JP7460250B2 - リチウム二次電池用正極活物質及びこの製造方法 - Google Patents
リチウム二次電池用正極活物質及びこの製造方法 Download PDFInfo
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- JP7460250B2 JP7460250B2 JP2022176534A JP2022176534A JP7460250B2 JP 7460250 B2 JP7460250 B2 JP 7460250B2 JP 2022176534 A JP2022176534 A JP 2022176534A JP 2022176534 A JP2022176534 A JP 2022176534A JP 7460250 B2 JP7460250 B2 JP 7460250B2
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- positive electrode
- active material
- electrode active
- lithium
- transition metal
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- 239000007774 positive electrode material Substances 0.000 title claims description 134
- 229910052744 lithium Inorganic materials 0.000 title claims description 90
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims description 87
- 238000004519 manufacturing process Methods 0.000 title claims description 20
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 136
- 239000002245 particle Substances 0.000 claims description 72
- 229910052759 nickel Inorganic materials 0.000 claims description 57
- 229910052723 transition metal Inorganic materials 0.000 claims description 47
- 150000003624 transition metals Chemical class 0.000 claims description 46
- 239000002243 precursor Substances 0.000 claims description 39
- 229910021437 lithium-transition metal oxide Inorganic materials 0.000 claims description 35
- 239000011572 manganese Substances 0.000 claims description 31
- 239000000203 mixture Substances 0.000 claims description 23
- 239000007864 aqueous solution Substances 0.000 claims description 20
- 229910052748 manganese Inorganic materials 0.000 claims description 18
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 claims description 16
- 229910052782 aluminium Inorganic materials 0.000 claims description 16
- 238000010304 firing Methods 0.000 claims description 16
- 229910052719 titanium Inorganic materials 0.000 claims description 16
- 229910017052 cobalt Inorganic materials 0.000 claims description 15
- 239000010941 cobalt Substances 0.000 claims description 15
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 15
- 239000000463 material Substances 0.000 claims description 13
- 229910052749 magnesium Inorganic materials 0.000 claims description 12
- 229910052726 zirconium Inorganic materials 0.000 claims description 12
- 239000000126 substance Substances 0.000 claims description 10
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- 230000000052 comparative effect Effects 0.000 description 41
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- 229910052712 strontium Inorganic materials 0.000 description 9
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- 229910000572 Lithium Nickel Cobalt Manganese Oxide (NCM) Inorganic materials 0.000 description 5
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- 229910003002 lithium salt Inorganic materials 0.000 description 5
- 159000000002 lithium salts Chemical class 0.000 description 5
- 238000001878 scanning electron micrograph Methods 0.000 description 5
- 238000007086 side reaction Methods 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 description 4
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- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 4
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- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 4
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
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- FBDMTTNVIIVBKI-UHFFFAOYSA-N [O-2].[Mn+2].[Co+2].[Ni+2].[Li+] Chemical compound [O-2].[Mn+2].[Co+2].[Ni+2].[Li+] FBDMTTNVIIVBKI-UHFFFAOYSA-N 0.000 description 2
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- SEVNKUSLDMZOTL-UHFFFAOYSA-H cobalt(2+);manganese(2+);nickel(2+);hexahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[Mn+2].[Co+2].[Ni+2] SEVNKUSLDMZOTL-UHFFFAOYSA-H 0.000 description 2
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- KLARSDUHONHPRF-UHFFFAOYSA-N [Li].[Mn] Chemical compound [Li].[Mn] KLARSDUHONHPRF-UHFFFAOYSA-N 0.000 description 1
- RTBHLGSMKCPLCQ-UHFFFAOYSA-N [Mn].OOO Chemical compound [Mn].OOO RTBHLGSMKCPLCQ-UHFFFAOYSA-N 0.000 description 1
- KFDQGLPGKXUTMZ-UHFFFAOYSA-N [Mn].[Co].[Ni] Chemical compound [Mn].[Co].[Ni] KFDQGLPGKXUTMZ-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
- KXKVLQRXCPHEJC-UHFFFAOYSA-N acetic acid trimethyl ester Natural products COC(C)=O KXKVLQRXCPHEJC-UHFFFAOYSA-N 0.000 description 1
- 239000011149 active material Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 239000005456 alcohol based solvent Substances 0.000 description 1
- 229910000272 alkali metal oxide Inorganic materials 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
- 229910001860 alkaline earth metal hydroxide Inorganic materials 0.000 description 1
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical compound [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 description 1
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 description 1
- 150000001408 amides Chemical class 0.000 description 1
- 235000019270 ammonium chloride Nutrition 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 150000003863 ammonium salts Chemical class 0.000 description 1
- 229910003481 amorphous carbon Inorganic materials 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 125000004429 atom Chemical group 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- INAHAJYZKVIDIZ-UHFFFAOYSA-N boron carbide Chemical compound B12B3B4C32B41 INAHAJYZKVIDIZ-UHFFFAOYSA-N 0.000 description 1
- YFSQMOVEGCCDJL-UHFFFAOYSA-N boron monofluoride Chemical compound F[B] YFSQMOVEGCCDJL-UHFFFAOYSA-N 0.000 description 1
- IAQRGUVFOMOMEM-UHFFFAOYSA-N butene Natural products CC=CC IAQRGUVFOMOMEM-UHFFFAOYSA-N 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 150000005678 chain carbonates Chemical class 0.000 description 1
- 239000011294 coal tar pitch Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- QGUAJWGNOXCYJF-UHFFFAOYSA-N cobalt dinitrate hexahydrate Chemical compound O.O.O.O.O.O.[Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O QGUAJWGNOXCYJF-UHFFFAOYSA-N 0.000 description 1
- CKFRRHLHAJZIIN-UHFFFAOYSA-N cobalt lithium Chemical compound [Li].[Co] CKFRRHLHAJZIIN-UHFFFAOYSA-N 0.000 description 1
- 229910000361 cobalt sulfate Inorganic materials 0.000 description 1
- 229940044175 cobalt sulfate Drugs 0.000 description 1
- 239000000571 coke Substances 0.000 description 1
- 239000008139 complexing agent Substances 0.000 description 1
- 229920001940 conductive polymer Polymers 0.000 description 1
- 238000012790 confirmation Methods 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 150000004292 cyclic ethers Chemical class 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 238000009831 deintercalation Methods 0.000 description 1
- 230000001687 destabilization Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 150000001993 dienes Chemical class 0.000 description 1
- 235000014113 dietary fatty acids Nutrition 0.000 description 1
- 150000004862 dioxolanes Chemical class 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000007580 dry-mixing Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000003487 electrochemical reaction Methods 0.000 description 1
- 239000008151 electrolyte solution Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000003759 ester based solvent Substances 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 229930195729 fatty acid Natural products 0.000 description 1
- 150000004665 fatty acids Chemical class 0.000 description 1
- 239000003365 glass fiber Substances 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 239000011357 graphitized carbon fiber Substances 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- 229910021385 hard carbon Inorganic materials 0.000 description 1
- 229920001519 homopolymer Polymers 0.000 description 1
- 150000002430 hydrocarbons Chemical group 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000003780 insertion Methods 0.000 description 1
- 230000037431 insertion Effects 0.000 description 1
- 238000009830 intercalation Methods 0.000 description 1
- 229910000765 intermetallic Inorganic materials 0.000 description 1
- 239000005453 ketone based solvent Substances 0.000 description 1
- XIXADJRWDQXREU-UHFFFAOYSA-M lithium acetate Chemical compound [Li+].CC([O-])=O XIXADJRWDQXREU-UHFFFAOYSA-M 0.000 description 1
- 229910052808 lithium carbonate Inorganic materials 0.000 description 1
- 229910001547 lithium hexafluoroantimonate(V) Inorganic materials 0.000 description 1
- 229910001540 lithium hexafluoroarsenate(V) Inorganic materials 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
- 229910001537 lithium tetrachloroaluminate Inorganic materials 0.000 description 1
- 229910001496 lithium tetrafluoroborate Inorganic materials 0.000 description 1
- 229910000686 lithium vanadium oxide Inorganic materials 0.000 description 1
- ACFSQHQYDZIPRL-UHFFFAOYSA-N lithium;bis(1,1,2,2,2-pentafluoroethylsulfonyl)azanide Chemical compound [Li+].FC(F)(F)C(F)(F)S(=O)(=O)[N-]S(=O)(=O)C(F)(F)C(F)(F)F ACFSQHQYDZIPRL-UHFFFAOYSA-N 0.000 description 1
- QSZMZKBZAYQGRS-UHFFFAOYSA-N lithium;bis(trifluoromethylsulfonyl)azanide Chemical compound [Li+].FC(F)(F)S(=O)(=O)[N-]S(=O)(=O)C(F)(F)F QSZMZKBZAYQGRS-UHFFFAOYSA-N 0.000 description 1
- 150000002696 manganese Chemical class 0.000 description 1
- 229940071125 manganese acetate Drugs 0.000 description 1
- 239000011656 manganese carbonate Substances 0.000 description 1
- 235000006748 manganese carbonate Nutrition 0.000 description 1
- 239000011565 manganese chloride Substances 0.000 description 1
- 235000002867 manganese chloride Nutrition 0.000 description 1
- 229940099607 manganese chloride Drugs 0.000 description 1
- 239000011564 manganese citrate Substances 0.000 description 1
- 235000014872 manganese citrate Nutrition 0.000 description 1
- 229940097206 manganese citrate Drugs 0.000 description 1
- 229940099596 manganese sulfate Drugs 0.000 description 1
- 239000011702 manganese sulphate Substances 0.000 description 1
- 235000007079 manganese sulphate Nutrition 0.000 description 1
- UOGMEBQRZBEZQT-UHFFFAOYSA-L manganese(2+);diacetate Chemical compound [Mn+2].CC([O-])=O.CC([O-])=O UOGMEBQRZBEZQT-UHFFFAOYSA-L 0.000 description 1
- PPNAOCWZXJOHFK-UHFFFAOYSA-N manganese(2+);oxygen(2-) Chemical class [O-2].[Mn+2] PPNAOCWZXJOHFK-UHFFFAOYSA-N 0.000 description 1
- 229910000016 manganese(II) carbonate Inorganic materials 0.000 description 1
- 229910000357 manganese(II) sulfate Inorganic materials 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 239000002931 mesocarbon microbead Substances 0.000 description 1
- 239000011302 mesophase pitch Substances 0.000 description 1
- 239000002905 metal composite material Substances 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 239000012046 mixed solvent Substances 0.000 description 1
- 230000003020 moisturizing effect Effects 0.000 description 1
- PYLWMHQQBFSUBP-UHFFFAOYSA-N monofluorobenzene Chemical compound FC1=CC=CC=C1 PYLWMHQQBFSUBP-UHFFFAOYSA-N 0.000 description 1
- 150000002815 nickel Chemical class 0.000 description 1
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 description 1
- 229940053662 nickel sulfate Drugs 0.000 description 1
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 description 1
- 150000002825 nitriles Chemical class 0.000 description 1
- 150000005181 nitrobenzenes Chemical class 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000011301 petroleum pitch Substances 0.000 description 1
- 239000011295 pitch Substances 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
- 229920000098 polyolefin Polymers 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 229920001384 propylene homopolymer Polymers 0.000 description 1
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 1
- 239000002296 pyrolytic carbon Substances 0.000 description 1
- 239000001008 quinone-imine dye Substances 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000002153 silicon-carbon composite material Substances 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 229910021384 soft carbon Inorganic materials 0.000 description 1
- 238000001694 spray drying Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- HXJUTPCZVOIRIF-UHFFFAOYSA-N sulfolane Chemical class O=S1(=O)CCCC1 HXJUTPCZVOIRIF-UHFFFAOYSA-N 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- TXEYQDLBPFQVAA-UHFFFAOYSA-N tetrafluoromethane Chemical compound FC(F)(F)F TXEYQDLBPFQVAA-UHFFFAOYSA-N 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
- 239000002733 tin-carbon composite material Substances 0.000 description 1
- BDZBKCUKTQZUTL-UHFFFAOYSA-N triethyl phosphite Chemical compound CCOP(OCC)OCC BDZBKCUKTQZUTL-UHFFFAOYSA-N 0.000 description 1
- 229910021642 ultra pure water Inorganic materials 0.000 description 1
- 239000012498 ultrapure water Substances 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
- 229910001935 vanadium oxide Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- PAPBSGBWRJIAAV-UHFFFAOYSA-N ε-Caprolactone Chemical compound O=C1CCCCCO1 PAPBSGBWRJIAAV-UHFFFAOYSA-N 0.000 description 1
Images
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- 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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- 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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-
- H—ELECTRICITY
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- 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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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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- 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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Description
本出願は、2018年11月20日付韓国特許出願第10-2018-0143804号及び2019年11月18日付韓国特許出願第10-2019-0147928号に基づく優先権の利益を主張し、当該韓国特許出願の文献に開示された全ての内容は本明細書の一部として含まれる。
従来では、リチウム二次電池の容量を高めるために、リチウムを除いた遷移金属の総モル数に対して60モル%以上のニッケルを含む高含量ニッケル含有正極活物質を用いた。しかし、この場合、正極活物質表面にリチウム副産物が過量生成されるに伴い二次電池のスウェリング現象が惹起され、また低い粒子強度により正極活物質の安定性が劣るという問題点があった。これを改善するために高含量ニッケル含有正極活物質を過焼成して単一粒子型正極活物質を製造する場合、安定性は改善されたが、高い焼成温度で焼成することにより、寿命特性及び抵抗特性の劣化などの問題点があった。
Li1+aNixCoyMnzM1 wO2
前記化学式1において、0≦a≦0.5、0.6≦x<1、0<y≦0.4、0<z≦0.4、0<w≦0.04、M1は、B、Zr、Mg、Ti、Sr、W及びAlからなる群から選択された少なくともいずれか一つ、さらに好ましくは0≦a≦0.5、0.8≦x<1、0<y≦0.2、0<z≦0.2、0<w≦0.01、M1はBである。
次に、本発明に係る正極活物質の製造方法に対して説明する。
次に、本発明に係る正極活物質を含む、リチウム二次電池用正極を提供する。
また、本発明は、前記正極を含む電気化学素子を製造することができる。前記電気化学素子は、具体的に電池、キャパシタなどであってよく、より具体的にはリチウム二次電池であってよい。
硫酸ニッケル、硫酸コバルト及び硫酸マンガンをニッケル:コバルト:マンガンのモル比が90:4:6となるようにする量でイオン交換水中に溶かして2.4Mの遷移金属水溶液を準備した。また、9%濃度のアンモニア水溶液と、25%濃度の水酸化ナトリウム水溶液をそれぞれ準備した。共沈反応器に前記遷移金属水溶液、アンモニア水溶液及び水酸化ナトリウム水溶液を一定速度で投入し、窒素雰囲気下で共沈反応を進めて、遷移金属水酸化物前駆体を合成した。
前記実施例1で製造した遷移金属水酸化物前駆体と、LiOHを混合して焼成するとき、焼成温度を830℃にすることを除き、前記実施例1と同様の方法を用いて正極活物質及びこれを含むリチウム二次電池を製造した。
前記実施例1で製造した正極活物質前駆体の全重量に対して1,000ppmのホウ酸を乾式混合した後、830℃で焼成して正極活物質(LiNi0.89Co0.04Mn0.06B0.009O2)を製造することを除き、前記実施例1と同様の方法を用いて正極活物質及びこれを含むリチウム二次電池を製造した。
遷移金属水酸化物前駆体の製造時、ホウ素をドーピングしないことを除き、前記実施例1と同様の方法を用いて正極活物質及びこれを含むリチウム二次電池を製造した。
遷移金属水酸化物前駆体の製造時、ホウ素をドーピングしないことを除き、前記実施例2と同様の方法を用いて正極活物質及びこれを含むリチウム二次電池を製造した。
前記比較例1で製造した遷移金属水酸化物前駆体と、LiOHを1:1.02のモル比で混合し、730℃で11時間焼成し、1次粒子等が凝集された2次粒子形態の正極活物質(LiNi0.90Co0.04Mn0.06O2)を製造し、これを使用したことを除き、前記比較例1と同様の方法を用いて正極活物質及びこれを含むリチウム二次電池を製造した。
前記実施例1で製造した遷移金属水酸化物前駆体と、LiOHを混合して焼成するとき、焼成温度を730℃にすることを除き、前記実施例1と同様の方法を用いて正極活物質及びこれを含むリチウム二次電池を製造した。
1)SEMイメージ
前記実施例1、比較例1及び3でそれぞれ製造した正極活物質の表面特性を確認するために走査電子顕微鏡を用いてSEMイメージを確認した。図1から図3に示すように、実施例1(図1)及び比較例1(図2)で製造した正極活物質は、単一粒子の形態を有することが確認できた。その反面、比較例3(図3)で製造した正極活物質は、1次粒子が凝集された2次粒子の形態であることが確認できた。
前記実施例1~3及び比較例1~4でそれぞれ製造したBドーピングされた正極活物質を簡易ミキサー(HMF600、ハンイルミキサー)を用いて4分間解砕し、レーザー回折粒度測定装置(例えば、Microtrac MT 3000)に導入して約28kHzの超音波を出力60Wで照射した後、測定装置における粒径による粒子個数累積分布の50%基準での平均粒子直径(D50)を算出し、これを下記表1に示した。また、前記実施例1~3及び比較例1~4で製造したBドーピングされた正極活物質を解砕し、3トンの圧力(3.1~3.2g/cm3)を加えて圧縮した後、前述した方法で測定した平均粒径(D50)もまた下記表1に示した。
実施例1~3及び比較例1~4でそれぞれ製造した正極活物質のペレット密度は、圧延密度測定器(4350、Carver社製)を用いて3.0トンの圧力時の内部体積を測定した。内部体積は、ノギス(Miltutoyo社製)を用いてSus内部の体積を測定し、この結果もまた下記表1に示した。
前記実施例1~3及び比較例3で製造した正極活物質をX線回折分析機(Bruker AXS D4-Endeavor XRD)を用いて、結晶子サイズを測定し、その結果を下記表2に示した。
前記実施例1~2及び比較例1~4で製造した正極活物質を用いてリチウム二次電池を製造し、実施例1~2及び比較例1~4の正極活物質を含むリチウム二次電池それぞれに対して容量特性を評価した。
前記実験例2でそれぞれ製造した実施例1~3及び比較例1~2によるリチウム二次電池それぞれに対して抵抗特性を評価した。
前記実験例2で製造した実施例1~2及び比較例3によるリチウム二次電池それぞれに対して60℃で4.5Vが維持されるように120時間充電しており、この際に発生する電流の量を測定し、これを図7に示した。
Claims (8)
- ニッケル(Ni)、コバルト(Co)及びマンガン(Mn)を含むリチウム遷移金属酸化物であり、
前記リチウム遷移金属酸化物のリチウムを除いた遷移金属の全モル数に対するニッケル(Ni)の含量が60モル%以上であり、
前記リチウム遷移金属酸化物がZr、Mg、Ti及びAlからなる群から選択された少なくともいずれか一つのドーピング元素でドーピングされ、
3.0g/cm3から3.3g/cm3の圧延密度で圧延という操作を行った時に平均粒径(D50)が4から10μmであるという性質を有し、単一粒子の形態を有する正極活物質。 - 前記リチウム遷移金属酸化物が下記化学式1で表され、
[化学式1]
Li1+aNixCoyMnzM1 wO2
前記化学式1において、0≦a≦0.5、0.6≦x<1、0<y≦0.4、0<z≦0.4、0<w≦0.01、M1は、Zr、Mg、Ti及びAlからなる群から選択された少なくともいずれか一つである、請求項1に記載の正極活物質。 - 前記リチウム遷移金属酸化物の結晶子サイズが170nmから220nmである、請求項1または2に記載の正極活物質。
- 前記ドーピング元素が前記リチウム遷移金属酸化物の全重量に対して100から4,000ppmで含まれる、請求項1から3のいずれか一項に記載の正極活物質。
- 請求項1に記載の正極活物質を製造するための製造方法であって、
ニッケル(Ni)、コバルト(Co)及びマンガン(Mn)を含む遷移金属水酸化物の全モル数に対して、ニッケル(Ni)を60モル%以上含む遷移金属水酸化物前駆体を準備する段階、
Zr、Mg、Ti及びAlからなる群から選択されたドーピング元素原料物質含有水溶液と前記遷移金属水酸化物前駆体を混合して乾燥させ混合物を形成する段階、及び
前記混合物にリチウム原料物質を混合し、810℃以上で焼成し、単一粒子形態のリチウム遷移金属酸化物を製造する段階、を含む、正極活物質の製造方法。 - 前記焼成が810℃から880℃で行われる、請求項5に記載の正極活物質の製造方法。
- 請求項1から4のいずれか一項に記載の正極活物質を含む、リチウム二次電池用正極。
- 請求項7に記載のリチウム二次電池用正極を含む、リチウム二次電池。
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