JP6662531B2 - 多層構造のリチウム金属酸化物を含むリチウム二次電池用正極活物質およびそれを含む正極 - Google Patents
多層構造のリチウム金属酸化物を含むリチウム二次電池用正極活物質およびそれを含む正極 Download PDFInfo
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- JP6662531B2 JP6662531B2 JP2018505447A JP2018505447A JP6662531B2 JP 6662531 B2 JP6662531 B2 JP 6662531B2 JP 2018505447 A JP2018505447 A JP 2018505447A JP 2018505447 A JP2018505447 A JP 2018505447A JP 6662531 B2 JP6662531 B2 JP 6662531B2
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- Prior art keywords
- positive electrode
- active material
- electrode active
- lithium
- shell
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- 239000007774 positive electrode material Substances 0.000 title claims description 76
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims description 31
- 229910052744 lithium Inorganic materials 0.000 title claims description 31
- 229910021450 lithium metal oxide Inorganic materials 0.000 title description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 58
- 229910021437 lithium-transition metal oxide Inorganic materials 0.000 claims description 36
- 239000011572 manganese Substances 0.000 claims description 28
- 229910017052 cobalt Inorganic materials 0.000 claims description 22
- 239000010941 cobalt Substances 0.000 claims description 22
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 22
- -1 SeO 3 Inorganic materials 0.000 claims description 20
- 229910052759 nickel Inorganic materials 0.000 claims description 20
- 239000000203 mixture Substances 0.000 claims description 17
- 150000001875 compounds Chemical class 0.000 claims description 15
- 239000000126 substance Substances 0.000 claims description 15
- 239000011258 core-shell material Substances 0.000 claims description 13
- 229910052723 transition metal Inorganic materials 0.000 claims description 13
- 150000003624 transition metals Chemical class 0.000 claims description 13
- 229910052748 manganese Inorganic materials 0.000 claims description 12
- 238000004519 manufacturing process Methods 0.000 claims description 12
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 claims description 11
- 229910052782 aluminium Inorganic materials 0.000 claims description 11
- 239000000843 powder Substances 0.000 claims description 11
- 229910052719 titanium Inorganic materials 0.000 claims description 11
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 claims description 10
- 239000002243 precursor Substances 0.000 claims description 8
- 229910052749 magnesium Inorganic materials 0.000 claims description 7
- 239000003960 organic solvent Substances 0.000 claims description 7
- 229910052796 boron Inorganic materials 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 6
- 229910052721 tungsten Inorganic materials 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 5
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 claims description 5
- 239000011259 mixed solution Substances 0.000 claims description 5
- 229910052726 zirconium Inorganic materials 0.000 claims description 5
- 230000007423 decrease Effects 0.000 claims description 4
- FUJCRWPEOMXPAD-UHFFFAOYSA-N lithium oxide Chemical compound [Li+].[Li+].[O-2] FUJCRWPEOMXPAD-UHFFFAOYSA-N 0.000 claims description 4
- 229910001947 lithium oxide Inorganic materials 0.000 claims description 4
- 238000000034 method Methods 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 239000011164 primary particle Substances 0.000 claims description 4
- 239000011163 secondary particle Substances 0.000 claims description 4
- 229910052758 niobium Inorganic materials 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims description 2
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 claims description 2
- 229910006404 SnO 2 Inorganic materials 0.000 claims description 2
- 238000009792 diffusion process Methods 0.000 claims description 2
- 239000011363 dried mixture Substances 0.000 claims description 2
- 238000010304 firing Methods 0.000 claims description 2
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 claims description 2
- 229910001416 lithium ion Inorganic materials 0.000 claims description 2
- 230000004931 aggregating effect Effects 0.000 claims 1
- 239000010410 layer Substances 0.000 description 28
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 17
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 12
- 230000000052 comparative effect Effects 0.000 description 11
- 239000010936 titanium Substances 0.000 description 11
- 239000006258 conductive agent Substances 0.000 description 9
- 239000011149 active material Substances 0.000 description 8
- 230000008901 benefit Effects 0.000 description 8
- 239000011230 binding agent Substances 0.000 description 8
- 239000011255 nonaqueous electrolyte Substances 0.000 description 8
- 239000011777 magnesium Substances 0.000 description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 7
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 6
- 239000007864 aqueous solution Substances 0.000 description 6
- 229910052799 carbon Inorganic materials 0.000 description 6
- 239000012153 distilled water Substances 0.000 description 6
- 230000001747 exhibiting effect Effects 0.000 description 6
- 239000012528 membrane Substances 0.000 description 6
- 238000000926 separation method Methods 0.000 description 6
- 239000007784 solid electrolyte Substances 0.000 description 6
- 239000002904 solvent Substances 0.000 description 6
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 5
- 230000008859 change Effects 0.000 description 5
- 239000013078 crystal Substances 0.000 description 5
- 230000001965 increasing effect Effects 0.000 description 5
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 5
- VSZWPYCFIRKVQL-UHFFFAOYSA-N selanylidenegallium;selenium Chemical compound [Se].[Se]=[Ga].[Se]=[Ga] VSZWPYCFIRKVQL-UHFFFAOYSA-N 0.000 description 5
- 239000002002 slurry Substances 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
- SBLRHMKNNHXPHG-UHFFFAOYSA-N 4-fluoro-1,3-dioxolan-2-one Chemical compound FC1COC(=O)O1 SBLRHMKNNHXPHG-UHFFFAOYSA-N 0.000 description 4
- 239000004698 Polyethylene Substances 0.000 description 4
- 239000011651 chromium Substances 0.000 description 4
- 230000001939 inductive effect Effects 0.000 description 4
- 229910003002 lithium salt Inorganic materials 0.000 description 4
- 159000000002 lithium salts Chemical class 0.000 description 4
- 239000007773 negative electrode material Substances 0.000 description 4
- 229920000573 polyethylene Polymers 0.000 description 4
- 229920000642 polymer Polymers 0.000 description 4
- 150000003839 salts Chemical class 0.000 description 4
- 229910052710 silicon Inorganic materials 0.000 description 4
- 229910001220 stainless steel Inorganic materials 0.000 description 4
- 239000010935 stainless steel Substances 0.000 description 4
- 239000004034 viscosity adjusting agent Substances 0.000 description 4
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 3
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 3
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-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
- XTHFKEDIFFGKHM-UHFFFAOYSA-N Dimethoxyethane Chemical compound COCCOC XTHFKEDIFFGKHM-UHFFFAOYSA-N 0.000 description 3
- 229910012851 LiCoO 2 Inorganic materials 0.000 description 3
- 229910015643 LiMn 2 O 4 Inorganic materials 0.000 description 3
- 229910014689 LiMnO Inorganic materials 0.000 description 3
- 229910013290 LiNiO 2 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
- 239000002033 PVDF binder Substances 0.000 description 3
- 235000011114 ammonium hydroxide Nutrition 0.000 description 3
- 229910021383 artificial graphite Inorganic materials 0.000 description 3
- 239000004917 carbon fiber Substances 0.000 description 3
- 229910052804 chromium Inorganic materials 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 229910000361 cobalt sulfate Inorganic materials 0.000 description 3
- 229940044175 cobalt sulfate Drugs 0.000 description 3
- KTVIXTQDYHMGHF-UHFFFAOYSA-L cobalt(2+) sulfate Chemical compound [Co+2].[O-]S([O-])(=O)=O KTVIXTQDYHMGHF-UHFFFAOYSA-L 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000011888 foil Substances 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 229910052709 silver Inorganic materials 0.000 description 3
- WNXJIVFYUVYPPR-UHFFFAOYSA-N 1,3-dioxolane Chemical compound C1COCO1 WNXJIVFYUVYPPR-UHFFFAOYSA-N 0.000 description 2
- YEJRWHAVMIAJKC-UHFFFAOYSA-N 4-Butyrolactone Chemical compound O=C1CCCO1 YEJRWHAVMIAJKC-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- XMWRBQBLMFGWIX-UHFFFAOYSA-N C60 fullerene Chemical class C12=C3C(C4=C56)=C7C8=C5C5=C9C%10=C6C6=C4C1=C1C4=C6C6=C%10C%10=C9C9=C%11C5=C8C5=C8C7=C3C3=C7C2=C1C1=C2C4=C6C4=C%10C6=C9C9=C%11C5=C5C8=C3C3=C7C1=C1C2=C4C6=C2C9=C5C3=C12 XMWRBQBLMFGWIX-UHFFFAOYSA-N 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 229920002134 Carboxymethyl cellulose Polymers 0.000 description 2
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 description 2
- 229920002943 EPDM rubber Polymers 0.000 description 2
- ZHNUHDYFZUAESO-UHFFFAOYSA-N Formamide Chemical compound NC=O ZHNUHDYFZUAESO-UHFFFAOYSA-N 0.000 description 2
- 229910013733 LiCo Inorganic materials 0.000 description 2
- 229910013870 LiPF 6 Inorganic materials 0.000 description 2
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 2
- 239000004743 Polypropylene Substances 0.000 description 2
- 239000004372 Polyvinyl alcohol Substances 0.000 description 2
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 2
- KAESVJOAVNADME-UHFFFAOYSA-N Pyrrole Chemical compound C=1C=CNC=1 KAESVJOAVNADME-UHFFFAOYSA-N 0.000 description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 2
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
- 239000002041 carbon nanotube Substances 0.000 description 2
- 229910021393 carbon nanotube Inorganic materials 0.000 description 2
- 239000002388 carbon-based active material Substances 0.000 description 2
- 239000003575 carbonaceous material Substances 0.000 description 2
- 239000006182 cathode active material Substances 0.000 description 2
- 229910000428 cobalt oxide Inorganic materials 0.000 description 2
- IVMYJDGYRUAWML-UHFFFAOYSA-N cobalt(ii) oxide Chemical compound [Co]=O IVMYJDGYRUAWML-UHFFFAOYSA-N 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 239000012792 core layer Substances 0.000 description 2
- 229910001873 dinitrogen Inorganic materials 0.000 description 2
- 239000003792 electrolyte Substances 0.000 description 2
- LYCAIKOWRPUZTN-UHFFFAOYSA-N ethylene glycol Natural products OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 2
- 239000000835 fiber Substances 0.000 description 2
- 239000000945 filler Substances 0.000 description 2
- 239000010408 film Substances 0.000 description 2
- 239000006260 foam Substances 0.000 description 2
- 229910003472 fullerene Inorganic materials 0.000 description 2
- 239000003365 glass fiber Substances 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 239000007770 graphite material Substances 0.000 description 2
- 229910003480 inorganic solid Inorganic materials 0.000 description 2
- AMXOYNBUYSYVKV-UHFFFAOYSA-M lithium bromide Chemical compound [Li+].[Br-] AMXOYNBUYSYVKV-UHFFFAOYSA-M 0.000 description 2
- KWGKDLIKAYFUFQ-UHFFFAOYSA-M lithium chloride Chemical compound [Li+].[Cl-] KWGKDLIKAYFUFQ-UHFFFAOYSA-M 0.000 description 2
- 229940099596 manganese sulfate Drugs 0.000 description 2
- 239000011702 manganese sulphate Substances 0.000 description 2
- 235000007079 manganese sulphate Nutrition 0.000 description 2
- SQQMAOCOWKFBNP-UHFFFAOYSA-L manganese(II) sulfate Chemical compound [Mn+2].[O-]S([O-])(=O)=O SQQMAOCOWKFBNP-UHFFFAOYSA-L 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- TZIHFWKZFHZASV-UHFFFAOYSA-N methyl formate Chemical compound COC=O TZIHFWKZFHZASV-UHFFFAOYSA-N 0.000 description 2
- 229910021382 natural graphite Inorganic materials 0.000 description 2
- 229910000480 nickel oxide Inorganic materials 0.000 description 2
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 description 2
- 229940053662 nickel sulfate Drugs 0.000 description 2
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 description 2
- 150000004767 nitrides Chemical class 0.000 description 2
- 239000004745 nonwoven fabric Substances 0.000 description 2
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 description 2
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- 239000004332 silver Substances 0.000 description 2
- 229910052596 spinel Inorganic materials 0.000 description 2
- 239000011029 spinel Substances 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- VZGDMQKNWNREIO-UHFFFAOYSA-N tetrachloromethane Chemical compound ClC(Cl)(Cl)Cl VZGDMQKNWNREIO-UHFFFAOYSA-N 0.000 description 2
- 229910052718 tin Inorganic materials 0.000 description 2
- PYOKUURKVVELLB-UHFFFAOYSA-N trimethyl orthoformate Chemical compound COC(OC)OC PYOKUURKVVELLB-UHFFFAOYSA-N 0.000 description 2
- MIZLGWKEZAPEFJ-UHFFFAOYSA-N 1,1,2-trifluoroethene Chemical compound FC=C(F)F MIZLGWKEZAPEFJ-UHFFFAOYSA-N 0.000 description 1
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- PPDFQRAASCRJAH-UHFFFAOYSA-N 2-methylthiolane 1,1-dioxide Chemical compound CC1CCCS1(=O)=O PPDFQRAASCRJAH-UHFFFAOYSA-N 0.000 description 1
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- 229910012722 Li3N-LiI-LiOH Inorganic materials 0.000 description 1
- 229910012716 Li3N-LiI—LiOH Inorganic materials 0.000 description 1
- 229910012734 Li3N—LiI—LiOH Inorganic materials 0.000 description 1
- 229910013043 Li3PO4-Li2S-SiS2 Inorganic materials 0.000 description 1
- 229910013035 Li3PO4-Li2S—SiS2 Inorganic materials 0.000 description 1
- 229910012810 Li3PO4—Li2S-SiS2 Inorganic materials 0.000 description 1
- 229910012797 Li3PO4—Li2S—SiS2 Inorganic materials 0.000 description 1
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- KDXKERNSBIXSRK-UHFFFAOYSA-N Lysine Natural products NCCCCC(N)C(O)=O KDXKERNSBIXSRK-UHFFFAOYSA-N 0.000 description 1
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- 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
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- BEKPOUATRPPTLV-UHFFFAOYSA-N [Li].BCl Chemical compound [Li].BCl BEKPOUATRPPTLV-UHFFFAOYSA-N 0.000 description 1
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- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 description 1
- 150000003863 ammonium salts Chemical class 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 229910052797 bismuth Inorganic materials 0.000 description 1
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- 229920001577 copolymer Polymers 0.000 description 1
- 239000011889 copper foil Substances 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
- 150000004862 dioxolanes Chemical class 0.000 description 1
- NJLLQSBAHIKGKF-UHFFFAOYSA-N dipotassium dioxido(oxo)titanium Chemical compound [K+].[K+].[O-][Ti]([O-])=O NJLLQSBAHIKGKF-UHFFFAOYSA-N 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 229920001971 elastomer Polymers 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000002657 fibrous material Substances 0.000 description 1
- 229920001973 fluoroelastomer Polymers 0.000 description 1
- 239000002803 fossil fuel Substances 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
- 239000007789 gas Substances 0.000 description 1
- 150000004820 halides Chemical class 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 150000002367 halogens Chemical class 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
- 229910052738 indium Inorganic materials 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 230000010220 ion permeability Effects 0.000 description 1
- 239000003273 ketjen black Substances 0.000 description 1
- 239000006233 lamp black 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
- 230000014759 maintenance of location Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005259 measurement Methods 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
- CAAULPUQFIIOTL-UHFFFAOYSA-N methyl dihydrogen phosphate Chemical compound COP(O)(O)=O CAAULPUQFIIOTL-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
- 150000002815 nickel 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
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 150000003014 phosphoric acid esters Chemical class 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 229920000098 polyolefin 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
- 239000011148 porous material Substances 0.000 description 1
- 238000010248 power generation Methods 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 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
- 239000002994 raw material Substances 0.000 description 1
- 239000004627 regenerated cellulose Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000002409 silicon-based active material Substances 0.000 description 1
- KKCBUQHMOMHUOY-UHFFFAOYSA-N sodium oxide Chemical compound [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 description 1
- 229910001948 sodium oxide Inorganic materials 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
- 235000019698 starch Nutrition 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
- 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
- 230000007704 transition Effects 0.000 description 1
- 229910000314 transition metal oxide Inorganic materials 0.000 description 1
- BDZBKCUKTQZUTL-UHFFFAOYSA-N triethyl phosphite Chemical compound CCOP(OCC)OCC BDZBKCUKTQZUTL-UHFFFAOYSA-N 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- 235000015041 whisky Nutrition 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
Classifications
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- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
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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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- H01M4/362—Composites
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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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- 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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Description
本発明は、多層構造のリチウム金属酸化物を含むリチウム二次電池用正極活物質およびそれを含む正極に関する。
現在、このような電気化学的エネルギーを用いる電気化学素子の代表例として二次電池が挙げられ、ますますその使用領域が拡大する傾向にある。
したがって、向上した容量および出力特性を発揮しながらも熱的安全性の問題を解決できる正極活物質に対する必要性が高い。
ニッケル(Ni)、マンガン(Mn)、およびコバルト(Co)を含むリチウム遷移金属酸化物からなるコアと;
コバルト(Co)を含むリチウム遷移金属酸化物からなるシェルと;を含んでおり、
前記シェルの表面上には無機物層がコーティングされて追加的に形成されており、
前記無機物層の含有量は、正極活物質の全体重量を基準として0.1重量%以上〜3.0重量%以下であることを特徴とする。
式中、
0.55≦a≦0.9、0.05≦b≦0.5、0≦c≦0.1、a+b+c≦1、0.98≦y≦1.10であり;
Mは、W、B、Al、Zr、Ti、Mg、Cr、およびSiからなる群より選択される1つ以上である;
式中、
0≦a≦0.1、0.98≦y≦1.10であり;
Zは、W、B、Al、Zr、Ti、Mg、Cr、およびSiからなる群より選択される1つ以上である。
一具体例において、前記無機物層は、Al2O3、ZrO2、PO4、SeO3、およびSnO2からなるグループより選択されたいずれか1つであってもよい。
一具体例において、前記無機物層は、厚さが1〜150nmであってもよい。
前記遷移金属は、ニッケル、マンガン、およびコバルトからなる群より1つ以上選択される。
また、前記正極活物質の粒径は、0.1〜1μmであってもよい。
具体的には、前記リチウム二次電池用正極活物質を製造する方法は、
(a)コア−シェル構造を有する正極活物質製造用前駆体をリチウム酸化物と均一に混合した後、焼成反応させてリチウム遷移金属酸化物粉末を製造する過程を含むことができる。
(b)有機溶媒内にAl、Ti、Zr、W、Mg、Co、B、およびNbからなる群より選択された1つ以上の無機元素が含まれている混合溶液を製造する過程と;
(c)前記混合溶液と製造されたリチウム遷移金属酸化物粉末とを混合してペースト状態に撹拌する過程と;
(d)前記ペースト状態の混合物を乾燥して有機溶媒を蒸発させる過程と;
(e)前記乾燥した混合物を熱処理して、前記リチウム遷移金属酸化物粒子の表面上に無機物層が形成されている正極活物質を製造する過程と;をさらに含んでもよい。
一方、前記リチウム二次電池は、一般に、前記正極、負極、分離膜、およびリチウム塩含有非水系電解質から構成されている。
このような電池パックの構造および作製方法は当業界で公知であるので、本明細書ではそれに関する詳細な説明を省略する。
具体的には、前記デバイスは、例えば、携帯電話、携帯用コンピュータ、ウェアラブル電子機器、タブレットPC、スマートパッド、ネットブック、およびスマートワッチ(watch)からなる群より選択される。
(正極活物質製造用前駆体の製造)
二次電池用正極活物質を製造するための前駆体を製造するために、まず、3L湿式反応器用タンクに蒸留水2Lを満たした後、窒素ガスをタンクに1L/minの速度で連続的に投入して溶存酸素を除去した。この時、タンク内の蒸留水の温度を温度維持装置を用いて45〜50℃に維持した。また、タンクの外部に設けられているモータに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1000〜1200rpmの速度で撹拌した。
前記反応器によって得られた前駆体を蒸留水で洗浄後にろ過し、120℃の恒温乾燥機で24時間乾燥させて残留水分を除去した。このように乾燥したコア−シェル構造を有する前駆体と、Li2CO3とを1:1の重量比で混合した後に、5℃/分の昇温速度で加熱して920℃で10時間焼成して、リチウム遷移金属酸化物粉末(正極活物質)を製造した。この時、正極活物質のコア層はLi[Ni0.55Mn0.3Co0.1Zr0.05]O2からなり、シェル層はLiCo0.95Zr0.05O2からなるコア−シェル(core−shell)構造を有する正極活物質粉末を得た。この時、コア層およびシェル層の含有量比は、重量を基準として50:50であった。
先に製造された正極活物質を導電剤およびバインダー(PVdF)と95:2.5:2.5の比率(活物質:導電剤:バインダー、重量比)で溶剤のNMP(N−methyl−2−pyrrolidone)に添加して正極混合物スラリーを製造し、負極活物質として人造黒鉛95重量%、導電剤(Super−P)1.5重量%、およびバインダー(PVdF)3.5重量%を溶剤のNMPに添加して負極混合物スラリーを製造した後、アルミニウム箔と銅箔上にそれぞれコーティング、乾燥およびプレスして、正極および負極を製造した。
ニッケル硫酸塩、マンガン硫酸塩、およびコバルト硫酸塩を0.6:0.2:0.2の比率(モル比)で混合して1.5M濃度の遷移金属水溶液を準備したことを除けば、実施例1と同様の方法で電池を製造した。
二次電池用正極活物質を製造するための前駆体の製造中において、ドーピング元素としてジルコニウム(Zr)を含む塩を供給しないことを除けば、実施例1と同様の方法で電池を製造した。
コア−シェル構造を有する正極活物質の表面に無機物層を形成させないことを除けば、実施例1と同様の方法で電池を製造した。
正極活物質の表面に形成された無機物層の含有量が正極活物質の全体重量を基準として0.1重量%となるようにしたことを除けば、実施例1と同様の方法で電池を製造した。
正極活物質の表面に形成された無機物層の含有量が正極活物質の全体重量を基準として3.0重量%となるようにしたことを除けば、実施例1と同様の方法で電池を製造した。
正極活物質の表面に形成された無機物層の含有量が正極活物質の全体重量を基準として1.1重量%となるようにしたことを除けば、実施例1と同様の方法で電池を製造した。
コア−シェル構造の正極活物質粉末を製造する代わりに、Li[Ni0.55Mn0.3Co0.1Zr0.05]O2の化合物粒子と、LiCo0.95Zr0.05O2の化合物粒子とが均一に混合された構造を有する正極活物質粉末を製造したことを除けば、実施例1と同様の方法で電池を製造した。
正極活物質の表面に形成された無機物層の含有量が正極活物質の全体重量を基準として5.0重量%となるようにしたことを除けば、実施例1と同様の方法で電池を製造した。
正極活物質の表面に形成された無機物層の含有量が正極活物質の全体重量を基準として0.05重量%となるようにしたことを除けば、実施例1と同様の方法で電池を製造した。
寿命特性
実施例1〜11、および比較例1〜3でそれぞれ製造されたコイン電池に対して、3.0V〜4.4V電圧範囲で0.5Cの電流で100回充放電して、寿命特性を評価した。その結果を下記表1に示した。
高速充電特性
実施例1〜7、および比較例1〜3でそれぞれ製造されたコイン電池に対して、3.0V〜4.4Vの電圧範囲で0.1Cの電流で充放電後、5.0Cの電流で充放電して、高速充電特性を評価した。その結果を下記表2に示した。
DSCによる熱安定性の測定
本願の実施例1、実施例5、実施例6および実施例7と、比較例2および比較例3で製造された各活物質を含む正極をそれぞれ4.4V充電させた状態で、示差走査熱分析器(DSC)を用いて、10℃/minの速度で昇温させながら測定し、その結果を表3に示した。
本発明の属する分野における通常の知識を有する者であれば、内容に基づいて本発明の範疇内で多様な応用および変形を行うことが可能であろう。
Claims (18)
- コア−シェル構造を有するリチウム二次電池用正極活物質であって、
ニッケル(Ni)、マンガン(Mn)、およびコバルト(Co)を含むリチウム遷移金属酸化物からなるコアと;
コバルト(Co)を含むリチウム遷移金属酸化物からなるシェルと;を含んでおり、
前記コアのリチウム遷移金属酸化物は、下記化学式1で表される化合物であり、前記シェルのリチウム遷移金属酸化物は、下記化学式2で表される化合物であり、
前記シェルの表面上には、Al2O3、ZrO2、PO4、SeO3、およびSnO2からなるグループより選択されたいずれか1つである無機物層がコーティングされて追加的に形成されており、前記無機物層の含有量は、正極活物質の全体重量を基準として0.1重量%以上〜3.0重量%以下であることを特徴とする正極活物質:
Liy[NiaMnbCo1−(a+b+c) Zr c]O2 (1)
式中、
0.55≦a≦0.9、0.05≦b≦0.5、0.05≦c≦0.1、a+b+c≦1、0.98≦y≦1.10であり;
LiyCo(1−a) Zr aO2 (2)
式中、
0.05≦a≦0.1、0.98≦y≦1.10である。 - 前記無機物層は、Alの無機元素を含んでいることを特徴とする請求項1に記載の正極活物質。
- 前記無機物層の含有量は、正極活物質の全体重量を基準として1.1重量%以上〜3.0重量%以下であることを特徴とする請求項1に記載の正極活物質。
- 前記無機物層の含有量は、正極活物質の全体重量を基準として2.0重量%以上〜3.0重量%以下であることを特徴とする請求項3に記載の正極活物質。
- 前記無機物層は、厚さが1〜150nmであることを特徴とする請求項1に記載の正極活物質。
- 前記コアおよびシェルの含有量比は、重量を基準として20:80〜80:20であることを特徴とする請求項1に記載の正極活物質。
- 前記コアおよびシェルの含有量比は、重量を基準として40:60〜60:40であることを特徴とする請求項6に記載の正極活物質。
- 前記コアは、ニッケル、マンガン、およびコバルトの濃度は外部表面へいくほど減少する濃度勾配を有し、前記シェルは、コバルトの濃度は外部表面へいくほど減少する濃度勾配を有することを特徴とする請求項1に記載の正極活物質。
- 前記コアは、ニッケル、マンガン、およびコバルトの濃度はコア領域内で濃度勾配なく一定であり、前記シェルは、コバルトの濃度はシェル領域内で濃度勾配なく一定であることを特徴とする請求項1に記載の正極活物質。
- 前記正極活物質は、前記コアの外郭とシェルの内郭との間に形成され、1つ以上の遷移金属の濃度が連続的に変化して濃度勾配を示す濃度勾配層をさらに含んでいることを特徴とする請求項1に記載の正極活物質。
- 前記正極活物質の粒径は、0.1〜1μmであることを特徴とする請求項1に記載の正極活物質。
- 前記正極活物質は、1次粒子が凝集してなる2次粒子であり、前記1次粒子内のリチウムイオン拡散経路(lithium ion diffusion path)が2次粒子の中心方向に形成されたことを特徴とする請求項1に記載の正極活物質。
- リチウム二次電池用正極活物質を製造する方法において、
(a)コア−シェル構造を有する正極活物質製造用前駆体をリチウム酸化物と均一に混合した後、焼成反応させて、コア−シェル構造を有するリチウム遷移金属酸化物粉末を製造する過程と;
(b)有機溶媒内に、Al、Ti、Zr、W、Mg、Co、B、およびNbからなる群より選択された1つ以上の無機元素が含まれている混合溶液を製造する過程と;
(c)前記混合溶液と前記コア−シェル構造を有するリチウム遷移金属酸化物粉末とを混合してペースト状態に撹拌する過程と;
(d)前記ペースト状態の混合物を乾燥して有機溶媒を蒸発させる過程と;および
(e)前記乾燥した混合物を熱処理して、前記リチウム遷移金属酸化物粉末の表面上に無機物層が形成されている正極活物質を製造する過程と;を含み、
前記コアのリチウム遷移金属酸化物は、下記化学式1で表される化合物であり、前記シェルのリチウム遷移金属酸化物は、下記化学式2で表される化合物であることを特徴とする製造方法:
Liy[NiaMnbCo1−(a+b+c) Zr c]O2 (1)
式中、
0.55≦a≦0.9、0.05≦b≦0.5、0.05≦c≦0.1、a+b+c≦1、0.98≦y≦1.10であり;
LiyCo(1−a) Zr aO2 (2)
式中、
0.05≦a≦0.1、0.98≦y≦1.10である。 - 前記リチウム酸化物は、炭酸リチウム(Li2CO3)および/または水酸化リチウム(LiOH)であることを特徴とする請求項13に記載の製造方法。
- 請求項1に記載の正極活物質を含むことを特徴とする正極。
- 請求項15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16に記載のリチウム二次電池を含んでいることを特徴とする電池パック。
- 請求項17に記載の電池パックを電源として含んでいることを特徴とするモバイルデバイス。
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CN107925065B (zh) | 2021-06-01 |
WO2017069410A1 (ko) | 2017-04-27 |
KR101982790B1 (ko) | 2019-05-27 |
JP2018523895A (ja) | 2018-08-23 |
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