JP2012516016A - 電極活物質であるアニオン不足型リン酸遷移金属リチウム化合物、その製造方法、及びそれを利用した電気化学素子 - Google Patents
電極活物質であるアニオン不足型リン酸遷移金属リチウム化合物、その製造方法、及びそれを利用した電気化学素子 Download PDFInfo
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- JP2012516016A JP2012516016A JP2011547778A JP2011547778A JP2012516016A JP 2012516016 A JP2012516016 A JP 2012516016A JP 2011547778 A JP2011547778 A JP 2011547778A JP 2011547778 A JP2011547778 A JP 2011547778A JP 2012516016 A JP2012516016 A JP 2012516016A
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- Prior art keywords
- lithium
- anion
- transition metal
- deficient
- compound
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- 150000001450 anions Chemical class 0.000 title claims abstract description 178
- 230000002950 deficient Effects 0.000 title claims abstract description 135
- -1 transition metal lithium compound Chemical class 0.000 title claims abstract description 115
- 229910052723 transition metal Inorganic materials 0.000 title claims abstract description 92
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 71
- 239000007772 electrode material Substances 0.000 title claims abstract description 16
- 150000001875 compounds Chemical class 0.000 claims abstract description 158
- 229910052744 lithium Inorganic materials 0.000 claims abstract description 119
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 81
- 239000002243 precursor Substances 0.000 claims abstract description 48
- 229910000319 transition metal phosphate Inorganic materials 0.000 claims abstract description 45
- 239000000126 substance Substances 0.000 claims abstract description 42
- 229910019142 PO4 Inorganic materials 0.000 claims abstract description 21
- 239000010452 phosphate Substances 0.000 claims abstract description 20
- 238000006243 chemical reaction Methods 0.000 claims abstract description 17
- 150000002642 lithium compounds Chemical class 0.000 claims abstract description 10
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 86
- 229910052751 metal Inorganic materials 0.000 claims description 56
- 239000002184 metal Substances 0.000 claims description 55
- 229910052748 manganese Inorganic materials 0.000 claims description 37
- 229910052759 nickel Inorganic materials 0.000 claims description 28
- 235000000346 sugar Nutrition 0.000 claims description 28
- 239000013078 crystal Substances 0.000 claims description 27
- 239000010450 olivine Substances 0.000 claims description 25
- 229910052609 olivine Inorganic materials 0.000 claims description 25
- 229910001386 lithium phosphate Inorganic materials 0.000 claims description 23
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 15
- 239000003795 chemical substances by application Substances 0.000 claims description 13
- 230000003113 alkalizing effect Effects 0.000 claims description 11
- 238000002156 mixing Methods 0.000 claims description 11
- 229910052804 chromium Inorganic materials 0.000 claims description 9
- 229910052802 copper Inorganic materials 0.000 claims description 9
- 229910052758 niobium Inorganic materials 0.000 claims description 9
- 229910052719 titanium Inorganic materials 0.000 claims description 9
- 229910052720 vanadium Inorganic materials 0.000 claims description 9
- 229910052725 zinc Inorganic materials 0.000 claims description 9
- 229910052726 zirconium Inorganic materials 0.000 claims description 9
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 8
- 229910052750 molybdenum Inorganic materials 0.000 claims description 8
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 6
- 229910052782 aluminium Inorganic materials 0.000 claims description 6
- 229910052795 boron group element Inorganic materials 0.000 claims description 6
- 239000007833 carbon precursor Substances 0.000 claims description 6
- 239000003638 chemical reducing agent Substances 0.000 claims description 6
- 239000003792 electrolyte Substances 0.000 claims description 6
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 6
- NLKNQRATVPKPDG-UHFFFAOYSA-M potassium iodide Chemical compound [K+].[I-] NLKNQRATVPKPDG-UHFFFAOYSA-M 0.000 claims description 6
- 239000011164 primary particle Substances 0.000 claims description 6
- 229910052727 yttrium Inorganic materials 0.000 claims description 6
- 229910052799 carbon Inorganic materials 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- 229910052749 magnesium Inorganic materials 0.000 claims description 5
- 235000006408 oxalic acid Nutrition 0.000 claims description 5
- 235000019422 polyvinyl alcohol Nutrition 0.000 claims description 5
- 229910052706 scandium Inorganic materials 0.000 claims description 5
- 239000005715 Fructose Substances 0.000 claims description 4
- 229930091371 Fructose Natural products 0.000 claims description 4
- RFSUNEUAIZKAJO-ARQDHWQXSA-N Fructose Chemical compound OC[C@H]1O[C@](O)(CO)[C@@H](O)[C@@H]1O RFSUNEUAIZKAJO-ARQDHWQXSA-N 0.000 claims description 4
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 claims description 4
- 239000002202 Polyethylene glycol Substances 0.000 claims description 4
- 235000010323 ascorbic acid Nutrition 0.000 claims description 4
- 239000011668 ascorbic acid Substances 0.000 claims description 4
- 229960005070 ascorbic acid Drugs 0.000 claims description 4
- 239000012528 membrane Substances 0.000 claims description 4
- 229920001223 polyethylene glycol Polymers 0.000 claims description 4
- 238000000926 separation method Methods 0.000 claims description 4
- LPXPTNMVRIOKMN-UHFFFAOYSA-M sodium nitrite Chemical compound [Na+].[O-]N=O LPXPTNMVRIOKMN-UHFFFAOYSA-M 0.000 claims description 4
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 claims description 4
- 229910052796 boron Inorganic materials 0.000 claims description 3
- 238000001354 calcination Methods 0.000 claims description 3
- 239000010439 graphite Substances 0.000 claims description 3
- 229910002804 graphite Inorganic materials 0.000 claims description 3
- 229920002472 Starch Polymers 0.000 claims description 2
- 239000001913 cellulose Substances 0.000 claims description 2
- 229920002678 cellulose Polymers 0.000 claims description 2
- 235000010980 cellulose Nutrition 0.000 claims description 2
- 229930195733 hydrocarbon Natural products 0.000 claims description 2
- 150000002430 hydrocarbons Chemical class 0.000 claims description 2
- 239000001257 hydrogen Substances 0.000 claims description 2
- 229910052739 hydrogen Inorganic materials 0.000 claims description 2
- 125000004435 hydrogen atom Chemical class [H]* 0.000 claims description 2
- 235000007715 potassium iodide Nutrition 0.000 claims description 2
- 235000010288 sodium nitrite Nutrition 0.000 claims description 2
- 235000010265 sodium sulphite Nutrition 0.000 claims description 2
- 235000019698 starch Nutrition 0.000 claims description 2
- 239000008107 starch Substances 0.000 claims description 2
- NCPXQVVMIXIKTN-UHFFFAOYSA-N trisodium;phosphite Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])[O-] NCPXQVVMIXIKTN-UHFFFAOYSA-N 0.000 claims description 2
- 239000004215 Carbon black (E152) Substances 0.000 claims 1
- 239000011203 carbon fibre reinforced carbon Substances 0.000 claims 1
- 238000010304 firing Methods 0.000 abstract description 20
- 230000007704 transition Effects 0.000 abstract description 5
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 abstract description 4
- 230000002194 synthesizing effect Effects 0.000 abstract description 3
- SMBQBQBNOXIFSF-UHFFFAOYSA-N dilithium Chemical compound [Li][Li] SMBQBQBNOXIFSF-UHFFFAOYSA-N 0.000 abstract 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 111
- 239000007864 aqueous solution Substances 0.000 description 106
- 239000011572 manganese Substances 0.000 description 87
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 description 78
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 77
- 238000000034 method Methods 0.000 description 66
- 229910001416 lithium ion Inorganic materials 0.000 description 61
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 59
- NBIIXXVUZAFLBC-UHFFFAOYSA-N phosphoric acid Substances OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 53
- 230000000052 comparative effect Effects 0.000 description 50
- 238000009792 diffusion process Methods 0.000 description 47
- 238000002441 X-ray diffraction Methods 0.000 description 43
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 43
- 239000000203 mixture Substances 0.000 description 41
- 230000003647 oxidation Effects 0.000 description 41
- 238000007254 oxidation reaction Methods 0.000 description 41
- 150000001768 cations Chemical class 0.000 description 38
- 239000012467 final product Substances 0.000 description 36
- 238000009616 inductively coupled plasma Methods 0.000 description 30
- 238000004611 spectroscopical analysis Methods 0.000 description 30
- 229910052742 iron Inorganic materials 0.000 description 29
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 28
- 238000003991 Rietveld refinement Methods 0.000 description 27
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 27
- 229910021529 ammonia Inorganic materials 0.000 description 21
- 239000012153 distilled water Substances 0.000 description 20
- DVATZODUVBMYHN-UHFFFAOYSA-K lithium;iron(2+);manganese(2+);phosphate Chemical compound [Li+].[Mn+2].[Fe+2].[O-]P([O-])([O-])=O DVATZODUVBMYHN-UHFFFAOYSA-K 0.000 description 19
- 239000012535 impurity Substances 0.000 description 18
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 description 17
- 235000021317 phosphate Nutrition 0.000 description 17
- 229910000358 iron sulfate Inorganic materials 0.000 description 16
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 description 16
- 229910052808 lithium carbonate Inorganic materials 0.000 description 15
- 239000007774 positive electrode material Substances 0.000 description 14
- 230000008569 process Effects 0.000 description 14
- 230000007547 defect Effects 0.000 description 13
- 239000008187 granular material Substances 0.000 description 13
- SQQMAOCOWKFBNP-UHFFFAOYSA-L manganese(II) sulfate Chemical compound [Mn+2].[O-]S([O-])(=O)=O SQQMAOCOWKFBNP-UHFFFAOYSA-L 0.000 description 13
- 150000003624 transition metals Chemical class 0.000 description 13
- 230000000694 effects Effects 0.000 description 12
- 229940099596 manganese sulfate Drugs 0.000 description 12
- 239000011702 manganese sulphate Substances 0.000 description 12
- 235000007079 manganese sulphate Nutrition 0.000 description 12
- 239000002245 particle Substances 0.000 description 12
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 description 11
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 description 11
- LFVGISIMTYGQHF-UHFFFAOYSA-N ammonium dihydrogen phosphate Chemical compound [NH4+].OP(O)([O-])=O LFVGISIMTYGQHF-UHFFFAOYSA-N 0.000 description 10
- 229910000387 ammonium dihydrogen phosphate Inorganic materials 0.000 description 10
- 229910001981 cobalt nitrate Inorganic materials 0.000 description 10
- 150000002500 ions Chemical class 0.000 description 10
- 235000019837 monoammonium phosphate Nutrition 0.000 description 10
- 239000006012 monoammonium phosphate Substances 0.000 description 10
- VEPSWGHMGZQCIN-UHFFFAOYSA-H ferric oxalate Chemical compound [Fe+3].[Fe+3].[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O VEPSWGHMGZQCIN-UHFFFAOYSA-H 0.000 description 9
- 238000010438 heat treatment Methods 0.000 description 8
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 7
- 230000007423 decrease Effects 0.000 description 7
- XKSGHSJZPRUMJX-UHFFFAOYSA-K P(=O)([O-])([O-])[O-].[Fe+2].[Co+2].[Li+] Chemical compound P(=O)([O-])([O-])[O-].[Fe+2].[Co+2].[Li+] XKSGHSJZPRUMJX-UHFFFAOYSA-K 0.000 description 6
- DLFKOMIAYYOZFC-UHFFFAOYSA-K P(=O)([O-])([O-])[O-].[Fe+2].[Ni+2].[Li+] Chemical compound P(=O)([O-])([O-])[O-].[Fe+2].[Ni+2].[Li+] DLFKOMIAYYOZFC-UHFFFAOYSA-K 0.000 description 6
- MQRWBMAEBQOWAF-UHFFFAOYSA-N acetic acid;nickel Chemical compound [Ni].CC(O)=O.CC(O)=O MQRWBMAEBQOWAF-UHFFFAOYSA-N 0.000 description 6
- 239000003990 capacitor Substances 0.000 description 6
- 230000008859 change Effects 0.000 description 6
- 229940011182 cobalt acetate Drugs 0.000 description 6
- QAHREYKOYSIQPH-UHFFFAOYSA-L cobalt(II) acetate Chemical compound [Co+2].CC([O-])=O.CC([O-])=O QAHREYKOYSIQPH-UHFFFAOYSA-L 0.000 description 6
- MNNHAPBLZZVQHP-UHFFFAOYSA-N diammonium hydrogen phosphate Chemical compound [NH4+].[NH4+].OP([O-])([O-])=O MNNHAPBLZZVQHP-UHFFFAOYSA-N 0.000 description 6
- ILXAVRFGLBYNEJ-UHFFFAOYSA-K lithium;manganese(2+);phosphate Chemical compound [Li+].[Mn+2].[O-]P([O-])([O-])=O ILXAVRFGLBYNEJ-UHFFFAOYSA-K 0.000 description 6
- 239000011777 magnesium Substances 0.000 description 6
- 229940078494 nickel acetate Drugs 0.000 description 6
- 239000002994 raw material Substances 0.000 description 6
- DJBQSLSCMPHXBH-UHFFFAOYSA-K P(=O)([O-])([O-])[O-].[Fe+2].[Li+].[Fe+2] Chemical compound P(=O)([O-])([O-])[O-].[Fe+2].[Li+].[Fe+2] DJBQSLSCMPHXBH-UHFFFAOYSA-K 0.000 description 5
- 239000011230 binding agent Substances 0.000 description 5
- 238000007599 discharging Methods 0.000 description 5
- 239000011259 mixed solution Substances 0.000 description 5
- 230000002829 reductive effect Effects 0.000 description 5
- 238000005245 sintering Methods 0.000 description 5
- 239000010936 titanium Substances 0.000 description 5
- 239000005696 Diammonium phosphate Substances 0.000 description 4
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 description 4
- 239000003513 alkali Substances 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 4
- 239000012300 argon atmosphere Substances 0.000 description 4
- 239000012298 atmosphere Substances 0.000 description 4
- 239000000470 constituent Substances 0.000 description 4
- 229910000388 diammonium phosphate Inorganic materials 0.000 description 4
- 235000019838 diammonium phosphate Nutrition 0.000 description 4
- 238000002050 diffraction method Methods 0.000 description 4
- 239000011267 electrode slurry Substances 0.000 description 4
- 230000006872 improvement Effects 0.000 description 4
- PQXKHYXIUOZZFA-UHFFFAOYSA-M lithium fluoride Chemical compound [Li+].[F-] PQXKHYXIUOZZFA-UHFFFAOYSA-M 0.000 description 4
- IIPYXGDZVMZOAP-UHFFFAOYSA-N lithium nitrate Chemical compound [Li+].[O-][N+]([O-])=O IIPYXGDZVMZOAP-UHFFFAOYSA-N 0.000 description 4
- RGVLTEMOWXGQOS-UHFFFAOYSA-L manganese(2+);oxalate Chemical compound [Mn+2].[O-]C(=O)C([O-])=O RGVLTEMOWXGQOS-UHFFFAOYSA-L 0.000 description 4
- 238000005259 measurement Methods 0.000 description 4
- 150000003013 phosphoric acid derivatives Chemical class 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- 150000008044 alkali metal hydroxides Chemical class 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 229910017052 cobalt Inorganic materials 0.000 description 3
- 239000010941 cobalt Substances 0.000 description 3
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 3
- 239000012141 concentrate Substances 0.000 description 3
- 239000006258 conductive agent Substances 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 230000000670 limiting effect Effects 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 229910044991 metal oxide Inorganic materials 0.000 description 3
- 150000004706 metal oxides Chemical class 0.000 description 3
- 229910052698 phosphorus Inorganic materials 0.000 description 3
- 150000003839 salts Chemical group 0.000 description 3
- 238000003980 solgel method Methods 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 238000001694 spray drying Methods 0.000 description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid group Chemical group S(O)(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 3
- 239000011882 ultra-fine particle Substances 0.000 description 3
- XTEGARKTQYYJKE-UHFFFAOYSA-M Chlorate Chemical compound [O-]Cl(=O)=O XTEGARKTQYYJKE-UHFFFAOYSA-M 0.000 description 2
- KMTRUDSVKNLOMY-UHFFFAOYSA-N Ethylene carbonate Chemical compound O=C1OCCO1 KMTRUDSVKNLOMY-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- 229910013275 LiMPO Inorganic materials 0.000 description 2
- 229910013870 LiPF 6 Inorganic materials 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical group O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 2
- JOKHBBPSSUZLQY-UHFFFAOYSA-K P(=O)([O-])([O-])[O-].[Ni+2].[Co+2].[Mn+2].[Li+] Chemical compound P(=O)([O-])([O-])[O-].[Ni+2].[Co+2].[Mn+2].[Li+] JOKHBBPSSUZLQY-UHFFFAOYSA-K 0.000 description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 150000001242 acetic acid derivatives Chemical class 0.000 description 2
- 239000011149 active material Substances 0.000 description 2
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 239000000908 ammonium hydroxide Substances 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 239000002134 carbon nanofiber Substances 0.000 description 2
- 229910010293 ceramic material Inorganic materials 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 239000002019 doping agent Substances 0.000 description 2
- JBTWLSYIZRCDFO-UHFFFAOYSA-N ethyl methyl carbonate Chemical compound CCOC(=O)OC JBTWLSYIZRCDFO-UHFFFAOYSA-N 0.000 description 2
- 238000005469 granulation Methods 0.000 description 2
- 230000003179 granulation Effects 0.000 description 2
- WQYVRQLZKVEZGA-UHFFFAOYSA-N hypochlorite Chemical compound Cl[O-] WQYVRQLZKVEZGA-UHFFFAOYSA-N 0.000 description 2
- XIXADJRWDQXREU-UHFFFAOYSA-M lithium acetate Chemical compound [Li+].CC([O-])=O XIXADJRWDQXREU-UHFFFAOYSA-M 0.000 description 2
- TYIQHQFQWOZFMP-UHFFFAOYSA-E lithium cobalt(2+) iron(2+) manganese(2+) nickel(2+) triphosphate Chemical compound P(=O)([O-])([O-])[O-].[Fe+2].[Ni+2].[Co+2].[Mn+2].[Li+].P(=O)([O-])([O-])[O-].P(=O)([O-])([O-])[O-] TYIQHQFQWOZFMP-UHFFFAOYSA-E 0.000 description 2
- GELKBWJHTRAYNV-UHFFFAOYSA-K lithium iron phosphate Chemical compound [Li+].[Fe+2].[O-]P([O-])([O-])=O GELKBWJHTRAYNV-UHFFFAOYSA-K 0.000 description 2
- SBWRUMICILYTAT-UHFFFAOYSA-K lithium;cobalt(2+);phosphate Chemical compound [Li+].[Co+2].[O-]P([O-])([O-])=O SBWRUMICILYTAT-UHFFFAOYSA-K 0.000 description 2
- LRVBJNJRKRPPCI-UHFFFAOYSA-K lithium;nickel(2+);phosphate Chemical compound [Li+].[Ni+2].[O-]P([O-])([O-])=O LRVBJNJRKRPPCI-UHFFFAOYSA-K 0.000 description 2
- 239000000395 magnesium oxide Substances 0.000 description 2
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 2
- 229910052943 magnesium sulfate Inorganic materials 0.000 description 2
- 235000019341 magnesium sulphate Nutrition 0.000 description 2
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 2
- 229940071125 manganese acetate Drugs 0.000 description 2
- UOGMEBQRZBEZQT-UHFFFAOYSA-L manganese(2+);diacetate Chemical compound [Mn+2].CC([O-])=O.CC([O-])=O UOGMEBQRZBEZQT-UHFFFAOYSA-L 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
- 150000002823 nitrates Chemical class 0.000 description 2
- 239000007800 oxidant agent Substances 0.000 description 2
- 239000011574 phosphorus Substances 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 229910052700 potassium Inorganic materials 0.000 description 2
- 239000000376 reactant Substances 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 239000007858 starting material Substances 0.000 description 2
- 150000003467 sulfuric acid derivatives Chemical class 0.000 description 2
- 150000005622 tetraalkylammonium hydroxides Chemical class 0.000 description 2
- 238000004448 titration Methods 0.000 description 2
- 239000004254 Ammonium phosphate Substances 0.000 description 1
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 description 1
- 239000006245 Carbon black Super-P Substances 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- 229940126062 Compound A Drugs 0.000 description 1
- NLDMNSXOCDLTTB-UHFFFAOYSA-N Heterophylliin A Natural products O1C2COC(=O)C3=CC(O)=C(O)C(O)=C3C3=C(O)C(O)=C(O)C=C3C(=O)OC2C(OC(=O)C=2C=C(O)C(O)=C(O)C=2)C(O)C1OC(=O)C1=CC(O)=C(O)C(O)=C1 NLDMNSXOCDLTTB-UHFFFAOYSA-N 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 229910012851 LiCoO 2 Inorganic materials 0.000 description 1
- 229910011281 LiCoPO 4 Inorganic materials 0.000 description 1
- 229910010707 LiFePO 4 Inorganic materials 0.000 description 1
- 229910015643 LiMn 2 O 4 Inorganic materials 0.000 description 1
- 229910013086 LiNiPO Inorganic materials 0.000 description 1
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- 239000002033 PVDF binder Substances 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 229910001860 alkaline earth metal hydroxide Inorganic materials 0.000 description 1
- 150000004703 alkoxides Chemical class 0.000 description 1
- JLDSOYXADOWAKB-UHFFFAOYSA-N aluminium nitrate Chemical compound [Al+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O JLDSOYXADOWAKB-UHFFFAOYSA-N 0.000 description 1
- BDUVKRQZXGREDK-UHFFFAOYSA-K aluminum lithium iron(2+) manganese(2+) phosphate Chemical compound P(=O)([O-])([O-])[O-].[Fe+2].[Mn+2].[Al+3].[Li+] BDUVKRQZXGREDK-UHFFFAOYSA-K 0.000 description 1
- 229910000148 ammonium phosphate Inorganic materials 0.000 description 1
- 235000019289 ammonium phosphates Nutrition 0.000 description 1
- 150000003863 ammonium salts Chemical class 0.000 description 1
- 125000000129 anionic group Chemical group 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000000889 atomisation Methods 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 229910052810 boron oxide Inorganic materials 0.000 description 1
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 description 1
- 229910052794 bromium Inorganic materials 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- OJIJEKBXJYRIBZ-UHFFFAOYSA-N cadmium nickel Chemical compound [Ni].[Cd] OJIJEKBXJYRIBZ-UHFFFAOYSA-N 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 150000004649 carbonic acid derivatives Chemical class 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical group [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 230000002542 deteriorative effect Effects 0.000 description 1
- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 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
- XPPKVPWEQAFLFU-UHFFFAOYSA-N diphosphoric acid Chemical compound OP(O)(=O)OP(O)(O)=O XPPKVPWEQAFLFU-UHFFFAOYSA-N 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000003487 electrochemical reaction Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 238000001879 gelation Methods 0.000 description 1
- 239000003349 gelling agent Substances 0.000 description 1
- 239000011361 granulated particle Substances 0.000 description 1
- 150000004820 halides Chemical class 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 150000004679 hydroxides Chemical class 0.000 description 1
- 230000033444 hydroxylation Effects 0.000 description 1
- 238000005805 hydroxylation reaction Methods 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 150000008040 ionic compounds Chemical class 0.000 description 1
- OWZIYWAUNZMLRT-UHFFFAOYSA-L iron(2+);oxalate Chemical compound [Fe+2].[O-]C(=O)C([O-])=O OWZIYWAUNZMLRT-UHFFFAOYSA-L 0.000 description 1
- 229910000625 lithium cobalt oxide Inorganic materials 0.000 description 1
- INHCSSUBVCNVSK-UHFFFAOYSA-L lithium sulfate Inorganic materials [Li+].[Li+].[O-]S([O-])(=O)=O INHCSSUBVCNVSK-UHFFFAOYSA-L 0.000 description 1
- HDCVHVAWSPSEET-UHFFFAOYSA-K lithium;magnesium;manganese(2+);phosphate Chemical compound [Li+].[Mg+2].[Mn+2].[O-]P([O-])([O-])=O HDCVHVAWSPSEET-UHFFFAOYSA-K 0.000 description 1
- BFZPBUKRYWOWDV-UHFFFAOYSA-N lithium;oxido(oxo)cobalt Chemical compound [Li+].[O-][Co]=O BFZPBUKRYWOWDV-UHFFFAOYSA-N 0.000 description 1
- 229910052987 metal hydride Inorganic materials 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 239000007773 negative electrode material Substances 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 150000003891 oxalate salts Chemical class 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 230000010287 polarization Effects 0.000 description 1
- 229920000137 polyphosphoric acid Polymers 0.000 description 1
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 229940005657 pyrophosphoric acid Drugs 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 239000007784 solid electrolyte Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000005563 spheronization Methods 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 230000007480 spreading Effects 0.000 description 1
- 238000003892 spreading Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000012916 structural analysis Methods 0.000 description 1
- 230000001629 suppression Effects 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000013076 target substance Substances 0.000 description 1
- RBTVSNLYYIMMKS-UHFFFAOYSA-N tert-butyl 3-aminoazetidine-1-carboxylate;hydrochloride Chemical compound Cl.CC(C)(C)OC(=O)N1CC(N)C1 RBTVSNLYYIMMKS-UHFFFAOYSA-N 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-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
- 229910021642 ultra pure water Inorganic materials 0.000 description 1
- 239000012498 ultrapure water Substances 0.000 description 1
- 239000011800 void material Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- 229910001928 zirconium oxide Inorganic materials 0.000 description 1
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Abstract
【選択図】図6
Description
(a)金属Mの前駆体、リン酸化合物、アルカリ化剤、及びリチウム前駆体を混合してリン酸遷移金属リチウム化合物前駆体を生成する段階;
(b)上記段階(a)のリン酸遷移金属リチウム化合物前駆体を温度200〜700℃、圧力180〜550barの反応条件下で水と混合し、アニオン不足型リン酸遷移金属リチウム化合物を合成し、合成された化合物を乾燥する段階;
(c)上記段階(b)の結果物を焼成するか、又は顆粒化した後焼成する段階。
最終製造物の粒子大きさと形状を評価するために走査電子顕微鏡(SEM)分析を行った。図1は顆粒化した粒子を1,000倍拡大して撮影したもので、約5〜30μmの顆粒体大きさを示している。図2は顆粒体一部を50,000倍拡大して撮影したもので、顆粒体を構成しているナノメートル(nanometer)大きさの超微粒子を示す。
最終製造物についてX線回折(XRD)パターンを分析した結果、オリビン構造の結晶質であることを確認した。また、誘導結合プラズマ(ICP)分光分析を行い、上記化合物がLi0.83(Mn0.25Co0.25Ni0.25Fe0.25)(PO4)0.94であることを確認した。
Claims (24)
- 電極活物質である、下記化学式1で表されるアニオン不足型リン酸遷移金属リチウム化合物。
[化学式1] Li1−xM(PO4)1−y
上記化学式1において、0≦x≦0.15であり、0<y≦0.05であり、Mは下記化学式2で表される。
[化学式2] MA aMB bMT tFe1−(a+b+t)
上記化学式2において、MAは第2族元素からなる群から選ばれる1種以上の元素であり、MBは第13族元素からなる群から選ばれる1種以上の元素であり、MTはSc、Ti、V、Cr、Mn、Co、Ni、Cu、Zn、Y、Zr、Nb、及びMoからなる群から選ばれる1種以上の元素であり、0≦a<1であり、0≦b<0.575であり、0≦t≦1であり、0≦(a+b)<1であり、0<(a+b+t)≦1である。 - 0.01≦y≦0.05である、請求項1に記載のアニオン不足型リン酸遷移金属チウム化合物。
- 0.02≦y≦0.05である、請求項1に記載のアニオン不足型リン酸遷移金属チウム化合物。
- 0.03≦y≦0.05である、請求項1に記載のアニオン不足型リン酸遷移金属リチウム化合物。
- MAはMg及びCaからなる群から選ばれる1種以上の元素であり、MBはB、Al、及びGaからなる群から選ばれる1種以上の元素であり、MTはTi、V、Cr、Mn、Co、Ni、Cu、Zn、Zr、Nb、及びMoからなる群から選ばれる1種以上の元素である、請求項1に記載のアニオン不足型リン酸遷移金属リチウム化合物。
- MAはMgであり、MBはAlであり、MTはMn、Co、及びNiからなる群から選ばれる1種以上の元素である、請求項1に記載のアニオン不足型リン酸遷移金属リチウム化合物。
- 0≦a≦0.30であり、0≦b≦0.20である、請求項1に記載のアニオン不足型リン酸遷移金属リチウム化合物。
- 0≦a≦0.15であり、0≦b≦0.10である、請求項1に記載のアニオン不足型リン酸遷移金属リチウム化合物。
- オリビン(olivine)結晶構造を有することを特徴とする、請求項1に記載のアニオン不足型リン酸遷移金属リチウム化合物。
- 請求項1乃至請求項9の何れか1項に記載のアニオン不足型リン酸遷移金属リチウム化合物を含む二次電池の正極。
- (a)請求項1乃至請求項9の何れか1項に記載のアニオン不足型リン酸遷移金属リチウム化合物を含む正極、
(b)負極、
(c)分離膜、及び
(d)電解質
を含む二次電池。 - (a)金属Mの前駆体、リン酸化合物、アルカリ化剤、及びリチウム前駆体を混合してリン酸遷移金属リチウム化合物前駆体を生成する段階;
(b)上記段階(a)のリン酸遷移金属リチウム化合物前駆体を温度200〜700℃、圧力180〜550barである反応条件下で水と混合してアニオン不足型リン酸遷移金属リチウム化合物を合成し、合成された化合物を乾燥する段階;
(c)上記段階(b)の結果物を焼成(calcination)するか、又は顆粒化した後焼成する段階を含む、
電極活物質である、下記化学式1で表されるアニオン不足型リン酸遷移金属リチウム化合物の製造方法。
[化学式1] Li1−xM(PO4)1−y
上記化学式1において、0≦x≦0.15であり、0<y≦0.05であり、Mは下記化学式2で表される。
[化学式2] MA aMB bMT tFe1−(a+b+t)
上記化学式2において、MAは第2族元素からなる群から選ばれる1種以上の元素であり、MBは第13族元素からなる群から選ばれる1種以上の元素であり、MTはSc、Ti、V、Cr、Mn、Co、Ni、Cu、Zn、Y、Zr、Nb、及びMoからなる群から選ばれる1種以上の元素であり、0≦a<1であり、0≦b<0.575であり、0≦t≦1であり、0≦(a+b)<1であり、0<(a+b+t)≦1である。 - 0.01≦y≦0.05である、請求項12に記載のアニオン不足型リン酸遷移金属リチウム化合物の製造方法。
- 0.02≦y≦0.05である、請求項12に記載のアニオン不足型リン酸遷移金属リチウム化合物の製造方法。
- 0.03≦y≦0.05である、請求項12に記載のアニオン不足型リン酸遷移金属リチウム化合物の製造方法。
- MAはMg及びCaからなる群から選ばれる1種以上の元素であり、MBはB、Al、及びGaからなる群から選ばれる1種以上の元素であり、MTはTi、V、Cr、Mn、Co、Ni、Cu、Zn、Zr、Nb、及びMoからなる群から選ばれる1種以上の元素である、請求項12に記載のアニオン不足型リン酸遷移金属リチウム化合物の製造方法。
- MAはMgであり、MBはAlであり、MTはMn、Co、及びNiからなる群から選ばれる1種以上の元素である、請求項12に記載のアニオン不足型リン酸遷移金属リチウム化合物の製造方法。
- 0≦a≦0.30であり、0≦b≦0.20である、請求項12に記載のアニオン不足型リン酸遷移金属リチウム化合物の製造方法。
- 0≦a≦0.15であり、0≦b≦0.10である、請求項12に記載のアニオン不足型リン酸遷移金属リチウム化合物の製造方法。
- オリビン(olivine)結晶構造を有することを特徴とする、請求項12に記載のアニオン不足型リン酸遷移金属リチウム化合物の製造方法。
- 段階(b)の上記反応条件のpHは4.0を超過し、12.0以下である、請求項12に記載のアニオン不足型リン酸遷移金属リチウム化合物の製造方法。
- 段階(b)において合成されたアニオン不足型リン酸遷移金属リチウム化合物の一次粒子平均大きさが0.01〜5μmである、請求項12に記載のアニオン不足型リン酸遷移金属リチウム化合物の製造方法。
- 段階(a)〜(c)のうち一つ以上の段階の前後或いは段階中に、ヒドラジン、亜リン酸ナトリウム、亜硫酸ナトリウム、亜硝酸ナトリウム、ヨード化カリウム、砂糖、果糖、シュウ酸、アスコルビン酸、水素、炭素、及び炭化水素からなる群から選ばれる1種以上の還元剤を投入することを特徴とする、請求項12に記載のアニオン不足型リン酸遷移金属リチウム化合物の製造方法。
- 段階(a)〜(c)のうち、一つ以上の段階の前後或いは段階中に、黒鉛、砂糖、果糖、シュウ酸、アスコルビン酸、澱粉、セルロース、ポリビニルアルコール(PVA)、ポリエチレングリコール(PEG)からなる群から選ばれる1種以上の炭素前駆体を投入することを特徴とする、請求項12に記載のアニオン不足型リン酸遷移金属リチウム化合物の製造方法。
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JP2014071968A (ja) * | 2012-09-28 | 2014-04-21 | Sumitomo Metal Mining Co Ltd | リチウム二次電池用正極活物質の前駆体とその製造方法、および該前駆体を用いたリチウム二次電池用正極活物質とその製造方法、並びに該正極活物質を用いたリチウム二次電池 |
JP2016129145A (ja) * | 2016-02-18 | 2016-07-14 | 住友金属鉱山株式会社 | リチウム二次電池用正極活物質の前駆体とその製造方法、および該前駆体を用いたリチウム二次電池用正極活物質とその製造方法、並びに該正極活物質を用いたリチウム二次電池 |
JP2020149927A (ja) * | 2019-03-15 | 2020-09-17 | 積水化学工業株式会社 | 非水電解質二次電池用正極及びリチウムイオン二次電池 |
JP7280722B2 (ja) | 2019-03-15 | 2023-05-24 | 積水化学工業株式会社 | 非水電解質二次電池用正極及びリチウムイオン二次電池 |
WO2022097400A1 (ja) * | 2020-11-06 | 2022-05-12 | 株式会社Gsユアサ | 蓄電素子用正極活物質、蓄電素子用正極、蓄電素子及び蓄電装置 |
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US20100183924A1 (en) | 2010-07-22 |
US7858233B2 (en) | 2010-12-28 |
CN102292855A (zh) | 2011-12-21 |
CN102292855B (zh) | 2014-01-22 |
JP5318969B2 (ja) | 2013-10-16 |
TW201036235A (en) | 2010-10-01 |
CN101789507A (zh) | 2010-07-28 |
TWI383533B (zh) | 2013-01-21 |
JP2010170997A (ja) | 2010-08-05 |
EP2211404A1 (en) | 2010-07-28 |
TW201032377A (en) | 2010-09-01 |
HK1144616A1 (en) | 2011-02-25 |
WO2010085104A2 (ko) | 2010-07-29 |
WO2010085104A9 (ko) | 2010-10-14 |
EP2390948A2 (en) | 2011-11-30 |
US20120021288A1 (en) | 2012-01-26 |
WO2010085104A3 (ko) | 2010-12-02 |
CN101789507B (zh) | 2013-08-14 |
JP4625536B2 (ja) | 2011-02-02 |
KR100939647B1 (ko) | 2010-02-03 |
CA2750328A1 (en) | 2010-07-29 |
CA2750328C (en) | 2014-03-18 |
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