KR101232836B1 - 리튬 이차 전지용 양극 활물질의 제조 방법, 상기 제조 방법에 따라 제조된 리튬 이차 전지용 양극 활물질, 및 이를 포함하는 리튬 이차 전지 - Google Patents
리튬 이차 전지용 양극 활물질의 제조 방법, 상기 제조 방법에 따라 제조된 리튬 이차 전지용 양극 활물질, 및 이를 포함하는 리튬 이차 전지 Download PDFInfo
- Publication number
- KR101232836B1 KR101232836B1 KR1020100090051A KR20100090051A KR101232836B1 KR 101232836 B1 KR101232836 B1 KR 101232836B1 KR 1020100090051 A KR1020100090051 A KR 1020100090051A KR 20100090051 A KR20100090051 A KR 20100090051A KR 101232836 B1 KR101232836 B1 KR 101232836B1
- Authority
- KR
- South Korea
- Prior art keywords
- active material
- lithium secondary
- secondary battery
- positive electrode
- source
- 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.)
- Expired - Fee Related
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- 229910052744 lithium Inorganic materials 0.000 title claims abstract description 296
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims abstract description 292
- 239000007774 positive electrode material Substances 0.000 title claims abstract description 101
- 238000000034 method Methods 0.000 title claims description 31
- 239000006182 cathode active material Substances 0.000 claims abstract description 122
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 59
- 239000002243 precursor Substances 0.000 claims abstract description 49
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 39
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 34
- 239000011572 manganese Substances 0.000 claims abstract description 31
- 238000004519 manufacturing process Methods 0.000 claims abstract description 29
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 24
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 claims abstract description 21
- 229910017052 cobalt Inorganic materials 0.000 claims abstract description 21
- 239000010941 cobalt Substances 0.000 claims abstract description 21
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims abstract description 21
- 229910052748 manganese Inorganic materials 0.000 claims abstract description 21
- 239000002904 solvent Substances 0.000 claims abstract description 21
- 239000011149 active material Substances 0.000 claims abstract description 20
- 238000002156 mixing Methods 0.000 claims abstract description 16
- 150000001875 compounds Chemical class 0.000 claims description 47
- 239000011164 primary particle Substances 0.000 claims description 33
- 229910052723 transition metal Inorganic materials 0.000 claims description 33
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 claims description 30
- 239000011148 porous material Substances 0.000 claims description 30
- 150000003624 transition metals Chemical class 0.000 claims description 25
- 239000000126 substance Substances 0.000 claims description 24
- 239000002245 particle Substances 0.000 claims description 20
- 238000010304 firing Methods 0.000 claims description 19
- 229910052596 spinel Inorganic materials 0.000 claims description 16
- 239000011029 spinel Substances 0.000 claims description 16
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 14
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 14
- 235000019422 polyvinyl alcohol Nutrition 0.000 claims description 14
- 239000003792 electrolyte Substances 0.000 claims description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 12
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 11
- 239000007773 negative electrode material Substances 0.000 claims description 11
- 229910052802 copper Inorganic materials 0.000 claims description 10
- 239000010949 copper Substances 0.000 claims description 10
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 10
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 10
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 10
- 239000011163 secondary particle Substances 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- IIPYXGDZVMZOAP-UHFFFAOYSA-N lithium nitrate Chemical compound [Li+].[O-][N+]([O-])=O IIPYXGDZVMZOAP-UHFFFAOYSA-N 0.000 claims description 8
- 229940099596 manganese sulfate Drugs 0.000 claims description 8
- 239000011702 manganese sulphate Substances 0.000 claims description 8
- 235000007079 manganese sulphate Nutrition 0.000 claims description 8
- SQQMAOCOWKFBNP-UHFFFAOYSA-L manganese(II) sulfate Chemical compound [Mn+2].[O-]S([O-])(=O)=O SQQMAOCOWKFBNP-UHFFFAOYSA-L 0.000 claims description 8
- 229920002125 Sokalan® Polymers 0.000 claims description 7
- 239000004584 polyacrylic acid Substances 0.000 claims description 7
- 229910052719 titanium Inorganic materials 0.000 claims description 7
- 229910052725 zinc Inorganic materials 0.000 claims description 7
- 229930006000 Sucrose Natural products 0.000 claims description 6
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 claims description 6
- 229910052804 chromium Inorganic materials 0.000 claims description 6
- 229910000361 cobalt sulfate Inorganic materials 0.000 claims description 6
- 229940044175 cobalt sulfate Drugs 0.000 claims description 6
- KTVIXTQDYHMGHF-UHFFFAOYSA-L cobalt(2+) sulfate Chemical compound [Co+2].[O-]S([O-])(=O)=O KTVIXTQDYHMGHF-UHFFFAOYSA-L 0.000 claims description 6
- 229910052750 molybdenum Inorganic materials 0.000 claims description 6
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 claims description 6
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 claims description 6
- 229910052758 niobium Inorganic materials 0.000 claims description 6
- 239000005720 sucrose Substances 0.000 claims description 6
- 229910052721 tungsten Inorganic materials 0.000 claims description 6
- 229910052720 vanadium Inorganic materials 0.000 claims description 6
- 229910052727 yttrium Inorganic materials 0.000 claims description 6
- 229910052726 zirconium Inorganic materials 0.000 claims description 6
- 229910052742 iron Inorganic materials 0.000 claims description 5
- 238000002360 preparation method Methods 0.000 claims description 5
- OORRCVPWRPVJEK-UHFFFAOYSA-N 2-oxidanylethanoic acid Chemical compound OCC(O)=O.OCC(O)=O OORRCVPWRPVJEK-UHFFFAOYSA-N 0.000 claims description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 4
- 208000006558 Dental Calculus Diseases 0.000 claims description 4
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims description 4
- 229910013553 LiNO Inorganic materials 0.000 claims description 4
- 229910021380 Manganese Chloride Inorganic materials 0.000 claims description 4
- GLFNIEUTAYBVOC-UHFFFAOYSA-L Manganese chloride Chemical compound Cl[Mn]Cl GLFNIEUTAYBVOC-UHFFFAOYSA-L 0.000 claims description 4
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 claims description 4
- 229910019142 PO4 Inorganic materials 0.000 claims description 4
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 claims description 4
- MQRWBMAEBQOWAF-UHFFFAOYSA-N acetic acid;nickel Chemical compound [Ni].CC(O)=O.CC(O)=O MQRWBMAEBQOWAF-UHFFFAOYSA-N 0.000 claims description 4
- 239000002253 acid Substances 0.000 claims description 4
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 claims description 4
- 229940011182 cobalt acetate Drugs 0.000 claims description 4
- GVPFVAHMJGGAJG-UHFFFAOYSA-L cobalt dichloride Chemical compound [Cl-].[Cl-].[Co+2] GVPFVAHMJGGAJG-UHFFFAOYSA-L 0.000 claims description 4
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 claims description 4
- 229910001981 cobalt nitrate Inorganic materials 0.000 claims description 4
- 229910000152 cobalt phosphate Inorganic materials 0.000 claims description 4
- ZBDSFTZNNQNSQM-UHFFFAOYSA-H cobalt(2+);diphosphate Chemical compound [Co+2].[Co+2].[Co+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O ZBDSFTZNNQNSQM-UHFFFAOYSA-H 0.000 claims description 4
- QAHREYKOYSIQPH-UHFFFAOYSA-L cobalt(II) acetate Chemical compound [Co+2].CC([O-])=O.CC([O-])=O QAHREYKOYSIQPH-UHFFFAOYSA-L 0.000 claims description 4
- GICLSALZHXCILJ-UHFFFAOYSA-N ctk5a5089 Chemical compound NCC(O)=O.NCC(O)=O GICLSALZHXCILJ-UHFFFAOYSA-N 0.000 claims description 4
- 239000008103 glucose Substances 0.000 claims description 4
- CPSYWNLKRDURMG-UHFFFAOYSA-L hydron;manganese(2+);phosphate Chemical compound [Mn+2].OP([O-])([O-])=O CPSYWNLKRDURMG-UHFFFAOYSA-L 0.000 claims description 4
- XIXADJRWDQXREU-UHFFFAOYSA-M lithium acetate Chemical compound [Li+].CC([O-])=O XIXADJRWDQXREU-UHFFFAOYSA-M 0.000 claims description 4
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 claims description 4
- 229940071125 manganese acetate Drugs 0.000 claims description 4
- 239000011565 manganese chloride Substances 0.000 claims description 4
- 235000002867 manganese chloride Nutrition 0.000 claims description 4
- 229940099607 manganese chloride Drugs 0.000 claims description 4
- 229940077478 manganese phosphate Drugs 0.000 claims description 4
- UOGMEBQRZBEZQT-UHFFFAOYSA-L manganese(2+);diacetate Chemical compound [Mn+2].CC([O-])=O.CC([O-])=O UOGMEBQRZBEZQT-UHFFFAOYSA-L 0.000 claims description 4
- MIVBAHRSNUNMPP-UHFFFAOYSA-N manganese(2+);dinitrate Chemical compound [Mn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MIVBAHRSNUNMPP-UHFFFAOYSA-N 0.000 claims description 4
- 229940078494 nickel acetate Drugs 0.000 claims description 4
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 claims description 4
- 229910000159 nickel phosphate Inorganic materials 0.000 claims description 4
- JOCJYBPHESYFOK-UHFFFAOYSA-K nickel(3+);phosphate Chemical compound [Ni+3].[O-]P([O-])([O-])=O JOCJYBPHESYFOK-UHFFFAOYSA-K 0.000 claims description 4
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 claims description 4
- XTQHKBHJIVJGKJ-UHFFFAOYSA-N sulfur monoxide Chemical compound S=O XTQHKBHJIVJGKJ-UHFFFAOYSA-N 0.000 claims description 4
- 239000011975 tartaric acid Substances 0.000 claims description 4
- 235000002906 tartaric acid Nutrition 0.000 claims description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 claims description 3
- TXKMVPPZCYKFAC-UHFFFAOYSA-N disulfur monoxide Inorganic materials O=S=S TXKMVPPZCYKFAC-UHFFFAOYSA-N 0.000 claims description 3
- 150000004767 nitrides Chemical class 0.000 claims description 3
- WNLRTRBMVRJNCN-UHFFFAOYSA-N adipic acid Chemical compound OC(=O)CCCCC(O)=O WNLRTRBMVRJNCN-UHFFFAOYSA-N 0.000 claims 2
- 239000001361 adipic acid Substances 0.000 claims 1
- 235000011037 adipic acid Nutrition 0.000 claims 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims 1
- 239000010452 phosphate Substances 0.000 claims 1
- 230000000052 comparative effect Effects 0.000 description 50
- -1 polytetrafluoroethylene Polymers 0.000 description 20
- 239000000243 solution Substances 0.000 description 11
- 239000004020 conductor Substances 0.000 description 10
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 9
- 229910001416 lithium ion Inorganic materials 0.000 description 9
- 229910052751 metal Inorganic materials 0.000 description 9
- 239000002184 metal Substances 0.000 description 9
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- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- 239000011230 binding agent Substances 0.000 description 6
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- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 5
- 239000002033 PVDF binder Substances 0.000 description 5
- 230000008859 change Effects 0.000 description 5
- 229940053662 nickel sulfate Drugs 0.000 description 5
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 5
- 239000010936 titanium Substances 0.000 description 5
- 229910052782 aluminium Inorganic materials 0.000 description 4
- 229910021383 artificial graphite Inorganic materials 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- 230000014759 maintenance of location Effects 0.000 description 4
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- 229920000642 polymer Polymers 0.000 description 4
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- 229920003048 styrene butadiene rubber Polymers 0.000 description 4
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- 229910015643 LiMn 2 O 4 Inorganic materials 0.000 description 3
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 3
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- 238000003780 insertion Methods 0.000 description 3
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- YEJRWHAVMIAJKC-UHFFFAOYSA-N 4-Butyrolactone Chemical compound O=C1CCCO1 YEJRWHAVMIAJKC-UHFFFAOYSA-N 0.000 description 2
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- 229920000049 Carbon (fiber) Polymers 0.000 description 2
- 229920002134 Carboxymethyl cellulose Polymers 0.000 description 2
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- 229910013870 LiPF 6 Inorganic materials 0.000 description 2
- 229910012513 LiSbF 6 Inorganic materials 0.000 description 2
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- 238000004220 aggregation Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 229910052783 alkali metal Inorganic materials 0.000 description 2
- 150000001340 alkali metals Chemical class 0.000 description 2
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 2
- 150000001342 alkaline earth metals Chemical class 0.000 description 2
- 235000011114 ammonium hydroxide Nutrition 0.000 description 2
- 229910003481 amorphous carbon Inorganic materials 0.000 description 2
- 229910052795 boron group element Inorganic materials 0.000 description 2
- 229910052791 calcium Inorganic materials 0.000 description 2
- 239000004917 carbon fiber Substances 0.000 description 2
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- 239000001768 carboxy methyl cellulose Substances 0.000 description 2
- 235000010948 carboxy methyl cellulose Nutrition 0.000 description 2
- 239000008112 carboxymethyl-cellulose Substances 0.000 description 2
- 150000005678 chain carbonates Chemical class 0.000 description 2
- 238000000975 co-precipitation Methods 0.000 description 2
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- 239000012153 distilled water Substances 0.000 description 2
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- 239000012535 impurity Substances 0.000 description 2
- 229910052738 indium Inorganic materials 0.000 description 2
- 238000009830 intercalation Methods 0.000 description 2
- 229910052745 lead Inorganic materials 0.000 description 2
- 150000002641 lithium Chemical class 0.000 description 2
- KWGKDLIKAYFUFQ-UHFFFAOYSA-M lithium chloride Chemical compound [Li+].[Cl-] KWGKDLIKAYFUFQ-UHFFFAOYSA-M 0.000 description 2
- 229910003002 lithium salt Inorganic materials 0.000 description 2
- 159000000002 lithium salts Chemical class 0.000 description 2
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- XBDQKXXYIPTUBI-UHFFFAOYSA-M Propionate Chemical compound CCC([O-])=O XBDQKXXYIPTUBI-UHFFFAOYSA-M 0.000 description 1
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- RLTFLELMPUMVEH-UHFFFAOYSA-N [Li+].[O--].[O--].[O--].[V+5] Chemical compound [Li+].[O--].[O--].[O--].[V+5] RLTFLELMPUMVEH-UHFFFAOYSA-N 0.000 description 1
- XHCLAFWTIXFWPH-UHFFFAOYSA-N [O-2].[O-2].[O-2].[O-2].[O-2].[V+5].[V+5] Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[V+5].[V+5] XHCLAFWTIXFWPH-UHFFFAOYSA-N 0.000 description 1
- 150000001242 acetic acid derivatives Chemical class 0.000 description 1
- KXKVLQRXCPHEJC-UHFFFAOYSA-N acetic acid trimethyl ester Natural products COC(C)=O KXKVLQRXCPHEJC-UHFFFAOYSA-N 0.000 description 1
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- 239000007864 aqueous solution Substances 0.000 description 1
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- 229910052792 caesium Inorganic materials 0.000 description 1
- MYWGVEGHKGKUMM-UHFFFAOYSA-N carbonic acid;ethene Chemical compound C=C.C=C.OC(O)=O MYWGVEGHKGKUMM-UHFFFAOYSA-N 0.000 description 1
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- 238000000151 deposition Methods 0.000 description 1
- 229920005994 diacetyl cellulose Polymers 0.000 description 1
- IEJIGPNLZYLLBP-UHFFFAOYSA-N dimethyl carbonate Chemical compound COC(=O)OC IEJIGPNLZYLLBP-UHFFFAOYSA-N 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 150000002170 ethers Chemical class 0.000 description 1
- JBTWLSYIZRCDFO-UHFFFAOYSA-N ethyl methyl carbonate Chemical compound CCOC(=O)OC JBTWLSYIZRCDFO-UHFFFAOYSA-N 0.000 description 1
- 238000000445 field-emission scanning electron microscopy Methods 0.000 description 1
- 239000011326 fired coke Substances 0.000 description 1
- 229910052730 francium Inorganic materials 0.000 description 1
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- HSZCZNFXUDYRKD-UHFFFAOYSA-M lithium iodide Inorganic materials [Li+].[I-] HSZCZNFXUDYRKD-UHFFFAOYSA-M 0.000 description 1
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- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
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- YKYONYBAUNKHLG-UHFFFAOYSA-N n-Propyl acetate Natural products CCCOC(C)=O YKYONYBAUNKHLG-UHFFFAOYSA-N 0.000 description 1
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- 239000005486 organic electrolyte Substances 0.000 description 1
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- 230000001590 oxidative effect Effects 0.000 description 1
- 239000003002 pH adjusting agent Substances 0.000 description 1
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- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 229910052699 polonium Inorganic materials 0.000 description 1
- 229920002239 polyacrylonitrile Polymers 0.000 description 1
- 229920000307 polymer substrate Polymers 0.000 description 1
- 229920000973 polyvinylchloride carboxylated Polymers 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 229940090181 propyl acetate Drugs 0.000 description 1
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 1
- RUOJZAUFBMNUDX-UHFFFAOYSA-N propylene carbonate Chemical compound CC1COC(=O)O1 RUOJZAUFBMNUDX-UHFFFAOYSA-N 0.000 description 1
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 229910052703 rhodium Inorganic materials 0.000 description 1
- 229910052701 rubidium Inorganic materials 0.000 description 1
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- 229910021481 rutherfordium Inorganic materials 0.000 description 1
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- 238000001878 scanning electron micrograph Methods 0.000 description 1
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- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
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- 229910052714 tellurium Inorganic materials 0.000 description 1
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- NQPDZGIKBAWPEJ-UHFFFAOYSA-N valeric acid Chemical compound CCCCC(O)=O NQPDZGIKBAWPEJ-UHFFFAOYSA-N 0.000 description 1
- 229910001935 vanadium oxide Inorganic materials 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
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Abstract
Description
도 2는 실시예 1의 리튬 이차 전지용 양극 활물질에 대한 SEM 사진이다.
도 3은 비교예 1의 리튬 이차 전지용 양극 활물질에 대한 SEM 사진이다.
도 4는 실시예 2의 리튬 이차 전지용 양극 활물질에 대한 SEM 사진이다.
도 5는 비교예 2의 리튬 이차 전지용 양극 활물질에 대한 SEM 사진이다.
도 6은 실시예 3 및 비교예 3에서 제조한 리튬 이차 전지의 사이클 수명 특성을 나타낸 그래프이다.
도 7은 실시예 4 및 비교예 4에서 제조한 리튬 이차 전지의 사이클 수명 특성을 나타낸 그래프이다.
114: 양극, 113: 세퍼레이터,
120: 전지 용기, 140: 봉입 부재
Claims (32)
- 니켈 공급원, 코발트 공급원 및 망간 공급원 중 적어도 하나, 탄소 공급원, 그리고 용매를 혼합하여 리튬 이차 전지용 양극 활물질 전구체를 형성하는 단계; 및 상기 리튬 이차 전지용 활물질 전구체와 리튬 공급원을 혼합하고 열처리하는 단계를 포함하는 리튬 이차 전지용 양극 활물질의 제조 방법으로서, 상기 리튬 이차 전지용 활물질 전구체와 상기 리튬 공급원은 1.0:0.95 내지 1.0:1.25의 몰비로 혼합되고, 상기 리튬 이차 전지용 양극 활물질은 하기 화학식 1로 표시되는 층상 구조의 화합물을 포함하는 것인 리튬 이차 전지용 양극 활물질의 제조 방법:
[화학식 1]
Li1+x[NiaCobMcMnd]1-xO2-yFy
상기 화학식 1에서,
M은 전이금속 원소이고,
-0.05≤x≤0.25이고,
0≤y≤0.05이고,
0.2≤a≤0.9이고, 0≤b≤0.5이고, 0≤c≤0.05이고, 0.1≤d≤0.9이고, a+b+c+d=1임. - 니켈 공급원, 코발트 공급원 및 망간 공급원 중 적어도 하나, 탄소 공급원, 그리고 용매를 혼합하여 리튬 이차 전지용 양극 활물질 전구체를 형성하는 단계; 및 상기 리튬 이차 전지용 활물질 전구체와 리튬 공급원을 혼합하고 열처리하는 단계를 포함하는 리튬 이차 전지용 양극 활물질의 제조 방법으로서, 상기 리튬 이차 전지용 활물질 전구체와 상기 리튬 공급원은 1.0:0.4 내지 1.0:0.6의 몰비로 혼합되고,
상기 리튬 이차 전지용 양극 활물질은 하기 화학식 2로 표시되는 스피넬 구조의 화합물을 포함하는 것인 리튬 이차 전지용 양극 활물질의 제조 방법:
[화학식 2]
Li1+x[NiaCobMcMnd]2-xO4-yFy
상기 화학식 2에서,
M은 전이금속 원소이고,
0≤x≤0.1이고,
0≤y≤0.2이고,
0≤a≤0.3이고, 0≤b≤0.2이고, 0≤c≤0.15이고, 0≤d≤1.0이고, a+b+c+d=1임. - 제1항 또는 제2항에 있어서,
상기 니켈 공급원은 황산 니켈, 질산 니켈, 아세트산 니켈, 염화 니켈, 인산 니켈 또는 이들의 조합을 포함하는 것인 리튬 이차 전지용 양극 활물질의 제조 방법. - 제1항 또는 제2항에 있어서,
상기 코발트 공급원은 황산 코발트, 질산 코발트, 아세트산 코발트, 염화 코발트, 인산 코발트 또는 이들의 조합을 포함하는 것인 리튬 이차 전지용 양극 활물질의 제조 방법. - 제1항 또는 제2항에 있어서,
상기 망간 공급원은 황산 망간, 질산 망간, 아세트산 망간, 염화 망간, 인산 망간 또는 이들의 조합을 포함하는 것인 리튬 이차 전지용 양극 활물질의 제조 방법. - 제1항 또는 제2항에 있어서,
상기 탄소 공급원은 수크로오스(sucrose), 글루코오스(glucose), 폴리비닐알코올(polyvinyl alcohol, PVA), 폴리비닐피롤리돈(polyvinyl pyrrolidone, PVP), 콜로이드 탄소(colloidal carbon), 시트르산(citric acid), 타타르산(tartaric acid), 글리콜산(glycolic acid), 폴리아크릴산(polyacrylic acid), 아디프산(adipic acid), 글리신(glycine) 또는 이들의 조합을 포함하는 것인 리튬 이차 전지용 양극 활물질의 제조 방법. - 제1항 또는 제2항에 있어서,
상기 용매는 물, 에탄올, 메탄올 또는 이들의 조합을 포함하는 것인 리튬 이차 전지용 양극 활물질의 제조 방법. - 제1항 또는 제2항에 있어서,
상기 리튬 이차 전지용 양극 활물질 전구체를 형성하는 단계에서, 상기 니켈 공급원을 0 중량% 내지 75 중량%, 상기 코발트 공급원을 0 중량% 내지 40 중량%, 상기 망간 공급원을 0 중량% 내지 95 중량%, 상기 탄소 공급원을 2 중량% 내지 40 중량%, 및 상기 용매를 잔부로 혼합시키되, 상기 니켈 공급원의 양, 상기 코발트 공급원의 양, 및 상기 망간 공급원의 양의 합을 100 중량부로 하는 경우, 탄소 공급원은 5 내지 30 중량부로 포함되는 것인 리튬 이차 전지용 양극 활물질의 제조 방법.
- 제1항 또는 제2항에 있어서,
상기 리튬 이차 전지용 양극 활물질 전구체를 형성하는 단계에서, 전이금속 공급원을 더 혼합하는 것인 리튬 이차 전지용 양극 활물질의 제조 방법.
- 제9항에 있어서,
상기 전이금속 공급원은 전이금속의 황산화물, 전이금속의 질산화물, 전이금속의 아세트산화물, 전이금속의 염화물, 전이금속의 인산화물 또는 이들의 조합을 포함하는 것인 리튬 이차 전지용 양극 활물질의 제조 방법.
- 제1항 또는 제2항에 있어서,
상기 리튬 공급원은 리튬 나이트레이트(LiNO3), 리튬 아세테이트(CH3COOLi), 리튬 카보네이트(Li2CO3), 리튬 하이드록사이드(LiOH) 또는 이들의 조합을 포함하는 것인 리튬 이차 전지용 양극 활물질의 제조 방법.
- 삭제
- 삭제
- 제1항에 있어서,
상기 M은 Ti, V, Cr, Fe, Cu, Zn, Y, Zr, Nb, Mo, W 또는 이들의 조합을 포함하는 것인 리튬 이차 전지용 양극 활물질의 제조 방법.
- 삭제
- 삭제
- 제2항에 있어서,
상기 M은 Ti, V, Cr, Fe, Cu, Zn, Y, Zr, Nb, Mo, W 또는 이들의 조합을 포함하는 것인 리튬 이차 전지용 양극 활물질의 제조 방법.
- 제1항 또는 제2항에 있어서,
상기 열처리하는 단계는 250℃ 내지 650℃의 온도에서 수행하는 예비 소성 단계 및 700℃ 내지 1000℃의 온도에서 수행하는 소성 단계를 포함하는 것인 리튬 이차 전지용 양극 활물질의 제조 방법.
- 삭제
- 제1항의 방법에 따라 제조된 리튬 이차 전지용 양극 활물질.
- 제20항에 있어서,
상기 리튬 이차 전지용 양극 활물질은 복수 개의 1차 입자가 모여 2차 입자를 형성하고 있는 것인 리튬 이차 전지용 양극 활물질.
- 제21항에 있어서,
상기 1차 입자는 1 nm 내지 500 nm의 평균 입자 직경을 가지는 것인 리튬 이차 전지용 양극 활물질.
- 제20항에 있어서,
상기 리튬 이차 전지용 양극 활물질은 1.5 g/cc 내지 3.0 g/cc의 탭밀도를 가지는 것인 리튬 이차 전지용 양극 활물질.
- 제20항에 있어서,
상기 리튬 이차 전지용 양극 활물질은 1.0 m2/g 내지 10.0 m2/g의 비표면적을 가지는 것인 리튬 이차 전지용 양극 활물질.
- 제20항에 있어서,
상기 리튬 이차 전지용 양극 활물질은 기공을 포함하며, 상기 기공은 1 nm 내지 50 nm의 평균 직경을 가지는 것인 리튬 이차 전지용 양극 활물질.
- 제2항의 방법에 따라 제조된 리튬 이차 전지용 양극 활물질.
- 제26항에 있어서,
상기 리튬 이차 전지용 양극 활물질은 복수 개의 1차 입자가 모여 2차 입자를 형성하고 있는 것인 리튬 이차 전지용 양극 활물질.
- 제27항에 있어서,
상기 1차 입자는 1 nm 내지 1000 nm의 평균 입자 직경을 가지는 것인 리튬 이차 전지용 양극 활물질.
- 제26항에 있어서,
상기 리튬 이차 전지용 양극 활물질은 1.5 g/cc 내지 3.0 g/cc의 탭밀도를 가지는 것인 리튬 이차 전지용 양극 활물질.
- 제26항에 있어서,
상기 리튬 이차 전지용 양극 활물질은 1.0 m2/g 내지 10.0 m2/g의 비표면적을 가지는 것인 리튬 이차 전지용 양극 활물질.
- 제26항에 있어서,
상기 리튬 이차 전지용 양극 활물질은 기공을 포함하며, 상기 기공은 1 nm 내지 50 nm의 평균 직경을 가지는 것인 리튬 이차 전지용 양극 활물질.
- 양극 활물질을 포함하는 양극;
음극 활물질을 포함하는 음극; 및
전해질을 포함하고,
상기 양극 활물질은 제20항 또는 제26항의 리튬 이차 전지용 양극 활물질인 것인 리튬 이차 전지.
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PCT/KR2011/006779 WO2012036463A2 (ko) | 2010-09-14 | 2011-09-14 | 리튬 이차 전지용 양극 활물질의 제조 방법, 상기 제조 방법에 따라 제조된 리튬 이차 전지용 양극 활물질, 및 이를 포함하는 리튬 이차 전지 |
US13/822,892 US20130266868A1 (en) | 2010-09-14 | 2011-09-14 | Method of preparing positive active material for rechargeable lithium battery, positive active material for rechargeable lithium battery prepared by using the method, and rechargeable lithium battery including the same |
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KR101407606B1 (ko) * | 2011-12-28 | 2014-06-16 | 세진이노테크(주) | 리튬 이차 전지용 양극 활물질의 제조방법, 이로부터 제조된 양극 활물질 및 이를 포함하는 리튬 이차 전지 |
KR101497909B1 (ko) * | 2012-05-04 | 2015-03-03 | 주식회사 엘지화학 | 리튬 복합 전이금속 산화물 제조용 전구체 및 그 제조방법 |
KR101541347B1 (ko) * | 2012-07-09 | 2015-08-04 | 주식회사 엘지화학 | 양극 활물질 및 이를 포함하는 리튬 이차전지 |
KR102273779B1 (ko) | 2014-04-04 | 2021-07-06 | 삼성에스디아이 주식회사 | 복합양극활물질 제조방법, 복합양극활물질 및 이를 채용한 양극과 리튬전지 |
KR101678410B1 (ko) | 2014-05-08 | 2016-11-23 | 한국화학연구원 | 리튬 이차전지용 전극 및 이의 제조방법 |
KR101702405B1 (ko) * | 2015-03-23 | 2017-02-03 | 울산과학기술원 | 이차 전지용 양극 활물질, 이의 제조 방법, 및 이를 포함하는 이차 전지 |
CN107431201B (zh) | 2015-07-23 | 2021-06-01 | 松下知识产权经营株式会社 | 正极活性物质和电池 |
JP6846628B2 (ja) | 2015-09-16 | 2021-03-24 | パナソニックIpマネジメント株式会社 | 正極活物質、および、電池 |
WO2017047017A1 (ja) * | 2015-09-16 | 2017-03-23 | パナソニックIpマネジメント株式会社 | 正極活物質、および、電池 |
JP6861399B2 (ja) | 2015-09-16 | 2021-04-21 | パナソニックIpマネジメント株式会社 | 電池 |
WO2017047019A1 (ja) | 2015-09-16 | 2017-03-23 | パナソニックIpマネジメント株式会社 | 電池 |
JP6846627B2 (ja) | 2015-09-16 | 2021-03-24 | パナソニックIpマネジメント株式会社 | 正極活物質、および、電池 |
WO2017047018A1 (ja) | 2015-09-16 | 2017-03-23 | パナソニックIpマネジメント株式会社 | 電池 |
WO2017047023A1 (ja) | 2015-09-16 | 2017-03-23 | パナソニックIpマネジメント株式会社 | 電池 |
CN107408737B (zh) | 2015-09-16 | 2021-03-23 | 松下知识产权经营株式会社 | 电池 |
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WO2018092359A1 (ja) | 2016-11-15 | 2018-05-24 | パナソニックIpマネジメント株式会社 | 電池用正極活物質、および、電池 |
JP6979586B2 (ja) | 2016-11-15 | 2021-12-15 | パナソニックIpマネジメント株式会社 | 電池用正極活物質、および、電池用正極活物質を用いた電池 |
JP6964246B2 (ja) | 2016-12-02 | 2021-11-10 | パナソニックIpマネジメント株式会社 | 正極活物質、および、正極活物質を用いた電池 |
JP7065341B2 (ja) | 2017-01-19 | 2022-05-12 | パナソニックIpマネジメント株式会社 | 正極活物質、および、電池 |
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