JP2013193888A - 非水電解質二次電池用リチウム複合酸化物粒子粉末及びその製造方法、並びに非水電解質二次電池 - Google Patents
非水電解質二次電池用リチウム複合酸化物粒子粉末及びその製造方法、並びに非水電解質二次電池 Download PDFInfo
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- JP2013193888A JP2013193888A JP2012059327A JP2012059327A JP2013193888A JP 2013193888 A JP2013193888 A JP 2013193888A JP 2012059327 A JP2012059327 A JP 2012059327A JP 2012059327 A JP2012059327 A JP 2012059327A JP 2013193888 A JP2013193888 A JP 2013193888A
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- composite oxide
- compound
- lithium composite
- particle powder
- oxide particle
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- 239000002245 particle Substances 0.000 title claims abstract description 152
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims abstract description 87
- 229910052744 lithium Inorganic materials 0.000 title claims abstract description 86
- 239000000843 powder Substances 0.000 title claims abstract description 85
- 239000002131 composite material Substances 0.000 title claims abstract description 75
- 238000004519 manufacturing process Methods 0.000 title claims description 15
- 239000011255 nonaqueous electrolyte Substances 0.000 title claims description 6
- 150000001875 compounds Chemical class 0.000 claims abstract description 40
- 239000007774 positive electrode material Substances 0.000 claims abstract description 21
- 239000000126 substance Substances 0.000 claims abstract description 7
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 91
- 229910052759 nickel Inorganic materials 0.000 claims description 41
- 229910017052 cobalt Inorganic materials 0.000 claims description 37
- 239000010941 cobalt Substances 0.000 claims description 37
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 37
- 150000002697 manganese compounds Chemical class 0.000 claims description 16
- 150000003755 zirconium compounds Chemical class 0.000 claims description 13
- 229910052782 aluminium Inorganic materials 0.000 claims description 7
- 150000002642 lithium compounds Chemical class 0.000 claims description 6
- 229910052749 magnesium Inorganic materials 0.000 claims description 6
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims description 6
- 239000011164 primary particle Substances 0.000 claims description 6
- 229910052718 tin Inorganic materials 0.000 claims description 6
- 229910001928 zirconium oxide Inorganic materials 0.000 claims description 6
- 229910052684 Cerium Inorganic materials 0.000 claims description 5
- 229910052727 yttrium Inorganic materials 0.000 claims description 5
- 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 description 2
- 230000003542 behavioural effect Effects 0.000 claims 1
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 abstract description 8
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 abstract description 8
- 229910001416 lithium ion Inorganic materials 0.000 abstract description 8
- 229910052726 zirconium Inorganic materials 0.000 abstract description 8
- 238000002156 mixing Methods 0.000 abstract description 5
- 238000010304 firing Methods 0.000 abstract description 4
- 239000002994 raw material Substances 0.000 abstract description 4
- KFDQGLPGKXUTMZ-UHFFFAOYSA-N [Mn].[Co].[Ni] Chemical compound [Mn].[Co].[Ni] KFDQGLPGKXUTMZ-UHFFFAOYSA-N 0.000 abstract description 3
- 230000001351 cycling effect Effects 0.000 abstract 2
- 239000011572 manganese Substances 0.000 description 27
- 229910052748 manganese Inorganic materials 0.000 description 16
- 238000006243 chemical reaction Methods 0.000 description 14
- 230000000694 effects Effects 0.000 description 12
- 239000000203 mixture Substances 0.000 description 11
- 229910013290 LiNiO 2 Inorganic materials 0.000 description 9
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 9
- IPJKJLXEVHOKSE-UHFFFAOYSA-L manganese dihydroxide Chemical compound [OH-].[OH-].[Mn+2] IPJKJLXEVHOKSE-UHFFFAOYSA-L 0.000 description 9
- 229910052751 metal Inorganic materials 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 8
- 239000013078 crystal Substances 0.000 description 8
- 239000008151 electrolyte solution Substances 0.000 description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 7
- 238000000034 method Methods 0.000 description 6
- 229910052719 titanium Inorganic materials 0.000 description 6
- 238000011156 evaluation Methods 0.000 description 5
- 239000010439 graphite Substances 0.000 description 5
- 229910002804 graphite Inorganic materials 0.000 description 5
- 239000002184 metal Substances 0.000 description 5
- 229910012851 LiCoO 2 Inorganic materials 0.000 description 4
- 239000007864 aqueous solution Substances 0.000 description 4
- 229910052791 calcium Inorganic materials 0.000 description 4
- 230000007423 decrease Effects 0.000 description 4
- 239000003792 electrolyte Substances 0.000 description 4
- 238000005259 measurement Methods 0.000 description 4
- 238000012986 modification Methods 0.000 description 4
- 230000004048 modification Effects 0.000 description 4
- 238000012856 packing Methods 0.000 description 4
- 239000002243 precursor Substances 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 239000011230 binding agent Substances 0.000 description 3
- IEJIGPNLZYLLBP-UHFFFAOYSA-N dimethyl carbonate Chemical compound COC(=O)OC IEJIGPNLZYLLBP-UHFFFAOYSA-N 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 239000011888 foil Substances 0.000 description 3
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 description 3
- 229910052808 lithium carbonate Inorganic materials 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- -1 polytetrafluoroethylene Polymers 0.000 description 3
- 238000001878 scanning electron micrograph Methods 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 2
- 229910000733 Li alloy Inorganic materials 0.000 description 2
- 229910015643 LiMn 2 O 4 Inorganic materials 0.000 description 2
- 239000002033 PVDF binder Substances 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical group [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 239000006230 acetylene black Substances 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 239000012670 alkaline solution Substances 0.000 description 2
- 229910000361 cobalt sulfate Inorganic materials 0.000 description 2
- 229940044175 cobalt sulfate Drugs 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
- 239000006258 conductive agent Substances 0.000 description 2
- 239000004020 conductor Substances 0.000 description 2
- 238000002149 energy-dispersive X-ray emission spectroscopy Methods 0.000 description 2
- 229910052731 fluorine Inorganic materials 0.000 description 2
- LBSANEJBGMCTBH-UHFFFAOYSA-N manganate Chemical compound [O-][Mn]([O-])(=O)=O LBSANEJBGMCTBH-UHFFFAOYSA-N 0.000 description 2
- 229940099596 manganese sulfate Drugs 0.000 description 2
- 239000011702 manganese sulphate Substances 0.000 description 2
- 235000007079 manganese sulphate Nutrition 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
- 239000007773 negative electrode material Substances 0.000 description 2
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 description 2
- 229940053662 nickel sulfate Drugs 0.000 description 2
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 description 2
- 229910052698 phosphorus Inorganic materials 0.000 description 2
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 2
- 239000012066 reaction slurry Substances 0.000 description 2
- 239000011163 secondary particle Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- DEXFNLNNUZKHNO-UHFFFAOYSA-N 6-[3-[4-[2-(2,3-dihydro-1H-inden-2-ylamino)pyrimidin-5-yl]piperidin-1-yl]-3-oxopropyl]-3H-1,3-benzoxazol-2-one Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)C1CCN(CC1)C(CCC1=CC2=C(NC(O2)=O)C=C1)=O DEXFNLNNUZKHNO-UHFFFAOYSA-N 0.000 description 1
- 229910000838 Al alloy Inorganic materials 0.000 description 1
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 1
- 238000004438 BET method Methods 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- 229920002134 Carboxymethyl cellulose Polymers 0.000 description 1
- OIFBSDVPJOWBCH-UHFFFAOYSA-N Diethyl carbonate Chemical compound CCOC(=O)OCC OIFBSDVPJOWBCH-UHFFFAOYSA-N 0.000 description 1
- XTHFKEDIFFGKHM-UHFFFAOYSA-N Dimethoxyethane Chemical compound COCCOC XTHFKEDIFFGKHM-UHFFFAOYSA-N 0.000 description 1
- KMTRUDSVKNLOMY-UHFFFAOYSA-N Ethylene carbonate Chemical compound O=C1OCCO1 KMTRUDSVKNLOMY-UHFFFAOYSA-N 0.000 description 1
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 1
- 229910003548 Li(Ni,Co,Mn)O2 Inorganic materials 0.000 description 1
- 229910013733 LiCo Inorganic materials 0.000 description 1
- 229910014689 LiMnO Inorganic materials 0.000 description 1
- 229910013870 LiPF 6 Inorganic materials 0.000 description 1
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 1
- 229910006025 NiCoMn Inorganic materials 0.000 description 1
- 229910001128 Sn alloy Inorganic materials 0.000 description 1
- QXZUUHYBWMWJHK-UHFFFAOYSA-N [Co].[Ni] Chemical compound [Co].[Ni] QXZUUHYBWMWJHK-UHFFFAOYSA-N 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000003125 aqueous solvent Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052797 bismuth Inorganic materials 0.000 description 1
- 239000006229 carbon black Substances 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
- 238000007796 conventional method Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000010828 elution Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 150000002170 ethers Chemical class 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 150000002222 fluorine compounds Chemical class 0.000 description 1
- 238000005755 formation reaction Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 150000004679 hydroxides Chemical class 0.000 description 1
- 230000001771 impaired effect Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000003273 ketjen black Substances 0.000 description 1
- 238000004898 kneading Methods 0.000 description 1
- 238000006138 lithiation reaction Methods 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
- 229910003002 lithium salt Inorganic materials 0.000 description 1
- 159000000002 lithium salts Chemical class 0.000 description 1
- 229910001496 lithium tetrafluoroborate Inorganic materials 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 238000013507 mapping Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 230000003472 neutralizing effect Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- 239000004810 polytetrafluoroethylene Substances 0.000 description 1
- 238000000634 powder X-ray diffraction Methods 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- RUOJZAUFBMNUDX-UHFFFAOYSA-N propylene carbonate Chemical compound CC1COC(=O)O1 RUOJZAUFBMNUDX-UHFFFAOYSA-N 0.000 description 1
- 238000004080 punching Methods 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000000550 scanning electron microscopy energy dispersive X-ray spectroscopy Methods 0.000 description 1
- 235000002639 sodium chloride Nutrition 0.000 description 1
- GCLGEJMYGQKIIW-UHFFFAOYSA-H sodium hexametaphosphate Chemical compound [Na]OP1(=O)OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])O1 GCLGEJMYGQKIIW-UHFFFAOYSA-H 0.000 description 1
- 235000019982 sodium hexametaphosphate Nutrition 0.000 description 1
- 229910052596 spinel Inorganic materials 0.000 description 1
- 239000011029 spinel Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 229920003048 styrene butadiene rubber Polymers 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 description 1
- 239000002562 thickening agent Substances 0.000 description 1
- 238000001132 ultrasonic dispersion Methods 0.000 description 1
- ZXAUZSQITFJWPS-UHFFFAOYSA-J zirconium(4+);disulfate Chemical compound [Zr+4].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O ZXAUZSQITFJWPS-UHFFFAOYSA-J 0.000 description 1
Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
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- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
- H01M4/366—Composites as layered products
-
- 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
- C01G53/50—Nickelates containing alkali metals, e.g. LiNiO2 containing manganese of the type [MnO2]n-, e.g. Li(NixMn1-x)O2, Li(MyNixMn1-x-y)O2
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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
- H01M10/052—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
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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/04—Processes of manufacture in general
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- H01M4/0416—Methods of deposition of the material involving impregnation with a solution, dispersion, paste or dry powder
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- H—ELECTRICITY
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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/04—Processes of manufacture in general
- H01M4/0471—Processes of manufacture in general involving thermal treatment, e.g. firing, sintering, backing particulate active material, thermal decomposition, pyrolysis
-
- 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
- H01M4/131—Electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
-
- H—ELECTRICITY
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- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
- H01M4/1391—Processes of manufacture of electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
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- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/485—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
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- 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
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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
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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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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/40—Electric properties
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Abstract
【解決手段】 ニッケル・コバルト・マンガン系化合物粒子粉末、ジルコニウム原料、リチウム原料を混合、焼成して得ることができる、Zr化合物が粒子表面に存在しており、且つ、前記Zr化合物の化学式がLix(Zr1−yAy)Oz(x、y及びzは、2.0≦x≦8.0、0≦y≦1.0、2.0≦z≦6.0)で表され、Zr含有量が0.05〜1.0wt%であるリチウム複合酸化物粒子粉末を正極活物質として用いることにより、高温での電気抵抗が低く、高温でのサイクル特性及び高温レート特性に優れたリチウムイオン二次電池を製造することが出来る。
【選択図】 なし
Description
x、y、zが前記範囲外の場合には、表面改質効果が十分とは言い難い。Zr化合物は好ましくは化学式:Li2ZrO3(空間群:C2/c)、Li6Zr2O7、Li4ZrO4、Li8ZrO6である。より好ましくはxが2のLi2ZrO3である。
本発明において重要な点は、リチウム複合酸化物粒子の粒子表面にLix(Zr1−yAy)OzからなるZr化合物を存在させることによって、該リチウム複合酸化物粒子粉末を二次電池の正極活物質として用いた場合には、高温での電気抵抗が低く、高温でのサイクル特性及びレート特性に優れた二次電池が得られるという事実である。
尚、試料にはヘキサメタリン酸ソーダーを添加し、超音波分散した後に測定を行った。
サイクル評価に係るコインセルについては、N−メチルピロリドン溶媒中に、本発明による正極活物質粒子粉末であるリチウム複合酸化物粒子粉末を94重量%、導電材としてケッチェンブラックを0.5重量%、グラファイトを2.5重量%、ポリフッ化ビニリデン3重量%とを投入混練した後、Al金属箔に塗布し120℃にて乾燥した。このシートを14mmΦに打ち抜いた後、3t/cm2で圧着し、正極とした。
対極は水溶媒中に、グラファイト負極活物質を94重量%、導電材としてアセチレンブラックを2重量%、増粘剤としてカルボキシメチルセルロースを2重量%、バインダーとしてスチレンブタジエンゴムを2重量%投入混練した後、Cu金属箔に塗布し90℃にて乾燥した。このシートを16mmΦに打ち抜いた後、3t/cm2で圧着し、負極とした。
電解液は1mol/LのLiPF6を溶解したECとDMCを体積比で1:2で混合した溶液を用いて2032型コインセルを作製した。
サイクル評価以外の充放電特性、レート特性および直流抵抗測定に用いるコインセルには、上記の正極電極の大きさを16mmΦとし、負極はリチウム箔を18mmΦに打ち抜いたものを用意した。
初期充放電特性は、室温で充電は4.3Vまで0.2Cの電流密度にて行った後、90分間低電圧充電を行い、放電を3.0Vまで0.2Cの電流密度にて行い、その時の初期充電容量、初期放電容量及び初期効率を測定した。
2mol/lの硫酸ニッケルと硫酸コバルトおよび硫酸マンガンをNi:Co:Mn=1:1:1になるように混合した水溶液と5.0mol/lアンモニア水溶液を、同時に反応槽内に供給した。反応槽は羽根型攪拌機で常に攪拌を行い、同時にpH=11.5±0.5となるように2mol/lの水酸化ナトリウム水溶液を自動供給した。生成したニッケル・コバルト・マンガン水酸化物はオーバーフローされ、オーバーフロー管に連結された濃縮槽で濃縮し、反応槽へ循環を行い、反応槽と沈降槽中のニッケル・コバルト・マンガン水酸化物濃度が4mol/lになるまで40時間反応を行った。
反応後、取り出した懸濁液を、フィルタープレスを用いて水洗を行った後、乾燥を行い、Ni:Co:Mn=1:1:1の平均二次粒子径(D50)が10.3μmのニッケル・コバルト・マンガン水酸化物粒子を得た。
一方、得られたリチウム複合酸化物粒子粉末のX線回折パターンによれば、Li(NiCoMn)O2系化合物の回折ピークとともに、Li2ZrO3のピークが確認された。
ニッケル・コバルト・マンガン水酸化物粒子粉末と酸化ジルコニウムの挙動粒子の平均粒径及びZrの含有量を種々変化させた以外は、前記実施例1と同様にして、リチウム複合酸化物からなる正極活物質を得た。
実施例1の前駆体の合成において、2mol/lの硫酸ニッケルと硫酸コバルトおよび硫酸マンガンをモル比においてNi:Co:Mn=1:1:1になるように混合するところを、そこに硫酸ジルコニウムを加えて、Ni:Co:Mn:Zr=33:33:33:1となるように混合し、その水溶液と5.0mol/lアンモニア水溶液を、同時に反応槽内に供給した。続けて実施例1と同様に反応し、さらに乾燥処理して、Ni:Co:Mn:Zr=33:33:33:1の平均二次粒子径(D50)が10.3μmのジルコニウム含有ニッケル・コバルト・マンガン水酸化物粒子を得た。その後、得られたジルコニウム含有ニッケル・コバルト・マンガン水酸化物粒子粉末と炭酸リチウムを、リチウム/(ニッケル+コバルト+マンガン)のモル比が1.05となるように所定量を十分混合し、この混合物を大気中で、950℃にて10時間焼成し、解砕した。
実施例1のように合成・乾燥して、前駆体のニッケル・コバルト・マンガン水酸化物粒子粉末を得て、続いて得られたニッケル・コバルト・マンガン水酸化物粒子粉末と炭酸リチウムを、リチウム/(ニッケル+コバルト+マンガン)のモル比が1.05となるように所定量を十分混合し、この混合物を大気中で、950℃にて10時間焼成し、解砕した。得られたリチウム複合酸化物粒子粉末に、酸化ジルコニウム粉末をモル比においてNi:Co:Mn:Zr=33:33:33:1となるように所定量を十分混合し、この混合物を大気中で、500℃にて3時間焼成して解砕した。
Claims (6)
- ニッケル、コバルト及びマンガンを含有するリチウム複合酸化物粒子粉末であって、該リチウム複合酸化物粒子粉末の粒子表面にZr化合物が存在しており、且つ、前記Zr化合物の化学式がLix(Zr1−yAy)Oz(x、y及びzは、2.0≦x≦8.0、0≦y≦1.0、2.0≦z≦6.0、A:Mg、Al、Ca、Ti、Y、Sn、Ceから選ばれる少なくとも1種)で表され、Zr含有量が0.05〜1.0wt%であることを特徴とするリチウム複合酸化物粒子粉末。
- 粒子表面に存在するZr化合物の一次粒子の平均粒径が2.0μm以下である請求項1記載のリチウム複合酸化物粒子粉末。
- 粒子表面に存在するZr化合物において、x=2である請求項1又は2記載のリチウム複合酸化物粒子粉末。
- ニッケル・コバルト・マンガン系化合物粒子粉末、ジルコニウム化合物及びリチウム化合物を混合し、次いで、焼成するリチウム複合酸化物粒子粉末の製造方法において、ニッケル・コバルト・マンガン系化合物粒子粉末の挙動粒子の平均粒径が1.0μmから25.0μmである請求項1〜3のいずれかに記載のリチウム複合酸化物粒子粉末の製造方法。
- ニッケル・コバルト・マンガン系化合物粒子粉末、ジルコニウム化合物及びリチウム化合物を混合し、次いで、焼成するリチウム複合酸化物粒子粉末の製造方法において、前記ニッケル・コバルト・マンガン系化合物粒子粉末の挙動粒子の平均粒径が1.0〜25.0μmであり、且つ、前記ジルコニウム化合物は、挙動粒子の平均粒径が4.0μm以下の酸化ジルコニウムである請求項4記載のリチウム複合酸化物粒子粉末の製造方法。
- 請求項1〜3のいずれかに記載のリチウム複合酸化物粒子粉末を正極活物質またはその一部として用いた非水電解質二次電池。
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KR1020147024811A KR20140135180A (ko) | 2012-03-15 | 2013-03-14 | 비수전해질 이차 전지용 리튬 복합 산화물 입자 분말 및 그의 제조 방법, 및 비수전해질 이차 전지 |
US14/384,784 US20150024273A1 (en) | 2012-03-15 | 2013-03-14 | Lithium composite oxide particles for non-aqueous electrolyte secondary batteries and process for producing the same, and non-aqueous electrolyte secondary battery |
CN201380013604.3A CN104169222B (zh) | 2012-03-15 | 2013-03-14 | 非水电解质二次电池用锂复合氧化物颗粒粉末及其制造方法和非水电解质二次电池 |
PCT/JP2013/057150 WO2013137380A1 (ja) | 2012-03-15 | 2013-03-14 | 非水電解質二次電池用リチウム複合酸化物粒子粉末及びその製造方法、並びに非水電解質二次電池 |
EP13760854.3A EP2826750A4 (en) | 2012-03-15 | 2013-03-14 | LITHIUM COMPOUND OXIDE PARTICLE POWDER FOR A SECONDARY BATTERY WITH NON-ACID ELECTROLYTE AND METHOD FOR THE PRODUCTION THEREOF, AND NON-AQUEOUS ELECTROLYTE SECONDARY BATTERY |
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JP5903956B2 (ja) | 2016-04-13 |
CN104169222B (zh) | 2018-03-16 |
KR20140135180A (ko) | 2014-11-25 |
CN104169222A (zh) | 2014-11-26 |
US20190157667A1 (en) | 2019-05-23 |
EP2826750A4 (en) | 2015-10-28 |
WO2013137380A1 (ja) | 2013-09-19 |
US20150024273A1 (en) | 2015-01-22 |
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