JP6072916B2 - 正極活物質及びこの製造方法 - Google Patents
正極活物質及びこの製造方法 Download PDFInfo
- Publication number
- JP6072916B2 JP6072916B2 JP2015528426A JP2015528426A JP6072916B2 JP 6072916 B2 JP6072916 B2 JP 6072916B2 JP 2015528426 A JP2015528426 A JP 2015528426A JP 2015528426 A JP2015528426 A JP 2015528426A JP 6072916 B2 JP6072916 B2 JP 6072916B2
- Authority
- JP
- Japan
- Prior art keywords
- active material
- positive electrode
- electrode active
- sodium
- polycrystalline
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- 239000007774 positive electrode material Substances 0.000 title claims description 98
- 238000004519 manufacturing process Methods 0.000 title claims description 46
- 239000011572 manganese Substances 0.000 claims description 98
- 239000002243 precursor Substances 0.000 claims description 89
- 239000011734 sodium Substances 0.000 claims description 76
- 229910052708 sodium Inorganic materials 0.000 claims description 67
- 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 claims description 66
- 229910002102 lithium manganese oxide Inorganic materials 0.000 claims description 63
- 239000002245 particle Substances 0.000 claims description 63
- VLXXBCXTUVRROQ-UHFFFAOYSA-N lithium;oxido-oxo-(oxomanganiooxy)manganese Chemical compound [Li+].[O-][Mn](=O)O[Mn]=O VLXXBCXTUVRROQ-UHFFFAOYSA-N 0.000 claims description 62
- 229910052748 manganese Inorganic materials 0.000 claims description 58
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 claims description 57
- 239000011247 coating layer Substances 0.000 claims description 49
- 229910052744 lithium Inorganic materials 0.000 claims description 38
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 35
- 239000013078 crystal Substances 0.000 claims description 27
- 238000000034 method Methods 0.000 claims description 22
- 150000001875 compounds Chemical class 0.000 claims description 19
- 239000011163 secondary particle Substances 0.000 claims description 18
- 238000002156 mixing Methods 0.000 claims description 17
- 239000011164 primary particle Substances 0.000 claims description 17
- 238000002441 X-ray diffraction Methods 0.000 claims description 16
- -1 aluminum compound Chemical class 0.000 claims description 16
- 239000000203 mixture Substances 0.000 claims description 14
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 12
- 229910052782 aluminium Inorganic materials 0.000 claims description 10
- 238000005259 measurement Methods 0.000 claims description 10
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical group [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 8
- 239000006182 cathode active material Substances 0.000 claims description 8
- 238000010304 firing Methods 0.000 claims description 8
- 239000000126 substance Substances 0.000 claims description 8
- 239000011248 coating agent Substances 0.000 claims description 7
- 238000000576 coating method Methods 0.000 claims description 7
- 230000007423 decrease Effects 0.000 claims description 7
- KKCBUQHMOMHUOY-UHFFFAOYSA-N sodium oxide Chemical compound [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 claims description 7
- 229910001948 sodium oxide Inorganic materials 0.000 claims description 7
- 238000000926 separation method Methods 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 5
- 238000000975 co-precipitation Methods 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 4
- 101100513612 Microdochium nivale MnCO gene Proteins 0.000 claims description 3
- 239000004115 Sodium Silicate Substances 0.000 claims description 2
- 230000002776 aggregation Effects 0.000 claims description 2
- 238000004220 aggregation Methods 0.000 claims description 2
- 238000001354 calcination Methods 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims description 2
- 230000008569 process Effects 0.000 claims description 2
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 2
- 229910052911 sodium silicate Inorganic materials 0.000 claims description 2
- 238000001694 spray drying Methods 0.000 claims description 2
- 238000002050 diffraction method Methods 0.000 claims 1
- 230000000052 comparative effect Effects 0.000 description 29
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 16
- 239000003792 electrolyte Substances 0.000 description 14
- 229910015643 LiMn 2 O 4 Inorganic materials 0.000 description 13
- 238000010828 elution Methods 0.000 description 9
- 239000002002 slurry Substances 0.000 description 9
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 7
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 7
- 239000011230 binding agent Substances 0.000 description 7
- 229910052799 carbon Inorganic materials 0.000 description 7
- 239000007773 negative electrode material Substances 0.000 description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 6
- 230000008859 change Effects 0.000 description 6
- 239000006258 conductive agent Substances 0.000 description 6
- 230000001965 increasing effect Effects 0.000 description 6
- 229910001416 lithium ion Inorganic materials 0.000 description 6
- 229910052751 metal Inorganic materials 0.000 description 6
- 239000002184 metal Substances 0.000 description 6
- 239000002904 solvent Substances 0.000 description 6
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 description 5
- 239000007864 aqueous solution Substances 0.000 description 5
- 150000002500 ions Chemical class 0.000 description 5
- 229920000642 polymer Polymers 0.000 description 5
- 238000007086 side reaction Methods 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 4
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 4
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 4
- 239000005977 Ethylene Substances 0.000 description 4
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 4
- 229920001577 copolymer Polymers 0.000 description 4
- 239000010949 copper Substances 0.000 description 4
- 239000002270 dispersing agent Substances 0.000 description 4
- 239000011255 nonaqueous electrolyte Substances 0.000 description 4
- 238000005096 rolling process Methods 0.000 description 4
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 3
- 229920000049 Carbon (fiber) Polymers 0.000 description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 3
- 239000002033 PVDF binder Substances 0.000 description 3
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 3
- 235000011114 ammonium hydroxide Nutrition 0.000 description 3
- 239000004917 carbon fiber Substances 0.000 description 3
- 239000003575 carbonaceous material Substances 0.000 description 3
- 238000005119 centrifugation Methods 0.000 description 3
- 229910052802 copper Inorganic materials 0.000 description 3
- 239000012153 distilled water Substances 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 235000019441 ethanol Nutrition 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 239000000835 fiber Substances 0.000 description 3
- 230000001678 irradiating effect Effects 0.000 description 3
- 238000007561 laser diffraction method Methods 0.000 description 3
- 229910052759 nickel Inorganic materials 0.000 description 3
- 239000004745 nonwoven fabric Substances 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 238000012856 packing Methods 0.000 description 3
- 239000011295 pitch Substances 0.000 description 3
- 239000002798 polar solvent Substances 0.000 description 3
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 229910052596 spinel Inorganic materials 0.000 description 3
- 239000011029 spinel Substances 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 229910052719 titanium Inorganic materials 0.000 description 3
- 239000010936 titanium Substances 0.000 description 3
- 230000007704 transition Effects 0.000 description 3
- 229920002943 EPDM rubber Polymers 0.000 description 2
- 229910013870 LiPF 6 Inorganic materials 0.000 description 2
- 239000004698 Polyethylene Substances 0.000 description 2
- 239000004743 Polypropylene Substances 0.000 description 2
- 229920002125 Sokalan® Polymers 0.000 description 2
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
- 239000011149 active material Substances 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 239000012298 atmosphere Substances 0.000 description 2
- 210000003323 beak Anatomy 0.000 description 2
- 239000006229 carbon black Substances 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [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 2
- 239000008151 electrolyte solution Substances 0.000 description 2
- 239000010408 film Substances 0.000 description 2
- 239000011888 foil Substances 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 230000001939 inductive effect Effects 0.000 description 2
- 239000004973 liquid crystal related substance Substances 0.000 description 2
- 239000011244 liquid electrolyte Substances 0.000 description 2
- IIPYXGDZVMZOAP-UHFFFAOYSA-N lithium nitrate Chemical compound [Li+].[O-][N+]([O-])=O IIPYXGDZVMZOAP-UHFFFAOYSA-N 0.000 description 2
- 229910003002 lithium salt Inorganic materials 0.000 description 2
- 159000000002 lithium salts Chemical class 0.000 description 2
- 229910001437 manganese ion Inorganic materials 0.000 description 2
- 239000007769 metal material Substances 0.000 description 2
- 235000013336 milk Nutrition 0.000 description 2
- 239000008267 milk Substances 0.000 description 2
- 210000004080 milk Anatomy 0.000 description 2
- 229910021382 natural graphite Inorganic materials 0.000 description 2
- 239000004584 polyacrylic acid Substances 0.000 description 2
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- 229910001220 stainless steel Inorganic materials 0.000 description 2
- 239000010935 stainless steel Substances 0.000 description 2
- 229920003048 styrene butadiene rubber Polymers 0.000 description 2
- 239000010409 thin film Substances 0.000 description 2
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 1
- 229920002134 Carboxymethyl cellulose Polymers 0.000 description 1
- 229910000925 Cd alloy Inorganic materials 0.000 description 1
- 229910020366 ClO 4 Inorganic materials 0.000 description 1
- OIFBSDVPJOWBCH-UHFFFAOYSA-N Diethyl carbonate Chemical compound CCOC(=O)OCC OIFBSDVPJOWBCH-UHFFFAOYSA-N 0.000 description 1
- KMTRUDSVKNLOMY-UHFFFAOYSA-N Ethylene carbonate Chemical compound O=C1OCCO1 KMTRUDSVKNLOMY-UHFFFAOYSA-N 0.000 description 1
- 229920002153 Hydroxypropyl cellulose Polymers 0.000 description 1
- 229910012851 LiCoO 2 Inorganic materials 0.000 description 1
- 229910014689 LiMnO Inorganic materials 0.000 description 1
- 229910013553 LiNO Inorganic materials 0.000 description 1
- WAEMQWOKJMHJLA-UHFFFAOYSA-N Manganese(2+) Chemical compound [Mn+2] WAEMQWOKJMHJLA-UHFFFAOYSA-N 0.000 description 1
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 description 1
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 229920000265 Polyparaphenylene Polymers 0.000 description 1
- 239000004372 Polyvinyl alcohol Substances 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 229920002472 Starch Polymers 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- 239000006230 acetylene black Substances 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 238000003915 air pollution Methods 0.000 description 1
- 230000003113 alkalizing effect Effects 0.000 description 1
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical compound [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 229910021383 artificial graphite Inorganic materials 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- IAQRGUVFOMOMEM-UHFFFAOYSA-N butene Natural products CC=CC IAQRGUVFOMOMEM-UHFFFAOYSA-N 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 239000006231 channel black Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 239000000571 coke Substances 0.000 description 1
- 239000008139 complexing agent Substances 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000005562 fading Methods 0.000 description 1
- 229920001973 fluoroelastomer Polymers 0.000 description 1
- NBVXSUQYWXRMNV-UHFFFAOYSA-N fluoromethane Chemical compound FC NBVXSUQYWXRMNV-UHFFFAOYSA-N 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- 239000006232 furnace black Substances 0.000 description 1
- 239000003502 gasoline Substances 0.000 description 1
- 239000003365 glass fiber Substances 0.000 description 1
- 229910021385 hard carbon Inorganic materials 0.000 description 1
- 229920001519 homopolymer Polymers 0.000 description 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
- 239000001863 hydroxypropyl cellulose Substances 0.000 description 1
- 235000010977 hydroxypropyl cellulose Nutrition 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000003273 ketjen black Substances 0.000 description 1
- 239000006233 lamp black Substances 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 description 1
- KWGKDLIKAYFUFQ-UHFFFAOYSA-M lithium chloride Chemical group [Li+].[Cl-] KWGKDLIKAYFUFQ-UHFFFAOYSA-M 0.000 description 1
- 229910000625 lithium cobalt oxide Inorganic materials 0.000 description 1
- QEXMICRJPVUPSN-UHFFFAOYSA-N lithium manganese(2+) oxygen(2-) Chemical class [O-2].[Mn+2].[Li+] QEXMICRJPVUPSN-UHFFFAOYSA-N 0.000 description 1
- 229910001386 lithium phosphate Inorganic materials 0.000 description 1
- BFZPBUKRYWOWDV-UHFFFAOYSA-N lithium;oxido(oxo)cobalt Chemical compound [Li+].[O-][Co]=O BFZPBUKRYWOWDV-UHFFFAOYSA-N 0.000 description 1
- VROAXDSNYPAOBJ-UHFFFAOYSA-N lithium;oxido(oxo)nickel Chemical compound [Li+].[O-][Ni]=O VROAXDSNYPAOBJ-UHFFFAOYSA-N 0.000 description 1
- 150000002697 manganese compounds Chemical class 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000002931 mesocarbon microbead Substances 0.000 description 1
- 239000011302 mesophase pitch Substances 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 239000004005 microsphere Substances 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 239000012046 mixed solvent Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 229920003229 poly(methyl methacrylate) Polymers 0.000 description 1
- 229920005569 poly(vinylidene fluoride-co-hexafluoropropylene) Polymers 0.000 description 1
- 229920002239 polyacrylonitrile Polymers 0.000 description 1
- 229920000139 polyethylene terephthalate Polymers 0.000 description 1
- 239000005020 polyethylene terephthalate Substances 0.000 description 1
- 239000004926 polymethyl methacrylate Substances 0.000 description 1
- 229920000098 polyolefin Polymers 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 229920000036 polyvinylpyrrolidone Polymers 0.000 description 1
- 239000001267 polyvinylpyrrolidone Substances 0.000 description 1
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 229920001384 propylene homopolymer Polymers 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
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- 239000004627 regenerated cellulose Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 229910021384 soft carbon Inorganic materials 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 229920005608 sulfonated EPDM Polymers 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 239000002345 surface coating layer Substances 0.000 description 1
- 230000008961 swelling Effects 0.000 description 1
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical group FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 description 1
- 239000006234 thermal black Substances 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- 239000011135 tin Substances 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical group 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
- 239000003981 vehicle Substances 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B35/00—Boron; Compounds thereof
- C01B35/08—Compounds containing boron and nitrogen, phosphorus, oxygen, sulfur, selenium or tellurium
- C01B35/10—Compounds containing boron and oxygen
- C01B35/12—Borates
- C01B35/128—Borates containing plural metal or metal and ammonium
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G45/00—Compounds of manganese
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G45/00—Compounds of manganese
- C01G45/12—Manganates manganites or permanganates
- C01G45/1207—Permanganates ([MnO]4-) or manganates ([MnO4]2-)
- C01G45/1214—Permanganates ([MnO]4-) or manganates ([MnO4]2-) containing alkali metals
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G45/00—Compounds of manganese
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Description
本明細書及び特許請求の範囲に用いられた用語や単語は、通常的且つ辞書的な意味に限定して解釈されてはならず、発明者は自分の発明を最良の方法で説明するために用語の概念を適宜定義することができるとの原則に即して、本発明の技術的思想に符合する意味と概念に解釈されなければならない。
MnSO4及びAlSO4を(98:2)で混合した後、N2パージングを経た蒸溜水を用いて濃度が2MであるAlSO4を含むMnSO4・7H2Oを製造した。製造されたMnSO4・7H2Oを連続撹拌タンク反応器(CSTR、製造社:EMSTech、製品名:CSTR−L0)に250mL/hの速度で投入した。
実施例1
段階i):ナトリウム含有化合物がコーティングされた多結晶マンガン前駆体を得る段階
前記段階i)で得たナトリウム含有化合物がコーティングされた多結晶マンガン前駆体135g及びリチウム前駆体としてLi2CO337.50gを共にミキサー(Waring Blender)に入れて、前記ミキサーの中心部rpmが18000rpmで、1分間混合して前駆体混合物を得た。
Li2CO3 37.50g、製造例1で製造された5μmの平均粒径を有する(Mn0.95Al0.05)3O4141.88g、炭酸ナトリウム0.62gをミキサー(Waring Blender)に入れて、前記ミキサーの中心部rpmが18000rpmで、1分間混合した。前記混合された粉末を500ccのアルミナるつぼに入れて約700℃で4時間の間大気(Air)雰囲気で焼成を行った。焼成後に得たケーキ(cake)を乳ばちで粉砕した後、400メッシュ篩(sieve)を用いて分級を行って表面にNa2Oを含むコーティング層を含むLi(1.09)Mn1.81Al0.1O4を得た。
実施例1の段階i)を行わず、段階ii)でナトリウム含有化合物がコーティングされた多結晶マンガン前駆体を用いる代わりに、コーティングされない多結晶マンガン前駆体を用いたことを除き、前記実施例1と同一の方法で行って、Li(1.09)Mn1.81Al0.1O4を得た。
マンガン前駆体として製造例1で製造された多結晶(Mn0.95Al0.05)3O4を用いる代わりに単結晶Mn3O4を用いたことを除いては、前記実施例1と同一の方法で行い、Na2Oを含むコーティング層を含むLiMn2O4を得た。
実施例3
正極の製造
前記実施例1で製造された正極活物質94重量%、導電剤としてカーボンブラック(carbon black)3重量%、バインダとしてポリビニリデンフルオライド(PVdF)3重量%を、溶媒であるN−メチル−2−ピロリドン(NMP)に添加して正極混合物スラリーを製造した。前記正極混合物スラリーを厚さが20μm程度の正極集電体であるアルミニウム(Al)薄膜に塗布し、乾燥して正極を製造した後、ロールプレス(roll press)を行って正極を製造した。
負極活物質として炭素粉末96.3重量%、導電剤としてsuper−p1.0重量%及びバインダとしてスチレンブタジエンゴム(SBR)及びカルボキシメチルセルロース(CMC)を1.5重量%と1.2重量%を混合し、溶媒であるNMPに添加して負極活物質スラリーを製造した。前記負極活物質スラリーを厚さが10umの負極集電体である銅(Cu)薄膜に塗布し、乾燥して負極を製造した後、ロールプレス(roll press)を行って負極を製造した。
一方、電解質としてエチレンカーボネート及びジエチルカーボネートを30:70の体積比で混合して製造された非水電解液溶媒にLiPF6を添加して、1MのLiPF6非水性電解液を製造した。
このように製造された正極と負極をポリエチレンとポリプロピレンの混合セパレータを介在させた後、通常の方法でポリマー型電池を製作した後、製造された前記非水性電解液を注液してリチウム二次電池の製造を完成した。
前記実施例2で製造された正極活物質を用いたことを除いては、実施例3と同一の方法でリチウム二次電池を製造した。
前記比較例1及び2で製造された正極活物質を用いたことを除いては、実施例3と同一の方法でリチウム二次電池を製造した。
前記実施例1と2、及び比較例1と2で製造された正極活物質に対して、それぞれSEM顕微鏡写真を確認し、その結果をそれぞれ図2から5に示した。
実施例1と2、及び比較例1と2で製造された多結晶リチウムマンガン酸化物粒子に対してX線回折分析を行った。その結果を下記表1で示した。
実施例3と4、及び比較例3と4で製造されたリチウム二次電池を定電流/定電圧(CC/CV)条件で、(電池容量3.4mAh)を2Cの定電流(CC)で充電し、その後、定電圧(CV)で充電して充電電流が0.17mAhになるまで1回目の充電を行った。その後20分間放置した後、0.1Cの定電流で10mVになるまで放電して1サイクル目の放電容量を測定した。次いで、各電池に対して前記充電及び放電を繰り返して行って容量を測定し、これを下記表2で示した。
タップ密度は、実施例1、及び比較例1と2で得た正極活物質を容器に充填した後、一定の条件で振動させて得られる粒子の見掛け密度を測定したものである。
実施例1と2、及び比較例1の正極活物質の結晶の大きさを測定した。
Claims (26)
- 多結晶リチウムマンガン酸化物;及び
前記多結晶リチウムマンガン酸化物の表面に酸化ナトリウム含有コーティング層を含み、
前記多結晶リチウムマンガン酸化物は、X線回折分析測定時に結晶の平均粒径が152nmから300nm範囲に含まれる二つ以上の一次粒子が凝集された二次粒子の形態であり、
前記多結晶リチウムマンガン酸化物は、下記化学式(1)で表される正極活物質:
- 前記酸化ナトリウムはNa2Oを含む請求項1に記載の正極活物質。
- 前記酸化ナトリウム含有コーティング層の厚さは、1nmから500nmの範囲である請求項1または請求項2に記載の正極活物質。
- 前記二次粒子の平均粒径D50は、3μmから20μmの範囲である請求項1に記載の正極活物質。
- 前記正極活物質のタップ密度は、1.7g/ccから2.5g/ccの範囲である請求項1から請求項4の何れか一項に記載の正極活物質。
- 前記正極活物質は、X線回折分析(X−ray diffraction)測定時にI(111)/I(111)ピーク強度比を100%と定義する場合、I(311)/I(111)が40%以上である請求項1に記載の正極活物質。
- 前記正極活物質は、X線回折分析(X−ray diffraction)測定時にI(111)/I(111)ピーク強度比を100%と定義する場合、I(400)/I(111)が40%以上であり、I(440)/I(111)が20%以上である請求項1または請求項6に記載の正極活物質。
- 前記正極活物質は、X線回折分析(X−ray diffraction)測定時に、(311)ピークの半値幅(Full Width at Half−Maximum;FWHM)が0.3度以下である請求項1、請求項6、または請求項7に記載の正極活物質。
- 前記正極活物質の比表面積(BET)は、0.1m2/gから1.0m2/gの範囲である請求項1から請求項8の何れか一項に記載の正極活物質。
- 前記リチウムマンガン酸化物の内部にナトリウム含有酸化物の一部のNa元素がドーピングされ、前記Na元素の含量は前記リチウムマンガン酸化物の表面から内部に行くほど減少する濃度勾配を有する請求項1から請求項9の何れか一項に記載の正極活物質。
- (i)多結晶マンガン前駆体及びナトリウム前駆体を混合して熱処理し、前記多結晶マンガン前駆体の表面をナトリウム含有化合物でコーティングさせる段階;及び
(ii)前記ナトリウム含有化合物がコーティングされた前記多結晶マンガン前駆体及びリチウム前駆体を混合した後、焼成して多結晶リチウムマンガン酸化物の表面にナトリウム含有コーティング層を形成する段階
を含む請求項1から請求項10の何れか一項に記載の正極活物質の製造方法。 - 多結晶マンガン前駆体、ナトリウム前駆体及びリチウム前駆体を混合して焼成する段階を含む請求項1から請求項11の何れか一項に記載の正極活物質の製造方法。
- 前記熱処理前に固液分離工程を行う段階をさらに含む請求項11に記載の正極活物質の製造方法。
- 前記固液分離工程は、遠心分離、フィルタプレス、フィルタドライ及びスプレードライ方法のうち選択された一つ以上の方法によって行われる請求項13に記載の正極活物質の製造方法。
- 前記多結晶マンガン前駆体は、X線回折分析測定時に結晶の平均粒径が100nmから300nm範囲に含まれる二つ以上の一次粒子が凝集されて形成された二次粒子の形態である請求項11から請求項14の何れか一項に記載の正極活物質の製造方法。
- 前記多結晶マンガン前駆体は、Alを0.01重量%から10重量%で含む請求項11から請求項15の何れか一項に記載の正極活物質の製造方法。
- 前記多結晶マンガン前駆体は、(Mn(1−y)Aly)3O4(0<y≦0.2)を含む請求項15および請求項16に記載の正極活物質の製造方法。
- 前記多結晶マンガン前駆体は、MnO2、MnCl2、MnCO3、Mn3O4、MnSO4及びMn2O3からなる群より選択されたいずれか一つ、またはこれらのうち2種以上の混合物をアルミニウム化合物とともに共沈させて形成されたものである請求項17に記載の正極活物質の製造方法。
-
前記アルミニウム化合物は、AlSO4、AlCl及びAlNO3からなる群より選択されたいずれか一つ、またはこれらのうち2種以上の混合物である請求項18に記載の正極活物質の製造方法。 - 前記ナトリウム前駆体は、炭酸ナトリウム、珪酸ナトリウム、水酸化ナトリウム、またはこれらの2種以上の混合物である請求項11から請求項19の何れか一項に記載の正極活物質の製造方法。
- 前記ナトリウム前駆体は、前記多結晶マンガン前駆体の総重量対比0.01重量%から20重量%の量で用いられる請求項11から請求項20の何れか一項に記載の正極活物質の製造方法。
- 前記焼成は、600℃以上から900℃の温度範囲で行われる請求項11に記載の正極活物質の製造方法。
- 前記焼成は、600℃以上から800℃未満の温度範囲で行われる請求項22に記載の正極活物質の製造方法。
- 多結晶リチウムマンガン酸化物;及び
前記多結晶リチウムマンガン酸化物の表面に酸化ナトリウム含有コーティング層を含み、
前記多結晶リチウムマンガン酸化物は、X線回折分析測定時に結晶の平均粒径が152nmから300nm範囲に含まれる二つ以上の一次粒子が凝集された二次粒子の形態である正極活物質の製造方法であって、
(i)多結晶マンガン前駆体及びナトリウム前駆体を混合して熱処理し、前記多結晶マンガン前駆体の表面をナトリウム含有化合物でコーティングさせる段階;及び
(ii)前記ナトリウム含有化合物がコーティングされた前記多結晶マンガン前駆体及びリチウム前駆体を混合した後、焼成して多結晶リチウムマンガン酸化物の表面にナトリウム含有コーティング層を形成する段階
を含む正極活物質の製造方法。 - 請求項1から請求項10の何れか一項に記載の正極活物質を含む正極。
- 請求項25に記載の正極を含むリチウム二次電池。
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