JP6296682B2 - 正極活物質およびリチウム2次電池 - Google Patents
正極活物質およびリチウム2次電池 Download PDFInfo
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- JP6296682B2 JP6296682B2 JP2013014428A JP2013014428A JP6296682B2 JP 6296682 B2 JP6296682 B2 JP 6296682B2 JP 2013014428 A JP2013014428 A JP 2013014428A JP 2013014428 A JP2013014428 A JP 2013014428A JP 6296682 B2 JP6296682 B2 JP 6296682B2
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- positive electrode
- electrode active
- active material
- lithium
- life
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- 239000007774 positive electrode material Substances 0.000 title claims description 87
- 229910052744 lithium Inorganic materials 0.000 title claims description 42
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims description 37
- -1 di Rukoniumu (Zr) Substances 0.000 claims description 21
- 239000000126 substance Substances 0.000 claims description 20
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 19
- 150000001875 compounds Chemical class 0.000 claims description 10
- 229910017052 cobalt Inorganic materials 0.000 claims description 9
- 239000010941 cobalt Substances 0.000 claims description 9
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 9
- 239000003792 electrolyte Substances 0.000 claims description 9
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical group [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 claims description 9
- 239000011572 manganese Substances 0.000 claims description 8
- 239000011164 primary particle Substances 0.000 claims description 8
- 229910052759 nickel Inorganic materials 0.000 claims description 7
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 claims description 4
- 229910052748 manganese Inorganic materials 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 description 51
- VZSRBBMJRBPUNF-UHFFFAOYSA-N 2-(2,3-dihydro-1H-inden-2-ylamino)-N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]pyrimidine-5-carboxamide Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)C(=O)NCCC(N1CC2=C(CC1)NN=N2)=O VZSRBBMJRBPUNF-UHFFFAOYSA-N 0.000 description 33
- 229910052751 metal Inorganic materials 0.000 description 25
- 239000002184 metal Substances 0.000 description 25
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 20
- 239000007773 negative electrode material Substances 0.000 description 12
- 239000002904 solvent Substances 0.000 description 12
- 238000002156 mixing Methods 0.000 description 11
- 239000002994 raw material Substances 0.000 description 11
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 10
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 10
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 10
- 229910001416 lithium ion Inorganic materials 0.000 description 10
- 239000000203 mixture Substances 0.000 description 10
- 239000011230 binding agent Substances 0.000 description 9
- 239000004020 conductor Substances 0.000 description 9
- 239000011777 magnesium Substances 0.000 description 8
- 239000000463 material Substances 0.000 description 6
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- YJLUBHOZZTYQIP-UHFFFAOYSA-N 2-[5-[2-(2,3-dihydro-1H-inden-2-ylamino)pyrimidin-5-yl]-1,3,4-oxadiazol-2-yl]-1-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethanone Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)C1=NN=C(O1)CC(=O)N1CC2=C(CC1)NN=N2 YJLUBHOZZTYQIP-UHFFFAOYSA-N 0.000 description 5
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- 239000003960 organic solvent Substances 0.000 description 5
- 235000011007 phosphoric acid Nutrition 0.000 description 5
- 229910052698 phosphorus Inorganic materials 0.000 description 5
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- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 4
- 229910010707 LiFePO 4 Inorganic materials 0.000 description 4
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- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 4
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 4
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- 159000000002 lithium salts Chemical class 0.000 description 4
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- LDXJRKWFNNFDSA-UHFFFAOYSA-N 2-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)-1-[4-[2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidin-5-yl]piperazin-1-yl]ethanone Chemical compound C1CN(CC2=NNN=C21)CC(=O)N3CCN(CC3)C4=CN=C(N=C4)NCC5=CC(=CC=C5)OC(F)(F)F LDXJRKWFNNFDSA-UHFFFAOYSA-N 0.000 description 3
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- CONKBQPVFMXDOV-QHCPKHFHSA-N 6-[(5S)-5-[[4-[2-(2,3-dihydro-1H-inden-2-ylamino)pyrimidin-5-yl]piperazin-1-yl]methyl]-2-oxo-1,3-oxazolidin-3-yl]-3H-1,3-benzoxazol-2-one Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)N1CCN(CC1)C[C@H]1CN(C(O1)=O)C1=CC2=C(NC(O2)=O)C=C1 CONKBQPVFMXDOV-QHCPKHFHSA-N 0.000 description 3
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- 229910013684 LiClO 4 Inorganic materials 0.000 description 1
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- 229910013417 LiN(SO3C2F5)2 Inorganic materials 0.000 description 1
- 229910013553 LiNO Inorganic materials 0.000 description 1
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- UEZVMMHDMIWARA-UHFFFAOYSA-N Metaphosphoric acid Chemical compound OP(=O)=O UEZVMMHDMIWARA-UHFFFAOYSA-N 0.000 description 1
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 description 1
- RJUFJBKOKNCXHH-UHFFFAOYSA-N Methyl propionate Chemical compound CCC(=O)OC RJUFJBKOKNCXHH-UHFFFAOYSA-N 0.000 description 1
- HSHXDCVZWHOWCS-UHFFFAOYSA-N N'-hexadecylthiophene-2-carbohydrazide Chemical compound CCCCCCCCCCCCCCCCNNC(=O)c1cccs1 HSHXDCVZWHOWCS-UHFFFAOYSA-N 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- 239000004677 Nylon Substances 0.000 description 1
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 1
- 239000004962 Polyamide-imide Substances 0.000 description 1
- 239000004642 Polyimide Substances 0.000 description 1
- XBDQKXXYIPTUBI-UHFFFAOYSA-M Propionate Chemical compound CCC([O-])=O XBDQKXXYIPTUBI-UHFFFAOYSA-M 0.000 description 1
- JYVXNLLUYHCIIH-ZCFIWIBFSA-N R-mevalonolactone, (-)- Chemical compound C[C@@]1(O)CCOC(=O)C1 JYVXNLLUYHCIIH-ZCFIWIBFSA-N 0.000 description 1
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- 150000001336 alkenes Chemical class 0.000 description 1
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- LFVGISIMTYGQHF-UHFFFAOYSA-N ammonium dihydrogen phosphate Chemical compound [NH4+].OP(O)([O-])=O LFVGISIMTYGQHF-UHFFFAOYSA-N 0.000 description 1
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- 229910052787 antimony Inorganic materials 0.000 description 1
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- 125000003118 aryl group Chemical group 0.000 description 1
- YCOXTKKNXUZSKD-UHFFFAOYSA-N as-o-xylenol Natural products CC1=CC=C(O)C=C1C YCOXTKKNXUZSKD-UHFFFAOYSA-N 0.000 description 1
- KCXMKQUNVWSEMD-UHFFFAOYSA-N benzyl chloride Chemical compound ClCC1=CC=CC=C1 KCXMKQUNVWSEMD-UHFFFAOYSA-N 0.000 description 1
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- 229910052796 boron Inorganic materials 0.000 description 1
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- 239000011329 calcined coke Substances 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
- 150000004649 carbonic acid derivatives Chemical class 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
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- 150000001805 chlorine compounds Chemical class 0.000 description 1
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- 229920001577 copolymer Polymers 0.000 description 1
- 239000011889 copper foil Substances 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 229920005994 diacetyl cellulose Polymers 0.000 description 1
- MNNHAPBLZZVQHP-UHFFFAOYSA-N diammonium hydrogen phosphate Chemical compound [NH4+].[NH4+].OP([O-])([O-])=O MNNHAPBLZZVQHP-UHFFFAOYSA-N 0.000 description 1
- 229910000388 diammonium phosphate Inorganic materials 0.000 description 1
- 235000019838 diammonium phosphate Nutrition 0.000 description 1
- SBZXBUIDTXKZTM-UHFFFAOYSA-N diglyme Chemical compound COCCOCCOC SBZXBUIDTXKZTM-UHFFFAOYSA-N 0.000 description 1
- 150000004862 dioxolanes Chemical class 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000003487 electrochemical reaction Methods 0.000 description 1
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- 238000004880 explosion Methods 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 150000002222 fluorine compounds Chemical class 0.000 description 1
- 229910052730 francium Inorganic materials 0.000 description 1
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- 230000008570 general process Effects 0.000 description 1
- 229910052732 germanium Inorganic materials 0.000 description 1
- 239000003365 glass fiber Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 229910052735 hafnium Inorganic materials 0.000 description 1
- 125000001188 haloalkyl group Chemical group 0.000 description 1
- 229910021385 hard carbon Inorganic materials 0.000 description 1
- 229910021473 hassium Inorganic materials 0.000 description 1
- 239000001863 hydroxypropyl cellulose Substances 0.000 description 1
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- 239000001866 hydroxypropyl methyl cellulose Substances 0.000 description 1
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- 235000010979 hydroxypropyl methyl cellulose Nutrition 0.000 description 1
- SNHMUERNLJLMHN-UHFFFAOYSA-N iodobenzene Chemical compound IC1=CC=CC=C1 SNHMUERNLJLMHN-UHFFFAOYSA-N 0.000 description 1
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- 229910052742 iron Inorganic materials 0.000 description 1
- KQNPFQTWMSNSAP-UHFFFAOYSA-N isobutyric acid Chemical compound CC(C)C(O)=O KQNPFQTWMSNSAP-UHFFFAOYSA-N 0.000 description 1
- 239000005453 ketone based solvent Substances 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- XIXADJRWDQXREU-UHFFFAOYSA-M lithium acetate Chemical compound [Li+].CC([O-])=O XIXADJRWDQXREU-UHFFFAOYSA-M 0.000 description 1
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 description 1
- 229910000625 lithium cobalt oxide Inorganic materials 0.000 description 1
- 229910002102 lithium manganese oxide Inorganic materials 0.000 description 1
- RSNHXDVSISOZOB-UHFFFAOYSA-N lithium nickel Chemical compound [Li].[Ni] RSNHXDVSISOZOB-UHFFFAOYSA-N 0.000 description 1
- 229910001386 lithium phosphate Inorganic materials 0.000 description 1
- SNKMVYBWZDHJHE-UHFFFAOYSA-M lithium;dihydrogen phosphate Chemical compound [Li+].OP(O)([O-])=O SNKMVYBWZDHJHE-UHFFFAOYSA-M 0.000 description 1
- BFZPBUKRYWOWDV-UHFFFAOYSA-N lithium;oxido(oxo)cobalt Chemical compound [Li+].[O-][Co]=O BFZPBUKRYWOWDV-UHFFFAOYSA-N 0.000 description 1
- VLXXBCXTUVRROQ-UHFFFAOYSA-N lithium;oxido-oxo-(oxomanganiooxy)manganese Chemical compound [Li+].[O-][Mn](=O)O[Mn]=O VLXXBCXTUVRROQ-UHFFFAOYSA-N 0.000 description 1
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- 239000006051 mesophase pitch carbide Substances 0.000 description 1
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- 229910052758 niobium Inorganic materials 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 150000002825 nitriles Chemical class 0.000 description 1
- 239000011255 nonaqueous electrolyte Substances 0.000 description 1
- 229920001778 nylon Polymers 0.000 description 1
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 description 1
- 229910052762 osmium Inorganic materials 0.000 description 1
- GHZRKQCHJFHJPX-UHFFFAOYSA-N oxacycloundecan-2-one Chemical compound O=C1CCCCCCCCCO1 GHZRKQCHJFHJPX-UHFFFAOYSA-N 0.000 description 1
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- 229910052763 palladium Inorganic materials 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
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- 229920002312 polyamide-imide Polymers 0.000 description 1
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- 229920000307 polymer substrate Polymers 0.000 description 1
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- 238000011160 research Methods 0.000 description 1
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- NNMHYFLPFNGQFZ-UHFFFAOYSA-M sodium polyacrylate Chemical compound [Na+].[O-]C(=O)C=C NNMHYFLPFNGQFZ-UHFFFAOYSA-M 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- HXJUTPCZVOIRIF-UHFFFAOYSA-N sulfolane Chemical class O=S1(=O)CCCC1 HXJUTPCZVOIRIF-UHFFFAOYSA-N 0.000 description 1
- 229910052713 technetium Inorganic materials 0.000 description 1
- 229910052714 tellurium Inorganic materials 0.000 description 1
- ZUHZGEOKBKGPSW-UHFFFAOYSA-N tetraglyme Chemical compound COCCOCCOCCOCCOC ZUHZGEOKBKGPSW-UHFFFAOYSA-N 0.000 description 1
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 1
- 229910052716 thallium Inorganic materials 0.000 description 1
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- 239000010409 thin film Substances 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 229910000314 transition metal oxide Inorganic materials 0.000 description 1
- DDXPLCBTGWFAIG-UHFFFAOYSA-N triazanium;phosphate;trihydrate Chemical compound [NH4+].[NH4+].[NH4+].O.O.O.[O-]P([O-])([O-])=O DDXPLCBTGWFAIG-UHFFFAOYSA-N 0.000 description 1
- TWQULNDIKKJZPH-UHFFFAOYSA-K trilithium;phosphate Chemical compound [Li+].[Li+].[Li+].[O-]P([O-])([O-])=O TWQULNDIKKJZPH-UHFFFAOYSA-K 0.000 description 1
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- 229910052726 zirconium Inorganic materials 0.000 description 1
- PAPBSGBWRJIAAV-UHFFFAOYSA-N ε-Caprolactone Chemical compound O=C1CCCCCO1 PAPBSGBWRJIAAV-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/45—Phosphates containing plural metal, or metal and ammonium
-
- 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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/136—Electrodes based on inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy
-
- 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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
- H01M4/1397—Processes of manufacture of electrodes based on inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy
-
- 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
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
-
- 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
-
- 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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
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Description
[化学式1]
LiFe1−x−zMxM’zPyO4
前記化学式1において、
Mは、バナジウム(V)であり、
M’は、コバルト(Co)、マンガン(Mn)、マグネシウム(Mg)、ジルコニウム(Zr)、ニッケル(Ni)またはこれらの組み合わせであり、
0<x<0.20、0≦z<0.20および0.90≦y<1.20を満たす。
〔製造例1−1〕
Li2CO3、FeC2O4・2H2O、NH4VO3および(NH4)2HPO4を水で混合してボールミル工程を行った。この時、FeC2O4・2H2O、NH4VO3および(NH4)2HPO4の混合比率は、原料物質に含まれているFe:V:PO4のモル比が0.99:0.01:1.00になるように混合した。
Fe:V:PO4のモル比が0.99:0.01:1.03になるように混合したことを除いては、製造例1−1と同様な方法でLiFe0.99V0.01P1.03O4で表される正極活物質を得た。
Fe:V:PO4のモル比が0.97:0.03:1.00になるように混合したことを除いては、製造例1−1と同様な方法でLiFe0.97V0.03PO4で表される正極活物質を得た。
Fe:V:PO4のモル比が0.95:0.05:1.00になるように混合したことを除いては、製造例1−1と同様な方法でLiFe0.95V0.05PO4で表される正極活物質を得た。
Fe:V:PO4のモル比が0.95:0.05:1.03になるように混合したことを除いては、製造例1−1と同様な方法でLiFe0.95V0.05P1.03O4で表される正極活物質を得た。
Fe:V:PO4のモル比が0.95:0.05:1.06になるように混合したことを除いては、製造例1−1と同様な方法でLiFe0.95V0.05P1.06O4で表される正極活物質を得た。
Fe:V:PO4のモル比が0.93:0.07:1.00になるように混合したことを除いては、製造例1−1と同様な方法でLiFe0.93V0.07PO4で表される正極活物質を得た。
Fe:V:PO4のモル比が0.91:0.09:1.00になるように混合したことを除いては、製造例1−1と同様な方法でLiFe0.91V0.09PO4で表される正極活物質を得た。
Fe:V:PO4のモル比が0.91:0.09:1.03になるように混合したことを除いては、製造例1−1と同様な方法でLiFe0.91V0.09P1.03O4で表される正極活物質を得た。
Fe:V:PO4のモル比が0.91:0.09:1.06になるように混合したことを除いては、製造例1−1と同様な方法でLiFe0.91V0.09P1.06O4で表される正極活物質を得た。
Li2CO3、FeC2O4・2H2O、NH4VO3、Co(NO3)2および(NH4)2HPO4を水で混合してボールミル工程を行った。この時、FeC2O4・2H2O、NH4VO3、Co(NO3)2および(NH4)2HPO4の混合比率は、原料物質に含まれているFe:V:Co:PO4のモル比が0.94:0.05:0.01:1.00になるように混合した。
Fe:V:Co:PO4のモル比が0.925:0.05:0.025:1.00になるように混合したことを除いては、製造例6−1と同様な方法でLiFe0.925V0.05Co0.025PO4で表される正極活物質を得た。
Fe:V:Co:PO4のモル比が0.90:0.05:0.050:1.00になるように混合したことを除いては、製造例6−1と同様な方法でLiFe0.90V0.05Co0.050PO4で表される正極活物質を得た。
NH4VO3およびCo(NO3)2を含まずに、FeC2O4・2H2O2および(NH4)2HPO4に含まれているFe:PO4のモル比が1:1になるように混合したことを除いては、実施例1−1と同様な方法にてLiFePO4で表される正極活物質を得た。
〔実施例1−1〕
製造例1−1による正極活物質90質量%、カーボンブラック5質量%およびポリフッ化ビニリデン5質量%をN−メチルピロリドン溶媒で混合して正極活物質スラリーを製造した。正極活物質スラリーをアルミニウム箔の上に塗布して薄い極板形態とした後、120℃で1時間乾燥し、圧延(pressing)して正極を製造した。
製造例1−1による正極活物質の代わりに製造例1−2による正極活物質を使用したことを除いては、実施例1−1と同様な方法でコインタイプの半電池を製作した。
製造例1−1による正極活物質の代わりに製造例2−1による正極活物質を使用したことを除いては、実施例1−1と同様な方法でコインタイプの半電池を製作した。
製造例1−1による正極活物質の代わりに製造例3−1による正極活物質を使用したことを除いては、実施例1−1と同様な方法でコインタイプの半電池を製作した。
製造例1−1による正極活物質の代わりに製造例3−2による正極活物質を使用したことを除いては、実施例1−1と同様な方法でコインタイプの半電池を製作した。
製造例1−1による正極活物質の代わりに製造例3−3による正極活物質を使用したことを除いては、実施例1−1と同様な方法でコインタイプの半電池を製作した。
製造例1−1による正極活物質の代わりに製造例4−1による正極活物質を使用したことを除いては、実施例1−1と同様な方法でコインタイプの半電池を製作した。
製造例1−1による正極活物質の代わりに製造例5−1による正極活物質を使用したことを除いては、実施例1−1と同様な方法でコインタイプの半電池を製作した。
製造例1−1による正極活物質の代わりに製造例5−2による正極活物質を使用したことを除いては、実施例1−1と同様な方法でコインタイプの半電池を製作した。
製造例1−1による正極活物質の代わりに製造例5−3による正極活物質を使用したことを除いては、実施例1−1と同様な方法でコインタイプの半電池を製作した。
製造例1−1による正極活物質の代わりに製造例6−1による正極活物質を使用したことを除いては、実施例1−1と同様な方法でコインタイプの半電池を製作した。
製造例1−1による正極活物質の代わりに製造例6−2による正極活物質を使用したことを除いては、実施例1−1と同様な方法でコインタイプの半電池を製作した。
製造例1−1による正極活物質の代わりに製造例6−3による正極活物質を使用したことを除いては、実施例1−1と同様な方法でコインタイプの半電池を製作した。
製造例1−1による正極活物質の代わりに比較製造例による正極活物質を使用したことを除いては、実施例1−1と同様な方法でコインタイプの半電池を製作した。
実施例1−1〜6−3および比較例による半電池の充放電特性を評価した。
実施例1−1〜6−3による半電池の寿命特性を評価した。
112 負極
113 セパレータ
114 正極
120 電池容器
140 封入部材
Claims (10)
- 下記化学式1で表されるリチウム含有化合物を含む、正極活物質:
LiFe1−x−zMxM’zPyO4 …化学式1
前記化学式1において、
Mは、バナジウム(V)であり、
M’は、コバルト(Co)、マンガン(Mn)、ジルコニウム(Zr)、ニッケル(Ni)またはこれらの組み合わせであり、
0<x<0.20、0<z<0.20および0.90≦y<1.20を満たす。 - 前記xとyの比率は、0.009≦x/y≦0.09を満たす、請求項1に記載の正極活物質。
- 前記xとyの比率は、0.03≦x/y≦0.07を満たす、請求項1又は2に記載の正極活物質。
- 前記xとyの比率は、x/y=0.05を満たす、請求項1〜3のいずれか一項に記載の正極活物質。
- 前記xとzの比率は、0.5≦x/z≦5を満たす、請求項1〜4のいずれか一項に記載の正極活物質。
- 前記xとzの比率は、x/z=2を満たす、請求項1〜5のいずれか一項に記載の正極活物質。
- 前記M’は、コバルト(Co)である、請求項1〜6のいずれか一項に記載の正極活物質。
- 前記正極活物質の1次粒子は、50〜1000nmの大きさを有する、請求項1〜7のいずれか一項に記載の正極活物質。
- 前記正極活物質の1次粒子は、50〜200nmの大きさを有する、請求項1〜8のいずれか一項に記載の正極活物質。
- 請求項1〜9項のいずれか一項に記載の正極活物質を含む正極、
負極、および
電解液
を含む、リチウム2次電池。
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