JP6877405B2 - 電極及びその製造方法、並びに二次電池 - Google Patents
電極及びその製造方法、並びに二次電池 Download PDFInfo
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- JP6877405B2 JP6877405B2 JP2018509094A JP2018509094A JP6877405B2 JP 6877405 B2 JP6877405 B2 JP 6877405B2 JP 2018509094 A JP2018509094 A JP 2018509094A JP 2018509094 A JP2018509094 A JP 2018509094A JP 6877405 B2 JP6877405 B2 JP 6877405B2
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- WLLOZRDOFANZMZ-UHFFFAOYSA-N bis(2,2,2-trifluoroethyl) carbonate Chemical compound FC(F)(F)COC(=O)OCC(F)(F)F WLLOZRDOFANZMZ-UHFFFAOYSA-N 0.000 description 1
- IQFAIEKYIVKGST-UHFFFAOYSA-N bis(fluoromethyl) carbonate Chemical compound FCOC(=O)OCF IQFAIEKYIVKGST-UHFFFAOYSA-N 0.000 description 1
- 229910052797 bismuth Inorganic materials 0.000 description 1
- YHASWHZGWUONAO-UHFFFAOYSA-N butanoyl butanoate Chemical compound CCCC(=O)OC(=O)CCC YHASWHZGWUONAO-UHFFFAOYSA-N 0.000 description 1
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- FNBZKEIQRUDONN-UHFFFAOYSA-N butyl ethyl 2,2,2-trifluoroethyl phosphate Chemical compound CCCCOP(=O)(OCC)OCC(F)(F)F FNBZKEIQRUDONN-UHFFFAOYSA-N 0.000 description 1
- HDJQAZXGZIWCQW-UHFFFAOYSA-N butyl propyl 2,2,2-trifluoroethyl phosphate Chemical compound CCCCOP(=O)(OCCC)OCC(F)(F)F HDJQAZXGZIWCQW-UHFFFAOYSA-N 0.000 description 1
- HXJNXHRCVBYKFI-UHFFFAOYSA-N butylsulfonyl butane-1-sulfonate Chemical compound CCCCS(=O)(=O)OS(=O)(=O)CCCC HXJNXHRCVBYKFI-UHFFFAOYSA-N 0.000 description 1
- 229910052793 cadmium Inorganic materials 0.000 description 1
- 150000001721 carbon Chemical group 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 150000004651 carbonic acid esters Chemical class 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 208000037998 chronic venous disease Diseases 0.000 description 1
- 239000011280 coal tar Substances 0.000 description 1
- 238000000748 compression moulding Methods 0.000 description 1
- 239000011889 copper foil Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 150000004292 cyclic ethers Chemical class 0.000 description 1
- 230000003111 delayed effect Effects 0.000 description 1
- 210000001787 dendrite Anatomy 0.000 description 1
- WJXUXCSXDUAXKT-UHFFFAOYSA-N dibutyl 2,2,2-trifluoroethyl phosphate Chemical compound CCCCOP(=O)(OCC(F)(F)F)OCCCC WJXUXCSXDUAXKT-UHFFFAOYSA-N 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- QHGJSLXSVXVKHZ-UHFFFAOYSA-N dilithium;dioxido(dioxo)manganese Chemical compound [Li+].[Li+].[O-][Mn]([O-])(=O)=O QHGJSLXSVXVKHZ-UHFFFAOYSA-N 0.000 description 1
- ODIPJXGRLMMPDM-UHFFFAOYSA-N dimethyl 2,2,2-trifluoroethyl phosphate Chemical compound COP(=O)(OC)OCC(F)(F)F ODIPJXGRLMMPDM-UHFFFAOYSA-N 0.000 description 1
- XVYIUIITVLUBGJ-UHFFFAOYSA-N dimethyl 2,2,3,3,3-pentafluoropropyl phosphate Chemical compound P(=O)(OCC(C(F)(F)F)(F)F)(OC)OC XVYIUIITVLUBGJ-UHFFFAOYSA-N 0.000 description 1
- 150000004862 dioxolanes Chemical class 0.000 description 1
- GGHDQFBKLBKWIY-UHFFFAOYSA-N dipropyl 2,2,2-trifluoroethyl phosphate Chemical compound CCCOP(=O)(OCCC)OCC(F)(F)F GGHDQFBKLBKWIY-UHFFFAOYSA-N 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000007606 doctor blade method Methods 0.000 description 1
- 239000011267 electrode slurry Substances 0.000 description 1
- REKZEFBSHHXSOM-UHFFFAOYSA-N ethenylsulfonyl ethenesulfonate Chemical compound C=CS(=O)(=O)OS(=O)(=O)C=C REKZEFBSHHXSOM-UHFFFAOYSA-N 0.000 description 1
- 125000005677 ethinylene group Chemical group [*:2]C#C[*:1] 0.000 description 1
- NIQAXIMIQJNOKY-UHFFFAOYSA-N ethyl 2,2,2-trifluoroethyl carbonate Chemical compound CCOC(=O)OCC(F)(F)F NIQAXIMIQJNOKY-UHFFFAOYSA-N 0.000 description 1
- DBOFMRQAMAZKQY-UHFFFAOYSA-N ethyl 2,2,3,3,3-pentafluoropropanoate Chemical compound CCOC(=O)C(F)(F)C(F)(F)F DBOFMRQAMAZKQY-UHFFFAOYSA-N 0.000 description 1
- JVHJRIQPDBCRRE-UHFFFAOYSA-N ethyl 2,2,3,3,4,4,4-heptafluorobutanoate Chemical compound CCOC(=O)C(F)(F)C(F)(F)C(F)(F)F JVHJRIQPDBCRRE-UHFFFAOYSA-N 0.000 description 1
- GZKHDVAKKLTJPO-UHFFFAOYSA-N ethyl 2,2-difluoroacetate Chemical compound CCOC(=O)C(F)F GZKHDVAKKLTJPO-UHFFFAOYSA-N 0.000 description 1
- ONLLXDPBECIJCM-UHFFFAOYSA-N ethyl 2-fluorobutanoate Chemical compound CCOC(=O)C(F)CC ONLLXDPBECIJCM-UHFFFAOYSA-N 0.000 description 1
- FMDMKDPUFQNVSH-UHFFFAOYSA-N ethyl 3,3,3-trifluoropropanoate Chemical compound CCOC(=O)CC(F)(F)F FMDMKDPUFQNVSH-UHFFFAOYSA-N 0.000 description 1
- ZJXZSIYSNXKHEA-UHFFFAOYSA-N ethyl dihydrogen phosphate Chemical compound CCOP(O)(O)=O ZJXZSIYSNXKHEA-UHFFFAOYSA-N 0.000 description 1
- AWIZDAABIHLIDY-UHFFFAOYSA-N ethyl methyl 2,2,2-trifluoroethyl phosphate Chemical compound CCOP(=O)(OC)OCC(F)(F)F AWIZDAABIHLIDY-UHFFFAOYSA-N 0.000 description 1
- CCJXQRNXZKSOGJ-UHFFFAOYSA-N ethylsulfonyl ethanesulfonate Chemical compound CCS(=O)(=O)OS(=O)(=O)CC CCJXQRNXZKSOGJ-UHFFFAOYSA-N 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 125000000457 gamma-lactone group Chemical group 0.000 description 1
- VANNPISTIUFMLH-UHFFFAOYSA-N glutaric anhydride Chemical compound O=C1CCCC(=O)O1 VANNPISTIUFMLH-UHFFFAOYSA-N 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 125000004474 heteroalkylene group Chemical group 0.000 description 1
- 125000005842 heteroatom Chemical group 0.000 description 1
- PJCGDVXUAOWKCY-UHFFFAOYSA-N hexylsulfonyl hexane-1-sulfonate Chemical compound CCCCCCS(=O)(=O)OS(=O)(=O)CCCCCC PJCGDVXUAOWKCY-UHFFFAOYSA-N 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 238000010191 image analysis Methods 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- 229910003437 indium oxide Inorganic materials 0.000 description 1
- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-UHFFFAOYSA-N 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- PNDPGZBMCMUPRI-UHFFFAOYSA-N iodine Chemical compound II PNDPGZBMCMUPRI-UHFFFAOYSA-N 0.000 description 1
- 125000000959 isobutyl group Chemical group [H]C([H])([H])C([H])(C([H])([H])[H])C([H])([H])* 0.000 description 1
- 229910052745 lead Inorganic materials 0.000 description 1
- 239000010985 leather Substances 0.000 description 1
- 239000001989 lithium alloy Substances 0.000 description 1
- 229910001547 lithium hexafluoroantimonate(V) Inorganic materials 0.000 description 1
- 229910001540 lithium hexafluoroarsenate(V) Inorganic materials 0.000 description 1
- 229910002102 lithium manganese oxide Inorganic materials 0.000 description 1
- FUJCRWPEOMXPAD-UHFFFAOYSA-N lithium oxide Chemical compound [Li+].[Li+].[O-2] FUJCRWPEOMXPAD-UHFFFAOYSA-N 0.000 description 1
- 229910001947 lithium oxide Inorganic materials 0.000 description 1
- MHCFAGZWMAWTNR-UHFFFAOYSA-M lithium perchlorate Chemical compound [Li+].[O-]Cl(=O)(=O)=O MHCFAGZWMAWTNR-UHFFFAOYSA-M 0.000 description 1
- 229910001486 lithium perchlorate Inorganic materials 0.000 description 1
- 159000000002 lithium salts Chemical class 0.000 description 1
- 229910001537 lithium tetrachloroaluminate Inorganic materials 0.000 description 1
- 229910001496 lithium tetrafluoroborate Inorganic materials 0.000 description 1
- ACFSQHQYDZIPRL-UHFFFAOYSA-N lithium;bis(1,1,2,2,2-pentafluoroethylsulfonyl)azanide Chemical compound [Li+].FC(F)(F)C(F)(F)S(=O)(=O)[N-]S(=O)(=O)C(F)(F)C(F)(F)F ACFSQHQYDZIPRL-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
- 230000007774 longterm Effects 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 238000003701 mechanical milling Methods 0.000 description 1
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- UANOJLOYSTZABR-UHFFFAOYSA-N methanesulfonic acid;propanoic acid Chemical compound CCC(O)=O.CS(O)(=O)=O UANOJLOYSTZABR-UHFFFAOYSA-N 0.000 description 1
- IZDROVVXIHRYMH-UHFFFAOYSA-N methanesulfonic anhydride Chemical compound CS(=O)(=O)OS(C)(=O)=O IZDROVVXIHRYMH-UHFFFAOYSA-N 0.000 description 1
- UZKWTJUDCOPSNM-UHFFFAOYSA-N methoxybenzene Substances CCCCOC=C UZKWTJUDCOPSNM-UHFFFAOYSA-N 0.000 description 1
- GBPVMEKUJUKTBA-UHFFFAOYSA-N methyl 2,2,2-trifluoroethyl carbonate Chemical compound COC(=O)OCC(F)(F)F GBPVMEKUJUKTBA-UHFFFAOYSA-N 0.000 description 1
- JMKJCPUVEMZGEC-UHFFFAOYSA-N methyl 2,2,3,3,3-pentafluoropropanoate Chemical compound COC(=O)C(F)(F)C(F)(F)F JMKJCPUVEMZGEC-UHFFFAOYSA-N 0.000 description 1
- MRPUVAKBXDBGJQ-UHFFFAOYSA-N methyl 2,2,3,3,4,4,4-heptafluorobutanoate Chemical compound COC(=O)C(F)(F)C(F)(F)C(F)(F)F MRPUVAKBXDBGJQ-UHFFFAOYSA-N 0.000 description 1
- CGMUKBZUGMXXEF-UHFFFAOYSA-N methyl 2,3,3,3-tetrafluoro-2-(trifluoromethyl)propanoate Chemical compound COC(=O)C(F)(C(F)(F)F)C(F)(F)F CGMUKBZUGMXXEF-UHFFFAOYSA-N 0.000 description 1
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- YPGCUXBNTDXTKF-UHFFFAOYSA-N methyl 2,3,3,3-tetrafluoropropanoate Chemical compound COC(=O)C(F)C(F)(F)F YPGCUXBNTDXTKF-UHFFFAOYSA-N 0.000 description 1
- PMGBATZKLCISOD-UHFFFAOYSA-N methyl 3,3,3-trifluoropropanoate Chemical compound COC(=O)CC(F)(F)F PMGBATZKLCISOD-UHFFFAOYSA-N 0.000 description 1
- RVNWLMWNUJPCQD-UHFFFAOYSA-N methyl 4,4,4-trifluorobutanoate Chemical compound COC(=O)CCC(F)(F)F RVNWLMWNUJPCQD-UHFFFAOYSA-N 0.000 description 1
- QPXDTULTYTZDQM-UHFFFAOYSA-N methyl bis(2,2,2-trifluoroethyl) phosphate Chemical compound FC(F)(F)COP(=O)(OC)OCC(F)(F)F QPXDTULTYTZDQM-UHFFFAOYSA-N 0.000 description 1
- CXHHBNMLPJOKQD-UHFFFAOYSA-M methyl carbonate Chemical compound COC([O-])=O CXHHBNMLPJOKQD-UHFFFAOYSA-M 0.000 description 1
- XZIOCKSAUMRABB-UHFFFAOYSA-N methyl propyl 2,2,2-trifluoroethyl phosphate Chemical compound CCCOP(=O)(OC)OCC(F)(F)F XZIOCKSAUMRABB-UHFFFAOYSA-N 0.000 description 1
- 230000000116 mitigating effect Effects 0.000 description 1
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- JFNLZVQOOSMTJK-KNVOCYPGSA-N norbornene Chemical compound C1[C@@H]2CC[C@H]1C=C2 JFNLZVQOOSMTJK-KNVOCYPGSA-N 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
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- LVVFKXHBKKOJTB-UHFFFAOYSA-N oxathiepane 2,2-dioxide Chemical compound O=S1(=O)CCCCCO1 LVVFKXHBKKOJTB-UHFFFAOYSA-N 0.000 description 1
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- 239000011236 particulate material Substances 0.000 description 1
- KXPYQQGRMTVAMD-UHFFFAOYSA-N pentylsulfonyl pentane-1-sulfonate Chemical compound CCCCCS(=O)(=O)OS(=O)(=O)CCCCC KXPYQQGRMTVAMD-UHFFFAOYSA-N 0.000 description 1
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- 239000000047 product Substances 0.000 description 1
- ASAXRKSDVDALDT-UHFFFAOYSA-N propan-2-yl 2,2,2-trifluoroacetate Chemical compound CC(C)OC(=O)C(F)(F)F ASAXRKSDVDALDT-UHFFFAOYSA-N 0.000 description 1
- FVSKHRXBFJPNKK-UHFFFAOYSA-N propionitrile Chemical compound CCC#N FVSKHRXBFJPNKK-UHFFFAOYSA-N 0.000 description 1
- OTRCLINFKXQIBG-UHFFFAOYSA-N propylsulfonyl propane-1-sulfonate Chemical compound CCCS(=O)(=O)OS(=O)(=O)CCC OTRCLINFKXQIBG-UHFFFAOYSA-N 0.000 description 1
- NGKFCGXPCNZTKS-UHFFFAOYSA-N propylsulfonyl propanoate Chemical compound CCCS(=O)(=O)OC(=O)CC NGKFCGXPCNZTKS-UHFFFAOYSA-N 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Chemical compound [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 230000005469 synchrotron radiation Effects 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000011269 tar Substances 0.000 description 1
- UQJLSMYQBOJUGG-UHFFFAOYSA-N tert-butyl 2,2,2-trifluoroacetate Chemical compound CC(C)(C)OC(=O)C(F)(F)F UQJLSMYQBOJUGG-UHFFFAOYSA-N 0.000 description 1
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- BUGOPWGPQGYYGR-UHFFFAOYSA-N thiane 1,1-dioxide Chemical compound O=S1(=O)CCCCC1 BUGOPWGPQGYYGR-UHFFFAOYSA-N 0.000 description 1
- 230000008719 thickening Effects 0.000 description 1
- CFRVORMUGQWQNZ-UHFFFAOYSA-N thiepane 1,1-dioxide Chemical compound O=S1(=O)CCCCCC1 CFRVORMUGQWQNZ-UHFFFAOYSA-N 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 1
- 229910001887 tin oxide Inorganic materials 0.000 description 1
- QHGNHLZPVBIIPX-UHFFFAOYSA-N tin(II) oxide Inorganic materials [Sn]=O QHGNHLZPVBIIPX-UHFFFAOYSA-N 0.000 description 1
- VJDDQSBNUHLBTD-UHFFFAOYSA-N trans-crotonic acid-anhydride Natural products CC=CC(=O)OC(=O)C=CC VJDDQSBNUHLBTD-UHFFFAOYSA-N 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
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- BHZCMUVGYXEBMY-UHFFFAOYSA-N trilithium;azanide Chemical compound [Li+].[Li+].[Li+].[NH2-] BHZCMUVGYXEBMY-UHFFFAOYSA-N 0.000 description 1
- 229930195735 unsaturated hydrocarbon Natural products 0.000 description 1
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- JLQFVGYYVXALAG-CFEVTAHFSA-N yasmin 28 Chemical compound OC1=CC=C2[C@H]3CC[C@](C)([C@](CC4)(O)C#C)[C@@H]4[C@@H]3CCC2=C1.C([C@]12[C@H]3C[C@H]3[C@H]3[C@H]4[C@@H]([C@]5(CCC(=O)C=C5[C@@H]5C[C@@H]54)C)CC[C@@]31C)CC(=O)O2 JLQFVGYYVXALAG-CFEVTAHFSA-N 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
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Images
Classifications
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- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/64—Carriers or collectors
- H01M4/66—Selection of materials
- H01M4/661—Metal or alloys, e.g. alloy coatings
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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/04—Processes of manufacture in general
- H01M4/0402—Methods of deposition of the material
- H01M4/0404—Methods of deposition of the material by coating on electrode collectors
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- H—ELECTRICITY
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- 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
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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
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/056—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
- H01M10/0564—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of organic materials only
- H01M10/0566—Liquid materials
- H01M10/0569—Liquid materials characterised by the solvents
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- H01M4/04—Processes of manufacture in general
- H01M4/0402—Methods of deposition of the material
- H01M4/0409—Methods of deposition of the material by a doctor blade method, slip-casting or roller coating
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- H01—ELECTRIC ELEMENTS
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- 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
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- H—ELECTRICITY
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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- 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
- H01M4/133—Electrodes based on carbonaceous material, e.g. graphite-intercalation compounds or CFx
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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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
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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
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Description
集電体と、該集電体上の活物質含有膜を含み、
前記活物質含有膜の体積あたりの空隙率が25%以下であり、
前記電極断面の膜厚方向の面積あたりの空隙率のトレンド解析による最大空隙率と最小空隙率の比が2.2以上となる高空隙率領域が、半径500μmの電極平面の範囲内に、1箇所以上ある電極が提供される。
集電体上に、活物質粒子と結着剤と溶媒を含むスラリーを塗工する工程と、
塗工工程において厚みの異なる領域を形成し、
前記塗工工程の後に、全面に圧力をかけて密度を上げる工程を有する電極の製造方法が提供される。
集電体上に、活物質粒子と結着剤と溶媒を含むスラリーを塗工する工程と、
前記塗工工程の後に、凹凸のあるローラーで電極に圧力をかける工程を有する電極の製造方法が提供される。
集電体上に、活物質粒子と結着剤と溶媒を含むスラリーを塗工する工程と、
前記塗工後の乾燥により塗工膜の表面にひび割れを起こさせる工程と、
ひび割れ形成後に、全面に圧力をかける工程とを含む電極の製造方法が提供される。
前記第1及び第2の電極の少なくとも一方に、上記の電極を用いた二次電池が提供される。
使用した固形分材料の体積と、集電体上に形成した活物質含有膜のプレス後の厚さから求めた体積との差を求め、この差を空隙の体積とし、この空隙の体積をプレス後の活物質含有膜の体積で割った値を体積空隙率とすることができる。
また、作製後の電極について、FIB(集束イオンビーム加工装置)で断面を形成して空隙形状を撮影、断面形成位置をずらして空隙形状の撮影を繰り返し、得られた断面像群から電極内の3D状態を再構成することで体積空隙率を得ることができる。
本実施形態によるリチウム二次電池の正極は、正極活物質として、リチウムイオンを吸蔵及び放出し得る材料を含むものであれば特に限定されない。たとえば、LiMn2O4あるいはLiCoO2などの4V級(平均動作電位=3.6〜3.8V:対リチウム電位)の材料を用いることができる。これらの正極活物質では、CoイオンもしくはMnイオンの酸化還元反応(Co3+←→Co4+もしくはMn3+←→Mn4+)によって発現電位が規定される。また、LiM1O2(M1はMn、Fe、CoおよびNiからなる群から選択される少なくとも1種の元素であり、M1の一部がMg、AlまたはTiで置換されていてもよい)、LiMn2−xM2xO4(M2はMg、Al、Co、Ni、FeおよびBからなる群から選択される少なくとも一種の元素であり、0≦x<0.4である。)などのリチウム含有複合酸化物、LiFePO4で表されるオリビン型材料なども用いることができる。
(式中、0.3≦x≦1.2、0≦y、x+y<2、0≦a≦1.2、0≦w≦1である。Mは、Co、Ni、Fe、Cr及びCuからなる群より選ばれる少なくとも一種である。Yは、Li、B、Na、Al、Mg、Ti、Si、K及びCaからなる群より選ばれる少なくとも一種である。Zは、F及びClからなる群より選ばれる少なくとも一種である。)
(式中、0.5≦x≦1.2、0≦y、x+y<2、0≦a≦1.2、0≦w≦1である。Mは、Co、Ni、Fe、Cr及びCuからなる群より選ばれる少なくとも一種である。Yは、Li、B、Na、Al、Mg、Ti、Si、K及びCaからなる群より選ばれる少なくとも一種である。Zは、F及びClからなる群より選ばれる少なくとも一種である。)
例えば、上述の4V級の活物質のみを含むものであってもよい。また、高エネルギー密度を得る観点では、上述のように、リチウムに対して4.5V以上の電位で動作する活物質を用いることがより好ましい。さらに4V級の活物質を含んでもよい。
負極は、負極活物質として、リチウムを吸蔵及び放出し得る材料を含むものであれば特に限定されない。
測定モード:マクロラマン
測定配置:60°
ビーム径:100μm
光源:Ar+レーザー/514.5nm
レザーパワー:10mW
回折格子:Single600gr/mm
分散:Single21A/mm
スリット:100μm
検出器:CCD/Jobin Yvon1024256
二次電池は、その構成として正極、負極、分離層、及びイオン伝導体との組み合わせからなることができる。分離層として通常のセパレータを用いることができ、例えば、織布、不織布、ポリエチレンやポリプロピレンなどのポリオレフィン系、ポリイミド、多孔性ポリフッ化ビニリデン膜等の多孔性ポリマー膜、又はイオン伝導性ポリマー電解質膜等が挙げられる。これらは単独または組み合わせで使用することができる。
イオン伝導体は、支持塩及び非水電解溶媒を含む電解液、もしくは固体電解質である。
(式(5)中、nは1,2又は3であり、mは1,2又は3であり、lは0から2n+1までのいずれかの整数であり、kは0から2m+1までのいずれかの整数であり、l及びkのうち少なくともいずれかは1以上の整数である。)
(式(2)において、A及びBはそれぞれ独立に置換又は無置換のアルキル基であって、A及びBの少なくとも1つはフッ素含有アルキル基である。)
(式(6)中、nは1,2,3又は4であり、mは1,2,3又は4であり、lは0から2n+1までのいずれかの整数であり、kは0から2m+1までのいずれかの整数であり、l及びkのうち少なくともいずれかは1以上の整数である。)
anhydride)、3H−パーフルオロプロピオン酸無水物(3H−Perfluoropropanoic anhydride)、3,3,3−トリフルオロプロピオン酸無水物(3,3,3−Trifluoropropionic anhydride)、無水ペンタフルオロプロピオン酸、2,2,3,3,4,4−ヘキサフルオロペンタン二酸無水物、テトラフルオロこはく酸無水物、トリフルオロ酢酸無水物等が挙げられる。また、ハロゲン化物に加えて、4−メチルフタル酸無水物など他の置換基を有する酸無水物も使用できる。
電池の形状としては、例えば、円筒形、角形、コイン型、ボタン型、ラミネート型等が挙げられる。電池の外装体としては、例えば、ステンレス、鉄、アルミニウム、チタン、又はこれらの合金、あるいはこれらのメッキ加工品等が挙げられる。メッキとしては例えばニッケルメッキを用いることができる。
本実施例の負極活物質としては、低結晶性炭素材料で被覆された人造黒鉛を用いた。人造黒鉛と、球状の炭素材料である導電助剤と、SBR(styrene-butadiene rubber)系バインダーとを97.7/0.3/2の質量比で混合し、N−メチルピロリドンに分散させ、負極用スラリーを調製した。この負極用スラリーを厚さ10μmのCu集電体上に均一に塗布した。乾燥させた後、ロールプレスで圧縮成形することにより負極を作製した。
比較例1は、実施例1で用いたバインダーとは異なるSBR系バインダーを用いた以外は、実施例1と同様の方法で電極を作製した。図5に、Arイオンビームにより断面加工し、その断面をSEM観察した結果を示す。比較例1の平均浸み込み時間は37.0秒であり、実施例1より浸み込みにくい結果となった。
比較例2は、実施例1及び比較例1で用いたバインダーとは異なるSBR系バインダーを用いた以外は、実施例1と同様の方法で電極を作製した。図7に、Arイオンビームにより断面加工し、その断面をSEM観察した結果を示す。比較例1の平均浸み込み時間は40.8秒であり、実施例1より浸み込みにくい結果となった。
2 負極活物質層
3 正極集電体
4 負極集電体
5 セパレータ
6 ラミネート外装体
7 ラミネート外装体
8 負極タブ
9 正極タブ
Claims (10)
- 第1の電極と、第2の電極と、これらの電極を空間的に分離する分離層と、イオン伝導体を含む二次電池用の電極であって、
集電体と、該集電体上の活物質含有膜を含み、
前記活物質含有膜の体積あたりの空隙率が25%以下であり、
前記電極断面の膜厚方向の面積あたりの空隙率の電極平面方向の位置に対するトレンド分布を評価するトレンド解析による最大空隙率と最小空隙率の比が2.2以上となる高空隙率領域が、半径500μmの電極平面の範囲内に、1箇所以上あり、
前記電極断面について、前記電極平面方向の位置に対する、前記電極断面の膜厚方向の面積あたりの空隙率のトレンド分布を、前記電極平面方向35〜70μmの範囲で平滑化し、
前記平滑化の手法が3次式への最小二乗法近似である電極。 - 前記活物質含有膜が、リチウムイオンを吸蔵、放出し得る活物質を含む、請求項1に記載の電極。
- 前記活物質含有膜が結着剤を含む、請求項1又は2に記載の電極。
- 請求項1から3のいずれか一項に記載の電極を製造する方法であって、
集電体上に、活物質粒子と結着剤と溶媒を含むスラリーを塗工する工程と、
塗工工程において厚みの異なる領域を形成し、
前記塗工工程の後に、全面に圧力をかけて密度を上げる工程を有する電極の製造方法。 - 前記塗工時に、凹凸を有するブレードを用いて前記スラリーの塗工量を調整して、厚みの異なる領域を形成する請求項4に記載の製造方法。
- 前記塗工工程において、同種又は異なるスラリーを部分的に重ね塗りして、厚みの異なる領域を形成する請求項4に記載の製造方法。
- 請求項1から3のいずれか一項に記載の電極を製造する方法であって、
集電体上に、活物質粒子と結着剤と溶媒を含むスラリーを塗工する工程と、
前記塗工工程の後に、凹凸のあるローラーで電極に圧力をかける工程を有する電極の製造方法。 - 請求項1から3のいずれか一項に記載の電極を製造する方法であって、
集電体上に、活物質粒子と結着剤と溶媒を含むスラリーを塗工する工程と、
前記塗工後の乾燥により塗工膜の表面にひび割れを起こさせる工程と、
ひび割れ形成後に、全面に圧力をかける工程とを含む電極の製造方法。 - 第1の電極と、第2の電極と、これらの電極を空間的に分離する分離層と、イオン伝導体を含む二次電池であって、
前記第1及び第2の電極の少なくとも一方に、請求項1から3のいずれか一項に記載の電極を用いた二次電池。 - 前記第1及び第2の電極の一方がリチウムイオンを吸蔵、放出し得る活物質を含む正極であり、他方が黒鉛系活物質を含む負極である、請求項9記載の二次電池。
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