JP6342488B2 - リチウム複合遷移金属酸化物製造用前駆体、その製造方法及びそれを用いたリチウム複合遷移金属酸化物 - Google Patents
リチウム複合遷移金属酸化物製造用前駆体、その製造方法及びそれを用いたリチウム複合遷移金属酸化物 Download PDFInfo
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- JP6342488B2 JP6342488B2 JP2016527951A JP2016527951A JP6342488B2 JP 6342488 B2 JP6342488 B2 JP 6342488B2 JP 2016527951 A JP2016527951 A JP 2016527951A JP 2016527951 A JP2016527951 A JP 2016527951A JP 6342488 B2 JP6342488 B2 JP 6342488B2
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- transition metal
- metal precursor
- reducing agent
- lithium composite
- metal oxide
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- 238000004519 manufacturing process Methods 0.000 title claims description 15
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- 150000003624 transition metals Chemical class 0.000 claims description 83
- 150000001450 anions Chemical class 0.000 claims description 29
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- 238000000034 method Methods 0.000 claims description 13
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- 239000000463 material Substances 0.000 claims description 10
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- 229910052759 nickel Inorganic materials 0.000 claims description 9
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- 229910012345 LiSiO4-LiI—LiOH Inorganic materials 0.000 description 1
- 229910012348 LiSiO4—LiI—LiOH Inorganic materials 0.000 description 1
- 229910006555 Li—Co—Ni Inorganic materials 0.000 description 1
- KDXKERNSBIXSRK-UHFFFAOYSA-N Lysine Natural products NCCCCC(N)C(O)=O KDXKERNSBIXSRK-UHFFFAOYSA-N 0.000 description 1
- 239000004472 Lysine Substances 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- ZHGDJTMNXSOQDT-UHFFFAOYSA-N NP(N)(N)=O.NP(N)(N)=O.NP(N)(N)=O.NP(N)(N)=O.NP(N)(N)=O.NP(N)(N)=O Chemical compound NP(N)(N)=O.NP(N)(N)=O.NP(N)(N)=O.NP(N)(N)=O.NP(N)(N)=O.NP(N)(N)=O ZHGDJTMNXSOQDT-UHFFFAOYSA-N 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 1
- 229920000265 Polyparaphenylene Polymers 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 229910004283 SiO 4 Inorganic materials 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 229910006404 SnO 2 Inorganic materials 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical class C1CCOC1 WYURNTSHIVDZCO-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
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 description 1
- BEKPOUATRPPTLV-UHFFFAOYSA-N [Li].BCl Chemical compound [Li].BCl BEKPOUATRPPTLV-UHFFFAOYSA-N 0.000 description 1
- KFDQGLPGKXUTMZ-UHFFFAOYSA-N [Mn].[Co].[Ni] Chemical compound [Mn].[Co].[Ni] KFDQGLPGKXUTMZ-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
- 239000002253 acid Substances 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 description 1
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical compound [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 description 1
- 239000001099 ammonium carbonate Substances 0.000 description 1
- 235000012501 ammonium carbonate Nutrition 0.000 description 1
- 150000003863 ammonium salts Chemical class 0.000 description 1
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 description 1
- 229910052921 ammonium sulfate Inorganic materials 0.000 description 1
- 235000011130 ammonium sulphate Nutrition 0.000 description 1
- 229910021383 artificial graphite Inorganic materials 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000006231 channel black Substances 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 229910000428 cobalt oxide Inorganic materials 0.000 description 1
- 229910000361 cobalt sulfate Inorganic materials 0.000 description 1
- 229940044175 cobalt sulfate Drugs 0.000 description 1
- KTVIXTQDYHMGHF-UHFFFAOYSA-L cobalt(2+) sulfate Chemical compound [Co+2].[O-]S([O-])(=O)=O KTVIXTQDYHMGHF-UHFFFAOYSA-L 0.000 description 1
- IVMYJDGYRUAWML-UHFFFAOYSA-N cobalt(ii) oxide Chemical compound [Co]=O IVMYJDGYRUAWML-UHFFFAOYSA-N 0.000 description 1
- 230000000295 complement effect Effects 0.000 description 1
- 229920001940 conductive polymer Polymers 0.000 description 1
- 238000012790 confirmation Methods 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 239000011258 core-shell material Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 150000004292 cyclic ethers Chemical class 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- IEJIGPNLZYLLBP-UHFFFAOYSA-N dimethyl carbonate Chemical compound COC(=O)OC IEJIGPNLZYLLBP-UHFFFAOYSA-N 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 150000004862 dioxolanes Chemical class 0.000 description 1
- 238000010494 dissociation reaction Methods 0.000 description 1
- 230000005593 dissociations Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 229920001973 fluoroelastomer Polymers 0.000 description 1
- BLBBMBKUUHYSMI-UHFFFAOYSA-N furan-2,3,4,5-tetrol Chemical compound OC=1OC(O)=C(O)C=1O BLBBMBKUUHYSMI-UHFFFAOYSA-N 0.000 description 1
- 239000006232 furnace black Substances 0.000 description 1
- 229910052732 germanium Inorganic materials 0.000 description 1
- PVADDRMAFCOOPC-UHFFFAOYSA-N germanium monoxide Inorganic materials [Ge]=O PVADDRMAFCOOPC-UHFFFAOYSA-N 0.000 description 1
- 150000004820 halides Chemical class 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 239000001863 hydroxypropyl cellulose Substances 0.000 description 1
- 235000010977 hydroxypropyl cellulose Nutrition 0.000 description 1
- 150000003949 imides Chemical class 0.000 description 1
- 230000010220 ion permeability Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000003273 ketjen black Substances 0.000 description 1
- 239000006233 lamp black Substances 0.000 description 1
- 229910052745 lead Inorganic materials 0.000 description 1
- 239000011244 liquid electrolyte Substances 0.000 description 1
- 239000001989 lithium alloy Substances 0.000 description 1
- HSZCZNFXUDYRKD-UHFFFAOYSA-M lithium iodide Inorganic materials [Li+].[I-] HSZCZNFXUDYRKD-UHFFFAOYSA-M 0.000 description 1
- 229910002102 lithium manganese 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
- RSNHXDVSISOZOB-UHFFFAOYSA-N lithium nickel Chemical compound [Li].[Ni] RSNHXDVSISOZOB-UHFFFAOYSA-N 0.000 description 1
- FUJCRWPEOMXPAD-UHFFFAOYSA-N lithium oxide Chemical compound [Li+].[Li+].[O-2] FUJCRWPEOMXPAD-UHFFFAOYSA-N 0.000 description 1
- 229910001947 lithium oxide Inorganic materials 0.000 description 1
- 239000011656 manganese carbonate Substances 0.000 description 1
- 235000006748 manganese carbonate Nutrition 0.000 description 1
- 229940093474 manganese carbonate Drugs 0.000 description 1
- AMWRITDGCCNYAT-UHFFFAOYSA-L manganese oxide Inorganic materials [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 description 1
- MIVBAHRSNUNMPP-UHFFFAOYSA-N manganese(2+);dinitrate Chemical compound [Mn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MIVBAHRSNUNMPP-UHFFFAOYSA-N 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
- XMWCXZJXESXBBY-UHFFFAOYSA-L manganese(ii) carbonate Chemical compound [Mn+2].[O-]C([O-])=O XMWCXZJXESXBBY-UHFFFAOYSA-L 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 229940017219 methyl propionate Drugs 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910021382 natural graphite Inorganic materials 0.000 description 1
- 229910000480 nickel oxide Inorganic materials 0.000 description 1
- 229940053662 nickel sulfate Drugs 0.000 description 1
- 229910000008 nickel(II) carbonate Inorganic materials 0.000 description 1
- ZULUUIKRFGGGTL-UHFFFAOYSA-L nickel(ii) carbonate Chemical compound [Ni+2].[O-]C([O-])=O ZULUUIKRFGGGTL-UHFFFAOYSA-L 0.000 description 1
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 150000005181 nitrobenzenes Chemical class 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- LYGJENNIWJXYER-UHFFFAOYSA-N nitromethane Chemical compound C[N+]([O-])=O LYGJENNIWJXYER-UHFFFAOYSA-N 0.000 description 1
- 229910021470 non-graphitizable carbon Inorganic materials 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical class [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-N phosphoric acid Substances OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 229920001197 polyacetylene Polymers 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 229920001451 polypropylene glycol 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
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 229910000027 potassium carbonate Inorganic materials 0.000 description 1
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 1
- 239000001008 quinone-imine dye Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000004627 regenerated cellulose Substances 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 229910052596 spinel Inorganic materials 0.000 description 1
- 239000011029 spinel Substances 0.000 description 1
- 229920003048 styrene butadiene rubber Polymers 0.000 description 1
- HXJUTPCZVOIRIF-UHFFFAOYSA-N sulfolane Chemical compound O=S1(=O)CCCC1 HXJUTPCZVOIRIF-UHFFFAOYSA-N 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
- 230000001629 suppression Effects 0.000 description 1
- 238000004381 surface treatment Methods 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
- TXEYQDLBPFQVAA-UHFFFAOYSA-N tetrafluoromethane Chemical compound FC(F)(F)F TXEYQDLBPFQVAA-UHFFFAOYSA-N 0.000 description 1
- 239000006234 thermal black Substances 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 229910001428 transition metal ion Inorganic materials 0.000 description 1
- BDZBKCUKTQZUTL-UHFFFAOYSA-N triethyl phosphite Chemical compound CCOP(OCC)OCC BDZBKCUKTQZUTL-UHFFFAOYSA-N 0.000 description 1
- MDCWDBMBZLORER-UHFFFAOYSA-N triphenyl borate Chemical compound C=1C=CC=CC=1OB(OC=1C=CC=CC=1)OC1=CC=CC=C1 MDCWDBMBZLORER-UHFFFAOYSA-N 0.000 description 1
- 239000011800 void material Substances 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
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- C01G45/00—Compounds of manganese
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- H—ELECTRICITY
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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
- H01M4/50—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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- C01G45/00—Compounds of manganese
- C01G45/12—Manganates manganites or permanganates
- C01G45/1221—Manganates or manganites with a manganese oxidation state of Mn(III), Mn(IV) or mixtures thereof
- C01G45/1228—Manganates or manganites with a manganese oxidation state of Mn(III), Mn(IV) or mixtures thereof of the type [MnO2]n-, e.g. LiMnO2, Li[MxMn1-x]O2
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- C01G45/1221—Manganates or manganites with a manganese oxidation state of Mn(III), Mn(IV) or mixtures thereof
- C01G45/125—Manganates or manganites with a manganese oxidation state of Mn(III), Mn(IV) or mixtures thereof of the type[MnO3]n-, e.g. Li2MnO3, Li2[MxMn1-xO3], (La,Sr)MnO3
- C01G45/1257—Manganates or manganites with a manganese oxidation state of Mn(III), Mn(IV) or mixtures thereof of the type[MnO3]n-, e.g. Li2MnO3, Li2[MxMn1-xO3], (La,Sr)MnO3 containing lithium, e.g. Li2MnO3, Li2[MxMn1-xO3
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- C01G51/00—Compounds of cobalt
- C01G51/40—Cobaltates
- C01G51/42—Cobaltates containing alkali metals, e.g. LiCoO2
- C01G51/44—Cobaltates containing alkali metals, e.g. LiCoO2 containing manganese
- C01G51/50—Cobaltates containing alkali metals, e.g. LiCoO2 containing manganese of the type [MnO2]n-, e.g. Li(CoxMn1-x)O2, Li(MyCoxMn1-x-y)O2
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- C01G51/42—Cobaltates containing alkali metals, e.g. LiCoO2
- C01G51/44—Cobaltates containing alkali metals, e.g. LiCoO2 containing manganese
- C01G51/56—Cobaltates containing alkali metals, e.g. LiCoO2 containing manganese of the type [MnO3]2-, e.g. Li2[CoxMn1-xO3], Li2[MyCoxMn1-x-yO3
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- 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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- C01G53/44—Nickelates containing alkali metals, e.g. LiNiO2 containing manganese
- C01G53/56—Nickelates containing alkali metals, e.g. LiNiO2 containing manganese of the type [MnO3]2-, e.g. Li2[NixMn1-xO3], Li2[MyNixMn1-x-yO3
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Description
上記式中、
Mは、Ni、Ti、Co、Al、Cu、Fe、Mg、B、Cr、Zr、Zn及び2周期の遷移金属からなる群から選択される1つ以上であり、
Aは、PO4、BO3、CO3、F及びNO3のアニオンからなる群から選択される1つ以上であり、
0.5≦a≦1.0、0≦b≦0.5、a+b=1、0<x<1.0、0<y≦0.02である。
(i)前駆体製造用遷移金属含有塩を含む遷移金属水溶液を準備する過程と、
(ii)前記遷移金属水溶液に、前記前駆体のアニオンサイトを置換するようにアニオンを混合する過程と、
(iii)過程(ii)の混合後に強塩基を添加して共沈させる過程と、
を含む方法で製造することができる。
上記式中、
M’は、MnaMbであり、
Mは、Ni、Ti、Co、Al、Cu、Fe、Mg、B、Cr、Zr、Zn及び2周期の遷移金属からなる群から選択される1つ以上であり、
Aは、PO4、BO3、CO3、F及びNO3のアニオンからなる群から選択される1つ以上であり、
0<x<1、0<y≦0.02、0<y’≦0.02、0.5≦a≦1.0、0≦b≦0.5、a+b=1である。
4Lの湿式反応器用タンクに蒸留水3Lを満たした後、窒素ガスをタンクに2L/minの速度で連続的に投入して溶存酸素を除去した。このとき、タンク内の蒸留水の温度を温度維持装置を用いて50℃に維持した。また、タンクの外部に設置されているモーターと連結されているインペラを用いて、タンク内部の蒸留水を1500rpmの速度で撹拌した。
遷移金属水溶液にスクロース(sucrose)を混合しなかったこと以外は、実施例1と同様の方法で遷移金属前駆体を製造した。
遷移金属水溶液にリン酸塩を混合しなかったこと以外は、実施例1と同様の方法で遷移金属前駆体を製造した。
遷移金属水溶液にスクロース(Sucrose)及びリン酸塩を混合しなかったこと以外は、実施例1と同様の方法で遷移金属前駆体を製造した。
実施例1、2及び比較例1、2でそれぞれ製造した前駆体のSEMイメージをFE−SEM(Hitachi社のS−4800モデル)で撮影し、下記の図1乃至図4に示した。
実施例1、2及び比較例1、2でそれぞれ製造した前駆体のタップ密度を測定し、下記表1に示す。
[コイン電池の製造]
実施例1、2及び比較例1、2でそれぞれ製造されたマンガン−ニッケル−コバルト複合遷移金属前駆体を各組成のモル比に合わせてLi2CO3と混合した後、3〜5℃/分の昇温速度で加熱して、900〜950℃で5〜10時間の間焼成させることで、正極活物質粉末を製造した。
[初期充放電特性]
前記実施例3、4及び比較例3、4でそれぞれ製造されたコイン電池に対して、電気化学分析装置(Toyo System、Toscat 3100U)を用いて、3.0〜4.4Vの領域で正極活物質の電気的特性を評価した。
[寿命特性]
前記実施例3、4及び比較例3、4でそれぞれ製造されたコイン電池に対して、0.5Cの電流で30回充放電して寿命特性を評価した。その結果を下記表3に示す。
[出力特性]
前記実施例3、4及び比較例3、4でそれぞれ製造されたコイン電池に対して、0.5Cの電流で充放電した後、1.0Cと2.0Cの電流で放電して出力特性を評価した。その結果を下記表4に示す。
Claims (22)
- 下記化学式1で表される組成を有することを特徴とする、遷移金属前駆体:
MnaMb(OH1−x)2−yAy (化学式1)
上記化学式1中、
Mは、Ni、Coであり、
Aは、PO4であり、
0.5≦a≦1.0、
0≦b≦0.5、
a+b=1、
0<x<1.0、
0<y≦0.02であり、
上記a、b、x、yは電荷バランスを満たすように選択される。 - 前記xは、0.2以上〜0.5未満であることを特徴とする、請求項1に記載の遷移金属前駆体。
- 前記Mnの酸化数は、+2〜+3.5であることを特徴とする、請求項1に記載の遷移金属前駆体。
- 前記遷移金属前駆体は、Mnの酸化を防止するために遷移金属水溶液に還元剤をさらに含んで製造されることを特徴とする、請求項1に記載の遷移金属前駆体。
- 前記還元剤は、前記遷移金属水溶液のモル量対比0.1〜30モル%であることを特徴とする、請求項4に記載の遷移金属前駆体。
- 前記還元剤は、前記遷移金属水溶液のモル量対比1.0〜10モル%であることを特徴とする、請求項4に記載の遷移金属前駆体。
- 前記還元剤は、前記遷移金属水溶液のモル量対比2.0〜7.0モル%であることを特徴とする、請求項4に記載の遷移金属前駆体。
- 前記還元剤は、ヒドラジン、シュウ酸、アスコルビン酸、水素、炭素、炭化水素、及びその他の砂糖系物質からなる群から選択される1つ以上であることを特徴とする、請求項4に記載の遷移金属前駆体。
- 前記還元剤は砂糖系物質であることを特徴とする、請求項4に記載の遷移金属前駆体。
- 前記砂糖系物質は、フルクトース、スクロース、グルコース、ガラクトース、ラクトース、マルトース、澱粉、及びデキストリンからなる群から選択される1つ以上であることを特徴とする、請求項9に記載の遷移金属前駆体。
- 請求項1に記載の遷移金属前駆体を製造する方法であって、
(i)前駆体製造用遷移金属含有塩を含む遷移金属水溶液を準備する過程と、
(ii)前記遷移金属水溶液に、前記前駆体のアニオンサイトを置換するようにアニオンを混合する過程と、
(iii)過程(ii)の混合後に強塩基を添加して共沈させる過程と、
を含むことを特徴とする、遷移金属前駆体の製造方法。 - 前記過程(ii)において、アニオン以外に還元剤をさらに添加して混合することを特徴とする、請求項11に記載の遷移金属前駆体の製造方法。
- 前記還元剤は、前記遷移金属水溶液のモル量対比2.0〜7.0モル%であることを特徴とする、請求項12に記載の遷移金属前駆体の製造方法。
- 請求項1に記載の遷移金属前駆体を使用して製造されたことを特徴とする、リチウム複合遷移金属酸化物。
- 前記リチウム複合遷移金属酸化物は、下記化学式2で表されることを特徴とする、請求項14に記載のリチウム複合遷移金属酸化物。
(1−x)LiM’O2−yAy −xLi2MnO3−y’Ay’ (化学式2)
上記化学式2中、
M’は、MnaMbであり、
Mは、Ni、Coであり、
Aは、PO4であり、
0<x<1、
0<y≦0.02、
0<y’≦0.02、
0.5≦a≦1.0、
0≦b≦0.5、
a+b=1であり、
上記a、b、x、y、y’は電荷バランスを満たすように選択される。 - 前記リチウム複合遷移金属酸化物は、固溶体または複合体の形態であることを特徴とする、請求項15に記載のリチウム複合遷移金属酸化物。
- 請求項14に記載のリチウム複合遷移金属酸化物を正極活物質として含むことを特徴とする、正極。
- 請求項17に記載の正極を含むことを特徴とする、リチウム二次電池。
- 請求項18に記載のリチウム二次電池を単位電池として含むことを特徴とする、電池モジュール。
- 請求項19に記載の電池モジュールを含むことを特徴とする、電池パック。
- 請求項20に記載の電池パックを含むことを特徴とする、デバイス。
- 前記デバイスは、電気自動車、ハイブリッド電気自動車、プラグインハイブリッド電気自動車、または電力貯蔵用システムであることを特徴とする、請求項21に記載のデバイス。
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