to say the GSM part, is constituted by a mobile telephone exchange MSC (Mobile Switching Center), a base station control unit (Base Station Controller) and base stations BTS (Base Transceiver Station). The GSM system communicates with its mobiles MS via its radio interface Um.
Both the DECT system and the GSM system are connected to the public telecommunication network PSTN.
Local databases like home location register (HLR) and visitor's location register (HLR) can also be connected to the CFP of the system or, like in the GSM case, supported by functions in the background network.
A DECT terminal, or portable PP, needs to be capable of handling the identity structure of GSM in order to be capable of being connected into the combined DECT/GSM environment. There are also requirements as far as security routines are concerned, e.g. authentication and ciphering of user data.
The user sees great value in only needing to use one terminal for his communication. Combined hand units for DECT and GSM, so-called dual mode terminals (FIG. 2), are therefore an essential component in integration of systems.
With a combined DECT/GSM terminal, it is natural that requirements will also arise for the communication to be capable of being maintained during a transition between the two different access systems, if they are used in the same geographical area. A transfer of calls in progress from DECT to GSM, that is to say a handover, is, as pointed out previously, not as yet described in any of the standards which relate to interaction between systems.
Handover is a very important function in order to be capable of offering users complete mobility over a number of application areas. It is of primary interest to find a solution for handover from DECT to GSM since the GSM access system can then function as an extension and support for DECT even if systems are operated by different operators.
There are many technical problems for operator-independent handover from DECT to GSM:
1) A DECT coverage area which lies "embedded" in a background GSM can utilize the mobility functions of GSM in order to effect handover between systems. The background systems must, however, be capable of communicating with one another (see FIG. 1), exchanging system information and also transmitting such information to the terminal.
2) A GSM handover in the traditional sense presupposes that the mobile station assists the network with measuring data about the radio environment. Handover in DECT has an entirely different functionality than in GSM. Therefore, the traditional handover methods which exist in DECT or GSM cannot be utilized for a transfer between systems.
3) Handover must not be a slow process. From DECT to GSM, it may be acceptable that handover is perceptible, but time requirements are still high. The users can be assumed to require that handover takes place with an interruption in the call of less than 1 second. When systems are operated by different operators, the fixed system parts must therefore prepare any coming handover in advance.
4) Necessary signaling should for two reason, be minimized.
5) In order to maintain a high connection quality, unnecessary transfers are to be avoided, that is to say handover to a GSM cell take place only when DECT coverage is lacking, or for other operator-dependent reasons.
6) Added to this is the further condition that the solution for handover is to be capable of being implemented at a reasonably low cost and without requiring comprehensive revisions of the software in terminals.
7) The DECT operator (owner, manager) will probably also want to be capable of controlling conditions for handover, e.g. where, when and to whom this service is to be available.
The present application describes how handover can be carried out from DECT to GSM, where it is not necessary that both access systems are operated by the same operator, but where they are in one manner or another connected to the same background mobile telephone exchange, MSC. The signaling interface is to have the possibility of transmitting mobility information which in GSM, is defined in the Mobile Application Part, MAP. This can take place either via the A-interface of GSM or via a future ISDN-based interface, e.g. DSS.1+ (see FIG. 1).
The solution is based on the following basic parts:
a) Control over conditions for handover
In FIG. 3, an example is shown of an area which has DECT coverage. In FIG. 3, the GSM coverage is not marked, but it is intended to exist over the entire area, possibly with the exception of some indoor cells. Marked cells are intended to provide the possibility of handover to GSM. Area P relates to an internal DECT area where handover to GSM is also possible (e.g., a parking place). Area G is an external edge area, in which the DECT operator will not allow a handover from DECT to GSM (e.g., an area such as a tunnel).
The DECT operator controls conditions for handover by defining, in its central unit CFP, the cells from which handover is allowed, and the cells from which handover is not allowed. The conditions for handover from DECT to GSM which are mentioned here can also be extended to include time spaces and also individual-related conditions. A further possibility, which also forms part of the invention, is that the central unit is programmed in order to adaptively change its conditions within the limits set by the operator. This adaptivity is based on available statistics in the central unit, where information is gathered about when and where DECT portables request (external) handover. The central unit is programmed to follow the path of each DECT portable through the cells of the cluster and analyze/calculate which "paths" lead to the request for external handover. The central unit "instructs" itself in this manner to predict, starting from a movement pattern of a DECT portable, where and when the latter will request external handover, thus can prepare a handover to a GSM system in very good time.
An example can demonstrate this.
Statistics in the central unit will show a relatively large number of requests for external handover at the end of work time (e.g., 1630 hours) from mobiles which a short time before were in the parking area (P in FIG. 3).
One of the major properties of DECT is the possibility of a single terminal simultaneously utilizing a number of different subscriptions/identities and, from the fixed unit FP, indicating which type of access rights belong together with these identities. In the case of DECT/GSM, this can be solved with the aid of a so-called multi-application card. The equivalent of DECT to the SIM card (Subscriber Identity Module) of GSM is the DECT Authentication Module. The functionality of this DAM card is standardized and will be capable of supporting requirements for the identities and the security which applies for the SIM card of GSM.
This means that the DECT/GSM dual mode terminal has the possibility of storing a number of sets of system parameters independently of one another and interpreting changes in these parameters. If the portable is provided with the parameters from the fixed side as is required on new registration in a new search area in a new system, this information can be utilized in order to activate external handover to this system. This functionality is a part of the invention and is used in order to reduce the set-up time on handover from DECT to GSM to an acceptable level (<approx. 1 sec.).
In this manner, the handover zone is not only a geographical area but also related to time, movement patterns and--even--the user (identity).
b) Preparation for handover
When the terminal is located in the handover zone during a call in progress, a handover is prepared by the system providing the terminal with necessary parameters so that, without delay, it is to be capable of establishing contact with a corresponding base station BTS in the GSM system, and a three-party connection is set up in the network between the DECT terminal in progress and a "waiting" connection in the GSM system.
c) Activation of handover
Handover can, as previously mentioned, be activated either from the terminal or from the fixed side of DECT. In FIG. 5, the message flow on handover activated by the terminal is shown. The terminal-controlled handover is usually activated because the field strength of the DECT connection has become so low that a call connection can no longer be maintained with sufficient quality. After acknowledgement has been received from the network, the connection to the DECT system is subsequently interrupted and the portable registers itself promptly in relation to the corresponding base station in the GSM system, whereupon the call can be set up once more via the waiting three-party connection.
The solution which is described in this application can, however, just as readily be activated from the central unit CFP in the event that the analysis is carried out based on information such as the geographical positioning of the terminal, time, earlier request for handover, etc. FIG. 6 shows messages in the event of a CFP-controlled handover. Which system part activates the handover has no influence on the complexity of the terminal. In the same system, handover can be activated by either party. Selection is dependent on e.g. the functionality which is programmed into the adaptive handover algorithm of the central unit CFP.
d) Termination of handover
If handover is prepared, but does not need to be brought about, the waiting three-party connection in GSM is terminated, as it is no longer required.
The transfer procedure is described in greater detail below.
A terminal which during a call in progress communicates via marked base stations in FIG. 3, is located within geographically and empirically obtained specific areas which are identified as handover zones.
The central unit CFP in DECT carries on the whole time analysis of calls in progress and, on the basis of the logical information which is built up, draws a conclusion about whether handover for this terminal is appropriate. The central unit CFP then collects, via the mobile telephone exchange MSC in GSM, system parameters from the network. CFP transmits this information to the terminal with the aid of the DECT procedure for parameter collection (see FIG. 5). The information which is collected from the GSM network and is transmitted to the terminal contains the radio frequency and the identity of the base station, GSM BTS, to which the terminal is to be connected. The terminal receives and stores the parameters together with a request from CFP that these are to be used for a handover from DECT to GSM. In the mobile telephone exchange MSC in GSM, a three-party connection is established from the usual-service range.
This is put into waiting state in order to be activated only when the terminal has registered itself in relation to the base station in question BTS in GSM.
It is worth noting that CFP-controlled handover can make possible further reductions in of the transfer time. A DECT system with a high functional level has an even greater possibility of preparing a handover. In this case (see also FIG. 6), further information can be transmitted to the terminal in the form of a ciphering code, search area and paging identity.
Transfer between systems can then take place, but bringing about of the prepared handover is carried out by the terminal or the central unit at a later stage. In the continued description below, the situation is shown, for the sake of simplicity, when the terminal activates a handover.
In this example, a handover initiated by the terminal is described, as it is the latter which has knowledge about the radio conditions, but the function can, as mentioned previously, just as well be initiated by the fixed side.
After a handover decision on handover, the terminal sends a message that the call in progress link is to be disconnected because of an external handover (see FIG. 5). The terminal remains connected, however, until a positive acknowledgement has been received from the network that transfer can take place. Subsequently, the call is interrupted temporarily and the terminal functionally switches off its DECT radio communication. The connection to the other party is maintained by the three-party connection established in advance, which is now in the waiting state.
Immediately afterwards, the GSM part in the terminal is activated and the communication with the GSM system set up. As information has already been transmitted from the network at an earlier stage, this registration takes place with the aid of the procedure for IMSI Attach which saves time and limits the signaling both over the radio route and in background network elements. The terminal can establish contact directly with the designated base station BTS on the control channel of the latter. On registration, the GSM identity of the terminal is used, which is assumed to be stored as a part of the active card DAM.
After registration, the mobile telephone exchange MSC once again established contact with the terminal by means of a normal mobile-terminated call connection. The terminal answers automatically the awaited call, which reduces the interruption time and makes the handover less perceptible for the user. Automatic answering (off-hook) requires no more extensive intelligence in the terminal, and today already exists in some GSM products.
The awaited connection is connected once again and the call between the parties can continue.
A prepared handover can be interrupted for a number of reasons. The terminal may e.g. via internal handover have exchanged a base station within the DECT system for a radio unit RFP which lies "deeper" in the DECT cluster than the defined handover zone. The fixed side receives information about this and can then terminate the waiting three-party connection in GSM. The call can continue to be served with DECT access without further measures needing to be taken.
Handover can also be interrupted for operator reasons, by the terminal not being provided with necessary GSM parameters, or by negative acknowledgement being given on disconnection of the call link. The terminal should in this case not interrupt the call in progress, but maintain the connection via DECT as long as this is possible.
The invention can be utilized within all application environments of DECT where there is a requirements for calls to be maintained across the boundaries when the radio coverage of DECT passes into GSM. For the user, this functionality is very important for the qualitative experience of the service, and for the operator a fully covering service is obtained which is a competitive advantage in relation to competitors on the market.
Thus, the present invention solves problems of transfer between a cordless communication systems and a cellular mobile communication system in an effective manner. The invention can be implemented with the protocols and functions which are available according to standards for DECT/GSM IWP and the protocols and network functions which are built into local exchanges, company systems and the GSM network. An expert in the field will understand easily how the invention is to be implemented in detail, which in itself can be effected in various ways. The invention is limited only by the patent claims below. | A method and arrangement for transfer between a cordless telecommunication system, preferably DECT, and a cellular mobile telecommunication system, preferably GSM. The cordless telecommunication system includes of a number of cells within a relatively small area, while the mobile telecommunication system includes of a number of cells within a relatively larger area which completely or partly overlaps the area of the cordless system. The system comprises at least one portable terminal capable of communicating with both the cordless and cellular communication systems. Accordingly a transfer zone is fixed by the cordless system and the terminal is monitored with regard to it identity and position so that transfer parameters can be transmitted to the terminal when it is located in the transfer zone. The transfer is prepared by setting up a three-party connection between the terminal and the telecommunication system and between the terminal and the mobile telecommunication system. The terminal disconnects the connection to the cordless telecommunication system and a transfer to the mobile system takes place. The method and arrangement reduce the transfer time between the different systems by transmitting transfer parameters to the portable terminal and setting up the preparatory three-party connection. | 7 |
BACKGROUND OF THE INVENTION
This invention relates to a process for chemically modifying nonwoven textile articles to impart pilling resistance and soil release properties to the article without compromising the strength and abrasion resistance of the article.
Nonwoven textile articles have historically possessed many attributes that led to their use for many items of commerce, such as air filters, furniture lining, and vehicle floorcovering, side panel and molded trunk linings. Among these attributes are lightweightness of the products, low cost and simplicity of the manufacturing process, and various other advantages. More recently, technological advances in the field of nonwovens, in areas such as abrasion resistance, fabric drape, fabric softness, and wash durability, have created new markets for nonwoven materials. For example, U. S. Pat. Nos. 5,899,785 and 5,970,583, both assigned to Freudenberg, describe a nonwoven lap of very fine continuous filament and the process for making such nonwoven lap using traditional nonwoven manufacturing techniques. The raw material for this process is a spun-bonded composite, or multi-component, fiber that is splittable along its length by mechanical or chemical action. As an example, after a nonwoven lap is formed, it may be subjected to high-pressure water jets which cause the composite fibers to partially separate along their length and become entangled with one another thereby imparting strength and microfiber-like softness to the final product. One such product manufactured and made available by Freudenberg according to these processes is known as Evolon®, and it is available in standard or point bonded variations. These manufacturing techniques allow for the efficient and inexpensive production of nonwoven fabrics having characteristics, such as strength, softness, and drapeability, equal to those of woven or knitted fabrics, which have end uses in products such as apparel, cleaning cloths, and artificial leather.
With the emergence of nonwovens into these new markets and increased consumer interest in such products, there has been a desire to produce fabrics with other characteristics, in addition to strength, similar to those of woven or knitted fabrics. Some of these characteristics include pilling resistance and soil release. Pilling typically results from fibers being pulled out of the fiber bundle and becoming entangled into a “ball” due to mechanical action, such as rubbing that, for example, fabrics encounter during normal use. These “pill balls” are a detriment to the appearance and comfort of textile articles. Reducing or eliminating the pilling propensity of textile articles would typically extend the useful life of the end-use product, such as a garment, by retaining its original appearance and comfort. Furthermore, soil release properties have obvious considerable importance for end-use products such as children's clothing, napery, and cleaning cloths since it is desirable to maintain the original appearance of these products for aesthetic reasons. Thus, it is an important attribute for nonwoven articles to possess pilling resistance and soil release characteristics without compromising strength and abrasion resistance of the articles for their emergence into these new markets.
SUMMARY OF THE INVENTION
In light of the foregoing discussion, it is one object of the current invention to achieve a nonwoven textile article which has been chemically modified to possess pilling resistance, soil release, and acceptable strength characteristics. Textile articles include fabrics, films, and combinations thereof. By pilling resistant, it is meant that the article achieves a minimum “B” rating after 18,000 cycles under a 9 kPa weight when tested for Martindale Pilling according to ASTM D4970 and using the Marks & Spencer Test Method P17 and rating the article on the Marks & Spencer Holoscope. Soil release is determined according to test method AATCC Method 130-2000 and is found to be acceptable for articles that achieve a minimum 3.0 rating after one wash cycle. The amount of strength that will generally be considered to be “acceptable” is the strength required for the treated article to function within its anticipated end product for a minimum number of use or wear cycles, which will generally also include intermittent cleaning cycles as well. The strength that is considered to be acceptable for a given article will therefore vary depending on the type of treated article, how it will be used in an end product, the type of end product, etc. By way of example, acceptable strength for an article intended for use as apparel is achieved with a minimum 2000 cycles when tested for Flex Abrasion according to ASTM D 3885. More specifically, by experience it has been determined that a certain nonwoven fabric comprised of spun-bonded continuous multi-component splittable fibers, wherein the fibers are 65% polyester and 35% nylon 6 or nylon 6, 6, to be used in shirting should achieve a minimum of 2000 cycles when tested according to ASTM D 3885. Other standard methods for evaluating the pilling resistance, soil release, and abrasion resistance of fabrics may be used and are known and available to those skilled in the art.
A second object of the current invention is to achieve a nonwoven textile article, which has been chemically modified, that maintains its aesthetic appearance and comfort properties due to its resistance to pilling. The formation of “pill balls” leads to an unsightly appearance of the article. In addition, these “pill balls,” when found in a garment, for example, generally result in a loss of garment comfort due to the abrasive nature of these protrusions against the skin. Therefore, reducing or eliminating the formation of “pill balls” allows for the extension of the useful life of textile articles, such as apparel, made from nonwoven fabric.
A further object of the current invention is to achieve a nonwoven textile article, which has been chemically modified, that maintains its aesthetic appearance due to its soil release characteristics. For example, garments or napery articles having food or soil stains are typically detracting to the appearance of those items. Thus, treating nonwoven textile articles with soil release chemicals would generally preserve the appearance of those articles and thereby extend the useful of those articles.
It is also an object of the current invention to achieve a method for chemically modifying nonwoven textile articles to impart pilling resistance and soil release properties to the articles while at the same time maintaining acceptable strength and abrasion resistance characteristics.
A further object of the current invention is to achieve a composition of matter for chemically modifying a nonwoven textile article to achieve pilling resistance, soil release, strength and abrasion resistance comprising a hydrophilic silicone, a soil release agent, an abrasion resistance agent, water, and optionally, a wetting agent and a defoaming agent.
Other objects, advantages, and features of the current invention will occur to those skilled in the art. Thus, while the invention will be described and disclosed in connection with certain preferred embodiments and procedures, such embodiments and procedures are not intended to limit the scope of the current invention. Rather, it is intended that all such alternative embodiments, procedures, and modifications are included within the scope and spirit of the disclosed invention and limited only by the appended claims and their equivalents.
DETAILED DESCRIPTION OF THE INVENTION
A nonwoven textile article is provided that has been chemically modified to achieve a useful change in certain of its properties. U.S. Pat. Nos. 5,899,785 and 5,970,583, both incorporated herein by reference, describe the composition and process for manufacturing the nonwoven lap that is the basis for the nonwoven textile article that is chemically modified by the current invention. Typically, the nonwoven article is a fabric comprised of spun-bonded continuous multi-component filament fiber that has been split, either partially or wholly, into its individual component fibers by exposure to mechanical or chemical means, such as high-pressure fluid jets. The fabric composition is generally 65% polyester fiber and 35% nylon 6 or nylon 6, 6 fiber, although other fiber variations and combinations described by the above-mentioned patents are contemplated to be within the scope of this invention.
The process for chemically treating the nonwoven article, typically a fabric made from polyester and nylon composite fibers, involves the use of several chemicals combined in a mixture. The chemicals typically function as wetting agents, defoaming agents, soil release agents, pilling resistance agents, and abrasion resistance agents.
Generally, the wetting agents are ethoxylated long chain alcohols, such as Solpon® 839 available from Boehme Filatex, such that the long chains comprise at least 9 carbon atoms. Without being bound by theory, it is thought that the wetting agent improves adhesion, and possibly the chemical reaction that occurs, between the fabric and the other chemicals in the mixture. Because the untreated fabric typically tends to be inherently hydrophilic (approximately 100% wet pickup on weight of fabric in laboratory scale testing), the use of a wetting agent is optional. However, if a wetting agent is employed, concentrations typically range from between about 0.20 and about 0.30 weight percent on weight of the chemical mixture.
Depending on the specific mixture of chemicals applied to the fabric, a defoaming agent may be needed to reduce foam during the manufacturing process. For example, a mineral oil such as Tebefoam® VP1868 available from Boehme Filatex may be used. Other defoamers include silicone defoamers and de-aerating agents. The use of a defoamer is generally optional. However, if a defoamer is employed, typical concentrations may range from between about 0.05 and about 2 weight percent on weight of the chemical mixture.
Chemicals used to impart pilling resistance to the fabric are typically hydrophilic silicones (such as SilTouch® SRS available from Yorkshire PatChem). It is generally known to those skilled in the art that silicones usually hinder the pilling characteristics of fabrics. However, with the unique combination of chemicals employed in this invention, these silicones have actually been found to improve the pilling resistance of these fabrics. Typical concentrations for hydrophilic silicones range from between about 2 and about 8 weight percent on weight of the chemical mixture.
Soil release chemicals are typically chosen from acrylic compounds (such as Millitex® PD 75 available from Milliken Chemical), fluorocarbon compounds (such as Zonyl® 7910 available from Ciba Specialty Chemicals), or liquid polyesters (such as Millitex® PD 92 available from Milliken Chemical). The soil release chemicals have a tendency to form films around the fibers. Typical concentrations of acrylic soil release chemicals range from between about 2 and about 12 weight percent on weight of the chemical mixture. Concentrations of fluorocarbon soil release compounds generally range from between about 0.5 and about 6 weight percent on weight of the chemical mixture, and concentrations of liquid polyester soil release compounds generally range from between about 2 and about 6 weight percent on weight of the chemical mixture.
Chemicals used to impart abrasion resistance and strength to the fabric are generally polyethylenes (such as Aqualene N available from Moretex) or polyurethanes (such as Prote-set FAI available from Synthron, Inc). Generally, polyethylenes with a higher melting point (usually referred to as high-density polyethylenes), such as greater than about 124 degrees Celsius, are preferred over low melting point polyethylenes (usually referred to as low-density polyethylenes), and they tend to form films around the fiber similar to the films formed by the soil release chemicals. Typical concentrations of polyethylenes range from between about 8 and about 16 weight percent on weight of the chemical mixture, while typical concentrations of polyurethanes range from between about 6 and about 18 weight percent on weight of the chemical mixture. Interestingly, the hydrophilic silicones, mentioned previously as pilling resistance chemicals, also tend to enhance the abrasion resistance of the fabric, while the polyethylenes mentioned above as abrasion resistance chemicals tend to enhance the pilling resistance of the fabric. It has been generally found that an intimate relationship exists between the use these two types of chemicals for generally enhancing both the abrasion resistance and the pilling resistance of the nonwoven textile article.
It should be noted that the concentrations of the chemicals used to treat the nonwoven textile articles can be varied within a relatively broad range, depending on the amount of pilling resistance and the amount of soil release desired for a particular end-use product, and is related to the inherent strength of the textile article to be processed. The inherent strength of the fiber which will ultimately be treated with the chemical mixture generally varies between different manufacturers of the fiber and between fiber types. As a result, these characteristics typically need to be examined in determining the concentration and amount of chemical to be used for a given treatment.
In one aspect of the invention, the process of the current invention requires no special equipment; standard textile dyeing and finishing equipment can be employed. By way of example, a nonwoven textile fabric may be treated either in a batch operation, wherein chemical contact is prolonged, or in a continuous operation, wherein chemical contact with the fabric is shorter. Generally, a predetermined amount of the desired chemical mixture is deposited onto the article, and the treated article is then dried, typically by exposing the article to a sufficient amount of heat for a predetermined amount of time. The application of the chemical mixture to the article may be accomplished by immersion coating, padding, spraying, foam coating, or by any other technique whereby one can apply a controlled amount of a liquid suspension to an article. Employing one or more of these application techniques may allow the chemical to be applied to a textile article in a uniform manner. As noted above, once the chemical has been applied to the article, the article is dried, generally by subjecting the article to heat. Heating can be accomplished by any technique typically used in manufacturing operations, such as dry heat from a tenter frame, microwave energy, infrared heating, steam, superheated steam, autoclaving, etc. or any combination thereof. The article may be dyed or undyed prior to chemical treatment. If undyed before treatment, the article may be dyed or printed after treatment. The article may also be subjected to various face-finishing processes and sanforization after chemical treatment. For example, U.S. Pat. Nos. 5,822,835, 4,918,795, and 4,837,902, incorporated herein by reference, disclose a face-finishing process wherein low pressure streams of gas are directed at high velocity to the surface of a fabric. The process ultimately softens and conditions the fabric due to vibration caused from airflow on the fabric.
The following examples illustrate various embodiments of the present invention but are not intended to restrict the scope thereof. In all examples, all percentages are by weight percent of the total chemical mixture (i.e., percent on weight of the chemical bath), unless otherwise noted.
All examples utilized nonwoven fabric comprised of spun-bonded continuous multi-component fibers which have been exposed to mechanical or chemical processes to cause the multi-component fibers to split, at least partially, along their length into individual polyester and nylon 6, 6 fibers, according to processes described in the two Freudenberg patents earlier incorporated by reference. The fabric, known by its product name as Evolon®, was obtained from Firma Carl Freudenberg of Weinheim, Germany.
Pilling was determined by Martindale Pilling according to ASTM D4970 and the Marks & Spencer Test Method P17, wherein “A” indicates optimal pilling resistance and “E” indicates poor pilling resistance, when rating the fabric on the Marks & Spencer Holoscope. The Martindale Pilling exposed the fabric to a 9 kPa weight (595 grams) for 18,000 revolutions, or cycles. A Home Laundry Tumble Dry (HLTD) wash procedure was also incorporated as part of the Martindale Pilling test method. The HLTD involves washing the fabric in a standard residential washing machine at 105 degrees F for 12 minutes using 10 g of Tide® laundry detergent (available from Procter & Gamble) at the high water level setting. The fabric was then dried in a standard residential dryer for 45 minutes on the cotton sturdy setting. A 4-pound load of laundry comprised of the test fabric and non-test (or “dummy”) fabric was used for each test.
Soil release was determined by AATCC Method 130-2000 using a scale from 1 to 5, wherein “5” indicates optimal soil release and “1” indicates poor soil release. Corn oil was applied to the fabric as the staining agent, and the fabric was rated for soil release after one wash (indicated as “0/1”) and two washes (indicated as “0/2”). Further testing in some examples below includes staining the fabric again after the fourth wash and rating the fabric for soil release after the fifth wash (indicated as “4/5”) and the sixth wash (indicated as “5/6”).
Abrasion resistance and strength were determined by a variety of methods: (a) Flex Abrasion, according to ASTM D3885; (b) Stoll Flat Abrasion, according to ASTM D3886; (c) Elmendorf Tear, according to ASTM D1424, wherein the warp direction was estimated to be the direction the fabric entered and exited the machine during manufacturing (machine direction), and the fill direction was estimated to be perpendicular to the machine direction; (d) Trap Tear, according to ASTM D5587, wherein the test was performed on the warp, or machine direction of the fabric; and (e) Grab Tensile, according to ASTM D5034, wherein the test was performed on the warp, or machine direction of the fabric.
Note that “N/T” indicates that a sample was not tested for a given parameter.
EXAMPLE 1
The following example shows treatment of the nonwoven fabric with the chemical mixture of the current invention in a laboratory setting. The fabric utilized here was 100 g/m 2 point bonded Evolon®.
A one-liter solution of the desired chemical mixture was place in a beaker. The solution was comprised of 0.25% wetting agent (Synthropol® KB from Clariant), 4.0% hydrophilic silicone (Duosoft® OH from Boehme Filatex), 2.0% fluorocarbon (Zonyl® 7910 from Ciba Specialty Chemicals), 10.0% polyethylene (Atebin® 1062 from Boehme Filatex), and 83.75% water. The chemical mixture was then padded onto a 20″×20″ piece of fabric by placing the fabric in the beaker and coating it with the mixture. The fabric was then removed from the beaker and run through a chemical padding machine to remove excess chemical. The fabric was then hung in an oven and dried at 360 degrees F for two minutes. The results are shown in Table 1 below.
TABLE 1
Comparison of Treated Nonwoven Fabric versus Untreated
Nonwoven Fabric
Flex Abrasion
Martindale Pilling/
(# Cycles to Failure)
Marks & Spencer
Soil Release
Sample
Warp
Fill
(18,000 Cycles, 9 Kpa)
0/1
0/2
Treated
No HLTD
11,129
4144
A
3.0
3.5
1 HLTD
N/T
A
N/T
5 HLTD
N/T
A
N/T
Untreated
No HLTD
2522
2599
A
1.5
2.0
1 HLTD
N/T
E
N/T
5 HLTD
N/T
D
N/T
Several observations can be made regarding the data in Table 1. First, the chemically treated samples exhibit greater abrasion resistance than the untreated samples in both the warp estimated and fill estimated directions according to the Flex Abrasion test method. The warp direction withstands a higher amount of abrasion than the fill direction, which is most likely explicable by the fact that the warp direction is estimated as the machine direction of the fabric during the manufacturing process, which typically tends to be inherently stronger than the fill direction. Martindale Pilling shows pilling resistance is greatly enhanced after laundering for the treated fabric sample. It also indicates that the fabric is strong enough to withstand at least the minimum number of cycles typical for end-use products such as apparel, bedding, napery, and upholstery. This minimum number of cycles is typically about 2000 cycles for these end-uses. Additionally, the soil release property of the fabric is increased for both the 0/1 and 0/2 tests after chemical treatment. These factors indicate the effectiveness of the chemical treatment for achieving pilling resistance and soil release on the nonwoven textile article without compromising (and actually improving) abrasion resistance in both the warp and fill estimated directions.
EXAMPLE 2
Example 1 was repeated, except that the concentration of Zonyl® 7910, a soil release agent according to the present invention, was increased from 2.0 weight percent to 4.0 weight percent on weight of the chemical mixture. The soil release results are shown in Table 2 below.
TABLE 2
Comparison of Soil Release Concentration on Treated
Nonwoven Fabric
Soil Release Results
Sample
0/1
0/2
4/5
5/6
2.0% Zonyl ® 7910
3.0
3.5
3.0
3.5
4.0% Zonyl ® 7910
3.5
4.0
3.0
3.5
Table 2 shows that increasing the amount of soil release chemical from 2.0 to 4.0 weight percent on weight of the chemical mixture, while maintaining unchanged concentrations of the other chemicals, increases the soil release properties of the treated fabric after 1 wash and after 2 washes. These results indicate the effectiveness of the soil release chemicals at optimal concentration for the present invention.
EXAMPLE 3
The following example shows treatment of the fabric with the chemical mixture of the current invention in a manufacturing or production setting. The fabric utilized here included both 100 g/m 2 and 120 g/m 2 standard and point bonded Evolon® fabric. Some fabric samples were undyed, while others were dyed using standard dyeing techniques (both jet-dye and continuous dyeing processes) and dye formulations known to those skilled in the art.
The chemical mixture was prepared using 0.25% wetting agent (Solpon® 839 from Boehme Filatex), 10% polyethylene (Atebin® 1062 from Boehme Filatex), 6% hydrophilic silicone (Duosoft® OH from Boehme Filatex), 4% fluorocarbon (Zonyl® 7910 from Ciba Specialty Chemicals), and 79.75% water. There were ten 100-yard fabric samples treated with the chemical mixture (Samples 3-7 and 10-14) and four 100-yard control fabric samples treated only with water (Samples 1-2 and 8-9). The samples included:
Sample
Number
Sample Description
1
Standard Greige, 100 g/m 2 (Control A)
2
Point Bonded Greige, 100 g/m 2 (Control B)
3
Standard Prepared For Print, 100 g/m 2
4
Point Bonded Prepared For Print, 100 g/m 2
5
Point Bonded Continous Dyed White, 100 g/m 2
6
Point Bonded Continuous Dyed Navy, 100 g/m 2
7
Point Bonded Jet-Dyed Burgandy, 100 g/m 2
8
Standard Greige, 120 g/m 2 (Control C)
9
Point Bonded Greige, 120 g/m 2 (Control D)
10
Standard Prepared For Print, 120 g/m 2
11
Standard Jet-Dyed Navy, 120 g/m 2
12
Point Bonded Jet-Dyed Green, 120 g/m 2
13
Point Bonded Jet-Dyed Tan, 120 g/m 2
14
PS33 (point bonded in herringbone pattern) Continuous
Dyed White, 120 g/m 2
The chemical mixture was padded on the fabric by dipping the fabric in the dip pad of a pin tenter range. The pad nip pressure was 55 psi with a wet pick up of 140%. The overfeed to chain speed was 2%, and all circulating fans were set on high. The vacuum slot was turned off. The fabric was then dried in the tenter by running the fabric at 40 yards per minute through the heat zones of the tenter which averaged 366 degrees F. The exhaust dampers were set at 50%, and the cooling cans were 80 degrees F. The winder oscillator was off.
After drying, the fabric was exposed to a face-finishing process (as described in U.S. Pat. Nos. 5,822,835, 4,918,795, and 4,837,902), wherein two zones of high velocity gaseous fluid were directed to the surface of the fabric in opposite directions at 20 psi and at 1.0 tension setting on the entry and exit rolls. Following this treatment, the fabric was sanforized. The fabric was then inspected and tested for abrasion resistance and strength. The results are shown in Table 3 below.
TABLE 3
Abrasion Resistance and Strength of Treated Nonwoven Fabric
versus Untreated Nonwoven Fabric
Elmendorf
Grab
Flex
Tear
Trap Tear
Tensile
Stoll Flat
Abrasion
(Pounds)
(Pounds)
(Pounds)
(# Cycles
(# Cycles
Sample
Warp
Warp
Warp
to Failure)
to Failure)
1
1.17
6.51
65.8
518.0
602
(Control A)
2
0.56
5.04
67.5
499.3
490
(Control B)
Control
0.87
5.78
66.7
508.7
546
Average
3
2.59
10.25
75.6
483.0
17,149
4
2.14
9.60
82.8
693.0
18,818
5
2.05
8.27
82.6
536.0
18,632
6
2.05
8.97
82.5
634.0
18,674
7
2.22
8.70
75.4
N/T
N/T
Sample 3-7
2.21
9.16
79.8
586.5
18,318
Average
8
1.07
6.57
80.4
602.0
475
(Control C)
9
0.75
4.85
85.3
758.7
675
(Control D)
Control
0.91
5.71
82.9
680.4
575
Average
10
3.01
10.09
84.2
693.0
19,673
11
3.15
11.49
85.4
1033.0
N/T
12
2.95
14.98
96.7
1299.0
14,797
13
2.87
12.43
93.2
N/T
N/T
14
2.33
9.97
105.6
1104.0
19,708
Sample
2.86
11.79
93.0
1032.3
18,059
10-14
Average
Several observations can be made regarding the results shown in Table 3. All of the treated samples, both the 100 g/m 2 and 120 g/m 2 fabrics, exhibit improved abrasion resistance after treatment with the chemical mixture of the present invention. The heavier weight 120 g/m 2 samples, both treated and untreated, generally exhibited higher strength and abrasion resistance characteristics. Exposure of the fabric to a wide variety of different abrasion and strength tests as shown in this example confirms the usefulness and applicability of this fabric treatment for a large array of end-use applications as previously discussed.
The above description and examples show that the present invention provides a novel method for imparting pilling resistance and soil release properties to nonwoven textile articles without compromising the strength and abrasion resistance characteristics of the articles. Accordingly, the invention has many applicable uses for incorporation into articles of apparel, bedding, residential upholstery, commercial upholstery, automotive upholstery, napery, residential and commercial cleaning cloths, and any other article wherein it is desirable to manufacture a pilling resistant product with soil release properties that retains its required strength and abrasion resistance characteristics for its intended end use.
The above description and examples also provide a novel composition of matter for imparting pilling resistance, soil release, strength, and abrasion resistance properties to nonwoven textile articles. The composition of matter comprises a hydrophilic silicone, a soil release agent, an abrasion resistance agent, water, and optionally a wetting agent and a defoaming agent. The concentration of the hydrophilic silicone is between about 2 and about 8 weight percent on weight of the composition of matter. The soil release agents are selected from the group consisting of acrylics, fluorocarbons, liquid polyesters, and combinations thereof. The concentration of acrylic is between about 2 and about 12 weight percent on weight of the composition of matter. The concentration of fluorocarbon is between about 0.5 and about 6 weight percent on weight of the composition of matter. The concentration of liquid polyester is between about 2 and about 6 weight percent on weight of the composition of matter. The abrasion resistance chemicals are selected from the group consisting of polyethylenes, polyurethanes, and combinations thereof. The concentration of polyethylene is between about 8 and about 16 weight percent on weight of the composition of matter. Generally, polyethylenes with a higher melting point (usually referred to as high-density polyethylenes), such as greater than about 124 degrees Celsius, are preferred over low melting point polyethylenes (usually referred to as low-density polyethylenes). The concentration of polyurethane is between about 6 and about 18 weight percent on weight of the composition of matter. A wetting agent, such as an ethoxylated long chain alcohol wherein the chain is at least 9 carbon atoms long, may be included as a component of this composition of matter in concentrations of between about 0.2 and about 0.3 weight percent on weight of the composition of matter. A defoaming agent, such as mineral oil, silicone defoamers, and de-aerating agents, may be included as a component of this composition of matter in concentrations of between about 0.05 and about 2 weight percent on weight of the composition of matter.
These and other modifications and variations to the present invention may be practiced by those of ordinary skill in the art, without departing from the spirit and scope of the present invention. Furthermore, those of ordinary skill in the art will appreciate that the foregoing description is by way of example only, and is not intended to limit the scope of the invention described in the appended claims. | A chemically modified nonwoven textile article and method for producing the same is provided that exhibits pilling resistance, soil release, strength, and abrasion resistance properties, thus rendering the article less prone to the formation of objectionable pill balls, staining, or loss of strength, thereby increasing wearer comfort and retaining the desired appearance of the article, and thereby extending the useful life of the article. A composition of matter for chemically modifying a nonwoven textile article to achieve pilling resistance, soil release, strength, and abrasion resistance is also provided. | 3 |
FIELD OF THE INVENTION
The present invention relates to an integrated circuit or semiconductor device. More particularly, the present invention relates to a method for decorating a semiconductor wafer to reveal defects.
BACKGROUND OF THE INVENTION
In the fabrication of integrated circuits (ICs), chemical mechanical planarization (CMP) is widely used for polishing inter-level dielectrics (ILD) on multi-layer devices which utilize interconnect structures. More recently, isolation schemes like shallow trench isolation (STI) have also made use of CMP.
In general, a CMP process involves holding a semiconductor wafer against a rotating polishing pad. A polishing slurry is added, e.g. a solution of alumina or silica, as the abrasive medium. The polishing slurry contains small, abrasive particles that polish the surface of the wafer. The content of this slurry determines its operability. Throughout the process, the wafer is kept under controlled chemical, pressure, velocity and temperature conditions.
CMP tends to leave surface defects, such as microscratches and particulate defects, on the surface or layer being planarized or polished. A microscratch is a small scratch, typically about 5 micrometers to 20 micrometers in length and 500 Å to 1000 Å in depth. These defects can result in connectivity problems between layers and components of the semiconductor device. Connectivity problems are compounded by subsequent mask and etch processes, the expected results of which can be disturbed by the presence of such defects, ultimately adversely effecting product yield and production cost.
Surface defects, such as microscratches, can be reduced or eliminated by adjusting the content and filtration of the slurry, and adjusting the composition of the layer being polished, e.g. an oxide layer, for greater resiliency to defects. However, microscratches are difficult to detect. Thus, in a fabrication process comprising multiple steps of etching, masking and deposition of layers on a substrate, it is difficult to identify which of these steps is causing the defects.
A variety of techniques currently exist for inspecting the surface of semiconductor wafers. These techniques include light scattering topography (LST), stylus profilometry, phase shift interferometry, and atomic force microscopy (FM). However, surface defects are not always readily visible with these conventional inspection methods due to the small size of microscratches and because they are typically filled with unwanted residual from a previously deposited layer. Thus, heretofore it has not been possible to identify microscratches in a post-CMP substrate and, consequently, it has not been possible to identify and optimize the step causing the microscratches.
Thus, there is a need for a semiconductor wafer inspection process that reveals surface defects, such as microscratches, to aid in isolation and optimization of defect-causing steps in the semiconductor fabrication process.
SUMMARY OF THE INVENTION
The present invention relates to a method of inspecting a semiconductor wafer for defects by providing a layer of material on the wafer, polishing the wafer to remove a portion of the layer, dipping the wafer in an etchant for a period of time, and inspecting the wafer for defects. The step of dipping reveals defects in the wafer that were previously undetectable, allowing isolation and optimization of the fabrication step causing the defects.
The present invention further relates to a method of inspecting a semiconductor wafer for defects due to chemical mechanical planarization (CMP) by providing an oxide layer on the wafer, polishing the wafer to remove a portion of the oxide layer, etching the wafer in a dilute etchant solution for a period of time, and inspecting the wafer for defects so that defects due to the CMP step can be examined.
The present invention further relates to a method of inspecting a semiconductor wafer for defects due to chemical mechanical planarization by providing a semiconductor wafer, providing an oxide layer on the wafer, polishing the wafer by CMP to remove at least a portion of the oxide layer, decorating the wafer with an etchant, and inspecting the wafer for defects using an optical inspection tool to determine a defect count.
BRIEF DESCRIPTION OF THE DRAWINGS
The preferred exemplary embodiment of the invention will hereinafter be described in conjunction with the appended FIGURES, in which like reference numerals denote like elements, and:
FIG. 1 is a cross-sectional view of a semiconductor substrate;
FIG. 2 is a cross-sectional view of the semiconductor substrate of FIG. 1 after CMP showing a microscratch;
FIG. 3 is a cross-sectional view of the semiconductor substrate of FIG. 2 after deposition of a second layer of material;
FIG. 4 is a perspective view of an inspection tool for identifying surface defects; and
FIG. 5 is a flowchart showing a process according to the present invention.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
Referring to FIG. 1, there is shown a cross-sectional view of a semiconductor wafer 10 . Semiconductor wafer 10 has a substrate 12 on which a plurality of IC components 14 have been formed. Components 14 may be any type of semiconductor device, transistor, or portion thereof made from any of the various semiconductor processes, such as complimentary metal oxide semiconductor (CMOS) process, bipolar process, etc. Substrate 12 is typically formed of a single crystal silicon material, or may be another semiconductive material such as germanium or gallium arsenide. IC components 14 are typically formed by an etch and mask process. Layer 16 is a layer of material, and may be any type of non-planar dielectric layer or insulative layer such as an oxide film, a pad oxide layer, an oxide layer deposited with tetraethylorthosilicate (TEOS), or a nitride layer. Layer 16 may be grown or deposited by chemical vapor deposition (CVD), physical vapor deposition (PVD), sputtering deposition, collimated sputtering deposition, dipping, evaporating, or other application techniques.
Referring now to FIG. 2, semiconductor wafer 10 is shown after planarization or polishing. The polishing can be by oxide CMP, reaction ion etching, or another polishing technique that may leave defects. Layer 16 has been polished to a level top surface 18 . It is now possible to apply subsequent layers, either conductive, semiconductive or insulative to the top surface 18 of layer 16 . FIG. 2 also shows a scratch or microscratch defect 20 having a gap 22 caused by the polishing step.
Referring to FIG. 3, semiconductor wafer 10 is shown after deposition of a second layer of material 24 , for example a layer of conductive material such as polysilicon. Second layer 24 is applied by one of a variety of application techniques, for example an etch and mask technique, to create a set of second components 28 above layer 16 . FIG. 3 also shows an unwanted portion 26 of material 24 that has accumulated in gap 22 of microscratch defect 20 . This unwanted portion 26 will create undesireable electrical properties of wafer 10 . In particular, unwanted portion 26 is shown electrically shorting together two of the second set of components 28 .
Referring now to FIG. 4, an inspection tool is shown for determining surface defects in semiconductor wafer 10 . Inspection tool 30 is a light-scattering optical inspection device. Tool 30 may be any of a number of optical inspection tools known in the art, and is preferably an INSPEX 8525 manufactured by Inspex of Bellerica, Massachusetts. After polishing, semiconductor wafer 10 is placed on a platform 32 of inspection tool 30 . Laser source 34 emits a laser 36 which produces scatter from wafer 10 into imaging camera 38 . An enlarged view 40 of a portion 42 of wafer 10 showing microscratches 20 can be viewed on the computer screen of a nearby computer (not shown). By inspecting wafer 10 and counting the number of defects 20 in a given area, the defectivity of the polishing technique used can be evaluated.
Referring now to FIG. 5, there is shown a flowchart of a preferred embodiment of the present invention. At a step 50 , semiconductor wafer 10 (FIG. 1) has layer of material 16 deposited thereon, preferably an oxide layer deposited by chemical vapor deposition (CVD). At a step 52 , layer 16 is polished or planarized, preferably by a chemical mechanical planarization technique. The result of step 52 typically leaves defects 20 (FIG. 2 ), such as microscratches, in semiconductor wafer 10 . These microscratches 20 are not detectable with conventional optical inspection tool 30 (FIG. 4 ).
Therefore, at a step 54 , wafer 10 is exposed to or decorated with an etchant. The etchant may be any one of a variety of wet solutions or dry compositions that make defects 20 more visible with optical inspection tool 30 . One suitable etchant is dilute hydrogen fluoride (HF). The HF may also be buffered (BHF or BOE, buffered oxide etch) with a mild acidic buffering agent to maintain a stable pH. HF can be readily obtained in a solution of water with a 30% concentration. The HF can then be diluted to about 100 parts water to 1 part HF. Suitable ratios of water to HF are from about 1:1 to about 200:1. The greater the concentration of HF used, the quicker microscratches 20 will be revealed. Another suitable etchant is phosphoric acid solution. However, phosphoric acid etches at approximately 3 Å/minute, an etching rate much slower than that of the HF solution. Thus, if a slower, more controlled etch is desired, phosphoric acid may be preferable. If a quicker etch is desired, the HF may be preferable. A dry etchant composition is typically a plasma etchant.
Decoration with etchant may be done in many ways, but preferably is done with a robotic arm that submerges or dips wafer 10 into the etchant for a period of time. The etchant acts on the entire exposed surface 18 of layer 16 (FIG. 2 ). However, because the microscratches 20 are weaker areas of surface 18 , these areas are etched faster than the rest of layer 16 . Thus, the greater the time that wafer 10 is submerged in the etchant, the more visible microscratches 20 become. Wafer 10 may be submerged in the HF for about 10 to about 100 seconds, but preferably about 30 seconds. If phosphoric acid is the etchant, perhaps a longer period may be necessary. Subsequent to the submersion step, wafer 10 is rinsed with deionized water and dried with isopropyl alcohol vapor. Other rinsing and drying steps may be employed as well, e.g. air drying, spin drying, etc.
At a step 56 , wafer 10 is inspected and defects 20 are counted. Defects 20 can now be seen with the use of conventional optical inspection tool 30 . Defects 20 can be counted and compared to the defect counts left by other polishing techniques or optimizations. As a result, the present invention makes it possible to evaluate different types of oxide polishing slurries, slurry filtration effectiveness, slurry dilution methods, etc., which can be evaluated and optimized to obtain minimal micro-scratches on polished oxide wafers. Also, different types and compositions of oxides for STI applications with respect to their tendency to develop micro-scratches due to oxide CMP can be evaluated and optimized.
EXAMPLE
A 7200 Å layer of insulating material was deposited on two 200 millimeter blank silicon wafers by low-pressure chemical vapor deposition (LPCVD) technique utilizing tetraethylorthosilicate (TEOS). The first wafer was polished on an oxide CMP tool using a typical oxide CMP process to a post-polish oxide thickness of about 5000 Å. The second wafer, the control wafer, did not go through the polishing step. Both wafers were subjected to a typical post-polish cleaning and were subsequently inspected using an optical inspection tool, in this case an INSPEX 8525. A baseline defectivity level, or defect count, was obtained for both wafers. No significant differences in defectivity were observable between the first polished/cleaned wafer and the control non-polished/cleaned wafer. Both wafers were then decorated in a dilute HF dip for 30 seconds, rinsed and dried. The wafers were once again inspected for defects on the INSPEX 8525. This time there was a significant increase in the defectivity of the first, polished wafer compared to the control wafer. Most of the defects on the first, polished wafer were microscratches. Other defects included particulate defects.
Before the decorating step of the present invention, the microscratches were undetectable with the INSPEX tool. Thus, it was indeterminate at which step in the multi-layer fabrication process the microscratches were being created. Once it was identified that the oxide CMP was causing the microscratches, steps were taken to improve the CMP process. In this case, the polishing slurry of the CMP process was adjusted, thereby reducing the incidence of microscratches by two-thirds. Thereafter, a filter was added to the line that carries the CMP slurry, thereby reducing microscratches by another five-sixths. Thus, it can be seen that the feedback of the present invention improved this step of the fabrication process significantly.
It is understood that, while the detailed drawings and specific examples given describe preferred exemplary embodiments of the present invention, they are for the purpose of illustration only. The present invention is not limited to the precise details, methods, materials, and conditions disclosed. For example, although a wet HF etchant solution was used, other etchants, including dry etchants, may be employed. Further, although the present invention was applied to chemical mechanical planarization, it may also find uses in determining defects for other polishing, planarizing and semiconductor fabrication processes. | A method of decorating a semiconductor substrate with an etchant solution is provided for revealing defects, such as microscratches, resulting from an oxide chemical-mechanical planarization (CMP) polishing. An oxide layer is provided over the substrate made from, for example, tetraethylorthosilicate (TEOS). The oxide layer is polished by a CMP process which tends to leave behind microscratches and other defects that can cause conductivity problems on the wafer. To reveal the microscratches, the wafer is decorated or submerged in an etchant, such as an HF etchant, for a period of time. Following the decorating, the wafer is rinsed, dried and inspected. The method improves the ability to identify and optimize steps in a semiconductor fabrication process that cause semiconductor defects. | 8 |
CROSS-REFERENCES TO RELATED APPLICATIONS
[0001] This application is a continuation in part of prior pending application Ser. No. 12/660,005 filed on Feb. 19, 2010.
STATEMENT REGARDING FEDERALLY SPONSORED RESEARCH OR DEVELOPMENT
[0002] Not Applicable
MICROFICHE APPENDIX
[0003] Not Applicable
BACKGROUND OF THE INVENTION
[0004] 1. Field of the Invention
[0005] This invention relates to the field of mower blades. More specifically, to the weight or mass distribution of the blades center compared to the blades outermost end.
[0006] 2. Description of the Related Art
[0007] When mower blades are new, they provide a clean and quick cut. After repeated uses and wear, the blade starts to loose mass or weight on the outer end. Additionally, repeated sharpening of the blade contributes to the loss of mass on the cutting edge, which is the outermost end of the blade. As the blade end loses mass or weight, it becomes less efficient at cutting and eventually has to be replaced with a new, unworn, blade.
[0008] Therefore what is needed is a mower blade that does not lose its cutting efficiency after wear from use and sharpening. And such remedy would also increase the cutting power of the blade. The present invention achieves this objective, as well as others that are explained in the following description.
BRIEF DESCRIPTION OF THE DRAWINGS
[0009] A complete understanding of the present invention may be obtained by reference to the accompanying drawings, when considered in conjunction with the subsequent, detailed description in which:
[0010] FIG. 1A is a top plan view of a prior art standard mower blade;
[0011] FIG. 1B is a top plan view of a prior art standard mower blade with a worn down prior art cutting edge;
[0012] FIG. 2A is a top plan view showing the present invention;
[0013] FIG. 2B is a top plan view showing the present invention with a worn down cutting edge worn;
[0014] FIG. 3A is a top plan view showing an alternate embodiment of the present invention;
[0015] FIG. 3B is a top plan view showing an alternate embodiment of the present invention;
[0016] FIG. 4A is a top plan view showing an alternate embodiment of the present invention with an extended outer cutting edge;
[0017] FIG. 5A is a top plan view showing an alternate embodiment of the present invention;
[0018] FIG. 5B is a top plan view showing an alternate embodiment of the present invention with an extended outer cutting edge;
[0019] FIG. 6A is a perspective view of a prior art standard mower blade;
[0020] FIG. 6B is a perspective view showing the present invention;
[0021] FIG. 6C is a perspective view showing the present invention;
[0022] FIG. 7 is a perspective view showing the present invention with added mass to the end section;
[0023] FIG. 8 is a cross section view showing the end section attached to the outer cutting edge of the present invention;
[0024] FIG. 9A is a perspective view showing the present invention;
[0025] FIG. 9B is a cross section view showing the end section attached to the outer cutting edge of the present invention;
[0000]
REFERENCE NUMERALS IN THE DRAWINGS
10
present blade
12
prior art rotor
14
prior art center
16
extension
18
end section
20
prior art outer cutting edge
26
inner blade portion
28
prior art outer end
30
outer cutting edge
32
rotor
34
center
36
rotor
38
outer end
42
bolts
DETAILED DESCRIPTION OF THE INVENTION
[0026] FIG. 1A is a top plan view, showing a prior art standard mower blade. FIG. 1B is also a top plan view showing a prior art standard mower blade with a worn away outer cutting edge. FIGS. 1A and 1B are prior art mower blades showing prior art attachment point 14 , prior art rotor 12 and prior art outer cutting edge 20 on prior art outer end 28 . In the prior art standard mower blade the prior art rotor 12 has basically the same size throughout. This includes the same thickness and width from prior art attachment point 14 to prior art outer end 28 at prior art outer cutting edge 20 . Some blades do have minor shape changes but not enough to be relevant to a substantial increase in mass on prior art outer end 28 . As illustrated in FIG. 1B , prior art outer cutting edge 20 is worn down. The wearing away of the prior art cutting edge 20 has reduced the mass on the outer cutting edge 20 , causing a significant decrease in cutting potential. Due to the decrease in mass, the energy delivered is now less, which equals less damage to the object being cut. This kind of wear on a standard blade 12 could greatly reduce its cutting efficiency.
[0027] FIG. 2A shows the present invention. The blade 10 generally consists of a rotor with added or increased weight or mass, shown as extension 16 on outer end 38 of rotor 32 . The added or increased weight provided by extension 16 generates more energy to the object(s) being cut even where the speed at which the rotor spins remains constant. Extension 16 lies in the same plane as outer end 38 , thereby preventing outer end 38 to generate unnecessary drag as it travels through the air. FIG. 2B shows the present invention with a worn down outer cutting edge 30 . Outer end 38 with cutting edge 30 has so much more added or increased weight or mass, shown here as extension 16 , that the loss from wear is insignificant. Even with the worn away outer cutting edge 30 , the present blade will still do damage and will not have to be replaced. Note: the arrows at the outer end 38 , show the direction of rotation. Extension 16 extends off of outer end 38 of present blade 10 and remains on the same plane as rotor 32 . It is important that the blade remains streamlined such that it does not produce additional drag as it travels through the air.
[0028] FIGS. 3A and 3B are top plan views of different embodiments of the present invention. In the alternate embodiments there is more mass on the outer end 38 where outer cutting edge 30 is located, and less mass at the “non cutting” attachment point 34 . End section 18 is shown on either side of the present blade 10 in both FIG. 3A and 3B . As shown in FIGS. 7 and 9A , end section 18 adds or increases weight further to outer end 38 by either sitting on top of outer end 38 or being integrated fully with outer end 38 . A perspective view of end section 18 is shown in FIG. 7 and a cross section view of end section 18 is shown in FIG. 8 . As shown in FIG. 7 , end section 18 sits on outer end 38 while extension 16 extends off of outer end 38 opposite outer cutting edge 30 and direction of blade (shown by arrows). In FIG. 8 end section 18 is shown bolted to outer end 38 by passing bolts 42 through outer end 38 and into end section 18 . While outer end 38 is shown attached in this manner any known method of attaching outer end 38 to the present blade 10 could be used. Additionally, end section 18 could be fully integrated with the present blade 10 . FIGS. 9A and 9B illustrate end section 18 set on top outer end 38 while extension 16 does not extend beyond end section 18 . Outer cutting edge 30 wraps around outer end 38 to provide an additional cutting edge. In the cross section view shown in FIG. 9B , end section 18 is flush with outer end 38 and can be attached by any known method, including, but not limited to, a glue or weld or end section 18 could be fully integrated with the present blade 10 .
[0029] FIG. 4A illustrates the present blade 10 in a slightly different shape which, by design, includes greater weight or mass to the outer end 38 of rotor 32 as opposed to at attachment point 34 of rotor 32 . While all of the blades shown are designed as a particular shape, the present invention should not be limited to the shapes shown.
[0030] FIGS. 5A and 5B show a top plan view of blades for “bush-hog” type mowers. In FIGS. 5A and 5B extensions 16 are located on outer end 38 for the purpose of adding weight to the outer end 38 of rotor 36 . FIG. 6A is a perspective view of a prior art standard blade 12 . Standard blade 12 is uniform in weight distribution from prior art attachment point 14 to prior art outer end 28 . The present invention, shown in FIG. 6B , creates more mass on outer end 38 by increasing blade width with the addition of extension 16 which lies in the same plane as rotor 36 . The present invention is also shown in 6 C, wherein the desired result is achieved by increasing the width of outer end 38 in comparison to the smaller blade portion 26 as it nears, attachment point 34 . The additional weight, shown by extension 16 or by increasing the width of rotor 36 at outer end 38 , increases the energy to be delivered by outer cutting edge 30 upon an external object, such as grass.
[0031] Since other modifications and changes varied to fit particular operating requirements and environments will be apparent to those skilled in the art, the invention is not considered limited to the example chose for purposes of disclosure, and covers all changes and modifications which do not constitute departures from the scope of this invention. | A mower blade generally comprised of a rotor which connects to the mower at an attachment point and at least one outer end of the rotor, wherein the outer end or ends of the rotor are heavier than the rotor proximate the attachment point. The added weight to the outer end can be by way of an extension or an end section. | 0 |
This application claims the benefit of priority under 35 U.S.C. §119 of U.S. Provisional Application Ser. No. 61/526,860 filed on Aug. 24, 2011 the content of which is relied upon and incorporated herein by reference in its entirety.
BACKGROUND
1. Field
The present invention relates to an apparatus and method for characterizing glass sheets, and in particular to an apparatus adapted to measure one or more selected attributes of a glass sheet while the glass sheet is in motion.
2. Technical Background
The invention relates to controlling motion and attitude of a glass sheet being conveyed along a predetermined path to enable high resolution online measurements, such as topography inspection (e.g. nanotopography, or topography on a nanometer scale). Accurate online measurements of thin glass sheets, and in particular the measurement of nanometer-scale features, is highly dependent upon consistently presenting the glass sheets in a predetermined plane at a predetermined orientation and eliminating the vast majority of vibrations and oscillations of the glass. Challenges such as high accuracy measurement of thickness, waviness, and cord are highly dependent on presenting the glass surface to measurement gauges with reproducible, high tolerance material handling.
Online process control and quality measurements, such as online cord and streak inspection, suffer from a lack of repeatability when performed while simply gripping the glass in a non-quality area. A large part of the material presentation challenge is keeping the sheet of glass moving down a production line while being suspended from a carrier on an overhead conveyor. This constraint often forces measurements to be performed either in a separate inspection portion of the process line, completely offline, or the measurement technology compatible with coarse traditional online material handling is limited in its performance (e.g. resolution).
High resolution metrology is performed online in other industries, such as silicon wafers or paper and plastic webs, but in these cases, the product is in direct contact with a supporting plate, as with wafers, or with rollers, as with most webs. The size and contact prohibition on glass sheets suitable for display applications presents a difficult challenge for handling.
SUMMARY
Measurement of thin glass sheets, generally equal to or less than 1 mm in thickness, may exhibit an amount of curvature or warping that creates difficulty when measuring certain attributes of the glass, particularly if the glass is large (e.g. greater than about 4 m 2 ). To overcome this deficiency, the glass must first be flattened. In the past, flattening and stabilizing the glass sheet has involved removing the sheet from the inline path, transferring the glass sheet to a precision granite base, then vacuuming individual glass sheets to a vacuum table, making the desired measurements, removing the glass sheets, and then performing the same operation with another glass sheet. Such a piecemeal approach adds considerable time and expense to a manufacturing process. The challenge of measuring large thin glass sheets is exacerbated if there is a need to measure the glass sheet while the glass sheet is transported along a manufacturing line.
In some manufacturing processes, glass sheets can be conveyed from one location to another location by clamping the glass sheet to a moving member in an overhead conveyor. It would be beneficial if one or more of the aforementioned characterizations could be accomplished while the glass sheet was in motion, without first dismounting the glass sheet and positioning the glass sheet on a measurement table as a stationary object.
To that end, an apparatus is disclosed for making precision measurements of moving glass sheets, such as glass sheets suitable for use in a liquid crystal display devices, by constraining the glass sheets while still held by a conveyor carrier. The material handling features of the apparatus include air knives and pressure-vacuum (PV) air bearings, arranged in linear fashion such that a glass sheet entering the apparatus is subjected to a non-contact but gradual increase in constraining force until the point where measurements can be performed. A gradual decrease in constraining force then occurs until the sheet is released from the apparatus. This graduated force technique is applied along the direction of travel of the glass sheets and also vertically upward along the height of the sheets to restrict the motion of the sheets without constraining it at pinch points near the conveyor carriers.
Accordingly, an air bearing is disclosed comprising an annular inner porous body portion comprising a circular groove in a surface of the inner porous body portion, and a plurality of radial grooves intersecting the circular groove, the inner porous body portion defining a central passage extending through a thickness of the air bearing; an outer porous body portion disposed about the inner porous body portion, wherein the outer porous body portion comprises a plurality of continuous grooves in a surface of the outer porous body portion; and wherein each continuous groove of the outer porous body portion comprises a plurality of vacuum ports. The circular groove of the inner porous body portion and the radial grooves of the inner porous body portion divide the surface of the inner porous body portion into a plurality of sub-surfaces, and a sub-surface of the plurality of sub-surfaces comprises a vacuum port. Preferably, each sub-surface of the plurality of sub-surfaces comprises a vacuum port.
The outer porous body portion preferably comprises an arcuate outer circumference, and preferably the outer porous body portion comprises a circular outer circumference such that the air bearing comprises an annular inner porous body portion and an annular inner porous body portion disposed about and concentric with the inner porous body portion. In some embodiments the air bearing comprises a plurality of inner porous body portions. For example, the plurality of inner porous body portions may be aligned along a horizontal axis.
In another embodiment, an apparatus for characterizing glass sheets as the glass sheets move past the apparatus is disclosed comprising: an air bearing comprising an annular inner porous body portion, and an outer porous body portion disposed about the inner porous body portion, the inner porous body portion defining a central passage extending through a thickness of the air bearing; a plurality of stabilizing air knives positioned upstream of the air bearing relative to a direction of travel of the glass sheets; and a measurement device to measure at least one attribute of the glass sheet, the measurement device being aligned with the central passage of the air bearing. The inner porous body portion comprises a circular groove in a surface thereof. The inner porous body portion may further comprise a plurality of radial grooves intersecting the circular groove. The surface of the inner porous body portion comprises a vacuum port. If the inner porous body portion comprises a circular groove and a plurality of radial grooves, the circular groove and the radial grooves define a plurality of sub-surfaces on the inner porous body portion. Preferably, each sub-surface comprises a vacuum port.
The outer porous body portion comprises a plurality of continuous (i.e. closed) grooves, each continuous groove comprising a plurality of vacuum ports. For example, each continuous groove can be a circular, oval, elliptical, or any other closed, continuous shape. Preferably, an outer circumference of the outer porous body portion is arcuate. For example, the outer circumference of the outer porous body portion may be circular. The air bearing may in some embodiments comprise a plurality of inner porous body portions.
The measurement device preferably measures the at least one attribute through the passage defined by the inner porous body portion.
The stabilizing air knives are oriented such that a flow of air from the stabilizing air knives is angled in a downward direction. That is, the flow of air from the stabilizing air knives is preferably directed in a downward direction relative to a horizontal plane so that the flow of air makes an acute angle with the glass sheet. For example, a direction of the flow of air may form an angle in a range from about 15 degrees to about 75 degrees relative to the glass sheet. Preferably, the stabilizing air knives are arcuate in shape.
The apparatus according to the present embodiment may further comprise a positioning air knife positioned downstream of the air bearing to force the glass sheet in a direction away from the air bearing.
In still another embodiment, a method of characterizing moving glass sheets is described comprising: moving a glass sheet in a first direction along a predetermined path, the glass sheet comprising a pair of opposing major surfaces, a bottom edge, and a leading edge relative to the first direction; dampening movement of the glass sheet in a second direction perpendicular to the first direction by passing the glass sheet between at least two stabilizing air knives as the glass sheet is moving in the first direction; engaging the glass sheet with a circular air bearing, the circular air bearing comprising an inner porous body portion and a outer porous body portion disposed about the inner porous body portion, the inner porous body portion defining a central passage therethrough; and measuring at least one attribute of the glass sheet as the glass sheet moves in the first direction. The method may further comprise guiding a bottom edge of the glass sheet with an edge guiding device comprising guide arms arranged to form a “V”-shaped slot therebetween.
A height of the air bearing, and more particularly a height of the outer porous body portion, is less than one half a height of the glass sheet. The air bearing is positioned such that an upper one half of the glass sheet is preferably not adjacent to the air bearing as the glass sheet is measured. The air bearing is preferably capable of maintaining the glass sheet within +/−15 μm of a predetermined distance from the inner porous body portion.
The first inner porous body portion comprises a circular groove in a surface thereof. The inner porous body portion preferably also comprises a plurality of radial grooves in the surface of the inner porous body portion, wherein the plurality of radial grooves intersect the circular groove.
The outer porous body portion of the air bearing preferably comprises a plurality of concentric grooves, wherein each groove of the plurality of concentric grooves comprising a plurality of vacuum ports.
In still another embodiment, a method of making a glass sheet is described comprising: heating a batch material in a melting furnace to form a molten glass material; flowing the molten glass material over converging forming surfaces of a forming body to produce a glass ribbon; cutting a glass sheet from the glass ribbon; suspending the glass sheet vertically from a conveyor, the conveyor moving the glass sheet in a first direction along a predetermined path; dampening movement of the glass sheet in a second direction perpendicular to the first direction by passing the glass sheet between at least two stabilizing air knives as the glass sheet is moving in the first direction; engaging the glass sheet with an air bearing, the air bearing comprising an annular inner porous body portion and a outer porous body portion disposed about the annular inner porous body portion, the annular inner porous body portion defining a central passage therethrough; and measuring at least one attribute of the glass sheet through the central passage as the glass sheet moves in the first direction. The outer porous body portion preferably comprises an arcuate outer circumference, such as a circular outer circumference.
The inner porous body portion comprises a circular groove in a surface thereof, and further preferably comprises a plurality of radial grooves intersecting the circular groove. The outer porous body portion comprises a plurality of continuous grooves in a surface thereof.
The method may further comprise using a first positioning air knife to move the glass sheet in a direction away from a leading edge of the air bearing. In a further optional step, the method may further comprise using a second positioning air knife to move the glass sheet in a direction toward the air bearing. In still another optional step, the method may further comprise using a third positioning air knife to move the glass sheet away from a trailing edge of the air bearing.
Each stabilizing air knife of the at least two stabilizing air knives directs a flow of air in a downward direction. A leading end of a stabilizing air knife of the at least two stabilizing air knives may optionally be pitched or inclined downward relative to a trailing end of the stabilizing air knife.
Additional features and advantages of the invention will be set forth in the detailed description which follows, and in part will be readily apparent to those skilled in the art from that description or recognized by practicing the invention as described herein, including the detailed description which follows, the claims, as well as the appended drawings.
It is to be understood that both the foregoing general description and the following detailed description present embodiments of the invention, and are intended to provide an overview or framework for understanding the nature and character of the invention as it is claimed. The accompanying drawings are included to provide a further understanding of the invention, and constitute a part of this specification. The drawings illustrate various embodiments of the invention and, together with the description, serve to explain the principles and operations of the invention.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a schematic diagram of an exemplary fusion glass making system for producing glass sheets;
FIG. 2 is a perspective view of an apparatus for characterizing a glass sheet according to an embodiment of the present invention;
FIG. 3 is a view of the apparatus of FIG. 2 seen looking down on the apparatus;
FIG. 4 is a top down view of an edge guiding device according to an embodiment of the present invention;
FIG. 5 is a top down view of an edge constraining device according to an embodiment of the present invention;
FIG. 6 is a side view of a roller of the edge constraining device of FIG. 5 showing the roller engaged with a rotary encoder;
FIG. 7 is a simplified front view of an air bearing according to an embodiment of the present invention illustrating the inner porous body portion and the outer porous body portion;
FIG. 8 is a side (edge) view of the air bearing of FIG. 7 ;
FIG. 9 is a front view of an air bearing according to an embodiment of the present invention shown in relation to a position of the air bearing relative to a glass sheet;
FIG. 10 is a detailed view of the air bearing of FIG. 7 ;
FIG. 11 is a frontal view of another embodiment of an air bearing wherein the air bearing comprises a plurality of inner piorous body portions;
FIG. 12A is a cross sectional view of a portion of the inner porous body portion of the air bearing of FIG. 10 ;
FIG. 12B is a cross sectional view of a portion of the outer porous body portion of the air bearing of FIG. 10 ;
FIG. 13 is a perspective view of an exemplary linear stabilizing air bearing according to the present invention, illustrating the flow of air from the elongated nozzle in a planar fashion;
FIG. 14 is a front view of the air bearing of FIG. 7 illustrating downward angle of an exemplary stabilizing air knife;
FIG. 15 is a top down view of the air bearing of FIG. 7 illustrating a sideways angle of an exemplary stabilizing air knife;
FIG. 16 is a side (edge) view of the air bearing of FIG. 7 illustrating a downward of a flow of air issuing from an exemplary stabilizing air knife;
FIG. 17 is a front view of the air bearing of FIG. 7 depicting the leading and trailing edges of the air bearing in relation to the direction of travel of the glass sheet;
FIG. 18 is a top down view of the apparatus of FIG. 2 showing the curvature produced in a glass sheet by the apparatus;
FIG. 19 is a cross sectional side view of a portion of the air bearing of FIG. 17 showing details of the curvature of the glass sheet adjacent to the air bearing;
FIG. 20 is a graph of fly height vs. time for two locations on the glass sheet as the glass sheet traveled at a speed of 100 mm/s, and illustrating the stability of the glass sheet position (i.e. fly height consistency).
DETAILED DESCRIPTION
In the following detailed description, for purposes of explanation and not limitation, example embodiments disclosing specific details are set forth to provide a thorough understanding of the present invention. However, it will be apparent to one having ordinary skill in the art, having had the benefit of the present disclosure, that the present invention may be practiced in other embodiments that depart from the specific details disclosed herein. Moreover, descriptions of well-known devices, methods and materials may be omitted so as not to obscure the description of the present invention. Finally, wherever applicable, like reference numerals refer to like elements.
In a down draw glass sheet making process, such as a fusion down draw process for example, glass sheets are formed by drawing a viscous glass material vertically downward under suitable conditions of viscosity and draw rate to form a ribbon of glass. The ribbon of glass comprises a viscous liquid at the upper-most extreme position of the ribbon and transitions from a viscous liquid to a solid glass ribbon as the material passes through the glass transition temperature range. When the descending bottom portion of the ribbon has reached a suitable temperature and viscosity, a glass sheet is cut from the ribbon, and so the process continues, with the glass sheets being cut from a continuously descending glass ribbon.
An exemplary fusion down draw glass making system 6 is shown in FIG. 1 . In accordance with FIG. 1 , batch materials 8 are loaded into melting furnace 10 and heated to form viscous molten glass material 12 . Molten glass material 12 is conveyed through finer 14 where bubbles are removed from the molten glass material, and then stirred in stirring apparatus 16 to homogenize the molten glass material. The stirring operation seeks to eliminate variations in the chemical consistency of the molten glass material, thereby avoiding variations in the physical and optical properties of the final glass. Once the molten glass material has been stirred, it flows through receiving vessel 18 and then to forming body 20 . Receiving vessel 18 functions as an accumulator by dampening minor flow fluctuations. Forming body 20 comprises a ceramic body having an open channel 22 in an upper portion of the body, and a pair of converging exterior forming surfaces 24 that join at a bottom of the forming body. The molten glass material overflows the open channel of the forming body and flows down the converging forming surfaces of the forming body as two separate flows of molten glass material. The separate flows of molten glass material join and form a single flow or ribbon 26 of material where the converging forming surfaces come together. The ribbon cools as it descends through the glass transition temperature region and forms a solid glass ribbon from which glass sheets 28 are cut along cut line 29 .
Melting furnace 10 is connected to and in fluid communication with finer 14 through melter-to-finer connecting tube 30 , and finer 14 is connected to and in fluid communication with stirring apparatus 16 through finer-to-stirring apparatus connecting tube 32 . Stirring apparatus 16 is connected to and in fluid communication with receiving vessel 18 through stirrer-to-receiving vessel tube 34 , and receiving vessel 18 is connected to and in fluid communication with forming body 20 through downcomer tube 36 and forming body inlet 38 . While melting furnace 10 is typically formed from a ceramic material, such as ceramic bricks (e.g. alumina or zirconia), those components involved in transporting and processing the molten glass material are typically formed from platinum, or a platinum alloy such as a platinum-rhodium alloy. Thus, melter-to-finer connecting tube 30 , finer 14 , finer-to-stirring apparatus connecting tube 32 , stirring apparatus 16 , stirring apparatus-to-receiving vessel tube 34 , receiving vessel 18 , downcomer tube 36 and forming body inlet 38 typically comprise platinum or a platinum rhodium alloy.
Since the glass sheets begin as vertically oriented sheets when they are removed from glass ribbon 26 , reduced handling is possible if the glass sheets can be maintained in a vertical orientation as they are transported through at least a portion of the manufacturing process downstream of the forming process. Thus, in certain manufacturing processes the glass sheet is attached to and supported from a raised conveyor after being cut from the ribbon and moved through at least a portion of the process line in a vertical orientation. In addition, it is more efficient to perform post-forming processing while the glass sheet is traveling rather than dismounting the sheet, placing the sheet in a fixture, processing the sheet, remounting the sheet and transporting it to a subsequent process. To that end, an apparatus is disclosed herein for measuring characteristics of a glass sheet after the sheet has been cut from the ribbon and as the glass sheet is moving. Measured characteristics can include cord, streak or thickness. Cord relates to a compositional inhomogeneity in the bulk glass. This composition inhomogeneity can lead to periodic nanometer-scale topography deviations. In the liquid crystal display (LCD) field, these deviations can lead to periodic cell gap variations in the display panel itself, which in turn lead to contrast streaks to which human perception is finely attuned. Streaks can cause the same distortions in LCD panels but are caused by flow distortions on the body used to form the glass sheet. In accordance with FIG. 2 , before entering apparatus 40 , the glass sheet is transported by securing the glass sheet only at the upper edge of the glass sheet so that the glass sheet hangs freely from this support.
While the preceding brief description is focused on a fusion down draw glass sheet manufacturing process, the present invention is not limited to a fusion down draw process, and could be practiced in other glass sheet manufacturing processes, such as a slot draw process.
FIGS. 2 and 3 depict an exemplary embodiment of an apparatus 40 for measuring characteristics of a glass sheet. As shown in both FIGS. 2 and 3 , apparatus 40 comprises a frame 42 supporting a circular air bearing 44 in an upright, vertical orientation. Air bearing 44 is a pressure-vacuum device designed to maintain a substrate, such as a glass sheet, at a predetermined distance, and within a maximum deviation, from the surface of the air bearing. The predetermined distance is referred to as the fly height. The fly height represents an equilibrium position of the substrate relative to the air bearing. As air is drawn from between the glass sheet and the air bearing through one or more vacuum ports, ambient air pressure forces the substrate toward the air bearing. However, as the substrate moves toward the air bearing, the force against the substrate produced by the air issuing from the porous surface(s) of the air bearing increases, until the substrate reaches a position where the forces are in equilibrium. Thus, the substrate is captured and held by the air bearing. The fly height exhibits some deviation about a given nominal fly height. As used herein, a vacuum port is any opening within a surface of air bearing 44 in fluid communication with a passage, such as a pipe, tube or other structure for the conveyance of a gas, and connected with or intended for connection to a vacuum source, such as a vacuum pump. Vacuum ports may be interconnected, such as through a common plenum disposed within air bearing 44 , through a common plenum external to air bearing 44 , or be individually supplied with a vacuum.
Air bearing 44 comprises a major surface 46 , which is the surface closest to the adjacent glass sheet to be measured, comprising channels or grooves, and vacuum ports, as will be discussed in more detail below. For the purpose of clarity, reference to angular locations on major surface 46 will be made in reference to an outer circumference of the circular air bearing, with a position of 0 degrees being located at the top-most point of the air bearing, and increasing angular position relative to a center of the circular air bearing occurs in a clockwise rotation through 360 degrees.
Referring to FIG. 2 , conveyor 48 may be used to transport a glass sheet in a direction of travel 50 along a predetermined path through apparatus 40 so that a measurement of the glass sheet may be made. For example, conveyor 48 may comprise an overhead rail equipped with a clamping mechanism 49 that travels along the rail and which also clamps to a top edge of the glass sheet to be measured. Preferably the clamping mechanism is configured to roll or slide along the rail. Moreover, conveyor 48 is preferably equipped with a drive mechanism that moves the clamping mechanism, and the glass sheet, along the rail assembly. For example, the rail assembly may be fitted with a driven chain or belt connected to the clamping mechanism, wherein a motor or other motive force is used to move the chain or belt, thereby causing the clamping mechanism, and therefore the glass sheet clamped by clamping mechanism 49 , to traverse along the rail assembly and through apparatus 40 . As used herein, the direction of travel 50 represents a forward movement of the glass sheet through apparatus 40 . In addition, the terms upstream and downstream are used relative to direction of travel 50 . That is, upstream is to be construed as a direction generally opposite to direction of travel 50 , whereas downstream is to be construed as being in a direction generally the same as direction 50 . However, it should be noted that upstream and downstream designations do not require that the direction referred to is identical, or exactly opposite the direction of travel 50 . It is only required that the direction referred to has no vector component in the opposite direction. For example, an upstream direction has no downstream vector component. Additionally, upstream and downstream may be used to refer to a stationary position with respect to the moving glass sheet. In this respect, upstream refers to a position that encounters the moving glass sheet first in respect of another stationary position. Thus, the glass sheet traveling in direction of travel 50 may pass one fixed point or object before passing a subsequent point or object. The first-passed point or object is referred to as the upstream point or object relative to the subsequent point, whereas the subsequent point or object is the downstream point or object relative to the first-passed point.
Apparatus 40 further comprises a plurality of glass sheet stabilizing air knives comprising a first stabilizing air knife 52 a positioned such that the first stabilizing air knife will be located opposite a first major surface of the glass sheet (where the first major surface of the glass sheet is the glass surface closest or adjacent to the air bearing), and a second stabilizing air knife 52 b located opposite a second major surface of the glass sheet. Put more simply, one air knife is positioned adjacent to one side of the glass sheet while the other air knife is positioned adjacent to the other or opposite side of the glass sheet. Additional glass sheet stabilizing air knives 52 a , 52 b may be positioned such that they are opposite the first or second major surface of the glass sheet as needed. For example, FIGS. 2 and 3 depict four pair of stabilizing air knives arrayed in rows and column. Apparatus 40 may comprise additional, positioning air knives positioned upstream of air bearing 44 , downstream of the air bearing and/or opposite the air bearing to assist in positioning the glass sheet relative to the air bearing, as described in more detail further below.
Apparatus 40 also comprises an edge guiding device 54 for guiding glass sheets into position for measurement. Edge guiding device 54 is located upstream of the stabilizing air knives relative to the travel direction of the glass sheet and functions to reduce or eliminate side-to-side sway of the glass sheet and to guide the glass sheet between the stabilizing air knives. In the embodiment shown in FIGS. 2 and 3 and as perhaps best shown in FIG. 4 , edge guiding device 54 comprises a pair of guide arms 56 a , 56 b configured to form guide slot 58 for receiving the lower edge of the glass sheet. Preferably guide slot 58 is wedge or V-shaped, where a distance d between the guide arms at an inlet (upstream) end of guide slot 58 (relative to glass sheet direction of travel 50 ) where a glass sheet enters the guide slot is greater than a distance d′ between guide arms 56 a , 56 b at an outlet (downstream) end of the guide slot. More simply put, the distance between the guide arms varies along a length of the guide slot and direction 50 such that the guide slot narrows as a glass sheet progresses through the guide slot, thereby forming a V-shaped slot that narrows in a direction toward air bearing 44 . Preferably, as shown in the embodiment of FIG. 4 , each guide arm may be rotatably mounted to frame 42 by axle pins or bolts that are inserted into a complimentary hole 60 in each guide arm and fasten to frame 42 . Alternatively, each guide arm may comprise a pin that is fit within a complimentary hole in frame 42 . Thus, the guide arms can be rotated to vary a shape of guide slot 58 . Means for locking the guide arms is also preferably provided, thereby allowing each guide arm to be immobilized when a suitable slot shape is implemented. For example, the guide arms may be fitted with clamps or locking screws. In some embodiments, apparatus 40 may comprise a plurality of edge guiding devices 54 . The width d of guide slot 58 should be sufficient to accommodate the largest anticipated side-to-side movement, or sway, of the glass sheet (where the glass sheet is rotating about clamping mechanism 49 ) to facilitate capture of the glass sheet. For example, if d is not sufficiently wide, a swaying glass sheet may not be captured within guide slot 58 but instead conveyed into contact with elements of apparatus 40 , thereby potentially damaging the glass sheet or the apparatus. Width d will be dependent on the parameters of a particular process configuration. As described, width d′ is smaller than width d, should be sufficiently large to prevent binding of the glass sheet as it travels through guide slot 58 , but should also be sufficiently narrow that side-to-side sway is reduced or eliminated. Width d′ is dependent, for example, on the thickness of the glass sheet and the magnitude of any curvature exhibited by the sheet. Alternatively, edge guiding device 54 may be a block of material comprising a slot machined into an upper surface of the block.
Apparatus 40 preferably also comprises an edge constraining device 62 , best seen in FIG. 5 , to hold the lower edge 63 of the glass sheet as the glass sheet is moving in the first direction 50 adjacent the air bearing. For example, edge constraining device 62 can be a plurality of guide rollers comprising one or more pairs of opposing rollers positioned along the path of the glass sheet as it traverses apparatus 40 . In accordance with the embodiment of FIG. 5 , each roller pair comprises a fixed position roller 64 and an opposing movable roller 66 . The fixed roller of a roller pair is configured to be rotatable, but not otherwise movable. That is, while fixed position roller 64 can rotate about an axis of rotation of the roller, it is not adapted to translate or swing (describe an arc). On the other hand, the opposing movable roller 66 of the roller pair is configured to be both rotatable and to be movable (e.g. translatable) such that a distance between a fixed position roller 64 and an opposing movable roller 66 can vary. Preferably, movable roller 66 is urged toward fixed position roller 64 , such as with a spring 68 . As shown by FIG. 5 , movable roller 66 is coupled to a pivot arm 70 that pivots about a pivot point 72 . Spring 68 is compressed between pivot arm 70 and spring stop 74 , whereby movable roller 66 is urged toward fixed position roller 64 . A glass sheet 28 that is inserted between fixed position roller 64 and movable roller 66 causes movable roller 66 to rotate about pivot point 72 and describe a circular arc centered about pivot point 72 . A simultaneous movement of pivot arm 70 against spring 68 further compresses spring 68 . That is, the axis of rotation of movable roller 66 itself rotates about pivot point 72 . Accordingly, movement of movable roller 66 away from fixed position roller 64 is resisted by the force exerted by spring 68 through pivot arm 70 , and movable roller 66 is urged against glass sheet 28 so that glass sheet 28 is pinched between the fixed roller and the movable roller.
To track progress of the glass sheet through apparatus 40 , at least one roller of constraining device 62 may include a rotary encoder device to sense the rotational movement of the rotating roller and convert the rotational movement to an electrical signal. FIG. 6 depicts a side view of a fixed position roller 64 comprising roller axle 76 and rotary encoder 78 coupled to the roller through roller axle 76 and drive belt 80 . Other methods of coupling rotary encoder 78 may be employed, as are known in the art. Rotary encoder 78 rotates as a ratio of the rotation of the roller and develops or modifies an electrical signal 79 . The developed or modified electrical signal 79 from rotary encoder 78 may then be conveyed to a receiving computational device (not shown), where a linear movement of the glass sheet can be calculated using the rotational data from the rotary encoder. As best shown in FIG. 6 , each fixed position roller 64 and each movable roller 66 comprises a resilient surface 82 to prevent damage resulting from contact between the roller and the glass sheet.
Referring now to FIGS. 7 and 8 , air bearing 44 comprises a porous body 84 comprising generally planar major surface 46 . As used herein porous means a rigid but sponge-like material in that it comprises millions of minute random channels through the thickness of the material resulting in a uniform distribution of holes at an external surface thereof, each hole almost insignificant by itself However, when the porous material is supplied with a gas under pressure the holes together supply a substantially uniform flow of air from a surface of the material. A suitable porous material in keeping with the present definition is graphite. Other materials, such as sintered metal powders may also be used, but the added risk of scratching the glass surface due to the hard abrasive nature of the metal argues for a softer material, such as graphite. As shown in FIG. 9 , the overall height D of porous body 84 is typically no more than one half the height H of the glass sheet 28 to be measured (where dashed line 88 represents H/2), and preferably the height of porous body 84 is no greater than one third the height of the glass sheet, or less, where the height of the glass sheet is the dimension of the glass sheet in a vertical direction when the glass sheet is hanging vertically from conveyor 48 . Moreover, as also shown in FIG. 9 , it is preferable that during operation the air bearing is positioned adjacent only the bottom portion of the glass sheet. That is, the air bearing is preferably positioned so that porous body 84 is adjacent only the lower one half or less of the glass sheet, or a portion thereof. If porous body 84 is positioned high on the glass sheet (e.g. above dashed line 88 ), the glass sheet may be subject to undue stress resulting from the constraint placed on the glass sheet by both the conveyor clamping mechanism and the constraint applied by the air bearing. The resulting stress may break the glass sheet.
Returning to FIG. 7 , porous body 84 is further divided into a first, or inner porous body portion 90 and a second, or outer porous body portion 92 disposed about the inner porous body portion. Accordingly, planar major surface 46 is divided into an inner planar surface 94 comprising inner porous body portion 90 , and an outer planar surface 96 comprising outer porous body portion 92 . Inner planar surface 94 and outer planar surface 96 may be coplanar.
Inner porous body portion 90 of air bearing 44 is annular in shape, having a circular inner circumference 98 defined at a radius r 1 from the center of the inner circumference and an outer circumference 100 defined at a radius r 2 from the center of the inner circumference. In addition, inner circumference 98 denotes the outer circumference of a passage 102 extending through air bearing 44 . In a typical embodiment, passage 102 is in a range from about 3 cm to about 8 cm in diameter. However, passage 102 may be larger or smaller, depending on need and the nature of the measurement to be taken. Measurement device 104 (see FIG. 2 ) is located such that air bearing 44 is positioned between glass sheet 28 and measurement device 104 and so that an optical axis 105 of the measurement device extends through passage 102 . Such a “through” measurement is beneficial that the plane of inspection (fixed by measurement device 104 ) and the plane of the glass are coplanar. Optical axis 105 , may, for example, coincide with the center of inner circumference 98 as shown in FIG. 7 . In other embodiments, measurement device 104 may be positioned so that glass sheet 28 is between measurement device 104 and air bearing 44 . Nevertheless, measurement device 104 should still be positioned such that optical axis 105 of measurement device is aligned to pass through passage 102 . However, in certain embodiments, passage 102 may be eliminated when the measurement is to be taken from the side of glass sheet 28 facing porous body 84 if reflection of light from porous body 84 does not affect the quality of, or otherwise interfere with, the particular measurement being performed. Optical axis 105 of measurement device 104 may be, for example, a laser beam emitted by the measurement device toward glass sheet 28 .
Referring now to FIG. 10 , inner porous body portion 90 comprises at least one circular groove 106 concentric with inner circumference 98 . Inner porous body portion 90 further comprises a plurality of grooves 108 extending radially on inner planar surface 94 and intersecting with circular groove 106 . Radial grooves 108 are preferably arranged at periodic angular positions in a spoke-like fashion. Circular groove 106 and intersecting radial grooves 108 divide inner planar surface 94 into a plurality of sub-surfaces 87 . Each sub-surface 87 comprises at least one vacuum port 110 in fluid communication with a vacuum source (not shown), as previously described.
Like inner porous body portion 90 , outer porous body portion 92 of air bearing 44 is arcuate in shape, but need not possess a circular outer circumference. For example, outer porous body portion may be elliptical or oval in shape. Outer porous body portion 92 is disposed about inner porous body portion 90 and comprises a circular inner circumference 112 defined at a radius r 3 from the center of inner porous body portion 90 described above. In embodiments wherein outer porous body portion 92 comprises a circular outer circumference, i.e. circumference 114 shown in FIG. 7 , outer circumference 114 is defined at a radius r 4 from the center of inner circumference 98 . In some embodiments, r 2 =r 3 and therefore inner circumference 112 of outer porous body portion 92 is the same as the outer circumference 100 of inner porous body portion 90 .
Still in regard to FIG. 10 , outer porous body portion 92 further comprises a plurality of continuous grooves 116 formed in outer planar surface 96 . Each continuous groove 116 comprises a plurality of vacuum ports 118 extending through the porous body and connected to a vacuum source. Preferably, the plurality of vacuum ports 118 are arrayed periodically within each continuous groove 116 so that the angular displacement between vacuum ports disposed in a given continuous groove is equal. For example, within a given continuous groove 116 , a vacuum port 118 may be positioned every 5 degrees, every 10 degrees or every 15 degrees around the groove. It is not necessary that the vacuum ports of one continuous groove 116 coincide angularly with the vacuum ports of another continuous groove 116 . In some cases, particularly when the outer circumference of outer porous body portion 92 is circular, continuous grooves 116 are preferably circular and concentric.
In some embodiments, such as that depicted in FIG. 11 , air bearing 44 may comprise a plurality of inner porous body portions 90 positioned within outer porous body portion 92 , each inner porous body portion defining a passage 102 . This can be particularly helpful when multiple measurements, for simultaneously determining multiple characteristics of the glass sheet, are to be taken and cannot be incorporated into a single measurement device.
The organization of grooves and vacuum ports can be better seen with the aid of FIGS. 12A and 12B , where FIG. 12A depicts a cross sectional view of a portion of inner porous body portion 90 , and FIG. 12B depicts a cross sectional view of a portion of outer porous body portion 92 . Both inner porous body portion 90 and outer porous body portion 92 are supplied with a pressurized gas, such as air, that issues from the planar surface of each porous body portion as represented by arrows 117 . Together, the vacuum produced at the vacuum ports, depicted by arrows 119 , and the air pressure produced over the planar surfaces of the porous body portions define two zones: a low precision capture zone adjacent outer planar surface 96 and a high precision capture zone coincident with inner planar surface 94 . In the low precision capture zone the fly height of the glass sheet may be greater than the fly height of the glass sheet adjacent the high precision capture zone. A fly height of the glass sheet adjacent the low pressure capture zone can typically by in the range from about 40 μm to 60 μm, whereas the fly height of the glass sheet adjacent the high precision zone can typically be less than 40 μm.
As previously described, and in accordance with the embodiment of FIGS. 2 and 3 , apparatus 40 comprises a plurality of stabilizing air knives 52 a , 52 b positioned upstream of air bearing 44 relative to the direction of travel 50 of glass sheet 28 through apparatus 40 . The plurality of stabilizing air knives comprises a first stabilizing air knife 52 a positioned such that the first stabilizing air knife will be located opposite first major surface 121 of glass sheet 28 (See FIG. 18 ), and a second stabilizing air knife 52 b positioned such that the second stabilizing air knife will be located opposite second major surface 123 of glass sheet 28 . First major surface 121 of glass sheet 28 is the surface of the glass sheet closest to porous body 84 when the glass sheet is adjacent to the air bearing, whereas second major surface 123 is the surface of glass sheet 28 farthest from porous body 84 under the same condition. The flow of air from the at least first and second stabilizing air knives of the plurality of stabilizing air knives stabilizes lateral (side-to-side) motion of the glass sheet in conjunction with the at least one edge guiding device 54 as the glass sheet enters the space between the stabilizing air knives, and helps to flatten the sheet. More simply put, even though the glass sheet may be impeded from lateral movement at the upper and lower edges of the glass sheet by conveyor clamping mechanism 49 at the upper edge of the glass sheet and edge guiding device 54 at the lower edge of the glass sheet, the glass sheet may still deform in a direction perpendicular to the general plane of the glass sheet, much the way a cloth sail can billow in the wind. This is because the glass sheet can be very large, and very thin, giving the glass sheet an increased flexibility when compared to much thicker glass plates. For example, a thickness of the glass sheet can be less than 1 mm.
Each stabilizing air knife is oriented such that the flow of air from each stabilizing air knife is directed toward the glass sheet in a downward direction, generally toward the bottom of the glass sheet, to create a more laminar flow of air over the major surfaces of the glass sheet and prevent turbulence and subsequent buffeting of the glass sheet. Preferably, although not necessarily, first and second stabilizing air knives 52 a , 52 b are arranged to mirror each other across the glass sheet. For example, in some embodiments, such as the embodiment of FIGS. 2 and 3 , the plurality of stabilizing air knives are preferably arranged as multiple pairs of partially or substantially opposing air knives. That is, while the air knives may be directly opposing each other, this is not necessary, and there may be some offset between such “pairs” of air knives. However, in some embodiments the offset may be substantial. The number of stabilizing air knives is process dependent, and will depend, for example, on the transport speed of the glass sheet, the size and weight of the glass sheet and the amount of side-to-side sway exhibited by a glass sheet in a particular manufacturing process line. Similarly, the exact placement of an air knife on one side of the glass sheet compared to the placement of another air knife on the other side of the glass sheet will depend on the particular process conditions of the installation.
FIG. 13 illustrates an exemplary stabilizing air knife (here designated generally by reference numeral 120 ) comprising a generally elongate body 122 having an elongate orifice 124 from which a flow 126 of air issues. For simplicity, the air knife is represented by a longitudinally extended rectangular block. Each elongate orifice 124 is in fluid communication with a source of pressurized gas that enters the air knife through a coupling. The air knife may include an interior plenum in fluid communication with orifice 124 . As air is quite satisfactory as a gas, being both plentiful and essentially free, the remaining description will assume an air-based air knife. Each elongate body 122 is arranged such that a direction of flow of the air emitted from each elongate orifice 124 is at a downward angle relative to a reference horizontal plane. Each stabilizing air knife, as represented by exemplary stabilizing air knife 120 , includes a forward or leading end L and a rearward or trailing end TR relative to the direction of travel 50 of the glass sheet. That is, the leading end of the air knife is farther upstream than the trailing end of the air knife. When the air knife is supplied with pressurized air, the air issues from elongate orifice 124 at a high velocity. While the air issuing from the elongate orifice 124 may eventually begin to diverge after leaving the stabilizing air knife, for at least a short distance, on the order of several 10s of millimeters, the air issues from the air knife as a substantially laminar flow 126 that can be approximated by a plane. Exemplary stabilizing air knife 120 further comprises a top surface T.
In the event that the stabilizing air knives are arranged in a complimentary opposing relationship (i.e. are mirrored across an intervening vertical plane between the stabilizing air knives that is parallel with air bearing major surface 46 ), a distance between the leading ends of an opposing stabilizing air knife pair may be greater than a distance between the trailing ends of the opposing stabilizing air knife pair. That is, the distance between the opposing air knives narrows as the glass sheet progresses between the air knives in a manner similar to the narrowing of guide slot 58 .
In still another optional characteristic, each stabilizing air knife of the plurality of stabilizing air knives may be oriented such that the trailing end of each stabilizing air knife is higher (or lower) than the leading end of the stabilizing air knife. In some embodiments each stabilizing air knife can be straight (i.e. rectangular shaped) similar to exemplary air knife 120 . However, preferably each stabilizing air knife is arcuate and may comprises a circular arc. Suitable stabilizing air knives of either the straight (linear) variety, or the arcuate design, can be obtained, for example, through Exair Corporation located in Cincinnati, Ohio, USA.
How each stabilizing air knife may be spatially oriented can be visualized in more detail with the following description and aid of FIGS. 14-16 . The orientation of a body in three-dimensional space requires a frame of reference, and a means of orienting the body in that frame of reference. FIG. 14 shows a vertical X-Y plane coplanar with major surface 46 of porous body 84 . For the purpose of further discussion, this X-Y plane forms one plane in a three-dimensional Cartesian coordinate reference frame. This X-Y plane lies within the plane of the page on which FIG. 14 is depicted. A second vertical plane, seen from an edge thereof in FIG. 14 , forms a Y-Z plane of the Cartesian coordinate system where the Z direction extends perpendicular to and therefore out of the page. The Y-Z plane is perpendicular to the X-Y plane. A third, X-Z plane, also seen from an edge thereof in FIG. 14 , is arranged to be perpendicular to both the X-Y and Y-Z planes. For the purpose of further discussion, and unless otherwise described, the origin of the Cartesian coordinate system formed by the three planes X-Y, Y-Z and X-Z described above lies at the center of inner porous body portion 90 , and this Cartesian coordinate system will be used to describe the orientation of the air knives in three dimensional space.
FIGS. 14-16 depict the three optional orientations of exemplary stabilizing air knife 120 , and by extension therefore the optional spatial orientations of each stabilizing air knife, shown separately to aid in visualizing the orientations. FIG. 14 depicts an outline of air bearing 44 as seen looking at major surface 46 and indicating the direction of travel 50 of the glass sheet. Exemplary stabilizing air knife 120 exhibits a downward pitch or incline in that the leading end L of the stabilizing air knife is lower than the trailing end TR of the stabilizing air knife relative to the horizontal X-Z plane. To wit, plane 128 representing the flow of air from the exemplary stabilizing air knife makes an angle α with the X-Z plane.
FIG. 15 shows a second view looking down on an edge of air bearing 44 and shows an edge of the Y-Z plane and an edge of the X-Y plane. The X-Z plane is perpendicular to both the X-Y plane and the Y-Z plane. Plane 130 is a plane longitudinally bisecting top surface T of exemplary stabilizing air knife 120 and is perpendicular to plane 126 representing the flow of air from the air knife. In accordance with FIG. 15 , exemplary stabilizing air knife 120 may be angled relative to the vertical X-Y plane such that a non-zero angle β is formed between plane 130 and the X-Y plane.
FIG. 16 shows a third view looking down on an edge of air bearing 44 and shows an edge of the X-Z plane and an edge of the X-Y plane. The Y-Z plane is perpendicular to both the X-Y plane and the X-Z plane. FIG. 16 illustrates exemplary stabilizing air knife 120 from an end thereof oriented such that the flow of air exiting the air knife is directed downward (from a reference horizontal flow, e.g. parallel with the horizontal X-Z plane) and the plane of the air flow makes an acute angle δ with the X-Y plane rather than being directed, for example, perpendicular to the glass sheet. Preferably, δ is in the range from about 15 degrees to about 75 degrees, preferably in the range from about 25 degrees to about 65 degrees, and more preferably in the range from about 35 degrees to about 55 degrees. In one embodiment, the angle of the air flow is about 45 degrees relative to the vertical X-Y plane. It should be noted that the preferred direction for the air flow is downward, since a low positioning of the air bearing relative to the glass sheet gives the lower portion of the glass sheet more stiffness to resist buckling of the glass sheet due to the air flow. However, in some embodiments, an upward air flow may be preferred depending on process conditions and the particular implementation, e.g. positioning, of the air bearing.
The preceding description presented three optional orientations of an exemplary stabilizing air knife 120 . Each stabilizing air knife of the plurality of stabilizing air knives may exhibit at least one orientation of the three optional orientations described above in respect of a representative exemplary stabilizing air knife. For example, each stabilizing air knife of the plurality of stabilizing air knives may exhaust air such that the direction of air flow from the air knives is generally downward (i.e. the flow vector comprises a vertical vector component). Thus, for example, two stabilizing air knives located on opposite sides of the glass sheet and wherein the stabilizing air knives are mirror images of each other, will form a generally V-shaped flow of air, with the “V” pointed downward.
Similarly, each stabilizing air knife of the plurality of stabilizing air knives may be oriented such that a leading end of each stabilizing air knife is farther from the glass sheet than a trailing end. Thus, for example, two stabilizing air knives located on opposite sides of the glass sheet and wherein the stabilizing air knives are mirror images of each other, will form a generally V-shaped flow of air, with the “V” pointed downstream toward the air bearing. This provides more lateral clearance for a glass sheet exhibiting lateral movement as it enters between the air knives. It also provides for a more gradual application of the curtain of air flowing from the stabilizing air knives, as the pressure on the glass sheet from the flow of air from the leading end of each stabilizing air knife becomes less than the pressure of the air on the glass sheet adjacent the trailing end of a stabilizing air knife.
Similarly, each stabilizing air knife of the plurality of stabilizing air knives may be oriented such that a leading end of each stabilizing air knife is lower relative to a horizontal reference plane (for example, the X-Z plane) than a trailing end. It can be said that the stabilizing air knives are pitched or inclined forward to flatten out any shape distortion (e.g. bow) in the sheet.
Each stabilizing air knife of the plurality of air knives may exhibit one or more of the orientations described above. In some embodiments, one or more of the stabilizing air knives may simultaneously exhibit all three orientations.
In addition to the stabilizing air knives and as seen in FIG. 3 , for example, a first positioning air knife 132 may be placed between the stabilizing air knives ( 52 a , 52 b ) and air bearing 44 such that the flow 126 of air from the first positioning air knife impinges on first major surface 121 of the glass sheet adjacent to the leading edge of the air bearing. For example, first positioning air knife 132 may be located at an approximately 270 degree position on air bearing 44 . The pressure produced on the glass sheet as it passes adjacent to first positioning air knife 132 forces the glass sheet away from the air bearing. This prevents contact between the leading or forward edge of the glass sheet as it approaches the air bearing until the glass sheet can be “captured” by the air bearing.
A second positioning air knife 134 may be positioned such that air from the second positioning air knife impinges on second major surface 123 of the glass sheet. The effect of the air from the second positioning air knife is to force the glass sheet in a direction toward the air bearing, thus bringing the glass sheet closer to the air bearing and allowing the air bearing to capture the glass sheet. Initial capture of the glass sheet is accomplished by the combination of pressure and vacuum produced by the outer porous body portion.
A third positioning air knife 136 may be positioned downstream from the air bearing and positioned such that air emitted by the third positioning air knife is directed against first major surface 121 of the glass sheet. The air pressure produced by third positioning air knife 136 forces the glass sheet away from the air bearing surface near the downstream edge of the air bearing and thereby prevents contact between the glass sheet and the air bearing as the glass sheet moves past and disengages from the air bearing. Each positioning air knife 132 , 134 and 136 may be similar in design to a stabilizing air knife. For example, each stabilizing air knife and each positioning air knife may be of the arcuate design or of the linear design. Preferably, the air emitted from each of the positioning air knives 132 , 134 and 136 is directed against the glass sheet such that the curtain of gas from each positioning air knife forms an angle less than 90 degrees but greater than zero with the surface of the glass sheet, for example, greater than 25 degrees and less than 75 degrees, and preferably greater than 35 degrees and less than 65 degrees, preferably greater than 35 degrees and less than 55 degrees. For example, a typical embodiment may orient each positioning air knife so that the flow of air impinges on the glass sheet at an angle of about 45 degrees. An angle of impingement less than 90 degrees produces less turbulence at the surface of the glass sheet than, for example, air flow that is perpendicular to the glass sheet.
The overall effect of the various non-contact glass sheet handling components of apparatus 40 is to provide gradually increasing constraint on the glass sheet to prepare the glass sheet for measurement. As previously noted, in some instances the glass sheet is conveyed vertically, secured only at the top of the glass sheet by the conveyor clamp. As the glass sheet may be very thin, equal to or less than 1 mm, and in some cases equal to or less than 0.7 mm, or in other cases equal to or less than 0.3 mm, the glass may easily exhibit lateral movement by swaying side-to-side (i.e. rotate about the fixed carrier contact points), or deform by various bending modes (as used herein, a bending mode is analogous to a vibrational mode). The glass can also be offset due to carrier-to-carrier variations in the clamping and the position of the carrier on the conveyor. As well, the glass can be bowed vertically.
Various glass sheet handling components of apparatus 40 serve to reduce or eliminate these motions, and fixed shapes, such as bow. Accordingly, operation of apparatus 40 may proceed along the following steps.
A glass sheet 28 is attached to conveyor 48 by one or more clamping mechanisms 49 that grip the glass sheet along a top edge of the glass sheet translate the glass sheet through apparatus 40 . Glass sheet 28 is thereby hanging from the one or more clamping mechanisms, and supported only by the one or more clamping mechanisms clamped to the glass sheet along a top portion of the glass sheet. The lower edge 63 of the glass sheet is unsupported and initially capable of lateral movement, i.e. a swaying movement, before entering apparatus 40 . In addition to lateral movement, the glass sheet may also exhibit flexure or bending. For example, the sheet may bend cylindrically or hyperbolically or be saddle shaped, dome shaped, or exhibit other bending modes, or combinations thereof.
As glass sheet 28 nears apparatus 40 , the glass sheet is guided by at least one edge guiding device 54 that engages with lower edge 63 of the glass sheet and guides the leading edge of the glass sheet between stabilizing air knives 52 a , 52 b . Lower edge 63 forms part of the “non-quality” portion of the glass sheet and may later be removed. The at least one edge guiding device 54 minimizes or eliminates side-to-side swaying. Testing has shown embodiments of edge guiding device 54 as disclosed herein can reduce the lateral motion of swaying from a maximum displacement of +/−75 mm to less than +/−10 mm. However, while the at least one edge guiding device 54 may provide excellent control of lateral movement of the lower edge of the glass sheet, the glass sheet is only substantially constrained at the top and bottom edges, and is still capable of exhibiting various bending modes and fixed shapes within the body of the glass sheet. To minimize or eliminate this additional movement or shape of the glass sheet before moving adjacent to porous body 84 , stabilizing air knives are employed.
The flow of air emitted by opposing stabilizing air knives, preferably in a downward direction, may further reduce lateral movement of the glass sheet to eliminate side-to-side swaying of the glass sheet, and in particular, reduces or eliminates bending modes. In effect, the stabilizing air knives help stiffen the glass sheet by at least reducing the magnitude of the bending and in some cases by eliminating one or more bending modes. The number and positioning of the stabilizing air knives is dependent on such factors as the size of the glass sheet, the thickness of the glass sheet, the density of the glass, and the traverse speed of the glass sheet through apparatus 40 .
As the glass sheet passes between the stabilizing air knives, lower edge 63 of the glass sheet may be guided by one or more additional edge guiding devices 54 to further guide and stabilize the glass sheet. For example, in some embodiments, multiple edge guiding devices may be employed; with a first edge guiding device employed upstream of the stabilizing air knives and a second edge guiding device positioned just prior to the edge constraining device 62 .
As the glass sheet approaches air bearing 44 , optional first positioning air knife 132 may be used to direct a flow of air at first major surface 121 of the glass sheet. The force of the air from first positioning air knife 132 against first major surface 121 of glass sheet 28 pushes the glass sheet away from the leading edge 140 (see FIG. 17 , and more particularly region A of FIG. 18 ) of air bearing 44 and prevents contact between leading edge 140 of the air bearing and leading edge 141 of glass sheet 28 as the glass sheet comes under the influence of outer porous body portion 92 of air bearing 44 . Contact between the glass sheet and the air bearing may result in damage, in some instances catastrophic, to the glass sheet.
As the glass sheet continues to move forward along direction of travel 50 , the glass sheet passes over a first vacuum port 118 of outer porous body portion 92 . Preferably, air bearing 44 is positioned such that a vacuum port 118 positioned within the outer-most groove of outer porous body portion 92 is positioned so that as the glass sheet advances, it first moves adjacent to this single vacuum port 118 . Referring to FIG. 10 , this first vacuum port 118 is the vacuum port farthest to the left and lying in the outermost continuous groove 116 in FIG. 8 , and intersecting with dashed line 119 . The effect of this initial encounter with a first vacuum port 118 is that leading edge 141 of glass sheet 28 is moved closer to outer porous body portion 92 . That is, while the region of the glass sheet adjacent leading edge 141 of the air bearing is being pushed away from the air bearing leading edge, a region of the glass sheet adjacent the first vacuum port 118 is forced in the direction of outer porous body portion 92 . By bringing at least this portion of the glass sheet adjacent the first vacuum port 118 close to the air bearing, that portion of the glass sheet is captured by the outer porous body portion 92 of air bearing 44 . Continued forward movement of the glass sheet brings the glass sheet adjacent to additional vacuum ports 118 of outer porous body portion 92 . Within a short distance of the leading edge of glass sheet 28 passing adjacent to the additional outer porous body portion vacuum ports 118 , sufficient force is exerted on the glass sheet as a result of air flow at the outer porous body portion that a substantial portion of the glass sheet adjacent to air bearing 44 exhibits a substantially uniform fly height relative to the first major surface of the air bearing.
Again, as the glass sheet continues to move forward adjacent to inner porous body portion 90 , the flatness and rigidity of the glass sheet increases, particularly those portions of glass sheet 28 directly adjacent to inner porous body portion 90 , such that measurements may be taken by measurement device 104 through passage 102 .
It should be recalled that measurements of the glass sheet, such as interferometric measurements for the purpose of determining surface topography of glass sheet 28 , may be taken simultaneously with the forward movement of the glass sheet (i.e. in direction 50 ). As the glass sheet trailing edge passes inner porous body portion 90 , and then outer porous body portion 92 , the constraint to the glass sheet applied by the action of the air bearing 44 decreases, and the air pressure from optional positioning air knife 136 is able to overcome the holding force applied by air bearing 44 such that the trailing edge of the glass sheet is pushed away from the air bearing so that contact between the glass sheet and the air bearing does not occur. The pressurized air supplied to inner porous body portion 90 , and the vacuum, may be adjusted, for example, such that the fly height of the glass sheet is maintained to have a deviation less than about 30 μm (+/−15 μm).
From the preceding it can be seen that a region of the glass sheet is opposite passage 102 as the glass sheet moves past air bearing 44 . Thus, passage 102 , while defining a circular measurement zone, “sweeps” a rectangular measurement region 138 of the glass sheet as shown in FIG. 9 . Measurement device 104 makes continuous measurements of the glass within this rectangular region. For example, measurement device 104 may be an interferometer for making surface topography measurements of the glass sheet within the rectangular measurement zone, or measurement device 104 may make measurement of the thickness of the glass sheet.
Eventually, continued forward travel of the glass sheet along direction of travel 50 brings the trailing edge 142 of the glass sheet past air bearing 44 . Air issuing from third positioning air knife 136 and impinging on first major surface 121 of the glass sheet forces the region of the glass sheet proximate the trailing edge 142 of air bearing 44 away from the air bearing, thereby avoiding contact between the glass sheet and the air bearing surface. This becomes particularly beneficial as the surface area of the glass sheet under the influence of the stabilizing air knives and/or the air bearing decreases.
The result of the forces supplied by positioning air knives 132 , 134 and 136 can be seen with the aid of FIG. 18 , showing apparatus 40 in a top view and depicting glass sheet 28 . The effect of positioning air knives 132 and 136 can be seen in the regions designated by reference numerals A and B and circled by dashed lines. Indeed, it can be seen from FIG. 18 that the glass sheet overall takes on a non-planar aspect until the glass sheet is fully engaged by the air bearing, at which point the glass sheet adjacent to the air bearing is fully flat, although it should be noted that the only region where planarity is needed is where a measurement is occurring, e.g. in the center of the measurement zone.
FIG. 19 depicts an edge view of the glass sheet extending from the center of the inner porous body portion to the leading edge of the air bearing and shows in more detail the shape of the glass sheet over the air bearing. It should be kept in mind that the illustration of FIG. 19 is greatly exaggerated, as the deflections involved are on the order of tens of microns. As shown, the glass sheet can be divided into several distinct regions separated by equally distinct boundaries, giving the portion of the glass sheet over the air bearing the appearance of a series of relatively flat plateaus 144 separated by S-shaped boundary features 145 , wherein the fly height of the plateaus decrease in a direction toward the center of the inner porous body portion (e.g. the area defined by passage 102 ).
FIG. 20 is a graph of measured fly heights for a glass sheet traveling through an embodiment of apparatus 40 with a travel speed of 100 mm/s measured at two different locations for a glass sheet. The vertical “Y” axis represents fly height in microns while the horizontal “X” axis represents time. The measurements were taken at a predetermined frequency (250 sec −1 ) for a given location. Thus, the graph of FIG. 20 can be used to obtain the fly height at a predetermined position over time as the glass sheet traverses adjacent to the air bearing. The glass sheet had an initial side-to-side sway of +/−75 mm from a nominal centerline position. Each stabilizing air knife directed air against the glass sheet at a downward angle of 45 degrees. The inner porous body portion of the air bearing was supplied with air at a pressure of 20 psi to 60 psi at a flow rate of 0.63+/−0.25 CFM, while the outer porous body portion was supplied with air at a pressure of 40 to 85 psi and a flow rate of 0.96+/−0.35 CFM. The fly height of the glass sheet over the circular measurement zone defined by passage 102 was nominally 28 μm with a variation of less than +/−2.5 μm. Curve 146 of FIG. 20 shows the fly height of the glass sheet at the outer circumference of inner porous body member 90 at a position of approximately 210 degrees, with the glass sheet traveling at a speed of 100 mm/s, while curve 148 of FIG. 20 depicts the fly height at the center of the inner porous body portion (i.e. the center of passage 102 ). The curves for travel of the glass sheet are particularly telling for showing the stability of the fly height at both locations of the glass sheet—the measurement location at the outer circumference of the outer porous body portion and the measurement location over the center of the porous body. While the nominal fly height differs between the two regions, being significantly greater for the outer porous body location than for the center of the porous body, the fly height at both locations is surprisingly stable, showing a variation less than about ±2.5 microns.
It will be apparent to those skilled in the art that various modifications and variations can be made to the present invention without departing from the spirit and scope of the invention. Thus it is intended that the present invention cover the modifications and variations of this invention provided they come within the scope of the appended claims and their equivalents. | Disclosed is an apparatus for characterizing attributes of a moving glass sheet comprising complementary mechanical material handling technologies that progressively stabilize, position, capture, flatten, and release the lower portion of glass sheets traveling past the apparatus while posing minimal constraint on the top section of the sheet. The apparatus includes a pressure-vacuum (PV)-type device comprising distinct regions such that the glass sheets experience a non-contact but gradual increase in constraining force until the point where measurements can be performed, then a gradual decrease in constraining force until the glass sheets are released from the inspection station. This graduated force technique is applied along the direction of travel of the sheets and may also be applied vertically upwards along the height of the sheet to restrict the motion of the sheet without constraining it at pinch points near the conveyor. | 2 |
RELATED APPLICATION
[0001] This application is a divisional of U.S. patent application Ser. No. 10/774,971, filed Feb. 9, 2004, issued as U.S. Pat. No. 7,267,268 on Aug. 14, 2007, which claims priority of nonprovisional application No. 60/451,083, filed Feb. 28, 2003, all hereby incorporated in their entirety by reference.
BACKGROUND
[0002] 1. Field of the Invention
[0003] The present invention generally relates to automated inspection of digitized microscope slides and more particularly relates to pattern recognition techniques employed in automated inspection of virtual slides.
[0004] 2. Related Art
[0005] An obstacle to automating microscopic inspection has been the inability to efficiently digitize entire microscope specimens at diagnostic resolutions. Conventional approaches for creating virtual slides have relied on image tiling. Image tiling involves the capture of multiple, small regions of a microscope slide using a traditional charge coupled device (“CCD”) camera. These tiles are typically “stitched” together (aligned) to create a large contiguous digital image (mosaic) of an entire slide. A minimum of 2,250 individual camera tiles are required to digitize a typical 15 mm×15 mm area of a slide at 50,000 pixels/inch (0.5 μm/pixel).
[0006] Image tiling carries several disadvantages. First, images frequently have distortion because image tiles are limited to a single focal plane from the camera's fixed area objective lens. Second, an image tiling system produces optical aberrations that are circularly symmetric about the center of the image tile. Third, full pixel resolution is usually unavailable because color CCD cameras lose spatial resolution upon interpolation of color values from non-adjacent pixels.
[0007] Conventional approaches to pattern recognition are also cumbersome. Despite many years of improvements in optical microscopy, in most cases a human operator is still required to manually evaluate a specimen through the eyepieces of a dedicated instrument. Worldwide, in thousands of clinical laboratories, more time is spent performing manual microscopy than any other in-vitro diagnostics testing procedure. In an estimated 20,000 research laboratories, manual microscopic inspection is an essential tool for screening drug targets and for conducting toxicology studies. While offering immense opportunities for automation, microscopic inspection remains a bastion of manual labor in an environment that is otherwise converting to automated solutions.
[0008] Some attempts at computer aided pattern recognition have been made. These approaches to pattern recognition in microscopic images are based on morphological features. A large number of feature metrics (e.g., cell size, nuclear-to-cytoplasmic ratio, roundness, density, color, texture, etc.) are computed to identify “objects” (e.g., cells) that appear in the image. Pattern recognition is achieved by correlating the feature metrics for an unknown object with those of a known object. Feature based approaches have had some success in cytology, where a high level of cell diversity is required to allow objects to be identified. These conventional approaches, however, are immensely complicated or completely untenable for histology imagery data where reliable object segmentation is difficult.
SUMMARY
[0009] Systems and methods for image pattern recognition comprise digital image capture and encoding using vector quantization (“VQ”) of the image. A vocabulary of vectors is built by segmenting images into kernels and creating vectors corresponding to each kernel. Images are encoded by creating vector index files with indices (“pointers”) to the vectors stored in the vocabulary. The vector index files can be used to reconstruct the images by looking up vectors stored in the vocabulary. Pattern recognition of candidate regions of images can be accomplished by correlating image vectors to a pre-trained vocabulary of vector sets comprising vectors that correlate with particular image characteristics. In virtual microscopy, the systems and methods are suitable for rare-event finding, such as detection of micrometastasis clusters, tissue identification, such as locating regions of analysis for immunohistochemical assays, and rapid screening of tissue samples, such as histology sections arranged as tissue microarrays (TMAs).
BRIEF DESCRIPTION OF THE DRAWINGS
[0010] The details of the present invention, both as to its structure and operation, may be gleaned in part by study of the accompanying drawings, in which like reference numerals refer to like parts, and in which:
[0011] FIG. 1 is a block diagram illustrating an example process for encoding and decoding an image using vector quantization according to an embodiment of the present invention;
[0012] FIG. 2 is a flow diagram illustrating an example method for image pattern recognition according to an embodiment of the present invention;
[0013] FIG. 3 is a block diagram illustrating an example client/server implementation according to an embodiment of the present invention;
[0014] FIG. 4 is a block diagram illustrating an example nested kernel logic according to an embodiment of the present invention;
[0015] FIG. 5 is a flow diagram illustrating an example process for creating variable sized kernels according to an embodiment of the present invention;
[0016] FIG. 6 is a table diagram summarizing a representative sample of slides used for a study according to an embodiment of the present invention;
[0017] FIG. 7 is a table diagram summarizing the results of a plurality of slides from a study according to an embodiment of the present invention;
[0018] FIG. 8 is a graph diagram illustrating an example change in vocabulary size as slides were processed during a study according to an embodiment of the present invention;
[0019] FIG. 9 is a graph diagram illustrating an example change in index size as slides were processed during a study according to an embodiment of the present invention; and
[0020] FIG. 10 is a block diagram illustrating an exemplary computer system as may be used in connection with various embodiments described herein.
DETAILED DESCRIPTION
[0021] Certain embodiments as disclosed herein provide for pattern recognition systems and methods. For example, one method as disclosed herein allows for a digitized image to be segmented into a plurality of image kernels. The image kernels are then analyzed to determine the intensity of each pixel in the kernel. The pixel intensities for an image kernel are then combined into a vector and the vector is stored in a data structure with other vectors for the image. Each vector is indexed to create a composite index for the digitized image that can later be reconstructed using the indices and the vectors.
[0022] After reading this description it will become apparent to one skilled in the art how to implement the invention in various alternative embodiments and alternative applications. However, although various embodiments of the present invention will be described herein, it is understood that these embodiments are presented by way of example only, and not limitation. As such, this detailed description of various alternative embodiments should not be construed to limit the scope or breadth of the present invention as set forth in the appended claims.
[0023] A first step in automating microscopic inspection is to create a virtual slide, i.e., a high resolution digital image of an entire slide. The systems and methods of the present invention overcome many of the disadvantages of the existing image pattern recognition techniques by employing a technique known as vector quantization (“VQ”). VQ is a computational technique for encoding bitstreams using a vocabulary. VQ is particularly suitable for encoding images that have significant redundancy.
[0024] VQ is a useful approach for pattern recognition in imagery data that is repetitive in nature. Fundamentally, pattern recognition using VQ is based on comparing previously encoded patterns (i.e., particular characteristics) with new imagery data. The computational challenges of organizing and retrieving significant volumes of imagery data are immense and prior to the present invention have prevented the application of VQ to pattern recognition in large images. The implementation of VQ in accordance with the systems and methods described herein overcomes these computational challenges and makes pattern recognition in virtual microscopic images feasible.
[0025] The systems and methods for VQ-based image pattern recognition of the present invention represent a significant improvement over the prior art for several reasons: First, VQ-based pattern recognition is efficient because encoding of image information is performed once, after which pattern matching can be performed solely by correlating VQ vector information, rather than comparison of image information. Second, VQ encodes all image characteristics without need for predetermined heuristics that identify significant features. Pattern matching can be morphometric, calorimetric, context-dependent, etc., depending upon the training used to create vectors of interest. Finally, VQ pattern recognition learns automatically as it is used. Statistical methods determine the significance of vectors that are characteristic for particular patterns.
[0026] FIG. 1 illustrates a process 100 for encoding an image using VQ. Process 100 begins after digital image 105 is analyzed and segmented into small rectangular regions called image kernels 108 . Image 105 can be, for example, a liver sample comprising one or more image characteristics. An image characteristic is any user-defined attribute that may be exhibited by a region of an image, such as a cluster of tumor cells or region of analysis (“ROA”) within a tissue microarray (“TMA”) spot. Kernels can vary in size from 1 to 64 pixels per side, or 1 to 4096 total pixels per kernel. Larger kernel sizes may also be employed as will be understood by those skilled in the art.
[0027] Next, a vector 112 corresponding to each kernel 108 is generated and stored in vocabulary 110 . Vocabulary 110 is a data structure comprising the vectors 112 corresponding to kernels 108 . The data structure may be a database, a file, a linked list, or some other collection of vectors 112 . A vector 112 is a one-dimensional array of scalars. In vector quantization, each vector represents the pixel intensities of all pixels in a kernel, for each of three color channels. For example, a kernel comprising 15 pixels by 15 pixels corresponds to a vector with 225*3=675 intensity values.
[0028] Vector index file 120 is a collection of indices 116 that correspond (i.e., “point”) to the vectors 112 that comprise image 105 . Each vector 112 in vocabulary 110 is assigned a unique index 116 . In one embodiment, an index 116 is a unique 4-byte integer. Once an image is completely segmented into a plurality of kernels 108 , corresponding vectors 112 are generated for each kernel 108 and the vectors 112 are indexed. At this point, the image is said to be vector quantized, or VQ-encoded. After image 105 has been VQ-encoded, it is completely represented by a series of indices 116 in vector index file 120 (together with the contents of the vocabulary 110 ).
[0029] Image 105 can be reconstructed (i.e., VQ-decoded) using the indices 116 to lookup each vector 112 in vocabulary 110 . Decoding uses the vectors 112 to recreate the corresponding kernels 108 necessary to render image 105 .
[0030] Capitalizing on redundant kernels is a significant component of VQ-encoding. During the VQ-encoding process, each newly identified kernel 108 is compared to the vectors 112 already stored in the vocabulary. If a sufficiently close match is found with a vector 112 already in vocabulary 110 , then the vector 112 for that newly identified kernel is re-used. If, however, a sufficiently close match is not found with a vector 112 already in vocabulary 110 , then the vector 112 for that newly identified kernel is appended to vocabulary 110 . As a result, over time vocabulary 110 is populated with nearly all kernels 108 which are found in the imagery data for a particular image type, e.g., samples of liver tissue. Thus, as slides of a given tissue type are encoded, more and more of the kernels 108 which appear in such slides are stored in the vocabulary 110 , and correspondingly fewer new vectors 112 need be added. In one embodiment, a mature vocabulary 110 may VQ-encode an image 105 without adding any new vectors 112 to the vocabulary 110 .
[0031] Searching vocabulary 110 for pre-existing vectors to reuse is computationally expensive. The systems and methods of the present invention achieve, by several orders of magnitude, a reduction in processing time and memory usage. One technique for accomplishing this improved processing efficiency includes the computation of a correlation between a vector and its corresponding image characteristic, as described in the next figure.
[0032] FIG. 2 is a flow diagram illustrating a method for image pattern recognition according to an embodiment of the invention. The image pattern recognition process can be divided into a training stage 201 and a pattern recognition stage 202 . In the first step 205 of the training stage 201 , a human expert identifies a region of an image as characteristic of an attribute. For example, an expert in the biological sciences might examine a tissue sample and visibly identify a group of tumor cells or ROAs within a TMA. Typically the attribute is recognized by the expert without regard to the specific visual characteristics which comprise the attribute, e.g. morphometric, colorimetric, and/or context-dependent features of the image.
[0033] In step 210 , a vector set is created to store each vector index that corresponds to a vector found in the image characteristic. Multiple vector sets can be created for different characteristics. For example, different vector sets can be created for different tumor types identified by experts in step 205 . For instance, one vector set might be developed for melanoma and another for leukemia.
[0034] In step 215 , the correlation of each vector to the image characteristic is computed. In one embodiment, the correlation is computed using the following ratio:
Number of times the vector is observed in the region exhibiting the characteristic Number of times the vector is observed overall
[0035] The correlation of each vector to the image characteristic is stored in the vector set along with the corresponding vector index in step 220 . Vector sets contain vector indices together with their associated correlation to the previously identified image characteristic. In step 225 , the training stage is repeated for the next expertly identified image. As a result of a series of images passing through training stage 201 , a correlation between individual vectors and a particular vector set will be computed. The more images used to train the system, the more statistically sound the correlation result will be for an individual vector and a particular vector set. When a sufficiently large number of images have been processed and the individual vectors correlated with a particular characteristic represented by a vector set, the training stage will be complete and pattern recognition can begin.
[0036] If a particular vector is only ever found in regions of images exhibiting the characteristic, then the correlation between the vector and the characteristic will have a maximum value of one (1), which is 100% correlation. In this case, the vector will have a high predictive value for the characteristic. On the other hand, if a particular vector is never found in regions of images exhibiting the characteristic, the correlation will have a minimum value of zero (0), which is 100% non-correlation. In this case, the vector will have a high predictive value for the absence of the characteristic. Finally, if a particular vector is sometimes found in regions exhibiting the characteristic and sometimes it is not, then the correlation value (also referred to as “ratio”) will be somewhere between 0 and 1. If the ratio is near one-half, the vector will have a low predictive value for the presence of absence of the characteristic.
[0037] In the first step of the pattern recognition stage, step 230 , a candidate region of a new image is identified. A candidate region is a region of an image that has not been expertly identified to possess any regions containing any image characteristic of one or more attributes. In many cases the candidate region of an image is the entire image, or that portion of the image which contains sample tissue. As such, the vectors corresponding to the candidate region may or may not have been encountered during the training stage. In step 235 , the average of the correlations to a particular vector set corresponding to the vectors in the candidate region is computed. In step 240 , the average is evaluated to determine the likelihood that the candidate region exhibits the characteristic represented by one or more vector sets. High average correlations indicate a high probability that the candidate region exhibits the characteristic, while low average correlations indicate a low probability. The candidate region may be compared to multiple vector sets to determine the probability that the region exhibits various different characteristics. For example, an image of histology tissue may be compared to various vector sets which represent the visual characteristics of different types of tumors, to determine the likelihood that the tissue contains a tumor, and if so, the type of tumor. A significant advantage of the described technique for pattern recognition is that not only are candidate regions classified by characteristics they are likely to exhibit, but the actual probability that they do so is computed.
[0038] In one embodiment, the systems and methods for image pattern recognition are implemented using a distributed client/server architecture. FIG. 3 illustrates a client/server embodiment of the present invention. Server 302 comprises the VQ-encoding server software 308 and vocabulary 310 , and server 302 communicates with one or more clients 301 over a network 303 , for example a LAN/WAN communications channel. Clients 301 comprise the VQ-encoding client software 307 , which process image files 305 to generate vector index files 320 . In this embodiment, vocabulary 310 is located centrally on server 302 , providing shared access to clients 301 . Vocabulary centralization facilitates database maintenance and eliminates the need to synchronize distributed vocabularies as additional vectors are appended. In addition, a client/server implementation permits the concentration of computationally intensive tasks, such as searching and indexing, to be performed at a central location, relieving clients 301 from the burden.
[0039] For large vocabularies the time required to index vocabulary 310 takes about twice as long as the time required for VQ-encoding a typical image 305 . For example, out of a total time of 60 minutes to process an image, the indexing time would be 60 minutes while the VQ-encoding time would be 20 minutes. Of the 20 minutes required for encoding, segmentation of image 305 into kernels requires about 5 minutes, and searching vocabulary 310 requires about 15 minutes. When implemented using the client/server embodiment, a server process 308 can be made continuously available with a pre-indexed vocabulary. The encoding process for any given image will not require re-indexing the vocabulary, eliminating that portion of the processing time. The client/server communication overhead is relatively small compared to the overhead of subdividing the image 105 into kernels (on the client side) and searching the vocabulary 310 for these kernels (on the server side). Thus, dividing the processing between two distributed computers does not add appreciably to the execution time. On the other hand, by distributing the processing, the client-side kernel subdivision may be overlapped against the server-side vocabulary searching, resulting in a net reduction of overall processing time by eliminating the client processing time from the critical path. In this way, an overall encoding time of 60 minutes per slide can be reduced to 15 minutes per slide.
[0040] Division of processing labor between client and server in this embodiment has other efficiencies. Indexing and searching the vocabulary 310 is a computer-intensive task, best performed by fast processors equipped with large amounts of memory. Segmenting images 305 into kernels and communicating over the network 303 requires comparatively less processing power. This embodiment enables a small number of powerful server machines 302 to perform processing on behalf of a large number of less-powerful client machines 301 , yielding an overall increase in the efficiency of the system. Additionally, vocabulary files 310 are typically quite large, and are often stored on large disk arrays (e.g. RAID), while vector index files 320 are several orders of magnitude smaller, and can be stored on ordinary computer disks.
[0041] In addition to a client/server embodiment, various other aspects of the systems and methods for image pattern recognition can be employed to improve both the efficiency and accuracy. In one embodiment, for example, encoder 307 can be programmed to transform the entire image from the RGB (“red-green-blue”) color-space to the YCRCB (“intensity-red-blue”) color space prior to encoding. As kernels are matched to vectors in the vocabulary 310 , the Y channel values are matched more carefully than the C channel values, because human perception of image resolution relies primarily on differences in intensity, rather than differences in color. This prioritization enables lower tolerances in certain comparisons without compromising the information content of the kernels. By allowing the lower tolerances, more correllations are found. Accordingly, the vocabulary 310 is smaller, which results in a decrease in size for the vector index 320 , and index search times are therefore reduced.
[0042] In another aspect of the invention, color channel optimization can be implemented to further reduce the size of vocabulary file 310 . Human perception of differences in image intensity values is non-linear; it is most sensitive in the middle of the range (moderate intensity), and least sensitive at the extremes (bright or dark). Encoder 307 can be configured to take advantage of this so that as kernels are matched to vectors in the vocabulary 310 , Y channel values in the middle of the intensity range are matched with a closer tolerance than Y channel values at the ends of the range. This prioritization similarly enables lower tolerances in certain comparisons without compromising the information content of the kernels 108 . As discussed above, the lower tolerances for certain less critical comparisons advantageously results in a significantly smaller size vocabulary 310 , thereby significantly reducing index search times.
[0043] In yet another aspect, differential encoding can be employed for reducing the bit-size of C channel values within the YCRCB color space. With differential encoding, each intensity value within a vector is replaced by the difference between the intensity value and the average value of the three nearest neighbors to its upper left. For example, if the value represents the pixel at coordinate position [x, y], the average is computed of the values for pixels [x−1, y], [x−1, y−1], and [x, y−1]. (Note that in the standard convention for digital images, [0, 0] is the upper left corner of the image, with x increasing to the right, and y increasing downward.) In addition, for the C channel intensity values, intensities are typically stored as 8-bit values, but the difference between adjacent intensities can be represented by 4-bit values without loss of fidelity. This reduces the range of each value from 256 (for intensity) to 16 (for differential). Accordingly, a substantial reduction in the size of the index trees for each value is gained, thereby yielding faster searching of vocabulary 310 .
[0044] The data structure used to search vocabulary indices by the encoder 308 is an important determinant of system resource usage and encoding performance. In one embodiment, a new data structure called a vector tree can be used to store and search vector indices. A vector tree comprises a balanced tree wherein each leaf node is the root of another tree. The top-level tree represents the first dimension of each kernel. The leaf nodes of this tree contain trees which represent the second dimension of each kernel, for each defined value of the first dimension. The leaf nodes of each second-level tree contain trees which represent the third dimensions, and so on. In addition to containing the root for the next-level tree, each leaf node may also represent the last dimension of a defined vector. In this case the vector's index is also stored in the leaf node. This arrangement enables multi-dimensional vectors of different sizes to be stored together in one structure, facilitating concurrent searching for multiple kernels having different dimensions.
[0045] In one embodiment, nested kernel logic is used to store vector intensity values more efficiently and thereby reducing index search times. Kernels of size k×k pixels have 3 k 2 intensity values. The size of these vectors is a key driver of the size of the vocabulary file 310 , as well as the size of vocabulary indices and the time required for vector index searches.
[0046] In one embodiment, kernels are represented in nested fashion which reduces the number of intensity values required for each kernel to 6 k. FIG. 4 is a diagram illustrating nested kernel logic that can be used to store vectors. Using this nested kernel logic, each kernel 408 of size k (“outer kernel”) is assumed to have a previously located kernel 405 of size k−1 inside it (“inner kernel”), with their upper-left corners aligned. In actual practice this always occurs, because the encoding logic tries searching the vocabulary for successively larger kernels at a pixel location until a “not found” occurs, as described below with reference to variable sized kernel logic.
[0047] This enables the outer kernel 408 to be represented by 6 k (i.e. 3(2 k)) values. The factor of three is from the three color channels. Of the 2 k, the first value is represented by the index of the inner kernel 405 and the next k values are the pixels 410 along the right edge of the outer kernel 408 . The remaining k−1 values are the pixels 415 along the bottom edge of the outer kernel 408 .
[0048] Representing kernels with 6 k intensity values instead of 3 k 2 intensity values provides a significant reduction in the number of valued needed to represent a vector. For example, for a kernel of size k=15 pixels, there would be 90 values to store (instead of 675) for that kernel. This dramatically reduces the size of the vocabulary file and the corresponding vector trees used by the VQ-encoder for index searching. The encoding search times are similarly reduced.
[0049] Referring back to FIG. 1 , another technique for decreasing search time involves VQ-encoding an image 105 using variable-size kernel logic. Exemplary kernels 108 comprising VQ-encoded image 105 in FIG. 1 are variable in size. This technique enables mapping of image data by kernels of varying size, accommodating a wide range of objects, structures, and features in the encoded images. It also removes the need for specifying or deriving an optimum kernel size for a given image.
[0050] FIG. 5 is a flow diagram illustrating an example process for creating variable sized kernels according to an embodiment of the present invention. In step 505 , the VQ-encoder, iterates through each pixel location from upper left to lower right. In step 510 (performed for each pixel location), the vocabulary is searched for a matching kernel of size n (a parameterized value for the smallest kernel size, typically 3 or 4). In step 515 , if the kernel is found, n is incremented in step 520 and the search for a kernel of size n+1 is invoked to try to find an existing kernel of size n×n that matches the identified square region. The encoder loops through the vocabulary trying sequentially larger kernels until a “not found” condition occurs in step 515 .
[0051] In step 525 , if a match between the identified image location and an existing n×n kernel is not found, then the identified square region is mapped to the existing kernel of size n−1×n−1 that was found in the previous iteration of the loop. The use count for the n−1×n−1 kernel will be incremented to indicate that another instance of the kernel is being used to map a region of the image. As for the n×n region that was searched but never found, in step 530 that region will be added to the vocabulary (and appropriately indexed) and the use count for the new kernel will be initialized to one. Each time a kernel is matched, the use count is incremented, and when the use count exceeds a parameterized threshold (typically 20) the kernel may be used for image encoding. In this way the vocabulary is continuously enlarged over time with ever-larger kernels which contain ever-more image information.
[0052] The above described embodiment describes the use of variable size square kernels. In another embodiment, rectangular kernels may also the employed by incrementing the size kernel to be searched for to n+1×n, rather than n+1×n+1. For example, in step 515 , if the kernel is found, the size of one side of the kernel is incremented in step 520 and the search for a kernel of size n+1×n is invoked to try to find an existing kernel of size n+1×n that matches the identified rectangular region. The encoder loops through the vocabulary trying sequentially larger rectangular or square kernels until a “not found” condition occurs in step 515 .
[0053] In an exemplary embodiment, a feasibility study was conducted using liver histology sections to determine the performance and storage requirements of systems and methods described herein. One goal of this study was to verify that VQ-encoding of virtual microscope slide images could be performed on readily available computing hardware in run times that are compatible with practical applications. Another goal was to determine how quickly vocabulary sizes and corresponding index sizes converge. Convergence occurs as slides of a given tissue type are encoded. Over time, as more and more of the kernels which appear in such slides are stored in the vocabulary, correspondingly fewer new vectors need be added.
[0054] The study was performing using 49 liver tissue slides. These slides were standard H&E-stained histology samples. The slides were scanned with a ScanScope® T108 scanner. A virtual slide TIFF file was created for each slide at 54,000 pixels per inch (0.5 μm per pixel) using a Nikon 20x/0.75 Plan Apochromat objective lens, and compressed at a compression ratio of 20:1 using Aperio Technologies, Inc.'s JPEG2000 compression software using 7/9 wavelets. In compressed form, each virtual slide TIFF file comprised approximately 250 MB. FIG. 6 is a table that summarizes a representative sample of the slides used for this study.
[0055] The method used in the study employed a tolerance parameter to determine how closely kernels from an image must match vectors in the vocabulary. The study was done three times with three different values for the tolerance parameter: 4% (high), 5% (medium), and 6% (low). In each case, the vocabulary was initially empty. In other words, the three studies began with no pre-existing kernels in the vocabulary. Each of the slide images was encoded against the vocabulary yielding a vector index file. The encoding process progressively added kernels to the vocabulary. Each slide was decoded after encoding and visually inspected using Aperio Technologies' ImageScope™ viewer to verify that the encoding/decoding process was successful.
[0056] The slides were encoded using a Dell Dimension 700 MHz Pentium III desktop computer with IGB RAM and 80 GB hard disk. This computer ran Windows 2000 Professional with all unneeded operating system services disabled. Timing, disk and memory measurements were performed by the VQ-encoding software itself.
[0057] A sample of the results from the first study is shown in the table in FIG. 7 . This table shows processing statistics for the first five slides processed, and for the last five slides processed (out of 49 total slides). The last three columns show the processing times. The average index load time was 30 minutes, which increased continuously throughout the study to a maximum of 39 minutes. The average encoding time was 17 minutes with a max of 24 minutes. The overall processing time averaged 48 minutes, with a maximum total time of 63 minutes.
[0058] A key observation from this study was whether the vocabulary size would converge, that is, reach a point where successive new slides added fewer and fewer kernels to the database. The cumulative total of vectors column (#vectors) in FIG. 7 shows that the first few slides added significantly more vectors to the vocabulary than the last few slides. After 49 slides, a substantial amount of convergence had taken place. FIG. 8 is a graph which shows the change in vocabulary size as slides were processed. Although the vocabulary never reached an asymptote, the rate of growth after 49 slides substantially slowed.
[0059] Another key observation from this study was whether the index size would “converge”, and how large the memory-resident index would be. The size of vector index column (idx MB) in FIG. 7 shows that the initial index size was 520 MB after only one slide, but thereafter the growth slowed considerably and nearly stopped altogether. FIG. 9 is a graph which shows the change in index size as slides were processed. The index size never exceeded the physical memory available on the machine (IGB), so paging was never required. If the index cannot remain memory-resident encoding performance would decrease dramatically. FIG. 9 also shows the index processing time increasing as slides are processed. In the study, the index load time did not stop growing as fast as the index size because as the total index becomes larger each new index requires more time to insert.
[0060] Micrometastasis is a practically useful rare-event finding application that can benefit greatly from the systems and methods of the present invention. For patients with tumors, a key question is whether cancer cells are metastasizing, i.e. breaking free from the tumor and traveling to other areas of the body through the bloodstream. Micrometastasis is the presence of small clusters of 1-10 cancer cells in blood. To determine whether such metastasis is taking place, up to fifty cytology slides are prepared with a patient's blood. These slides are then examined with a microscope by a pathologist to determine if micrometastasis clusters are present.
[0061] An enrichment procedure is typically used to increase the occurrence of potential tumor cells in a block sample. Tumor cells are differentiated from normal cells based on the following morphological features:
a) Size: typically at least 20 μm diameter (normal white blood cells are 10 μm-15 μm). b) Nuclear size: Large and usually round (normal nuclei are smaller and/or irregular in shape). c) Nuclear morphology: Usually one or more nucleoli are present (small dark blue staining regions within the nuclei). d) Nuclear staining: Usually stained lighter (less hematoxylin) compared to a normal white blood cell. e) Cytoplasm staining: May be stained bluer (more basophilic) than a normal white blood cell. f) Nuclear to cytoplasmic ratio: Usually higher than normal white blood cell indicating a larger nucleus.
[0068] Differentiation based on these attributes is subtle and requires an experienced pathologist for detection. In this type of rare event detection application it is important not to have false negatives, i.e., it is important not to miss micrometastasis clusters despite their sparse occurrence and difficulty of detection.
[0069] To reduce the probability of false negatives, slides are treated with an immunocytochemical antibody that is specific to epithelial cells (a type of cell from which tumors frequently derive). The antibody is prepared as a stain which colors cells of epithelial origin red, whereas normal white blood cells remain unstained. This significantly increases the contrast of micrometastasis clusters, simplifying visual detection and reducing the probability of false negatives. With this stain, micrometastasis slides samples can be scanned at a lower resolution, enabling scanning to be performed more quickly.
[0070] To further reduce the probability of false negatives, up to fifty slides are visually scanned, and in a typical case 1-10 clusters occur per slide, a very sparse distribution, and it is important for each cluster to be found to ensure a reliable diagnosis. Some false positives may also occur, for example, dust particles which absorb the immunocytochemical stain and appear as red globs, and other debris in the blood sample. All located potential clusters must be examined visually at high magnification to distinguish false positives from genuine micrometastasis clusters.
[0071] A threshold is required to determine when a region constitutes a found target. The method can be run iteratively with different threshold values to determine the value which yields the best results. In practical application this threshold would be kept on the low side of optimal to bias the pattern recognition in favor of false positives (reducing the possibility of false negatives).
[0072] FIG. 10 is a block diagram illustrating an exemplary computer system 550 that may be used in connection with the various embodiments described herein. For example, the computer system 550 may be used in conjunction with a server computer or client computer previously described with respect to FIG. 3 . However, other computer systems and/or architectures may be used, as will be clear to those skilled in the art.
[0073] The computer system 550 preferably includes one or more processors, such as processor 552 . Additional processors may be provided, such as an auxiliary processor to manage input/output, an auxiliary processor to perform floating point mathematical operations, a special-purpose microprocessor having an architecture suitable for fast execution of signal processing algorithms (e.g., digital signal processor), a slave processor subordinate to the main processing system (e.g., back-end processor), an additional microprocessor or controller for dual or multiple processor systems, or a coprocessor. Such auxiliary processors may be discrete processors or may be integrated with the processor 552 .
[0074] The processor 552 is preferably connected to a communication bus 554 . The communication bus 554 may include a data channel for facilitating information transfer between storage and other peripheral components of the computer system 550 . The communication bus 554 further may provide a set of signals used for communication with the processor 552 , including a data bus, address bus, and control bus (not shown). The communication bus 554 may comprise any standard or non-standard bus architecture such as, for example, bus architectures compliant with industry standard architecture (“ISA”), extended industry standard architecture (“EISA”), Micro Channel Architecture (“MCA”), peripheral component interconnect (“PCI”) local bus, or standards promulgated by the Institute of Electrical and Electronics Engineers (“IEEE”) including IEEE 488 general-purpose interface bus (“GPIB”), IEEE 696/S-100, and the like.
[0075] Computer system 550 preferably includes a main memory 556 and may also include a secondary memory 558 . The main memory 556 provides storage of instructions and data for programs executing on the processor 552 . The main memory 556 is typically semiconductor-based memory such as dynamic random access memory (“DRAM”) and/or static random access memory (“SRAM”). Other semiconductor-based memory types include, for example, synchronous dynamic random access memory (“SDRAM”), Rambus dynamic random access memory (“RDRAM”), ferroelectric random access memory (“FRAM”), and the like, including read only memory (“ROM”).
[0076] The secondary memory 558 may optionally include a hard disk drive 560 and/or a removable storage drive 562 , for example a floppy disk drive, a magnetic tape drive, a compact disc (“CD”) drive, a digital versatile disc (“DVD”) drive, etc. The removable storage drive 562 reads from and/or writes to a removable storage medium 564 in a well-known manner. Removable storage medium 564 may be, for example, a floppy disk, magnetic tape, CD, DVD, etc.
[0077] The removable storage medium 564 is preferably a computer readable medium having stored thereon computer executable code (i.e., software) and/or data. The computer software or data stored on the removable storage medium 564 is read into the computer system 550 as electrical communication signals 578 .
[0078] In alternative embodiments, secondary memory 558 may include other similar means for allowing computer programs or other data or instructions to be loaded into the computer system 550 . Such means may include, for example, an external storage medium 572 and an interface 570 . Examples of external storage medium 572 may include an external hard disk drive or an external optical drive, or and external magneto-optical drive.
[0079] Other examples of secondary memory 558 may include semiconductor-based memory such as programmable read-only memory (“PROM”), erasable programmable read-only memory (“EPROM”), electrically erasable read-only memory (“EEPROM”), or flash memory (block oriented memory similar to EEPROM). Also included are any other removable storage units 572 and interfaces 570 , which allow software and data to be transferred from the removable storage unit 572 to the computer system 550 .
[0080] Computer system 550 may also include a communication interface 574 . The communication interface 574 allows software and data to be transferred between computer system 550 and external devices (e.g. printers), networks, or information sources. For example, computer software or executable code may be transferred to computer system 550 from a network server via communication interface 574 . Examples of communication interface 574 include a modem, a network interface card (“NIC”), a communications port, a PCMCIA slot and card, an infrared interface, and an IEEE 1394 fire-wire, just to name a few.
[0081] Communication interface 574 preferably implements industry promulgated protocol standards, such as Ethernet IEEE 802 standards, Fiber Channel, digital subscriber line (“DSL”), asynchronous digital subscriber line (“ADSL”), frame relay, asynchronous transfer mode (“ATM”), integrated digital services network (“ISDN”), personal communications services (“PCS”), transmission control protocol/Internet protocol (“TCP/IP”), serial line Internet protocol/point to point protocol (“SLIP/PPP”), and so on, but may also implement customized or non-standard interface protocols as well.
[0082] Software and data transferred via communication interface 574 are generally in the form of electrical communication signals 578 . These signals 578 are preferably provided to communication interface 574 via a communication channel 576 . Communication channel 576 carries signals 578 and can be implemented using a variety of communication means including wire or cable, fiber optics, conventional phone line, cellular phone link, radio frequency (RF) link, or infrared link, just to name a few.
[0083] Computer executable code (i.e., computer programs or software) is stored in the main memory 556 and/or the secondary memory 558 . Computer programs can also be received via communication interface 574 and stored in the main memory 556 and/or the secondary memory 558 . Such computer programs, when executed, enable the computer system 550 to perform the various functions of the present invention as previously described.
[0084] In this description, the term “computer readable medium” is used to refer to any media used to provide computer executable code (e.g., software and computer programs) to the computer system 550 . Examples of these media include main memory 556 , secondary memory 558 (including hard disk drive 560 , removable storage medium 564 , and external storage medium 572 ), and any peripheral device communicatively coupled with communication interface 574 (including a network information server or other network device). These computer readable mediums are means for providing executable code, programming instructions, and software to the computer system 550 .
[0085] In an embodiment that is implemented using software, the software may be stored on a computer readable medium and loaded into computer system 550 by way of removable storage drive 562 , interface 570 , or communication interface 574 . In such an embodiment, the software is loaded into the computer system 550 in the form of electrical communication signals 578 . The software, when executed by the processor 552 , preferably causes the processor 552 to perform the inventive features and functions previously described herein.
[0086] Various embodiments may also be implemented primarily in hardware using, for example, components such as application specific integrated circuits (“ASICs”), or field programmable gate arrays (“FPGAs”). Implementation of a hardware state machine capable of performing the functions described herein will also be apparent to those skilled in the relevant art. Various embodiments may also be implemented using a combination of both hardware and software.
[0087] While the particular systems and methods herein shown and described in detail are fully capable of attaining the above described objects of this invention, it is to be understood that the description and drawings presented herein represent a presently preferred embodiment of the invention and are therefore representative of the subject matter which is broadly contemplated by the present invention. It is further understood that the scope of the present invention fully encompasses other embodiments that may become obvious to those skilled in the art and that the scope of the present invention is accordingly limited by nothing other than the appended claims. | Systems and methods for image pattern recognition comprise digital image capture and encoding using vector quantization (“VQ”) of the image. A vocabulary of vectors is built by segmenting images into kernels and creating vectors corresponding to each kernel. Images are encoded by creating a vector index file having indices that point to the vectors stored in the vocabulary. The vector index file can be used to reconstruct an image by looking up vectors stored in the vocabulary. Pattern recognition of candidate regions of images can be accomplished by correlating image vectors to a pre-trained vocabulary of vector sets comprising vectors that correlate with particular image characteristics. In virtual microscopy, the systems and methods are suitable for rare-event finding, such as detection of micrometastasis clusters, tissue identification, such as locating regions of analysis for immunohistochemical assays, and rapid screening of tissue samples, such as histology sections arranged as tissue microarrays (TMAs). | 7 |
CROSS-REFERENCE TO RELATED APPLICATIONS
[0001] This application is based upon and claims the benefit of priority from the prior Japanese Patent Application No. 2000-351074, filed Nov. 17, 2000, the entire contents of which are incorporated herein by reference.
BACKGROUND OF THE INVENTION
[0002] 1. Field of the Invention
[0003] This invention relates to an image forming apparatus which performs both sides printing by re-feeding paper on which image formation on one side thereof is finished by using an image formation mechanism for performing the image formation on one side of paper to the image formation mechanism after reversing the paper at a paper carry route, and by performing the image formation by using the image formation mechanism, and to a controlling method of paper carry at the image forming apparatus.
[0004] 2. Description of the Related Art
[0005] Both sides printing by an electrophotographic apparatus and the like is realized by reversing paper on which image formation on one side thereof is finished and by re-feeding the paper to an image formation position by an image formation mechanism.
[0006] In such an image forming apparatus, a paper carry route becomes extremely long. Owing to this, if it is designed so as to perform printing on another sheet of paper after completing the both sides printing on one sheet of paper, a printing speed of the both sides printing becomes extremely slow.
[0007] Here, high-speed both sides printing can be realized by taking a design where plural sheets of paper can individually be carried in the paper carry route by providing plural motors. However, if plural motors are provided in this manner, cost of parts increases while a process burden of a CPU for controlling the motors increases since it becomes necessary to control more motors individually.
BRIEF SUMMARY OF THE INVENTION
[0008] An object of the present invention is to enable high-speed both sides printing with a number of drive sources limited to the minimum.
[0009] According to an aspect of the invention, there is provided an image forming apparatus as below.
[0010] An image forming apparatus comprising;
[0011] an image formation mechanism which forms an image on a paper; a paper carry mechanism which carries the paper at a paper carry route having an image formation section which carries the paper toward one direction so as to make the image formation mechanism perform image formation on the paper, a return section which once takes in the paper carried out from the image formation section and carries out the paper toward a predetermined return direction being different from the direction toward the image formation section while reversing a carry direction, and a paper side reversal section which feeds the paper reversed to the other side after passing the image formation section at the last time to the image formation section at a predetermined timing after temporally stopping and holding the paper carried out from the return section; a drive source which rotates both a return roller provided in the paper carry mechanism in order to take in the paper carried out from the image formation section to the return section and to carry out the paper from the return section to the return direction, and at least one carry roller provided in the paper carry mechanism in order to carry the paper at the paper side reversal section; a clutch which transmits a driving force of the drive source to the carry roller having a possibility to nip and hold the paper when the paper is temporally stopped and held among the carry rollers only when the drive source is operating so that the return roller will carry the paper toward the return direction; and a carry control section which controls the paper carry by repeating a step of feeding the n-th sheet of paper on which the image formation on only one side is completed from the paper side reversal section to the image formation section, and feeding the n+1-th sheet of paper on which the image formation on only one side is completed from the return section to the paper side reversal section, and a step of, under the state where the n+1-th sheet of paper is held at the paper side reversal section, ejecting the n-th sheet of paper on which the image formation on both sides is completed, and feeding the n+2-th sheet of paper from the image formation section to the return section after taking-in the paper to the image formation area and performing the image formation on one side.
[0012] According to another aspect of the invention, there is provided a paper carry controlling method as below.
[0013] A paper carry controlling method in an image forming apparatus comprising;
[0014] an image formation mechanism which forms an image on a paper; a paper carry mechanism which carries the paper at a paper carry route having an image formation section which carries the paper toward one direction so as to make the image formation mechanism perform image formation on the paper, a return section which once takes in the paper carried out from the image formation section and carries out the paper toward a predetermined return direction being different from the direction toward the image formation section while reversing a carry direction, and a paper side reversal section which feeds the paper reversed to the other side after passing the image formation section at the last time to the image formation section at a predetermined timing after temporally stopping and holding the paper carried out from the return section; a drive source which rotates both a return roller provided in the paper carry mechanism in order to take in the paper carried out from the image formation section to the return section and to carry out the paper from the return section to the return direction, and at least one carry roller provided in the paper carry mechanism in order to carry the paper at the paper side reversal section; and a clutch which transmits a driving force of the drive source to the carry roller having a possibility to nip and hold the paper when the paper is temporally stopped and held among the carry rollers only when the drive source is operating so that the return roller will carry the paper toward the return direction, the paper carry controlling method being performed by repeating a step of feeding the n-th sheet of paper on which the image formation on only one side is completed from the paper side reversal section to the image formation section, and feeding the n+1-th sheet of paper on which the image formation on only one side is completed from the return section to the paper side reversal section, and a step of, under the state where the n+1-th sheet of paper is held at the paper side reversal section, ejecting the n-th sheet of paper on which the image formation on both sides is completed, and feeding the n+2-th sheet of paper from the image formation section to the return section after taking-in the paper to the image formation area and performing the image formation on one side.
[0015] 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 hereinafter.
BRIEF DESCRIPTION OF THE SEVERAL VIEWS OF THE DRAWING
[0016] The accompanying drawings, which are incorporated in and constitute a part of the specification, illustrate embodiments of the invention, and together with the general description given above and the detailed description of the embodiments given below, serve to explain the principles of the invention.
[0017] [0017]FIG. 1 is a diagram showing a structure of a mechanism portion of an electrophotographic apparatus according to an embodiment of the present invention.
[0018] [0018]FIG. 2 is a block diagram of a control system for paper carry of the electrophotographic apparatus shown in FIG. 1.
[0019] [0019]FIG. 3 is a timing diagram showing timing for the paper carry for a case where both sides printing is performed.
DETAILED DESCRIPTION OF THE INVENTION
[0020] Hereinafter, an explanation will be given of an embodiment of the present invention with reference to the drawings.
[0021] [0021]FIG. 1 is a diagram showing a structure of a mechanism portion of an electrophotographic apparatus according to this embodiment.
[0022] As shown in FIG. 1, the electrophotographic apparatus in this embodiment has a photosensitive drum 1 , an electrification device 2 , a developing device 3 , a transferring device 4 , a fixing roller 5 , a first feeding roller 6 , a second feeding roller 7 , a third feeding roller 8 , a fourth feeding roller 9 , an anti-side-slide roller (referred to as RGT roller hereinafter) 10 , an ejecting roller 11 , an ADU gate 12 , ADU rollers 13 , 14 , and 15 , a main motor 16 , a first feeding clutch 17 , a second feeding clutch 18 , a third feeding clutch 19 , a fourth feeding clutch 20 , an RGT clutch 21 , an ADU motor 22 , one-way clutches 23 , 24 , and 25 , a first carry route sensor (referred to as TR 1 sensor hereinafter) 26 , a second carry route sensor (referred to as TR 2 sensor hereinafter) 27 , an RGT sensor 28 , an ejection sensor 29 , a first jam detection sensor (referred to as first ADU sensor hereinafter) 30 , and a second jam detection sensor (referred to as second ADU sensor hereinafter) 31 .
[0023] The electrification device 2 , the developing device 3 , and the transferring device 4 are arranged along a surface of the photosensitive drum 1 with a predetermined position relation, and perform processes of the respective steps of an electrophotographic process with exposure performed separately at a predetermined position. Owing to this, a toner image is formed for the paper passing through between the photosensitive drum 1 and the transferring device 4 . The toner image is formed on a side of the paper which contacts the photosensitive drum 1 . By pressing and melting the toner image formed on the paper by using the fixing roller 5 , the image is fixed.
[0024] A paper route is indicated by dashed lines in FIG. 1. The paper route is formed with the photosensitive drum 1 , the fixing roller 5 , the first feeding roller 6 , the second feeding roller 7 , the third feeding roller 8 , the fourth feeding roller 9 , the RGT roller 10 , the ejecting roller 11 , the ADU gate 12 and the ADU rollers 13 , 14 , and 15 , and guide members (not shown).
[0025] The photosensitive drum 1 , the fixing roller 5 , the first feeding roller 6 , the second feeding roller 7 , the third feeding roller 8 , the fourth feeding roller 9 , and the RGT roller 10 all rotate in an arrowed direction shown in FIG. 1 by receiving a driving force from the main motor 16 . Moreover, the ejecting roller 11 and the ADU rollers 13 , 14 , and 15 all rotates in the arrowed direction shown in FIG. 1 by receiving the driving force from the ADU motor 22 .
[0026] The first feeding roller 6 feeds paper from a paper cassette PC 1 , the second feeding roller 7 feeds paper from a paper cassette PC 2 , and the third feeding roller 8 and the fourth feeding roller 9 feed paper from a paper cassette PC 3 respectively to the RGT roller 10 .
[0027] The RGT roller 10 feeds the paper to the fixing roller 5 through between the photosensitive drum 1 and the transferring device 4 .
[0028] The ejecting roller 11 can rotate in a normal direction and a reverse direction in accordance with a rotation direction of the ADU motor 22 . Under a reverse rotation state, the ejecting roller 11 pulls in the paper to be carried by the fixing roller 5 , and ejects the paper to a stacker ST as need arises. Moreover, under a normal rotation state, the ejecting roller 11 feeds the paper which is nipped and held to the ADU roller 13 .
[0029] When the paper is fed to the ejecting roller 11 by the fixing roller 5 , the ADU gate 12 is pushed-up by the paper as shown in FIG. 1 so that it does not interfere with the paper carry. Moreover, the ADU gate 12 falls with its own weight so as to block the route from the fixing roller 5 to the ejecting roller 11 after a back edge from a carry direction of the paper to be fed to the ejecting roller 11 by the fixing roller 5 passes through, and it forms the route reaching the ADU roller 13 from the ejecting roller 11 .
[0030] The ADU rollers 13 , 14 , and 15 carry the paper to be carried from the ejecting roller 11 in order, and feed the paper to the RGT roller 10 in the same carry direction.
[0031] The main motor 16 generates the driving force for rotating the photosensitive drum 1 , the fixing roller 5 , the first feeding roller 6 , the second feeding roller 7 , the third feeding roller 8 , the fourth feeding roller 9 , and the RGT roller 10 , respectively.
[0032] The first feeding clutch 17 , the second feeding clutch 18 , the third feeding clutch 19 , and the fourth feeding clutch 20 transmit/intercept driving from the main motor 16 to the first feeding roller 6 , the second feeding roller 7 , the third feeding roller 8 , and the fourth feeding roller 9 , respectively.
[0033] The ADU motor 22 generates the driving force for rotating the ejecting roller 11 , and the ADU rollers 13 , 14 , and 15 , respectively. The ADU motor 22 can perform both the normal rotation and the reverse rotation, and generates the driving force for normally-rotating the ejecting roller 11 during the normal rotation and the driving force for reversely-rotating the ejecting roller 11 during the reverse rotation, respectively.
[0034] The one-way clutches 23 , 24 , and 25 have a well-known structure which transmits only the driving force in one direction. The one-way clutches 23 , 24 , and 25 have a mesh direction being the normal-rotation direction of the ADU motor 22 , and rotate the ADU rollers 13 , 14 , and 15 in the arrowed direction shown in FIG. 1 when the ADU motor 22 is in the normal rotation. Moreover, concerning the one-way clutches 23 , 24 , and 25 , the reverse-rotation direction of the ADU motor 22 is an idle rotation direction.
[0035] The TR 1 sensor 26 is arranged at a position through which the paper to be carried by the second feeding roller 7 and the paper to be carried by the third feeding roller 8 pass, and detects the existence of the paper at the position.
[0036] The TR 2 sensor 27 is arranged at a position through which the paper carried by the third feeding roller 8 passes, and detects the existence of the paper at the position.
[0037] The RGT sensor 28 is arranged near the RGT roller 10 at a position through which the paper to be fed to the RGT roller 10 by the first feeding roller 6 , the second feeding roller 7 , the third feeding roller 8 , and the ADU roller 15 passes, and detects the existence of the paper at the position.
[0038] The ejection sensor 29 is arranged near the ADU gate 12 at a position through which the paper fed from the fixing roller 5 to the ejecting roller 11 passes, and detects the existence of the paper at the position.
[0039] The first ADU sensor 30 and the second ADU sensor 31 are respectively arranged at a position through which the paper to be fed from the ADU roller 13 to the ADU roller 14 passes and at a position through which the paper to be fed from the ADU roller 14 to the ADU roller 15 passes, and detect the existence of the paper at the positions, respectively.
[0040] The carry route of the paper formed with the arrangement as described above can roughly be classified into a feed section 101 , an image formation section 102 , a ejection/return section 103 , and a paper side reversal section 104 as shown by circling with broken lines in FIG. 1.
[0041] The feeding section 101 is a section for feeding a new sheet of paper to the image formation section 102 . The image formation section 102 is a section for performing an image formation operation to the paper. The paper ejection/return section 103 is a section for ejecting the paper on which the necessary image formation is completed to the stacker ST. Moreover, the ejection/return section 103 is a section for returning the paper on which the image formation on only one side is completed to the paper side reversal section 104 . The paper side reversal section 104 is a section for reversing the paper when it passes the image formation section 102 .
[0042] [0042]FIG. 2 is a block diagram showing a control system for the paper carry of the electrophotographic apparatus in this embodiment. Besides, the parts being the same as those in FIG. 1 are given the same numerals respectively, and the detailed explanations thereof are omitted.
[0043] As shown in FIG. 2, there are comprised a CPU 32 , a ROM 33 , a RAM 34 , an interface portion (referred to as IF portion hereinafter) 35 , and an input/output portion (referred to as I/O portion hereinafter) 36 as the control system, and they are connected to each other via a bus 37 .
[0044] The CPU 32 controls the main motor 16 and the ADU motor 22 , or the first feeding clutch 17 , the second feeding clutch 18 , the third feeding clutch 19 , the fourth feeding clutch 20 , and the RGT clutch 21 while referring to the respective detected results of the TR 1 sensor 26 , the TR 2 sensor 27 , the RGT sensor 28 , the ejection sensor 29 , the first ADU sensor 30 , and the second ADU sensor 31 . The CPU 32 realizes the control by a software process based on an operation program stored in the ROM 33 .
[0045] The ROM 33 stores data and the like that are necessary for the operation program used by the CPU 32 or the CPU 32 to perform various sorts of processes.
[0046] The RAM 34 is used as a work area and the like for the CPU 32 to perform the various sorts of processes.
[0047] The IF portion 35 performs an interface process for a main CPU (not shown) and the like for totally-controlling the operation of the whole electrophotographic apparatus in this embodiment and the CPU 32 to give/receive the various sorts of data.
[0048] To the I/O portion 36 , there are connected the main motor 16 , the ADU motor 22 , the first feeding clutch 17 , the second feeding clutch 18 , the third feeding clutch 19 , the fourth feeding clutch 20 , the RGT clutch 21 , the TR 1 sensor 26 , the TR 2 sensor 27 , the RGT sensor 28 , the ejection sensor 29 , the first ADU sensor 30 , and the second ADU sensor 31 , respectively. The I/O portion 36 performs the input/output process of a signal relating to each of these portions.
[0049] Next, an explanation will be given of the operation of the electrophotographic apparatus composed as above. Besides, the operation itself for the image formation on the paper is similar to that of the conventional electrophotographic apparatus so that an explanation thereof is omitted. Here, an explanation will mainly be given of the operation of the paper carry for the both sides printing.
[0050] [0050]FIG. 3 is a timing drawing showing the timing of the paper carry of the case where the both sides printing is performed by using the paper stored in the paper cassette PC 3 in FIG. 1.
[0051] An explanation will be given of the operation of each portion at the time with reference to FIG. 3.
[0052] At first, the CPU 32 starts up the main motor 16 when a start of printing operation is requested by the main CPU (not shown). However, the CPU 32 keeps the first to the fourth feeding clutches 17 to 20 and the RGT clutch 21 under an intercepted state at the time. Owing to this, the photosensitive drum 1 and the fixing roller 5 start the rotation here (timing T 1 ).
[0053] After this, when performing the image formation becomes possible, the CPU 32 rotates the third feeding roller 8 and the fourth feeding roller 9 by making the third feeding clutch 19 and the fourth feeding clutch 20 into a transmission state, and feeds the first sheet of paper to the RGT roller 10 (period PA).
[0054] Now, when the paper is carried by the third feeding roller 8 and the fourth feeding roller 9 , the TR 2 sensor 27 , the TR 1 sensor 26 , and the RGT sensor 28 are turned-on in order (timings T 2 , T 3 , and T 4 ). Then, the CUP 32 makes the RGT clutch 21 into the transmission state and starts the rotation of the RGT roller 10 responding to the fact that the RGT sensor 28 is turned-on (timing T 5 ). In this manner, the first sheet of paper is taken-in to the image formation section 102 by the rotation of the RGT roller 10 , and the image formation on the obverse side of the paper (the side facing to the photosensitive drum 1 at the time) is performed. Then, if the back edge of the first sheet of paper passes through the RGT sensor 28 and the RGT sensor 28 is turned-off (timing T 6 ), the CPU 32 makes the RGT clutch 21 into the intercepted state and stops the rotation of the RGT roller 10 at about the timing at which the back edge of the first sheet of paper passes thorough the RGT roller 10 (timing T 7 ). At the time, the first sheet of paper is already nipped and held by the fixing roller 5 , and is carried toward the ejecting roller 11 by the fixing roller 5 .
[0055] When the first sheet of paper arrives at the feed sensor 29 and the ejection sensor 29 is turned-on, the CPU 32 reverses the ADU motor 22 during the period where the ejection sensor 29 continues to be on (period PB). In this manner, during the period PB, the first sheet of paper is taken-in to the ejection/return section 103 , and the ejecting roller is suspended under the state where the back edge of the first sheet of paper is nipped and held by the ejecting roller 11 .
[0056] Although the first sheet of paper is carried as above, when the back edge of the first sheet of paper passes through the TR 1 sensor 26 and the TR 1 sensor 26 is turned-off, the CPU 32 rotates the third feeding roller 8 and the fourth feeding roller 9 by making the third feeding clutch 19 and the fourth feeding clutch 20 into the transmission state, and feeds the second sheet of paper to the RGT roller 10 (period PC). That is to say, the second sheet of paper is fed to the RGT roller 10 at the same time as carrying the first sheet of paper from the image formation section 102 to the ejection/return section 103 .
[0057] Now, if the period PB during which the ejection sensor 29 is turned-on by the first sheet of paper ends, the CPU 32 then starts the rotation of the ADU motor 22 from the timing at which some time has passed (timing T 8 ). Owing to this, the first sheet of paper nipped and held by the ejecting roller 11 is fed from the ejection/return section 103 to the paper side reversal section 104 by the ejecting roller 11 . The mash direction of the one-way clutches 23 , 24 , and 25 is the normal rotation so that the ADU rollers 13 , 14 , and 15 also rotate at the time, and the first sheet of paper fed by the ejecting roller 11 is pulled-in to the paper side reversal section 104 by these ADU rollers 13 , 14 , and 15 .
[0058] On the other hand, the CPU 32 starts the rotation of the RGT roller 10 responding to the fact that a fixed time t (for example, 0.5 second) has passed from the timing T 8 at which the normal rotation of the ADU motor 22 starts (timing T 9 ). Owing to this, the second sheet of paper carried to the RGT roller 10 is taken-in to the image formation section 102 , and the image formation on the obverse side is performed. Besides, although the timing at which the rotation of the RGT roller 10 is started is determined on the basis of the timing besides an ON-timing of the RGT sensor 28 , it is only for the case where the second sheet of paper is fed. After this, the CPU 32 performs a rotation control of the RGT roller 10 in accordance with the state of the RGT sensor 28 at the timing that is similar to relations between the above-mentioned a timings T 4 and T 5 , and between the above-mentioned timings T 6 and T 7 .
[0059] In this manner, when the second sheet of paper is carried, and it arrives at and turns on the ejection sensor 29 , the CPU 32 makes the ADU motor 22 start the reversal rotation (timing T 10 ). Owing to this, the normal rotation of the ADU motor 22 is finished, and the carry of the first sheet of paper from the ejection/return section 103 to the paper side reversal section 104 is performed during the period from the timing T 8 to the timing T 10 , during which the ADU motor 22 is normally-rotating (period PD). Besides, the fixed period t is a waiting time for adjusting the period PD to the length in which the entire first sheet of paper can surely be carried to the paper side reversal section 104 , and it is set as it is considered appropriate by considering a paper carry speed or a dimension condition among the respective rollers.
[0060] Then, the CPU 32 reverses the ADU motor 22 while there continues the state where the ejection sensor 29 is turned-on by the second sheet of paper (period PE). In this manner, the ejecting roller 11 is suspended under the state where the second sheet of paper is taken-in to the ejection/return section 103 , and the back edge of the second sheet of paper is nipped and held by the ejecting roller 11 during the period PE. At the time, although the first sheet of paper exists in the paper side reversal section 104 and is nipped and held by at least any one of the ADU rollers 13 , 14 , and 15 , the first sheet of paper stays at the paper side reversal section 104 since these ADU rollers 13 , 14 , and 15 are stopped due to the fact that the reverse rotation of the ADU motor 22 is in the idle-rotation direction of the one-way clutches 23 , 24 , and 15 .
[0061] If the period PE during which the ejection sensor 29 is turned-on by the second sheet of paper ends, the CPU 32 then starts the normal rotation of the ADU motor 22 from the timing at which some time has passed (timing T 11 ). Owing to this, the second sheet of paper nipped and held by the ejecting roller 11 is fed from the ejection/return section 103 to the paper side reversal section 104 by the ejecting roller 11 . Since the ADU rollers 13 , 14 , and 15 also rotate at the time, the second sheet of paper that is fed by the ejecting roller 11 is pulled-in to the paper side reversal section 104 by these ADU rollers 13 , 14 , and 15 .
[0062] Moreover, the ADU rollers 13 , 14 , and 15 rotate in this manner so that the first sheet of paper stacked at the paper side reversal section 104 is delivered from the paper surface reversing section 104 by the ADU rollers 13 , 14 , and 15 . Then, responding to the fact that the first sheet of paper arrives at the RGT sensor 28 , there are performed taking-in the paper to the image formation section 102 , the image formation on the paper, and delivery of the paper from the image formation section 102 in a similar manner to above. At the time, the side of the paper facing the photo-sensitive drum 1 is a reverse side of the side that passed through the image formation section 102 at the last time, and the image formation on the reverse side is performed. Then, until when the first sheet of paper arrives at the ejection sensor 29 and the ejection sensor 29 is turned-on (timing T 12 ), there is continued the state where pulling-in the second sheet of paper to the paper side reversal section 104 as above and the delivery of the first sheet of paper from the paper side reversal section 104 are performed (period PF).
[0063] Now, when the back edge of the first sheet of paper fed to the image formation section 102 for the image formation on the reverse side passes through the RGT sensor 28 and the RGT sensor 28 is turned-off (timing T 13 ), the CPU 32 rotates the third feeding roller 8 and the fourth feeding roller 9 responding to it, and feeds the third sheet of paper to the RGT roller 10 (period PG). In this manner, at the same time as performing the image formation on the reverse side of the first sheet of paper and the delivery of the first sheet of paper from the image formation section 102 , there are performed the feed of the third sheet of paper, taking-in the third sheet of paper to the image formation section 102 , and the image formation on the obverse side of the third sheet of paper.
[0064] At the time, the CPU 32 reverses the ADU motor 22 sometime between the timing T 12 at which the first sheet of paper arrives at the ejection sensor 29 and the timing (timing T 14 ) at which the ejection sensor 29 is turned-off at the second time since the timing T 12 . That is to say, the CPU 32 reverses the ADU motor 22 sometime between the time at which the first sheet of paper arrives at the ejection sensor 29 and the time at which the back edge of the third sheet of paper passes through the ejection sensor 29 . As a result, even after the back edge of the first sheet of paper reaches to the ejecting roller 11 , the ejecting roller 11 continues the reverse rotation so that the first sheet of paper on which the image formation on the reverse side is completed, that is to say, the first sheet of paper on which the both sides printing is completed is ejected to the stacker ST by the ejecting roller 11 (period PH). Then, the third sheet of paper that reaches to the ejecting roller 11 following the first sheet of paper is taken-in to the eject/return section 103 by the ejecting roller 11 and is stopped under the state where the back edge thereof is nipped and held by the ejecting roller 11 (period PI).
[0065] Although the second sheet of paper is taken-in to the paper side reversal section 104 at the start timing T 12 during the period PH, the paper stays at the paper side reversal section 104 during the period PH and the period PI since the ADU rollers 13 , 14 , and 15 do not rotate.
[0066] Hereinafter, at similar timings to the relation of the above-mentioned carry timings of the first, second, and third sheets of paper, there are repeatedly performed the image formation on the reverse side of an n-th sheet of paper and ejection thereof, taking-in an n+1-th sheet of paper to the paper side reversal section 104 , the feed of an n+2-th sheet of paper, the image formation on the obverse side of the n+2-th sheet of paper, and taking-in the n+2-th sheet of paper to the ejection/return section 103 .
[0067] In this manner, according to this embodiment, the image formation operation by circulating two sheets of paper can be performed all the time at the image formation section 102 , the ejection/return section 103 , and the paper side reversal section 104 at the time of performing the both sides printing, and the high-speed both sides printing is possible.
[0068] In addition, since this embodiment is designed so that the drive of the ADU rollers 13 , 14 , and 15 for performing the paper carry at the paper side reversal section 104 will be performed by the ADU motor 22 for driving the ejecting roller 11 , a structure thereof is simpler and the process burden of the CPU 32 is less than the case where the drive of the ejecting roller 11 and the drive of the ADU rollers 13 , 14 , and 15 are performed by individual motors.
[0069] Moreover, in this embodiment, clutch control is unnecessary since the one-way clutches 23 , 24 , and 25 are used in order to make the rotation of the ADU rollers 13 , 14 , and 15 only in one direction so that the burden to the CPU 32 is less.
[0070] Besides, the present invention is not limited by the above-mentioned embodiment. For example, although driving force transmission to the ADU rollers 13 , 14 , and 15 is performed via the one-way clutches 23 , 24 , and 25 in the above-mentioned embodiment, other sorts of clutches may also be used. However only, in that case, it is necessary to additionally perform a new clutch control by using the CPU 32 .
[0071] Moreover, although it is assumed that three ADU rollers 13 , 14 , and 15 are provided to the paper side reversal section 104 , and the one-way clutches 23 , 24 , and 25 are provided to all of these three ADU rollers 13 , 14 , and 15 in the above-mentioned embodiment, a number of the rollers provided to the paper side reversal section 104 may be an optional, and moreover, it is sufficient that the one-way clutches are provided only to the rollers having a possibility to nip and hold the paper that is kept at the paper side reversal section 104 .
[0072] Moreover, factors such as the position relations of various sorts of roller or various sorts of sensor, or a shape of the paper carry route can optionally be changed as long as it does not mar the original function, and the concrete timings for the paper carry are to be changed in accordance with these functional structures.
[0073] Moreover, although there is shown an example in which the image forming apparatus according to the present invention is applied to the electrophotographic apparatus in the above-mentioned embodiment, a method of the image formation may be optional, and the present invention is not limited to the application to the electrophotographic apparatus.
[0074] 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 embodiments 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. | Return roller and carry roller are rotated by one drive source. To the carry roller which nips and holds paper when the paper is held, a driving force of the drive source is transmitted by a clutch only when the return roller carries out the paper toward a return direction. There is controlled paper carry by repeating a step of feeding an n-th sheet of paper on which the image formation on one side is completed to an image formation section, and feeding an n+l-th sheet of paper to a paper side reversal section, and a step of, under the state where the n+1-th sheet of paper is held at the paper side reversal section, ejecting the n-th sheet of paper on which the image formation on both sides is completed, and feeding an n+2-th sheet of paper to the return section. | 6 |
BACKGROUND OF THE INVENTION
The invention is based on a valve as generically defined hereinafter. German Offenlegungsschrift No. 35 01 973 discloses a valve having the disadvantage that despite reducing the size of the surfaces of the armature and stop that strike one another, a substantial reduction in the armature mass is still unattainable, and upon armature actuation a large surface area must be moved counter to the fluid, resulting in undesirable delays in the closing or opening movement of the valve.
This application is an improvement of U.S. Pat. No. 4,733,822, granted Mar. 29, 1988, which is assigned to the assignee of this application.
OBJECT AND SUMMARY OF THE INVENTION
The valve having the armature embodied according to the invention has the advantage over the prior art that a reduction in the armature mass and of the armature surface area that must be moved through the medium is attainable while maintaining adequate rigidity, resulting in faster armature actuation and hence shorter valve opening and closing times.
It is advantageous if each stop lobe protrudes axially beyond the tooth surface and is narrower than a tooth.
It is also advantageous to produce the flat armature from soft magnetic material by sintering.
The invention will be better understood and further objects and advantageous thereof will become more apparent from the ensuing detailed description of a preferred embodiment taken in conjunction with the drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a fragmentary cross-sectional view of a fuel injection valve provided with an armature according to the invention;
FIG. 2 is a top plan view on an armature according to the invention; and
FIG. 3 is a section taken along the line III--III of FIG. 2.
DESCRIPTION OF THE PREFERRED EMBODIMENT
The fuel injection valve for a fuel injection system which is shown by way of example in FIG. 1 serves for instance to inject fuel into the intake tube of mixture-compressing internal combustion engines having externally supplied ignition. A liner 2 of ferromagnetic material is secured in a cylindrical, ferromagnetic valve housing and simultaneously acts as the core. A cylinder 3 is positioned within the liner 2 and is guided inside the liner 2 in the portion of the valve that is not shown. Between the cylinder 3 and the liner 2 there is an annular gap 4, through which the valve is vented. An insulating holder body 8 is mounted on the outside diameter of the liner 2, in the interior 7 of the valve housing 1 between the liner 2 and the valve housing 1; the holder body 8 at least arranged to partly surround a magnetic coil 9 disposed coaxially with the valve housing 1 and liner 2. The holder body 8 and magnetic coil 9 are surrounded by an insulator 10 and are secured on the valve housing 1 by means of an element, not shown but made of the same material as the insulator 10. Inside the element, and again not shown in the drawing, there is an electric connection line leading to the magnetic coil 9. An annular gap 14, through which the fuel flow enters, is left between the outside diameter of the insulator 10 and the housing bore 13 surrounding the interior 7 of the valve housing 1. A spacer ring 18 rests on an end face 17 of the valve housing 1 oriented toward the intake manifold of the engine, and the spacer ring 18 is adjoined by a guide diaphragm 19. The other side of the guide diaphragm 19 is engaged by a collar 22 of a nozzle holder 23, which partly surrounds the valve housing 1 and is crimped at 24 to the valve housing 1, thereby exerting an axial clamping force for the positional fixation of the spacer ring 18 and guide diaphragm 19. Remote from the valve housing 1, the nozzle holder 23 has a coaxial receiving bore 28, into which a nozzle body 29 is inserted and secured, for instance by welding or soldering. The nozzle body 29 has a preparation bore 30, for instance of frustoconical shape, opening in the direction remote from the valve, and at least one fuel guide bore 32 which serves to meter fuel discharged at the bottom 3 of the preparation bore 30. To make the fuel more turbulent, the fuel guide bore 32 may discharge onto the bottom 31 at a tangent. The fuel guide bores 32 begin at a spherical chamber 35 formed in the nozzle body 23, upstream of which a circular valve seat 36 is formed in the nozzle body 29, with a valve closing element 37 of approximately hemispherical shape being arranged to cooperate with the valve seat 36.
Remote from the valve seat 36, the valve closing element 37 is connected to a flat armature 38. The flat armature 38 has an annular ring 41, which is axially raised toward the valve seat 36 and rests on the side of the guide diaphragm 19 remote from the valve seat 36. Flow apertures 44 in the guide diaphragm 19 enable an unhindered flow of fuel around the flat armature 38 and the guide diaphragm 19. The guide diagram 19, which is fastened integrally with the housing on its outer circumference, between the spacer ring 18 and the collar 22 of the nozzle holder 23, ha a centering opening 47, through which the movable valve closing element 37 protrudes and by which this element is guided in the radial direction. The fastening of the guide diaphragm 19 integrally with the housing between the spacer ring 18 and the collar 22 of the nozzle holder 23 is effected in a plane which, when the valve closing element 37 is resting on the valve seat 36, passes through the center, or as close as possible to the center, of the ball-like valve closing element. By means of the guide diaphragm 19 resting on the ring 41 of the flat armature 38, the flat armature 38 is guided as nearly parallel as possible to the end face 17 of the valve housing 1, the flat armature 38 being adapted to protrude somewhat beyond this end face 17 with an outer magnetic zone 48. A second magnetic zone exists between the end face 52 of the liner 2 and the flat armature 38. When current is flowing through the magnetic coil, the flat armature 38 rests with its outer magnetic zone 48 on the end face 17 of the valve housing 1, while between the flat armature 38 and the end face 52 of the liner 2 a gap 53 remains. A compression spring 59 is supported in an indentation bore 56 in the valve closing element 37 and on the other end is supported on a step 57 of the cylinder 3, being centered by a protruberance 58 formed on the cylinder 3.
As also shown in FIGS. 2 and 3, the flat armature 38 is embodied in the form of a gear wheel and has at least three teeth 62, extending radially outward from the ring 41. In the exemplary embodiment shown, eight teeth 62 are provided. Between the teeth 62, tooth gaps 63 are provided, which like the teeth 62 are virtually rectangular in cross section. A stop lobe 64 of relatively large surface area is provided on each tooth 62, and like the teeth 62, these stop lobes 64 are located in the outer magnetic zone 48 of the flat armature 38, and being oriented toward the end face 17 of the valve housing 1 and are adapted to rest on the end face 17 when the magnetic coil 9 is excited. The stop lobes 64 of the flat armature 38 terminate at the same height, or in other words all terminate in a single plane. Each of the stop lobes 64 which protrude beyond the tooth surface 65 extends radially inward from the end face 66 of a given tooth 62 and is narrower than that tooth. A central face 68 extends from the annular ring 41 on the side oriented toward the valve seat 36, remote from the teeth 62; the valve closing element 37 is arranged to rest on this central face 68 and is secured to it, for example by welding. The central face 68 is interrupted by a central bore 69, through which the compression spring 59 protrudes. On the surface of the flat armature remote from the valve seat 36, there is a radially extending reinforcement rib 70 oriented toward each tooth 62 and spanning the ring 41. Advantageously, the flat armature 38 is made from soft magnetic material by sintering.
Because of its gear-wheel-like shape, the flat armature 38 embodied according to the invention has the advantage that the large tooth gaps 63 provided between the teeth 62 reduce the mass of the flat armature substantially, while lending it sufficient strength, and at the same time the medium to be controlled can flow around the flat armature sufficiently well upon a movement of the flat armature, thus assuring very fast actuation of the flat armature and hence of the valve wheel like device. In the claims reference is made to the gear wheel-like device having a root area 63 and the teeth 62 having opposed flank portions all of which is considered clearly shown from the plan view of FIG. 2.
The foregoing relates to a preferred exemplary embodiment 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. | In valves having flat armatures, in order to attain the shortest possible switching times, the goal is to to reduce the mass of the armature and the surface area of the stops. A particularly advantageous design is obtained by embodying the flat armature in the manner of a gear wheel and providing at least three radially extending teeth, spaced uniformly apart from one another, on which the stop lobes that cooperate with a stop integral with the housing upon actuation of the valve by excitation of the magnetic coil are formed. A flat armature embodied in this way can be used in any correspondingly embodied valve. | 8 |
CROSS-REFERENCE TO RELATED APPLICATIONS
This application claims the benefit of priority from U.S. Provisional Application No. 60/943,397, filed Jun. 12, 2007, the disclosure of which is hereby incorporated in its entirety by reference thereto.
TECHNICAL FIELD
Embodiments of the present invention relate to syringe assemblies having a passive locking mechanism which restricts distal movement of the plunger rod after injection to prevent reuse, syringe assemblies wherein the stopper and plunger rod operate using relative motion to passively disable the syringe, syringe assemblies including a removeably connected stopper and plunger rod to prevent disassembly of the syringe prior to use and syringe assemblies including visual indication or markings to indicate use of the syringe or a disabled syringe.
BACKGROUND
Reuse of hypodermic syringe products without sterilization or sufficient sterilization is believed to perpetuate drug abuse and facilitate the transfer of contagious diseases. The reuse of syringes by intravenous drug users further exacerbates the transfer of contagious diseases because they comprise a high-risk group with respect to certain viruses such as the AIDS virus and hepatitis. A high risk of contamination also exists in countries with shortages of medical personnel and supplies.
A syringe which can be rendered inoperable after use presents a viable solution to these issues. Various syringes have been proposed and are commercially available that can be disabled by the user by taking active steps to disable the syringe. Single-use syringes that do not require the user to actively disable the syringe are also thought to offer a solution. It would be desirable to provide syringes that are automatically or passively disabled from reuse and can be manufactured in a cost-effective manner by, for example, utilizing fewer parts. Further, markings or other indicators which visually indicate whether a syringe has been used or is disabled would also be desirable.
SUMMARY
A passive disabling system for a syringe assembly that activates after completion of an injection cycle is provided. A syringe assembly incorporates a stopper and plunger rod attached in a manner to prevent users from disassembling the syringe prior to completion of the injection cycle. In one or more embodiments of the invention, a user can fill, inject and/or reconstitute medication.
In this disclosure, a convention is followed wherein the distal end of the device is the end closest to a patient and the proximal end of the device is the end away from the patient and closest to a practitioner.
A syringe assembly is provided which includes a barrel, an elongate plunger rod and stopper having respective structures and assembly which allow the user to passively lock the plunger rod within the barrel to prevent reuse of the syringe assembly. The barrel includes a distal end, an open proximal end, a cylindrical sidewall, which defines a chamber in which fluid may be held, and a distal wall. An opening in the distal wall permits fluid to flow from the chamber through the opening. In one embodiment, the barrel includes a marker or indicator which indicates whether the syringe has been disabled or the plunger has been locked within the barrel.
In one or more embodiments, the sidewall of the barrel has a continuous diameter or first inner diameter. As used throughout this application, the term “diameter” is a measurement of the longest distance between the walls of the barrel having any cross-sectional shape. However, it will be appreciated that conventional syringes are typically cylindrical with a circular cross-sectional shape. In accordance with some embodiments of the present invention, the barrel includes a rib, locking rib or other such impediment suitable for restricting the proximal movement of the plunger rod, adjacent to its proximal end. In one embodiment, the rib has a second inner diameter, wherein the second diameter is less than the first diameter. One or more embodiments of the present invention include an increased diameter region located proximally from the rib having a third inner diameter, wherein the third diameter is greater than the first diameter and second diameter. A diameter transition region having an axial length located between the rib and the increased diameter region may be included. The diameter transition region can have a varying inner diameter, which increases in the proximal direction.
Embodiments of the present invention also include an extended plunger rod which has a proximal end, a distal end, and a main body between the proximal and distal end. In some embodiments, the plunger rod slides or otherwise moves proximally and distally within the chamber of the barrel.
The distal end of the plunger can include a stopper-engaging portion having a distal and proximal end. The stopper-engaging portion provides a means for the stopper and plunger rod to move proximally and distally within the barrel. The stopper-engaging portion allows the stopper and plunger rod to move proximally and distally relative to each other. In a specific embodiment, the stopper-engaging portion may include a rim at its distal end, or a retainer or alternate means suitable for restraining the stopper.
The stopper-engaging portion according to one or more embodiments may also include a visual indicator or a visual display that indicates use of the syringe or whether the syringe is disabled.
The plunger rod can further include means for locking the plunger rod in the barrel to prevent reuse of the syringe assembly when the syringe is fully injected or “bottomed.” The means can have an outer diameter greater than the inner diameter of the barrel at the rib or the second inner diameter. As used herein, the term “bottomed” shall refer to the position of the syringe assembly wherein the stopper, while attached to the plunger rod, is in contact with the distal wall of the barrel and the plunger rod can no longer move in the distal direction.
One or more embodiments of the present invention utilize a protrusion, or annular protrusion that extends radially from the plunger rod. In some embodiments, the protrusion is located between the thumb press and the main body, as an example of a means for locking the plunger rod in the barrel. According to an embodiment of the invention, the protrusion is integrally molded to the plunger rod.
In one configuration, the protrusion has an outer diameter greater than the second inner diameter. Once the protrusion distally moves through the diameter transition region, past the rib and into the barrel, it becomes locked by the rib, thereby preventing proximal movement of the plunger rod. The protrusion of one embodiment is tapered or otherwise shaped in such a manner such that it may move in the distal direction past the rib more easily.
The plunger rod can further comprise at least one frangible portion for separating a portion of the plunger rod from the body. In this configuration, when a user attempts to reuse the syringe assembly or otherwise pull the plunger in the proximal direction out of the barrel, after the plunger rod has been locked, the plunger rod breaks at the frangible portion, leaving a portion of the plunger rod locked within the barrel. In a specific embodiment, the frangible portion is located between the protrusion and the thumb press.
The stopper has a proximal end and a distal end and the stopper is attached the stopper-engaging portion of the plunger rod. In some embodiments, the stopper moves distally and proximally within the barrel. The stopper also moves distally and proximally along a pre-selected axial distance relative to the stopper-engaging portion of the plunger rod, thereby allowing the protrusion to move distally past the rib into the locked position, when the syringe assembly is bottomed.
The stopper may further comprise a stopper body or stopper boss at the proximal end of the stopper. A peripheral lip may be included at the proximal end of the stopper body. A frangible connection may be provided to connect the stopper to the plunger rod, which may connect the stopper and the peripheral lip.
The stopper-engaging portion of the plunger rod and the stopper may be connected in a manner such that when the user applies a force in the proximal direction for aspiration or filling the syringe, the stopper remains stationary until plunger rod moves in the proximal direction the length of the pre-selected axial distance. In one embodiment, when a user continues to aspirate or fill the syringe assembly, the stopper begins to move in the proximal direction in tandem with the plunger rod, after the plunger rod has traveled the pre-selected axial distance in the proximal direction. An optional visual indicator or display disposed on the stopper-engaging portion of the plunger rod is visible when the user fills the syringe assembly.
In one or more embodiments of the present invention, when a user injects the contents of the syringe assembly, the attachment of the stopper and the stopper-engaging portion allow the plunger rod to move distally for a length of the pre-selected axial distance, while the stopper remains stationary. After the plunger rod travels distally for the length of the pre-selected axial distance, the stopper begins to move distally with the plunger rod. During such distal movement, where a visual indicator or display is utilized, the visual indicator or display disposed on the stopper-engaging portion of the plunger rod is no longer visible. Where a visual marker is utilized, the visual marker disposed on the barrel continues to be visible, even after the plunger rod is locked. As will be more fully described herein, the marker provides an alternative means of indicating the syringe has been disabled.
According to one embodiment of the present invention, the total length of the plunger rod is decreased by pre-selected axial distance when the stopper and plunger rod move together in the distal direction during injection of the contents of the syringe assembly. As such, the stopper and stopper-engaging portion of the syringe assembly are attached in a manner such that when a user has fully completed the injection cycle, the protrusion of the plunger rod advances past the rib of the barrel. In some embodiments, once the protrusion advances past the rib of the barrel, it locks the plunger rod within the barrel and prevents the user from reusing the syringe assembly or otherwise pulling the plunger rod out of the barrel. Once the plunger rod is locked within the barrel, the optional visual indicator or display on the stopper-engaging portion of the plunger rod is no longer visible, indicating the syringe has been disabled.
The syringe assembly may include one or more frangible portions of the plunger rod, which break when a user attempts to move the plunger rod in a proximal direction after the protrusion has advanced past the rib of the barrel. Other suitable means may be utilized for separating a portion of the plunger rod from the main body when the user applies sufficient proximal force to the plunger rod or otherwise attempts to reuse the syringe assembly after it is bottomed.
In accordance with one embodiment of the invention, the stopper and the stopper-engaging portion are attached in such a manner such that when a user attempts to disassemble the syringe assembly prior to aspiration, injection or bottoming, the stopper-engaging portion disengages from the stopper, leaving the stopper inside the barrel and allowing the separated plunger rod to be removed. In some embodiments, inner diameter of the barrel at the rib, or the second inner diameter, is less than the outer diameter of the stopper, and thereby prevents the stopper from moving proximally past the rib and causes the stopper-engaging portion to detach from the stopper, leaving the stopper inside the barrel. An optional frangible connection of the stopper breaks when a user attempts to disassemble the syringe assembly by applying a continuous force in the proximal direction to the plunger rod prior to aspiration, injection or bottoming.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 illustrates a perspective view of a syringe assembly according to an embodiment of the invention shown;
FIG. 2 illustrates a disassembled perspective view of a syringe assembly according to an embodiment of the invention;
FIG. 3 shows a cross-sectional view of the barrel shown in FIG. 2 taken along line 3 - 3 ;
FIG. 4 is an enlarged view of a portion of the barrel shown in FIG. 3 ;
FIG. 5 is a cross-sectional view of the stopper shown in FIG. 2 taken along line 5 - 5 ;
FIG. 6 is a cross-sectional view of the plunger rod shown in FIG. 2 taken along line 6 - 6 ;
FIG. 7 is a cross-sectional view taken along line 7 - 7 of FIG. 1 ;
FIG. 8 is an illustration of FIG. 7 showing the plunger rod being moved in the proximal direction;
FIG. 9 is an illustration of FIG. 8 showing the plunger rod being moved in the distal direction;
FIG. 10 is an illustration of FIG. 9 showing the plunger rod in a locked position in the syringe barrel;
FIG. 11 is an enlarged view of a proximal portion of the assembly shown in FIG. 10 ;
FIG. 12 illustrates a perspective view of an embodiment of a syringe assembly having a visual marker disposed on the barrel;
FIG. 13 illustrates a disassembled perspective view of an embodiment of a syringe assembly visual indicators or markers disposed on the barrel and the stopper-engaging portion of the plunger rod;
FIG. 14 is a cross-sectional view taken along line 14 - 14 of FIG. 12 ;
FIG. 15 is an illustration of FIG. 14 showing the plunger rod in a locked position in the syringe barrel;
FIG. 16 is an enlarged view of a proximal portion of the assembly shown in FIG. 15 ;
FIG. 17 is an illustration of FIG. 10 showing a proximal portion of the plunger rod being broken from the syringe assembly after the plunger rod has been locked in the syringe barrel;
FIG. 18 is an illustration of FIG. 7 showing the plunger rod being moved in the proximal direction and the stopper disengaging from the plunger rod;
FIG. 19 a disassembled perspective view of a syringe assembly according to another embodiment of the invention;
FIG. 20 is a perspective view of the plunger rod shown in FIG. 19 ;
FIG. 21 is a side elevational view of the stopper shown in FIG. 19 ;
FIG. 22 is a cross-sectional view taken along line 22 - 22 of the syringe assembly shown in FIG. 19 ;
FIG. 23 is an illustration of FIG. 22 showing the plunger rod being moved in the proximal direction;
FIG. 24 is an illustration of FIG. 23 showing the plunger rod being moved in the distal direction;
FIG. 25 is an illustration of FIG. 24 showing the plunger rod in a locked position in the syringe barrel;
FIG. 26 is an illustration of FIG. 25 showing a proximal portion of the plunger rod being broken from the syringe assembly after the plunger rod has been locked in the barrel; and
FIG. 27 is an illustration of FIG. 22 showing the plunger rod being moved in the proximal direction and the stopper disengaging from the plunger rod.
DETAILED DESCRIPTION
Before describing several exemplary embodiments of the invention, it is to be understood that the invention is not limited to the details of construction or process steps set forth in the following description. The invention is capable of other embodiments and of being practiced or being carried out in various ways.
One aspect of the present invention provides for a syringe assembly including a barrel, plunger rod and stopper having individual features and construction which allow the user to passively lock the plunger rod within the barrel to prevent reuse of the syringe assembly.
FIG. 1 shows a syringe assembly 100 according to one or more embodiments. As shown in FIG. 2 , the syringe assembly includes a barrel 120 , a plunger rod 140 and a stopper 160 , arranged such that the proximal end 169 of stopper is attached to the distal end 141 of the plunger rod. The connected stopper 160 and plunger rod 140 are inserted into the proximal end 129 of the barrel 120 .
As best shown in the FIG. 3 , the barrel 120 has a cylindrical sidewall 110 with an interior surface 126 that defines a chamber 128 . In one embodiment, the chamber 128 holds the contents of the syringe assembly which may include medication in powdered or fluid form. The barrel 120 is shown as having an open proximal end 129 , a distal end 121 , and a distal wall 122 . The distal wall 122 has an opening 111 in fluid communication with the chamber 128 .
The sidewall 110 of the barrel 120 defines a chamber having a continuous inner diameter along the longitudinal axis of the syringe. Alternatively, the barrel can include a sidewall has an inner diameter, which decreases linearly from the proximal end to the distal end. It is to be understood that the configuration shown is merely exemplary, and the components can be different in shape and size than shown. For example, the barrel can have an exterior prism shape, while retaining a cylindrical interior shape. Alternatively, both the exterior and interior surfaces of the barrel can have non-circular cross-sectional shapes.
The syringe barrel 120 is shown as having a peripheral flange 124 attached at the proximal end 129 of the barrel 120 . The barrel 120 further includes a needle cannula 150 , having a lumen 153 attached to the opening 111 in the distal wall 122 of the barrel 120 . As is known in the art, attachment means 152 is provided for attaching the needle cannula 150 to the distal wall 122 . The assembly 100 may also include a protective cap over the needle cannula (not shown).
As shown more clearly in FIG. 4 , the barrel 120 further includes a rib 123 adjacent its proximal end 129 . The inner diameter of the barrel at the location of the rib 123 is smaller than the inner diameter of the barrel 120 at other locations along the length of the barrel. One or more optional tabs or detents can be used to create a region of the barrel having a diameter smaller than the inner diameter of the barrel 120 . In a specific embodiment, the rib can include a ring formed along entire circumference of the interior surface 126 or a portion of the interior surface 126 of the inner diameter of the barrel 120 (not shown). The barrel 120 also includes a diameter transition region 127 adjacent to the rib 123 at the proximal end 129 of the barrel 120 . The inner diameter of the barrel at the diameter transition region 127 increases from the distal end 121 to the proximal end 129 of the barrel 120 . In the embodiment shown, the barrel includes an increased diameter region 125 adjacent to the diameter transition region at the proximal end 129 of the barrel. The inner diameter of the barrel 120 at the increased diameter region 125 is greater than the inner diameter of the barrel of the entire diameter transition region 127 .
The barrel may be made of plastic, glass or other suitable material. The barrel further includes optional dosage measurement indicia (not shown).
Referring now to FIG. 5 , the stopper 160 has a distal end 161 , a proximal end 169 , a stopper body 164 and a peripheral edge 162 which forms a seal with the interior surface 126 of the barrel. In one or more embodiments, the peripheral edge 162 of the stopper 160 has a larger diameter than the diameter of the interior surface of the rib 123 . The stopper 160 shown in FIG. 5 includes an optional elongate tip 166 on its distal end 161 to facilitate reduction of the residual fluid and expulsion of fluid from the syringe barrel.
The stopper 160 is shown as further having a tapered portion 165 adjacent to the stopper body 164 at its proximal end 169 . A neck 163 is adjacent to the tapered portion 165 at the proximal end 169 of the stopper 160 . The stopper body 164 is shown as also including an interior recess 168 , which allows the stopper-engaging portion 146 of the plunger rod 140 to connect to the stopper 160 . A peripheral rim 147 may be provided to help retain the stopper 160 on the plunger rod 140 . As with the rib of the barrel, detents or tabs can be used to retain the stopper 160 on the plunger rod 140 .
The stopper is typically made of plastic or other easily disposable and/or recyclable material. It may be desirable to incorporate natural or synthetic rubber in the stopper or use a natural or synthetic rubber seal with the stopper. It will be understood that the stopper may incorporate multiple seals.
Referring now to FIG. 6 , the syringe assembly includes a plunger rod 140 having a proximal end 149 , a distal end 141 , and a main body 148 extending between the proximal end 149 and distal end 141 . The plunger rod 140 further includes a thumb press 142 at the proximal end 149 of the plunger rod 140 . In the embodiment shown, the thumb press 142 further includes a textured surface, writeable surface and/or label.
Still referring to FIG. 6 , the plunger rod 140 further includes a protrusion 144 shown as an annular protrusion 144 between the thumb press 142 and the main body 148 . The outer diameter of the plunger rod at the protrusion 144 is greater than the inner diameter of the barrel 120 at the rib 123 . In some embodiments of the invention, the protrusion 144 includes a tapered portion 145 that facilitates distal movement of the protrusion past the rib 123 and into the barrel 120 , as will become apparent in the subsequent discussion of operation of the syringe. In at least one embodiment, the syringe assembly is configured to allow the protrusion 144 to advance distally past the rib 123 , to lock the plunger rod in the barrel when the user bottoms out the plunger rod in the barrel (as more clearly shown in FIGS. 10-11 ). In certain embodiments, the plunger rod 140 further includes at least one frangible connection or point 143 for separating at least a portion of the plunger rod from the main body when a user applies sufficient proximal force to the plunger rod after it has been locked. In the embodiment shown, the frangible point 143 is located between the protrusion 144 and the thumb press 142 . It will be understood that the frangible connection or point 143 shown is exemplary, and other suitable means for permanently damaging the plunger rod or otherwise separating at least a portion of the plunger rod from the main body may be provided.
In the embodiment shown, the stopper 160 is permitted to move distally and proximally within the barrel when connected to the stopper-engaging portion 146 of the plunger rod 140 . As will be understood better with the description of operation of the syringe assembly and with reference to FIG. 7 , the stopper is capable of moving distally and proximally a pre-selected axial distance 132 relative to the stopper-engaging portion.
The plunger rod may be made of plastic or other suitable material. The protrusion may also be comprised of plastic or a harder material suitable for locking the plunger rod within the barrel.
In FIG. 7 , the barrel 120 holds the stopper 160 and plunger rod 140 in the chamber, wherein the stopper is bottomed, “parked” or is in contact with the distal wall 122 of the barrel 120 . The peripheral edge of the stopper 162 forms a seal with the interior surface 126 of the barrel 120 . In one embodiment, the stopper 160 is connected to the stopper-engaging portion 146 of the plunger rod 140 . The stopper-engaging portion 146 is removeably held in the recess 168 of the stopper body 164 by the neck 163 .
In FIG. 7 , a gap between stopper 160 and the distal end of the main body 148 defines a pre-selected axial distance 132 prior to the injection cycle. In at least one embodiment, the protrusion 144 remains on the proximal side of the rib 123 because the length of the plunger rod 140 and stopper combined, along with the pre-selected axial distance 132 , is greater than the length of the barrel 120 from the distal wall 122 to the proximal end of the barrel 120 . The distance between the protrusion 144 and the peripheral edge 162 of the stopper body 164 defines a first distance, D 1 .
FIG. 8 illustrates the syringe assembly in use and specifically shows an aspiration or filling step, according to one or more embodiments of the present invention. When the user applies a force to the plunger rod 140 in the proximal direction shown by the arrow in FIG. 8 , the plunger rod 140 and the stopper 160 move together in the proximal direction, while the stopper-engaging portion 146 is connected to the stopper 160 by the rim 147 . In one or more embodiments, the gap defining the pre-selected axial distance 132 is maintained while the stopper 160 and plunger rod 140 move together in the proximal direction along the interior surface of the syringe barrel. The user terminates the application of proximal force on the plunger rod 140 once the desired amount of medicament is drawn into the syringe. During the aspiration step, the plunger rod and the stopper body move in the proximal direction together to draw medication into the syringe, while maintaining the first distance D 1 .
FIG. 9 also shows the syringe assembly in use and specifically demonstrates application of distal force to the plunger rod during injection. In one embodiment, when the user applies a force in the distal direction to the plunger rod 140 as indicated by the arrow, the plunger rod 140 moves in a distal direction for the length of the gap defining the pre-selected axial distance 132 in FIG. 7 , while the stopper 160 remains stationary. The stopper 160 remains stationary because the frictional force created by the peripheral edge 162 of the stopper on the interior surface 126 of the barrel is greater than the frictional force created by the stopper-engaging portion 146 entering the recess 168 of the stopper 160 . Consistent with at least one embodiment, once the stopper-engaging portion has distally moved the length of the pre-selected axial distance 132 and is in contact with the proximal end of the recess 169 , the stopper 160 and the plunger rod 140 begin to move in tandem in the distal direction. Further, the force applied by the user is greater than the friction between the peripheral edge 162 of the stopper 160 and the interior surface 126 of the barrel, and therefore the stopper 160 is forced to move in the distal direction with the plunger rod 140 . In one embodiment, the user may inject a limited amount of the fluid aspirated or exert a limited force on the plunger rod in the distal direction to flush or expel some of the aspirated fluid, without locking the plunger rod, provided that the syringe assembly is not bottomed. However, as will be described further with respect to FIG. 10 , a user may bottom the stopper against the distal wall of the syringe barrel, locking the plunger rod in the barrel.
When expelling the contents of the syringe, the plunger rod moves in a distal direction the length of the pre-selected axial distance 132 shown in FIG. 7 while the stopper body remains stationary, consequently closing the gap defining the pres-selected axial distance 132 . After the contents of the syringe have been fully expelled, the distance between the protrusion 144 and the peripheral edge 162 defines a second distance, D 2 , wherein D 2 is the difference between the first distance, D 1 , and the gap defining a pre-selected axial distance 132 .
FIG. 10 illustrates an embodiment of the syringe assembly after the plunger rod has been locked inside the barrel. In one or more embodiments, the entry of the stopper-engaging portion into the recess 168 of the stopper 160 (as also shown in FIG. 9 ) closes the gap defining the pre-selected axial distance 132 , allowing the protrusion 144 to advance past the locking rib 123 (as more clearly shown in FIG. 11 ). The protrusion 144 has an outer diameter greater than the inner diameter of the barrel at the rib 123 . Accordingly, in one or more embodiments, the rib 123 locks the protrusion 144 inside the barrel 120 , and prevents proximal movement of the plunger rod 140 .
FIG. 12 shows a syringe assembly 100 in which the barrel 120 includes a visual marker 300 . The marker is aligned with the rib 123 , as more clearly shown in FIG. 16 . The marker can be integrally formed on the sidewall of the barrel or can be added to the exterior surface of the sidewall. The marker can be printed in ink, adhesively applied, a textured surface or a separate piece that is fixed around the syringe barrel. The marker can form a ring around the circumference of the side wall or be in the form of tabs disposed at regular intervals around the circumference of the side wall. In a specific embodiment, the marker is a colored stripe. In a more specific embodiment, the marker can include text in the form of one or more letters and/or numbers, geometric shapes, symbols or combinations thereof to inform users the syringe is disabled.
FIG. 13 shows a plunger rod 140 having a visual indicator or display 310 disposed on the stopper-engaging portion 146 . As with the visual marker 300 , the visual indicator 310 can be integrally formed with the stopper-engaging portion of the plunger rod or be added to the exterior surface thereof. The indicator or display can be printed in ink, adhesively applied, a textured surface or a separate piece that is fixed to the stopper engaging portion. In one or more embodiments, the indicator or display can comprise a pattern, a solid portion and or can cover the entire surface of the stopper-engaging portion. In a specific embodiment, the indicator is a colored stripe disposed along the length of the stopper-engaging portion 146 between the distal end 141 and the main body 148 of the plunger rod. In a more specific embodiment, the indicator is a colored stripe disposed along the circumference of the stopper-engaging portion 146 of the plunger rod. In an even more specific embodiment, the marker can include text in the form of one or more letters and/or numbers, geometric shapes, symbols or combinations thereof.
As more clearly shown in FIG. 14 a gap between stopper 160 and the distal end of the main body 148 defines a pre-selected axial distance 132 prior to the injection cycle. The visual indicator 310 is visible when the gap is present. The visual marker 300 is disposed on the exterior surface of the barrel 120 and aligned with the rib 123 . As described with reference to FIG. 8 , when the user applies a force to the plunger rod 140 in the proximal direction shown by the arrow in FIG. 8 , the plunger rod 140 and the stopper 160 move together in the proximal direction, while the stopper-engaging portion 146 is connected to the stopper 160 by the rim 147 . In one or more embodiments, the gap defining the pre-selected axial distance 132 is maintained while the stopper 160 and plunger rod 140 move together in the proximal direction along the interior surface of the syringe barrel. Accordingly, the visual indicator 310 continues to be visible.
As described with reference to FIG. 9 , when expelling the contents of the syringe, the plunger rod moves in a distal direction the length of the pre-selected axial distance 132 shown in FIGS. 7 and 14 while the stopper body remains stationary, consequently closing the gap defining the pre-selected axial distance 132 . The movement of the stopper-engaging portion, in the distal direction relative to the stopper allows the stopper-engaging portion 146 of the plunger rod to move into the recess 168 of the stopper (as shown in FIG. 9 ). As can be more clearly seen in FIG. 15 , this relative movement allows the stopper body 164 covers the stopper-engaging portion and blocks visibility of the visual indicator 310 .
As more clearly shown in FIGS. 15 and 16 , the visual marker 300 disposed on the barrel 120 and aligned with the rib 123 also shows advancement of the protrusion 144 past the rib 123 . In addition, the entry of the stopper-engaging portion into the recess 168 of the stopper 160 (as also shown in FIG. 9 ) also closes the gap defining the pre-selected axial distance 132 , allowing the protrusion 144 to advance past the rib 123 (as more clearly shown in FIGS. 11 and 16 ). The location of the protrusion relative to the visual marker indicates whether the plunger rod has been locked within the barrel and the syringe assembly has been disabled. Before the plunger rod is locked, the protrusion 144 is proximally adjacent to the visual marker 300 . Once the plunger rod is locked, the protrusion 144 is distally adjacent to the visual marker 300 .
It will be appreciated that each of the visual marker 300 and the visual indicator 310 can be used alone or in combination.
FIG. 17 shows the assembly after the plunger rod 140 has been locked in the barrel 120 . An attempt to reuse the syringe assembly by applying a force to the plunger rod 140 in the proximal direction causes a portion of the plunger rod 140 to separate at the frangible connection or point 143 . The frangible connection or point 143 is designed so that the force holding exerted on the protrusion by the locking rib 123 while proximal force is being applied to the plunger rod 140 is greater than the force needed to break the plunger rod at the frangible point 143 and, therefore, the frangible point breaks or separates before the user is able to overcome the force exerted on the protrusion by the rib.
FIG. 18 shows the syringe assembly in a configuration in which the stopper 160 has separated from the stopper-engaging portion 146 . According to one or more embodiments of the invention, the stopper 160 and stopper-engaging portion 146 disengage to prevent a user from disassembling the parts of the syringe assembly prior to use. As otherwise described in reference to FIG. 5 , the peripheral edge 162 of the stopper 160 has a diameter greater than the diameter of the interior surface of the rib 123 . Consistent with at least one embodiment of the invention, when a user applies a force to the plunger rod 140 in the proximal direction, the rib 123 locks the peripheral edge 162 of the stopper 160 , and the rim 147 of the stopper-engaging portion 146 disconnects from the neck 163 of the stopper. The rib 123 exerts a greater force on the peripheral edge of the stopper than the force or friction exerted by the rim of the stopper-engaging portion of the plunger rod and neck portion of the stopper while proximal force is applied to the plunger rod.
FIG. 19 shows an example of a syringe assembly according to another embodiment of the present invention. In the embodiment shown in FIG. 19 , the assembly includes a barrel 220 , a plunger rod 240 and a stopper 260 , arranged so that the proximal end of stopper 269 is attached to the distal end of the plunger rod 241 . The stopper 260 then plunger rod 240 is inserted into the proximal end of the barrel 229 . A flange 224 is attached at the proximal end 229 of the barrel 220 . The barrel 220 further includes a needle cannula 250 having a lumen 253 , attached to the opening in the distal wall 222 at the distal end 221 of the barrel 220 . One or more embodiments also include an attachment hub 252 for attaching the needle cannula 250 to the distal wall 222 . The assembly may also include a protective cap over the needle cannula (not shown).
Similar to the barrel illustrated previously in FIGS. 3 and 4 , and as shown in FIG. 22 , the barrel further include a rib 223 , locking rib or other means for locking the plunger rod within the barrel, having an interior surface with a smaller diameter than the diameter of the interior surface of the barrel.
Referring now to FIG. 20 , a perspective view of a plunger rod 240 is shown as having a main body 248 , a distal end 241 and a proximal end 249 . The plunger rod 240 further includes a thumb press 242 at its proximal end and a stopper-engaging portion 246 at its distal end. Plunger rod 240 also includes a protrusion in the form of an annular protrusion 244 between the thumb press 242 and the main body 248 . The protrusion 244 may include a tapered portion 245 to facilitate distal movement of the protrusion 244 past the rib 223 into the barrel 220 . In some embodiments, the protrusion 244 has an outer diameter greater than the inner diameter of the barrel at the rib 223 . In at least one embodiment, the configuration of the syringe assembly allows for the protrusion 244 to advance distally past the rib 223 , to lock the plunger rod 240 in the barrel 220 , when the user bottoms the syringe assembly (as more clearly shown in FIGS. 25-26 and discussed further below).
The plunger rod 240 shown further includes at least one frangible point 243 . In the embodiment shown, the frangible point 243 of the plunger rod 240 is located between the protrusion 244 and the thumb press 242 , but the frangible point could be in another location. A stopper-engaging portion 246 is included on the distal end 241 of the plunger rod 240 . As shown, the stopper-engaging portion 246 also includes a plunger recess and a retainer 247 . At least one embodiment of the invention includes a press-fit attachment or other suitable means for retaining the end of the stopper.
Referring now to FIG. 21 , which shows an embodiment of the stopper 260 having a distal end 261 and a proximal end 269 . According to at least one embodiment, the stopper 260 includes a peripheral edge 262 which forms a seal with the interior wall of the barrel 220 and has a diameter greater than the diameter of the interior surface of the barrel at the location of the rib 223 (as more clearly shown in FIGS. 22-24 ). As shown, an elongate tip 266 is provided at the distal end 261 of the stopper 260 to help expel the entire contents of the syringe. The stopper 220 can further include a stopper body 264 having a peripheral lip 263 at its proximal end 269 , according to at least one embodiment of the invention. Further, the stopper 260 can include a stopper frangible connection 265 connecting the stopper body 264 to the stopper 260 .
In this configuration, the stopper 260 and plunger rod 240 occupy the chamber of the barrel 220 and the stopper is bottomed against the distal wall of the barrel. Further, the peripheral edge 262 of the stopper 260 forms a seal with the interior surface of the barrel 220 . The stopper 260 is connected to the stopper-engaging portion 246 of the plunger rod 240 . As shown, the retainer 247 of the stopper-engaging portion 246 retains the peripheral lip 263 of the stopper 260 .
Embodiments of the syringe assembly of FIGS. 19-27 can also include a visual marker 300 , visual indicator 310 or both, as described with reference to FIGS. 13-16 . In a specific embodiment, the barrel 220 of one or more embodiments can also include a visual marker aligned with the locking rib 223 . In a more specific embodiment, the syringe assembly can include a visual indicator disposed on the stopper body 264 .
According to one or more embodiments, there is a gap between the stopper 260 and the distal end of the main body 248 defining a pre-selected axial distance 232 . In one or more embodiments, the distance between the protrusion 244 and the peripheral edge 262 of the stopper 260 defines a first distance, D 1 .
FIG. 23 illustrates the syringe assembly in use and specifically shows movement of the plunger rod during an aspiration or filling step according to one or more embodiments of the present invention. When the user applies a force to the plunger rod in the proximal direction, the plunger rod 240 and the stopper 260 move together in the proximal direction as indicated by the arrow, while the stopper-engaging portion 246 is connected to the stopper 260 by the rim 263 . In this configuration, the gap defining the pre-selected axial distance 232 is maintained while the stopper 260 and plunger rod 240 move together in the proximal direction. The user applies proximal force to the plunger rod until a predetermined or desired amount of medicament is aspirated or drawn into the syringe. During the aspiration step, the plunger rod and the stopper body move in the proximal direction together to draw medication into the syringe, while maintaining the first distance D 1 .
FIG. 24 also shows the syringe assembly when distal force is applied to the plunger rod during an injection step according to at least one embodiment of the present invention. Application of a force in the distal direction closing the gap and moving the pre-selected axial distance 232 shown in FIG. 22 , while the stopper 260 remains stationary. Consistent with at least one embodiment, once the stopper-engaging portion 246 has distally moved the pre-selected axial distance 232 and is in contact with stopper frangible connection 265 , the stopper 260 and the plunger rod 240 begin to move in tandem in the distal direction.
When expelling the contents of the syringe, the plunger rod moves in a distal direction the length of the pre-selected axial distance 232 while the stopper body remains stationary. During and after the contents of the syringe have begun to be or have been fully expelled, the distance between the protrusion 244 and the peripheral edge 262 defines a second distance, D 2 , wherein D 2 is the difference between the first distance, D 1 , and the gap defining a pre-selected axial distance 232 .
In one embodiment, the user may inject a limited amount of the fluid aspirated or exert a limited force on the plunger rod in the distal direction to flush or expel some of the aspirated fluid, without locking the plunger rod, provided that the syringe assembly is not bottomed. However, as will be described further below, a user will typically expel substantially all of the contents of the syringe by bottoming the stopper on the distal wall of the barrel.
Referring now to FIG. 25 , which illustrates the syringe assembly after the plunger rod 240 has been locked inside the barrel 220 , the distal movement of the stopper-engaging portion 246 to the stopper frangible connection 265 of the stopper 260 (as also shown in FIG. 24 ) closes the gap defining the pre-selected axial distance and allows the protrusion 244 to advance past the rib 223 , thereby locking the plunger rod 240 inside the barrel 220 , preventing re-use of the syringe assembly.
Referring now to FIG. 26 , the syringe assembly is shown in a configuration in which a user attempts to reuse the syringe assembly after the plunger rod 240 is locked inside the barrel 220 by applying a force to the plunger rod 240 in the proximal direction. Application of sufficient proximal force to the plunger rod causing a portion of the plunger rod 240 to separate at the frangible connection or point 243 , as the holding force of the protrusion 244 and the rib exceeds the breaking force of the frangible point or connection.
FIG. 27 shows the syringe assembly in a configuration after which proximal force has been applied to the plunger rod and the stopper has moved to the proximal end of the barrel. As shown in FIG. 27 , the stopper 260 has separated from the stopper-engaging portion 246 of the plunger rod. The stopper frangible connection 265 breaks to prevent a user from disassembling the parts of the syringe assembly. As otherwise described herein, the peripheral edge of the stopper 262 has an outer diameter greater than the inner diameter of the interior surface of the barrel at the location of the rib 223 . Consistent with at least one embodiment of the invention, when a user applies a force to the plunger rod 240 in the proximal direction, the rib 223 of the barrel 220 locks the peripheral edge 262 of the stopper 260 , and the stopper frangible connection 265 breaks, separating the stopper body 264 from the stopper 260 . Without being limited by theory, it is believed that the force required to break the frangible connection is less than the force exerted on the peripheral edge of the stopper.
According to one or more embodiments, the syringe barrel may include identifying information on the syringe assembly. Such information can include, but is not limited to one or more of identifying information regarding the contents of the syringe assembly or information regarding the intended recipient.
Reference throughout this specification to “one embodiment,” “certain embodiments,” “one or more embodiments” or “an embodiment” means that a particular feature, structure, material, or characteristic described in connection with the embodiment is included in at least one embodiment of the invention. Thus, the appearances of the phrases such as “in one or more embodiments,” “in certain embodiments,” “in one embodiment” or “in an embodiment” in various places throughout this specification are not necessarily referring to the same embodiment of the invention. Furthermore, the particular features, structures, materials, or characteristics may be combined in any suitable manner in one or more embodiments.
Although the invention herein has been described with reference to particular embodiments, it is to be understood that these embodiments are merely illustrative of the principles and applications of the present invention. It will be apparent to those skilled in the art that various modifications and variations can be made to the method and apparatus of the present invention without departing from the spirit and scope of the invention. Thus, it is intended that the present invention include modifications and variations that are within the scope of the appended claims and their equivalents. | Syringe assemblies having a passive disabling system to prevent reuse are provided. According to one or more embodiments, the syringe assembly comprises a barrel, plunger rod and stopper wherein the plunger rod further comprises a locking protrusion that locks the plunger rod within the barrel. Certain embodiments further include a frangible portion on the plunger rod that breaks when reuse is attempted. One or more embodiments include a plunger rod and stopper attachment that prevents disassembly of the syringe assembly prior to use. Syringe assemblies of one or more embodiments also include visual indicators or markers indicating whether a syringe assembly is used or the plunger rod is locked within the barrel. | 0 |
FIELD OF THE INVENTION
[0001] The invention relates generally to semiconductor fabrication and, more particularly to capacitor container structures.
BACKGROUND OF THE INVENTION
[0002] Continuing advances in miniaturization and densification of integrated circuits have led to smaller areas available for devices such as transistors and capacitors. With shrinkage of the cell size, maintaining a sufficient amount of cell charge storage capacitance is a challenge in a dynamic random access memory (DRAM).
[0003] Several techniques have been developed to increase the storage capacity of a capacitor in a limited space. One such technique is to fabricate a cup-shaped bottom electrode defining an interior surface and an exterior surface within a container formed in an insulative layer. A recess between adjacent bottom electrodes is formed in the insulating layer to expose a portion of the electrodes' exterior surfaces. A capacitor dielectric and then a top electrode are deposited over the interior of the cup-shaped bottom electrode and the interior of the recess. The structure provides additional capacitance.
[0004] Conventionally, the bottom electrode is formed of N-type hemispherical grain silicon (HSG). Using a double-sided HSG bottom electrode provides a higher surface area for increased capacitance. However, the growth of HSG on the exterior container surface can cause cell to cell shorts, requiring the space between containers to be enlarged.
[0005] Thus, a need exists for a structure and process therefor that overcomes such problems.
SUMMARY OF THE INVENTION
[0006] The present invention provides capacitor structures and methods of forming such structures.
[0007] In one aspect, the invention provides methods for forming a container capacitor. In one embodiment of the method, the lower electrode of the capacitor is fabricated by forming a layer of doped polysilicon within a container in an insulative layer disposed on a substrate; forming a barrier layer over the polysilicon layer within the container; removing the insulative layer to expose the polysilicon layer outside the container; nitridizing the exposed polysilicon layer at a low temperature, preferably at about 550° C. or less and by remote plasma nitridation; removing the barrier layer to expose the polysilicon layer within the container; optionally cleaning the exposed polysilicon layer to remove native oxide and remaining barrier layer using a wet etch selective to the nitride layer overlying the exterior surface of the polysilicon layer; and forming HSG polysilicon over the polysilicon layer within the opening. The capacitor can be completed by forming a dielectric layer over the lower electrode, and an upper electrode over the dielectric layer.
[0008] In another embodiment of the method, a plurality of capacitors can be formed on a semiconductor substrate. The capacitors can be fabricated by forming a conformal layer of doped polysilicon over an insulative layer disposed on a substrate and within a plurality of containers formed in the insulative layer; depositing a conformal layer of a barrier material over the polysilicon layer; removing the barrier layer and the polysilicon layer overlying the insulative layer outside the containers; removing the insulative layer to expose the exterior surfaces of the polysilicon layer outside the containers and form a recess between adjacent bottom electrodes; nitridizing the exterior surface of the polysilicon layer outside the containers, preferably by remote plasma nitridation at a temperature of about 550° C. or less to form a nitride layer; removing the barrier layers from the interior surface of the polysilicon layer within the containers; optionally cleaning the interior surface of the polysilicon layer within the containers; and forming HSG polysilicon over the polysilicon layer within the containers. The capacitor can be completed by forming a dielectric layer over the lower electrodes and into the recesses between electrodes, and an upper electrode over the dielectric layer.
[0009] In another aspect, the invention provides a container capacitor. In one embodiment, the capacitor comprises a cup-shaped bottom electrode defining an interior surface and an exterior surface within a container formed in an insulative layer; the interior surface comprising HSG polysilicon, and the exterior surface comprising smooth polysilicon. The bottom electrode is preferably 300 to about 400 angstroms. The capacitor can further comprises a dielectric layer overlying the inner and outer surfaces of the bottom electrode; and a top electrode overlying the dielectric layer. The cup-shaped bottom electrode can be, for example, circular, square, rectangular, trapezoidal, triangular, oval, or rhomboidal shaped, in a top down view.
[0010] In yet another aspect, the invention provides a semiconductor device. In one embodiment, the semiconductor device comprises a plurality of cup-shaped bottom electrodes, each electrode defining an interior surface and an exterior surface within a container formed in an insulative layer; the interior surface comprising HSG polysilicon, and the exterior surface comprising smooth polysilicon; a recess formed within the insulative layer between adjacent electrodes; a dielectric layer disposed over the bottom electrodes and the recess between the adjacent electrodes; and a top electrode disposed over the dielectric layer. The bottom electrodes can be, for example, circular, square, rectangular, trapezoidal, triangular, oval, or rhomboidal shaped, in a top down view. In another embodiment of the semiconductor device, an etch stop layer (e.g., silicon nitride) can underlie the insulative layer, and the recess within the insulative layer between adjacent electrodes can be formed to the etch stop layer.
[0011] Advantageously, the present invention provides for the manufacture of a double-sided electrode having a smooth outer surface and a rough inner surface, which enables an increase in container critical dimensions (CD) and capacitance and provides a capacitor having a large electrode surface area. The invention also proves a semiconductor device comprising multiple closely-spaced capacitors for increased density of the device.
BRIEF DESCRIPTION OF THE DRAWINGS
[0012] Preferred embodiments of the invention are described below with reference to the following accompanying drawings, which are for illustrative purposes only. Throughout the following views, the reference numerals will be used in the drawings, and the same reference numerals will be used throughout the several views and in the description to indicate same or like parts.
[0013] [0013]FIG. 1 is a diagrammatic cross-sectional view of a semiconductor wafer fragment at a preliminary step of a processing sequence.
[0014] FIGS. 2 - 10 are views of the wafer fragment of FIG. 1 at subsequent and sequential processing steps, showing fabrication of a capacitor according to an embodiment of the method of the invention.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0015] The invention will be described generally with reference to the drawings for the purpose of illustrating the present preferred embodiments only and not for purposes of limiting the same. The figures illustrate processing steps for use in the fabrication of semiconductor devices in accordance with the present invention. It should be readily apparent that the processing steps are only a portion of the entire fabrication process.
[0016] In the current application, the terms “semiconductive wafer fragment” or “wafer fragment” or “wafer” will be understood to mean any construction comprising semiconductor material, including but not limited to bulk semiconductive materials such as a semiconductor wafer (either alone or in assemblies comprising other materials thereon), and semiconductive material layers (either alone or in assemblies comprising other materials). The term “substrate” refers to any supporting structure including, but not limited to, the semiconductive wafer fragments or wafers described above.
[0017] An embodiment of a method of the present invention is described with reference to FIGS. 1 - 10 , in a method of forming a capacitor.
[0018] Referring to FIG. 1, a portion of a semiconductor wafer 10 is shown at a preliminary processing step. The wafer fragment 10 in progress can comprise a semiconductor wafer substrate or the wafer along with various process layers formed thereon, including one or more semiconductor layers or other formations, and active or operable portions of semiconductor devices.
[0019] The wafer fragment 10 is shown as comprising a substrate 12 , a first insulative layer 14 , a wet etch stop layer 16 , and a second overlying insulative layer 18 . An exemplary substrate 12 is monocrystalline silicon that is lightly doped with a conductivity enhancing material. Exemplary insulative materials include silicon dioxide (SiO 2 ), phosphosilicate glass (PSG), borosilicate glass (BSG), and borophosphosilicate glass (BPSG), in a single layer or multiple layers, with the insulative layers 14 , 18 , being BPSG in the illustrated example. Multiple containers or openings 20 a - c have been conventionally dry etched through the first and second BPSG insulative layers 14 , 18 , and the wet etch stop layer 16 to an active area in the substrate 12 using a dry etch process using, for example, CF 4 , C 4 F 6 , among others.
[0020] The wet etch stop layer 16 , which is conformally deposited over the first insulative layer 14 , has a characteristic etch rate in which etchants will selectively remove the second insulative layer 18 in a later processing step without significantly etching the etch stop layer 16 in a later wet etch processing step. The wet etch stop layer 16 can comprise, for example, silicon nitride (SiN x ) at about 100 to about 200 angstroms, or silicon dioxide formed by decomposition of a tetraethylorthosilicate (TEOS) precursor at about 500 to about 1000 angstroms.
[0021] Referring to FIG. 2, a layer 22 of smooth, conductively doped polysilicon is conformally deposited over the BPSG insulative layer 18 and within each of the openings 20 a - c of each container capacitor structure, to form a cup-shaped structure (lower electrode) within the openings. By cup-shaped, it is understood to include any of circular, square, rectangular, trapezoidal, triangular, oval, or rhomboidal, among other shapes, with respect to the top down view of the lower electrodes.
[0022] The polysilicon electrode layer 22 can be deposited from a silicon source material such as dichlorosilane (SiH 2 Cl 2 , DCS), silicon tetrachloride (SiCl 4 ), silicon trichlorosilane (SiHCl 3 , TCS), and a silicon precursor that contains a hydride such silane (SiH 4 ) and disilane (Si 2 H 6 ). The silicon material can be deposited utilizing a known deposition process including plasma enhanced chemical vapor deposition (PECVD), low pressure chemical vapor deposition (LPCVD), and rapid thermal chemical vapor deposition (RTCVD). For example, the silicon material can be deposited by LPCVD of SiH 4 at a temperature of about 450° C. to about 650° C., a pressure of about 0.2 to about 1 Torr, and an SiH 4 flow rate of about 250 sccm, for a duration of about 20 to about 60 minutes, to a preferred thickness of about 300 to about 400 angstroms. The polysilicon can be doped during deposition or after deposition by diffusion or ion implantation.
[0023] As shown in FIG. 3, a thin barrier layer 24 is then formed over the interior surface 26 of the polysilicon electrode layer 22 , being titanium nitride (TiN) in the illustrated example. A TiN barrier layer 24 can be formed by a conventional thermal chemical vapor deposition (TCVD), plasma enhanced CVD (PECVD), or atomic layer deposition (ALD), utilizing a source gas comprising precursors of tetrakisdimethyl-amidotitanium (TDMAT) ((CH 3 ) 2 N) 4 Ti) and ammonia (NH 3 ), or titanium tetrachloride (TiCl 4 ) and NH 3 . Preferably, the titanium nitride layer 24 is about 100 to about 200 angstroms.
[0024] Referring to FIG. 4, the TiN barrier layer 24 and the polysilicon electrode layer 22 overlying the second BPSG insulative layer 18 and outside the openings 20 a - c, are subjected to a conventional dry etch or chemical mechanical polishing (CMP) 28 to expose the upper surface of the BPSG layer 18 . A suitable dry etch comprises exposing the wafer 10 to CF 4 , C 4 F 6 , among others, at a temperature of about 25° C. to about 150° C., a pressure of about 30 to about 100 mTorr, and gas flow rate of about 30 to about 100 sccm.
[0025] As depicted in FIG. 5, a portion of the BPSG insulative layer 18 is removed by wet etch 30 using a hydrofluoric acid (HF) solution to form an opening or recess 28 to expose the exterior surface 34 of the polysilicon lower electrode 22 , resulting in a cup-shaped lower electrode structure. As shown, the insulative layer 18 has been downwardly etched to expose the nitride etch stop layer 16 . The HF wet etch is selective to the TiN layer 24 and the polysilicon electrode 22 . An example and preferred HF solution comprises a 10:1 HF solution. For an about 1.7 μm (17,000 angstroms) BPSG insulative layer, the etch can comprise the use of a 10:1 HF solution for about 345 seconds.
[0026] The exterior surface 34 of the polysilicon electrode layer 22 is then nitridized by exposure to a nitrogen-containing gas 36 , as shown in FIG. 6, to form an overlying passivating layer 38 comprising silicon nitride (SiN x ). The nitridizing process step can be performed by remote plasma nitridization (RPN) or decoupled plasma nitridization (DPN) over a temperature range of about 400° C. to about 550° C. Examples of nitrogen-containing gases for use in such methods include nitrogen (N 2 ) and ammonia (NH 3 ).
[0027] An example and preferred nitridation process is a RPN at a low temperature of about 550° C. or less, a pressure of about 1 Torr to about 100 Torr, with a nitrogen precursor flow rate of about 10 sccm to about 1000 sccm, for a duration of about 5 seconds to about 5 minutes, to form a nitride layer 38 of about 15 to about 25 angstroms thick. The use of a low temperature RPN prevents the interior surface 26 of the polysilicon electrode 22 from being nitridized by the reaction of the TiN barrier layer 24 with the polysilicon.
[0028] Referring to FIG. 7, the TiN barrier layer 24 is then stripped from the interior surface 26 of the polysilicon electrode 22 using a conventional piranha wet etch 40 , for example, by immersing the wafer 10 in a solution of sulfuric acid (H 2 SO 4 ) and an oxidant such as hydrogen peroxide (H 2 O 2 ).
[0029] The wafer fragment 10 can then be subjected to a wet etch to remove native oxide and titanium silicide (TiSi x ) that may have formed over the interior surface 26 of the polysilicon electrode 22 , and prepare the surface 26 for formation of hemispherical silicon grain (HSG) polysilicon in the next step. An example of a suitable etchant comprises a mixture of NH 4 F and H 3 PO 4 , which provides etch rates of native oxide, TiSi x , and nitride at about 48, 50 and 2 angstroms per minute. Immersion of the wafer in the etchant solution for up to about 2 minutes, preferably about 60 to about 100 seconds, provides cleaning of the interior surface 26 of the polysilicon electrode 22 while maintaining a sufficient thickness of the RPN nitride passivating layer 38 over the exterior surface 34 of the electrode.
[0030] A selective HSG conversion of the interior surface 26 of the polysilicon electrode 22 is then performed, resulting in a layer 42 of HSG polysilicon, as depicted in FIG. 8. Due to the presence of the RPN nitride passivating layer 38 overlying the exterior surface 34 of the polysilicon electrode 22 , HSG growth is limited to the interior surface 26 of the electrode 22 , resulting in the lower electrode 22 having a smooth exterior surface 34 and a rough (HSG) interior surface 26 .
[0031] HSG formation is well known in this art and many different known processes may be used in conjunction with the present invention. An example and preferred method of forming HSG is by silicon seeding and annealing in vacuum or at low pressure. To selectively create HSG on the interior surface 26 of the polysilicon electrode 22 , the wafer 10 is exposed, for example, to silane or disilane, to form a seed layer of amorphous silicon, and the seed layer is then thermally annealed to convert to HSG.
[0032] As shown in FIG. 9, a nitride wet strip 44 is then preformed to selectively etch the RPN nitride layer 38 remaining on the exterior surface 34 of the polysilicon lower electrode 22 . An example of a suitable wet etch of the nitride layer 38 can be performed using a conventional hot phosphoric acid (H 3 PO 4 ) strip.
[0033] The structure can then be processed by conventional methods to complete the capacitor structure.
[0034] Referring to FIG. 10, a cell nitride layer 46 comprising silicon nitride (SiN x ) can be conformally deposited over the polysilicon lower electrode 22 and into the openings 20 a - c and the recesses 32 , typically by low pressure chemical vapor deposition (LPCVD) of a silicon source gas such as SiH 2 Cl 2 , SiCl 4 , SiH 4 , and Si 2 H 6 , and a nitrogen source gas such as NH 3 . Conventional silicon nitride deposition processes other than LPCVD can also be used, including physical deposition, plasma enhanced chemical vapor deposition, and rapid thermal chemical vapor deposition, among others.
[0035] A conductive material can then be deposited over the cell nitride layer 46 to form the top capacitor electrode 48 . The top electrode 48 can comprise a conductive material such as doped polysilicon or a conductive metal. The conductive material can be deposited on the cell nitride layer 46 and into the openings 20 a - c and the recesses 32 , by conventional methods, such as chemical vapor deposition (CVD), or physical vapor deposition (e.g., sputtering) for a metal plate, to complete the capacitor structures 50 a - c.
[0036] In compliance with the statute, the invention has been described in language more or less specific as to structural and methodical features. It is to be understood, however, that the invention is not limited to the specific features shown and described, since the means herein disclosed comprise preferred forms of putting the invention into effect. The invention is, therefore, claimed in any of its forms or modifications within the proper scope of the appended claims appropriately interpreted in accordance with the doctrine of equivalents. | A container capacitor and method of forming the container capacitor are provided. The container capacitor comprises a lower electrode fabricated by forming a layer of doped polysilicon within a container in an insulative layer disposed on a substrate; forming a barrier layer over the polysilicon layer within the container; removing the insulative layer to expose the polysilicon layer outside the container; nitridizing the exposed polysilicon layer at a low temperature, preferably by remote plasma nitridation; removing the barrier layer to expose the inner surface of the polysilicon layer within the container; and forming HSG polysilicon over the inner surface of the polysilicon layer. The capacitor can be completed by forming a dielectric layer over the lower electrode, and an upper electrode over the dielectric layer. The cup-shaped bottom electrode formed within the container defines an interior surface comprising HSG polysilicon, and an exterior surface comprising smooth polysilicon. | 7 |
INCORPORATION BY REFERENCE TO ANY PRIORITY APPLICATIONS
[0001] Any and all applications for which a foreign or domestic priority claim is identified in the Application Data Sheet as filed with the present application are hereby incorporated by reference under 37 CFR 1.57. The present application is a continuation of PCT International Application No. PCT/NZ2013/000175, filed Sep. 23, 2013, which claims priority to U.S. Provisional Application No. 61/705,340, filed Sep. 25, 2012, the entirety of each of which is hereby incorporated by reference herein.
BACKGROUND OF THE INVENTION
[0002] 1. Field of the Invention
[0003] The present invention generally relates to respiratory devices. More particularly, the present invention relates to respiratory devices in which respiratory gases are supplied at a positive pressure after passing over a surface of liquid in a reservoir.
[0004] 2. Description of the Related Art
[0005] CPAP treatment of obstructive sleep apnea involves the delivery of pressurized, breathable gas, usually air, to a user's airways using a conduit and a user interface, such as a mask. The gas pressures employed for CPAP typically range from about 4 cm H2O to about 28 cm H2O at flow rates of up to about 180 L/min (measured at the user interface), depend upon the requirements of the user. The pressurized gas acts as a pneumatic splint for the airway of the user. As such, the pressurized gas reduces the likelihood of collapsing of the airway.
SUMMARY OF THE INVENTION
[0006] CPAP machines include an airflow generator to supply the pressurized gas and many CPAP machines include a heated water bath or other source of water for humidification of the pressurized gas. CPAP machines often are used in bedrooms or other sleeping quarters and are placed on nightstands, for example. As such, reducing the footprint of CPAP machines is desirable. In addition, given the limited space of nightstand tops, CPAP machines often are pushed as close to a wall as possible.
[0007] Because of the cramped spaces in which CPAP machines are used, easy manipulation of a lid or other component used to enclose a water reservoir or the like is desired. Preferably, the lid or other such component can be easily pivoted about hinges. More preferably, the hinges are configured to be generally flush with, or recessed into, the adjoining outer surfaces Even more preferably, the hinges provide a restraint against forces generated by air pressure within the machine (e.g., vertical forces with a generally horizontal lid) while allowing detachment of the lid when the lid is overextended during opening.
[0008] Moreover, to improve the ability to access the water reservoir, the lid preferably carries a latch mechanism such that a user can open the lid with a single hand. In other words, the latch can be operated and the lid can be opened with a single hand and, preferably, with the single hand in a single position. Such configurations are a welcomed improvement over configurations requiring one hand to operate the latch and another hand to subsequently raise the lid.
[0009] In some configurations, a breathing assistance apparatus comprises a lid and a main body with the lid and the main body selectively enclosing a cavity. The lid comprises a button member and at least one hinge assembly.
[0010] In some configurations, the lid further comprises a component adapted to be engaged with one or more fingertips while the button member is depressed.
[0011] In some configurations, the button member is spring biased away from the at least one hinge assembly.
[0012] In some configurations, the at least one hinge assembly allows pivotal movement of the lid relative to the main body.
[0013] In some configurations, the hinge assembly comprises at least one post and at least one support, the supports overlying the post and the post being positioned inboard of an outer perimeter of the lid.
[0014] Preferably, the hinge assembly comprises a clip extending along at least an axial length of the post, the clip being positioned on an opposite side of the post from the supports such that the post is captured between the clip and the supports.
[0015] In some configurations, the at least one hinge assembly comprises a guide structure and cam structure, the guide structure and the cam structure configured to cause sliding movement of the post during rotation of the post.
[0016] In some configurations, the guide structure comprises a guide surface, wherein in use the guide surface contacts the cam structure to move the lid from a detached state to an attached state relative to the main body via the sliding movement of the post as a result of closing motion of the lid.
[0017] Preferably, the sliding movement only occurs when the lid is moved from a disengage state to an engaged state with respect to the main body.
[0018] Preferably, the sliding movement of the post is substantially horizontal with the supports being positioned at least vertically above the post with the lid in the closed position.
[0019] In some configurations, the at least one support defines an opening that permits the at least one post to pass through the opening such that in use the lid can be moved from a detached state to an attached state relative to the main body.
[0020] In some configurations, a method of opening a lid of a breathing apparatus comprises moving a button member toward an engagement component to unlatch the lid and then rotating the lid to an opened position without the user having to reposition a hand.
[0021] In some configurations, a method of engaging a lid on a main body of a breathing apparatus comprises placing a post alongside at least one support member with the lid in an open position, pivoting the lid toward a closed position such that at least one engaging structures formed on the lid and at least one engaging structure formed on the main body cause the lid to translate into an engaged structure with the lid being pivotable while in the engaged structure.
BRIEF DESCRIPTION OF THE DRAWINGS
[0022] These and other features, aspects and advantages of the present invention will be described with reference to the following drawings.
[0023] FIG. 1 is a rear perspective view of a breathing assistance apparatus that is arranged and configured in accordance with certain features, aspects and advantages of the present invention.
[0024] FIG. 2 is an enlarged rear top perspective view of a hinge of the breathing assistance apparatus of FIG. 1 with a lid in a closed position.
[0025] FIG. 3 is an enlarged front perspective view of the hinge of FIG. 2 showing the lid in an opened position.
[0026] FIG. 4 is a sectioned perspective view of the hinge of FIG. 2 showing the lid in a partially closed position.
[0027] FIG. 5 is a front perspective view of the lid of the breathing assistance apparatus of FIG. 1 , which lid is arranged and configured in accordance with certain features, aspects and advantages of the present invention.
[0028] FIG. 6 is a rear bottom perspective view of a latch member of the lid of FIG. 5 .
[0029] FIG. 7 is a rear bottom perspective view of the latch member of FIG. 6 shown assembled to the lid.
[0030] FIGS. 8A-8D are side views of a guide structure of the hinge of FIG. 2 in several positions from opened to closed.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0031] FIG. 1 illustrates a breathing assistance apparatus 100 that is arranged and configured in accordance with certain features, aspects and advantages of the present invention. The apparatus 100 comprises a main body 102 and a lid 104 . Together, the main body 102 and the lid 104 define a housing 106 that encloses, or generally encases, a reservoir, tub, tank or other body of liquid (not shown) within a cavity.
[0032] The illustrated body 102 comprises at least one outer surface 110 . In the illustrated configuration, the body 102 comprises four generally planar outer surfaces 110 that are connected by rounded corners 112 . Other configurations are possible.
[0033] The lid 104 is connected to the body 102 with hinge assemblies 114 . In the illustrated configuration, the lid 104 is connected to a rear of the main body 102 using two hinge assemblies. The lid 104 can be connected to other surfaces. In addition, the lid 104 can be connected to the main body 102 using as few as one hinge assembly 114 or more than two hinge assemblies 114 . Preferably, the hinge assemblies 114 are constructed such that, with the lid 104 in the closed position (e.g., as shown in FIG. 1 ), the hinge assemblies 114 are generally flush with or recessed into the rear outer surface 110 . In some configurations, the hinge assemblies 114 are constructed such that the hinge assemblies do not protrude rearward of the rear outer surface 110 . In some configurations, some of the hinge features may protrude very slightly from one or more surrounding surface of the rear outer surface or other surrounding portion of the apparatus. In some configurations, the lid 104 comprises an outer perimeter 116 and the hinge assemblies 114 do not protrude significantly outward of the outer perimeter 116 of the lid 104 .
[0034] With reference to FIG. 2 , the hinge assemblies 114 comprise at least one post 120 and at least one support 122 . Preferably, the at least one post 120 is mounted such that the post is recessed and located inside of the outer perimeter 116 of the lid. The illustrated configuration comprises a single post 120 that is connected to two supports 122 . In some configurations, the at least one post 120 is mounted to the lid 104 while the at least one support 122 is mounted to the main body 102 . In some configurations, the at least one post 120 can be mounted to the main body 102 while the at least one support 122 can be mounted to the lid 104 .
[0035] The at least one post 120 can be secured to the lid 104 using one or more standoffs 124 . In the illustrated construction, the standoffs 124 are positioned between the two supports 122 . The standoffs reduce the deflection of the post 120 in the region of the supports 122 . In some configurations, the portion 126 of the post 120 extending between the standoffs 124 can be omitted. In the illustrated configuration, however, the portion 126 of the post 120 can be secured by a clip 130 . The clip 130 can have a recess that accommodates the post 120 or any other suitable configuration.
[0036] A force generated by the clip 130 on the post 120 in the illustrated configuration is opposed by forces generated by the supports 122 , for example. The clip 130 can contact an opposite side of the post 120 relative a contact region between the supports 122 and the post 120 . In some configurations, the clip 130 can be configured to deflect away from the post 120 during assembly of the post 120 and the clip 130 . For example, the clip 130 can be a deflectable finger that extends rearward from the main body 102 . The supports 122 can have a recess that defines a rearwardly-opening mouth that receives at least a portion of a circumference of the post 120 . Accordingly, movement of the post 120 in the directions shown by the arrow can result in attachment and detachment of the post 120 relative to the supports 122 and the clip 130 . The rearwardly-opening mouth of the supports 122 also results in a structure that overlies the post 120 such that vertical movement of the post 120 relative to the supports 122 is not possible with the post 120 fully received within the mouths of the supports 122 . As such, the lid 104 is unlikely to separate from the main body 102 during therapy.
[0037] With reference to FIG. 3 , the lid 104 and the main body 102 can include structures that guide the post 120 and the clip 130 and supports 122 into connection. In some configurations, the structures facilitate movement of the at least one post 120 into the mouth of the supports 122 and into engagement with the clip 130 when the lid 104 is brought toward the closed position on the main body 102 . In the illustrated configuration, two guide structures 140 are positioned outboard of the two supports 122 . Other configurations also are possible.
[0038] With reference to FIG. 4 , the guide structure 140 comprises a recess 142 that receives a cam structure 144 . The cam structure 144 is received within the recess 142 such that, with the lid 104 moved to the fully closed position on the main body 102 , the cam structure 144 does not prevent the lid 104 from fully closing. The cam structure 144 tapers toward a point with a sloping surface 146 such that the thickness of the cam structure 144 increases from back to front while the guide structure has an opposing surface 150 . The sloping surface 146 and the opposing surface 150 engage each other such that the sloping surface 146 and the opposing surface 150 resists movement of the lid 104 relative to the main body 102 in the detachment direction (see FIG. 2 ) when the lid 104 is in an at least partially closed position.
[0039] Moreover, as the lid 104 is rotated toward a closed position (e.g., FIG. 1 ), the sloping surface 146 and the opposing surface 150 act to draw the lid 104 forward into the attachment position (e.g., the at least one post 120 connected to the supports 122 and the clip 130 ). Thus, rotation of the lid 104 can result in the hinge assemblies 114 being operatively connected from a detached state. In some configurations, the difference in thicknesses of the sloping surface 146 and the opposing surface 150 from initial contact to fully closed is substantially the same as a distance from the outer surface of the post 120 and the first contact with the supports 122 such that as the sloping and opposing surfaces 146 , 150 are moved into full engagement along their lengths, the post 120 is pulled into position within the supports 122 and the clip 130 .
[0040] Notably, with the lid 104 in the open position (e.g., FIG. 3 ) relative to the main body 102 , sufficient space exists between the sloping surface 146 and the opposing surface 150 such that the lid 104 can be separated from the main body 102 with the application of force. Advantageously, such a construction allows separation between the lid 104 and the main body 102 by disconnection of the posts 120 from the supports 122 and the clips 130 . Such a separation can protect the apparatus 100 from damage resulting from forces that result from over-opening of the lid or from possible misuse of the apparatus 100 . Accordingly, the ability to separate the lid 104 from the main body 102 can protect the apparatus 100 from permanent damage. As discussed above, the lid 104 can be easily reconnected by placing the posts 120 alongside the supports 122 and rotating the lid 104 toward a closed position, which results in the sloping surface 146 of the cam structure 144 and the opposing surface 150 of the guide structure drawing the components back together.
[0041] With reference now to FIG. 5 , a release and handle assembly 160 of the lid 104 will be described. As illustrated, the release and handle assembly 160 comprises at least one button member 162 that is mounted on the lid 104 . In some configurations, the button member 162 is mounted for movement toward and away from the hinge assemblies 162 . In some configurations, the button member 162 can be mounted along a side of the lid 104 that is adjacent to the side of the lid 104 having the hinge assemblies 162 . In the illustrated configuration, the button member 162 is mounted on an opposing side of the lid 104 relative to the hinge assemblies 114 and capable of movement toward and away from the hinge assemblies 114 .
[0042] The button member 162 is illustrated in FIG. 6 . The button member comprises an exterior surface 164 , which is best shown in FIG. 5 . The exterior surface 164 is sufficiently large for contact with a finger or thumb. As also illustrated in FIG. 5 , the lid 104 can comprise a component 166 that is used to raise the lid 104 . In the illustrated configuration, the component 166 is a recessed region that has a wall 170 extending generally parallel with the exterior surface 164 . Preferably, the recessed region 166 is sufficiently large as to accommodate at least tips of fingers. In some configurations, the component 166 is one or more lip, ridge, protrusion, recess or the like. Accordingly, the component 166 (e.g., having the wall 170 ) and the exterior surface 164 can allow a simple squeezing action to accomplish both an unlatching of the button member 162 as well as providing a grasping action to allow movement of the lid 104 away from the main body 102 .
[0043] With reference again to FIG. 6 , the illustrated button member 162 comprises two outer posts 172 . The posts 172 are sized and configured to engage with biasing members, such as compression springs or the like, for example but without limitation. The posts 172 are received within corresponding housings 174 that are formed in the lid 104 . The housings 174 can contain the biasing members and the posts 172 can slide into and out of the housings 174 against the biasing force of the biasing members.
[0044] The illustrated button member 162 also comprises at least one tab 176 . In the illustrated configuration, the button member 162 comprises two tabs 176 . The tabs 176 are bayonet shaped with a barb 180 at the end. As shown in FIG. 7 , the tabs 176 can engage a structure 182 formed in the lid 104 . Thus, the tabs 176 in cooperation with the structure reduce the likelihood of the button member 162 coming out of a recess of the lid 104 while allowing inward depression of the button member 162 relative to the lid 104 .
[0045] The structure 182 also comprises a passage 184 that receives a finger 186 mounted to, or formed on, the button member 162 . The passage 184 facilitates generally only linear translation of the button member 162 relative to the lid 104 . In other words, the passage 184 receives the finger 186 and the finger 186 is generally limited by the passage 184 to substantially linear movement.
[0046] The finger 186 supports a locking post 190 . The locking post 190 can engage with a structure formed on the main body 102 . In some configurations, the locking post 190 engages with a structure formed on an inner surface of the main body 102 such that the depression of the button member 162 results in separation between the locking post 190 and the structure with which it normally engages. Releasing of the button member 162 results in the biasing members moving the locking post 190 into position for reengagement with the structure with which it normally engages.
[0047] FIGS. 8A-8D illustrate the lid 104 in several positions relative to the main body 102 . FIG. 8A illustrates the lid 104 in a first opened position. FIGS. 8B and 8C illustrate the lid 104 in progressively further closed positions relative to the first opened position of FIG. 8A . FIG. 8D illustrates the lid 104 in a closed position. In particular, FIGS. 8A-8D further illustrate the interaction between the sloping surface, or cam surface, 146 of the cam structure 144 and the opposing surface (also referred to as a guide surface or cam follower surface) 150 of the lid recess 142 as the lid 104 moves from an opened position to a closed position. As described herein, the cam structure 144 and the recess 142 can interact to move the lid 104 from a detached position relative to the main body 102 to an attached position relative to the main body 102 when the lid 104 is moved from an opened position to a closed position.
[0048] As described herein, the support 122 includes the recess 200 comprising the mouth 202 , which opens in a rearward direction in the illustrated arrangement. Preferably, the recess 200 is elongate in shape and extends in a generally fore-aft direction. In the illustrated arrangement, the recess 200 is generally or substantially horizontal or aligned with a bottom support surface of the main body 102 such that the recess 200 is generally or substantially horizontal when the apparatus 100 is rested on a flat surface. The recess 200 includes upper and lower guide surfaces 204 that extend forwardly from the mouth 202 to an end surface 206 . As described herein, the support 122 also assists in retaining the lid 104 on the main body 102 in response to forces within the housing 106 (e.g., forces resulting from internal pressure) tending to separate the lid 104 from the main body 102 . Thus, the upper portion of the end surface 206 and/or the upper guide surface 204 can form a retention surface that contacts the post 120 to retain the lid 104 , or at least a portion of the lid 104 near the support 122 and/or hinge 114 (e.g., a rearward portion), on the main body 102 in response to forces tending to separate the lid 104 from the main body 102 .
[0049] In the illustrated arrangement, the end surface 206 is curved (e.g., semi-circular) in shape from a side view and connects the upper guide surface 204 and the lower guide surface 204 . The illustrated support 122 is elongate in a lateral or side-to-side direction and, thus, defines a substantially semi-cylindrical shape in three dimensions. However, for convenience, the hinge 114 , guide structure 140 and cam structure 144 may be described herein in the context of the side views of FIGS. 8A-8D in two-dimensional terms. It will be appreciated that the described structures also have a width dimension relative to the apparatus 100 or a depth dimension relative to the side view of FIGS. 8A-8D .
[0050] The illustrated end surface 206 is defined by a curve having a radius 208 from a center point 210 (or an axis in three dimensions). The recess 200 can have a longitudinal axis 212 that extends along a length of the recess 200 generally from the mouth 202 to the end surface 206 and, in the illustrated configuration, passes through the center point 210 . The axis 212 can be aligned with or parallel to one or both of the upper and lower guide surfaces 204 or can be centrally-located between the guide surfaces 204 (such as in the event of a tapered recess, for example and without limitation). In the illustrated configuration, the axis 212 is generally or substantially horizontal (or parallel to a bottom surface of the main body 102 ). However, in other configurations, the axis 212 could be non-horizontal or angled relative to the bottom surface of the main body 102 ).
[0051] As described herein, the post 120 preferably is cylindrical in shape or circular in shape from a side view, as illustrated in FIGS. 8A-8D . The post 120 defines a center point 214 (or an axis in three dimensions) and a radius 216 . Preferably, the radius 216 of the post 120 is substantially equal to the radius 208 of the end surface 206 such that the post 120 can be snugly positioned against the end surface 206 and restrained in a vertical direction within recess 200 with the center points 210 , 214 substantially aligned or coaxial with one another.
[0052] Preferably, the cam surface or sloping surface 146 of the cam structure 144 is positioned or oriented relative to the end surface 206 and/or center point 210 such that the post 120 is moved along the axis 212 of the recess 200 toward the end surface 206 as the lid 104 is moved from the opened toward the closed position. In the illustrated arrangement, a first distance 220 is defined between a first point or location 222 on the sloping surface 146 and the center point 210 and a second distance 224 is defined between a second point or location 226 on the sloping surface 146 and the center point 210 . Preferably, the first point 222 is located on an initial portion of the sloping surface 146 and the second point 226 is located on a subsequent portion of the sloping surface 146 such that the opposing surface 150 will contact the first point 222 before the second point 226 as the lid 104 is moved from an opened position to a closed position. The first point 222 can be at or near the location that is first contacted by the opposing surface 150 during closing of the lid 104 and the second point 226 can be at or near the furthest location along the sloping surface 146 contacted by the opposing surface 150 when the lid 104 is in the closed position. The first distance 220 preferably is smaller than the second distance 224 , which causes the movement of the post 120 along the axis 212 of the recess 200 as the lid 104 is moved from an opened position to a closed position and the opposing surface 150 moves along the sloping surface 146 in a direction from the first point 222 towards the second point 226 .
[0053] A distance 228 traveled by the center point 214 of the post 120 within the recess 200 when the lid 104 is closed preferably is substantially equal to a difference 230 between the second distance 224 and the first distance 220 . The distance 228 can be less than an overall length of the recess 200 because the post 120 can be at least partially located within the recess 200 prior to being drawn to the end surface 206 by the guide structure 140 . In other arrangements, the distance 228 could be substantially equal to a length of the recess 200 . Although the distances described immediately above are in relation to the center points 210 and 214 , the distances similarly could be measured relative to other points on locations on the recess 200 (e.g., end surface 206 ) and post 120 , respectively, if desired, such as in the context of non-circular (or non-cylindrical) recess or post shapes.
[0054] FIG. 8A illustrates the lid 104 in a first open position relative to the main body 102 , which may be a fully opened position, such as when initiating a process of reattachment of the lid 104 . As illustrated, the opposing surface 150 is clear of the sloping surface 146 such that rearward movement (e.g., detachment) of the lid 104 is permitted. Advantageously, such an arrangement reduces the likelihood of permanent damage resulting from excessive opening forces applied to the lid 104 . FIG. 8B illustrates the lid 104 in a second open position that is further towards a closed position relative to the first open position of FIG. 8A . In FIG. 8B , the opposing surface 150 remains clear of the sloping surface 146 . That is, a vertical gap exists between a bottom of the opposing surface 150 and a top of the sloping surface 146 .
[0055] FIG. 8C illustrates the lid 104 in a third open position that is further towards a closed position relative to the positions of FIGS. 8A and 8B . In the position of FIG. 8C , a leading portion or engagement portion 232 of the opposing surface 150 is engaged with or contacts an initial portion of the sloping surface 146 , which may be at or near the first point or location 222 . In the illustrated arrangement, the post 120 is spaced away from the end surface 206 of the recess 200 . FIG. 8D illustrates the lid 104 in a position that is further towards a closed position than the positions of FIGS. 8A-8C . The position of FIG. 8D can be a fully closed position of the lid 104 . In the illustrated arrangement, at least the leading portion or engagement portion 232 of the opposing surface 150 is engaged with or contacts a subsequent portion of the sloping surface 146 spaced from the initial portion. The subsequent portion may be at or near the second point or location 226 . Preferably, the post 120 is snugly positioned against the end surface 206 in the position of FIG. 8D . Thus, preferably, a distance between the engagement surface 232 and the center point 214 is preferably substantially equal to the second distance 224 .
[0056] As described herein, the interaction of the guide structure 140 and the cam structure 144 as illustrated in FIGS. 8A-8D may occur only during a reattachment or engagement procedure for the lid 104 . In normal opening and closing movement, sliding of the post 120 (or significant sliding of the post 120 ) within the recess 200 may not occur. Advantageously, such an arrangement reduces wear by reducing the amount of sliding movement between components during normal use. However, other arrangements are possible in which the sliding movement of the post 120 occurs more often than only during engagement of the lid 104 , such as during normal opening and closing of the lid 104 .
[0057] Although the illustrated opposing surface 150 has a similar size and shape as the sloping surface 146 and extends along a substantial portion of the sloping surface 146 when the lid 104 is in the closed position, other arrangements are also possible. For example, the opposing surface 150 could be a smaller surface, such as a cam follower surface, defining an engagement portion 232 that contacts only a point or small length of the sloping surface 146 in any one position. The engagement portion 232 could be rotatable such that it rolls along the sloping surface 146 , if desired. Moreover, as disclosed herein, the illustrated arrangements could be reversed such that the cam surface or sloping surface 146 is carried by the lid 104 and the opposing surface 150 (or cam follower with engagement portion 232 ) is carried by the main body 102 .
[0058] Unless the context clearly requires otherwise, throughout the description and the claims, the words “comprise”, “comprising”, and the like, are to be construed in an inclusive sense as opposed to an exclusive or exhaustive sense, that is to say, in the sense of “including, but not limited to”.
[0059] Reference to any prior art in this specification is not, and should not be taken as, an acknowledgement or any form of suggestion that that prior art forms part of the common general knowledge in the field of endeavour in any country in the world.
[0060] The invention may also be said broadly to consist in the parts, elements and features referred to or indicated in the specification of the application, individually or collectively, in any or all combinations of two or more of said parts, elements or features.
[0061] Where, in the foregoing description reference has been made to integers or components having known equivalents thereof, those integers are herein incorporated as if individually set forth.
[0062] It should be noted that various changes and modifications to the presently preferred embodiments described herein will be apparent to those skilled in the art. Such changes and modifications may be made without departing from the spirit and scope of the invention and without diminishing its attendant advantages. It is therefore intended that such changes and modifications be included within the scope of the invention. | A breathing assistance apparatus has a lid and latch assembly configured for one-handed operation. The apparatus also includes a hinge assembly that separates when over-rotated but that reengages upon closing of the lid onto the main body of the apparatus. | 1 |
TECHNICAL FIELD
[0001] The current invention is generally related to condensing photovoltaic electricity generating technology, in which sun light is concentrated and projected to condensing lens and compound-eye lens condenser of photovoltaic batteries. The current invention is further related to a compound-eye concentrating-type solar cell assembly based on above mentioned condensing lens and compound-eye lens condenser.
BACKGROUND ART
[0002] Concentrating photovoltaic electricity generation technology is widely accepted as an effective way to reduce cost of photovoltaic electricity generation. At present, a complete system for concentrating photovoltaic electricity generation mainly comprises a compound-eye concentrating photovoltaic assembly, a sun-tracker, and electric energy storage or inversion equipment. As a photo-electric conversion element, the compound-eye concentrating photovoltaic assembly comprises a compound-eye lens condenser and a circuit board installed with photovoltaic wafers.
[0003] The compound-eye lens condenser comprises a plurality of planar-arrayed condensing lens. During operation, the sun-tracker keeps the condensing lenses facing the sun perpendicularly for most of the time, then the condensing lenses focus the sun light and project it to the receiving surfaces of corresponding photovoltaic wafers on the circuit board to generate electric current in each of the photovoltaic wafer, then the electric current is exported by the circuits on the circuit board.
[0004] The concentrating solar cell assembly disclosed in patent application with disclosure number CN101640502A is very typical. The point-focusing Fresnel lens implemented in the assembly is widely recognized as the optimal option for condensing lens. There are additional references that disclose concentrating Fresnel lens as the condensing lens for concentrating photovoltaic electricity generation, such additional references are not included herein.
[0005] Actually, implementing Fresnel lens is not without shortcomings. For example, manufacturing defects on the surface texture of Fresnel lens cause loss in incoming light, resulting in a relatively low transmission rate of around 75%; such manufacturing defects are very hard to avoid under current technologies. As another example, Fresnel lens can be considered a combination of multiple co-axis convex lenses; as a result, the energy distribution of the focus light spot produced by Fresnel lens is not sufficiently uniform.
[0006] Replacing Fresnel lens with widely used ordinary spherical lens can solve the problem of low transmission rate. Spherical lens can only, however, focus light on the focal point of the lens, so no matter where the photovoltaic wafer is located, either in the front of the focal point, or further away from the focal point, uneven energy distribution will result on the receiving surface of the photovoltaic wafer, in the center and on the rim of the light spot, causing internal voltage difference in the wafer, producing internal current, such internal current is partially consumed inside the wafer, resulting in reduced output power from the wafer; additionally, internal current is the major cause for wafer internal temperature rise, while wafer internal temperature rises in term reduces efficiency of concentrating photovoltaic assembly.
DETAILED DESCRIPTION
[0007] The current invention offers technical solution by providing a condensing lens that provides a high transmission rate and produces uniformly distributed energy on the focus spot after condensing; the current invention further provides a compound-eye lens condenser that utilizes the condensing lens.
[0008] The technical solution provided in the current invention is implemented by: a condensing lens, in which, the lens is a convex lens that refracts parallel incoming light to a receiving surface located on the outer side of the lens to form a light spot, which is characterized by: assuming x being the perpendicular distance between the point of intersection, where an arbitrary incoming light intersecting the lens, and the optical axis of the lens, m being the perpendicular distance between the projection point, generated by the refracted incoming light projecting on the receiving surface, and the center of the light spot, a being the radius of the lens, b being the radius of the light spot, then the lens satisfies the following condition: x/m=a/b.
[0009] As a preferred embodiment of the above technical solution, the lens having a rotating convex surface with the optical axis as the rotating axis and a flat end surface opposite to the rotating convex surface, the curve on the intersection between the rotating convex surface and an arbitrary longitudinal section which crosses the lens optical axis is a curve which can refract incoming light, said light is radially distributed within the longitudinal section and parallel to the optical axis, to the receiving surface to form a focal line, the curve function for the curve, in a planar coordinate system located on the longitudinal sectional surface with the origin of the coordinate system being the center of the flat end surface, can be described as follows:
[0000]
(
h
+
y
)
n
y
x
1
+
(
y
x
)
2
-
y
x
1
-
n
2
(
y
x
)
2
1
+
(
y
x
)
2
1
-
n
2
(
y
x
)
2
1
+
(
y
x
)
2
+
n
(
y
x
)
2
1
+
(
y
x
)
2
=
(
1
+
b
a
)
x
[0000] where, the coefficient h is the distance between the flat end surface and the receiving surface; coefficient a is the radius of the lens; coefficient b is the half length of the focal line; coefficient n is the refractive index of the lens; variable x is the horizontal distance between an arbitrary point on the curve and the lens optical axis, variable y is the longitudinal distance between the point and flat end surface.
[0010] It should be pointed out, that the curve function cannot be obtained through limited number of experiments conducted by the applicant under the guidance of existing technology. In fact, the curve function is based on applicant's creative realization that, in order to produce uniformly distributed energy on the focus spot after condensing, a better solution is to proportionally condense light onto the receiving surface through the rotating convex surface of the lens. That is, after incoming light passes through an arbitrary point on the curve and is refracted to the receiving surface, the ratio between x and m, x being the x coordinate of the point on the curve function, m being horizontal distance between the projection point on the receiving surface and optical axis of the lens, should be equal to the ratio between a and b, a being the radius of the lens, b being the half length of the projection line, i.e., x/m=a/b. Based on known rules of refraction for lens and above equations, the following equations can be obtained:
[0000]
x
/
m
=
a
/
b
(
1
)
sin
(
θ
)
=
n
sin
(
β
)
(
2
)
x
-
m
=
(
h
-
y
)
tan
(
β
-
θ
)
(
3
)
tan
(
θ
)
=
y
x
(
4
)
[0000] in which, variables and β represent respectively angle of incidence and angle of refraction when light beam passes through the curve. Other coefficients and variables are already explained above. Based on the above equations, the above curve function can be obtained through mathematical derivation.
[0011] The shape of the rotating convex surface determined by the curve function can be fully achieved in industrial engineering settings. Currently, lenses are typically manufactured through molding; the molded shape of the rotating convex surface is controlled by design of the mold. During the process of mold design, it is as simple as entering the above curve function into the mold design software, then the curve is generated from the curve function, then the curve is rotated to generate the theoretical digital model of the rotating convex curve surface; during the process of mold manufacturing, the corresponding mold cavity is manufactured by CNC machine tool.
[0012] The applicant further points out, that the condensing lens with the special curve function disclosed above is an example of the condensing lenses claimed in the current invention, the example is to be understood for illustration purpose only. Actually, the condensing lens characterized by the special curve is a plano-convex lens, so incoming light parallel to the optical axis of the lens is refracted only once by the rotating convex surface of the lens, accordingly, x is the perpendicular distance between the point of intersection, where an arbitrary incoming light intersecting the lens, and the optical axis of the lens, x is also the abscissa of the point where incoming light crossing the curve function; b is the radius of the light spot, or the half length of the focal line formed by refracting the parallel incoming light and focusing them on the receiving surface; m is the perpendicular distance between the projection point, generated by the refracted incoming light projected on the receiving surface, and the center of the light spot.
[0013] In spite of the fact that plano-convex lens is structurally simple and has the advantage of being easy for design and manufacturing, other equivalent designs can be implemented to replace the curve function disclosed above. For example, double convex lens with two rotating convex surfaces can be implemented. As long as the condition x/m=a/b is satisfied (in which, x is the perpendicular distance between the point of intersection, where an arbitrary incoming light intersecting the lens, and the optical axis of the lens, x is also the abscissa of the point where incoming light crossing the curve function; m is the perpendicular distance between the projection point, generated by the refracted incoming light projected on the receiving surface, and the center of the light spot; b is the radius of the light spot, or the half length of the focal line formed by refracting the parallel incoming light and focusing them on the receiving surface; a is the radius of the lens), with additional known lens refractive rules, curve functions of the two rotating convex curve surface can be derived, and accordingly the theoretical digital model of the two rotating convex curve surface.
[0014] The compound-eye lens condenser, in which, a plurality of planar arrayed condensing lenses are adhered on a transparent glass panel, combined with circuit board, to form a box-structured compound-eye concentrating-type solar cell assembly. The condensing lenses can also be one piece with the glass panel.
[0015] Specifically, each of the condensing lens has a rotating convex surface with the optical axis as the rotating axis and a flat end surface opposite to the rotating convex surface, the curve on the intersection between the rotating convex surface and an arbitrary longitudinal section which crosses the lens optical axis is a curve which can refract incoming light, which is radially distributed within the longitudinal section and parallel to the optical axis, to the receiving surface to form a focal line, the curve function for the curve, in a planar coordinate system located on the longitudinal sectional surface with the origin of the coordinate system being the center of the flat end surface, can be described as follows:
[0000]
(
h
+
y
)
n
y
x
1
+
(
y
x
)
2
-
y
x
1
-
n
2
(
y
x
)
2
1
+
(
y
x
)
2
1
-
n
2
(
y
x
)
2
1
+
(
y
x
)
2
+
n
(
y
x
)
2
1
+
(
y
x
)
2
=
(
1
+
b
a
)
x
[0000] where, the coefficient h is the distance between the flat end surface and the receiving surface; coefficient a the radius of the lens; coefficient b is the half length of the focal line; coefficient n is the refractive index of the lens; variable x is the horizontal distance between an arbitrary point on the curve and the lens optical axis, variable y is the longitudinal distance between the point and flat end surface.
[0016] Further, the edge of each the lens is cut into polygon structure with at least three cylindrical surfaces; any two neighboring condensing lenses in the compound-eye lens condenser are adhered together at their adjacent cylindrical surfaces. Evidently, that the purpose for doing so is for the convenience of forming planar arrays of condensing lenses to produce a compound-eye lens condenser.
[0017] Specifically, the edge of each of the individual lens is cut into quadrilateral structure with four cylindrical surfaces, in which, neighboring cylindrical surfaces are perpendicular to each other; any two neighboring condensing lenses in the compound-eye lens condenser are adhered together by their adjacent cylindrical surfaces to form a rectangular array of the condensing lenses for the compound-eye lens condenser. Additional benefit of cutting the edge of the condensing lens into quadrilateral structure is that the shape of focused light spot through the lens is quadrilateral, making it practical to make corresponding photovoltaic wafers quadrilateral during manufacturing. Quadrilateral structure is easy to process during wafer cutting and such quadrilateral cutting saves large amount of wafer materials.
[0018] The current invention further provides a compound-eye concentrating-type solar cell assembly that implements the compound-eye lens condenser.
[0019] The advantages of the current invention include: the transmission rate of the condensing lens is proved by optical simulation to be as high as 90% to 93%, and the energy distribution curve of the focused light spot is almost saddle-shaped, that is, the light spot energy is uniformly distributed. The condensing lens disclosed in the current invention can not only be used in focusing photovoltaic electricity generation, it can also be utilized in other optical equipment where uniform focusing is required.
DESCRIPTION OF THE FIGURES
[0020] FIG. 1 is a schematic illustration of the compound-eye lens condenser.
[0021] FIG. 1( a ) is the overall schematic illustration of the compound-eye lens condenser.
[0022] FIG. 1( b ) is the schematic illustration of a single condensing lens in the compound-eye lens condenser.
[0023] FIG. 2 is an amplified view of FIG. 1( b ).
[0024] FIG. 3 is a full cut away view of FIG. 2 in A direction (section is longitudinal section 2 ).
[0025] FIG. 4 is the energy distribution figure of a light spot obtained through traditional spherical convex lens.
[0026] FIG. 4 , brightness of light pot illustrates the level of energy, the brighter the higher energy.
[0027] FIG. 5 the energy distribution curve of a light spot obtained through traditional spherical convex lens.
[0028] FIG. 5 , abscissa is the width of light spot, ordinate is energy intensity. Accordingly, FIG. 5 can be considered as light spot energy distribution observed on the horizontal section or longitudinal section of FIG. 4 .
[0029] FIG. 6 is the light spot energy distribution figure of the condensing lens disclosed in the current invention.
[0030] FIG. 7 is the light spot energy distribution curve of the condensing lens disclosed in the current invention.
[0031] FIG. 7 , abscissa is the width of light spot, ordinate is energy intensity. Accordingly, FIG. 7 can be considered as light spot energy distribution observed on the horizontal section or longitudinal section of FIG. 6 .
[0032] FIG. 8 is the illustration of another embodiment of the condensing lens disclosed in the current invention.
[0033] FIG. 9 is the structural illustration of the compound-eye concentrating-type solar cell assembly disclosed in the current invention.
EMBODIMENTS
[0034] The current invention is further described with reference to the figures.
[0035] FIG. 9 illustrates a compound-eye concentrating-type solar cell assembly, which is a box structure comprising: a compound-eye lens condenser ( 5 ) and a plurality of photovoltaic wafer ( 7 ) installed on a circuit board ( 6 ); in which, as illustrated in FIGS. 1-3 , the compound-eye lens condenser ( 5 ) comprising a plurality of planar arrayed condensing lens ( 1 ), each of the condensing lens ( 1 ) is a convex lens which is capable of refracting incoming light ( 3 ) parallel to the optical axis ( 103 ) to a receiving surface ( 4 ) of a photovoltaic wafer ( 7 ) located on the outer side of the lens to form a light spot; in which, as illustrated in FIGS. 2-3 , the lens has a rotating convex surface ( 101 ) with the optical axis ( 103 ) as the rotating axis and a flat end surface ( 102 ) opposite to the rotating convex surface ( 101 ), the curve ( 104 ) on the intersection between the rotating convex surface ( 101 ) and an arbitrary longitudinal section ( 2 ) which crosses the lens optical axis ( 103 ) is a curve which can refract incoming light ( 3 ), which is radially distributed within the longitudinal section ( 2 ) and parallel to the optical axis ( 103 ), to the receiving surface ( 4 ) to form a focal line, the curve function for the curve ( 104 ), in a planar coordinate system located on the longitudinal sectional surface ( 2 ) with the origin of the coordinate system (A) being the center of the flat end surface ( 102 ), can be described as follows:
[0000]
(
h
+
y
)
n
y
x
1
+
(
y
x
)
2
-
y
x
1
-
n
2
(
y
x
)
2
1
+
(
y
x
)
2
1
-
n
2
(
y
x
)
2
1
+
(
y
x
)
2
+
n
(
y
x
)
2
1
+
(
y
x
)
2
=
(
1
+
b
a
)
x
[0000] where, the coefficient h is the distance between the flat end surface ( 102 ) and the receiving surface ( 4 ); coefficient a the radius of the lens; coefficient b is the half length of the focal line; coefficient n is the refractive index of the lens; variable x is the horizontal distance between an arbitrary point (B) on the curve ( 104 ) and the lens optical axis ( 103 ), variable y is the longitudinal distance between the point (b) and flat end surface ( 102 ).
[0036] The curve function is based applicant's creative realization that, in order to produce uniformly distributed energy on the focus spot after condensing, a better solution is to proportionally condense light onto the receiving surface ( 4 ) through the rotating convex surface ( 101 ) of the lens. That is, after incoming light ( 3 ) passes through an arbitrary point (B) on the curve ( 104 ) and is refracted to the receiving surface ( 4 ), the ratio between x and m, x being the abscissa of the point on the curve function, m being horizontal distance between the projection point on the receiving surface and optical axis of the lens, should be equal to the ratio between a and b, a being the radius of the lens, b being the half length of the projection line, i.e., x/m=a/b. Based on known rules of refraction for lens and above equations, the following equations can be obtained:
[0000]
x
/
m
=
a
/
b
(
1
)
sin
(
θ
)
=
n
sin
(
β
)
(
2
)
x
-
m
=
(
h
-
y
)
tan
(
β
-
θ
)
(
3
)
tan
(
θ
)
=
y
x
(
4
)
[0000] in which, variables and β represent respectively angle of incidence and angle of refraction when light beam passes through the curve. Other coefficients and variables are already explained above. Based on the above equations, the above curve function can be obtained through mathematical derivation.
[0037] As illustrated in FIG. 2 , the edge of each of the individual lens ( 1 ) is cut into polygon structure with at least three cylindrical surfaces ( 105 ); any two neighboring condensing lenses ( 1 ) in the compound-eye lens condenser are adhered together by their adjacent cylindrical surfaces ( 105 ). Evidently, that the purpose for doing such is for the convenience of forming planar arrays of condensing lenses ( 1 ) to produce a compound-eye lens condenser.
[0038] Specifically, the edge of each of the individual lens ( 1 ) is cut into quadrilateral structure with four cylindrical surfaces ( 105 ), in which, neighboring cylindrical surfaces ( 105 ) are perpendicular to each other; any two neighboring condensing lenses ( 1 ) in the compound-eye lens condenser are adhered together by their adjacent cylindrical surfaces ( 105 ) to form a rectangular array of the condensing lenses ( 1 ) for the compound-eye lens condenser.
[0039] Additional benefit of cutting the edge of the condensing lens ( 1 ) into quadrilateral structure is that the shape of focused light spot through the lens is quadrilateral, making it practical to make corresponding photovoltaic wafers ( 7 ) quadrilateral during manufacturing. Quadrilateral structure is easy to process during wafer cutting and such quadrilateral cutting saves large amount of wafer materials.
[0040] The following is a comparison of the energy distribution in the focused light spot between a spherical convex lens and the condensing lens ( 1 ) disclosed in the current invention, which is implemented in the compound-eye lens condenser of compound-eye concentrating-type solar cell assembly disclosed in the current invention. The focused light spot energy distribution of an ordinary spherical convex lens is illustrated in FIG. 4 , the brightness is the highest in the center of the light spot, and the brightness decreases abruptly toward the edge; a wave curve with abrupt drop is illustrated in FIG. 5 . FIGS. 4-5 show that energy is concentrated in the center of the light spot and not uniformly distributed. As illustrated in FIG. 6 , the rectangular light spot produced by the condensing lens ( 1 ) disclosed in the current invention has an uniformly distributed brightness; as illustrated in FIG. 7 , the curve is almost saddle-shaped, showing that the energy levels in different locations of the light spot are all close to the peak of the saddle-shaped curve, thus energy distribution is relatively uniform.
[0041] Further, the transmission rate of the condensing lens is proved by optical simulation to be as high as 90% to 93%, while the transmission rate of Fresnel lens is around 75%. It shows that the condensing lens disclosed in the current invention has a good transmission rate.
[0042] Additionally, it should be pointed out that the total energy of incident light in the above two experiments is adjusted to the same level, and the areas of light spot on the receiving surface are kept the same. As illustrated in FIG. 7 , the peak of the curve is not very smooth and fluctuates in certain range, the reason for that is, in the simulation; solar spectrum is simulated whose energy does not have a uniform distribution.
[0043] The condensing lens ( 1 ) disclosed in the current invention can also be implemented as illustrated in FIG. 8 . FIG. 8 show a double-convex lens with two rotating convex surfaces. Curve 106 and curve 107 , as illustrated in FIG. 8 , are produced by crossing between any longitudinal section ( 2 ) which contains the lens optical axis ( 103 ) and those two rotating convex surfaces. If, as illustrated in FIG. 8 , F is set as origin of the coordinate system(optical center of the lens), a is the radius of the lens, b is the perpendicular distance between the optical axis 103 and projection point on receiving surface 4 produce by the light beam refracted by the lens, point C(x, y) is the point of intersection between curve 106 and an arbitrary incoming light 3 , point D(x 1 , y 1 ) is the point of intersection between curve 107 and the incoming light 3 which has already been refracted by curve 106 , the incoming light 3 is refracted twice by the lens to produce a projection point E(m, h) on the receiving surface, γ is the angle between optical axis 103 and the normal line at point D on the curve 107 , is the incident angle, β is the refractive angle, ε is the incident angle at point D, α is the refractive angle at point D, where γ, , β, ε and α are all unknown variables, the following equations can be obtained:
[0000]
x
/
m
=
a
/
b
(
1
)
sin
(
θ
)
=
n
sin
(
β
)
(
2
)
tan
(
θ
)
=
y
x
(
3
)
tan
(
θ
-
β
)
=
(
x
-
x
1
)
/
(
y
+
y
1
)
(
4
)
sin
(
a
)
=
n
sin
[
γ
+
(
θ
-
β
)
]
(
5
)
tan
(
a
-
γ
)
=
(
x
1
-
m
)
/
(
h
-
y
1
)
(
6
)
tan
γ
=
y
1
x
1
(
7
)
[0044] In addition, the following boundary conditions are satisfied because both surfaces of the condensing lens are rotating convex surfaces:
[0045] If x=0, tan =0; if x 1 =0, tan γ=0.
[0046] The curve functions of curves 106 and 107 can thus be derived.
[0047] According to the two embodiments discussed above, the key to current invention is the idea that: x is the perpendicular distance between the point of intersection, where an arbitrary incoming light 3 intersecting the lens, and the optical axis 103 of the lens, m is the perpendicular distance between the projection point, generated by the refracted incoming light projected on the receiving surface 4 , and the center of the light spot, a is the radius of the lens, b is the radius of the light spot, then the condition x/m=a/b is satisfied by the lens. | A condensing lens, compound-eye lens condenser, and compound-eye concentrating-type solar cell assembly. The condensing lens is a convex lens that can reflect mutually parallel incident lights ( 3 ) onto a receiving surface ( 4 ) on the outer side of the lens and thus form spots. If the vertical distance from the contact point of any incident lights ( 3 ) contacting the lens to a light axis ( 103 ) of the lens is x, the vertical distance between a projection point formed from the incident light ( 3 ) reflecting onto the receiving surface ( 4 ) and the center of the spot is m, the radius of the lens is a, and the radius of the spot is b, then the lens meets the following condition: x/m=a/b. The condensing lens has a high transmission rate, and the energy distribution of the spots is more even after condensing, the transmission rate is 90% to 93%, and the energy distribution curve of the spots transmitted through the condensing lens is similar to saddle-shaped. | 8 |
CROSS REFERENCE TO RELATED APPLICATION
[0001] The present application claims priority to U.S. Provisional Application No. 61/666,301, filed Jun. 29, 2012 entitled “Templated Mass Production of Ultra-Sharp Metallic Probes for Near-Field Optical Microscopy,” the entire disclosure of which is incorporated herein by reference.
BACKGROUND OF THE INVENTION
[0002] The present invention relates generally to micro- and nano-scale patterned, metallic structures and methods of making such structures. More particularly, the present invention relates to metallic structures comprising precise, three-dimensional structures replicated from a patterned template substrate and methods of making such structures.
[0003] Several methods are known for fabricating patterned metal surfaces with features on a sub-micrometer or nanometer length scale. For example, in one method a metal film is deposited on a surface of a substrate such as by using thermal evaporation or sputtering. After depositions the metal film is patterned to have sub-wavelength scale features by conventional lithography steps such as by using photolithography or e-beam lithography. Alternatively, after deposition, focused ion beam (FIB) milling is used to pattern the metal film. Using either approach, sub-micrometer features can be formed in the metal film. These features, however, have several shortcomings. For example, one limitation is the surface roughness. Another limitation is the low throughput of lithography steps such as e-beam or FIB milling.
[0004] Additional known methods for fabricating patterned metal surfaces include nanoimprinting and nanomolding. Although nanoimprinting and nanomolding can pattern metals on the proper length scales, again, undesirable surface roughness is usually present in metal surfaces formed by nanoimprinting and nanomolding. In a typical proem, a patterned polymeric mold is filled with metal to form a replica. This produces undesirable surface roughness because metals do not easily wet the surfaces of the polymeric mold. Moreover, an additional shortcoming of nanoimprinting and nanomolding is that the polymeric mold needs to be etched away from the metal film to release the metal film. Accordingly, each mold can only be used once to produce a single metal film.
[0005] Another technique that can be used to fabricate smooth metal surfaces is generally referred to as template stripping. Template stripping utilizes the poor adhesion and good wettability of noble metals on solids such as mica, glass, and silicon. In a typical template stripping process, a freshly cleaved mica surface is coated with a film of gold. The exposed surface of the metal is then attached to another substrate with an epoxy adhesive. When the mica and substrate are separated the gold adheres to the substrate by the epoxy and is released by the mica surface. Such a method, however, is limited to use with generally flat surfaces and has not successfully been utilized with surfaces including three-dimensional features such as those typically found on patterned metal films. This is because the addition of three-dimensional features generally increases the area of mica in contact with gold. As this contact area increases it becomes more difficult to separate the gold film from the mica surface. Moreover, such three-dimensional features can interfere with separation of the gold from the three-dimensional surface features. Where a patterned metal having three-dimensional features is desired, the above nanoimprinting and nanomolding techniques are typically used wherein the mold is etched away from the metal film.
[0006] Yet another technique provides methods for replicating patterned metal films from a template substrate, the metal films being suitable for use in plasmonic devices and metamaterials. The template substrate is reusable and can provide plural copies of the structure of the template substrate. Moreover, because high-quality substrates that are inherently smooth and flat are available, patterned metal films can provide surfaces that replicate the surface characteristics of the template substrate both in the patterned regions and in the unpatterned regions. See, for example, PCT application WO 2010/065071 to the Regents of the University of Minnesota.
SUMMARY
[0007] The present disclosure provides advancements over conventional replicating and patterning techniques. This disclosure describes the formation of individual, precisely shaped nano- or micro-scale metallic structures. With this technique, mass fabrication of high-quality, uniform, and ultra-sharp pyramids, cones and wedges is achieved. The high yield, reproducibility, durability and massively parallel fabrication methods of this disclosure provide structures suitable for reliable optical sensing and detection and for cementing near-field optical imaging and spectroscopy as a routine characterization method.
[0008] Pyramidal, conical, and wedge structures formed in accordance with the present invention are smooth, highly reproducible, and comprise sharp tips with radii of curvature as small as 10 nm and even 5 nm, although smaller radii of curvature can be achieved.
[0009] The pyramids produced by the methods are suitable for single-molecule fluorescence imaging, tip-enhanced Raman spectroscopy (TERS), and other near-field or super-resolution imaging techniques. Single-molecule imaging with sub-20 nanometer spatial resolution and fluorescence enhancement factors of up to 200 can be achieved. Similar results can be obtained for TERS imaging of carbon nanotubes. Each pyramidal structure can be used on-demand, one at a time, and can be stored for extended periods of time without degradation.
[0010] A first particular embodiment of this disclosure is a method of making a plurality of three-dimensional, individual and unconnected metallic microstructures. The method includes masking a substrate (such as a silicon-based substrate or a semiconductor substrate) with a mask having a plurality of apertures therethrough, and etching the masked substrate to form a plurality of cavities in the substrate. The method further includes depositing a metallic layer over the mask and in the plurality of cavities in contact with the substrate, thus forming a metallic structure in each of the cavities. Subsequently, the method includes removing the metallic layer from over the mask, and removing the mask from the substrate to provide a plurality of individual metallic microstructures. A single step may used to remove the metallic layer from over the mask and the mask. Additionally or alternatively, the step of removing the metallic layer from over the mask may be done by physically stripping the metallic layer from the mask.
[0011] Another particular embodiment of this disclosure is a method of making a plurality of three-dimensional, individual and unconnected metallic microstructures. The method includes masking a substrate (such as a silicon-based substrate or a semiconductor substrate) with a mask having a plurality of apertures therethrough, and etching the masked substrate to form a plurality of cavities in the substrate. Subsequently, the method includes removing the mask from the substrate and applying a photoresist layer over the etched substrate, and then depositing a metallic layer over the photoresist and in the plurality of cavities in contact with the substrate, thus forming a metallic structure in each of the cavities. Rhe photoresist and the metallic layer are removed from the substrate to provide a plurality of individual metallic microstructures.
[0012] The metallic layer, and thus the resulting metallic microstructure, may comprise any of gold, silver, copper, tungsten, tantalum, molybdenum, titanium, nickel, cobalt, mixtures thereof and layers thereof. The silicon-based substrate may be a semiconductor material or a silicon wafer. In some embodiments, a non-silicon-based semiconductor substrate may be used. The individual metallic microstructures may be pyramids, cones, or wedges having a tip angle of 70.52 degrees, or, have a tip angle less than 70 degrees. The tip may have a radius of about 10 nm, or less than 10 nm, such as about 5 nm.
[0013] The microstructures, particularly those structures having an ultra-sharp tip, may have a protective coating such as aluminum oxide (Al 2 O 3 ) applied on the metallic structure to inhibit molecular migration and tip dulling.
[0014] The microstructures may have graded, stepped or otherwise patterned sidewalls, formed by the cavity surface having the inverse topography on the sidewalls. The patterned sidewalls may be made, for example, by self-aligned stencil lithography.
[0015] The microstructures may include an aperture therethrough at the tip; such an aperture is particularly suited for embodiments when the microstructure is illuminated internally. The aperture may be a circular aperture, a slot, or a C-shaped aperture.
[0016] These and various other features and advantages will be apparent from a reading of the following detailed description.
BRIEF DESCRIPTION OF THE DRAWINGS
[0017] The invention may be more completely understood in consideration of the following detailed description of various embodiments of the invention in connection with the accompanying drawings, in which:
[0018] FIG. 1A is a schematic plan view of a pyramidal metallic structure; FIG. 1B is a cross-sectional view of the structure of FIG. 1A .
[0019] FIGS. 2A-2H schematically illustrate steps of a method for forming high-quality, uniform, ultra-sharp, metallic structures.
[0020] FIG. 3A is a scanning electron microscope (SEM) image of a plurality of high-quality, uniform, ultra-sharp, pyramidal metallic structures prior to being removed from the mold; FIG. 3B is an enlarged SEM image of a single pyramidal metallic structure prior to being removed from the mold.
[0021] FIG. 4 is an SEM image of a pyramidal metallic structure after being removed from the mold.
[0022] FIG. 5 is an SEM image of a side view of a pyramidal metallic structure.
[0023] FIG. 6 is a cross-sectional view of a metallic structure.
[0024] FIG. 7 is a cross-sectional view of another embodiment of a metallic structure.
[0025] FIG. 8 is a cross-sectional view of another embodiment of a metallic structure.
[0026] FIG. 9 schematically illustrates a step of a method for forming the metallic structure of FIG. 8 .
[0027] FIG. 10 is a cross-sectional view of yet another embodiment of a pyramidal metallic structure.
[0028] FIGS. 11A-11I schematically illustrate steps of a method for forming the metallic structure of FIG. 10 ; FIG. 11J is an alternate step of a method for forming an alternate metallic structure; FIG. 11K is another alternate step of a method for forming another alternate metallic structure.
[0029] FIG. 12 is a top view of an embodiment of a pyramidal metallic structure configured for internal illumination.
[0030] FIG. 13 is a top view of another embodiment of a pyramidal metallic structure configured for internal illumination.
[0031] FIG. 14 is a schematic side view of a set-up used for near-field imaging.
[0032] FIGS. 15A and 15B are images from near-field fluorescence imaging; FIG. 15C is a graph showing the fluorescence rate as a function of tip-molecule separation.
[0033] FIGS. 16A and 16B are images from near-field Raman imaging; FIG. 16C is a graph shown the Raman scattering spectrum.
[0034] FIG. 17A is a schematic diagram illustrating a pyramidal nanostructure tip and a dipole;
[0035] FIG. 17B is a graph showing the backwards radiation efficiency of the dipole as a function of wavelength.
DETAILED DESCRIPTION OF THE INVENTION
[0036] The present disclosure provides a method for mass fabrication of high-quality, uniform, ultra-sharp, metallic structures that have features and dimensions in the nano- and micro-scale. Briefly, the method includes masking a substrate (e.g., a monocrystalline substrate) with a mask that has at least one aperture, and etching the exposed substrate to create a cavity in the substrate. A metallic layer is deposited onto the mask and into the cavity in contact with the substrate. The mask, and the metallic layer present thereon, is stripped from the substrate, leaving the metallic layer and thus a three-dimensional structure in the cavity. A pyramidal metallic structure can be made from a symmetrical (e.g., circular) aperture in the mask, whereas an elongated metallic structure, such as a wedge, can be made from an elongated aperture in the mask. The resulting metallic structure is precise with smooth surfaces and sharp edges and corners. The precise shape of the resulting structure can be modified by the type of etching used, e.g., crystallographic etching, plasma etching, etc. and by modifying various steps. Additionally, the metallic structures can undergo various post-processing steps.
[0037] In the following description, reference is made to the accompanying drawings that form a part hereof and in which are shown by way of illustration several specific embodiments. The following description provides additional specific embodiments. It is to be understood that other embodiments are contemplated and may be made without departing from the scope or spirit of the present disclosure. The following detailed description, therefore, is not to be taken in a limiting sense. While the present disclosure is not so limited, an appreciation of various aspects of the disclosure will be gained through a discussion of the examples provided below.
[0038] Unless otherwise indicated, all numbers expressing feature sizes, amounts, and physical properties are to be understood as being modified by the term “about.” Accordingly, unless indicated to the contrary, the numerical parameters set forth are approximations that can vary depending upon the desired properties sought to be obtained by those skilled in the art utilizing the teachings disclosed herein.
[0039] As used herein, the singular forms “a”, “an”, and “the” encompass embodiments having plural referents, unless the content clearly dictates otherwise. As used in this specification and the appended claims, the term “or” is generally employed in its sense including “and/or” unless the content clearly dictates otherwise.
[0040] Referring to FIGS. 1A and 1B , a pyramidal metallic structure 10 is illustrated. Structure 10 has a base 12 , sidewalls 14 that converge at tip 15 , and wall edges 16 where adjacent sidewalls 14 intersection and base edges 18 wherein sidewalls 14 intersect with base 12 . The particular structure illustrated, pyramidal structure 10 , is a four-sided pyramid, having four sidewalls 14 of equal dimension and a square base 12 . A wedge (not illustrated) would have two parallel sidewalls having a length greater than the other two sidewalls; the two elongate sidewalls would converge at an elongate tip. Returning to FIGS. 1A and 1B , sidewalls 14 and edges 16 are straight, uncurved, and high quality. Tip 15 is sharp, having a curvature of radius of, for example, less than 10 nm. Structure 10 has dimensions (both base 12 and sidewall 14 dimensions) of less than 10 micrometers, although structures having dimensions large as 50 micrometers could readily be made. Similarly, structures 10 with dimensions as small as 1 micrometer could readily be made. Additional discussion regarding the dimensions of structure 10 is provided below.
[0041] Seen in FIG. 1B , sidewalls 14 of structure 10 have an outer surface 17 and an inner surface 19 . As will be apparent from the discussion below, outer surface 17 is defined by the surface of the cavity in which structure 10 is made. Outer surfaces 17 of sidewalls 14 intersect to form tip 15 with angle α. Sidewalls 14 have a thickness, between outer surface 17 and inner surface 19 , of between 30 and 250 nm, although sidewalls 14 could be thicker or thinner, depending on the method of making structure 10 and the intended use of structure 10 .
[0042] Structure 10 is formed by a template technique that has been shown to produce a variety of metallic structures, including ultra-sharp tips, with ultra-smooth patterned metallic surfaces. The structure is of such high quality because of the high-quality silicon or silicon-based mold in which it is made. In some embodiments, sidewalls 14 have a roughness that approaches that of the silicon mold, as measured by atomic force microscopy. For example, sidewalls 14 have a root mean square (rms) roughness of less than 1 nm (e.g., less than 0.9 nm, or less than 0.75 nm, or leaven less than 0.5 nm). The smoothness of the metal microstructure is generally limited by the silicon substrate and the method used to pattern the silicon template.
[0043] As an example, for a silicon substrate with a root mean square (rms) roughness of 0.19 nm, a roughness 0.65 nm was measured for a silver structure formed in that substrate, the largest contribution to this value being the grain boundaries in the polycrystalline silver. Within a single grain, the rms roughness was 0.26 nm, much closer to that of the silicon. No techniques were used, such as ultra-flat wafers or high-temperature deposition, to decrease the roughness.
[0044] FIGS. 2A through 211 illustrate a method for making structure 10 in a silicon or silicon-based substrate. FIG. 2A shows a Si 3 Ni 4 mask 20 (e.g., approximately 100 nm thick) with a plurality of apertures 22 therein. Apertures 22 are illustrated as circular, but may be any shape. Because the size of apertures 22 affects the size of the resulting structure 10 , apertures 22 can be any size, although in most embodiments, apertures 22 are within the range of 1 to 50 micrometers. For a pyramidal structure, such as structure 10 , apertures 22 have generally equal lateral and longitudinal dimensions; that is, apertures 22 generally symmetric in both direction; examples of such apertures 22 include circles and squares. For a wedge structure, the apertures are longer in one dimension that the other; examples of such apertures include rectangles. The distance between adjacent apertures 22 may be, for example, within the range of 25 to 100 micrometers, e.g., 50 micrometers. Apertures 22 can be formed by standard photolithography exposure, development, and etching, either prior to or after mask 20 is positioned on the silicon or silicon-based substrate (e.g., silicon wafer, glass, or Si substrate) which will eventually be the mold. In FIG. 2B , mask 20 with aperture 22 is positioned on a conventional silicon wafer 24 .
[0045] A subsequent crystallographic etch, such as with potassium hydroxide (KOH), creates inverted pyramidal cavities 26 in Si wafer 24 ( FIG. 2C ). This anisotropic etching process exposes the {111} crystal facets of the silicon, which join to form an open angle of 70.52 degrees. The etching process and recipe will affect the smoothness and sharpness of the sidewalls and edges. An example of a suitable process includes prolonged over-etching (1 hour or more) in a mixture of 30% KOH, 10% isopropyl alcohol (IPA) and water at 80° C.
[0046] In FIG. 2D , a metal is deposited over mask 20 and into cavity 26 , resulting in a metal layer 28 and metal structure 30 . The metal can be any of the noble metals like silver, gold, copper, tungsten, tantalum, molybdenum, and titanium, as well as refractory metals, semiconductors, oxides, and magnetic materials, for example, and can be applied by, for example, evaporation or sputtering. In some embodiments, metal layer 28 and metal structure 30 may be formed of multiple layers and/or of multiple metals. As illustrated in FIG. 2D , metal structure 30 is not connected to metal layer 28 , but is separate therefrom. This occurs when cavity 26 undercuts mask 20 , resulting in a portion of cavity 26 positioned below and thus masked by mask 20 .
[0047] After the metal deposition ( FIG. 2D ), metal layer 28 is removed (e.g., stripped or physically lifted off), leaving mask 20 and metal structure 30 in cavity 26 , as seen in FIG. 2E . Metal layer 28 may be removed by chemical methods, or may simply be removed by physically stripping or peeling layer 28 off. For example, an adhesive and its carrier may be applied to layer 28 and then pulled off after sufficiently adhered to layer 28 , resulting in layer 28 being removed with the adhesive and its carrier. Cellophane tape and Scotch® tape are examples of suitable pressure-sensitive adhesive products that can be used to remove metal layer 28 . After removal of metal layer 28 , mask 20 is removed from wafer 24 , for example, by a hydrofluoric acid lift-off bath, leaving metal structure 30 in cavity 26 , as seen in FIG. 2F .
[0048] After removal of mask 20 , remaining is Si wafer 24 with a metal structure 30 in each cavity 26 . Multiple metal structures 30 may be removed at a time or metal structures 30 may be removed individually. To remove multiple structures 30 , an adhesive material 32 (e.g., an epoxy) can be applied over Si wafer 24 and into cavities 26 . Adhesive 32 has a higher bonding force with metal structure 30 than with wafer 24 , thus allowing adhesive 32 to lift metal structure 30 out from cavity 26 , as in FIG. 2H . Adhesive 32 can then be dissolved, releasing individual metal structures 30 .
[0049] The above-outlined method is relative fast and cost efficient, as it does not require the use of slow and expensive nanofabrication tools such as FIB milling or electron-beam lithography. The use of standard photolithography allows parallel fabrication of thousands, hundreds of thousands, and even millions of metallic structures on a single 4 inch wafer, each with uniform properties. The thousands or millions of metallic structures can be simultaneously made, but individually retained for later use. FIG. 3A is a scanning electron microscope (SEM) image of a portion of a Si wafer having multiple, individual and unconnected metallic structures positioned in cavities in the wafer mold, and FIG. 3B shows a single structure in the mold.
[0050] FIG. 4 is a scanning electron microscope (SEM) image of a single pyramidal metallic structure removed from the mold and mounted on a 15 micrometer diameter tungsten wire. The single structure was removed from the mold cavity by attaching the wire to the structure with epoxy adhesive and then lifting the structure out of the mold.
[0051] FIG. 5 illustrates a metallic structure formed by the process described above; particularly, FIG. 5 shows the ultrasharp, nano-scale tip of the structure. In the illustrated embodiment, the tip has an angle of 70.52 degrees (due to the crystal facets of the silicon) with a radius of curvature of about 10 nanometers or less. It is noted that the large apex angle (i.e., 70.52 degrees) is particularly well suited for optical imaging applications, particularly to scatter near-field optical signals into far-field, as is discussed below. Additionally, the structures are particularly suited as probes for single-molecule fluorescence, single-molecule tip-enhanced Raman spectroscopy (TERS), and other techniques where the local field enhancement must be large and lateral imaging resolution must be high. It was found that over 95% of the metallic structure pyramids tested, made by the process described above, were useable for near-field imaging and provided similar resolution, both in fluorescence and Raman scattering. A method utilizing thermal oxidation of the silicon template, to adjust or tune the tip angle to an angle other than 70.52 degrees, if desired, is described below.
[0052] FIG. 6 schematically shows a cross-section of a pyramid structure made by the process described above; shown are two opposing sidewalls (e.g., sidewalls 14 of FIGS. 1A and 1B ). Structure 40 has a first sidewall 42 having an outer surface 44 and an inner surface 46 that define a thickness there between. On the opposite side, structure 40 has a second sidewall 43 having an outer surface 45 and an inner surface 47 that define a thickness there between. The two sidewalls 42 , 43 meet at tip 48 . When crystallographic etching is used to form structure 40 in a Si wafer mold, tip 48 has an angle of 70.52 degrees. Structure 40 is symmetrical, and sidewalls 42 , 43 have the same thickness.
[0053] An alternate embodiment is shown in FIG. 7 , where a cross-section of an asymmetric pyramidal structure is shown. Structure 50 has a first sidewall 52 having an outer surface 54 and an inner surface 56 that define a thickness there between. On the opposite side, structure 50 has a second sidewall 53 having an outer surface 55 and an inner surface 57 that define a thickness there between. The two outer surfaces 54 , 55 meet at tip 58 and the two inner surfaces 56 , 57 meet at interior tip 59 . When crystallographic etching is used to form structure 50 in a Si wafer mold, both tip 58 and interior tip 59 have an angle of 70.52 degrees. Although structure 50 is symmetrical on its exterior, sidewall 53 has a greater thickness than sidewall 52 and interior tip 59 is not aligned with tip 58 . Structure 50 can be used for, e.g., optical applications that desire non-even or non-symmetric illumination.
[0054] Structure 50 is formed by generally the same steps as outlined above in reference to FIGS. 2B through 2H , except that the metal deposition ( FIG. 2D ) is applied at an angle to wafer 24 and cavity 26 , rather than directly straight on or orthogonal thereto.
[0055] Another embodiment is shown in FIG. 8 , wherein a cross-section of a symmetrical, yet non-linear pyramidal structure having an ultra-sharp tip is shown. Structure 60 has a sidewall 62 having an outer surface 64 and an inner surface 66 . Two opposite sidewalls 62 meet at tip 68 , which has an angle less than 70.52 degrees. For example, tip 68 may have an angle between about 27 and 70 degrees. Exemplary structures include tips that have an angle of 54 degrees and a radius of curvature of 33 nanometers, an angle of 54 degrees and a radius of curvature of 26.8 nanometers, an angle of 44.4 degrees and a radius of curvature of 14.3 nanometers, and an angle of 27.5 degrees and a radius of curvature of 8.9 nanometers. Additionally, both outer surface 64 and inner surface 66 are non-linear, having an arcuate portion proximate tip 68 .
[0056] Structure 60 can be formed by generally the same steps as outlined above in reference to FIGS. 2B through 2H , except that prior to the metal deposition, the mask is removed and the surface of cavity 26 is oxidized (e.g., via thermal oxidation), forming a layer of SiO 2 in the cavity.
[0057] Because of the constricted area at the tip of cavity 26 , the growth of the SiO 2 is hindered, leaving a sharp well at the bottom of cavity 26 , as illustrated in FIG. 9 . FIG. 9 shows cavity 26 in Si wafer 24 having a SiO 2 layer 65 lining cavity 26 . The thickness of SiO 2 layer 65 is generally constant except for near the tip of cavity 26 , where SiO 2 layer 65 narrows in thickness. The angle of the resulting tip can be tuned by adjusting the thickness of the SiO 2 . After SiO 2 layer 65 is present, the entire surface of SiO 2 layer 65 can be coated with a metal layer (e.g., Au, Ag). The metal in the cavities can then be masked with a photoresist to protect the structures from a subsequent etching step, which removes the metal connecting the structures. The remaining metal structure can be removed by filling the structure with adhesive (e.g., epoxy) and pulling the structure from the cavity.
[0058] Alternately, structure 60 can be formed by, after forming cavities 26 , coating and then patterning photoresist on the Si wafer 24 so that only cavities 26 remain exposed. The surface of cavities 26 is oxidized (e.g., via thermal oxidation), forming a layer of SiO 2 in the cavity. After SiO 2 layer 65 is present in cavity 26 , a metal layer (e.g., Au, Ag) can be applied, and then the photoresist is removed. Alternatively, other layers that do not adhere well to metal(s) can be deposited on the silicon to reshape the tips and edges of the pyramid.
[0059] Onto this structure, photoresist layer (e.g., photoresist layer 88 of FIG. 11E ) is applied over wafer 84 and oxide layer 96 , and then metal is deposited. The resulting metallic structure has non-linear side walls, such as structure 60 of FIG. 8 .
[0060] The previous embodiments of the structures (e.g., structure 10 of FIGS. 1A and 1B , structure 40 of FIG. 6 , structure 50 of FIG. 7 , and structure 60 of FIG. 8 ) have all been four sided pyramids. FIG. 10 shows an embodiment of a cone, having a circular base. Similar to the pyramidal embodiments, conical structure 70 of FIG. 10 has a sidewall 72 having an outer surface 74 and an inner surface 76 , both which are linear in this embodiment. Sidewall 72 forms a tip 78 , which has an angle, for example, between about 27 and 70 degrees. Again similar to the pyramidal embodiments, structure 70 is formed by a technique that has been shown to produce a variety of metallic structures, including ultra-sharp tips, with ultra-smooth patterned metallic surfaces.
[0061] Conical structure 70 can be made by the following method. A cylindrical cavity is formed in a silicon-based substrate (e.g., Si wafer) using photolithography and plasma etching (similar to the process of FIGS. 2A through 2C ). A conformal dielectric film (such as SiO 2 or Al 2 O 3 ) is deposited on the exposed wafer surface. The sharp edges and walls of the cylinder will be covered with a coating of the film, forming a circular cross-sectional structure with non-linear or rounded walls, similar to that of FIG. 9 . A metal layer is applied into the cavity (similar to the process of FIG. 2D ), creating a sharp tip in the middle of the cavity. The dielectric film and metal are stripped (either sequentially, as per the process of FIGS. 2E and 2F , or in one step), resulting in a metallic, non-linear cone in the cavity. The radius of curvature of the tips of thus-formed metallic cones are as sharp as that of template-stripped pyramids (e.g., 5 nm, 10 nm).
[0062] FIGS. 11A through 11I illustrate an alternate method for making pyramidal metallic structure 10 . FIG. 11A shows a Si 3 Ni 4 mask 80 (e.g., 100 DM thick) with a plurality of circular apertures 82 therein. Because the size of apertures 82 affects the size of the resulting structure 10 , apertures 82 can be any size, although in most embodiments, apertures 82 are within the range of 10 to 50 micrometers. Apertures 82 can be formed by standard photolithography exposure, development, and etching, either prior to or after mask 80 is positioned on the wafer or other silicon-based substrate which will eventually be the mold. In FIG. 11B , mask 80 with aperture 82 is positioned on a conventional silicon wafer 84 . A subsequent etch, such as a wet KOH etch, creates a pyramidal cavity 86 in Si wafer 84 ( FIG. 11C ).
[0063] In FIG. 11D , mask 80 has been removed from wafer 84 (e.g., via etching either hydrofluoric acid (HF) or phosphoric acid (H 3 PO 4 ), or by physically stripping) leaving cavity 86 . A photoresist layer 88 is applied over wafer 84 in FIG. 11E , leaving the area over cavity 86 open.
[0064] In FIG. 11F , a metal (e.g., silver, gold, copper, tungsten, tantalum, molybdenum, titanium, refractory metal, semiconductor, oxide, or magnetic material) is deposited (e.g., by evaporation or sputtering) over photoresist 88 and into cavity 86 , resulting in a metal layer 90 on water 84 and metal structure 92 in cavity 86 . After the metal deposition, metal layer 90 and photoresist 88 are removed, for example, by dissolving photoresist 88 in acetone or other suitable solvent, leaving wafer 84 with a metal structure 92 in each cavity 26 .
[0065] As described in above in respect to FIGS. 2G and 2H , multiple metal structures 92 may be removed at a time or metal structures 92 may be removed individually. To remove multiple structures 92 , an adhesive material 94 (e.g., an epoxy) can be applied over wafer 84 and into the cavities and metal structure 92 . Metal structure 92 can then be lifted out from cavity 86 , as in FIG. 11I , after which adhesive 94 can be dissolved, releasing individual metal structures 92 . The remaining wafer 84 with cavities 86 can be reused.
[0066] Various alternate and optional features may be incorporated in to or in with the structures described above and/or made by the described methods.
[0067] FIG. 11J illustrates a process where the surface of cavity 86 is oxidized (e.g., via thermal oxidation), forming a layer 96 of SiO 2 in cavity 86 . Onto this structure, photoresist layer (e.g., photoresist layer 88 of FIG. 11E ) is applied over wafer 84 and oxide layer 96 , and then metal is deposited. The resulting metallic structure has non-linear side walls, such as structure 60 of FIG. 8 . Additionally, the resulting metallic structure has a tip (e.g., tip 68 of FIG. 8 ) that is less than 70.52 degrees. For example, tip 68 may have an angle between about 27 and 70 degrees. Exemplary structures include tips that have an angle of 54 degrees and a radius of curvature of 33 nanometers, an angle of 54 degrees and a radius of curvature of 26.8 nanometers, an angle of 44.4 degrees and a radius of curvature of 14.3 nanometers, and an angle of 27.5 degrees and a radius of curvature of 8.9 nanometers.
[0068] As another variation, the metallic structure may have graded, stepped or otherwise patterned sidewalls, formed by the cavity surface having the inverse topography on the sidewalls. The patterned sidewalls may be made, for example, by self-aligned stencil lithography. FIG. 11K illustrates a process where the surface of cavity 86 includes a plurality of topographical features 98 . Onto this structure, photoresist layer (e.g., photoresist layer 88 of FIG. 11E ) is applied over wafer 84 and cavity 86 with features 98 , and then metal is deposited. The resulting metallic structure has sidewalls with the inverse pattern of features 98 .
[0069] As indicated briefly above, the ultra-sharp and ultra-smooth metallic structures are particularly suited for optical sensing and detection and in near-field optical imaging and spectroscopy. In some of these applications, the structures, particularly their tips, are illuminated externally. In other applications, the structures can be illuminated internally; in the embodiments where the structures are illuminated internally, the structure is preferably filled with an optically transparent material, such as transparent epoxy. In FIGS. 12 and 13 , two embodiments of pyramidal structures adapted for internal illumination are illustrated. In FIG. 12 , structure 100 has a C-shaped aperture 102 located at the tip or apex of structure 100 , and in FIG. 13 , structure 105 has a circular aperture 107 located at the tip or apex of structure 105 . Such apertures 102 , 107 can be formed via focused ion beam (FIB) milling of the metal layer while still in the cavity (see, for example, FIG. 2F , which illustrates metal structure 30 in cavity 26 ). See, for example, “Ultrahigh light transmission through a C-shaped nanoaperture” by Xiaolei Shi, Lambertus Hesselink and Robert Thornton (Optics Letters, Vol. 28, No. 15, pp 1320-1322, Aug. 1, 2003).
[0070] As yet another option, particularly for those structures having an ultra-sharp tip (e.g., tip angles of about 45 degrees or less, or, a tip with a radius of 5 nm or less), a protective coating can be applied on the metallic structure to inhibit molecular migration and tip dulling. For example, a sharp gold tip will dull over time due to the atomic migration of the Au molecules. A suitable protective coating is an ultra-thin (i.e., less than 5 nm thick, in some embodiments about 2 nm thick) coating of aluminum oxide (Al 2 O 3 ). A 2 nm thick Al 2 O 3 coating on Au can maintain a 2 nm radius on the tip.
[0071] As indicated briefly above, the metallic structures are particularly suited for optical sensing and detection and in near-field optical imaging and spectroscopy. The following discussion provides details of near-field and Raman imaging experiments.
[0072] FIG. 14 illustrates an experimental set-up used for near-field imaging using a pyramidal structure. The sample to be viewed is placed onto an x-y piezo scan-stage on top of an inverted confocal optical microscope. An atomic force microscope scan head is placed on top of the microscope, allowing the pyramidal nanostructure tip to be positioned in the center of the optical focus. A tightly focused radially-polarized optical excitation (i.e., laser beam) is used, providing a strong longitudinal electric field at the optical focus and giving maximum electric field enhancement from the pyramidal tip. The sample is raster-scanned below the pyramidal tip, allowing for simultaneous topographical and optical images. The tip—sample separation (approx. 5 nm) is maintained by using either shear-force or dynamic normal mode feedback. Photons emitted from the sample are collected by the objective and sent to either an avalanche photodiode (MD) or a spectrometer and liquid nitrogen cooled charge coupled device (CCD).
[0073] FIGS. 15A and 15B show corresponding confocal and near-field fluorescence images of single dye molecules recorded with a pyramidal nanostructure tip. FIG. 15A is the confocal fluorescence image (contrast enhanced 5-fold), and FIG. 15B is the near-filed fluorescence image of the same sample area acquired with a pyramidal nanostructure tip. The full-width-half maximum (FWHM) of individual fluorescence spots is 18 nm. In both FIGS. 15A and 15B , the scale bar is 200 nm.
[0074] In these experiments, a He—Ne laser (λ=632.8 nm, P=21 nW) was used to match the absorption line of Atto 647N dye molecules. The large fluorescence enhancement due to the pyramidal tip allowed for a very low near-filed imaging excitation power of 21 nW, minimizing unwanted photobleaching of molecules within the confocal excitation volume. Single dye molecule samples were prepared by spin-casting a dilute dye solution onto coverglass coated with a thin (approx. 2 nm) layer of polymer (PMMA) to increase the photo-stability of the dye molecules. In the detection path, a 650 nm long-pass filter was placed in front of the APD to reject the laser excitation.
[0075] Although the resolution of confocal fluorescence imaging was too limited to identify individual molecules, near-field fluorescence imaging not only resolved individual molecules but also identified the orientation of the molecular transition dipole axis. Molecules oriented along the axis of the pyramidal structure (z-axis) revealed an optical enhancement of around 200-fold and an optical resolution of 18 nm, both due to the pyramidal tip. In-plane molecules exhibited a characteristic double-lobe pattern, FIG. 15C shows the fluorescence emission rate of a single z-oriented dye molecule as a function of the pyramid-sample distance. A maximum fluorescence rate enhancement of approximately 200-fold was observed. The resolution and enhancement far exceeded that of an 80 nm gold sphere that has been used in previous near-field fluorescence imaging.
[0076] Pyramidal structure probes with nanostructure tips were also tested for near-field Raman imaging. The pyramidal structures of this disclosure allowed for higher measurement reproducibility than tips produced by chemical etching, and for better quantitative models because of the well-defined probe geometry. To demonstrate the feasibility of using the pyramidal structures for TERS and near-field Raman imaging, a sample of carbon nanotubes (CNTs) produced by arc-discharge method were used, because the same tube bundle can be located and measured repeatedly.
[0077] FIGS. 16A through 16C are directed to near-filed Ram scattering from single-wall carbon nanotube bundles grown by arc-discharge.
[0078] FIG. 16A shows a near-field image of the Raman G band (G-band intensity at ν=1600 cm −1 ) from the bundle, excited with a 785 nm laser, and the corresponding topographic image for an arc-discharge CNT bundle. The scale bar is 250 nm. The cross section of the near-field optical signal (arrow in FIG. 16A ) yielded a width of 40 nm (see FIG. 16A inset). This 40 nm corresponds to the convolution of the optical field localization (the resolution) with the actual width of the nanotube bundle. The corresponding topographic image, FIG. 16B , shows a nanotube bundle width of 6.2 nm. The spectra of the CNT bundle with the tip close to the surface and retracted are shown in FIG. 16C . Taking the ratio of these two spectra for a Raman band, provides a measure of the enhancement factor, which in this case was approximately 10.
[0079] Finite-Difference Time-Domain (FDTD) calculations were performed for both pyramidal nanostructure tips and conical nanostructure tips of variable tip angle α and for different wavelengths λ. The calculations were used to determine the radiative properties of a quantum emitter placed in front of a tip. The tip was irradiated from the front by a focused higher-order laser beam. The same objective lens that was used for focusing was also used to collect photons due to the tip-sample interaction. Thus, it was evident that the signal-to-noise depends on the fraction of power that is radiated in the backwards direction, away from the tip and towards the objective lens. The fraction of power that was radiated in the forward direction coupled predominantly to surface plasmons propagating along the sides of the tip. The energy associated with these modes was ultimately dissipated to heat, although a structured tip shaft could be used to release some of this energy into the far-field.
[0080] To calculate the fraction of power radiated in a backwards direction, an electric dipole was placed at a distance of 3.75 nm in front of a gold nanostructure tip and used to evaluate the radiation patterns. The dipole orientation was parallel to the nanostructure tip axis. Perfectly matched layers were used at the boundaries to avoid spurious reflections and to evaluate the backwards radiation (BR) efficiency, defined as the power flux through the bottom half space (z<0) normalized with the corresponding power radiated by an isolated dipole in free space. Accordingly, the BR efficiency in absence of the tip was one. Calculations were performed for both pyramidal structures and conical structures with variable tip angles α; the results were similar, and thus, only the data for pyramidal tips is shown in FIG. 16C . Note: a tip represents an infinitely extended structure and that terminating its length for computational reasons can generate severe artifacts. This is even the case if perfectly absorbing layers are used. It is thus necessary that the computational window is comparable to or larger than the surface plasmon propagation length. Because the latter increases with wavelength, memory and processing time constraints prevent accurate calculation of the BR efficiency at near-infrared wavelengths.
[0081] Theoretical results, shown in FIGS. 17A and 17B , show that the BR efficiency increases as the wavelength λ and the cone angle α is increased as expected, because plasmon propagation along the tip shaft becomes strongly mode-mismatched for large a. It was found that increasing the angle α from 10 to 70 degrees enhanced the backwards radiation by more than a factor of 10 at a wavelength of λ=650 nm. This enhancement was due not only to a redistribution of the radiation pattern but mostly to electromagnetic back-action, by which the tip enhances the dipole's ability to release energy. Thus, an enhanced BR efficiency corresponds to an increased radiative decay rate. This increased BR efficiency thus prevents a quantum emitter from complete quenching and allows high quality near-field fluorescence imaging on samples with single molecules.
Experimental Method
[0082] The following non-limiting procedure was used to form nanoscale pyramidal structures using template stripping techniques of the present disclosure.
[0083] First, 100 nm of low-stress nitride was grown on new Si wafers. A photoresist (“MEGAPOSIT SPR-955” photoresist, from Rohm and Haas) was spin-coated on the wafers and exposed with an i-line stepper (Canon 2500 i3) using a mask to produce 5, 10, 15, and 20 micrometer diameter holes. The photoresist was developed (using “MF CD 26” developer from Rohm and Haas) for 70 seconds using a spray developer (“CEE 200X from Brewer Science). Next, using the resist as an etch mask, the nitride was etched using a reactive ion etching system (model 320 from Surface Technology Systems) with CF 4 . The resist was then removed with an oxygen plasma and the wafers were put in a bath of 30% KOH, 10% isopropyl alcohol, and water for 90 minutes at 80° C. for the anisotropic etching. After etching, the wafers were rinsed for 30 minutes and cleaned with a 1:1 solution of sulfuric acid and hydrogen peroxide, removing any excess KOH salt crystals, and dried. Next, 200 nm of Au was evaporated on the patterned wafers using an electron-beam evaporator (CHW, SEC600). Next, the wafers were soaked in 49% hydrofluoric acid for 20 min to remove the nitride mask, giving isolated Au pyramids.
[0084] Thus, embodiments of the METHOD OF FORMING INDIVIDUAL METALLIC MICROSTRUCTURES are disclosed. Presented is a highly reproducible and effective method for the fabrication of precise pyramidal nanostructures and assembly of high-quality near-field probes. The implementations described above and other implementations are within the scope of the following claims. One skilled in the art will appreciate that the present invention can be practiced with embodiments other than those disclosed. The disclosed embodiments are presented for purposes of illustration and not limitation, and the present invention is limited only by the claims that follow. | Methods for the formation of individual, precisely shaped nano- or micro-scale metallic structures, particularly pyramids. With this technique, mass fabrication of high-quality, uniform, and ultra-sharp pyramids, cones and wedges is achieved. The high yield, reproducibility, durability and massively parallel fabrication methods of this disclosure provide structures suitable for reliable optical sensing and detection and for cementing near-field optical imaging and spectroscopy as a routine characterization. | 8 |
BACKGROUND OF THE INVENTION
I. Field of the Invention
This invention pertains to the art of polymers, and more particularly, to polymer modifying agents for use in increasing the shelf life of rubber compounds.
II. Description of the Related Art
The short shelf life of uncured rubber has been a problem in the industry for quite some time. Oxygen and light activate the sulfur cure system and the accelerators in the rubber, causing premature curing, completely destroying the rubber. Different additives have been added to the virgin rubber to modify the properties of the rubber.
Mixing additives with virgin rubber is well known in the art. One known type is described in U.S. Pat. No. 5,650,454 to Hoover et al. Hoover et al disclose a rubber additive which increases tear resistance when added to a rubber compound. This compound comprises a cross-linked fatty acid, starch, and an asphalt carrier. One drawback of the Hoover patent is that the asphalt-based processes give a lower yield than the present invention, and the individual compounds are more toxic. A problem that is not addressed by the Hoover patent is the long-term storage of the tires. The current invention allows for an increased shelf life of the rubber. Another drawback of the Hoover patent is the length of time needed to process the compound.
Another known type of rubber additive is disclosed in U.S. Pat. No. 5,710,200 to Toratani et al. Toratani et al disclose natural rubber, containing viscosity stabilizers, treated with a strainer after compounding hydrazide stearate into the natural rubber. Storage hardening is purportedly suppressed and a decrease in molecular weight is prevented. One drawback of the Toratani patent is the toxicity of the hydrazide compound.
The present invention contemplates a new polymer-modifying agent for use in increasing the shelf life of uncured rubber, and for dispersing silica in the rubber compound. Thus, this invention is simple in design, effective in use, and overcomes the foregoing difficulties and others while providing better and more advantageous overall results.
SUMMARY OF THE INVENTION
In accordance with one aspect of the present invention a new and improved polymer-modifying agent includes a zeolite, a catalyst, and a starch. The zeolite, catalyst and starch are blended together with a high-speed blender.
In accordance with another aspect of the present invention the polymer- modifying agent also includes a lubricant, and dispersing means for dispersing silica and carbon black. The lubricant is a high molecular weight fatty acid, preferably stearic acid. The dispersing means is a combination of an aliphatic hydrocarbon resin and a rubber processing oil.
In accordance with yet another aspect of the invention the compound comprises 32-42% by weight of the zeolite, 0.5-7% by weight of lubricant, 3-13% by weight of the starch, 2-12% by weight of the catalyst, 15-35% by weight of the aliphatic hydrocarbon resin, and 6-21% by weight of the rubber processing oil.
One advantage of the present invention is the improved tear strength of the rubber.
Another advantage of the current invention is the increased shelf life of the rubber.
A further advantage of the current invention is that the compounds used are non-toxic.
Still another advantage of the current invention is the increased dispersion of the mineral fillers, and the stabilization of scorch and cure rates.
Yet another advantage of the current invention is that the compound is a simple mechanical blend, that is consistent in its production.
Still other benefits and advantages of the invention will become apparent to those skilled in the art upon a reading and understanding of the following detailed specification.
DESCRIPTION OF THE PREFERRED EMBODIMENT
It has been seen throughout the development of chemicals for the rubber and plastic industry that certain compounds can help in the production or processing of the rubbers and plastics. Use of such compounds as stearic acid, and other high molecular-weight fatty acids, aid in dispersion of filler materials, such as carbon black, in the compound and in the time element involved in the milling of these elastomers. The chemicals used as process improvement modifiers are usually organic chemicals, very few, if any, being organo-metallic in nature. The current invention uses an inclusion process aid, and for the first time a compound can truly extend the shelf life of a rubber compound by a minimum of one month or longer.
In the preferred embodiment, the modifying agent comprises a zeolite-based material. The zeolite, which has a morphology of cavities, incorporates the starch, high molecular weight fatty acid, the catalyst, the processing oil, and the aliphatic resin. The preferred zeolite is a magnesium-alumino silicate, but any anionic zeolite, including sodium-magnesium-alumino silicate, calcium-alumino silicate, and calcium-magnesium-alumino silicate, may be used. The zeolite acts as a molecular sieve, trapping smaller compounds in the geometric spaces created by the structure of the zeolite. The zeolite has large enough spaces that the polymer chains in the rubber compound can fit inside the zeolite. In the preferred embodiment, the zeolite also incorporates the starch, processing oil, fatty acid, and resin, in order to create the inventive compound.
Any kind of starch maybe used, however, cornstarch is preferred because it is relatively inexpensive. The starch helps improve tear strength of the rubber.
The preferred high molecular weight fatty acid is stearic acid, again due to its relative cost. The fatty acid works as a lubricant and a dispersive aid in the rubber. The invention would work without the use of a fatty acid; however, the preferred embodiment includes this fatty acid. The fatty acid helps to disperse the inventive compound throughout the rubber.
Calcium chloride may be used as a catalyst to begin the reaction; however, any Lewis acid would work as a catalyst in this reaction. Calcium chloride is chosen for the preferred embodiment because it is relatively inexpensive.
Any rubber processing oil known in the art, and any aliphatic hydrocarbon resin known in the art, may be used. However, in the preferred embodiment, the processing oil used is the Sunthene™ series by SunOil™. The aliphatic hydrocarbon resin used in the preferred embodiment is terpene resin.
EXAMPLE 1
Natural Rubber/Sbr Samples
______________________________________Compound: Natural Rubber/SBR (Proprietary) 3% of New InventionWeek# Scorch Time(T.sub.s 2) Cure Time(T.sub.c (90) Shore A______________________________________Control 4.22 6.47 45.671 3.95 6.25 47.252 3.88 6.10 43.333 3.73 5.95 42.0055 3.97 6.20 45.00______________________________________
The inventive compound creates stereohindrance of oxidation and light. The compound is so large that it ties up the polymer chains in the rubber. The polymer chains in the rubber are encapsulated in the zeolite, which in effect blocks any light or air from coming in contact with the rubber. In the preferred embodiment, the inventive compound is added at 2-5 parts per hundred with the rubber. There is no significant measurable difference between the ranges of 2-5 parts per hundred of the inventive compound. However, anything in excess of 5 parts per hundred of the inventive compound begins a regression to a softer rubber. The compound is added as the rubber is being milled, and the talc or calcium carbonate filler and carbon black are being added. Alternatively, the compound can be added when the pigments are added.
As seen in Example 1, a proprietary natural rubber/SBR (styrene-butadiene rubber) compound showed excellent data on the effect on scorch time, cure time, and Shore A hardness. [The scorch time is defined as the initiation time for the rubber curing process, and the cure time is defined as the end time, when the rubber has been completely cured. The Shore A hardness is measured on a Shore durometer, and is a scale from 0-100 (0 being the softest, 100 being the hardest) determining the hardness of the rubber.] The natural rubber/SBR compound was tested without the inventive compound and EXAMPLE 1 shows the results of that test. In another sample, the inventive compound was then added at 3% by weight and tested after the first week, EXAMPLE 1 again showing the data for that. The compound was then successively tested on week 2 and week 3, EXAMPLE 1 showing the data for those particular tests. EXAMPLE 1 shows no measurable effect on scorch time, cure time, or Shore A hardness. The compound was also tested after a 55-week storage period, again showing little measurable effect on the scorch or cure times.
EXAMPLE II
Natural Rubber Eraser Samples
______________________________________Compound: Proprietary Natural Rubber ErasureCompound, 3% of Invention Compound AddedWeek# Scorch Time(T.sub.s 2) Cure Time(T.sub.c (90) Shore A______________________________________Control 1.28 2.30 45.331 1.27 2.13 43.33______________________________________
A proprietary natural rubber eraser compound, which is extremely sensitive to air and light pre-cure, was tested as a control and the data for that test is shown in EXAMPLE 2. In another sample, 3% by weight of the inventive compound was then added to the proprietary natural rubber eraser compound and the compound was tested after one week, EXAMPLE 2 showing little measurable effect on scorch time, cure time, or Shore A hardness. The proprietary natural rubber eraser compound usually pre- cures in air within one to two days. However, with the inventive compound added, after one week of storage no measurable difference on scorch or cure time was shown.
EXAMPLE III
Highly Loaded Silica/Rubbber Samples
______________________________________Compound: Proprietary Automotive Compound UsingD-706 SBR and Budene 1207. Compound Highly Loaded with Silica.Special Testing to Show No Changes on Same Processing,Control and Control + 3% of Invention Added. CompressionCompound 100% MOD Rebound Set % Silica Incorp______________________________________Control 780 26.6 22.5 2Control + 3% 864 27.5 22.4 1Invention added______________________________________
The inventive compound also acts as a good silica dispersion aid in highly loaded compounds. Most tires are composed of a significant percentage of silica (up to 70% by weight) as a filler in the rubber, because the supply of virgin rubber is limited. However, this silica is not uniformly distributed throughout the rubber. The silica can build up static electricity, which, in large enough quantities, can be dangerous. The processing oil and aliphatic resin act as dispersing agents in the rubber compound. The oil and resin are able to disperse the silica in a highly loaded compound. The oil and resin ensure that the silica is evenly distributed throughout the rubber. This even distribution of silica creates a more even wear on the rubber, which in turn allows for a longer life for the rubber.
EXAMPLE 3 shows that a highly loaded silica compound shows no change in physicals. Highly loaded silica compound is defined as 30-70% silica by weight. A first sample of a proprietary automotive compound highly loaded with silica, was tested and EXAMPLE 3 shows the results of that data. In another sample, 3% by weight of the inventive compound was then added and no measurable difference was shown in the 100% modulus, rebound percentage, or a compression percentage. [The modulus is defined as the stiffness of the rubber, the rebound is defined as the percentage that the rubber rebounds back to its original form after stretching, the compression set is defined as the percentage that the rubber returns to its original shape after being compressed, and the silica incorporation is defined as the percentage at which the silica is dispersed throughout the rubber.] These results also show the strong potential of the inventive compound as a good silica dispersion aid in highly loaded compounds.
EXAMPLE IV
Compound Preparation
The inventive compound is created by a mixture of the following powders: a zeolite, a catalyst, a fatty acid, a starch, a rubber processing oil, and a resin. The powders are charged in a Henshel blender. The powders are blended at 25000 rpm for 5-10 minutes. The temperature created in the blender is between 130-140° F. This temperature activates the catalyst, which provides the reaction creating the inventive compound. In the preferred embodiment the compound comprises 37% by weight of zeolite, 2% by weight of stearic acid, 8% by weight of corn starch, 7% by weight of calcium chloride, 30% by weight of the aliphatic resin, and 16% by weight of the processing oil. The zeolite can range between 32-42% by weight, the stearic acid 0.5-7% by weight, the corn starch 3-13% by weight, the calcium chloride 2-12% by weight, the resin 15-35% by weight and the oil 6-21% by weight. The average rubber additive for the elastomer industry has to undergo a chemical reaction between two or more raw materials under reaction kettle conditions in production. Many parameters such as temperature, pre-cure, and mix rate are necessarily controlled. It is found that these reaction products are costly and vary from production to production. The inventive compound is a high-speed physical blend which, by the shear and torque of the Henshel blender, is chelated together and production of the compound is constant from batch to batch. The compound will work without the stearic acid, the resin, or the oil, but the compound will not have the dispersive effect that it has with these compounds added.
The invention has been described with reference to the preferred embodiment. Obviously, modifications and alterations will occur to others upon a reading and understanding of the specification. It is intended by applicant to include all such modifications and alterations insofar as they come within the scope of the appended claims or the equivalents thereof. | A polymer modifying agent for use in increasing the shelf life of natural rubber. The polymer modifying agent consists of a zeolite, a high molecular weight fatty acid, a starch, a catalyst, and rubber processing oil and aliphatic resin. The compound bonds with the rubber, particularly the polymer chains of the rubber being encapsulated by the zeolite, preventing the aging effect caused by oxidation and light. The compound also acts to disperse the silica evenly throughout the rubber. The inventive compound is also composed of components that are non-toxic. A method of blocking the effects of premature curing of rubber is also provided. The method includes a step of adding the inventive compound to the rubber. | 2 |
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to a washing machine or laundry machine equipped with an optical sensor for detecting the light permeability of a detergent solution or rinse water in a washer tank.
2. Description of the Prior Art
A washing machine of the type referred to above, namely, a washing machine equipped with an optical sensor for detecting the light permeability of a solution of washing detergent, i.e., for detecting the amount of light that can penetrate the detergent solution, been disclosed in Japanese Patent Laid-open Publication No. 61-50595. More specifically, the washing machine of Tokkaisho 61-50595 is provided with an optical sensor comprised of light emitting and light receiving elements confronting each other in a washer tank, whereby the light permeability of the detergent solution in the washer tank is detected using an output of the light receiving element. A control circuit to which is generated an output of the optical sensor obtains data depicting the dirt content of the laundries on the basis of the time period consumed from the start of washing until the light permeability detected by the optical sensor decreases to a predetermined value (20% of the light permeability of clear water), and the washing machine is operated according to the dirt content data of the control circuit.
Meanwhile, a washing machine disclosed in Japanese Patent Laid-open Publication No. 61-159999 has been devised taking note of the fact that the light permeability detected by the optical sensor gradually increases after the start of washing, and thereafter it gradually decreases. A time point at the interface between the increase and decrease of the light permeability is set as an initial value of the data. In this washing machine, the type of detergent and the like are detected on the basis of both the time spent before the light permeability reaches the interface point after the start of washing, and the changing width of the light permeability.
In the washing machine disclosed in Japanese Patent Laid-open Publication No. 61-50595, however, if the light emitting surface of the light emitting element or the light receiving surface of the light receiving element is stained, the light intensity coming from the light emitting element to the light receiving element lessens to thereby diminish an output from the light receiving element. Accordingly, the light permeability detected by the optical sensor is a lower value than the actual value of the light permeability of the detergent in the washer tank. In consequence, the light permeability detected by the optical sensor reaches the predetermined value after the start of washing more quickly in comparison to the case where the elements are not stained. Therefore, the dirt content degree is erroneously detected. Particularly, since during use of the washing machine laundries and detergent are put in the washer tank, the light emitting and receiving elements provided in the washer tank are unavoidably stained. Moreover, the amount of the stain is generally increased in proportion to the usage time of the washing machine. As a result, the detecting accuracy of the optical sensor is deteriorates with time. Accordingly, the optical sensor cannot be relied upon for a long service in the detection of the dirt content of laundries.
Meanwhile, the change in the light permeability of the detergent solution in the washer tank is greatly influenced by the type of the detergent being used. Liquid detergent changes the light permeability significantly less than powdery detergent, and the light permeability of liquid detergent may not be reduced as to 20% of that of clear water. In such case, it is impossible to obtain the dirt content data. Therefore, the washing machine disclosed in Tokkaisho 61-50595 is not able to control washing operation in a manner which is responsive to the type of the detergent being used.
On the other hand, the washing machine disclosed in Tokkaisho 61-159999 is designed to detect the type of cleanser. However, according to the disclosed detecting method the type of the detergent can be detected only when the detergent is supplied into the tank before the water is added at the start of washing. In other words, if the detergent is put into the tank after the start of washing (after the start of stirring), the light permeability detected by the optical sensor declines after the start of washing. However, since the washing machine is arranged to operate based on the notion that the light permeability detected by the optical sensor increases at the start of washing and then, gradually decreases, the washing machine cannot detect the type of the detergent if the detergent is put into the tank after the start of washing. In addition, the change in the light permeability of the optical sensor is dependent not only on the type of detergent, but is also dependent on the amount of the detergent, and accordingly the light permeability detected by the optical sensor does not always follow a constant pattern of increasing once after the start of washing and thereafter decreasing.
SUMMARY OF THE INVENTION
A primary object of the present invention is to provide a washing machine which is arranged to detect the dirt content of the laundries with a high degree of accuracy, even when light emitting and light receiving elements of an optical sensor are stained.
A second object of the present invention is to provide a washing machine which is arranged to control washing and rinsing operation without being influenced by the staining on the optical sensor.
A third object of the present invention is to provide a washing machine which is arranged to control washing and rinsing operations using the data of the volume of laundries in a washer tank and the light permeability detected by an optical sensor.
A fourth object of the present invention is to provide a washing machine which is arranged to correctly detect the type of detergent in use without being influenced by the amount of the detergent used or the time the detergent is placed into the washer tank.
A fifth object of the present invention is to provide a washing machine which is arranged to control washing and rinsing operations in accordance with the type of detergent in use.
A sixth object of the present invention is to provide a washing machine which is arranged to control washing and rinsing operations on the basis of three data sets, namely data directed to the volume of laundries in a washer tank, the light permeability detected by an optical sensor and the type of detergent being used.
In accomplishing the above-described objects, a washing machine according to a first embodiment of the present invention is provided with an optical sensor comprised of a light emitting element and a light receiving element for detecting the light permeability of a detergent solution and rinse water in a washer tank, an output control unit for controlling an output generated from the light emitting element, and a storage unit. The control unit controls the light emitting element such that the light permeability of water or air in the washer tank becomes a reference value for the storage unit. In the washing machine, a reference value of the light permeability of supplied water is made different from that of air. An output of the light emitting element is controlled by the output control unit based on the reference value of the light permeability of the water or air, which is determined by a signal from a water level detecting unit.
Moreover, the above output control based on the reference value of supplied water is effected when the water level detecting unit detects the water as not being lower than a predetermined level. The data of outputs of the light emitting element or data of the light permeability when the optical sensor is set at the reference value is stored in the storage unit, which is utilized for a succeeding output control.
According to a second embodiment of the present invention, the washing machine is provided with an optical sensor comprised of a light emitting and light receiving elements for detecting the light permeability of a detergent solution and rinse water in a washer tank, an output control unit for controlling an output from the light emitting element, a storage device, and a control unit for controlling washing and rinsing operations. The output control unit controls the light emitting element such that the light permeability of water or air fed into the washer tank becomes a reference value, to thereby initialize the optical sensor. Moreover, the control unit controls the washing or rinsing operation based on the change of the light permeability indicated by the optical sensor. The output control is carried out during the supply of clear water. The washing operation is controlled by the saturating time from the start of washing until the light permeability of the optical sensor becomes approximately constant, and the changing width of the light permeability of the optical sensor, so that an additional washing time from the saturating time point is arranged on the basis of the changing width of the light permeability.
According to a third embodiment, the washing machine is provided with an optical sensor comprised of a light emitting and light receiving elements for detecting the light permeability of a detergent solution and rinse water in a washer tank, a storage device, a control unit for controlling washing and rinsing operations, and a volume sensor for detecting the volume of laundries in the washer tank. The control unit controls the washing or rinsing operation based on the data of the volume sensor and the changing width of the light permeability of the optical sensor indicated during washing or rinsing operation. Moreover, according to this embodiment, the control unit sets the upper and lower limits of the washing time from the volume of laundries detected by the volume sensor.
According to a fourth embodiment of the present invention, the washing machine is provided with an optical sensor comprised of a light emitting and a light receiving elements for detecting the light permeability of a detergent solution and rinse water in a washer tank, and a judging unit for judging the detergent. The judging unit judges whether liquid detergent or powdery detergent is used through comparison of a reference light permeability of the optical sensor which is based on the light permeability of water or air fed into the washer tank with the light permeability of the optical sensor shown during the washing operation.
According to a fifth embodiment of the present invention, the washing machine is provided with an optical sensor comprised of a light emitting and a light receiving elements for detecting the light permeability of a detergent solution and rinse water in a washer tank, a judging unit for judging a detergent type, and a control unit for controlling washing and rinsing operations. The judging unit judges the kind of detergent type, i.e., liquid or powder, through comparison of a reference light permeability of the optical sensor with the light permeability indicated during the washing operation, whereby the control unit controls washing or rinsing operation in accordance with the judged detergent type.
According to a sixth embodiment of the present invention, the washing machine is provided with an optical sensor comprised of a light emitting and a light receiving elements for detecting the light permeability of a detergent solution and rinse water in a washer tank, a volume sensor for detecting the volume of laundries in the washer tank, a judging unit for judging the detergent type, and a control unit for controlling washing and rinsing operations. The control unit controls the washing or rinsing operation based on the data of the laundry volume detected by the volume sensor and the detergent type judged by the judging unit.
In the washing machine of the first embodiment of the invention, an output of the light emitting element is controlled based on a reference value of the light permeability of water or air which has a high light permeability, to initialize the optical sensor. Consequently, the dirt content of the laundries is detected by the relative change of the light permeability from that of water or air, without being influenced by stains at a drainage path in which the optical sensor is provided, thus accomplishing an accurate detection of dirt content.
Moreover, since the light permeability of water is different from that of air, the reference value is changed between water and air, so that the initial setting of the optical sensor is enabled both in the case of water and in the case of air. Further, if the water level detecting device detects no water, the light emitting element of the optical sensor is controlled on the basis of the reference value of air. On the contrary, if water is detected by the detecting device, the light emitting element is controlled on the basis of the reference value of water. Moreover, the light emitting element is controlled during a previous supplying time of rinse water such that an output signal of the optical sensor becomes a set value, and this controlling data is stored. Therefore, at the coming start of washing, the light emitting element is so controlled by the stored controlling data as to generate an output of a fixed value, to thereby detect the change of data after washing and stirring. In the case where only the air is present in the washer tank before the start of washing, since it is feared that the optical axis of each element of the optical sensor may be deviated because of the adhesion of water drops, an output of the light emitting element is controlled relatively larger as compared in the case where there is clear water in the tank. Although the output signal from the optical sensor becomes a Hi level and may exceed beyond the dynamic range when the water is actually fed in the tank, the data stored in the storage device is useful to solve such problem. Therefore, the change of the output signal due to the real dirt content can be detected.
Further, in the second embodiment of the present invention, the light permeability is detected by the optical sensor after the sensor is initialized, so as to control the washing or rinsing operation. Accordingly, the optical sensor positively works for a long period of time without being affected by staining. Moreover, the optical sensor is initialized during the supply of rinse water, the light permeability of the clear water can be used as a reference value. Since washing is controlled by the saturating time spent before the saturating time point of the change of the optical sensor and by the changing width of the output of the optical sensor, the quality of stains related to the saturating time and the volume of stains related to the output changing ratio of the optical sensor can be detected, to thereby facilitate an optimum control of washing and rinsing operations.
In the washing machine according to the third embodiment of the present invention, washing by detergent solution or by clear water can be controlled in consideration not only of the dirt content of the laundries shown by the optical sensor, but also in consideration of the laundry volume in the washer tank. Therefore, the washing machine can operate in the similar manner as if it were by a user's own control.
According to the fourth embodiment of the present invention, taking note of the fact that the type of a detergent can be known through comparison of the light permeability after the start of washing with that when the water is not supplied, that is, the light permeability of air as a reference, in the case where liquid detergent is used, for example, the light permeability after the start of washing is reduced to approximately 80% based on the reference light permeability of the air, while, in the case of powdery detergent, the light permeability after the start of washing is decreased to about 40-60%. Therefore, this conspicuous change of the light permeability enables the judgement as to the type of the detergent.
Since the change of the output from the optical sensor is detected while rinse water is being supplied, namely, based on the light permeability of clear water, the relative change of the output is approximately equivalent to the change corresponding to the absolute volume of dirt content, and therefore it becomes possible to detect the volume of dirt content. In the case of powdery detergent, the output change of the optical sensor caused only by the dirt content of the detergent solution is approximately 50% and accordingly, the change thereafter, i.e., over 50% corresponds to the amount or degree of dirt. In other words, it becomes possible to detect the presence of the detergent and the dirt content thereof by the present embodiment.
According to the fifth embodiment of the present invention, since washing is arranged to be controlled in accordance with the detergent type, and data of types which greatly affect the detection by the optical sensor is added, washing or rinsing control with high accuracy can be realized.
According to the sixth embodiment of the present invention, since the data of detergents types and the data of volume of the laundries are added to the dirtiness data obtained by the optical sensor, washing can be performed under more accurate control.
BRIEF DESCRIPTION OF THE DRAWINGS
These and other objects and features of the present invention will become apparent from the following description taken in conjunction with preferred embodiments thereof with reference to the accompanying drawings in which throughout like parts are designated by like reference numerals and in which:
FIG. 1 is a circuit diagram of an optical sensor of a washing machine according to one embodiment of the present invention;
FIG. 2 is a block diagram showing the circuit structure of the washing machine of FIG. 1;
FIG. 3 is a flow-chart showing the controlling operation of the washing machine of FIG. 1;
FIG. 4 is a graph showing the change of an output of the optical sensor of FIG. 1;
FIG. 5 is a table showing judging contents in the controlling operation of the washing machine of FIG. 1;
FIG. 6 is a cross sectional view of the washing machine;
FIG. 7 is a circuit diagram of an optical sensor of a washing machine according to a modified embodiment of the present invention;
FIG. 8 is a graph showing an output of the optical sensor of FIG. 7;
FIG. 9 is a flow chart showing the setting of the optical sensor at the start of washing;
FIG. 10 is a flow chart showing the change detecting operation of the optical sensor;
FIG. 11 is a flow chart of a subroutine for setting and storing an output of the optical sensor to a reference value;
FIG. 12 is a flow chart showing the controlling operation of the optical sensor before washing;
FIG. 13 is a graph showing the relation between the dirt content degree and the changing ratio of an optical sensor output V1 with respect to an optical sensor output Vo during the supply of water;
FIG. 14 is a timing chart of an output signal of the optical sensor from the start of washing to drying;
FIG. 15 is a graph showing the controlling contents for the washing time;
FIG. 16 is a flow chart showing the controlling operation of washing; and
FIG. 17 is a flow chart showing the output controlling operation for the optical sensor.
DESCRIPTION OF PREFERRED EMBODIMENTS
Referring to FIGS. 1-6, the structure of an automatic washing machine according to one preferred embodiment of the present invention will be described.
The washing machine shown in FIG. 6 is provided with a washer tank 1 which serves also as a dryer tank (hereinafter referred to as a washer tank). A stirring vane 2 is rotatively placed in the bottom section inside the washer tank 1. A water reservoir 3 housing the washer tank 1 is supported by a main body 5 of the washing machine through a suspension 4, so that the water reservoir 3 is restricted from vibrating. A lid 5a which is freely openable and closable is provided in the upper portion of the main body 5. There is a motor 6 below the water reservoir 3, the rotation of which is transmitted to the stirring vane 2 through a transmission mechanism 7. At the time of drying, the transmission mechanism 7 also transmits the rotating force of the motor 6 to the washer tank 1. Further, a water exit 9 formed in the bottom portion of the water reservoir 3 is communicated to a drain valve 10 through a drainage path 11. A light emitting and receiving unit 8 comprised of a light emitting element and a light receiving element is installed in a part of the drainage path 11.
Referring to a block diagram of FIG. 2, the circuit construction of the washing machine will be described hereinbelow.
In FIG. 2, an alternating current source 12 supplies power to a control unit 13, the motor 6 provided with a phase advancing capacitor 14, the drain valve 10 and a feed valve 15. The control unit 13 has a microcomputer 16 which is the center of the controlling operations. At an input of the microcomputer 16 are connected a cover opening/closing detecting device 17 which detects whether the lid 5a is opened or closed, a water level detecting device 18 for detecting the water level within the washer tank 1, an optical sensor 19 including the light emitting and receiving unit 8 which detects the light permeability of a detergent solution and rinse water in the washer tank 1, and a volume detecting device 20 for detecting the volume of laundries in the washer tank 1 using the change of a terminal voltage of the capacitor 14 when the motor 6 is turned off. The volume detecting device 20 counts the number of pulses of the capacitor 4 when the motor 6 is controlled in the normal or reverse rotation thereof or the motor 6 is turned off, and determine that there are a relatively large amount of laundries in the washer tank when the number of pulses is small. On the other hand, at an output side of the microcomputer 16 is connected a switching device 21 which controls the load of the motor 6 and the like in response to an output signal from the microcomputer. Moreover, the microcomputer 16 is further connected with an operation display device 22 for transmitting and receiving signals therewith.
The above-mentioned control unit 13 will operate in the following manner.
In the first place, when the microcomputer 16 receives a start signal from the operation display device 22, the microcomputer carries out the programmed operation processes that is, washing using a detergent solution, rinsing using clear water and drying. More specifically, when the water is supplied in the washing process, the microcomputer 16 controls the feed valve 15 to be opened and the drain valve 10 to be closed through the switching device 21. In the middle of the supply of water, when the water level is low, the motor 6 is driven to rotate the stirring vane 2 for a predetermined time. Immediately after the rotation of the motor 6 is stopped, the microcomputer 16 reads a signal from the volume detecting device 20 so as to determine the volume of the laundries from the attenuating change of the terminal voltage of the capacitor of the motor 6. Consequently, a water stream, washing time, rinsing time, drying time, etc., which are appropriate for the detected volume of laundries are determined, and each process is carried out.
Referring now to FIG. 1, the specific structure of the optical sensor 19 which is a main feature of the present invention will be explained.
The microcomputer 16 is provided with a PWM output terminal 16a which freely controls an output pulse width. An output pulse from the PWM output terminal 16a is, via a D/A converter 19a, inputted to a base of a transistor 19b. In other words, an anode current in a light emitting diode 8a which is a light emitting element of the light emitting and receiving unit 8 and connected to a collector of the transistor 19b is controlled in accordance with the pulse width. The D/A converter 19a and transistor 19b constitute a current variable means for the light emitting element. A phototransistor 8b which is a light receiving element for receiving light from the light emitting diode 8a has an emitter connected to a resistor 19d, and an output signal V e (light permeability) of the phototransistor 8b can be output as a voltage. This output signal Ve is connected to an A/D input terminal of the microcomputer 16 to be A/D converted.
The microcomputer 16 controls the optical sensor 19 as follows.
Referring to a flow chart of FIG. 3, the water level detecting device 18 detects the presence or absence of water in the washer tank 1 in step 140. Without water, the current of the light emitting diode 8a is increased in step 141 and, the optical sensor is initialized such that the output voltage Ve of the phototransistor 8b becomes a reference value Vo in step 142. That is to say, the light permeability of air is set as a reference value. The pulse width from the PWM output terminal 16a should be increased when the current of the light emitting diode 8a is to be increased. Because of this initial setting of the optical sensor, a decrease in the detecting accuracy due to the decline of the output voltage of the phototransistor 8b resulting from the staining of the surface of the light emitting diode 8a or phototransistor 8b can be prevented. In the case where the water is already supplied in the washer tank 1, the optical sensor is set with the current of the light emitting diode 8a employed in the previous operation, in step 143. Then, in step 144, a constant current is fed to the light emitting diode 8a. It is detected in step 145 whether the washing process is selected. In the event that the washing process is not selected, the flow proceeds to a succeeding process in step 146 (for example, rinsing process). In the washing process, if there is no water in the tank 1, the volume detecting device 20 detects the volume of laundries, and the water is fed to a predetermined water level, and thereafter the stirring vane 2 is rotated to produce the water stream. The change in the output voltage Ve of the phototransistor 8b after the start of stirring is indicated in the graph of FIG. 4 in which lines A and B show the voltage Ve change when a powder detergent is used, and a line C indicates the change when a liquid detergent is used. If washing is completed before a time point T1 (e.g., the user sets the washing time period shorter than T1), the operation flow advances to a next process (steps 147 and 148). In step 149, the output voltage Ve is set to be Ve1 at the time point T1 after the start of washing. In step 150, it is judged whether Ve1 is larger than the judging value Vx set for judging the type of detergent. If Ve1>Vx holds (in the case shown by line C in FIG. 4), a flag denoting liquid detergent is set in step 151. Or, if Ve1≦Vx holds (in the case shown by lines A and B in FIG. 4), a flag denoting powder detergent is set up in step 152. Since the light permeability of the liquid detergent is decreased to 80% in comparison with the reference value Vo, which is the light permeability when no water is present in the washer tank, namely, the light permeability of the air, while the light permeability of powder detergent is lowered to 40-60%, Vx is set to be at about the middle of the light permeability between the liquid and powder detergents, to thereby enable the detection of the detergent type. The changing ratio ΔVe of the output voltage Ve is detected in step 153. It is regarded as a saturating point of the light permeability when ΔVe is smaller than a set value. A difference of ΔV between the reference value Vo of the light permeability of air and the output voltage Ve1 is obtained in step 154. The time to the saturating point is T3.
With reference to a table of FIG. 5, how the difference ΔV and the time T3 are utilized for the control of washing will be described.
In FIG. 5, the difference ΔV and the time T3 are classified into three groups, respectively, large, middle and small. By way of example, when both ΔV and T3 are small, the washing time is shortened, whereas, when both ΔV and T3 are in the middle group, the washing time is ordinary (middle). In the manner as above, data on the difference ΔV and time T3 is fuzzy-controlled for washing.
Furthermore, according to the present invention, washing can be controlled by three data sets, i.e., volume data of laundries detected by the volume detecting device 20 in addition to the data of ΔV and T3, which will be described hereinbelow.
In other words, the judging result from ΔV and T3 is classified into three groups, namely, large, middle and small. By comparing the result with the washing time determined by the volume of laundries detected by the detecting device 20, the washing time is controlled 3 minutes longer in the event that the result is large. If the result is middle, the washing time is maintained as it is. On the other hand, if the result is small, the washing time is shortened by two minutes. Thus, washing can be controlled in an optimum manner. If the washing time is determined from the total point of view based on the detected volume of the laundries W1 and the dirt content W2 (determined by ΔV and T3), washing can be controlled as if it were done by the user himself or herself, with the volume and dirt content of laundries taken into consideration as when the user selects the washing time.
Although the foregoing description is related to the detecting of the dirt content and to the controlling operation therefor in the washing process, the same also holds true in the rinsing process.
Since ΔV changes in accordance with the detergent type as shown in FIG. 4, the value ΔV classified in the groups, large, middle and small in FIG. 5 may be changed corresponding to the detergent type. Moreover, the detecting accuracy of the saturating point of dirt may be rendered variable corresponding to the type of detergent.
In the foregoing embodiment, since the optical sensor is set at the initial stage when the clear air is in the washer tank, the detection of dirt is based on the relative change of the light permeability from that of air, and accordingly the detection is free from influences of stains in the drainage path where the optical sensor is installed or the stains interfering with the light detection of the optical sensor, thereby realizing an accurate detection of dirt.
In addition, since it is possible to detect the detergent type by the relative change of the output of the optical sensor between the time when the air is in the washer tank and after the start of washing, the data of the detergent type can be utilized for an accurate detection of dirt and accordingly for an accurate control of washing.
Hereinafter, an optical sensor and its control circuit of a washing machine according to a modified embodiment of the present invention will be explained with reference to FIG. 7.
In FIG. 7, a pulse width controlling circuit (referred to a PWM circuit hereinafter) for controlling the current of the light emitting diode 8a in the light emitting and receiving unit 8, and an A/D converter for converting an analog signal to a digital signal is built in the microcomputer 16. A storage device 23 stores a control signal for controlling the current of the light emitting diode 8a (output controlling signal), namely, it stores data of PWM signals. This storage device 23 uses, for example, a non-volatile memory. The PWM signal from the microcomputer 16 is added to the D/A converter 19a (generally, an integrating circuit) to be converted to a direct current voltage to thereby control the voltage at the base of the transistor 19b. The collector of the transistor 19b is connected to the light emitting diode 8a, and the emitter thereof is connected to an emitter resistor 19c, thereby constituting a constant current circuit able to control the current of the light emitting diode 8a responsive to the base voltage. A switching transistor 19e is connected in series to the emitter resistor 19c, so that the current of the light emitting diode 8a is controlled on and off and pulse-driven by an output signal P1 of the microcomputer 16. A load resistor 19f of the phototransistor 8b, an emitter follower circuit of a transistor 19g, a resistor 19h and a capacitor 19i form a peak hold circuit so as to stabilize an output signal of the pulse-driven light emitting and receiving unit 8, thus reducing errors in A/D conversion.
The change of an output of the optical sensor 19 in the entire process of operation is indicated in the graph of FIG. 8. In this case, the change denotes a change after the current of the light emitting diode 8a is controlled to generate a preset output. As is clear from FIG. 8, the light permeability during washing is detected by the change of the output of the optical sensor from the reference value Vo which is set when the rinse water is supplied (the light permeability is represented by ΔV/Vo×100% wherein ΔV indicates the difference between the output V1 and reference output Vo). The light permeability expresses the dirt content and cleanliness of the laundries. Also, the change of the output from the clear water at the time of rinsing is seen from FIG. 8.
FIG. 9 is a flow chart showing how the optical sensor is set at the start of washing. Upon supply of the power in step 212, it is detected in step 213 whether or not the current I F of the light emitting diode 8a is set. If I F is set, the set value is inputted from the storage device (memory) 23 in step 214, and the microcomputer 16 sets If by the PWM signals based on the inputted data in step 215. If I F is not set in step 213, it is adjusted in step 216, and the PWM signal is controlled such that the output signal Vc of the optical sensor 19 is a set value, thereby controlling the output of the D/A converter circuit 19a of FIG. 7. The data read out from the storage device 23 is the data set at the previous rinsing time.
The detecting flow of the change of the output of the optical sensor 19 during the washing process is indicated in FIG. 10.
The light emitting diode 8a is pulse-driven at a set level periodically in step 221 to input data of outputs Vc of the optical sensor 19. Since the output data includes bubbles and noise components, such data at an extraordinarily low level is removed, and only signals of a suitable level are taken out in step 222. The changing ratio of the data Vc is obtained in step 223, and judged in step 224 whether it is a predetermined ratio. The light permeability when the changing ratio, becomes a predetermined ratio and the saturating time are stored in step 225 to determine the washing time in step 226. When the determined washing time has passed, washing is completed in step 227. Then, discharging of water and drying are carried out in step 228. After it is detected in step 229 whether the rinse water is filled in the tank, the current of the light emitting diode 8a is controlled such that the output signal Vc of the optical sensor 19 shows the reference value Vo.
A flow chart of FIG. 11 explains the controlling process when the output signal of the optical sensor is set to be the reference value Vo.
In step 232, the current If of the light emitting diode 8a is controlled. In step 233, the switching transistor is turned on to input the signal Vc of the optical sensor 19 into the microcomputer 16 for A/D conversion. Then, the switching transistor 19d is turned off in step 235. A difference ΔX between the reference value Vo and the input signal Vc is calculated in step 236. In step 237, PWM control is performed such that the difference ΔX is within a predetermined value. If the difference is within the predetermined value, the output controlling data is stored in the storage means 23, and the optical sensor 19 is fixed by the stored data thereafter turning on and off the current of the light emitting diode 8a.
In the above-described embodiment, the output voltage of the optical sensor is set at the reference value at the supplying time of the rinse water, so that the dirt content or cleanliness of the laundries is detected by the change of the output voltage from the reference value. In general, the water supplied as rinse water has 100% light permeability. Therefore, the light permeability or dirt content of the water can be detected by the changing ratio of the output voltage of the optical sensor with respect to the reference value. Particularly, for detecting the dirt content of the laundries at the time of washing, the change of the light permeability from the clear water will carry out the detection.
Further, since the previous reference value is arranged to be stored in the storage device 23, it may be useful during case where washing is continuously performed subsequent to the previous one (in the case where water drops are still adhered to the optical sensor 19 because of the previous washing, resulting in an erroneous detection). Accordingly, no complicated control is required even in the continuous washing.
The controlling process without the output controlling data will be described with reference to FIG. 12.
In the event that the output controlling data is not found in step 240, or the data is found to be inappropriate, the presence or absence of water is detected in step 241. If the water is found to be above the minimum water level in step 241, that is, if there is some water in the washer tank, the output voltage of the optical sensor is set at the reference value Vo in step 243. On the contrary, if there is no water in the washer tank, the output voltage is set to a second reference value Vo'. This is because the refractive index is different for air and water. Since the reference value Vo for the clear water is 1.1 times larger in comparison with the reference value Vo' for air, Vo' is set smaller than Vo.
With reference to FIG. 13, the basic principle of the detection of dirt content and cleanliness will be described.
Specifically, when the output from the light emitting diode 8a is made constant, the ratio between the generated light amount Io and the penetrating light amount I1 when the water is clear water is represented by I1/Io=e -k1 ., wherein k1 is a light absorbing factor and l is an optical path length. Similarly, when the water is dirty, the ratio between the generated light amount Io and the penetrating light amount I2 is indicated by I2/Io=e -k2 ., wherein k2 represents a light absorbing factor of the dirty liquid. If Io is constant, the following equation is held;
I2/I1=e.sup.-e(k2-k1)
Since the penetrating light amount I1 when the water is clear is proportional to Vo shown in FIG. 14, and the penetrating light amount I2 when the water is dirty is proportional to V1 of FIG. 14, an equation;
V1/Vo=e.sup.-e(k2-k1)
is obtained. Accordingly, it is understood that the changing ratio V1/Vo of the sensor output for the voltage Vo when the rinse water is supplied is changed logarithmically to the change of dirt content (the change of the light absorbing factor), as viewed from the graph of FIG. 13. In other words,
ln(V1-Vo)=-Δk.l (Δk=k2-k1)
Therefore, it is so determined that the larger the changing ratio is, the greater the dirt content is, thus increasing the washing time, or strengthening the stirring force.
Although the current of the light emitting diode 8a is controlled through D/A conversion by the PWM controlling and integrating circuit in the foregoing embodiment, it may be effected by direct D/A conversion. Moreover, in setting the optical sensor at the reference voltage Vo, although it is easy if the current of the light emitting diode 8a is increased from 0, it takes much time. In addition, since the output control requires a good responding capability, the capacity of the capacitor 19i should be rendered small.
The washing time can also be controlled also in the other modification of the present invention, which will be described with reference to FIG. 15.
The washing time TW is expressed by TW=TS+TF (wherein TS is a saturating time until the change of the output of the optical sensor becomes constant after the start of washing, and TF is the time corresponding to the changing ratio V1/Vo (Vo being the reference value and V1 being the output of the optical sensor at the saturating time point)). In considering the case where the light permeability does not reach the saturating point, a minimum value Tmin and a maximum value Tmax are set for the washing time, which are changed corresponding to the volume of the laundries. Therefore, when a relatively large amount of laundries are to be washed, Tmin and Tmax are large. The changing ratio V1/Vo is different for liquid detergent and powder detergent, that is, not smaller than 0.5 and smaller than 0.5, respectively. When the powder detergent is used for lightly soiled laundries, V1/Vo is approximately 0.5. As the dirtiness of the laundries increases, the changing ratio becomes smaller than 0.5. On the other hand, when the liquid detergent is used, if the laundries are a little dirty, V1/Vo becomes closer to 1, and it becomes smaller than 1 as the dirtiness increases. Since the logarithmic value of V1/Vo is inversely proportional to the dirt content, the laundries are much dirtier as the changing ratio V1/Vo becomes smaller. TF should be increased logarithmically in order to increase the washing time.
The control of washing according to the present embodiment is carried out as shown in FIG. 16.
When washing is started in step 300, IF controlling data stored in the previous rinsing process and the voltage data Vo are read from the storage device in step 301, thus controlling the output of the optical sensor. Step 302 is a volume detecting routine in which the volume of the laundries is detected, and the minimum and maximum washing times are determined in accordance with the detected volume of the laundries. After the start of stirring, the optical sensor is periodically controlled in step 303, generating the sensor output. In step 304, it is detected whether the sensor voltage is saturated to a predetermined value. When the output voltage is saturated, a saturation detecting flag is checked in step 305. Thereafter, the saturating time TS is stored in step 306, and further the changing ratio V1/Vo from the time of clear water (supplied as rinse water into the washer tank) is calculated in step 307. In step 308, TF is obtained based on the graph of FIG. 15. Then, in step 309, the washing time TW is obtained. When the washing time TW is consumed in step 310, the washing process is completed. It is possible to control the washing time to TW=TS+TF+TG in step 309. The time TG is changed corresponding to the volume of laundries. The dirt content is inversely proportional to the logarithmic value of the changing ratio V1/Vo, and accordingly, the optimum washing time can be obtained in accordance with the dirt content.
The output control and storing operations in the rinsing process according to a modified embodiment will be described with reference to FIG. 17.
At the first rinsing time in step 312, the output of the optical sensor is controlled during the supply of rinse water, i.e., before the rinse water is supplied to a set level, so that the output voltage Vo becomes a set value. In step 313, the water level of the supplied rinse water is detected. If the water level is not sufficient, rinse water is fed again in step 314. Then, if the sensor voltage does not reach the set value in step 316, the current IF of the light emitting diode is controlled by PWM signals in step 317. When the sensor voltage reaches the set value, the output controlling data (PWM signal data) and output signals Vo from the sensor are stored in steps 318 and 319, respectively.
In the control of washing described above, even if the laundries are soiled with mud, and accordingly when the saturating time of the sensor voltage becomes short, the washing time can be changed and lengthened in accordance with the dirt content of the laundries (light permeability). Therefore, a large washing and cleansing power is secured. Likewise, when the oily stains are to be washed and therefore the saturating time is long, the washing time can be lengthened. In short, according to the washing machine of the present invention, it is possible to control washing in accordance with the quality and quantity of the dirt. Since the dirt of the laundries in general domestic use is easy to decompose by water and detergent, in such case, it will fit the user's sense to control the washing time in accordance with the changing ratio V1/Vo, with reducing the saturating time. In other words, when the changing ratio is small and the saturating time TS is short, the laundries are judged to be lightly soiled, whereby the washing time is set shorter. On the other hand, when the changing ratio is large, with a small saturating time TS, the laundries are judged to be considerably dirty, and the washing time is set longer. The washing machine of the present invention can realize this type of control.
As is made clear from the foregoing description of preferred embodiments, the washing machine of the present invention is significantly effective as follows:
(1) Since the optical sensor is initialized on the basis of the light permeability of water (clear water) or air supplied into the washer tank, a situation can be prevented in which an output of the optical sensor is erroneously decreased as a result of staining. Therefore, an erroneous detection by the optical sensor is avoided, and an accurate detection of dirt is ensured.
(2) Since the reference value is changed between the water and air, the optical sensor can be initialized both for water and for air.
(3) Since it is so arranged as to detect the dirt of the laundries through detection of the light permeability of the optical sensor after the sensor is initialized, the detection is free from influences of stains to the optical sensor, and accordingly the optical sensor is reliably accurate for a long period of use.
(4) Since the dirt of the laundries is detected on the basis of both the saturating time of the output of the optical sensor and the changing width of the output, the quality and quantity of the dirt can be taken into consideration in control of washing and rinsing.
(5) Since there is provided, in addition to the optical sensor, a volume sensor for detecting the volume of the laundries, control of washing and rinsing can be carried out based on the data of the dirt detected by the optical sensor and the data of the laundry volume detected by the volume sensor. Therefore, control of washing and rinsing can be realized as if by the operator himself or herself.
(6) Since the detergent type is detected through detection of the output from the optical sensor after the optical sensor is initialized at the reference value, the washing machine can utilize a wide variety of detergents.
(7) Since washing and rinsing are controlled corresponding to the detergent type which greatly influences the optical sensor in detection of the light permeability, a highly accurate control is gained.
(8) Since the data of the kind of detergent type, data of the laundry volume and dirt content data from the optical sensor are all together utilized for control, washing and rinsing can be controlled with a much higher accuracy.
Although the present invention has been fully described by way of example with reference to the preferred embodiments thereof, it is to be noted here that various changes and modifications would be apparent to those skilled in the art. Such changes and modifications are to be understood as defined by the appended claims unless they depart therefrom. | A washing machine includes an optical sensor for detecting a light permeability of detergent solution and rinse water in a washer tank. The optical sensor includes a light emitting element and a light receiving element. A microprocessor is provided for controlling a luminous intensity of the light emitted from the light emitting element. More specifically, the microprocessor sets the luminous intensity of the light emitting element such that an intensity of the light detected by the light receiving element is equal to or greater than a stored reference value during at least one of two operating states. The first of the two operating states is a state in which water is absent from the water tank. A second of the two operating states is a state in which water is present in the water tank and prior to agitation of the water in the water tank. Various processing cycles of the washing machine are carried out in accordance with the light permeability detected by the optical sensor. | 3 |
Applicants claim the benefit of U.S. Provisional Patent Application 61/347,075, filed May 21, 2010.
BACKGROUND OF THE INVENTION
Hydroxy-terminated polybutadiene is widely used as a binder for polyurethane-based solid propellants because of its low viscosity and good low-temperature properties. The main chain in the isocyanate cured hydroxy-terminated polybutadiene is hydrocarbon. Binders with energetic groups on the chain are desirable for increased performance.
One of the most attractive examples on the basis of energy that has been studied is poly(glycidyl nitrate).
R. L. Willer and R. S. Day, Proceedings of the APDA Joint International Symposium on the Compatibility of Plastics and Other Materials with Explosives, Propellants and Ingredients , American Defense Preparedness Association, October, 1989, 258, Poly(Glycidyl Nitrate) Revisited; R. L. Willer, A. G. Stern, D. K. McGrath, 1990 JANNAF Propulsion Meeting , CPIA Publication 550, 3, 223, Poly(Glycidyl Nitrate) and Poly(Glycidyl Nitrate) Propellants. Unfortunately, isocyanate-cured PGN binders exhibits a cure reversion on aging, W. B. H. Leeming, E. J. Marshall, H. Bull, M. J. Rodgers, and N. C. Paul, Int. Ann. Conference of ICT, 99, 1-99 (1996) (CA 125:225892), that has limited its usefulness. The cure reversion has been ascribed to interaction of urethane nitrogens with hydrogens adjacent to the nitrate groups.
SUMMARY OF INVENTION
Briefly, the present invention comprises two novel compounds:
(1) 3-nitratooxetane, and
(2) poly-(3-nitratooxetane).
Still further, the invention comprises the method of synthesizing 3-nitratooxetane comprising reacting 3-hydroxyoxetane with a nitration agent, preferably concentrated nitric acid in a solution of acetic anhydride, and recovering 3-nitratooxetane.
This invention further comprises the method of synthesizing poly-(3-nitratooxetane) comprising polymerizing 3-nitratooxetane in the presence of a polyol, typically a diol or triol, and preferably 1,4-butanediol, as an initiator.
DESCRIPTION OF PREFERRED EMBODIMENTS
The synthesis of 3-hydroxyoxetane has been reported by a 4-step process. Acetic acid is added to epichlorohydrin, and the hydroxyl of the product is blocked with ethyl vinyl ether. Aqueous base hydrolyzes the acetate and closes the oxetane ring in one step. Removing the blocking group with acid gives 3-hydroxyoxetane. K. Baum, P. T. Berkowitz, V. Grakauskas, and T. G. Archibald, J. Org. Chem., 26:2953 (1983); and K. Baum, V. Grakauskas and P. T. Berkowitz, U.S. Pat. No. 4,395,561 (1983). Variations on this method using larger carboxylic acids instead of acetic acid have also been reported. W. Stutz, R. Waditschatka, K. Winter, M. von Frieling, R. Gressly, B. Jau, and S. Bürki, U.S. Pat. No. 5,663,383 (1997).
The present invention relates to the synthesis of poly-(3-nitratooxetane), PNO, which is isomeric with PGN. PNO has the formula:
wherein n is an integer of from about 10 to about 10,000. Preferably, the molecular weight is from about 10,000 to 50,000.
PNO was prepared by the nitration of 3-hydroxyoxetane using a nitration agent, preferably nitric acid in acetic anhydride, to yield 3-nitratooxetane. The 3-nitratooxetane is then polymerized in the presence of a polyol initiator to yield PNO. The polyol initiator is typically a diol, or trial. The preferred initiator is 1,4-butanediol.
The nitration reaction was complete in 1 hour at 0-5° C., and the product was isolated by aqueous work-up. Other nitration agents can be similarly used. For example, trifluoroacetyl nitrate or nitrogen pentoxide in halogenated solvents, would be suitable in lieu of nitric acid in acetic anhydride. Typically, the nitration reaction is carried out at a temperature of from about minus 20° C. to about plus 20° C.
In polymerization, best results are obtained when BF 3 etherate or BF 3 tetrahydrofuran complex are first contacted with the polyol. After about 0.2 to about 3.0 hours, the BF 3 etherate or BF 3 tetrahydrofuran complex are vacuumed to remove evolved ether or tetrahydrofuran. The 3-nitratooxetane is then added along with an organic solvent such as halohydrocarbon, preferably, methylene chloride. The solution is stirred at or around room temperature until the PNO has formed. The PNO is then recovered.
Example 1
Synthesis of 3-nitratooxetane
A nitrating mixture was prepared by adding 100% nitric acid (13 g, 210 mmol) to a solution of acetic anhydride (20 g, 200 mmol) in anhydrous methylene chloride (15 ml) at 0-5° C. over a period of 5 min with stirring. The solution was stirred for one hour at 0-5° C., and a solution of 3-hydroxyoxetane (10 g, 135 mmol) in methylene chloride (10 ml) was added over 5 min. The solution was stirred at 5° C. for one hour. The solution was poured onto 20 ml of ice and the mixture was stirred until the ice melted. The organic layer was separated and washed with water (10 ml), saturated sodium bicarbonate (4×10 ml), and again with water (10 ml), and was dried over magnesium sulfate. Solvent was removed under vacuum, and distillation using a 3 inch Vigreux column gave 8.8 g (55% yield) of 3-nitratooxetane, by 55-57° C. at 10 mm Hg. H NMR (CDCl 3 ): 5.69 (1H, p), 4.95 (1H, d), 4.92 (1H, d), 4.70 (1H, d), 4.67 (1H, d) ppm. IR (neat): 2959 (m), 2888 (m), 1643 (s, —NO 2 ), 1478 (vw), 1459 (vw), 1373 (w), 1327 (s), 1281 (s), 1176 (m), 1115 (w), 1072 (s), 1041 (w), 978 (s), 928 (w), 885 (s), 855 (s), 755 (m), 692 (m) cm −1 . Mass spectrum: 120.02913; therefor [M H] + 120.02954.
Example 2
Synthesis of poly-(3-nitratooxetane)
1,4-Butanediol (0.133 g, 1.48 mmol) and BF 3 etherate (0.207 g, 1.46 mmol) were weighed in a 1-neck 50 ml round bottom flask. After stirring for 1 hour under nitrogen, the ether was removed by pumping at room temperature for 2 hours. Anhydrous methylene chloride (4 ml) was added to the mixture followed by the addition of 3-nitratooxetane (5.3 g, 44.5 mmol) in anhydrous methylene chloride (6 ml) over a period of 25 min. The solution was stirred at 25° C. for 16 hours. Additional methylene chloride (20 ml) was added. The solution was washed with saturated sodium bicarbonate solution (20 ml), water, and dried over anhydrous magnesium sulfate. Solvent was removed by rotary evaporation, followed by pumping at 35-40° C. for 5 hours to give 4.0 g (74% yield) of poly-(3-nitratooxetane), a is viscous light-yellow oil. Anal. Calcd. for C 3 H 5 NO 4 : C, 30.30; H, 4.20; N, 11.80. Found: C, 30.53; H, 4.31; N, 11.89.
The following is a list of relevant properties for the poly-3-(nitratooxetane) (PNO).
Density( g/cc )=1.44(averaged over several batches; range 1.42-1.45).
Impact 10/10 NF@200 cm (single batch, molecular weight 25,000, some variability in this number depending on batch but generally nothing fires below 95 cm). The impact test was carried out by placing a metal cup containing PNO on a metal anvil. A 1 kg weight is dropped onto the anvil from increasing heights until the PNO goes off, in this case, at a height of about 95 cm. By contrast, RDX goes off at about 25 cm.
Friction 10/10 NF@ 1000 lbs (single batch, molecular weight 25,000. The vast majority of batches have no registered sensitivity but very rarely we have irregular go's in friction sensitivity test. In the friction test, PNO is applied between two metal plates, weight is applied on the top of the upper plate and the upper plate is pulled laterally to create rubbing friction.
Electrostatic 10/10 NF@0.25 J (single batch, molecular weight 25,000, no variation across batches). In the electrostatic test, the PNO is hit with an electric spark to measure reproducibility of the PNO synthesis. The test showed little or no batch to batch variation.
DSC 177/202 (single batch, molecular weight 25,000, some variation across batches but onset and peak only shift by a few degrees). The differential scanning calorimetry (DSC) test involves putting the PNO in a cup and heating it. A temperature sensors detects the onset of an exotherm, indicating that decomposition has begun.
VTS (cc/g)=0.85 (single batch, molecular weight 25000, some variation across batches but always <2 cc/g). The VTS test also provides a measure of the batch-to-batch consistency of decomposition and stability. The PNO was maintained at elevated temperature and the volume of gas evolved from the PNO sample was measured.
Heat of formation data: based on formula; did not perform mass spectrometry measurement so the heat of formation is approximate.
TABLE 1 Δ c H° Δ c H° Δ f H° Sample Cal/g kJ/g kJ/g PNO 1 −3201.70 ± 25.29 −13.41 ± 0.11 −2.53 ± 0.10 PNO 2 −3308.70 ± 15 −13.84 ± 0.06 −2.04 PGN Lot E-15 −3233.20 ± 11 −13.53 ± 0.05 −2.42 C 3 H 5 O 4 N( s )+9/4O 2 →3CO 2 ( g )+5/2H 2 O( l )+½N 2 ( g )
Δ f H° is obtained with the equation:
Δ f H°(polymer)=3Δ f H°(CO 2 )+5/2Δ f H°(H 2 O)−Δ c H° (polymer)
where Δ f H° (CO 2 )=−393.5 kJ/mol and Δ f H° (H 2 O)=−285.8 kJ/mol.
Liquid Drop weight test. The following results show the results comparing PNO with N-propyl nitrate and isopropyl nitrate.
PNO: E 50 :173 kg cm (low fire 164 kg cm)
N-propyl nitrate: E 50 :29 kg cm (low fire 28 kg cm)
Isopropyl nitrate: E 50 :30 kg cm (low fire 28 kg cm)
TABLE 2
The comparative properties of PNO and PGN are shown
in the following table:
PNO
PGN
Impact sensitivity
89 cm (50%)
110 cm (50%)
63 cm (low fire)
100 cm (low fire)
Friction
10/10 no fire
10/10 no fire
@ 1000 lbs
@ 398 lbs
ESD
10/10 no fire
10/10 no fire
@ 0.25 joules
@ 0.25 joules
VTS
1.6 cc/g @ 80° C.
0.1 cc/g @ 80° C.
(no stabilizer)
(With stabilizer)
DSC
Onset 180° C.
Onset 164-194° C.
Max 210° C.
Max 215° C.
Gumstocks were prepared by reacting PGN and PNU with the same organic polyisocyanate and the two resulting polyurethanes observed for two months. The poly(glycidyl nitrate) samples showed depolymerization while the poly-(3-nitratooxetane) samples showed no changes at all.
The superior long term stability of the PNO based gumstock is important in applications where high energy binders are required such as in explosives and rocket propellants. | 3-nitratooxetane.
Poly-(3-nitratooxetane).
The method of synthesizing 3-nitratooxetane comprising reacting 3-hydroxyoxetane with a nitration agent.
The method of synthesizing poly-(3-nitratooxetane) by polymerizing 3-nitratooxetane using a polyol initiator. | 2 |
[0001] This invention was made with U.S. Government support through Government Contract Number DE-FC26-01 NT41261 awarded by the Department of Energy, and, in accordance with the terms set forth in said contracts, the U.S. Government may have certain rights in the invention.
FIELD OF THE INVENTION
[0002] This invention relates in general to clothes washing machines and more particularly to a clothes washing machine having apparatus for water extraction from clothes during spin cycles of the washing machine.
BACKGROUND OF THE INVENTION
[0003] Conventional washing machines typically include a cabinet that houses an outer tub for containing wash and rinse water, a perforated clothes basket within the tub for holding articles such as clothes to be washed and an agitator disposed within the basket for agitating the clothes during a wash cycle. A drive and motor assembly for driving the agitator and the basket may be mounted underneath the outer tub. The motor is typically an AC induction motor, which can reverse its rotation direction to achieve different modes in a wash cycle. A pump assembly may pump water from the outer tub to a drain during a wash cycle. Conventional wash cycles will spin the basket at various times to extract water and wash fluids from clothes.
[0004] Extracting water from clothes during spin cycles is desirable because it reduces the amount of energy required to dry the clothes after washing, such as in a conventional dryer. The energy efficiency rating of washers may include the energy required to dry clothes after washing. Spinning the wash basket is a common method of extracting water from clothes prior to the drying cycle. Using the mechanical energy of the spin cycle to extract water is more energy efficient than using the heat in a clothes dryer. More stringent energy usage standards imposed on washing machines can require new and costly washer platforms. This is because efforts to increase water extraction have mainly been achieved through increased basket spin speed. This often requires more expensive drive systems that typically include costly motors and transmissions. Also, increased spin speed may result in problems with the high forces associated with possible out-of-balance conditions and the associated higher stresses in the basket.
[0005] The retained moisture content (RMC) of clothes is a variable used to determine the amount of energy required to dry clothes after a wash cycle. Several factors affect clothing's RMC during a washing machine's spin cycle. These factors may include clothing material, clothing load, basket diameter, spin speed, spin duration, rinse temperature and chemical rinse agents.
BRIEF DESCRIPTION OF THE INVENTION
[0006] A method of fabricating a wash basket for a washing machine is provided that may include providing a substantially cylindrical housing having a bottom and an inner wall, providing a plurality of geometric structures and connecting the plurality of geometric structures to the inner wall.
[0007] A wash basket for a washing machine is provided that may include a housing having an inner wall fabricated by a first process and a plurality of geometric structures fabricated by a second process where the plurality of geometric structures are attached to and extend radially inwardly from the inner wall, the geometric structures comprising a separate structure relative to the housing.
BRIEF DESCRIPTION OF THE DRAWINGS
[0008] FIG. 1 is a perspective cutaway view of an exemplary washing machine.
[0009] FIG. 2 is a front elevational schematic view of the washing machine shown in FIG. 1 .
[0010] FIG. 3 is a schematic block diagram of a control system for the washing machine shown in FIGS. 1 and 2.
[0011] FIG. 4 is a partial vertical cross sectional view of an exemplary wash basket for the washing machine shown in FIGS. 1 and 2 .
[0012] FIG. 5 is a partial horizontal cross section of the wash basket along line 5 - 5 shown in FIG. 4 .
[0013] FIG. 6 is a partial plan view of an exemplary configuration of ribs insertable into a wash basket in accordance with aspects of the invention.
[0014] FIG. 7 is a plan view of an exemplary rib of FIG. 6 .
[0015] FIG. 8 is a side elevational schematic view of the washing machine of FIGS. 1 and 2 .
DETAILED DESCRIPTION OF THE INVENTION
[0016] FIG. 1 is a perspective view partially broken away of an exemplary washing machine 50 in which aspects of the present invention may be practiced. It is recognized, however, that the various benefits of the present invention may be demonstrated in other types of washing machines. The description of washing machine 50 below is therefore offered just for illustrative purposes, and in no way should be construed to limit application of the present invention in any aspect.
[0017] Washing machine 50 includes a cabinet 52 and a cover 54 . A backsplash 56 extends from cover 54 , and a variety of appliance control input selectors 58 , 60 may be mounted onto backsplash 56 . Input selectors 58 , 60 comprise a user interface for operator selection of operational machine cycles and modes of operation. A lid 62 is mounted to cover 54 and may be movable between an open position facilitating access to a wash tub 64 located within cabinet 52 , and a closed position forming a covered enclosure over wash tub 64 .
[0018] Tub 64 includes a bottom wall 66 and a sidewall 68 , and a basket 70 may be rotatably mounted within washtub 64 . An agitator, impeller, or oscillatory basket mechanism 116 (shown in FIG. 2 ) may be disposed in basket 70 to agitate the articles and liquid in basket 70 . The agitator 116 and/or wash basket 70 may be positioned to rotate or otherwise have motion, e.g., oscillatory or wobbling motion, about an axis, such as a vertical axis, an axis with some degree of tilt or a horizontal axis. Such an oscillatory mechanism 116 is not necessary to implement embodiments of the invention.
[0019] FIG. 2 is a view of washing machine 50 including wash basket 70 movably disposed and rotatably mounted in washtub 64 in a spaced apart relationship from tub side wall 64 and tub bottom 66 . Wash basket 70 may include a plurality of perforations therein to facilitate fluid communication between an interior 100 of wash basket 70 and washtub 64 . A dispenser (not shown in FIG. 2 ) may be provided to produce a wash solution by mixing fresh water with a detergent or other composition for cleansing of articles in wash basket 70 . The agitator, impeller, or oscillatory basket mechanism 116 may be disposed in wash basket 70 to impart an oscillatory motion to articles and liquid in wash basket 70 . As illustrated in FIG. 2 , agitator 116 is exemplarily oriented to rotate about a vertical axis. It will be appreciated, however, that various embodiments of the present invention may be used with horizontal axis washing machines as well. Wash basket 70 and agitator 116 may be driven by motor 120 through a transmission and clutch system 122 . Clutch system 122 facilitates driving engagement of wash basket 70 and agitator 116 for rotatable movement within washtub 64 . The clutch system 122 facilitates relative rotation of wash basket 70 and agitator 116 for selected portions of wash cycles. Motor 120 , transmission and clutch system 122 may form a multiple speed drive that is capable of spinning wash basket 70 at multiple speeds to accomplish different objectives at different points in the wash cycle.
[0020] Operation of machine 50 may be controlled by a controller 138 , which is operatively coupled to the user interface input located on washing machine backsplash 56 (shown in FIG. 1 ) for user manipulation to select washing machine cycles and features. In response to user manipulation of the user interface input, controller 138 operates the various components of machine 50 to execute selected machine cycles and features. For example, clothes are loaded into wash basket 70 , and washing operation is initiated through operator manipulation of control input selectors 60 (shown in FIG. 1 ). Tub 64 is filled with water and mixed with detergent to form a wash fluid then wash basket 70 is agitated with agitator 116 for cleansing of clothes in wash basket 70 . After a predetermined period of wash action, tub 64 is drained and wash basket 70 is spun to extract wash fluid from the clothes. Clothes are then rinsed with fresh water and wash basket 70 is spun again to remove water from clothes. Depending on the particular wash cycle selected, multiple wash and spin portions of the wash cycle may be executed.
[0021] FIG. 3 is a schematic block diagram of an exemplary washing machine control system 150 for use with washing machine 50 . Control system 150 includes controller 138 , which may, for example, be a microcomputer 140 coupled to a user interface input 141 . An operator may enter instructions or select desired washing machine cycles and features via user interface input 141 , such as through input selectors 60 (shown in FIG. 1 ). A display or indicator 144 coupled to microcomputer 140 displays appropriate messages and/or indicators, such as a timer, and other known items of interest to washing machine users. A memory 142 is also coupled to microcomputer 140 and stores instructions, calibration constants, and other information as required to satisfactorily complete a selected wash cycle.
[0022] Power to control system 150 is supplied to controller 138 by a power supply 146 configured to be coupled to a power line L. Analog to digital and digital to analog converters (not shown) are coupled to controller 138 to implement controller inputs and executable instructions to generate controller output to washing machine components such as those described above in relation to FIGS. 1 and 2 . More specifically, controller 138 may be operatively coupled to motor 120 , clutch system 122 , drive system 148 , brake system 151 , water valves 152 and drain pump/drain valve 154 as well as other components of machine 50 according to known methods. Water valves of machine 50 (not shown) may be in flow communication with a dispenser 153 (shown in phantom in FIG. 3 ) so that water may be mixed with detergent or other composition of benefit to washing of garments in wash basket 70 .
[0023] In response to manipulation of user interface input 141 controller 138 monitors various operational factors of washing machine 50 with one or more sensors or transducers 156 and executes operator selected functions and features according to known methods. While an electronic controller 138 is described and illustrated in FIG. 3 , it is contemplated that known electromechanical control mechanisms may be employed in alternative embodiments.
[0024] The retained moisture content (RMC) of clothes after the final spin cycle may be defined as:
RMC = ( wet weight of clothes - dry weight of clothes ) dry weight of clothes × 100
Reducing or lowering the RMC after final spin will reduce the amount of dryer energy needed to dry the clothes. Shorter drying cycles may also be obtained thereby synchronizing the length of a drying cycle with that of a wash cycle. This enables a user to do laundry more efficiently (drying cycles are typically longer that wash cycles thereby creating a bottleneck when transitioning loads from the washing machine to the dryer). Reducing RMC also allows for more efficient rinsing of clothes. A wash cycle separates soil from clothes and a rinse cycle rinses the loosened soil from the load to avoid deposition on other areas of the clothes. It has been shown through testing that a 20% reduction in RMC over three rinsing cycles (typical in a household washing machine) may reduce the amount of suspended, non-adsorbed particles in the wash solution by 50%. More efficient rinsing produces cleaner clothes after washing.
[0025] One aspect of the invention allows for a plurality of geometric structures 159 , such as ribs 160 , to be formed on the periphery of inner wall 162 of wash basket 70 as shown in FIGS. 2 and 4 . It has been found that such structures 159 may reduce RMC as a function of at least the structures' height, spacing from one another and geometry. With respect to ribs 160 , it will be appreciated that ribs 160 may be orientated vertically or circumferentially relative to inner wall 162 , or at any angle between vertical and circumferential. Ribs 160 increase the local force per area, or provide discrete pressure points on clothing during a spin cycle. This compresses the clothing thereby squeezing clothing fibers and decreasing the size of local capillaries, which increases the local wicking action towards ribs 160 due to the capillary action within the clothing. This increases the amount of water extracted from the clothing during the spin cycle. It will be appreciated that various embodiments of the invention may be formed as part of an injection molding process for fabricating a wash basket 70 .
[0026] Ribs 160 may be shaped or formed in various ways other than being linear members. Embodiments of ribs 160 may include curves, waves or other combinations of geometric shapes. Embodiments of other geometric structures 159 , such as a plurality of protrusions or protuberances, are not limited to being continuous members and may also be formed as dimples or nubs extending from the inner wall 162 of wash basket 70 . Various embodiments of the invention allow for flexibility during manufacture.
[0027] Another aspect allows for various embodiments of geometric structures 159 to be formed independently of or as a separate structure from wash basket 70 . As a separate structure the geometric structures 159 may then be attached to the wash basket as illustrated in FIG. 6 . Exemplary embodiments of structures 159 , such as ribs 160 , may be formed as a unitary piece or as individual ribs that may be attached to the inner wall 162 of wash basket 70 . In an embodiment, wash basket 70 and/or structures 159 may be stainless steel, it being appreciated that basket 70 and attachable structures 159 may be fabricated of various compositions. In this respect, it has proved difficult to fabricate stainless steel wash baskets with integral structures 159 , such as ribs 160 , as a unitary product without compromising the basket's structural integrity.
[0028] One aspect allows for wash basket 70 to be fabricated of various materials such as stainless steel, plastic or porcelain steel, for example, or wash basket 70 may be enameled. Wash basket 70 may be configured to have attached thereto a secondary geometry or geometric structure 159 shown in FIG. 2 . Geometric structures 159 , which may be ribs 160 , promote improved washing of, and/or water extraction from, articles being washed. Further, because the secondary geometry 159 may be a separate structure and attachable to the inside-of wash basket 70 , the structural integrity of the basket is not compromised in any respect. The secondary geometry 159 may be fabricated of various materials and combinations thereof such as synthetics, thermoplastic, plastic, synthetic resins, ceramics, steel and/or stainless steel, it being appreciated that other materials and combinations thereof will be recognized by those skilled in the art of fabricating wash basket 70 and the secondary geometric structure 159 .
[0029] The secondary geometry 159 may be formed as elongated ribs 160 or semi-spherical protrusions, for example. It will be recognized that embodiments of the attachable secondary geometry 159 may assume a wide range of geometries provided they are suitably attachable to the inside of wash basket 70 . The secondary geometry 159 may be attached to the inner wall 162 of wash basket 70 by various attaching means such as screws, snaps, bolting, adhesives, spot or ultrasonic welding, or interlocking joints, for example. Other attaching means will be recognized by those skilled in the art. The secondary geometry 159 may be rigidly attached to the inner wall 162 so it does not move relative to the wash basket 70 thereby functioning in cooperation with the basket during wash and spin cycles. In this respect, during a wash cycle the clothes within wash basket 70 will impinge or rub against the secondary geometry 159 thereby promoting mechanical cleaning of the clothes, much in the same way an agitator does in a vertical axis washing machine. During a spin cycle, the secondary geometry 159 , such as ribs 160 , cause stress concentrations in clothes under spin at points where the clothes contact the secondary geometry 159 . This promotes a local wicking and/or ringing action in clothes that causes more moisture to be removed from the clothes thereby reducing the RMC.
[0030] One aspect of the invention allows for ribs 160 to extend vertically from the bottom 164 of wash basket 70 a distance that is less than the height of the inner wall 162 of wash basket 70 . It has been found that this configuration enhances the wicking action of the clothing to reduce RMC while maximizing the volume of water contained in the washtub 64 . This may allow for an improved energy rating of the washing machine 50 . An exemplary standard for energy standard compliance is the Modified Energy Factor (MEF), which may be defined as:
MEF = washer basket volume hot water energy + mechanical energy + dryer energy
[0031] Dryer energy is typically greater than that of a washing machine, such as machine 50 , so reducing dryer energy may have a significant effect of the MEF. In this respect, one way to reduce dryer energy is to extract more water from the clothes during the final spin cycle. Sizing ribs 160 so they extend a distance less then the height of wash basket 70 allows for a reduction in RMC while maximizing the volume of the washer basket.
[0032] Ribs 160 may have a constant cross section. This may inhibit clothes from moving to the top of wash basket 70 during spin. A plurality of ribs 160 may be disposed around the entire circumference of the wash basket 70 that extend substantially perpendicularly from the bottom 164 of the wash basket 70 to approximately the midpoint of the basket's height, for example. The cross section of ribs 160 may be a constant semi-circular cross section, as shown in FIG. 5 , or other geometrical cross-sections. Ribs 160 may be tapered and in one embodiment the lower portion of the ribs 160 may extend further away from the inner wall 162 of wash basket 70 than the upper portions of ribs 160 . Tapering ribs 160 may increase the volume of water that may be contained in washtub 64 thereby improving the energy rating of washing machine 50 . In one aspect, the length, spacing and cross section dimensions of ribs 160 , or other geometric structures 159 , may be optimized to maximize the reduction in RMC and water volume in washtub 64 for that machine. This optimization may be based at least in part on the operational characteristics or parametrics of a washing machine. These may include wash basket diameter, volume, spin rate and duration of spin, load size, water temperature and clothing composition, for example. Other factors will be recognized by those skilled in the art.
[0033] Ribs 160 may extend radially inwardly toward the center of basket 70 with a constant radius of curvature measured from the inner basket wall 162 . The radius of curvature may vary and in one aspect may be greater than about 0.25 inches and less than about 1.00 inch. In an exemplary embodiment the radius of curvature may range between about 0.25 and 0.625 inches. Alternate embodiments allow for the radius of curvature to be less than 0.25 inches or greater than 1.00 inch as a function of the type of articles under spin, and various operating parameters and performance requirements of machine 50 , for example. Ribs 160 may be circumferentially spaced apart varying distances, and in an embodiment may be spaced apart approximately 1.25 inches between longitudinal centerlines. In alternate exemplary embodiments ribs 160 may have a constant cross section formed with a varying radius of curvature.
[0034] An exemplary embodiment of attachable geometric structures 159 , such as attachable ribs 160 , shown in FIG. 6 , allows for a cross section of ribs 160 to be formed substantially as a bell-shaped curve with concave portions 163 that transition ribs 160 to integrate with the inner wall 162 of the wash basket 70 . Other curvatures will be recognized by those skilled in the art. In an embodiment, the distance from the inner wall 162 of the wash basket 70 to proximate the apex of a rib 160 extending radially toward the center of the basket may be between about 0.25 inches and 1.00 inch. Alternate embodiments allow for the attachable geometric structures 159 to be protrusions, dimples, waveforms or other shapes. Heights of the geometric structures 159 may extend away from the inner wall 162 of wash basket 70 varying distances.
[0035] Geometric structures 159 , such as ribs 160 , may comprise a flexible or resilient material so that they conform to the surface of inner wall 162 of wash basket 70 when attached. The portions of structures 159 that interface with inner wall 162 may be manufactured using a spring or biasing feature for conformance with inner wall 162 . Insert or rotary molding, for example, may be used to manufacture geometric structure 159 with a spring or biasing feature. Alternate embodiments may use an interface material that may be bonded to structures 159 so it is positioned between the structures and inner wall 162 when they are attached. These aspects allow for larger tolerances in manufacturing both wash basket 70 and geometric structures 159 , such as ribs 160 , which may lower production costs and allow for a tight interface so that clothes are not caught in the interface area.
[0036] Further, it has been determined that for a given spacing of ribs 160 , which may be measured between centerlines, the width W and angle Θ may be optimized to increase a pressure component F A proximate the top or apex of ribs 160 during spin. During a spin cycle of machine 50 , clothes may impinge the surface of ribs 160 at various points. Referencing FIG. 7 , portions of clothes may impinge the top of ribs 160 and portions of clothes may drape over a rib 160 impinging one or both sides of the rib, such as along concave portion 163 . In this respect, portions of clothes may impinge and extend along each side of ribs 160 , to varying distances, toward inner wall 162 of basket 70 . When this occurs, width W and angle Θ may be optimized to increase pressure component F A , which increases the local wicking action proximate the top of a respective rib 160 . Increasing angle Θ will correspondingly increase force component F T , which causes the portions of clothes draped over rib 160 to “pull” toward inner wall 162 . This pulls corresponding portions of clothes against the top of rib 160 thereby increasing the local wicking action.
[0037] If ribs 160 are sufficiently spaced apart, portions of clothes may impinge inner wall 162 between ribs 160 . This reduces force component F T relative to a force component resulting from portions of clothes not impinging inner wall 162 . In an exemplary embodiment, ribs 160 are sufficiently spaced apart so that portions of clothes only impinge ribs 160 proximate their respective tops. It has been determined that the local wicking action proximate the top of the ribs 160 is maximized if portions of clothes do not impinge or only slightly impinge a ribs' sidewalls. Alternate embodiments allow for ribs 160 to be sufficiently spaced apart so that clothes impinge a portion of a rib's sidewall but not the inner wall 162 of wash basket 70 . Spacing of ribs 160 , and the optimization of width W and angle Θ for a given spacing, may be optimized based on the operational characteristics and parametrics of a washing machine 50 .
[0038] An embodiment allows for ribs 160 to have a textured or rough surface area to create sufficient friction between ribs 160 and clothes in wash basket 70 to hold the clothes in place against ribs 160 . This allows for ensuring that the clothes positioned between adjacent ribs 160 are suspended away from the inner wall 162 of the wash basket 70 during spin. Suspending clothes increases the pressure or force exerted against the clothes along the surface of ribs 160 impinging the clothes during spin, such as proximate the top of individual ribs, relative to the exerted pressure if the portions of clothes positioned between ribs 160 rested against the inner wall 162 during spin. The texturing also effectively decreases the wetting angle allowing more water to move away from clothing more easily during spin.
[0039] One aspect of the invention allows for the geometric structures 159 , such as ribs 160 , to be formed entirely or partially of a porous material to enhance the wicking action at the surface of the structure 159 . This is due to small porous apertures formed in structures 159 . Various porous materials may be used to form structures 159 including ceramic, metal, plastic, and fabric materials, for example. It will be appreciated that other materials known to those skilled in the art may be used. Another aspect allows for a porous material 165 (as illustrated in FIG. 5 ) to be formed over all or a combination of ribs 160 , or other structures 159 , to achieve a similar enhancement to the wicking action proximate a rib surface. The material may be placed over solid or porous ribs 160 , either of which may be hollow. In an embodiment a commercially available fabric known as CoolMax, manufactured by Dupont, may be used to cover a combination of ribs vertically and circumferentially. This fabric or wicking material enhances the wicking effect of ribs 160 . Exemplary embodiments of geometric structures 159 that are hollow may have apertures formed therein for draining water, which prevents mildew and detergent build-up.
[0040] In one aspect of the invention a means for supplying or introducing air to the wash basket is provided. This allows for air to flow onto clothes in the wash basket 70 during spin for enhancing evaporation of water from the clothes thereby reducing the RMC. One aspect allows for air to flow internal to porous ribs 160 , or other structures 159 , to enhance the evaporative effect proximate the surface of the ribs. With reference to FIG. 8 , in an embodiment the means for introducing air may include an aperture 170 formed in cabinet 52 , such as in the cabinet's back panel 172 , for example. Aperture 170 may be formed in other parts of cabinet 52 , lid 62 or other parts of machine 50 . Aperture 170 may be an appropriately sized vent that allows air to be drawn into the cabinet 52 by the spinning of the wash basket 70 , which effectively functions as a centrifugal pump during spin.
[0041] The means for introducing air may include a duct 174 that directs airflow from aperture 170 to an outlet port 176 , which in an embodiment may be coaxial with an agitator 116 when lid 62 is closed. This allows for air to be drawn down the agitator shaft into wash basket 70 and circulate up the basket inner wall and over clothes during spin. It is expected that some air will flow out of the cabinet 52 after flowing up the inner walls. A heating device 178 may be provided for heating air flowing through duct 174 , and a device 180 for moving air, such as a commercially available blower, may be provided for pushing or pulling air into duct 174 . In an embodiment, duct 174 may be integral with lid 62 . It will be appreciated that duct 174 , heating device 178 and the device 180 may be used in various combinations and located in various places within washing machine 50 .
[0042] An alternate embodiment allows for a blower, such as device 180 , to be located for pulling saturated air out of the wash basket 70 during spin so that less humid air may be drawn or pushed into the wash basket. This allows for metering air into and/or out of the wash basket 70 during spin so air with relatively low humidity is continuously introduced into the wash basket 70 to enhance the evaporation of water from clothes being spun. Air may be metered into and/or out of wash basket 70 at a constant flow rate or a pulsating rate, for example, to account for operating parameters or characteristics of machine 50 and environmental factors such as the relative humidity of ambient air.
[0043] Alternate embodiments allow for a removable or permanently affixed device (not shown) to attach to an upper rim of wash basket 70 , or other appropriate mounting location such as the balance ring, for directing air onto clothes during spin. The device may be substantially rectangular while conforming to the basket's curvature, for example, and include an inlet port that directs air into the device during spin. The device may be configured to direct the air entering the inlet port downwardly toward clothes being spun in the basket. The speed of the spinning basket forces air through the inlet port to flow over the clothes.
[0044] While the exemplary embodiments of the present invention have been shown and described by way of example only, numerous variations, changes and substitutions will occur to those of skill in the art without departing from the invention herein. Accordingly, it is intended that the invention be limited only by the spirit and scope of the appended claims. | A method of fabricating a wash basket for a washing machine including providing a substantially cylindrical housing having a bottom and an inner wall, providing a plurality of geometric structures and connecting the plurality of geometric structures to the inner wall. The plurality of geometric structures may be configured to optimize a relationship between mechanically agitating an article contained within the wash basket during a wash cycle and reducing a residual moisture content of the article during a spin cycle. A wash basket for a washing machine may include a housing having an inner wall fabricated by a first process and a plurality of geometric structures fabricated by a second process where the plurality of geometric structures are attached to and extend radially inwardly from the inner wall, the geometric structures comprising a separate structure relative to the housing. | 3 |
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