JP2023500220A - 正極活物質、これを含む正極およびリチウム二次電池 - Google Patents
正極活物質、これを含む正極およびリチウム二次電池 Download PDFInfo
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- JP2023500220A JP2023500220A JP2022524004A JP2022524004A JP2023500220A JP 2023500220 A JP2023500220 A JP 2023500220A JP 2022524004 A JP2022524004 A JP 2022524004A JP 2022524004 A JP2022524004 A JP 2022524004A JP 2023500220 A JP2023500220 A JP 2023500220A
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- Prior art keywords
- active material
- positive electrode
- electrode active
- formula
- lithium
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- 239000007774 positive electrode material Substances 0.000 title claims abstract description 87
- 229910052744 lithium Inorganic materials 0.000 title claims abstract description 50
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims abstract description 49
- 229910021437 lithium-transition metal oxide Inorganic materials 0.000 claims abstract description 33
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 31
- 229910052723 transition metal Inorganic materials 0.000 claims abstract description 21
- 150000003624 transition metals Chemical class 0.000 claims abstract description 21
- 239000011164 primary particle Substances 0.000 claims abstract description 17
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 13
- 239000011163 secondary particle Substances 0.000 claims abstract description 11
- 239000013078 crystal Substances 0.000 claims description 51
- 238000002441 X-ray diffraction Methods 0.000 claims description 23
- 229910052782 aluminium Inorganic materials 0.000 claims description 16
- 239000006182 cathode active material Substances 0.000 claims description 15
- 238000000034 method Methods 0.000 claims description 12
- 239000000126 substance Substances 0.000 claims description 12
- 229910052748 manganese Inorganic materials 0.000 claims description 9
- 239000011247 coating layer Substances 0.000 claims description 8
- 229910052796 boron Inorganic materials 0.000 claims description 4
- 229910052721 tungsten Inorganic materials 0.000 claims description 4
- 229910052726 zirconium Inorganic materials 0.000 claims description 4
- 229910052804 chromium Inorganic materials 0.000 claims description 3
- 229910052750 molybdenum Inorganic materials 0.000 claims description 3
- 229910052758 niobium Inorganic materials 0.000 claims description 3
- 229910052715 tantalum Inorganic materials 0.000 claims description 3
- 229910052720 vanadium Inorganic materials 0.000 claims description 3
- 229910052727 yttrium Inorganic materials 0.000 claims description 3
- 239000002245 particle Substances 0.000 description 25
- -1 LiMnO2 or LiMn2O4) Chemical class 0.000 description 24
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 21
- 239000003792 electrolyte Substances 0.000 description 17
- 239000000203 mixture Substances 0.000 description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 16
- 239000007773 negative electrode material Substances 0.000 description 15
- 239000002243 precursor Substances 0.000 description 15
- 239000004020 conductor Substances 0.000 description 14
- 239000011572 manganese Substances 0.000 description 14
- 239000010410 layer Substances 0.000 description 13
- 238000004519 manufacturing process Methods 0.000 description 13
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- 239000011230 binding agent Substances 0.000 description 11
- 239000002904 solvent Substances 0.000 description 9
- 239000007864 aqueous solution Substances 0.000 description 8
- JBTWLSYIZRCDFO-UHFFFAOYSA-N ethyl methyl carbonate Chemical compound CCOC(=O)OC JBTWLSYIZRCDFO-UHFFFAOYSA-N 0.000 description 8
- 238000002360 preparation method Methods 0.000 description 8
- 229910052799 carbon Inorganic materials 0.000 description 7
- 238000006243 chemical reaction Methods 0.000 description 7
- 238000010304 firing Methods 0.000 description 7
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 6
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 description 6
- 239000002033 PVDF binder Substances 0.000 description 6
- 239000002131 composite material Substances 0.000 description 6
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- 229910044991 metal oxide Inorganic materials 0.000 description 6
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- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 5
- 239000011149 active material Substances 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 5
- 229910001416 lithium ion Inorganic materials 0.000 description 5
- 229910003002 lithium salt Inorganic materials 0.000 description 5
- 159000000002 lithium salts Chemical class 0.000 description 5
- 150000004706 metal oxides Chemical class 0.000 description 5
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 4
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 description 4
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 4
- 239000005977 Ethylene Substances 0.000 description 4
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 4
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 4
- 229910021383 artificial graphite Inorganic materials 0.000 description 4
- 239000003575 carbonaceous material Substances 0.000 description 4
- 238000000975 co-precipitation Methods 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 4
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- 238000005259 measurement Methods 0.000 description 4
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- 239000004745 nonwoven fabric Substances 0.000 description 4
- 239000003960 organic solvent Substances 0.000 description 4
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- 239000000843 powder Substances 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- 229920000049 Carbon (fiber) Polymers 0.000 description 3
- OIFBSDVPJOWBCH-UHFFFAOYSA-N Diethyl carbonate Chemical compound CCOC(=O)OCC OIFBSDVPJOWBCH-UHFFFAOYSA-N 0.000 description 3
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- 229910012851 LiCoO 2 Inorganic materials 0.000 description 3
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 3
- 239000004698 Polyethylene Substances 0.000 description 3
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 3
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 3
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- 239000004917 carbon fiber Substances 0.000 description 3
- 238000005266 casting Methods 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 239000010949 copper Substances 0.000 description 3
- 229910052802 copper Inorganic materials 0.000 description 3
- IEJIGPNLZYLLBP-UHFFFAOYSA-N dimethyl carbonate Chemical compound COC(=O)OC IEJIGPNLZYLLBP-UHFFFAOYSA-N 0.000 description 3
- 239000008151 electrolyte solution Substances 0.000 description 3
- 229910002804 graphite Inorganic materials 0.000 description 3
- 239000010439 graphite Substances 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 3
- 230000000704 physical effect Effects 0.000 description 3
- 229920000573 polyethylene Polymers 0.000 description 3
- 229920000642 polymer Polymers 0.000 description 3
- RUOJZAUFBMNUDX-UHFFFAOYSA-N propylene carbonate Chemical compound CC1COC(=O)O1 RUOJZAUFBMNUDX-UHFFFAOYSA-N 0.000 description 3
- 230000002441 reversible effect Effects 0.000 description 3
- 238000005096 rolling process Methods 0.000 description 3
- 229910052709 silver Inorganic materials 0.000 description 3
- 239000004332 silver Substances 0.000 description 3
- 238000005245 sintering Methods 0.000 description 3
- 239000002002 slurry Substances 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 229910052719 titanium Inorganic materials 0.000 description 3
- 239000010936 titanium Substances 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- DURPTKYDGMDSBL-UHFFFAOYSA-N 1-butoxybutane Chemical compound CCCCOCCCC DURPTKYDGMDSBL-UHFFFAOYSA-N 0.000 description 2
- YEJRWHAVMIAJKC-UHFFFAOYSA-N 4-Butyrolactone Chemical compound O=C1CCCO1 YEJRWHAVMIAJKC-UHFFFAOYSA-N 0.000 description 2
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 2
- 229920002134 Carboxymethyl cellulose Polymers 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 229920002153 Hydroxypropyl cellulose Polymers 0.000 description 2
- 229910013290 LiNiO 2 Inorganic materials 0.000 description 2
- 229910013870 LiPF 6 Inorganic materials 0.000 description 2
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 2
- 229920000265 Polyparaphenylene Polymers 0.000 description 2
- 239000004743 Polypropylene Substances 0.000 description 2
- 239000004372 Polyvinyl alcohol Substances 0.000 description 2
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 2
- KAESVJOAVNADME-UHFFFAOYSA-N Pyrrole Chemical compound C=1C=CNC=1 KAESVJOAVNADME-UHFFFAOYSA-N 0.000 description 2
- 238000003991 Rietveld refinement Methods 0.000 description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 229920002472 Starch Polymers 0.000 description 2
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 239000006230 acetylene black Substances 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 239000003660 carbonate based solvent Substances 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 239000006231 channel black Substances 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 229910017052 cobalt Inorganic materials 0.000 description 2
- 239000010941 cobalt Substances 0.000 description 2
- GSOLWAFGMNOBSY-UHFFFAOYSA-N cobalt Chemical compound [Co][Co][Co][Co][Co][Co][Co][Co] GSOLWAFGMNOBSY-UHFFFAOYSA-N 0.000 description 2
- KTVIXTQDYHMGHF-UHFFFAOYSA-L cobalt(2+) sulfate Chemical compound [Co+2].[O-]S([O-])(=O)=O KTVIXTQDYHMGHF-UHFFFAOYSA-L 0.000 description 2
- 150000005676 cyclic carbonates Chemical class 0.000 description 2
- JHIVVAPYMSGYDF-UHFFFAOYSA-N cyclohexanone Chemical compound O=C1CCCCC1 JHIVVAPYMSGYDF-UHFFFAOYSA-N 0.000 description 2
- 238000006731 degradation reaction Methods 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 229910001873 dinitrogen Inorganic materials 0.000 description 2
- NJLLQSBAHIKGKF-UHFFFAOYSA-N dipotassium dioxido(oxo)titanium Chemical compound [K+].[K+].[O-][Ti]([O-])=O NJLLQSBAHIKGKF-UHFFFAOYSA-N 0.000 description 2
- 238000007599 discharging Methods 0.000 description 2
- 239000012153 distilled water Substances 0.000 description 2
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- 239000011267 electrode slurry Substances 0.000 description 2
- LYCAIKOWRPUZTN-UHFFFAOYSA-N ethylene glycol Natural products OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 2
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- KWGKDLIKAYFUFQ-UHFFFAOYSA-M lithium chloride Chemical compound [Li+].[Cl-] KWGKDLIKAYFUFQ-UHFFFAOYSA-M 0.000 description 2
- RSNHXDVSISOZOB-UHFFFAOYSA-N lithium nickel Chemical compound [Li].[Ni] RSNHXDVSISOZOB-UHFFFAOYSA-N 0.000 description 2
- SQQMAOCOWKFBNP-UHFFFAOYSA-L manganese(II) sulfate Chemical compound [Mn+2].[O-]S([O-])(=O)=O SQQMAOCOWKFBNP-UHFFFAOYSA-L 0.000 description 2
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- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 description 2
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 description 2
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- XNWFRZJHXBZDAG-UHFFFAOYSA-N 2-METHOXYETHANOL Chemical compound COCCO XNWFRZJHXBZDAG-UHFFFAOYSA-N 0.000 description 1
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- 229910000838 Al alloy Inorganic materials 0.000 description 1
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 1
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- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 description 1
- 229910010238 LiAlCl 4 Inorganic materials 0.000 description 1
- 229910010090 LiAlO 4 Inorganic materials 0.000 description 1
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- 229910013372 LiC 4 Inorganic materials 0.000 description 1
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- 229910003005 LiNiO2 Inorganic materials 0.000 description 1
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- 229910002097 Lithium manganese(III,IV) oxide Inorganic materials 0.000 description 1
- ZHGDJTMNXSOQDT-UHFFFAOYSA-N NP(N)(N)=O.NP(N)(N)=O.NP(N)(N)=O.NP(N)(N)=O.NP(N)(N)=O.NP(N)(N)=O Chemical compound NP(N)(N)=O.NP(N)(N)=O.NP(N)(N)=O.NP(N)(N)=O.NP(N)(N)=O.NP(N)(N)=O ZHGDJTMNXSOQDT-UHFFFAOYSA-N 0.000 description 1
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- GELKBWJHTRAYNV-UHFFFAOYSA-K lithium iron phosphate Chemical class [Li+].[Fe+2].[O-]P([O-])([O-])=O GELKBWJHTRAYNV-UHFFFAOYSA-K 0.000 description 1
- 229910000686 lithium vanadium oxide 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
- BFZPBUKRYWOWDV-UHFFFAOYSA-N lithium;oxido(oxo)cobalt Chemical compound [Li+].[O-][Co]=O BFZPBUKRYWOWDV-UHFFFAOYSA-N 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 239000002931 mesocarbon microbead Substances 0.000 description 1
- 239000011302 mesophase pitch Substances 0.000 description 1
- 150000002736 metal compounds Chemical class 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- PYLWMHQQBFSUBP-UHFFFAOYSA-N monofluorobenzene Chemical compound FC1=CC=CC=C1 PYLWMHQQBFSUBP-UHFFFAOYSA-N 0.000 description 1
- 150000005181 nitrobenzenes Chemical class 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 239000011301 petroleum pitch Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011295 pitch Substances 0.000 description 1
- 229920002239 polyacrylonitrile Polymers 0.000 description 1
- 229920000139 polyethylene terephthalate Polymers 0.000 description 1
- 239000005020 polyethylene terephthalate Substances 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 229920000098 polyolefin Polymers 0.000 description 1
- 229920001384 propylene homopolymer Polymers 0.000 description 1
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 1
- 239000002296 pyrolytic carbon Substances 0.000 description 1
- 239000001008 quinone-imine dye Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000002153 silicon-carbon composite material Substances 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 229910021384 soft carbon Inorganic materials 0.000 description 1
- 239000010959 steel Substances 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
- 239000011593 sulfur Substances 0.000 description 1
- TXEYQDLBPFQVAA-UHFFFAOYSA-N tetrafluoromethane Chemical compound FC(F)(F)F TXEYQDLBPFQVAA-UHFFFAOYSA-N 0.000 description 1
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- 239000002733 tin-carbon composite material Substances 0.000 description 1
- BDZBKCUKTQZUTL-UHFFFAOYSA-N triethyl phosphite Chemical compound CCOP(OCC)OCC BDZBKCUKTQZUTL-UHFFFAOYSA-N 0.000 description 1
- 229910001935 vanadium oxide Inorganic materials 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- PAPBSGBWRJIAAV-UHFFFAOYSA-N ε-Caprolactone Chemical compound O=C1CCCCCO1 PAPBSGBWRJIAAV-UHFFFAOYSA-N 0.000 description 1
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Abstract
Description
式(1) -0.021x+4.0≦y≦-0.021x+5.5
前記式(1)中、xは、前記正極活物質の結晶粒のサイズ(nm単位)であり、前記yは、前記正極活物質の結晶粒のアスペクト比である。
[化学式1]
Li1+xNiyCozM1 wM2 eO2
前記化学式1中、M1は、Mn、Alまたはこれらの組み合わせであり、M2は、B、Al、Zr、Y、Mo、Cr、V、W、TaおよびNbからなる群から選択される少なくともいずれか一つであり、-0.1≦x≦0.2、0.6≦y<1.0、0<z<0.4、0<w<0.4、0≦e≦0.1である。好ましくは、前記化学式1中、M1がMnまたはMnおよびAlの組み合わせであり、0.85≦y<1.0、0<z<0.15、0<w<0.15、0≦e≦0.05であることができる。
本発明による正極活物質は、リチウム以外の遷移金属の全モル数に対して60モル%以上のニッケルを含み、一次粒子が凝集した二次粒子の形態であるリチウム遷移金属酸化物を含み、下記式(1)の条件を満たすことを特徴とする。
光源:Cu-ターゲット、45kV、40mA出力
検出器:GaliPIX3D
試料準備:約5g程度の試料を直径2cmのホルダーに満たし、回転ステージ(rotation stage)にローディング
測定時間:約30分
測定領域:2θ=15゜~85゜
Li1+xNiyCozM1 wM2 eO2
また、本発明は、上述の正極活物質を含むリチウム二次電池用正極を提供する。
また、本発明は、前記正極を含む電気化学素子を製造することができる。前記電気化学素子は、具体的には、電池、キャパシタなどであることができ、より具体的には、リチウム二次電池であることができる。
NiSO4、CoSO4、およびMnSO4をニッケル:コバルト:マンガンのモル比が88:6:6になるようにする量で蒸留水の中で混合し、2.4M濃度の遷移金属水溶液を準備した。
NiSO4、CoSO4、およびMnSO4をニッケル:コバルト:マンガンのモル比が88:6:6になるようにする量で蒸留水の中で混合し、2.4M濃度の遷移金属水溶液を準備した。
共沈反応を12時間行った以外は、前記製造例2と同じ方法で、平均粒径5μmのNi0.88Co0.06Mn0.06(OH)2で表される正極活物質前駆体Cを製造した。
製造例1で製造された正極活物質前駆体AとLiOHをLi/Meのモル比が1.03になるように混合し、760℃で10時間焼成してリチウム遷移金属酸化物を製造した。
Li/Meのモル比が1.05になるように混合する以外は、前記実施例1と同じ方法で正極活物質を製造した。
770℃で10時間焼成してリチウム遷移金属酸化物を製造し、これを用いる以外は、前記実施例1と同じ方法で正極活物質を製造した。
780℃で10時間焼成してリチウム遷移金属酸化物を製造し、これを用いる以外は、前記実施例1と同じ方法で正極活物質を製造した。
製造例2で製造された正極活物質前駆体BとLiOHをLi/Meのモル比が1.01になるように混合し、750℃で15時間焼成してリチウム遷移金属酸化物を製造した。
製造例3で製造された正極活物質前駆体CとLiOHをLi/Meのモル比が1.09になるように混合し、780℃で15時間焼成してリチウム遷移金属酸化物を製造した。
前記実施例1~4および比較例1~2で製造した正極活物質粉末に対するX線回折分析(Empyrean、Malvern panalytical社)を行って結晶粒のサイズ、結晶粒のアスペクト比および変形率を測定した。この際、X線回折分析条件および結晶粒のサイズ、変形率および結晶粒のアスペクト比の測定方法は、上述のとおりである。測定結果は、下記表1に示す。
前記実施例1~4および比較例1~2でそれぞれ製造した正極活物質、カーボンブラック導電材およびポリビニリデンフルオライドバインダーを97.5:1.0:1.5の重量比でN‐メチルピロリドン溶媒の中で混合し、正極スラリーを製造した。前記正極スラリーをアルミニウム集電体の一面に塗布した後、130℃で乾燥してから圧延して正極を製造した。一方、負極活物質としてカーボンブラックおよびポリビニリデンフルオライドバインダーを97.5:2.5の重量比で混合し、溶媒であるN‐メチルピロリドンに添加して負極活物質スラリーを製造した。これを厚さが16.5μmの銅箔上に塗布し、乾燥した後、ロールプレス(roll press)を実施して負極を製造した。
Claims (12)
- リチウム以外の遷移金属の全モル数に対して60モル%以上のニッケルを含み、一次粒子が凝集した二次粒子の形態であるリチウム遷移金属酸化物を含み、
下記式(1)の条件を満たす正極活物質であって、
式(1) -0.021x+4.0≦y≦-0.021x+5.5
前記式(1)中、xは、前記正極活物質の結晶粒のサイズ(nm単位)であり、前記yは、前記正極活物質の結晶粒のアスペクト比である、正極活物質。 - 前記式(1)において、100≦x≦180である、請求項1に記載の正極活物質。
- 前記式(1)において、120≦x≦160である、請求項1に記載の正極活物質。
- 前記式(1)において、1≦y≦2.5である、請求項1に記載の正極活物質。
- 前記式(1)において、1.3≦y≦2.5である、請求項1に記載の正極活物質。
- 前記結晶粒のサイズxは、前記正極活物質をX線回折分析して得られたXRDデータに示されるすべてのピークの半値全幅(FWHM)をCagliotiの式でフィッティングして測定された値である、請求項1に記載の正極活物質。
- 前記リチウム遷移金属酸化物は、下記化学式1で表され、
[化学式1]
Li1+xNiyCozM1 wM2 eO2
前記化学式1中、M1は、Mn、Alまたはこれらの組み合わせであり、M2は、B、Al、Zr、Y、Mo、Cr、V、W、TaおよびNbからなる群から選択される少なくともいずれか一つであり、-0.1≦x≦0.2、0.6≦y<1.0、0<z<0.4、0<w<0.4、0≦e≦0.1である、請求項1に記載の正極活物質。 - 前記化学式1中、M1がMn、またはMnおよびAlの組み合わせであり、
0.85≦y<1.0、0<z<0.15、0<w<0.15、0≦e≦0.05である、請求項8に記載の正極活物質。 - 前記リチウム遷移金属酸化物の表面にコーティング層をさらに含む請求項1に記載の正極活物質。
- 請求項1に記載の正極活物質を含むリチウム二次電池用正極。
- 請求項11に記載のリチウム二次電池用正極を含むリチウム二次電池。
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