JP2016522147A - 球状粒子、その生成およびそれを使用する方法 - Google Patents
球状粒子、その生成およびそれを使用する方法 Download PDFInfo
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- JP2016522147A JP2016522147A JP2016512301A JP2016512301A JP2016522147A JP 2016522147 A JP2016522147 A JP 2016522147A JP 2016512301 A JP2016512301 A JP 2016512301A JP 2016512301 A JP2016512301 A JP 2016512301A JP 2016522147 A JP2016522147 A JP 2016522147A
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- transition metal
- particle
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- 239000012798 spherical particle Substances 0.000 title claims abstract description 30
- 238000004519 manufacturing process Methods 0.000 title claims description 27
- 238000000034 method Methods 0.000 title claims description 27
- 229910052723 transition metal Inorganic materials 0.000 claims abstract description 129
- 239000002245 particle Substances 0.000 claims abstract description 96
- 150000003624 transition metals Chemical class 0.000 claims abstract description 89
- -1 transition metal cations Chemical class 0.000 claims abstract description 81
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 73
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 31
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 20
- 229910017052 cobalt Inorganic materials 0.000 claims abstract description 19
- 239000010941 cobalt Substances 0.000 claims abstract description 19
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims abstract description 19
- 229910000299 transition metal carbonate Inorganic materials 0.000 claims abstract description 17
- 229910052742 iron Inorganic materials 0.000 claims abstract description 12
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 claims abstract description 12
- 229910052804 chromium Inorganic materials 0.000 claims abstract description 11
- 239000011651 chromium Substances 0.000 claims abstract description 11
- 229910052720 vanadium Inorganic materials 0.000 claims abstract description 11
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 9
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims abstract description 8
- JYYOBHFYCIDXHH-UHFFFAOYSA-N carbonic acid;hydrate Chemical compound O.OC(O)=O JYYOBHFYCIDXHH-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 8
- 239000010936 titanium Substances 0.000 claims abstract description 8
- 239000007864 aqueous solution Substances 0.000 claims description 55
- 239000000243 solution Substances 0.000 claims description 44
- 239000011572 manganese Substances 0.000 claims description 29
- 239000000203 mixture Substances 0.000 claims description 18
- 229910052744 lithium Inorganic materials 0.000 claims description 16
- 150000001768 cations Chemical class 0.000 claims description 15
- 150000008044 alkali metal hydroxides Chemical class 0.000 claims description 13
- 229910052748 manganese Inorganic materials 0.000 claims description 13
- 238000001556 precipitation Methods 0.000 claims description 12
- 229910000288 alkali metal carbonate Inorganic materials 0.000 claims description 11
- 150000008041 alkali metal carbonates Chemical class 0.000 claims description 11
- 238000006243 chemical reaction Methods 0.000 claims description 10
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 claims description 8
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 claims description 8
- 229910001416 lithium ion Inorganic materials 0.000 claims description 8
- GPPXJZIENCGNKB-UHFFFAOYSA-N vanadium Chemical compound [V]#[V] GPPXJZIENCGNKB-UHFFFAOYSA-N 0.000 claims description 7
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 claims description 6
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- 238000012885 constant function Methods 0.000 claims description 4
- 230000001376 precipitating effect Effects 0.000 claims description 3
- 229910018068 Li 2 O Inorganic materials 0.000 claims description 2
- 239000010419 fine particle Substances 0.000 claims description 2
- 125000004435 hydrogen atom Chemical class [H]* 0.000 claims description 2
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 abstract 1
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- 150000003839 salts Chemical class 0.000 description 20
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- 239000011230 binding agent Substances 0.000 description 12
- 239000003446 ligand Substances 0.000 description 11
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- 239000000463 material Substances 0.000 description 10
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 9
- 229910052799 carbon Inorganic materials 0.000 description 9
- 238000003756 stirring Methods 0.000 description 9
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- 230000008859 change Effects 0.000 description 8
- 229910021529 ammonia Inorganic materials 0.000 description 7
- 235000011121 sodium hydroxide Nutrition 0.000 description 7
- KAKZBPTYRLMSJV-UHFFFAOYSA-N Butadiene Chemical compound C=CC=C KAKZBPTYRLMSJV-UHFFFAOYSA-N 0.000 description 6
- 239000004743 Polypropylene Substances 0.000 description 6
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 6
- 239000011149 active material Substances 0.000 description 6
- 239000002041 carbon nanotube Substances 0.000 description 6
- 229910021393 carbon nanotube Inorganic materials 0.000 description 6
- 150000001868 cobalt Chemical class 0.000 description 6
- 239000011888 foil Substances 0.000 description 6
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- 238000001035 drying Methods 0.000 description 5
- 150000002431 hydrogen Chemical class 0.000 description 5
- 229910052739 hydrogen Inorganic materials 0.000 description 5
- 239000001257 hydrogen Substances 0.000 description 5
- 229910052751 metal Inorganic materials 0.000 description 5
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- CRSBERNSMYQZNG-UHFFFAOYSA-N 1-dodecene Chemical compound CCCCCCCCCCC=C CRSBERNSMYQZNG-UHFFFAOYSA-N 0.000 description 4
- KWKAKUADMBZCLK-UHFFFAOYSA-N 1-octene Chemical compound CCCCCCC=C KWKAKUADMBZCLK-UHFFFAOYSA-N 0.000 description 4
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 4
- XTHFKEDIFFGKHM-UHFFFAOYSA-N Dimethoxyethane Chemical compound COCCOC XTHFKEDIFFGKHM-UHFFFAOYSA-N 0.000 description 4
- 229910013870 LiPF 6 Inorganic materials 0.000 description 4
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 description 4
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 4
- 229910052783 alkali metal Inorganic materials 0.000 description 4
- 229910052782 aluminium Inorganic materials 0.000 description 4
- 239000012298 atmosphere Substances 0.000 description 4
- 238000009826 distribution Methods 0.000 description 4
- 239000010408 film Substances 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 229920001519 homopolymer Polymers 0.000 description 4
- 150000002642 lithium compounds Chemical class 0.000 description 4
- 230000003647 oxidation Effects 0.000 description 4
- 238000007254 oxidation reaction Methods 0.000 description 4
- YWAKXRMUMFPDSH-UHFFFAOYSA-N pentene Chemical compound CCCC=C YWAKXRMUMFPDSH-UHFFFAOYSA-N 0.000 description 4
- 229920001223 polyethylene glycol Polymers 0.000 description 4
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 description 4
- 239000011164 primary particle Substances 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
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- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 3
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 3
- 239000002033 PVDF binder Substances 0.000 description 3
- 238000013019 agitation Methods 0.000 description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 3
- 150000001412 amines Chemical class 0.000 description 3
- 238000000149 argon plasma sintering Methods 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 125000004122 cyclic group Chemical group 0.000 description 3
- 229910021389 graphene Inorganic materials 0.000 description 3
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- 239000007788 liquid Substances 0.000 description 3
- 229910003002 lithium salt Inorganic materials 0.000 description 3
- 159000000002 lithium salts Chemical class 0.000 description 3
- 150000002696 manganese Chemical class 0.000 description 3
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 3
- 150000002815 nickel Chemical class 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Substances N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
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- 239000002243 precursor Substances 0.000 description 3
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- BQCIDUSAKPWEOX-UHFFFAOYSA-N 1,1-Difluoroethene Chemical compound FC(F)=C BQCIDUSAKPWEOX-UHFFFAOYSA-N 0.000 description 2
- SPEUIVXLLWOEMJ-UHFFFAOYSA-N 1,1-dimethoxyethane Chemical compound COC(C)OC SPEUIVXLLWOEMJ-UHFFFAOYSA-N 0.000 description 2
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- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 2
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- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 1
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- XTXRWKRVRITETP-UHFFFAOYSA-N Vinyl acetate Chemical compound CC(=O)OC=C XTXRWKRVRITETP-UHFFFAOYSA-N 0.000 description 1
- 150000001242 acetic acid derivatives Chemical class 0.000 description 1
- 239000006230 acetylene black Substances 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- XYLMUPLGERFSHI-UHFFFAOYSA-N alpha-Methylstyrene Chemical compound CC(=C)C1=CC=CC=C1 XYLMUPLGERFSHI-UHFFFAOYSA-N 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 229910052921 ammonium sulfate Inorganic materials 0.000 description 1
- 235000011130 ammonium sulphate Nutrition 0.000 description 1
- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- CQEYYJKEWSMYFG-UHFFFAOYSA-N butyl acrylate Chemical compound CCCCOC(=O)C=C CQEYYJKEWSMYFG-UHFFFAOYSA-N 0.000 description 1
- 150000004649 carbonic acid derivatives Chemical class 0.000 description 1
- 239000001768 carboxy methyl cellulose Substances 0.000 description 1
- 235000010948 carboxy methyl cellulose Nutrition 0.000 description 1
- 239000008112 carboxymethyl-cellulose Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000006182 cathode active material Substances 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- CXULZQWIHKYPTP-UHFFFAOYSA-N cobalt(2+) manganese(2+) nickel(2+) oxygen(2-) Chemical class [O--].[O--].[O--].[Mn++].[Co++].[Ni++] CXULZQWIHKYPTP-UHFFFAOYSA-N 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 239000011889 copper foil Substances 0.000 description 1
- 239000011258 core-shell material Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 150000004292 cyclic ethers Chemical class 0.000 description 1
- 238000010908 decantation Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- NKDDWNXOKDWJAK-UHFFFAOYSA-N dimethoxymethane Chemical compound COCOC NKDDWNXOKDWJAK-UHFFFAOYSA-N 0.000 description 1
- IEJIGPNLZYLLBP-UHFFFAOYSA-N dimethyl carbonate Chemical compound COC(=O)OC IEJIGPNLZYLLBP-UHFFFAOYSA-N 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- UIWXSTHGICQLQT-UHFFFAOYSA-N ethenyl propanoate Chemical compound CCC(=O)OC=C UIWXSTHGICQLQT-UHFFFAOYSA-N 0.000 description 1
- KLKFAASOGCDTDT-UHFFFAOYSA-N ethoxymethoxyethane Chemical compound CCOCOCC KLKFAASOGCDTDT-UHFFFAOYSA-N 0.000 description 1
- SUPCQIBBMFXVTL-UHFFFAOYSA-N ethyl 2-methylprop-2-enoate Chemical compound CCOC(=O)C(C)=C SUPCQIBBMFXVTL-UHFFFAOYSA-N 0.000 description 1
- JBTWLSYIZRCDFO-UHFFFAOYSA-N ethyl methyl carbonate Chemical compound CCOC(=O)OC JBTWLSYIZRCDFO-UHFFFAOYSA-N 0.000 description 1
- 229920000840 ethylene tetrafluoroethylene copolymer Polymers 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000012065 filter cake Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000006232 furnace black Substances 0.000 description 1
- 239000003365 glass fiber Substances 0.000 description 1
- 150000004820 halides Chemical class 0.000 description 1
- 229920001903 high density polyethylene Polymers 0.000 description 1
- 239000004700 high-density polyethylene Substances 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000010954 inorganic particle Substances 0.000 description 1
- 150000002500 ions Chemical class 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
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 1
- 239000006233 lamp black Substances 0.000 description 1
- 229910052808 lithium carbonate Inorganic materials 0.000 description 1
- 229920001684 low density polyethylene Polymers 0.000 description 1
- 239000004702 low-density polyethylene Substances 0.000 description 1
- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 description 1
- 239000011976 maleic acid Substances 0.000 description 1
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 description 1
- 229940099596 manganese sulfate Drugs 0.000 description 1
- 239000011702 manganese sulphate Substances 0.000 description 1
- 235000007079 manganese sulphate Nutrition 0.000 description 1
- SQQMAOCOWKFBNP-UHFFFAOYSA-L manganese(II) sulfate Chemical compound [Mn+2].[O-]S([O-])(=O)=O SQQMAOCOWKFBNP-UHFFFAOYSA-L 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 150000004682 monohydrates Chemical class 0.000 description 1
- 125000004108 n-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- 125000004123 n-propyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- 229940006444 nickel cation Drugs 0.000 description 1
- 229910001453 nickel ion Inorganic materials 0.000 description 1
- 150000002823 nitrates Chemical class 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- AHKZTVQIVOEVFO-UHFFFAOYSA-N oxide(2-) Chemical compound [O-2] AHKZTVQIVOEVFO-UHFFFAOYSA-N 0.000 description 1
- PNJWIWWMYCMZRO-UHFFFAOYSA-N pent‐4‐en‐2‐one Natural products CC(=O)CC=C PNJWIWWMYCMZRO-UHFFFAOYSA-N 0.000 description 1
- 229910052698 phosphorus Chemical group 0.000 description 1
- 239000011574 phosphorus Chemical group 0.000 description 1
- 229920000058 polyacrylate Polymers 0.000 description 1
- 229920006267 polyester film Polymers 0.000 description 1
- 229920001721 polyimide Polymers 0.000 description 1
- 229920001195 polyisoprene Polymers 0.000 description 1
- 229920005596 polymer binder Polymers 0.000 description 1
- 239000002491 polymer binding agent Substances 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 229920005606 polypropylene copolymer Polymers 0.000 description 1
- 229920005629 polypropylene homopolymer Polymers 0.000 description 1
- 229920002620 polyvinyl fluoride Polymers 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 235000011056 potassium acetate Nutrition 0.000 description 1
- 239000011736 potassium bicarbonate Substances 0.000 description 1
- 229910000028 potassium bicarbonate Inorganic materials 0.000 description 1
- 235000015497 potassium bicarbonate Nutrition 0.000 description 1
- TYJJADVDDVDEDZ-UHFFFAOYSA-M potassium hydrogencarbonate Chemical compound [K+].OC([O-])=O TYJJADVDDVDEDZ-UHFFFAOYSA-M 0.000 description 1
- 239000004323 potassium nitrate Substances 0.000 description 1
- 235000010333 potassium nitrate Nutrition 0.000 description 1
- OTYBMLCTZGSZBG-UHFFFAOYSA-L potassium sulfate Chemical compound [K+].[K+].[O-]S([O-])(=O)=O OTYBMLCTZGSZBG-UHFFFAOYSA-L 0.000 description 1
- 229910052939 potassium sulfate Inorganic materials 0.000 description 1
- 235000011151 potassium sulphates Nutrition 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 1
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000012047 saturated solution Substances 0.000 description 1
- 125000002914 sec-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 235000015424 sodium Nutrition 0.000 description 1
- 239000001632 sodium acetate Substances 0.000 description 1
- 235000017281 sodium acetate Nutrition 0.000 description 1
- 229910000030 sodium bicarbonate Inorganic materials 0.000 description 1
- 235000017557 sodium bicarbonate Nutrition 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 239000004317 sodium nitrate Substances 0.000 description 1
- 235000010344 sodium nitrate Nutrition 0.000 description 1
- 229910052938 sodium sulfate Inorganic materials 0.000 description 1
- 235000011152 sodium sulphate Nutrition 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000001694 spray drying Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 150000003467 sulfuric acid derivatives Chemical class 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 1
- 239000006234 thermal black Substances 0.000 description 1
- 230000008646 thermal stress Effects 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- PJANXHGTPQOBST-UHFFFAOYSA-N trans-Stilbene Natural products C=1C=CC=CC=1C=CC1=CC=CC=C1 PJANXHGTPQOBST-UHFFFAOYSA-N 0.000 description 1
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 description 1
- PJANXHGTPQOBST-VAWYXSNFSA-N trans-stilbene Chemical group C=1C=CC=CC=1/C=C/C1=CC=CC=C1 PJANXHGTPQOBST-VAWYXSNFSA-N 0.000 description 1
- 229910001428 transition metal ion Inorganic materials 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
- 238000005303 weighing Methods 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
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G53/00—Compounds of nickel
- C01G53/006—Compounds containing, besides nickel, two or more other elements, with the exception of oxygen or hydrogen
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G53/00—Compounds of nickel
- C01G53/40—Nickelates
- C01G53/42—Nickelates containing alkali metals, e.g. LiNiO2
- C01G53/44—Nickelates containing alkali metals, e.g. LiNiO2 containing manganese
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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
- H01M10/00—Secondary cells; Manufacture thereof
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- 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
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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
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/50—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- 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
- H01M4/36—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
- H01M4/50—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
- H01M4/505—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese of mixed oxides or hydroxides containing manganese for inserting or intercalating light metals, e.g. LiMn2O4 or LiMn2OxFy
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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- 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
- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
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- 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
- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
- H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
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- H01M10/052—Li-accumulators
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Abstract
Description
aは、0.4から0.8、好ましくは0.48から0.65の範囲内であり、
bは、0.1から0.4、好ましくは0.15から0.25の範囲内であり、
cは、0.1から0.5、好ましくは0.15から0.35の範囲内であり、
dは、ゼロから0.2、好ましくはゼロから0.02の範囲内であり、
a+b+c+d=1であり、
eは、ゼロから1、好ましくは0.5から0.8の範囲内であり、
fは、0.5から2、好ましくは1.1から1.6の範囲内であり、
Ni、CoおよびMnの平均酸化状態は、2.1から3.2の範囲内である。
a’は、0.1から0.4、好ましくは0.18から0.35の範囲内であり、
b’は、ゼロから0.3、好ましくは0.1から0.3の範囲内であり、
c’は、0.4から0.75、好ましくは0.48から0.67の範囲内であり、
d’は、ゼロから0.2、好ましくはゼロから0.05の範囲内であり、
a’+b’+c’+d’=1であり、
e’は、ゼロから1.2、好ましくは0.1から0.6の範囲内であり、
f’は、0.5から2、好ましくは1.0から1.9の範囲内であり、
Ni、CoおよびMnの平均酸化状態は、2.1から3.2の範囲内である。
a’は、0.1から0.4、好ましくは0.18から0.35の範囲内であり、
b’は、ゼロから0.3、好ましくは0.1から0.3の範囲内であり、
c’は、0.4から0.75、好ましくは0.48から0.67の範囲内であり、
d’は、ゼロから0.2、好ましくはゼロから0.05の範囲内であり、
a’+b’+c’+d’=1であり、
e’は、ゼロから0.6、好ましくはゼロから0.2の範囲内であり、
hは、0.4から1、好ましくは0.7から1の範囲内であり、
jは、ゼロから0.2、好ましくは0.01から0.1の範囲内である。
(A)少なくとも1種のアルカリ金属炭酸(水素)塩または少なくとも1種のアルカリ金属水酸化物、および任意に少なくとも1種の化合物Lの水溶液を準備する工程と、
(B)全体として少なくとも2種の遷移金属を含む、遷移金属塩の少なくとも2種の水溶液(B1)および(B2)を準備する工程であって、水溶液(B1)および(B2)は、異なるモル比の遷移金属を有する工程と、
(C)少なくとも2つの撹拌槽の撹拌槽カスケード、またはバッチ反応器において、混合された遷移金属炭酸塩、遷移金属水酸化物または遷移金属炭酸水酸化物の沈殿を行い、
(C1)溶液(B1)および(B2)を、撹拌槽カスケードの様々な撹拌槽内に供給することにより、または
(C2)溶液(B1)および(B2)を、異なる時点または異なる量でバッチ反応器内に供給することにより、
異なる遷移金属濃度で沈殿をもたらす工程と、
(D)このようにして沈殿した球状粒子を取り出す工程とを含む。
(C1)水溶液(B1)および(B2)を、撹拌槽カスケードの様々な撹拌槽内に供給することにより、または
(C2)溶液(B1)および(B2)を、異なる時点または異なる量でバッチ反応器内に供給することにより、
異なる遷移金属濃度で沈殿がもたらされる。
60質量%から98質量%、好ましくは70質量%から96質量%の範囲内の本発明の遷移金属混合酸化物と、
1質量%から20質量%、好ましくは2質量%から15質量%の範囲内の結合剤と、
1質量%から25質量%、好ましくは2質量%から20質量%の範囲内の電気伝導性炭素質材料とを含む。
Yが窒素およびリンから選択される場合、t=2、および
Yが炭素およびケイ素から選択される場合、t=3。
I.1 前駆体−遷移金属水酸化物の球状粒子の生成
実施例および比較例は、8lの全容積を有する反応器システムにおいて行われ、反応器システムは、7lの容積を有する撹拌槽、および、1lの容積を有する、セジメンタを備える傾斜浄化器の組合せの形態をとる固体/液体分離装置を備えていた。分離装置を使用して、反応の間、同時に固体を引き出すことなくポンプを用いて撹拌槽から液相を取り除くことが可能であった。
溶液(C)を添加することにより、上述の硫酸アンモニウム溶液を、23℃で測定してpH11.82まで調整した。次いで、計量ポンプを使用して、反応器システムの撹拌槽の撹拌ブレードに近い乱流ゾーン内に、溶液(B1)、(B2)および(A)を一定の質量流量(780/170/516g/h)で量り入れた。溶液(B1)および(B2)は、反応器に入れる前に静的混合機内で予め混合した。制御デバイスを用いて、溶液(C)の添加により、pHを11.82(23℃で測定)で一定に維持した。懸濁液が形成された(粒子中のモル比:Ni:Co:Mn=70:22:8)。6時間後、(B1)の場合170g/h、および(B2)の場合780g/hの流量が3時間後に達成されるように、(B1)および(B2)の流量を変更した(モル比Ni:Co:Mn=43:21:36)。流量は、直線的に、すなわち単位時間当たり一定の流量変化で変化させた。次いで、流量(B1)および(B2)を、それぞれ170g/hまたは780g/hで1時間維持した。この後に、以下のように流量をさらに変化させた。
− 780g/h(B1)および170g/h(B2)で1時間の一定流量、
− 170g/h(B1)および780g/h(B2)への3時間にわたる直線的変化、
− 170g/h(B1)および780g/h(B2)で3時間の一定流量、
− 780g/h(B1)および170/h(B2)への3時間にわたる直線的変化、
− 780g/h(B1)および170g/h(B2)で3時間の一定流量、
− 170g/h(B1)および780g/h(B2)への3時間にわたる直線的変化、
− 170g/h(B1)および780g/h(B2)で4時間の一定流量。
このようにして得られた粒子を、微細化された炭酸リチウムと密に混合し、存在する遷移金属の総計に対するリチウムのモル比は、1.03であった。この混合物の一部(40g)を、マッフル炉内で、酸素雰囲気中で熱処理した(最高温度:900℃)。約30gの本発明の活性材料(AM.1)が得られた。これを篩い分けした(メッシュサイズ32μm;粗材料なし)。事実上凝集体のない粉末が得られ、これは、本発明の電極を製造するために加工可能であった。
結合剤(BM.1):溶液としてのフッ化ビニリデンのポリマー、NMP中10質量%、Arkema, Inc.からKynar(登録商標)HSV900として粉末が市販されている。
炭素1:カーボンブラック、約60m2/gのBET表面積、Timcalから「Super C65」として市販されている。
炭素2:グラファイト、Timcalから「SFG6L」として市販されている。
0.87gの炭素1、1.46gの炭素2および17.25gの結合剤(BM.1)を、19.5gのN−メチルピロリドン(NMP)の添加と共に混合すると、ペーストが得られた。次の工程において、4.35gのこのペーストを、6.0gの本発明の活性材料(AM.1)と混合した。厚さ30μmのアルミニウム箔を、上述のペーストでコーティングした(活性材料投入量約12mg/cm2)。105℃で乾燥させた後、このようにしてコーティングされたアルミニウム箔の円形部(直径17.5mm)を打ち出した。このようにして得ることができる電極を使用して、本発明の電気化学セルEC.1を製造した。
Claims (20)
- ニッケル、コバルト、マンガン、チタン、バナジウム、クロムおよび鉄から選択される少なくとも2種の遷移金属のカチオンを含む、遷移金属炭酸塩、遷移金属水酸化物または遷移金属炭酸水酸化物の球状粒子であって、当該粒子の半径に対してプロットされた遷移金属カチオンの少なくとも1種の濃度が、当該粒子の中心にも縁部にもない少なくとも1つの相対極値を有する、球状粒子。
- 当該粒子の半径に対してプロットされた少なくとも2種の遷移金属のカチオンの濃度が、それぞれの場合において、当該粒子の中心にも縁部にもない少なくとも1つの相対極値を有する、請求項1に記載の球状粒子。
- 当該粒子の半径に対してプロットされた遷移金属の少なくとも1種のカチオンの濃度が、少なくとも1つの極点を有する、請求項1または2に記載の球状粒子。
- ニッケル、コバルトおよびマンガン、ならびに任意に少なくとも1種のさらなる遷移金属のカチオンを含む、請求項1から3のいずれか一項に記載の球状粒子。
- ニッケルの濃度が、当該粒子の半径にわたり測定して、40モル%から80モル%の範囲内である、請求項1から4のいずれか一項に記載の球状粒子。
- 遷移金属の少なくとも1種のカチオンの濃度が、定数関数の様式で、または10モル%以下のステップで粒子内で変化する、請求項1から5のいずれか一項に記載の球状粒子。
- 1μmから30μmの範囲内のメジアン径(D50)を有する、請求項1から6のいずれか一項に記載の球状粒子。
- 直径にわたり一定の濃度のコバルトを有する、請求項1から7のいずれか一項に記載の球状粒子。
- 直径にわたり一定の濃度のマンガンを有する、請求項1から7のいずれか一項に記載の球状粒子。
- 請求項1から9のいずれか一項に記載の球状粒子を生成するための方法であって、
(A)少なくとも1種のアルカリ金属炭酸(水素)塩または少なくとも1種のアルカリ金属水酸化物、および任意に少なくとも1種の化合物Lの水溶液を準備する工程と、
(B)全体として少なくとも2種の遷移金属を含む、遷移金属塩の少なくとも2種の水溶液(B1)および(B2)を準備する工程であって、水溶液(B1)および(B2)は、異なるモル比の遷移金属を有する工程と、
(C)少なくとも2つの撹拌槽の撹拌槽カスケード、またはバッチ反応器において、混合された遷移金属炭酸塩、遷移金属水酸化物または遷移金属炭酸水酸化物の沈殿を行い、
(C1)溶液(B1)および(B2)を、撹拌槽カスケードの様々な撹拌槽内に供給することにより、または
(C2)溶液(B1)および(B2)を、異なる時点または異なる量でバッチ反応器内に供給することにより、
異なる遷移金属濃度で沈殿をもたらす工程と、
(D)このようにして沈殿した球状粒子を取り出す工程と
を含む方法。 - リチウム化遷移金属混合酸化物の生成のために、請求項1から9のいずれか一項に記載の球状粒子を使用する方法。
- リチウム化遷移金属混合酸化物を生成するための方法であって、請求項1から9の少なくとも一項に記載の球状粒子を、LiOH、Li2OおよびLi2CO3から選択される少なくとも1種のリチウム化合物と混合する工程と、それらを600℃から1000℃の範囲内の温度で互いに反応させる工程とを含む方法。
- ニッケル、コバルト、マンガン、チタン、バナジウム、クロムおよび鉄から選択される少なくとも2種の遷移金属のカチオンを有する、微粒子形態のリチウム化遷移金属混合酸化物であって、当該遷移金属混合酸化物の半径に対してプロットされた遷移金属カチオンの少なくとも1種の濃度が、当該粒子の中心にも縁部にもない少なくとも1つの相対極値を有する、リチウム化遷移金属混合酸化物。
- 当該粒子の半径に対してプロットされた少なくとも2種の遷移金属のカチオンの濃度が、それぞれの場合において、当該粒子の中心にも縁部にもない少なくとも1つの相対極値を有する、請求項13に記載のリチウム化遷移金属混合酸化物。
- 当該粒子の半径に対してプロットされた遷移金属の少なくとも1種のカチオンの濃度が、少なくとも1つの極点を有する、請求項13または14に記載のリチウム化遷移金属混合酸化物。
- ニッケル、コバルトおよびマンガンのカチオン、ならびに任意にイオン形態の少なくとも1種のさらなる遷移金属を含む、請求項13から15のいずれか一項に記載のリチウム化遷移金属混合酸化物。
- ニッケルの濃度が、当該粒子の半径にわたり測定して、40モル%から80モル%の範囲内である、請求項13から16のいずれか一項に記載のリチウム化遷移金属混合酸化物。
- 遷移金属の少なくとも1種のカチオンの濃度が、定数関数の様式で、または10モル%以下のステップで粒子内で変化する、請求項13から17のいずれか一項に記載のリチウム化遷移金属混合酸化物。
- 直径にわたり一定の濃度のコバルトを有する、請求項13から18のいずれか一項に記載のリチウム化遷移金属混合酸化物。
- リチウムイオン電池用のカソードの製造のために、請求項13から19のいずれか一項に記載のリチウム化遷移金属混合酸化物を使用する方法。
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KR20160005765A (ko) | 2016-01-15 |
CN105377765B (zh) | 2018-01-26 |
US10069144B2 (en) | 2018-09-04 |
EP2994424A1 (de) | 2016-03-16 |
KR102223214B1 (ko) | 2021-03-04 |
EP2994424B1 (de) | 2018-07-11 |
WO2014180743A1 (de) | 2014-11-13 |
JP6367313B2 (ja) | 2018-08-01 |
CN105377765A (zh) | 2016-03-02 |
US20160118662A1 (en) | 2016-04-28 |
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