text:
|Publication number
|Publication type
|Application number
|Publication date
|Dec 10, 1996
|Filing date
|Nov 9, 1995
|Priority date
|Oct 12, 1994
|Fee status
|Publication number
|Rodney M. Lafollette
|Original Assignee
|Bipolar Technologies, Inc.
|Export Citation
|BiBTeX, EndNote, RefMan
|Patent Citations (17), Non-Patent Citations (3), Referenced by (18), Classifications (27), Legal Events (5)
|External Links: USPTO, USPTO Assignment, Espacenet
This application is a continuation-in-part of my U.S. patent application Ser. No. 08/440,376, filed May 12, 1995, now abandoned, which is a division of U.S. patent application Ser. No. 08/321,692, filed Oct. 12, 1994, now abandoned.
The present invention relates generally to the field of batteries and more particularly to novel bipolar battery cells, bipolar batteries and related methods, which batteries overcome or substantially alleviate problems of the past and which provide long-term reliability, large energy storage capacity, and accommodate delivery of energy at very high power levels. As used herein, the term battery is intended to mean any self-contained source of electrical power.
The battery field is historically old. Secondary (rechargeable), multi-cell batteries are divided broadly into two types of configurations, i.e., (1) parallel plate batteries, such as are commonly used in automobiles for starting and lighting; and (2) bipolar batteries.
Each cell of a parallel plate battery comprises positive and negative electrodes, a porous separator to prevent the electrodes of opposite polarity from touching, and electrolyte. Each cell usually contains several positive plates connected to one another by a conductive strap, and several positive and negative plates are alternated.
The typical parallel plate battery comprises many individual cells. For example, the battery in automobiles typically have six cells. The cells are connected in series, such that the positive electrode from one cell connects through another conductive metal strap, to the negative electrode of the adjacent cell. The negative electrode from one "end" cell of the battery is the negative battery post, and the positive electrode from the other end cell is the positive battery post. Current flows through the battery from the negative post to the negative electrode of one end cell, through the electrolyte in that cell to the positive electrode, through the strap from that positive electrode to the negative electrode of the adjacent cell, and so on, exiting at the positive electrode of the other end cell at the end post. The battery voltage (potential) is the sum of the voltages from each individual cell.
The parallel plate battery has been used successfully for decades. It has the chief advantage of preventing leakage of electrolyte from one cell to the other. Its disadvantages, especially in respect to high specific energy and specific power, are:
1. Extra weight associated with the intercell straps;
2. Extra weight associated with the electrode grids, or the "skeleton" of the electrodes;
3. Comparatively large distances between the positive and negative electrodes within a given cell, which results in ohmic losses (i.e., losses of potential or voltage) as the current flows through the electrolyte in the cell;
4. Ohmic losses as the current travels through the electrode grids and intercell straps;
5. For some battery systems, excess electrolyte (which adds weight);
6. For some battery systems, uneven current distribution (i.e., more current per area flowing in the middle of the electrode plates than at the edges, or vide versa, a consequence of the geometry of the parallel plate cell design, which reduces the number of times the battery can be recharged).
On the other hand, a bipolar battery typically comprises a stack of bipolar electrodes, each prevented from touching the adjacent electrodes by a separator. Each separator holds electrolyte. Around the edges of the bipolar electrode, a seal is used to prevent the electrolyte from leaving the cell and to prevent shorts. The bipolar electrode traditionally comprises a thin, electronically conductive material known as the bipolar plate or bipolar electrode substrate, with the positive electrode active material applied to one side, and the negative electrode active material applied to the opposite side. On the ends of the bipolar battery are placed single-sided (monopolar) electrodes.
In general, the bipolar battery has several advantages over the parallel-plate battery design. First, the cumulative weight of several components is much less. Second, the efficiency of each cell is typically much higher, since it is possible to maintain a very small intercell gap (distance between facing electrodes) thereby minimizing internal losses. Well designed bipolar batteries offer peak specific powers which are often an order of magnitude (or more) higher than those of parallel plate batteries, and specific energies (W-hr/kg) can be higher for bipolar batteries.
In the early part of this century, battery manufacturers elected to use the parallel plate design as opposed to the bipolar design for greater reliability. Since then, periodic efforts have been made to develop secondary (rechargeable) bipolar batteries, mostly in response to certain applications particularly where high specific power was of principal concern. However, none of these efforts resulted in commercialization. There have been two apparently successful commercial (non-rechargeable) bipolar batteries, one by Polaroid (a four cell LeClanche battery for cameras) and one by Gould (in conjunction with Polaroid), a two cell lithium-manganese dioxide battery.
In the 1980's the Strategic Defense Initiative Organization was formed and began efforts to develop batteries which could deliver huge amounts of energy as sub-second pulses, to power certain defense systems (such as lasers). LaFollette and Bennion developed the design principles for bipolar lead acid batteries which provide high specific power. During recent years, other efforts have been made at high specific power bipolar battery development. The renewed electric vehicle development of the past four years, funded largely by the three U.S. automakers and the U.S. government, has also increased activity in bipolar battery development.
Notwithstanding bipolar battery efforts prior to the present invention, development of a rechargeable lightweight bipolar battery capable of storing large amounts of energy and of delivering energy at very high power levels has not been achieved.
In brief summary, the present invention overcomes or substantially alleviates problems in the field of bipolar battery technology. Novel bipolar battery cells, bipolar batteries and related methods are provided. A unique bipolar plate, having exceptional characteristics, is provided. A novel technique for sealing individual bipolar cells is also provided.
The bipolar plate provides high electronic conductivity, is impervious to liquid penetration, is thin though possessed of sufficient mechanical strength and flexibility to withstand anticipated loads and abuses, is electrochemically and chemically inert, is capable of bonding effectively with the seal material and electrode active materials, and is possessed of low specific gravity.
The seal prevents contact between adjacent electrodes, prevents loss of electrolyte, is stable when in contact with the electrolyte, and forms a good bond with the edges of the electrodes.
Bipolar batteries embodying principles of the present invention can accommodate high specific power energy storage. Any desired voltage and power availability can be accommodated as can various configuration by which pulse or long-term discharge is accommodated.
With the foregoing in mind, it is a primary object to overcome or substantially alleviate problems associated in the past with bipolar battery cells, bipolar batteries and/or methods by which such cells and batteries are produced.
Another object of importance is the provision of a novel bipolar plate for bipolar cells and bipolar batteries, as well as unique related methods.
A further object of significance is the provision of a novel seal for bipolar cells and bipolar batteries, as well as unique related methods.
A further dominate object of the present invention is the provision of a novel bipolar plate material and methods by which the material is produced.
An additional valuable object is the provision of a bipolar plate which is strong, flexible, high conductive, chemically stable, adequately electrochemically inactive, ultrathin, and/or of low specific gravity.
A paramount object is the provision of a novel peripheral bipolar seal comprised of fluoroelastomeric material which chemically bonds with the edges of the bipolar electrodes.
Another significantly important object is the provision of one or more of the following: a bipolar plate comprising one or more fluoroelastomers; a bipolar plate comprising carbon fibers; a bipolar plate comprised of glassy carbon; a bipolar plate comprising a backbone of overlapping carbon filaments or strands; a bipolar plate comprising matted carbon fibers; a structurally reliable bipolar plate comprised of a carbon backbone and carbon fluoroelastomer plate filler; a bipolar plate treated with organosilane; a bipolar carbon/fluoroelastomer plate coated with tin dioxide; a bipolar battery comprising one or more carbon/fluoroelastomeric bipolar plates; a bipolar battery comprising a peripheral seal comprising an anti-leak fluoroelastomeric material; methodology for making reliable carbon/polymer bipolar plates having a long useful life expectancy.
A further object of value is provision of a bipolar battery which can accommodate high specific power energy storage.
Another object of importance is the provision of low weight bipolar batteries and battery cells.
An additional dominate object is the provision of novel bipolar batteries and battery cells wherein the current path therethrough is relatively short and internal losses are minimized.
Another object is the provision of bipolar battery technology which lowers the weight and volume of each cell.
An object of paramount value is provision of bipolar cells and bipolar batteries which accommodates use of either alkaline or acid electrolyte and which accommodates a wide range of voltage and power levels.
A further object of significance is the provision of novel bipolar cells and bipolar batteries which can be stored without use for long periods of time without significant deleterious effects and which provide a long service or cycle life.
An additional object of value is the provision of novel bipolar cells and batteries which are highly corrosion resistant over a protracted period of time and are also strong, flexible, and able to withstand various forms of abuse.
Also, an object of importance is the provision of bipolar cells and bipolar batteries, the useful life of which is very long because they are rechargeable.
Another object of note is the provision of a bipolar battery which comprises a combination of a bipolar plate, well adhered electrodes and a sealed periphery insuring superior long-term performance.
These and other objects and features of the present invention will be apparent from the detailed description taken with reference to the accompanying drawings.
FIG. 1 is a perspective representation of a bipolar battery cell embodying principles of the present invention;
FIG. 2 is an exploded perspective of the bipolar battery cell of FIG. 1;
FIG. 3 is a cross-section taken along lines 3--3 of FIG. 1;
FIG. 4 is a cross-sectional schematic of a bipolar battery comprising a series of bipolar battery cells of the type illustrated in FIG. 1;
FIG. 5 is an enlarged diagrammatic representation of the long carbon fiber backbone from which the bipolar plate of this invention is formed; and
FIG. 6 is a flow chart of one way of forming a bipolar plate in accordance with the principles of the present invention.
The two most difficult aspects of bipolar battery technology have been the bipolar plate and the seal of the individual cells. Needed or desired properties are not found in readily available plate or seal materials.
Lead metal has previously been used as a bipolar plate material. Lead has the advantages of inertness with respect to both oxygen evolution at the positive electrode and hydrogen evolution at the negative electrode, as well as most other undesirable battery reactions. It forms an excellent interface with the active material. The disadvantages include softness, high specific gravity and most serious of all, inadequate corrosion resistance over extended charge/discharge cycling.
Attempts have been made to use other metals, such as titanium, in the construction of a bipolar battery. Titanium is of low specific gravity, is mechanically strong, and can be made in ultrathin layers. Unfortunately, titanium is partially soluble in sulfuric acid electrolyte, and promotes the evolution of oxygen at the positive electrode. Further, adhesion of the active material to the plate can be difficult.
The use of tin dioxide as a protective coating for a bipolar plate has also been proposed.
Most other metals either promote oxygen evolution at the positive electrode, or are not stable in sulfuric acid.
Titanium suboxides have also been considered. Titanium suboxides are semiconductive. There is a range of these compositions (grouped in phases), some of which have quite high conductivity. Further, they are virtually inert, chemically and electrochemically. The main difficulty, which has caused titanium suboxides to be rejected for bipolar battery use, is in creating thin material which is not brittle, and in causing adhesion with the electrode active materials to the substrate.
Several composite materials have been proposed, which to one extent or another, combine desirable properties of two or more materials. Most are mixtures of carbon powder and a polymer. The advantages of these materials are ease of sealing the individual cells of the bipolar battery under some conditions, low specific gravity, and some electronic conductivity. The current flows through the carbon only, the polymers being insulators. If the carbon is not present in a high enough concentration to allow the individual carbon particles to be in contact with each other, as is typically the case, the carbon/polymer plate provides unacceptable conductivity. Conversely, the polymer must also be present in sufficient amount to ensure that voids between carbon particles are not present, to prevent pinholes and establish and maintain sufficient mechanical strength. A commercially acceptable balance between conductive and long-term polymer-induced strength in a bipolar plate formed of carbon powder and polymer has not been achieved adequate for high rate applications. The main problem is believed to be in disruptions in particle-to-particle contact of the carbon component. Other disadvantages of such carbon/polymer composites in the past include the difficulty of creating ultrathin, pinhole-free layers, brittleness, and oxidation of the polymer. Another serious problem with carbon powder/polymer composites is the ease with which oxygen evolution at the positive electrode occurs. This leads to build up of cell pressure and detachment of the electrode active material. Corrosion of carbon over time is also of concern, which undesirably leads to passage of electrolyte between cells as the solid carbon is consumed.
The novel bipolar plates of the present invention, unlike prior proposals, achieve the following significant advantages:
1. High electronic conductivity, i.e., electrical current is conducted between adjacent cells without significant loss of electrical potential because the conductivity is high and the resistance is low.
2. Impervious to liquid penetration, i.e., the electrolyte is not permitted to pass from one cell to another thereby preventing electrolytic shorts.
3. Ultrathin, i.e., the thickness is ultrathin whereby battery volume and weight are minimized, drop in potential is minimized.
4. High mechanical strength with flexibility, i.e., the integrity of each cell and battery are insured such that abusive conditions, such as overcharge, vibrations, and abrupt impact are inconsequential.
5. Electrochemical and chemical inertness, i.e., will not react with any of the other battery components, such as the electrolyte, electrode active materials, or seal material.
6. Capability of bonding effectively with the seal and the electrode, i.e., good electronic contact with the electrode is established and maintained so that cell resistance is kept to a minimum and a good interface with the seal material is provided to avoid leakage of electrolyte.
7. Low specific gravity (density), i.e., the weight of the battery is low because the specific gravity of the bipolar plate is low.
The peripheral seal is a critical element of a bipolar battery. The seal must be compatible with the bipolar plate, must function to prevent contact between adjacent electrodes, and prevent loss of electrolyte. In addition, seal must be inert, over the life of the cell or battery, to the electrolyte. A good bond must be formed between with the peripheral edges of the electrodes.
Epoxies are typically not a suitable seal, as they are not stable in sulfuric acid. Use of gaskets made from India rubber, and held in a bipolar stack under compression to avoid electrolyte from passing between the gaskets and the electrodes has been proposed. This material, when used with lead bipolar plates, works for short times, but over a period of months or years, the soft lead creeps. The continued application of pressure will allow for effective sealing even after the lead creeps, as long as the seals are absorbing the compressive pressure and not the electrode active regions (i.e., the battery core). For very high power designs, however, small intercell gap must be maintained. Only small changes in intercell gap can be tolerated. As the electrode edges (i.e., the seal region) grow thinner due to creep, excessive pressure applied to the battery core risks crushing of the electrode porous structure or other problems.
Numerous polymers have been proposed as a bipolar sealant. Polyethylene and polypropylene are effective when a carbon powder/polymer bipolar plate comprises unreliable polyethylene or polypropylene. These materials, as well as teflon (polytetrafluoroethylene), are inadequate due to recurring leakage between the bipolar plate and the seal.
The novel peripheral sealant of the present invention is compatible with the bipolar plate, serves to maintain requisite spacing between adjacent electrodes, prevents loss of electrolyte, is continuously inert to the electrolyte, and bonds excellently with the peripheral edges of the electrodes.
In one form of the present invention, long carbon fibers, arranged at random in a ultrathin mat configuration, provides the initial backbone for the bipolar plate. A commercially available mat of long carbon filaments can be used which has a void volume of approximately 90% by volume. Nevertheless, the carbon strands overlap and remain collectively contiguous both as the bipolar plate is fabricated and when the finished plate comprises part of a battery or battery cell. The long strands of carbon forming the mat may be rendered stable, individually and collectively by use of a phenolic binder, which leaves the mat stable in acid. The mat is diagrammatically represented in FIG. 5.
The carbon/fluoroelastomer mixture was prepared by first dissolving the fluoroelastomer polymer (which may be any of the FLUOREL� fluoroelastomers available from 3M) in a co-solvent of methanol and methyl isobutyl ketone. The carbon was then added, and the suspension was mechanically stirred. Finally, the mixture was ultrasonically blended to break up any carbon particle agglomerations and to provide for uniform solids distribution throughout the suspension. Both graphite powder (Union Carbide Grade 48), and glassy carbon (Johnson Matthey 38008, spherical powder, 0.4-12 um diameter, production temperature=2200� C.) were used. The solvent/fluoroelastomer ratio was typically 4:1.
Carbon fiber mat was obtained from Veratec Corporation. The carbon fibers were made with a phenolic resin binder to improve stability in acid environments. The mats (Veratec 8000020) consisted of long fibers which were laid upon one another somewhat randomly, as diagrammatically depicted in FIG. 5. Samples were provided in numerous sizes, from 0.50 opsy (ounce/yd2 ; uncompressed thickness of 0.0075-0.010 cm) to 2.0 opsy (0.0370 cm thick). Only the thinnest samples (0.50 opsy) were used. The 0.50 opsy material was approximately 4-6 fibers thick.
Samples of the mat were cut into squares 8cm�8 cm. A mat was then laid on a low porosity paper (Schleicher and Schuell B-2 weighing paper), and the carbon/fluoroelastomer suspension was loaded into the mat with a spatula, to the level of the top of the mat. The solvent was removed through evaporation. The loading procedure was repeated several times to fill the voids left by the solvent. The sample was then placed in a holder in a hydraulic press, and subjected to pressures of up to 5000 psi for an interval of at least ten minutes. After removal from the press, the sample was cured in nitrogen at 180� C. for ten minutes, to promote cross-linkage within the polymer phase.
An essential feature of a bipolar plate is the complete absence of pinholes. After visual inspection of the sample failed to reveal any pinholes, the sample was placed in an apparatus where one side of the material was contacted with liquid. If liquid was passed, the material was either discarded or patched.
After curing, the resulting thin sheet was then placed in container with KOH/H2 O (4M) and electrochemically oxidized for at least 15 minutes.
After rinsing the bipolar plate with deionized/distilled water, it was dried and quickly placed in a vessel for silanization. The vessel contained heptane (250 ml) and methyl trimethoxysilane (25 ml). The silanization reaction is run by heating the vessel and maintaining the temperature of associated condensers such that any heptane which boils returns to the vessel, while the methanol, dimethyl ether, and any other volatile or gaseous species are removed. The bipolar plate (sometimes also known as the bipolar electrode substrate), being complete, was immediately subjected to electrode plating in the manner described below.
Lead plating onto the bipolar plate was accomplished using a fluoborate bath (Bode, 1977). The plating was done at room temperature, and at a current density of less than 10 mA/cm2. Deposits of 0.002 cm were typical.
The Plante process was used to create a porous active mass at the exposed extension portion of the lead electrodeposit. The formation solution was 0.5 M KCIO4, 0.5 M H2 SO4 in H2 O, and the oxidation current density used was 2-3 mA/cm2. Experience showed that care had to be exercised to keep the potential of the electrode under 1.80 V (vs. a calomel reference), to avoid excessive oxygen evolution and possible subsequent loss of active material; therefore, in some situations, current densities were lower than 2 mA/cm2. The formation was accomplished by first oxidizing the lead for one hour, then reversing the current to form pure (porous) lead, and then removing the formation solution by carefully and repeatedly rinsing the electrodes. This procedure resulted in a suitable negative electrode. The lead was oxidized for several hours in aqueous sulfuric acid (without potassium perchlorate) to form porous lead dioxide. Bipolar electrodes were created by electrodepositing lead on both sides of the bipolar plate, and then creating a positive electrode active region on one side, and a negative electrode mass on the other side.
Bipolar batteries were made by using monopolar electrodes (one positive and one negative), and the appropriate number of bipolar electrodes sandwiched in between the monopolar electrodes, with a cellulose-based separator between adjacent electrodes. Prior to use, all electrodes (positive and negative) were partially discharged to a common point, typically 1 C/cm2. A separator (0.0025 cm wet thickness) large enough to cover both the electrode active area and the surrounding seal region, was placed over both the electrode active region and the edge of the electrode (i.e., the sealing region; see FIG. 4). The separator was placed over the electrode wet, to prevent expansion which occurred on wetting.
Both cellulose-based separators (such as various papers) or fiberglass separators can be used between adjacent electrodes in an electrolyte bath, as well as other materials. Each separator is held in place by contact with the electrodes, even though spaces are shown in FIG. 4 to improve clarity. Each separator is cut to match the dimensions of the electrode active material, placed over one of the electrodes, and then the facing electrode is placed next to the separator, as the battery is assembled. The electrolyte is added either before or after final assembly and placement of the sealant.
If desired, each separator can extend into the seal (surrounding the electrode active material region). When a seal is made, sometimes a gasket made from the appropriate seal material (in this case fiuoroelastomer is used), with the seal material having been previously applied to the bipolar plate edges. The gasket is then placed between adjacent electrodes as previously described. The gasket may be made by filling some thin structure, such as a porous paper, with the polymer. The structure allows careful definition of the gasket thickness. For example, if a gasket of 0.002 inches is desired, a porous paper of 0.002 inches thickness is cut to the appropriate shape, and the paper is filled with the fiuoroelastomer. After drying the gasket can be used. If, however, a cell separator is used which extends out from the active material region into the seal area, that part of the separator which is in the seal region is filled with the fluoroelastomer material, so that the gasket is but an extension of the separator itself.
A viscous fluoroelastomer solution (without the addition of carbon) was placed around the edge of the electrode, soaking through the paper to the edge of the electrode underneath. A temporary capillary was left through the seal region for filling the cell. Care was exercised so that the fluoroelastomer did not spread from the seal region where it was initially applied, into the inner part of the cell, which would block part of the electrode. When the fluoroelastomer solution was still tacky (i.e., before all solvent was completely removed), the adjacent (facing) electrode was placed over the electrode, so that the fluoroelastomer on the seal area also contacted the adjacent electrode. This process was repeated for each cell in the battery. The solvent was allowed to completely evaporate, and heat was applied to the edges of the battery to cure the fluoroelastomer. Finally, the cells were filled with electrolyte, the battery was compressed, and the capillaries were removed.
Cells were tested for their performance in test hardware specially designed for high current application. Performance data were recorded using a GW Instruments MacAdios A/D board, installed in a Macintosh II computer.
Some of the material tests involved the use of cyclic voltammetry. The sample was inserted into a 1000 ml Berzellius beaker containing electrolytically purified sulfuric acid (5 M) . A calomel reference was placed in the solution close to the sample. A pure lead counter electrode (99.9% pure) was used. A PAR 362 scanning potentiostat was used to control the potential, and the samples were scanned potentiostatically. All data shown are IR-corrected (unless noted). Scan rates were 50 mV/second, unless otherwise specified.
The electronic conductivity of bipolar plate, both with and without the presence of the backbone was tested. The reinforcing fibers or backbone material (comprising the mat) was prepared as discussed earlier, without the silanization treatment. Strips (1 cm�8 cm) were cut for measurement of conductivity. Similar strips were cut from material not containing the mat. The conductivity was measured using the four electrode technique, at room temperature. Samples of both types were prepared with various carbon loadings, over a range thought to bracket the practical region of interest.
Similar samples were also tested for rupture strength. An apparatus, shown in FIG. 5, was used to test this property. Material strips were held carefully at either end, and increasing amounts of force applied to one end to create a tensile stress. The amount of force that resulted in material rupture was recorded. If it was apparent that the break occurred at the point at which the material was clamped on either end, then the test was repeated so that there could be confidence that the rupture had not occurred due to improper clamping.
The specific gravity was measured simply by weighing the mass of a sample and then determining the volume displacement in a container of isopropanol. The specific gravity of the composite materials turned out to correlate with the arithmetic average of the specific gravity of the carbon and fluoroelastomer, so that the density could be calculated from the relative quantities of the ingredients used. The specific gravity of both the carbon and the fluoroelastomer was 1.80-1.84 g/cm3, so that a value of 1.82 g/cm3 was used in all calculations.
The supported materials were more than an order of magnitude increase in conductivity above the unsupported material. The carbon fibers are believed to be the major conducting phase. Conductivities of over 10 Ω-1 cm-1 were achieved in every case. A current density of 10 A/cm2 could be sustained with a potential loss of only 1 V/cm.
Conductivity tests were also done with samples with a silanized surface. The results (not shown) were comparable to those from samples without the silanized surface. Thus, it appears that the silane treatment did not provide any significant addition to electronic resistance of the material.
Even the weakest material, with the highest carbon loadings, had a rupture strength above the range likely to be encountered in a sealed battery. The presence of the polymer phase enhanced the strength of the carbon fiber mat, for high polymer volume fraction. The fluoroelastomer obtained from 3M Corporation, and used for this study, contained a small amount of carbon (15% ) as a filler. Thus, the carbon loadings shown represent the sum of this carbon and any additional carbon that was added.
It can be concluded from these data that the material possesses sufficient mechanical strength, even in very thin layers, for reliable use in a bipolar battery. The data also show that the fluoroelastomer has sufficient strength and other characteristics for use as a seal material, even should high pressures develop within a cell. No material degradation of the polymer occurred. The glassy carbon, due to its chemically stable surface and low surface area, significantly improved the electrochemical performance of the composite material. Further, the electrochemical improvement of the glassy carbon/fluoroelastomer composites (over materials with graphite or other carbons) does not come at the expense of conductivity. Oxygen evolution is suppressed with the use of silane treatment. The magnitudes of current densities is significant.
Batteries comprising the above-described bipolar plates and electrodes were built and tested. The sealing technique described proved to be completely effective. No shorts were observed when the separator is allowed to extend slightly outside the perimeter of the electrodes.
Several other batteries (5-20 cm2) were built using lead foil electrode substrates, to determine how long the high power outputs could be sustained, and how many pulses could be obtained. Pulses of at least 3 ms can be sustained at power outputs of over 10 W/cm2. Numerous high power pulses are possible without a significant recharge. For example, the fifth such pulse delivered an average power of 8 W/cm2. A small rest period, 22 ms, was chosen because of instrumentation limitations. The open circuit potential recovers after each pulse, but the recovery time increases with successive pulses. This suggests that acid diffusion is occurring during the rest. The implication is that even more high power pulses are possible, if a longer rest period is used, allowing time for the acid to move from the separator region into the electrodes. It also suggests that acid availability may be a limiting factor in the useful length of high power pulses.
In an alternative approach, the carbon fiber mat/carbon powder/fluoroelastomer bipolar material was prepared as described above. The silanization of the surface was done. Then, a slurry of lead powder (-325 mesh; Aldrich Chemical) in fluoroelastomer solution was used to coat each side of the bipolar plate. After solvent removal, the material was subjected to mild pressure. Since the lead was softer than the polymer, it was easily flattened. The lead deposition and the rest of the electrode process was then done as described above.
There are two benefits of this approach. First, there is no carbon exposed to the electrolyte. The only conductive material initially exposed to the electrolyte is lead metal. Thus, the silanized carbon surface is protected from any degradation which might have occurred. Second, the adhesion of the electrodeposited lead to the bipolar plate is enhanced. Although the lead in the fiuoroelastomer/lead surface might be subjected to eventual corrosive attach, the process is slow. Even if electrolyte eventually is able to reach the silanized carbon surface, this surface significantly inhibits corrosion and oxygen evolution. The lead/fluoroelastomer thus significantly extends the cycle life and shelf life of bipolar lead acid batteries. If the lead/polymer layer is kept very thin, then the weight and thickness of the bipolar plate are not substantially increased.
Reference is now made to the drawings, wherein like numerals are used to designate like parts through. FIGS. 1-3 illustrate a bipolar cell, generally designated 10, embodying principles of the present invention. As can be seen from inspection of FIGS. 1-3, the fundamental construction of bipolar cell 10 is one of lamination, achieved in the manner described above. Bipolar cell 10 comprises an ultrathin bipolar plate or semiconductive substrate, generally designated 12, shown as being disc-shaped in its configuration, although other shapes could be used as appropriate and desirable. The diameter of bipolar plate 12 is of a predetermined amount, which exceeds the diameter of other components forming a part of bipolar cell 10. Bipolar disc or plate 12 is formed in the manner described above, the flow chart for which appears in FIG. 6, so as to comprise a backbone of randomly oriented overlapping carbon fibers, strands, or filaments the voids of which are impregnated with a mix of carbon and fluoroelastomer which cures to form a composite membrane-like plate.
The composite bipolar cell 10 also comprises first and second, opposed electrodes respectively designated 14 and 16. One electrode functions as a positive electrode and the other as a negative electrode. Each disc-shaped electrode (14 and 16) is formed as one piece, but comprises two distinct layers or strata. Each electrode is electroplated generally concentrically directly upon and is, therefore, contiguous with a circular surface of the plate 12 in such a way as to ensure long-term adherence using the above-described methodology. More specifically, electrode 14 has a diameter substantially smaller than the diameter of bipolar plate 12 and comprises a first layer 18 comprising deposited lead, contiguous with and adhered to one surface of the plate 12, and an outer layer 20 comprising a porous lead dioxide, formed in the manner described above. Electrode 14 comprises an exposed, generally circular surface 22 which, when comprising a portion of a bipolar battery, is in direct contact with electrolyte.
Similarly, disc-shaped electrode 16 comprises a diameter substantially less than the diameter of the plate 12 and is generally concentrically aligned with the disc 12. Electrode 16 is formed as one piece, but comprises two layers or strata, i.e., an inner layer 24 comprising deposited lead, the interior surface of which is contiguously adhered to the associated surface of the plate 12, and an outer disc-shaped layer comprising porous lead, formed using the above-described methodology.
While the bipolar cell is illustrated in FIG. 2 in exploded perspective, the components, i.e., plate 12 and electrodes 14 and 16, are inseparable in their manufactured state. Thus, FIG. 1, although the dimensions are exaggerated for clarity of illustration, represents the manufactured configuration of the bipolar cell 10. The exposed generally circular surface 28 of the electrode 16 is in direct contact with electrolyte when cell 10 comprises part of a bipolar battery.
The nature of the carbon backbone comprising its long carbon strands is diagrammatically illustrated in FIG. 5.
Reference is now made to FIG. 4 which illustrates the manner in which bipolar cells 10 are combined sequentially to form a bipolar battery, generally designated 40. Each bipolar cell 10 and the components thereof are identified in FIG. 4 as those used in FIGS. 1-3, and no further description thereof is necessary at this point for one skilled in the art. In addition, bipolar battery 40 comprises positive and negative monopolar terminal cells, generally designated 42 and 44, respectively. Each monopolar cell 42 and 44 comprises, as illustrated, an exposed bipolar plate 12, as earlier described and a monopolar electrode, generally designated 46 and 48, respectively. Electrode 46 is identical to the previously described electrode 16, while the electrode 48 is identical to the previously described electrode 14. Accordingly, the portions of the electrode 46 and 48 are numbered in FIG. 4 so as to correspond with the numbers used for the electrode parts in FIGS. 1-3.
Between each cell of which battery 40 is comprised, is disposed an electrolyte reservoir 50 of ultrathin dimensions. Disposed in each electrolyte reservoir 50 is a thin planar separator 52, which may be formed of cellulose material and which functions to prevent adjacent electrodes from coming in contact with each other.
An annular, peripherably located cured fluoroelastomeric seal 54 spans between each adjacent pair of bipolar plates 12 in hermetically sealed relation, which in turn seals each electrolyte reservoir 50 against leakage. Each annular fluoroelastomeric seal 54 is formed as described above and accomplishes the objectives heretofore mentioned.
In partial summary, the above-mentioned work produced bipolar plates possessed all of the desirable properties mentioned above. A thin carbon fiber mat, which is approximately 90% void volume, is impregnated with a slurry consisting of carbon powder and fluoroelastomer. The surface of the material is then treated in any of several ways (such as application of an organosilane surface or coating the surface with tin dioxide) to reduce electrochemical activity of that surface, while still maintaining electronic conductivity. In this manner, oxygen evolution within the cell is significantly reduced. The resulting material is strong, flexible, highly conductive, chemically stable, quite electrochemically inactive, and can be made into layers which are ≦0.01 cm in thickness. Further, the specific gravity of the material is significantly lower than metals, approximately 1.8 g/cm3.
Typical preparation procedures are recited below. The fluoroelastomer material (any of the FLUOREL� fluoroelastomers; from 3M may been used) is dissolved in an alcohol/ketone cosolvent. A suitable fluoroelastomer is any of the FLUOREL� fluoroelastomers available from 3M. FLUOREL� designates commercially available fluoroelastomers used in injection molding, transfer molding, compression molding, extrusion, and other polymer forming applications. These fluoroelastomers come in a range of viscosities and other chemical and mechanical properties to allow a practitioner skilled in the an to choose a polymer suitable for the particular processing and manufacturing equipment used. While all of the FLUOREL� fluoroelastomers are suitable for the bipolar plates of the present invention, it is within the skill of an artisan to pick the particular fiuoroelastomer to optimize the desired properties of the bipolar plate. For example, certain of the fluoroelastomers are described as having enhanced stability in extreme chemical environments, having superior elongation retention after thermal aging and having a superior chemical and acid resistance. In the table below are shown descriptions of various FLUOREL� fluoroelastomers which may be used with the present invention, as disclosed in data sheets currently available from 3M Corporation.
FLUOREL� Fluoroelastomer Product Information Index
FLUOREL� Fluoroelastomers are highly fluorinated synthetic elastomers developed by 3M for long service under severe temperature and chemical conditions. Their composition and molecular weight are carefully controlled to combine easy processing with high mechanical strength, fuel and solvent resistance, and thermal stability. In addition to these properties, their non-flammability and resistance to oxidation, ozone and weathering make them especially applicable to advancing technologies in the aerospace, automotive, pollution control and chemical industries.
FLUOREL� Fluoroelastomers are sold as raw polymers to the rubber fabricating industry by the Commercial Chemicals Division of 3M. 3M does not manufacture molded fiuoroelastomer products.
The FLUOREL� Fluoroelastomers described in this book are as follows:
FLUOREL� Fluoroelastomers: Incorporated Cure Polymers for O-Rings
A low viscosity fiuoroelastomer designed for injection molding of sealing components that meet the major fluoroelastomer O-ring specifications. FLUOREL� FC 2121 exhibits excellent processability, improved mold release characteristics and ultra-fast cure cycles (30 seconds @ 400� F. (204� C.)).
A fluoroelastomer designed to provide excellent processing safety, excellent compression set resistance, low compound viscosity, and good scorch resistance while maintaining fast cure rates. In addition, it meets AMS-7259, AMS-7280, MIL-R-83248-Amendment 2-Type 1, and MIL-R-25897, Type 1* O-ring specifications.
A fluoroelastomer designed to provide excellent processing safety, ultrafast cure cycles, improved mold release characteristics, low compression set and high tensile strength necessary to meet the critical major O-ring specifications of AMS-7259, AMS-7280, AMS-7276B, and MIL-R-8328 Amendment 2-Type 1.
A high viscosity fluoroelastomer that provides maximum compression set resistance. It has excellent processability for a high molecular weight polymer. FLUOREL� FC 2179 is recommended for high pressure, severe environment applications.
A medium viscosity fluoroelastomer similar to FLUOREL� FC 2174 but designed to have less mold shrinkage. FLUOREL� FC 2180 possesses superior processing safety, good mold release and excellent compression set resistance.
FLUOREL� Fluoroelastomers: Incorporated Cure Polymers for Molded Goods
A low viscosity fluoroelastomer designed for injection molding of elastomeric molded goods items. The inate mold flow and release, in addition to hot tear characteristics of FLUOREL� FC 2122 have been optimized for injection molding of elastomeric articles with complex geometric profiles.
A low viscosity fluoroelastomer designed for injection and transfer molding of custom molded shapes. FLUOREL� FC 2123 has excellent hot tear properties that are essential for molding elastomeric articles with complex geometric profiles. In addition, FLUOREL� FC 2123 has excellent resistance to compression set.
A medium viscosity fluoroelastomer designed with a high tear strength and elongation to allow ale molding of molded goods with complex shapes. As a result, reject rates due to part tearing can be sharply reduced.
A low viscosity fluoroelastomer offering greatly improved mold release and mold flow without the usual sacrifice in physical properties associated with higher levels of process aids. It exhibits essentially the same cured physical properties as FLUOREL� FC 2170. FLUOREL� FC 2173 can be used alone or can be blended with other FLUOREL� fluoroelastomers to improve their mold release and flow.
A fluoroelastomer that is specifically designed for molded goods applications. It offers fast cure cycles with excellent processing safety for injection, compression and transfer molding operations. It offers incorporated mold release, good compression set resistance and high elongation at elevated temperatures to facilitate demolding without tearing.
A fluoroelastomer that combines high elongation for ease in demolding complex parts with exceptionally good compression set resistance. With a viscosity slightly higher than conventional molded goods fluoroelastomers, FLUOREL� FC 2181 offers improved mold release and is less susceptible to air entrapment. Since FLUOREL� FC 2181 shares the ultrafast cure rate, processing safety, and improved mold release of FLUOREL� FC 2174, it is also an excellent choice for low compression set O-ring cord.
A higher fluorine content (69% by weight) fluoroelastomer that offers improved chemical resistance, high elongation and good tear strength. The concept behind FLUOREL� FLS 2330 has been to combine these improvements with the processing advantages previously designed in our other molded good polymers. FLUOREL� FLS 2330 is recommended for molded goods designed to operate in extreme chemical environments.
FLUOREL� Fluoroelastomers: Incorporated Cure Polymers for Bonded Seal Applications
A fluoroelastomer for molded goods application with a slower cure rate, higher compression set and better bondability to metal than FLUOREL�FC 2176. It features the high elongation and good tear strength required for easy part removal from hot molds.
FLUOREL�Fluoroelastomers: Incorporated Cure Polymers for Extrusion Applications
A low viscosity fluoroelastomer optimized for scorch safety and improved flow characteristics. Excellent for use in difficult extrusion operations and also is an excellent choice for injection or transfer molding applications. Meets major automotive fuel hose specifications.
A fluoroelastomer polymer that has been optimized for scorch safety and the development of excellent physical properties at lower curing temperatures (e.g. 290�-300� F.). This makes FLUOREL� FC 2182 ideally suited for extrusion applications such as hose, thin-wall tubing and profiles. It is also an excellent choice for injection or transfer molding applications where exceptionally good mold flow, high elongation and good tear strength are required.
A low viscosity fluoroelastomer containing a higher level of fluorine (approximately 67% by weight) which contributes to improved retention of elongation after long-term heat aging. The lower viscosity of FLUOREL� FT 2320 enables this material to be processed on extrusion and transfer molding equipment.
FLUOREL� Fluoroelastomers: Incorporated Cure Polymers for Reinforced Composite Applications
A fluoroelastomer containing a higher level of fluorine (67% by weight) which contributes to improved retention of elongation after long-term heat aging and improved chemical and acid resistance compared to conventional fluoroelastomers. These properties lend themselves to meeting the thermal and acid resistance requirements of flue gas desulfurization systems.
FLUOREL� Fluoroelastomers: Raw Gums Without Curatives
A low viscosity fluoroelastomer gum that allows the fabricator to modify and blend different grade of FLUOREL� fluoroelastomers to achieve a broader range of processing and property characteristics. FLUOREL� FC 2145 can also be used as the base polymer in fluoroelastomer compounds cured with commercially available vulcanizing agents (e.g. diamines, bisphenols).
A medium viscosity fluoroelastomer gum which mills easily, calendars well, and can be extruded. FLUOREL� FC 2230 is amine or hisphenol curable. Conforms with FDA 21 CFR 177.2600 (c) (4) (1).
A high viscosity fluoroelastomer gumstock providing flexibility in the choice of curing systems for differing applications. Blend with incorporated cure grades to increase viscosity and green strength. Conforms with FDA 21 CFR 177.2600 (c) (4) (1).
A medium to high viscosity peroxide curable fluoroelastomer gum specifically designed to be used in convulcanizable blends with fluorosilicone or other synthetic elastomers to obtain products with a unique combination of physical properties, heat and fluid resistance, and low temperature characteristics. This feature makes compounds based on FLUOREL� FC 2260 extremely attractive in automotive applications.
A low viscosity fluoroelastomer gumstock designed for improved retention of elongation after long-term heat aging, improved resistance to volume swell by organic solvents, and improved acid resistance. The low viscosity enables this material to be processed on extrusion and transfer molding equipment.
A medium to high viscosity terpolymer gumstock designed for improved retention of elongation after long-term heat aging, improved acid resistance, and improved resistance to volume swell by organic solvents. FLUOREL� FT 2481 is amine or hisphenol curable.
A low fluid swell, high fluorine (69% by weight) tetrapolymer gumstock that can be vulcanized by peroxide, bisphenols, or aliamines. Compounds made from FLUOREL� FLS 2690 show excellent resistance to methanol and methanol containing fuel blends and other aggressive fluid environments.
FLUOREL� Fluoroelastomers: Masterbatch Polymers
A fluoroelastomer "masterbatch" of cure accelerators designed to be used with FLUOREL� incorporated cure polymers to accelerate the cure rate at both low and high temperatures. After dissolving the fluoroelastomer material in the cosolvent, the carbon powder is then added to the mixture, and the resulting slurry is stirred, either mechanically or ultrasonically. The slurry then is loaded into the carbon fiber mat, which has been laid on a flat surface. The solvent is removed, usually by evaporation. A new application of the carbon/fluoroelastomer slurry is done, and the process can be repeated as often as necessary to ensure adequate amounts of the material throughout the carbon fiber mat structure. After removal of the solvent, the material is then held in compression (for example, in a hydraulic press) for several minutes at high pressure, at least 100 psi. After removal from the press, the material is then cured by heating to 180� C. in an inert (nitrogen, argon, etc.) atmosphere). Curing can also be done in the open air, although some of the carbon on the surface will be oxidized in the process. Finally, the semiconductive layer is deposited on the surface. Preferably, that layer has been subjected to an organosilane surface treatment. This is done typically by immersing the material in a solution of heptane and methyltrimethoxysilane and heating. The resulting surface is quite electrochemically inert, raising the potential at which oxygen evolution occurs by at least 200 mV.
Each of the parts of this material has an important function. The carbon backbone contributes several desirable properties. It comprises long (≧1 cm), thin (˜0.002 cm) carbon fibers (which can be created by decomposing fibers of rayon, phenolic resin, polyacrylontrile, or other materials), which are superimposed upon one another. The use of this backbone significantly enhances the electronic conductivity, sometimes up to 20 times. It increased the mechanical strength (rupture strength) by an order of magnitude. It makes the formation of very thin layers easier to accomplish, as it serves as a skeleton of sorts for the bipolar plate. When a phenolic binder is used the backbone is stable in acid.
The fluoroelastomer of the admix also contributes valuable properties. The fluoroelastomer material is strong and flexible as well. This allows higher carbon loadings than are possible with polyethylene or polypropylene, which enhances the conductivity of the fluoroelastomeric/carbon powder phase of the bipolar plate. Perhaps the most attractive feature is the ease with which a seal is accomplished. When the fluoroelastomer (of course without the carbon powder added) is used as the seal material, a chemical bond between the electrode edges and the seal occurs, resulting in a highly reliable, long-term seal. The fluoroelastomeric seal is impervious to liquid or gas penetration.
Several carbon powders were used. The most successful was glassy carbon, due to its low internal surface area (and hence low electrochemical activity).
The deficiencies in past materials were largely overcome. These deficiencies were excessive activity for oxygen evolution at the potentials of the positive electrode, low conductivity, poor mechanical strength, excessive thickness, and in some cases inadequate bonding with the electrode active material and/or the seal material. The use of a carbon strand backbone for mechanical strength, enhanced conductivity, and reduced material thickness is a major contribution of the present invention. The use of glassy carbon in the filler additive reduced electrochemical activity. The treatment of the surface of the bipolar plate using silanization decreased electrochemical activity. Use of a fluoroelastomer material in the filler additive increased chemical stability, improved flexibility, and reduced material thickness.
The carbon backbone causes an increase in electronic conductivity.
The carbon/fluoroelastomer bipolar plates are ultrathin, are pinhole-free, have a low density and possess excellent flexibility and mechanical strength.
Uniform lead electrodeposits on the bipolar plates were achieved and porous electrode active material layers of high uniformity and high surface area were produced.
The use of glassy carbon lowered the electrochemical activity of the bipolar plate significantly when compared to other materials containing graphitic powder, resulting in benefits over previous carbon/polymer materials.
The silanization process proved effective in suppressing electrochemical activity of the bipolar plate. The evolution of oxygen due to electrolyte decomposition, which takes place at the positive electrode in a lead acid battery, and has been a major problem with previous carbon/polymer is significantly suppressed. The application of this process to a fluoroelastomer/carbon composite, not previously undertaken or proposed, proved successful. Silanization of both graphitic and glassy carbon composites was done. Endurance testing of silane-treated bipolar plate materials showed that a very low level of electrochemical activity can be maintained over at least the equivalent of 250 hours of battery operation. Cyclic voltammetry revealed no evidence of faradale degradation of the silane-treated surface at high potentials.
Cyclic voltammetry failed to reveal any evidence of decomposition of the fluoroelastomer in sulfuric acid, at either high or low potentials.
The use of the backbone/carbon/fluoroelastomer bipolar plate, in conjunction with a fluoroelastomer seal, results in a superb seal of the individual bipolar cells.
The invention may be embodied in other specific forms without departing from the spirit of essential characteristics thereof. The present embodiments therefore to be considered in all respects as illustrative and are not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
|Cited Patent
|Filing date
|Publication date
|Jan 11, 1974
|Jan 7, 1975
|United Aircraft Corp
|Novel composite fuel cell electrode
|Feb 2, 1976
|Dec 20, 1977
|United Technologies Corporation
|Fibrillar carbon fuel cell electrode substrates and method of manufacture
|Jun 27, 1977
|Jul 4, 1978
|Polaroid Corporation
|Flat batteries and method of making the same
|Jan 20, 1975
|Jul 4, 1978
|Gould Inc.
|Electrochemical system using conductive plastic
|Dec 19, 1977
|Aug 14, 1979
|Exxon Research & Engineering Co.
|Method of making bipolar carbon-plastic electrode structure-containing multicell electrochemical device
|Jun 11, 1979
|Jun 17, 1980
|General Motors Corporation
|Bipolar battery
|Dec 22, 1978
|Mar 31, 1981
|United Technologies Corporation
|High pressure-low porosity wet seal
|Jan 26, 1981
|Apr 20, 1982
|General Electric Company
|Positive electrode for lead acid battery
|Dec 17, 1982
|Mar 19, 1985
|Kureha Kagaku Kogyo Kabushiki Kaisha
|Process for preparing a fuel cell electrode substrate comprising carbon fibers
|Jan 3, 1985
|Jun 10, 1986
|Sanyo Electric Co., Ltd.
|Lead storage battery
|Dec 21, 1984
|Jan 20, 1987
|Allied Corporation
|Lead-titanium, bipolar electrode in a lead-acid battery
|Nov 20, 1986
|Jul 19, 1988
|Electric Power Research Institute, Inc.
|Stable carbon-plastic electrodes and method of preparation thereof
|May 14, 1990
|Aug 25, 1992
|Brigham Young University
|Electrochemical system using bipolar electrode
|Feb 1, 1991
|Dec 22, 1992
|Globe-Union, Inc.
|Composite substrate for bipolar electrodes
|Feb 26, 1992
|Aug 3, 1993
|Ensci, Inc.
|Bipolar plate battery
|Dec 28, 1992
|Dec 7, 1993
|International Fuel Cells Corporation
|Fluoropolymer laminated separator plate
|Jan 28, 1992
|Feb 22, 1994
|Daikyo Gomu Seiko, Ltd.
|Laminated sanitary rubber article
|Article in J. Electrochem. Soc., vol. 127, No. 12, Dec., 1990, by Rodney M. LaFollette and Douglas N. Bennion Entitled Design Fundamentals of High Power Density, Pulsed Discharge, Lead Acid Batteries.
|Article in New Scientist dated Nov. 22, 1989, entitled Technology: Bi Polar Batteries Break an Energy Barrier . . . .
|Article in New Scientist dated Nov. 22, 1989, entitled Technology: Bi-Polar Batteries Break an Energy Barrier . . . .
|Citing Patent
|Filing date
|Publication date
|Jul 1, 1999
|Oct 2, 2001
|Squirrel Holdings Ltd.
|Bipolar electrode for electrochemical redox reactions
|Mar 23, 1998
|Mar 5, 2002
|Volvo Technology Transfer Ab
|Lead battery with acid reservoirs mixed with active material in particles
|Mar 19, 2004
|Jan 30, 2007
|Nec Tokin Corporation
|Electrode and electrochemical cell therewith
|Jan 22, 2013
|Advanced Battery Concepts, LLC
|Bipolar battery assembly
|Mar 23, 2011
|Dec 10, 2013
|Xerox Corporation
|Coating composition and surface layer
|Mar 23, 2011
|Feb 11, 2014
|Xerox Corporation
|Intermediate transfer member
|Mar 23, 2011
|Apr 22, 2014
|Xerox Corporation
|Fuser member
|Dec 31, 2009
|Sep 2, 2014
|Lightening Energy
|Modular battery with polymeric compression sealing
|Mar 23, 2009
|Oct 21, 2014
|Lightening Energy
|Modular battery, an interconnector for such batteries and methods related to modular batteries
|Dec 3, 2001
|Jun 5, 2003
|Jeremy Chervinko
|Method for bipolar plate manufacturing
|Dec 18, 2002
|Oct 2, 2003
|Colley Kenneth J.
|Therapeutic angiogenic factors and methods for their use
|May 23, 2002
|Nov 27, 2003
|Lecostaouec Jean-Francois
|Carbon fiber reinforced plastic bipolar plates with continuous electrical pathways
|Mar 19, 2004
|Sep 30, 2004
|Tomoki Nobuta
|Electrode and electrochemical cell therewith
|Jan 20, 2010
|Jul 22, 2010
|Advanced Battery Concepts, LLC
|Bipolar battery assembly
|Dec 31, 2009
|Jun 30, 2011
|Lightening Energy
|Modular battery with polymeric compression sealing
|Mar 23, 2011
|Sep 27, 2012
|Xerox Corporation
|Coating composition and surface layer
|May 27, 2011
|Jan 29, 2014
|Bipolar all-solid-state battery
|May 27, 2011
|Mar 2, 2016
|U.S. Classification
|29/623.1, 29/623.2, 29/623.4, 29/623.5, 429/210
|International Classification
|Cooperative Classification
|European Classification
|Dec 10, 1999
|Fee payment
Year of fee payment: 4
|Dec 11, 2003
|Fee payment
Year of fee payment: 8
|Jun 16, 2008
|Maintenance fee reminder mailed
|Dec 10, 2008
|Lapse for failure to pay maintenance fees
|Jan 27, 2009
|Expired due to failure to pay maintenance fee
Effective date: 20081210


text:
Top Definition
To beat someone so bad they are only left with their basic human and life functions.
I'm going to beat the fuck out of you so bad that you'll be sent "back to the essence" of your life.
додав Jim Pigeon 16 Березня 2013
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subset: commoncrawl


text:
If you need immediate assistance, call 877-SSRNHelp (877 777 6435) in the United States, or +1 585 442 8170 outside of the United States, 8:30AM to 6:00PM U.S. Eastern, Monday - Friday.
net international investment position, current account, exchange rate movements
currency crises, Asia, international capital markets
international capital flows, portfolio allocation, home bias
home bias, international capital flows, portfolio allocation
Financial Panics, Sunspot-Like Equilibria
Financial panic, Sunspot-like equilibria
invoicing, vehicle currency, pass-through, exchange rate, producer currency pricing, local currency pricing
exchange rate, pass-through, international role of the dollar, trade balance, current account, vehicle currency
terms of trade, exchange rate regime
competitive devaluations, exchange rate shocks, contagion, global trade links, law of one price
productivity, exchange rate
Asset Pricing, Risk Management, Leverage
income, liabilities, current, account, international
current account deficit, valuation effect, intangible capital
foreign assets, valuation effect, exchange rate, interdependence
unemployment, labor market reforms, wage moderation
optimal monetary policy, exchange rate flexibility, competitiveness
balance of payments, U.S. current account, international assets and liabilities, financial integration, globalization, asset income
exchange rate, pass-through, center-periphery, invoicing, monetary policy, interdependence
center-periphery, exchange rate pass-through, invoicing, monetary policy
beggar-thy-neighbor, imports distribution
welfare, exchange rate fluctuations, international competitiveness
invoicing currency, vehicle currency, pass-through, international trade
Invoicing Currency, Vehicle Currency, Pass-Through, International Trade
international trade, Invoicing currency, pass-through, vehicle currency
international leverage, valuation effect, external position
International Capital Flows, Information Dispersion
information dispersion, international capital flows
International Capital Flows, Banking Integration, Crisis
currency, invoicing
currency invoicing, exchange rate
international risk sharing, terms of trade
Swiss franc lending, foreign currency lending, cross-border transmission of shocks, European bank balance sheets
cross-border transmission of shocks, foreign currency lending, Swiss franc lending
currency crises, exchange rate, international capital flows, lending boom, small open economy macroeconomics
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Top Definition
Catholic school down in GA that used to be called Pacelli High School. They won the state championship for baseball in 2009, but their football team sucks.
Go vikings!
Go vikings!
I go to St. Anne-Pacelli. It used to be just called Pacelli til they merged it with some stupid middle school where the 8 year-olds think they're 18.
লিখেছেন- phsclassof2014 17 de এপ্রিল de 2011
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text:
At the end of the October, IxDA Taiwan will hold a party for Halloween.
This time, we are cooperating with the magician of Taiwan Magic development Association (TMA).
The event should be the most fantastic interactive magic show that you've never learned.
Welcome to join us!
Date: 10/27 18:30 ~ 21:30 (GMT +8:00)
Venue: Taipei Stock ( http://www.taipeistock.org.tw/ )
Event Site: http://ixda.org.tw/yearend2012/
Registration: http://www.accupass.com/go/ixda_yearend2012


text:
Washout at Headingley
Click here for exclusive match highlights from every day's play, latest scores, reports, news and interviews during the LV= County Championship campaign
Day one of Yorkshire's LV= County Championship Division Two clash with Essex at Headingley Carnegie was abandoned without a ball being bowled due to persistent rain and a waterlogged outfield.
The inclement weather means White Rose fans will have to wait a little longer to see Australian batsman Phil Jaques in action following his return to the county he represented in 2004 and 2005.
The good news for Yorkshire was that Jaques' registration as a non-overseas player had been cleared at Lord's yesterday after the left-hander had met the England and Wales Cricket Board on Monday.
Want to know what's happening at your county? Interested in how your rivals are faring? Look no further than ecb.co.uk's county-by-county page


text:
These are for my mother. They are made out of a 3-ply yarn called Wings classic elite yarns. Its 55% alpaca 23 % silk 22% wool and its a dream to work with. Its spun 15% hollow to hold air like goose down and create "warmth without weight". Which is perfect for my mother who wants these to keep her feet warm during the winter months. I used elastic in the ankles to get the tightness mother wanted too.
The stitch is UOU/OUOO, just like the purple and green socks and uses the same double spiral technique.
One heel done
Detail of ankle/heel join
Finished Socks


text:
In message
, Peter M.
>James -
>I really enjoyed reading your comments as you obviously grasp the situation
>and the nuances of what it would take to implement!
Reading what James has to say, you certainly get the feeling that here
is somebody who knows *exactly* what he is talking about. I wish I
>On Wed, Oct 29, 2008 at 12:49 AM, James Hofmeister <
>email@example.com> wrote:
>> Hello All,
>> It would be very cool to see MPE running as a Xen virtual machine on Linux.
>> How to do this is something that donna and I have discussed over a glass of
>> California wine more than once...
Why not have two glasses and really blue-sky this thing? :-)
Given the above 'I wish I did', I can't comment much on the gory
technical details. But Pete replied to your:
>>- Capture all MPE Network calls at the socket interface replacing
>> sockets code, TCP, UDP, NIC drivers, etc. with the Xen Virtual machine
>> Network abstraction layer.
>Business apps shouldn't need to worry about this. Create a simple
>business app oreinted interface that calls the Linux network layer.
and I wonder if this is not to misunderstand what business users will be
looking for. The paradigm here must be the PA-RISC machine's HP3000
Compatibility Mode (even if HP can't spell it properly) which let users
of Classic systems port them, at the binary level and with the absolute
minimum of change, often none, to PA-RISC.
For an MPEmulator to attract existing HP3000 business users, it must
aspire to that level of compatibility, and even if the underlying
processes handle things quite differently, the goal must be that every
invocation of an openly documented MPE process is accepted, and produces
effectively the same results as it would have on a real HP3000.
Even if that process is three levels down in the binary of an app the
customer does not have the source code for. The MPEmulator can't turn
round and say 'Well, gee, I'm sorry, but none of this stuff exists here
and you'll have to go make Linux network calls now'.
Roy Brown 'Have nothing in your houses that you do not know to be
Kelmscott Ltd useful, or believe to be beautiful' William Morris
* To join/leave the list, search archives, change list settings, *
* etc., please visit http://raven.utc.edu/archives/hp3000-l.html *


text:
Top Definition
The act of placing ones horn betwixt two baps.
作者 Jane Amplebosom 2010年7月03日
Trending Now
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What Craig Ferguson ate while he was in Paris, France. Aired on the intro to the July 15th 2009 show when he was talking about what the French eat.
作者 Duncdar 2009年7月14日


text:
It was a tough start to the CT Whale season for Marek Hrivik, who missed the entire preseason and first two games of the year due to an undisclosed injury.
And that setback really seemed to affect him on the ice as he went scoreless in his first 14 games. Hrivik had 5g, 4a in nine playoff games with Whale last year after signing as a free agent at the end of the season.
But that's all changed for the big, physical forward as after last night's power play goal he now has 3g, 5a in the last six games.
…i was a big advocate for Hrivik this offseason, so I was beyond disappointed after his slow start. I should have figured he'd be in for a bit of a let down after taking the AHL by storm in the playoffs last year. But his physical game and soft hands are too good to keep him down for long. Really excited to see what Hrivik can do for the rest of the season.
Here's video of Hrivik's power play goal during the Whale's 4-3 loss to the Syracuse Crunch last night (1:20 mark)…
Chris Kreider was held scoreless last night and is in the middle of a five game goal drought.
Remember to follow me on Twitter & Facebook or e-mail me at email@example.com.


text:
Welcome to the Outpost Universe!
The Outpost Universe is a fan site devoted to the Sierra released games Outpost 1 and Outpost 2: Divided Destiny. Feel free to drop by our chatroom for a few games of Outpost 2, or some realtime chat with other fans. Or perhaps drop by our forums and leave us a message or join in on one of the topics. Here we have extensive discussions of gameplay, storylines, modding, or the latest patches, releases and projects being worked on.
The Outpost Universe has managed to attract both gamers and programmers alike. If you're a gamer, than join up with the other gamers for a few quick skirmishes, or perhaps discuss strategy on the forums. If you're a programmer, or looking to get into programming, then you are sure to find a few like minded people who can share what they know, or help you along. Or if you're a gamer who is looking for precise descriptions of how Outpost 2 works internally so you can perfectly optimize your next killer strategy, well, we have people that can probably help with that too.
Currently, the Outpost Universe offers a NetFix patch to help people play Outpost 2 over the internet who are behind a home router. It's not a complete WON replacement, but it's a significant step in the right direction. We also have a Hamachi network setup for people who would prefer to play over a VPN. For level designers, we have a mission development kit and map editor if you want to try your hand at making new Outpost 2 levels, but be warned, you pretty much have to be a programmer to use these tools, and you'll need a C++ compiler. Bug fixes and enhancement patches are also provided for various issues that have cropped up over the years, such as the option button highlighting, screen resolution issues, network gameplay problems, or just wanting to build twice as many units. We also provide a patched version with the cheats disabled, so you'll never again have to worry about cheats ruining your next online game of Outpost 2. Please be advised that different versions of Outpost 2 are not compatible with each other in network games, and most people here choose to use the patched version from the download section. The list of bug fixes and enhancments included is too large to list here, but if you're curious to see what we've done with the game, then check out ChangeLog.txt included in the download package.
So, why not stop by our forums to signup and say "Hello!", and see our current projects.
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About DGFT India
Directorate General of Foreign Trade – DGFT is a government organization in India working under Ministry of Commerce & Industry, DGFT is responsible to issue and formulation of Foreign Trade Laws, Rules and Regulations, Foreign Trade Policy, Foreign Trade Procedures, granting Importer Exporter - IEC code Number to Importers and Exporters, granting Pre Export and Post Export Benefits, Licences to restricted products in special cases and resolving the committee and cases relevant with Foreign Trade.
Major Roles and Functions of DGFT:
- DGFT granting 10 digits IEC Code Number.
- Promoting Foreign Trade with neighboring countries.
- To grant permission of goods to import and export under Policy condition "free" of Import Policy Schedule1 and Export Policy Schedule 2.
- Export Incentive/Benefits issuing authority, Standard Input Output Norms, DFIA etc under duty exemption and remission scheme of foreign Trade Policy chapter 4.
- DGFT provided Digital Signature facility to Importers and Exporters online eCommerce application filling since 2004.
- Issuing Notifications, Public notices and Circulars about changes in Foreign Trade rules, Regulations and amendments in existing Policy and procedure.
DGFT made recent changes in notifications include prohibition on any milk or milk products being imported from China, amendments in the Exam policy, a new standard for import and export of radial tires, various other major amendments in ITC HC policies and standard code of conduct, prohibition on export of non-basmati rice.
DGFT India - Export Benefits / Incentives
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Our DGFT Consultancy Matters :
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Contact to Us :
Email : firstname.lastname@example.com Mobile : 91+9312349598


text:
San Antonio Spurs 125, Miami Heat 95: The Spurs have been around longer than the Heat, and it showed
AT&T Center–In the Miami Heat locker room before the game, on the white board coaches like to put together with pre-game notes for players, Heat head coach Eric Spoelstra asked his team a question: Where do we stand?
Among the list of keys to the game, along with strategic things like denying three-point shooters open looks and swarming Tim Duncan, was a call to show resolve when things were not going well, trust under pressure, and play with enthusiasm.
The Miami Heat literally did none of those things, letting Manu Ginobili score on the opening tip on their way to a 36-12 first quarter deficit and a 30-point loss.
Where do the Heat stand? The same place as where they started when the Decision trio first united, as an undeniably dominating collection of talent hastily thrown together with scraps, that is still learning how to deal with adversity.
"We need this adversity. I've learned that the quickest way to bring change in this league is through adversity," Spoelstra said before the game. "Those events, as long as they don't break you, can fast track you towards what you want to do."
These San Antonio Spurs have seen those battles and fought those fights, having long ago proven themselves a hundred times over. In a question of talent versus chemistry, chalk tonight up to the team that wasn't practically  just assembled yesterday.
As LeBron James pointed out before the game, the players on the Heat have played plenty of close games, but this is the first go around that they have played them as a team. The difference in experience is noticeable.
"They know exactly what you're going to do defensively. Whatever you do or whatever you try and take away, they have a counter for," James said. "You take away the roll on the pick-and-rolls and they'll hit the guy in the corner for the three. Take away the threes and they hit the guy going to the rim.
"They've seen every situation and they've seen every defense, and right now they're just clicking on all cylinders," he added. "Everyone on their team has confidence. They all believe that when they get the ball they can make a play to help their team."
You can accuse LeBron James of many things, but you cannot question his basketball intelligence–his assessment is spot on. Of the eight rotation players that played (Antonio McDyess was given the night off), every single one of them reached double digits in scoring.
Manu Ginobili was the catalyst once again, scoring 11 of his 20 points in the first quarter, and seven assists. He and Parker (15 points and eight assists in a surprise start) might not be the top five players that LeBron James and Dywane Wade are, but they do enough to open up the games of the rest of their teammates.
And while Tony Parker was passing to Richard Jefferson who was driving and kicking to Matt Bonner for an open three-pointer, or Neal was passing up an open three-pointer of his own to find Bonner for a better look, or Bonner was catching a pass out of a Ginobili pick and roll (Bonner was open a lot), the Heat were a mess.
When adversity struck, it was LeBron James and Dywane Wade going one against the world, each picking up two fouls apiece in the first quarter, each of them on offensive fouls.
At times they're talented enough individually to put together successful runs in stretches, as they did in getting the lead back within 10 in the first half behind LeBron James' 15-point second quarter outburst.
But the singular approach eventually gave the Spurs something to focus their defense on, while the Heat defensive rotations were three, sometimes four steps behind where the Spurs were moving the ball.
"We were really focused, Â starting the game strong defensively and offensively," Ginobili said. "That gave us a lead pretty quick and that really got us going. We were feeling great, shots were falling, and of course when that happens, everything becomes easier.
"We know they jump out on pick-and-rolls hard and were were trying to move the ball, find the open teammate, and we did that great."
Spoken like a man who has been there before.


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Strength of Bond Covenants and Bond Assessment Framework
Noel Yahanpath
Eastern Institute of Technology
SzeKee Koh
Singapore Institute of Technology
May 21, 2012
Australasian Accounting Business and Finance Journal, 2012, 6(2), 71-90
We examine bond covenants of 29 New Zealand bond issues between 2001 and 2007. Results from the study indicate that protection provided for bondholders is weak and limited. On average, only 2-3 types of covenants are embedded with the issues and only 27% of these covenants provide full protection to the bondholders. However, bondholders are not compensated for taking the additional risk. We propose an alternative assessment framework that directly assesses the level of protection offered to bondholders. We calculate the covenant quality score for the issues and classify them into four levels of protection: very high protection, moderate, low and very low. Recent legislative changes will go some way towards improving investor protection and confidence, but the effect is yet to be seen. This proposed scoring framework can be used by potential investors to complement the traditional credit ratings when making their investment decisions.
Keywords: Government policy and regulation, bond covenants, bondholder protection
JEL Classification: G18, G31, G33
Date posted: October 18, 2010 ; Last revised: December 16, 2013
Suggested Citation
Contact Information
© 2016 Social Science Electronic Publishing, Inc. All Rights Reserved.
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text:
People with insomnia have troubles falling asleep, staying asleep or may wake up too early in the morning. Symptoms of insomnia can include:
Insomnia can be a disorder of its own or it can be the symptom or side effect of another problem. Some of the problems that can cause insomnia include:
People suffering from insomnia should talk with their healthcare provider. For people with mild insomnia, the answer to a better night's sleep may be as simple as practicing good sleep habits. Learn more about healthy sleep habits.
If the cause of insomnia is unclear, the doctor may recommend a sleep study. The Gundersen Sleep Center has 10 multi-function sleep study suites to help diagnose sleep problems.


text:
Its just a loose cable. The 10 inch cable that goes from your HD-DVR to the little adapter box that has the ethernet cable and is attached to the cable from the wall. That small cable is loose. Tighten the end that attaches to the small adapter box. The part with the rubber sleave should be tight and not twist at all. After you tighten, you will see the power and th network light stay a solid green. Its good to tighten the same on all boxes.
I was troubleshooting for hours, reboot, reset, manual IP programming. All it was was a loose cable. Goes to show that you have to do the basics before anything.
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Playback failed. No audio/video data packets received from server SOLVED!!
Started by xrism , Dec 14 2012 01:57 AM
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Posted 14 December 2012 - 01:57 AM


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by Colette Bouchez
Regardless of how much or how little you spend on your pregnancy wardrobe, the one area where you probably shouldn't skimp is in your undergarments. While some stores can go overboard in trying to convince you of what you need (will you really be all that comfortable in a pregnancy thong?) still, there are some basic undergarments that can make an important difference in not only how you look, but also how you feel.
According to Colette Bouchez, author of the new book Your Perfectly Pampered Pregnancy (Doubleday/Broadway Books, NY - Feb. 10, 2004), among the most important is a well-made pregnancy bra.
"Depending on how quickly your breasts enlarge, you may have to change sizes or even styles more than once during your pregnancy, so it's not necessary to buy a lingerie wardrobe right from the start," says Bouchez. That said, she advises that's a good idea to do a little window-shopping early on in your pregnancy so you can familiarize yourself with what's available. When the time comes for a new size or style you'll have an idea where to go to find what you like and need.
For most women, Bouchez says that a bra with wide set straps that are also thicker in width helps give much needed support while minimizing pressure on your shoulders.
"Remember, together, your breasts can gain as much as 5 pounds during pregnancy, which in case you don't already know, can feel a lot like hanging a watermelon around your neck and expecting your shoulders to carry the weight," says Bouchez. So, she says, the thicker the straps the more the extra weight will be distributed, which means the less your shoulders and upper back will feel the strain.
You should also seek out the smoothest, softest fabrics possible, choosing bras with a minimum of seaming in the cup area. In fact, the smoother and softer the cup is, the more comfortable your growing and tender breasts will feel. Also remember, says Bouchez, you are going to need more coverage than you did before, to help support painful and tender breasts, so by pass the décolletage styles and instead look for full cup coverage.
In general, she advises that when purchasing pregnancy lingerie look for fabrics and styles that will hold up to repeated washing. Remember, you probably won't purchase as many pieces as you normally might do, so each one is going to get more than the average number of washing. Styles with lots of lace or other trims, or thin or fragile fabrics may not hold up as long as you need them. What can also help: Hand wash and line dry your pregnancy lingerie. This puts less wear and tear on fabrics than a washer and dryer, the heat of which can also quickly beat up elastic and spandex.
Bottoms Up!
Whether or not you need to purchase pregnancy panties - or simply buy a larger version of what you already wear - is strictly a matter of personal taste. In fact, if you still want to wear those old bikinis, and they feel comfortable, and then feel free to do so - being pregnant doesn't have to mean starting every day by pulling on a pair of billowy Grandma Bloomers.
But Bouchez reminds us that during pregnancy you're likely to have extra vaginal discharge as as well as some degree of incontinence, so you'll want to choose fabrics that are easy to wash, dry quickly and don't stain easily. You may also need to choose a style with a substantial crotch width. In the event that you will want to wear a sanitary pad during your pregnancy, it helps if the crotch is wide enough for the pad to fit comfortably and adhere.
The one specialty lingerie item Bouchez insists you should definitely consider is maternity pantyhose.
"It seems no matter how large a size you choose in regular hose, the top is likely to slide off your belly and end up in an uncomfortable puddle at the top of your crotch. Maternity pantyhose have a wider, softer, stretchier top that can more easily smooth up and over your tummy, and remain relatively secure on your stomach for the whole day," she says. Another must-have for many women: A pregnancy girdle.
"While you may have detested even the thought of wearing this type of garment before you conceived, there is no question that you have to change your thinking. Not only will a pregnancy girdle help your clothes to look and fit better, the extra support it provides to your tummy AND your back can help ease many pregnancy aches and pains, and even prevent some from occurring at all," says Bouchez.
But if you are tempted to skip the maternity department and instead shop for a regular girdle in a larger size, don't. While support is important, Bouchez points out that it's equally important that your stomach does not experience extreme compression.
"Most maternity girdles concentrate on back support and have ultra stretchy, soft front panels that won't bind or cut your stomach in front. So, they are both safer and more comfortable to wear," says Bouchez.
After your baby is born she suggests investing in a postpartum girdle. These garments offer extra support under the stomach, while keeping waist compression to a minimum. Many also come with a snap closure on the crotch, allowing you to easily change a menstrual pad without having to pull the girdle down.
Colette Bouchez is an award winning medical journalist with more than twenty years experience. She is the former medical writer for the New York Daily News, and the top selling author of The V Zone, co-author of Getting Pregnant and upcoming book, Your Perfectly Pampered Pregnancy. Currently a daily medical correspondent for HealthDay News Service/The New York Times Syndicate, and WebMD, her popular consumer health articles appear daily online, as well as in newspapers nationwide and in Europe and Japan. She is a regular contributor to USAToday.com, ABCNews.com, MSNBC.com and more than two dozen radio and television news stations nationwide. She lives in New York City.
Copyright © Colette Bouchez. Permission to republish granted to Pregnancy.org, LLC.


text:
Government shutdown: What happens next?
POSTED: 06:21 AM PST Dec 24, 2013 UPDATED: 12:59 PM PDT Oct 01, 2013
The views expressed are not those of this company or its affiliated companies. Please note by clicking on "Post" you acknowledge that you have read the Terms Of Service and the comment you are posting is in compliance with such terms.blog comments powered by Disqus


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text: Alan Karp: >David Wagner wrote: >> I don't understand why anyone thinks that limiting the bandwidth of >> covert channels is a very useful solution. If you set the limit at no >> more than a few hundred bits/second (as the Orange Book did), then you >> can leak a crypto key in seconds (or less). > >Since the people in an MLS system are trusted, but some of the programs >they run are not, there's no reason for the untrusted app to have access >to the crypto key. Absolutely. That's what I advocate, too: solve this with simple access control stuff to ensure that untrusted code never learns any secrets, instead of fancy MLS stuff to try to prevent untrusted code from leaking the secrets it is given. If do what I advocate, then you don't need Bell-Lapadula-style MLS, you don't need the *-property, you don't need complicated information flow tracking mechanisms... So I don't see the point of BL-style MLS.


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|Regular Price:
|Our Sale Price:
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|$2.00 (20%)
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|7.99 (Whats this?)
Our SKU #SR3036V
Brand: Sable and Rosenfeld
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Manufacturer: Sable and Rosenfeld
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UPC / EAN Code: 069702900513
Tags: vodka, fiery, peppers, Spanish, Turkish, cocktails, bar, All Natural Ingredients, Gluten Free, Fat Free, Cholesterol Free
Vodka Tipsy Fiery Olives by Sable & Rosenfeld is an all-natural product essential to a well stocked bar. Large Spanish olives are stuffed with a large Turkish red pepper and then bathed in Vodka. These olives are fiery hot, crunchy and delicious. Use as a garnish for martinis, Bloody Marys (recipe for a Mexican Mary is printed on each bottle) or other cocktails. Or simply serve with your favorite sandwich or relish tray.
Each bottle of Sable & Rosenfeld Vodka Tipsy Fiery Olives contains approximately 27 olives.
Best by 7/1/16
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