US20050084755A1 - High capacity alkaline cells - Google Patents

High capacity alkaline cells Download PDF

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Publication number
US20050084755A1
US20050084755A1 US10/914,958 US91495804A US2005084755A1 US 20050084755 A1 US20050084755 A1 US 20050084755A1 US 91495804 A US91495804 A US 91495804A US 2005084755 A1 US2005084755 A1 US 2005084755A1
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Prior art keywords
recited
electrochemical cell
anode
cathode
separator
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US10/914,958
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English (en)
Inventor
David Boone
William Bushong
Paul Cheeseman
Gregory Davidson
Mario Destephen
Zihong Jin
Jon Luecke
Erik Mortensen
Ernest Ndzebet
Karthik Ramaswami
Sergey Sazhin
Viet Vu
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Spectrum Brands Inc
Bank of New York Mellon Corp
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Individual
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Priority to US10/914,958 priority Critical patent/US20050084755A1/en
Priority to ARP050100436A priority patent/AR047875A1/es
Priority to PCT/US2005/004488 priority patent/WO2005122301A2/en
Priority to AU2005253513A priority patent/AU2005253513A1/en
Priority to CA002569105A priority patent/CA2569105A1/en
Priority to JP2007515050A priority patent/JP2008502107A/ja
Priority to EP05713430A priority patent/EP1779450B1/en
Priority to US11/055,508 priority patent/US7740984B2/en
Publication of US20050084755A1 publication Critical patent/US20050084755A1/en
Priority to US11/354,729 priority patent/US20060257728A1/en
Assigned to RAYOVAC CORPORATION reassignment RAYOVAC CORPORATION ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: RAMASWAMI, KARTHIK, VU, VIET H., BOONE, DAVID, DESTEPHEN, MARIO, DAVIDSON, GREGORY J., SAZHIN, SERGEY, BUSHONG, WILLIAM C., LUEKE, JON, MORTENSEN, ERIK, NDZEBET, ERNEST, JIN, ZIHONG, CHEESEMAN, PAUL
Assigned to ROVCAL, INC. reassignment ROVCAL, INC. ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: RAYOVAC CORPORATION
Assigned to GOLDMAN SACHS CREDIT PARTNERS L.P., AS COLLATERAL AGENT reassignment GOLDMAN SACHS CREDIT PARTNERS L.P., AS COLLATERAL AGENT SECURITY AGREEMENT Assignors: AQUARIA, INC., AQUARIUM SYSTEMS, INC., ROVCAL, INC., SOUTHERN CALIFORNIA FOAM, INC., SPECTRUM BRANDS, INC. (FORMERLY KNOWN AS RAYOVAC CORPORATION), TETRA HOLDING (US), INC., UNITED INDUSTRIES CORPORATION, UNITED PET GROUP, INC.
Assigned to THE BANK OF NEW YORK MELLON, AS COLLATERAL AGENT reassignment THE BANK OF NEW YORK MELLON, AS COLLATERAL AGENT ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: GOLDMAN SACHS CREDIT PARTNERS L.P.
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
    • H01M4/5825—Oxygenated metallic salts or polyanionic structures, e.g. borates, phosphates, silicates, olivines
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/24—Alkaline accumulators
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M2004/021—Physical characteristics, e.g. porosity, surface area
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries

Definitions

  • FIG. 6 is a graph plotting the discharge behavior of pure CuO and various CuO/CuS mixtures in a half cell vs. a Hg/HgO reference electrode.
  • FIG. 9 shows a graph representing the discharge behavior of a layered cathode containing (EMD) MnO 2+ CuO under conditions using jet-milled CuO, 66% BIP Sieved anode, with 34-2 electrolyte and 25-0 pre-wet electrolyte, and a 5 mA discharge;
  • EMD layered cathode containing
  • FIG. 23 is a graph plotting the discharge profile of a pair of cells having CuO/CuS cathodes to illustrate the effect of including PVA in the cathode;
  • an axially extending cylindrical cell 18 has a positive terminal 21 , a negative terminal 23 , and a positive current collector in the form of an unplated cylindrical steel container 20 .
  • Container 20 is initially closed at its positive end 25 proximal the positive terminal 21 and open at its end proximal the negative terminal 23 such that the negative end of container is crimped to close the cell 18 as is understood generally by a skilled artisan.
  • One aspect of the present invention provides a cathode having an active material whose discharge voltage is higher than CuO while providing cell service life at least 60% as long as a CuO electrode.
  • the discharge voltage of the battery incorporating a cathode additive having either 1) a higher discharge voltage than the first cathode active material or 2) a lower discharge voltage than the first cathode active material but, when combined with the first cathode active material, produces a combination having a discharge voltage higher than the first cathode active material, produces a discharge voltage greater than 1.05 V for at least an initial 5% of the cell discharge period (meaning the first 5% of a total length of time that the cell is discharged continuously until the operating voltage is reduced to a level of 0.8V) at a current density of 5 mA/g.
  • a cathode constructed in accordance with aspects of the present invention achieves a higher discharge voltage than prior art cells including copper oxide cathode active materials, whose discharge voltages were not sufficiently high to operate modern devices.
  • Suitable examples of positive electrode materials can include, but are not limited to, MnO 2 (EMD or CMD), NiO, NiOOH, Cu(OH) 2 , Cobalt Oxide, PbO 2 , AgO, Ag 2 O, Ag 2 Cu 2 O 3 , CuAgO 2 , CuMnO 2 , and suitable combinations thereof.
  • the anode is already partially discharged when the CuO discharge commences, contributing anode polarization to the cell voltage.
  • the presumed net effect of these processes is that the CuO material operates at a lower voltage than it otherwise would, resulting in a lower than desirable battery voltage as shown in FIG. 2 .
  • cathode densities of about 3.5 g/cc up to about 4.5 g/cc of cathode volume can be achieved.
  • processing conditions e.g., using a standard hydraulic or pelletting press
  • cathode densities of about 3.5 g/cc up to about 4.5 g/cc of cathode volume can be achieved.
  • concentrations can also produce the stated cathode densities. This allows significantly more active material to be packed into a cell, to provide batteries with longer service life than previously known. AA cells with delivered capacities up to 4 Ah may be produced, which are significantly improved OVER present day commercial alkaline batteries having deliverable capacities of about 2.5-2.8 Ah.
  • Chemically synthesized agglomerates of a nano-CuO may also be used for the cathode.
  • Such materials can be obtained from NanoScale Materials, Inc. 1310 Research Park Drive, Manhattan, Kans. 66502 USA.
  • the particle size is within a range whose lower end is between, and includes, 0.1 microns and 10 microns, and whose upper end is between, and includes, 50 microns and 150 microns.
  • Various versions of the present invention recognize the good lubricating properties and high conductivity of CuS in practice. Use of CuS in a mixture therefore allows the reduction or elimination of conducting carbons in the cathode and provides an additional 5-7 wt. % room for active material, thereby further increasing cell capacity.
  • the conductive and lubricating properties of CuS may be utilized to replace the conductive carbon coating 22 currently used on the internal can surfaces in alkaline batteries (See FIG. 1 ).
  • anode-fouling species examples include various Cu, Ag, S, Fe, Ni, and Sb species.
  • one or more sulfur species such as sulfide, sulfate, sulfite, or thiosulfate may be produced that tend to migrate to the anode, thereby fouling the anode.
  • sulfur species such as sulfide, sulfate, sulfite, or thiosulfate
  • the additive can be included in the anode, cathode, electrolyte, or separator and operate at the location where anode-fouling species would be generated, at the separator where the fouling species would migrate through the separator, or after anode-fouling species migrate through the separator from the cathode towards the anode but prior to the fouling species interact with and foul the anode.
  • the additive can operate either by binding to the sulfur species or chemically interacting (e.g. by oxidation, reduction complexing, coordinating, etc . . .
  • a high capacity anode-formulation is also provided for use in alkaline cells.
  • cathodes of conventional alkaline cells for example cathodes whose cathode active ingredient is MnO 2 , consume more water by the cathodic reaction than is produced by the anodic reaction (i.e., the reaction of zinc anode and electrolyte).
  • the total cell reaction as represented, consumes water as shown below and are thus said to be “water consuming” Zn+MnO 2 +H 2 O ⁇ ZnO+MnOOH
  • the particle size distributions of this invention also provide increased porosity, which allow for less precipitation of ZnO on the zinc particle surface, thereby delaying anode passivation compared to the particle size distributions typically found in conventional cells.
  • This approach is effective for use in the anodes of various aspects of the invention and can be used alone or in combination with other improvements disclosed herein.
  • a suitable zinc particle size distribution is one in which at least about 70% of the particles have a standard mesh-sieved particle size within a 100 micron size range and in which the mode of the distribution is between about 100 microns and about 300 microns. It is desirable that 70% of the particles be distributed in a size distribution range even more narrow than 100 microns, for example 50 microns or even 40 microns or less.
  • a suitable gelled anode as described herein comprises a metal alloy powder (desirably an alloyed zinc powder), a gelling agent and an alkaline electrolyte.
  • a metal alloy powder desirably an alloyed zinc powder
  • a gelling agent and an alkaline electrolyte.
  • a suitable zinc powder alloyed with In, Bi, Ca, Al, Pb, etc.
  • zinc refers to a zinc particle that may include an alloy of zinc as is well known to one skilled in the art.
  • the anode may contain little or no mercury (e.g., less than about 0.025% by weight).
  • known gelling agents other than the desirable sodium polyacrylate gelling agent are suitable for use in various aspects of the present invention. Such gelling agents include carboxymethyl cellulose, crosslinked-type branched polyacrylate acid, natural gum, and the like.
  • the present inventors recognize that another factor that controls cell performance relates to the surface area of the anode. Specifically, increasing the active anode electrode surface area provides sufficient active reaction sites needed to keep up with the cathode reaction at high discharge rates. Accordingly, cells are provided having a predetermined amount of zinc particles (which may either be in the form of zinc or a zinc alloy) added to the anode gel.
  • the anode may include zinc particles between 75 and 105 micrometers, with the advantages in cell performance being enhanced when the anode gel has an electrolyte (KOH) concentration less than 30%, alternatively between 20% and 30%.
  • KOH electrolyte
  • KOH concentration is between 30% and 40%, and desirably between 33% and 38%.
  • Another suitable range is between 20% and 34%, alternatively, between 25% and 33%, and alternatively, between 25% and 30%.
  • a “low KOH concentration” as used in this disclosure refers to a KOH concentration within or below any of the above-stated ranges.
  • cathodes that contain oxides that comprise copper, but wherein the cathode contains not CuO alone, but CuO in combination with other oxides, sulfides, or mixed copper oxide materials.
  • the cathode may be more water consuming than in others.
  • one skilled in the art will be able to determine the acceptable modification to the anode that corresponds to the reduced water consumption of such cathodes.
  • the zinc PSD's disclosed herein desirably can be distributed within a narrow window of 200 microns and, alternatively, 150 microns, meaning that between and including 90% and 95%, and up to 100%, of the particle sizes, by weight, are within the 150, or 200, micron window, and in particular are tight distributions substantially centered around 100 ⁇ m, 175 ⁇ m and 250 ⁇ m, and 300 ⁇ m (meaning that between and including 90% and 95%, and up to 100% of the zinc particles have particle sizes centered around the specified sizes).
  • mesh sizes corresponding to these particle sizes can be identified using ASTM Designation: B214-99.
  • the PSD's herein increase the zinc anode porosity, thereby reducing passivation.
  • a zinc powder with a tight PSD centered around 100 ⁇ m is illustrated, for example, in FIG. 12 .
  • the invention includes similar distributions centered about 175 ⁇ m and 250 ⁇ m, as described above.
  • the zinc powder illustrated in FIG. 12 includes additives including bismuth, indium, and lead as will be understood by those having ordinary skill in the art.
  • FIG. 13 illustrates cell performance for 1) a first control cell having a 37% electrolyte concentration (concentration by weight of KOH with respect to the electrolyte mixture) and a 2% zinc oxide concentration in the anode, and a conventionally distributed anode, and 2) a second cell constructed in accordance with the principles discussed herein having an electrolyte at 30% KOH concentration and 2% zinc oxide concentration by weight in the anode, and an anode distribution as described herein.
  • FIG. 13 thus illustrates the increase in operating voltage when anodes as described herein are used in Zinc-CuO cells.
  • suitable polymers retain electrolyte in the separator where, in the separator, the retained electrolytes have a pH value lower than the bulk electrolyte found in the cathode and the anode.
  • the separator-retained electrolyte desirably has a pH value that is 0.5 to 3 pH units lower than the pH of the bulk electrolyte.
  • the extent to which electrolyte is retained in the separator, and the extent to which the pH of the retained electrolyte can vary from that of the bulk electrolyte, can be modulated by polymer side groups provided on the backbone.
  • an alkaline electrochemical cell constructed in accordance with the principles of the present invention can be significantly enhanced by providing in the cell an improved barrier-separator system that effectively limits the migration of anode-fouling soluble species from the cathode into the anode compartment while permitting migration of hydroxyl ions.
  • cathode materials such as CuO, CuS, CuAg 2 O 4 and Cu 2 Ag 2 O 3
  • the cathode of the invention can also be provided with an agent that effectively limits anode-fouling soluble species from migrating from the cathode toward the anode by interacting with the soluble species.
  • Agents such as polyvinyl alcohol, activated carbon, natural and synthetic clays and silicates such as Laponite, etc. have shown an ability to adsorb or block ionic species.
  • Sulfur species can also dissolve from the sulfide additives or other sulfur containing coumpounds present to form soluble sulfur species in the additives or other sulfur-containing compounds present to form soluble sulfur species in the alkaline electrolytes. These species can further react with each other and with other ions dissolved in the electrolyte, precipitating out either within the separator or at the separator-to-electrode interface, thereby hindering electrolyte transport between the cathode and anode or causing bridge shorting.
  • the above mentioned species can also react with each other and with other ions dissolved in the electrolyte, precipitating out either within the separator or at the separator-to-electrode interface, thereby blocking desirable ionic and electrolytic transport between the cathode and anode.
  • cylindrical cell separators have seams (in particular along one or more ends and the side of a cylindrical cell separator) that, if not adequately sealed, can provide avenues for these species to still diffuse and migrate into the anode.
  • Conventional cylindrical cell separators cannot adequately limit such soluble species from migrating into the anode compartment.
  • a “side seam” is defined herein as a seam located at overlapping ends (or potentially adjacent ends) of a cylindrical separator.
  • An “end seam” is defined herein as a seam disposed at one of the open ends of a cylindrical cell separator. It should thus be appreciated that the terms “positive end” and “negative end” refers to the ends of the separator that are disposed proximal the positive and negative ends of a cylindrical cell, respectively, after separator installation into the cell.
  • a “peripheral end seam” is defined herein as the outer periphery of a flat and round, square or rectangular separator that is to be sealed when installed into a button or prismatic cell.
  • PVA film samples containing significant amounts of plasticizer are less effective at limiting migration of soluble species while maintaining acceptably low ionic resistance. It may be appreciated by those skilled in the art, that effective limitation of the migration of soluble species can be attained by selecting the polymer properties, including the chemical composition, molecular weight, molecular weight distribution, additives and by appropriate cross-linking.
  • polymer solutions may also be used to coat or impregnate non-woven or cellophane separators and achieve effects similar to those seen with PVA when used as a separator for electrochemical cells having a zinc anode and a cathode that contains anode-fouling soluble species.
  • polymer solutions can coat the anode or cathode directly, thereby providing a conformal separator.
  • a hybrid separator e.g., a non-woven fabric separator coated or impregnated with the polymer
  • a conformal separator that enables hydroxide ion transport while effectively limiting the migration of soluble copper, silver, and sulfur species.
  • This type of separator can also minimize the need for separate side seam or bottom seal.
  • EVA ethyl vinyl acetate
  • vinyl acetate-ethylene copolymers vinyl acetate polymers that can be coated or impregnated onto a nonwoven separator to effectively limit the migration of anode-fouling soluble species such as, for example, copper, silver, sulfides, polysulfides, thiosulfates, sulfites, iodates, iodides, phosphates, silicates, or carbonates as described in Example 7 below.
  • Another suitable polymer is EVOH.
  • Air permeability of the separator can be measured in Gurley seconds, as appreciated by one having ordinary skill in the art. Because the Gurley test measures the length of time necessary to pass a predetermined volume of air through a separator, a longer time measurement is an indication of low air permeability.
  • Gurley Air Permeability of 500 Gurley seconds or higher has been found suitable for use in an electrochemical cell described above, while overcoming difficulties 1, 2, and 3. The Gurley measurement was taken using Model No.
  • routes of fluid communication between the cathode and the anode, including the separator seams are sealed to minimize or eliminate fluid communication (e.g., of bulk electrolyte) except through the separator material, at least one layer of which is provided.
  • fluid communication e.g., of bulk electrolyte
  • substantially all anode-fouling species in the bulk electrolyte are desirably retained on the cathode side of the separator and do not migrate to the anode.
  • the separator is thus associated with an “Exclusion Value” that refers to a percentage of soluble species that is prevented from migrating from the cathode through the separator to the anode.
  • the cell can tolerate some migration through the separator of anode-fouling soluble species.
  • a suitable separator effectively limits the migration of anode-fouling soluble species if the separator passes less of the species than the anode active material can tolerate without becoming fouled. Substantially lower amounts of the soluble species are desired, however.
  • a substantial portion of the electrolyte retained in the separator is associated with (typically, non-covalently associated with) the polymer backbone or its side groups.
  • a suitable measure of such an association is obtained by analyzing the separator material to determine the temperature at which water retained in the separator melts after freezing. Whereas free water retained in, but not physically associated with, the polymer melts at about 0° C., a lower melting temperature indicates an association with the polymer and, accordingly, a desirable separator.
  • a suitable method for determining the temperature at which separator-retained water transitions to the liquid phase employs a simple differential scanning calorimetric (DSC) test.
  • a sealed separator while applicable to all battery systems, finds particular applicability to a system such as that described herein, where soluble species from one electrode can migrate to the other electrode, thereby degrading performance or shelf life. These are generally referred to as anode-fouling soluble species. In such cases, separator material alone can be insufficient because soluble species can migrate around a seam or end of the separator, unless a substantially impervious seal is provided.
  • fluid communication between the cathode and the anode via routes around the separator is minimized or eliminated by sealing the separator such that the anode is in substantial fluid isolation from the cathode except via a route through the separator.
  • the method of sealing the separator material can be achieved by known methods, including adhesive sealing, heat sealing, ultrasonic sealing, and the like.
  • the separator so formed can take the shape of a tube having a closed end.
  • water-soluble separator materials including polyvinyl alcohol, softening the materials with a limited amount of water and then sealing with heat or pressure or both can form the seal. This arrangement is desirable as the fused separator seal typically limits the likelihood of an undesired channel for direct fluid communication between the cathode and the anode.
  • a seam-sealed and bottom sealed separator configuration can be produced externally and then inserted into a cell, or can be produced in situ after insertion of a spirally wound, convolute or cross-placed separator tube into a cell cavity.
  • Two suitable separator materials are presented as examples of ex-situ seals.
  • One material is cellophane and the other is a hybrid separator, which comprises a non-woven fabric coated with PVA, which is cross-linked using a cross-linking agent.
  • PVA polyvinyl alcohol
  • Gurley air permeability >500 sec. Low air permeability ensures that in a battery, when the polymer swells upon absorbing electrolyte, there would be substantially no paths for the transport of the anode-fouling soluble species through the material.
  • a layer of viscous PVA solution e.g., 2-10% by weight in water
  • a cross-linking agent such as sodium borate or others known in the art.
  • the seal area cross-links immediately, while also bonding the two surfaces together.
  • a simple test of 5 days soak in concentrated KOH electrolyte shows that the seam is intact and cannot be physically torn apart, suggesting good operational characteristics in a battery.
  • the efficacy of the seal in effectively limiting anode-fouling soluble species may be tested using the Exclusion Test described herein.
  • Other suitable cross-linkable polymers suitable or use as the adhesive include but are not limited to polyethylene glycol, polyvinylbutyral, and polyvinylpyrrolidone.
  • the substantially dry PVA/boric acid coated separator is wound around a mandrel (as in present day alkaline cell manufacturing) with at least some overlap between layers.
  • a mandrel as in present day alkaline cell manufacturing
  • One end is folded to form a cup shaped bottom, and the tube is inserted into a cathode cavity.
  • a bottom disk comprising the same or other separator material coated with a cross-linkable polymer and cross-linking agent, as above, is next inserted into the tube so as to rest inside the folded bottom of the wound separator tube.
  • Another method of achieving the same objective is to start with a non-woven paper, which has a sufficient amount of cross-linkable polymer, e.g. PVA (but without cross-linking agent) coated on it to render it substantially impervious (Gurley air permeability>500 sec).
  • a folded bottom is created and it is inserted into a cathode cavity as described above, followed by insertion of a bottom cup coated or impregnated with PVA.
  • Cross-linking agent e.g. sodium borate
  • polymers and/or cross-linking agents can be used to achieve the same end result.
  • carboxylic groups can be introduced into PVA and cross-linked with glutaraldehyde to improve film properties, as can regenerated cellulose coated or laminated on PVA or modified PVA.
  • PVA can be copolymerized with acrylic acid to significantly lower ionic resistance.
  • Acetylized PVA films can be modified with polyacrylic acid.
  • Acrylic- or methacrylic acid-grafted PVA can also be used.
  • grafted methacrylic acid on a polyethylene or polypropylene membrane is also suitable as a separator.
  • a second general method of producing a sealed separator is physical, using a heat-sealable polymeric material, such as PVA, polyethylene, polypropylene, nylon, and the like.
  • the seal is formed by providing a layer of the polymeric material, in the form of a continuous film, or porous fibrous film, and inserting the layer into the area to be sealed (e.g., the outer periphery of a separator to be installed into a size AA cell).
  • the separator then can form a seal under controlled heating with or without application of pressure.
  • the heat sealable polymeric layer can also be applied to one surface of a separator layer (that may or may not be heat sealable), and subsequently wound into a cylinder, such that the overlapping region will comprise a layer of the sealable polymeric material interfacing with another separator layer.
  • the heat sealable polymeric material will thus seal against the other separator layer under a controlled heating condition.
  • the polymeric material may further be positioned adjacent the outer periphery or the inner periphery cylindrical separator prior to forming the separator into a cylinder.
  • the polymeric material can be applied to the interface of two overlapping ends (that would not otherwise bond with each other) of a cylindrical separator. The polymeric seal would thus bond the two ends together under a controlled heating condition, and form a seal.
  • a suitably shaped polymeric layer can also be laminated or coated onto either side of a separator to be installed into a button cell, such that the polymeric material seals the outer periphery of the separator during a controlled heating condition.
  • seamless separator tubes using a variety of polymer processing methods such as extrusion, injection molding, or blow moulding/blown films can be employed.
  • seamless tubes can be prepared by, e.g., completely coating a seamed material such as a fibrous material with a suitable separator forming polymer such as regenerated cellulose such that the seam is not present in the separator, but rather in the underlying material.
  • a suitable separator forming polymer such as regenerated cellulose
  • Cylindrical cells typically include an annular grommet disposed proximal the negative cell terminal end that is compressed either axially or radially against the cathode and separator to prevent anode spillover.
  • the negative end of the separator can abut and be sealed against the grommet by dispensing a polymer to the periphery of the separator at the negative end, and sealing the polymer against the grommet under controlled heating conditions.
  • a chemical bond including cross-linking may also be used to create a seal.
  • At least a portion of an end of the fully side-sealed cylinder should be sealed.
  • an impulse heat-sealing apparatus (Fuji FS-315)
  • at least a portion of an end of the cylinder is sealed in a line substantially perpendicular to that of the side seal ( FIG. 18 ).
  • the sealed end can then be folded and formed into a cylindrical shape via multiple methods such that the internal bag volume is maximized and the tube is given the shape of the bottom of the can into which it is subsequently inserted ( FIG. 19 ).
  • Any other suitable end sealing method including ultrasonics, adhesive sealing or the like may be employed as described so long as anode-fouling soluble species are effectively limited from migrating to the anode.
  • a gas pressure of 2-3 psig is supplied to the tube, and sufficient time is allowed for the bag to fill with gas and reach an ultimate pressure of 2-3 psig.
  • a glass tube was provided having a first end (Side A) and a second end (Side B) divided by two L-shaped O-ring seal joints with an o-ring size of ⁇ 112 (Ace Glass, located in Vineland, N.J.).
  • the separator or sealed seam of the separator sample was placed in the center of the tube, between the O-ring seal joints.
  • Side A of the glass tube was filled with 10 mL of 34 wt. % KOH containing a mixture of 0.25 g CuO and 0.25 g of CuS. This ensured that there was a constant supply of soluble copper and sulfur species in the bulk solution substantially close to the equilibrium concentration under those conditions for the duration of the experiment.
  • Side B was filled with 10 mL of 34 wt.
  • a 357 size button cell is provided including the separator to be tested.
  • the cathode includes 92% active material, 5% graphite, 2.5% electrolyte, and 0.5% polyethylene binder.
  • the anode includes 68% sieved zinc with 31.25% 34-2 electrolyte and 0.75% of a combination of gelling agents and corrosion inhibitors.
  • the cell was stored in an oven at a temperature of 60 C.
  • Cell open circuit voltage (OCV), impedance, and cell expansion was monitored.
  • Cell impedance was measured using a frequency response analyzer (e.g. Model 12 from Schlumberger Inc.). Reduction in OCV implies the potential of one or both electrodes is deteriorating from its thermodynamic value, and indicates that anode-fouling soluble species are migrating through the separator.
  • Soluble Cu species were analyzed in KOH using standard inductively coupled plasma (ICP) analytical techniques utilizing a Thermo Iris Intrepid II (radial unit) supplied by Thermo Electron Corporation (Waltham, Mass.).
  • ICP inductively coupled plasma
  • samples were prepared using 1 g of electrolyte sample diluted to 50 ml with 10% nitric acid solution prior to analysis.
  • Calibration curves consisted of three solutions: blank, 0.5 ppm, and 1 ppm where all solutions were 10% nitric acid.
  • Copper is calibrated using a 1000 ppm Spex standard. Measurements for copper were made using the average of four wavelengths (223.0, 224.7, 324.7, 327.3).
  • a Scandium internal standard was used in each sample and standard ( 20 ppm) measured.
  • Soluble sulfur species were analyzed in KOH using standard inductively coupled plasma (ICP) analytical techniques utilizing a Thermo Iris Intrepid II (radial unit) supplied by Thermo Electron Corporation (Waltham, Mass.).
  • ICP inductively coupled plasma
  • samples were prepared using 1 g of electrolyte sample diluted to 50 ml with 10% nitric acid solution. Normally an additional 5:50 or 10:50 dilution was made, which was measured by volume to provide suitable results in this technique.
  • Calibration curves consisted of three solutions: blank, 0.5 ppm, and 1 ppm where all solutions were 10% nitric acid.
  • Sulfur was calibrated using standards prepared from Spex SO 4 (K 2 SO 4 starting source) standard. Measurements for sulfur were made using the average of two wavelengths (180.7, 182.0). A Scandium internal standard was used in each sample and standard (20 ppm) measured.
  • plasticizers or processing aids used in manufacture of films such as polyvinyl alcohol can adversely affect the ability of the film to effectively limit the migration of anode-fouling soluble species when used as a separator in a cell, and, as such, films prepared with substantial quantities of one or more plasticizers are disfavored. It is desirable that a film separator for use in accordance with the invention contain less than about 15% plasticizers by weight, alternatively, contain less than about 10% or less than about 5% plasticizers by weight. Particularly suitable film separators contain about 3% plasticizers by weight or less.
  • One possible separator is non cold-water soluble, non-crosslinked polyvinyl alcohol film separator comprising less than about 3% plasticizers by weight.
  • Two such suitable polyvinyl alcohol films are M-1000 and M-2000 (Monosol).
  • separator of the invention can be provided as described, the separator can optionally be coupled with (e.g., laminated or tacked to) a conventional non-woven fabric layer in an otherwise conventional manner.
  • the OCV was compared for a plurality of 357 cells made with various separators both initially and after 1 day room temperature of storage.
  • the cathode was CuO (commercially available from Aldrich), and the cell anode was a conventional alkaline Zn gel anode having conventional zinc and electrolyte concentrations.
  • the cellophane and the TiO 2 filled HMWPE (high molecular weight polyethylene) membranes outperform the microporous-type membranes (e.g. Celgard 3407 PE, B10ab Nylon and Excellerator Alkaline PTFE, etc), indicating that they are more effective in limiting migration of anode-fouling copper species.
  • HMWPE high molecular weight polyethylene
  • FIG. 20 This is an example that illustrates the utility of effectively limiting the migration of anode-fouling soluble species in stored 357 size button cells.
  • FIG. 20 shows that cellophane separators are better than FAS 350Z separator for cells containing CuO cathodes. Also, thicker cellophane separators (SF-586, 3 mil thick) outperform the thinner separator (350P00, and SC216 both are 1 mil thick) confirming results from the Exclusion Test experiments.
  • FIG. 21 shows that the cell built with 2 layers of Viskase Cellophane separator (SC-216) discharges to full capacity if it is discharged immediately, but has a very short capacity if it is discharged after 17 hrs rest.
  • a separator material may demonstrate an adequate Exclusion Value
  • the seal in a battery such as a button cell may affect its ability to effectively limit the migration of anode-fouling soluble species.
  • Example 4 thus shows that a combination of cellophane and hybrid separator is more effective in limiting the migration of soluble copper and sulfur species than 2 layers of SC 216 cellophane.
  • FIG. 22 shows, similar to FIG. 21 , that for mixtures of CuO and CuS, a combination of cellophane separator and hybrid separator (cross linked PVA coating on F3T23) is more effective than 2 layers of cellophane alone.
  • FIG. 23 shows that with a cathode comprising a CuO/CuS mixture, 2 layers of hybrid separator are effective in limiting migration of anode-fouling soluble copper and sulfur species even after 5 days, thereby allowing the cell to discharge to full capacity. Furthermore, adding 0.2 wt % PVA to the cathode is shown to extend cell discharge capacity by enabling better utilization of the cathode capacity.
  • FIG. 24 a pair of size 357 button cells were provided.
  • the cathodes were made with a 1-to-1 molar ratio of CuO and CuS mixture.
  • the first cell had a separator comprising a pair of hybrid layers (cross linked PVA coated onto F3T23).
  • the other cell had one layer of EVA emulsion coated onto F3R23 (commercially available from Kuraray).
  • the first cell was discharged at 5 mA after 5 days.
  • the second cell was discharged at 5 mA after 4 days.
  • the anode consisted of a 68% sieved BIP anode and the separator was a single ply of M 2000 PVA film. Both cells were discharged after a 7 day period of ambient storage. Both cells were exposed to an intermittent test regime involving a 12.5 mA current for 1 hour followed by open circuit rest, repeated 4 times per day.
  • the results shown in the Table 5 below demonstrate that the cell with 2% ZnO delivered 240 mA/g discharge capacity as compared to only 100 mAh/gm for the control cell with no ZnO. The results demonstrate the beneficial aspects of added ZnO on battery shelf life. TABLE 5 Cell Discharge Capacity to Cathode 0.7 V, mAh/g 95% 1:1 M CuO/CuS + 5% KS4 100 95% 1:1 M CuO/CuS, 3% KS4, 240 2% ZnO

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US11/055,508 US7740984B2 (en) 2004-06-04 2005-02-08 Alkaline cells having high capacity
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JP2007515050A JP2008502107A (ja) 2004-06-04 2005-02-08 高容量アルカリ電池
EP05713430A EP1779450B1 (en) 2004-06-04 2005-02-08 Alkaline cells having high capacity
PCT/US2005/004488 WO2005122301A2 (en) 2004-06-04 2005-02-08 Alkaline cells having high capacity
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WO2005015665A2 (en) 2005-02-17
US7763384B2 (en) 2010-07-27
US7931981B2 (en) 2011-04-26
AR045347A1 (es) 2005-10-26
JP2007502006A (ja) 2007-02-01
TW200520292A (en) 2005-06-16
US20050079415A1 (en) 2005-04-14
AU2004264243A1 (en) 2005-02-17
EP1661196A2 (en) 2006-05-31
JP2007502007A (ja) 2007-02-01
AU2004264238A1 (en) 2005-02-17
US7645540B2 (en) 2010-01-12
EP1665418A2 (en) 2006-06-07
WO2005015664A3 (en) 2006-06-01
WO2005015664A2 (en) 2005-02-17
JP2007502008A (ja) 2007-02-01
EP1665419B1 (en) 2011-11-16
US20050074674A1 (en) 2005-04-07
WO2005015665A3 (en) 2006-06-29
US20100112431A1 (en) 2010-05-06
EP1661196B1 (en) 2010-10-13
WO2005015662A2 (en) 2005-02-17
EP1665419A2 (en) 2006-06-07
AU2004264244A1 (en) 2005-02-17
DE602004029587D1 (de) 2010-11-25

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