JP7459288B2 - リチウム金属負極、その製造方法及びそれに関連するリチウム金属電池並びに装置 - Google Patents
リチウム金属負極、その製造方法及びそれに関連するリチウム金属電池並びに装置 Download PDFInfo
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- JP7459288B2 JP7459288B2 JP2022558231A JP2022558231A JP7459288B2 JP 7459288 B2 JP7459288 B2 JP 7459288B2 JP 2022558231 A JP2022558231 A JP 2022558231A JP 2022558231 A JP2022558231 A JP 2022558231A JP 7459288 B2 JP7459288 B2 JP 7459288B2
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- Prior art keywords
- lithium
- negative electrode
- lithium metal
- battery
- monomer
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- 229910052744 lithium Inorganic materials 0.000 title claims description 221
- 238000004519 manufacturing process Methods 0.000 title claims description 18
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 79
- 229920000642 polymer Polymers 0.000 claims description 68
- 239000007784 solid electrolyte Substances 0.000 claims description 54
- 239000012528 membrane Substances 0.000 claims description 53
- 239000000178 monomer Substances 0.000 claims description 52
- 229910052751 metal Inorganic materials 0.000 claims description 48
- 238000012986 modification Methods 0.000 claims description 48
- 230000004048 modification Effects 0.000 claims description 48
- 239000002184 metal Substances 0.000 claims description 47
- 239000002841 Lewis acid Substances 0.000 claims description 41
- 150000007517 lewis acids Chemical class 0.000 claims description 41
- 239000011256 inorganic filler Substances 0.000 claims description 39
- 229910003475 inorganic filler Inorganic materials 0.000 claims description 39
- 229910003002 lithium salt Inorganic materials 0.000 claims description 36
- 159000000002 lithium salts Chemical class 0.000 claims description 36
- -1 cyclic ester Chemical class 0.000 claims description 34
- 125000004432 carbon atom Chemical group C* 0.000 claims description 31
- 239000011259 mixed solution Substances 0.000 claims description 28
- 238000000034 method Methods 0.000 claims description 27
- 239000007774 positive electrode material Substances 0.000 claims description 25
- 125000000217 alkyl group Chemical group 0.000 claims description 24
- 238000006243 chemical reaction Methods 0.000 claims description 24
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 22
- 239000011701 zinc Substances 0.000 claims description 21
- 229910005143 FSO2 Inorganic materials 0.000 claims description 20
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 15
- 229910052731 fluorine Inorganic materials 0.000 claims description 15
- 229910052782 aluminium Inorganic materials 0.000 claims description 14
- 150000001875 compounds Chemical class 0.000 claims description 14
- 150000001768 cations Chemical class 0.000 claims description 13
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims description 12
- 229910045601 alloy Inorganic materials 0.000 claims description 11
- 239000000956 alloy Substances 0.000 claims description 11
- 150000002641 lithium Chemical class 0.000 claims description 11
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 11
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims description 10
- 229910052801 chlorine Inorganic materials 0.000 claims description 10
- 229920001940 conductive polymer Polymers 0.000 claims description 10
- TZIHFWKZFHZASV-UHFFFAOYSA-N methyl formate Chemical compound COC=O TZIHFWKZFHZASV-UHFFFAOYSA-N 0.000 claims description 10
- OIFBSDVPJOWBCH-UHFFFAOYSA-N Diethyl carbonate Chemical compound CCOC(=O)OCC OIFBSDVPJOWBCH-UHFFFAOYSA-N 0.000 claims description 9
- KMTRUDSVKNLOMY-UHFFFAOYSA-N Ethylene carbonate Chemical compound O=C1OCCO1 KMTRUDSVKNLOMY-UHFFFAOYSA-N 0.000 claims description 9
- 239000011149 active material Substances 0.000 claims description 9
- 239000011248 coating agent Substances 0.000 claims description 9
- 238000000576 coating method Methods 0.000 claims description 9
- VUPKGFBOKBGHFZ-UHFFFAOYSA-N dipropyl carbonate Chemical compound CCCOC(=O)OCCC VUPKGFBOKBGHFZ-UHFFFAOYSA-N 0.000 claims description 9
- 239000002245 particle Substances 0.000 claims description 9
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 8
- 229910052794 bromium Inorganic materials 0.000 claims description 8
- JBTWLSYIZRCDFO-UHFFFAOYSA-N ethyl methyl carbonate Chemical compound CCOC(=O)OC JBTWLSYIZRCDFO-UHFFFAOYSA-N 0.000 claims description 8
- FKRCODPIKNYEAC-UHFFFAOYSA-N ethyl propionate Chemical compound CCOC(=O)CC FKRCODPIKNYEAC-UHFFFAOYSA-N 0.000 claims description 8
- 229910052740 iodine Inorganic materials 0.000 claims description 8
- 229910052718 tin Inorganic materials 0.000 claims description 8
- 239000011135 tin Substances 0.000 claims description 8
- 229910052725 zinc Inorganic materials 0.000 claims description 8
- 229910019142 PO4 Inorganic materials 0.000 claims description 7
- IEJIGPNLZYLLBP-UHFFFAOYSA-N dimethyl carbonate Chemical compound COC(=O)OC IEJIGPNLZYLLBP-UHFFFAOYSA-N 0.000 claims description 7
- 229910052732 germanium Inorganic materials 0.000 claims description 7
- 229910021437 lithium-transition metal oxide Inorganic materials 0.000 claims description 7
- RUOJZAUFBMNUDX-UHFFFAOYSA-N propylene carbonate Chemical compound CC1COC(=O)O1 RUOJZAUFBMNUDX-UHFFFAOYSA-N 0.000 claims description 7
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 6
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims description 6
- ATHHXGZTWNVVOU-UHFFFAOYSA-N N-methylformamide Chemical compound CNC=O ATHHXGZTWNVVOU-UHFFFAOYSA-N 0.000 claims description 6
- 150000005676 cyclic carbonates Chemical class 0.000 claims description 6
- 125000003709 fluoroalkyl group Chemical group 0.000 claims description 6
- 239000000395 magnesium oxide Substances 0.000 claims description 6
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 6
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 6
- 229910052717 sulfur Inorganic materials 0.000 claims description 6
- 150000001450 anions Chemical class 0.000 claims description 5
- 229910052787 antimony Inorganic materials 0.000 claims description 5
- 229910052739 hydrogen Inorganic materials 0.000 claims description 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 5
- 239000004417 polycarbonate Substances 0.000 claims description 5
- 229920000515 polycarbonate Polymers 0.000 claims description 5
- 229920000570 polyether Polymers 0.000 claims description 5
- 239000011592 zinc chloride Substances 0.000 claims description 5
- 235000005074 zinc chloride Nutrition 0.000 claims description 5
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 claims description 5
- UHOPWFKONJYLCF-UHFFFAOYSA-N 2-(2-sulfanylethyl)isoindole-1,3-dione Chemical compound C1=CC=C2C(=O)N(CCS)C(=O)C2=C1 UHOPWFKONJYLCF-UHFFFAOYSA-N 0.000 claims description 4
- JGFBQFKZKSSODQ-UHFFFAOYSA-N Isothiocyanatocyclopropane Chemical compound S=C=NC1CC1 JGFBQFKZKSSODQ-UHFFFAOYSA-N 0.000 claims description 4
- 229910013188 LiBOB Inorganic materials 0.000 claims description 4
- XBDQKXXYIPTUBI-UHFFFAOYSA-M Propionate Chemical compound CCC([O-])=O XBDQKXXYIPTUBI-UHFFFAOYSA-M 0.000 claims description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 4
- 229910002113 barium titanate Inorganic materials 0.000 claims description 4
- PWLNAUNEAKQYLH-UHFFFAOYSA-N butyric acid octyl ester Natural products CCCCCCCCOC(=O)CCC PWLNAUNEAKQYLH-UHFFFAOYSA-N 0.000 claims description 4
- 230000003197 catalytic effect Effects 0.000 claims description 4
- UUIQMZJEGPQKFD-UHFFFAOYSA-N n-butyric acid methyl ester Natural products CCCC(=O)OC UUIQMZJEGPQKFD-UHFFFAOYSA-N 0.000 claims description 4
- 229910052760 oxygen Inorganic materials 0.000 claims description 4
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 4
- 239000010452 phosphate Substances 0.000 claims description 4
- 229920000728 polyester Polymers 0.000 claims description 4
- 235000012239 silicon dioxide Nutrition 0.000 claims description 4
- 239000000377 silicon dioxide Substances 0.000 claims description 4
- HXJUTPCZVOIRIF-UHFFFAOYSA-N sulfolane Chemical compound O=S1(=O)CCCC1 HXJUTPCZVOIRIF-UHFFFAOYSA-N 0.000 claims description 4
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims description 3
- QMMFVYPAHWMCMS-UHFFFAOYSA-N Dimethyl sulfide Chemical compound CSC QMMFVYPAHWMCMS-UHFFFAOYSA-N 0.000 claims description 3
- 229910015015 LiAsF 6 Inorganic materials 0.000 claims description 3
- 229910013063 LiBF 4 Inorganic materials 0.000 claims description 3
- 229910013684 LiClO 4 Inorganic materials 0.000 claims description 3
- 229910013870 LiPF 6 Inorganic materials 0.000 claims description 3
- OHLUUHNLEMFGTQ-UHFFFAOYSA-N N-methylacetamide Chemical compound CNC(C)=O OHLUUHNLEMFGTQ-UHFFFAOYSA-N 0.000 claims description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 3
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 3
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 claims description 3
- GUJOJGAPFQRJSV-UHFFFAOYSA-N dialuminum;dioxosilane;oxygen(2-);hydrate Chemical compound O.[O-2].[O-2].[O-2].[Al+3].[Al+3].O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O GUJOJGAPFQRJSV-UHFFFAOYSA-N 0.000 claims description 3
- NVJBFARDFTXOTO-UHFFFAOYSA-N diethyl sulfite Chemical compound CCOS(=O)OCC NVJBFARDFTXOTO-UHFFFAOYSA-N 0.000 claims description 3
- BDUPRNVPXOHWIL-UHFFFAOYSA-N dimethyl sulfite Chemical compound COS(=O)OC BDUPRNVPXOHWIL-UHFFFAOYSA-N 0.000 claims description 3
- NKZSPGSOXYXWQA-UHFFFAOYSA-N dioxido(oxo)titanium;lead(2+) Chemical compound [Pb+2].[O-][Ti]([O-])=O NKZSPGSOXYXWQA-UHFFFAOYSA-N 0.000 claims description 3
- WBJINCZRORDGAQ-UHFFFAOYSA-N formic acid ethyl ester Natural products CCOC=O WBJINCZRORDGAQ-UHFFFAOYSA-N 0.000 claims description 3
- YQNQTEBHHUSESQ-UHFFFAOYSA-N lithium aluminate Chemical compound [Li+].[O-][Al]=O YQNQTEBHHUSESQ-UHFFFAOYSA-N 0.000 claims description 3
- 239000002808 molecular sieve Substances 0.000 claims description 3
- 229910052901 montmorillonite Inorganic materials 0.000 claims description 3
- 239000010450 olivine Substances 0.000 claims description 3
- 229910052609 olivine Inorganic materials 0.000 claims description 3
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims description 3
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims description 3
- BHZCMUVGYXEBMY-UHFFFAOYSA-N trilithium;azanide Chemical compound [Li+].[Li+].[Li+].[NH2-] BHZCMUVGYXEBMY-UHFFFAOYSA-N 0.000 claims description 3
- 229910001928 zirconium oxide Inorganic materials 0.000 claims description 3
- 229910010093 LiAlO Inorganic materials 0.000 claims description 2
- 239000004721 Polyphenylene oxide Substances 0.000 claims description 2
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 2
- 239000002322 conducting polymer Substances 0.000 claims description 2
- 230000000379 polymerizing effect Effects 0.000 claims 1
- 239000003792 electrolyte Substances 0.000 description 36
- 229910003480 inorganic solid Inorganic materials 0.000 description 27
- 239000002904 solvent Substances 0.000 description 22
- 239000000463 material Substances 0.000 description 16
- 238000012360 testing method Methods 0.000 description 16
- 238000000151 deposition Methods 0.000 description 15
- 230000008021 deposition Effects 0.000 description 15
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 13
- 239000000853 adhesive Substances 0.000 description 13
- 230000001070 adhesive effect Effects 0.000 description 13
- 229910001416 lithium ion Inorganic materials 0.000 description 13
- 238000006116 polymerization reaction Methods 0.000 description 11
- 239000007787 solid Substances 0.000 description 11
- 239000011888 foil Substances 0.000 description 10
- SBLRHMKNNHXPHG-UHFFFAOYSA-N 4-fluoro-1,3-dioxolan-2-one Chemical compound FC1COC(=O)O1 SBLRHMKNNHXPHG-UHFFFAOYSA-N 0.000 description 9
- 239000002002 slurry Substances 0.000 description 9
- 229910000733 Li alloy Inorganic materials 0.000 description 8
- 239000002033 PVDF binder Substances 0.000 description 8
- 239000000654 additive Substances 0.000 description 8
- 239000001989 lithium alloy Substances 0.000 description 8
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 7
- 239000002131 composite material Substances 0.000 description 7
- 238000001035 drying Methods 0.000 description 7
- 230000008569 process Effects 0.000 description 7
- 239000002203 sulfidic glass Substances 0.000 description 7
- 229910052726 zirconium Inorganic materials 0.000 description 7
- KLZUFWVZNOTSEM-UHFFFAOYSA-K Aluminium flouride Chemical compound F[Al](F)F KLZUFWVZNOTSEM-UHFFFAOYSA-K 0.000 description 6
- 229910010941 LiFSI Inorganic materials 0.000 description 6
- 239000006258 conductive agent Substances 0.000 description 6
- 230000001351 cycling effect Effects 0.000 description 6
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 6
- 239000011968 lewis acid catalyst Substances 0.000 description 6
- VDVLPSWVDYJFRW-UHFFFAOYSA-N lithium;bis(fluorosulfonyl)azanide Chemical compound [Li+].FS(=O)(=O)[N-]S(F)(=O)=O VDVLPSWVDYJFRW-UHFFFAOYSA-N 0.000 description 6
- BHHYHSUAOQUXJK-UHFFFAOYSA-L zinc fluoride Chemical compound F[Zn]F BHHYHSUAOQUXJK-UHFFFAOYSA-L 0.000 description 6
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 5
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 5
- 239000011267 electrode slurry Substances 0.000 description 5
- 238000010828 elution Methods 0.000 description 5
- 229910052736 halogen Inorganic materials 0.000 description 5
- 150000002367 halogens Chemical class 0.000 description 5
- 150000002430 hydrocarbons Chemical group 0.000 description 5
- 238000011065 in-situ storage Methods 0.000 description 5
- 150000002500 ions Chemical class 0.000 description 5
- 238000002156 mixing Methods 0.000 description 5
- 239000003960 organic solvent Substances 0.000 description 5
- 238000003825 pressing Methods 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
- 239000000758 substrate Substances 0.000 description 5
- 229910052719 titanium Inorganic materials 0.000 description 5
- 239000010936 titanium Substances 0.000 description 5
- BTBUEUYNUDRHOZ-UHFFFAOYSA-N Borate Chemical compound [O-]B([O-])[O-] BTBUEUYNUDRHOZ-UHFFFAOYSA-N 0.000 description 4
- 239000004743 Polypropylene Substances 0.000 description 4
- 229910006095 SO2F Inorganic materials 0.000 description 4
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 4
- 229910052796 boron Inorganic materials 0.000 description 4
- 238000007596 consolidation process Methods 0.000 description 4
- 210000001787 dendrite Anatomy 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 229920001971 elastomer Polymers 0.000 description 4
- 125000005843 halogen group Chemical group 0.000 description 4
- 229910052757 nitrogen Inorganic materials 0.000 description 4
- 235000021317 phosphate Nutrition 0.000 description 4
- 229920001155 polypropylene Polymers 0.000 description 4
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 4
- 239000004810 polytetrafluoroethylene Substances 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 description 4
- 239000005060 rubber Substances 0.000 description 4
- 229910052710 silicon Inorganic materials 0.000 description 4
- 229920003048 styrene butadiene rubber Polymers 0.000 description 4
- 229920000468 styrene butadiene styrene block copolymer Polymers 0.000 description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 239000004215 Carbon black (E152) Substances 0.000 description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 3
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 3
- XTHFKEDIFFGKHM-UHFFFAOYSA-N Dimethoxyethane Chemical compound COCCOC XTHFKEDIFFGKHM-UHFFFAOYSA-N 0.000 description 3
- 239000002202 Polyethylene glycol Substances 0.000 description 3
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 150000001408 amides Chemical class 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- 239000002134 carbon nanofiber Substances 0.000 description 3
- 239000006257 cathode slurry Substances 0.000 description 3
- 229920001577 copolymer Polymers 0.000 description 3
- 239000011889 copper foil Substances 0.000 description 3
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 150000008282 halocarbons Chemical class 0.000 description 3
- 229930195733 hydrocarbon Natural products 0.000 description 3
- 238000004255 ion exchange chromatography Methods 0.000 description 3
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 3
- MHCFAGZWMAWTNR-UHFFFAOYSA-M lithium perchlorate Chemical compound [Li+].[O-]Cl(=O)(=O)=O MHCFAGZWMAWTNR-UHFFFAOYSA-M 0.000 description 3
- 229910001486 lithium perchlorate Inorganic materials 0.000 description 3
- 229910001496 lithium tetrafluoroborate Inorganic materials 0.000 description 3
- 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 3
- 229910052749 magnesium Inorganic materials 0.000 description 3
- 239000011777 magnesium Substances 0.000 description 3
- 229910052748 manganese Inorganic materials 0.000 description 3
- 239000011572 manganese Substances 0.000 description 3
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 3
- 150000002825 nitriles Chemical class 0.000 description 3
- 229920003023 plastic Polymers 0.000 description 3
- 239000004033 plastic Substances 0.000 description 3
- 230000010287 polarization Effects 0.000 description 3
- 229920002239 polyacrylonitrile Polymers 0.000 description 3
- 239000010935 stainless steel Substances 0.000 description 3
- 229910001220 stainless steel Inorganic materials 0.000 description 3
- 238000003860 storage Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- FYGHSUNMUKGBRK-UHFFFAOYSA-N 1,2,3-trimethylbenzene Chemical compound CC1=CC=CC(C)=C1C FYGHSUNMUKGBRK-UHFFFAOYSA-N 0.000 description 2
- VXNZUUAINFGPBY-UHFFFAOYSA-N 1-Butene Chemical compound CCC=C VXNZUUAINFGPBY-UHFFFAOYSA-N 0.000 description 2
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- NIQCNGHVCWTJSM-UHFFFAOYSA-N Dimethyl phthalate Chemical compound COC(=O)C1=CC=CC=C1C(=O)OC NIQCNGHVCWTJSM-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 239000002227 LISICON Substances 0.000 description 2
- 229910005317 Li14Zn(GeO4)4 Inorganic materials 0.000 description 2
- 229920000459 Nitrile rubber Polymers 0.000 description 2
- OFBQJSOFQDEBGM-UHFFFAOYSA-N Pentane Chemical compound CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 2
- 239000004698 Polyethylene Substances 0.000 description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 230000004308 accommodation Effects 0.000 description 2
- 239000005456 alcohol based solvent Substances 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- FACXGONDLDSNOE-UHFFFAOYSA-N buta-1,3-diene;styrene Chemical compound C=CC=C.C=CC1=CC=CC=C1.C=CC1=CC=CC=C1 FACXGONDLDSNOE-UHFFFAOYSA-N 0.000 description 2
- IAQRGUVFOMOMEM-UHFFFAOYSA-N butene Natural products CC=CC IAQRGUVFOMOMEM-UHFFFAOYSA-N 0.000 description 2
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 2
- 238000004364 calculation method Methods 0.000 description 2
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Images
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Description
本出願は、2020年11月23日に提出された名称が「リチウム金属負極、その製造方法及びそれに関連するリチウム金属電池並びに装置」の中国特許出願番号202011320607.Xの優先権を主張しており、同出願の内容の全ては、ここに参照として取り込まれる。
ただし、XとYは、それぞれF、Cl、Br、I、炭素原子数が1~4であるアルキル基、又は炭素原子数が1~4であるハロゲン化アルキル基を独立して表し、任意選択的に、XとYは、それぞれF又はFで置換された、炭素原子数が1~4であるアルキル基を独立して表し、zは0、1、2、3又は4であり、nとmは、Aの価数×n=Lの価数×mを満たす。
負極集電体及び負極集電体の少なくとも一つの表面に設置されるリチウム系金属層を含む被修飾リチウム金属負極を提供するステップと、
リチウムと合金系活物質を形成可能な金属のカチオンを含むルイス酸とモノマーとを含む混合溶液を提供するステップと、
混合溶液を少なくとも一つのリチウム系金属層の表面に被覆し、ルイス酸はモノマーを触媒して重合させて、イオン伝導性のポリマー修飾層を形成し、リチウム金属負極を得るステップとを含む。
ただし、QはO又はSを表し、R1とR2はH、F、又は炭素原子数が1~4であるフルオロアルキル基を独立して表し、R3は炭素原子数が1~3であるフルオロアルキレン基を表す。
E=σ・l/(S・Δl)であり、式において、Eは圧縮弾性率(単位、Pa)を表し、σは圧力(単位、N)を表し、lはサンプルの圧縮変形前の厚さ(単位、m)を表し、Sはサンプルの圧縮変形前の面積(単位、m2)を表し、Δlは圧力を受けて変形した後の厚さ(単位、m)を表す。
式(I)において、QはO又はSを表す。式(I)に示される環状エステルは、(I-1)と(I-2)のうちの一つ又は複数を含んでもよい。
本出願のリチウム金属電池において、正極板は、正極集電体及び正極集電体の少なくとも一つの表面に設置され且つ正極活物質を含む正極膜層を含む。例えば、正極集電体は、自体厚さ方向で対向する二つの表面を有し、正極膜層は、正極集電体の対向する二つの表面のうちのいずれか一つ又は両方に設置されている。
LiaNibCocMdOeAf(3)、
式(3)において、0.8≦a≦1.2、0.5≦b<1、0<c<1、0<d<1、1≦e≦2、0≦f≦1であり、MはMn、Al、Zr、Zn、Cu、Cr、Mg、Fe、V、Ti及びBから選択される一つ又は複数であり、AはN、F、S及びClから選択される一つ又は複数である。
本出願のリチウム金属電池において、電解質は、当分野で既知の電解質を採用してもよく、当業者は需要に応じて選択することができる。例えば、電解質は、固体電解質膜、又は液体電解質(即ち電解液)から選択されてもよい。
下記実施例は、本出願が開示した内容をより具体的に記述した。本出願が開示した内容の範囲内で様々な修正及び変更が行われることは当業者にとって明白であるため、これらの実施例は、例示的な説明に過ぎない。特に説明のない限り、以下の実施例において報告されている全ての部、百分率、と比は、いずれも重量基準であるとともに、実施例において使用される全ての試薬は、いずれも市販されているものを用いてもよく、又は一般的な方法で合成してもよく、そしてさらに処理することなく直接使用することができ、及び実施例において使用される器具は、いずれも市販されているものを購入してもよい。
1、混合溶液の調製
LiFSI/FEC/EMC(質量比15:30:55)のモノマー溶液に3%のルイス酸AlCl3を加え、均一に混合して、混合溶液を得る。ここでは、ルイス酸の添加量(%)=ルイス酸の質量/モノマー溶液の質量×100%である。計算により、100重量部のモノマーFECに対して、ルイス酸AlCl3は10重量部であり、リチウム塩LiFSIは50重量部であり、反応緩和剤は183.3重量部である。
乾燥室において、25μmのリチウム金属箔を圧延法によって銅箔表面に貼り付け、スライスする。ドクターブレードを使用して、上記混合溶液をリチウム系金属層表面に塗布し、50min静置した後、リチウム系金属層表面に厚さ3μmのポリマー修飾層を形成する。
グローブボックスにおいて、正極活物質LiNi0.6Co0.2Mn0.2O2(NCM622)、硫化物固体電解質Li3PS4、導電剤VGCF、接着剤のスチレンブタジエンゴム(数平均分子量約50万)を70:20:5:5の重量比で、THF溶媒に混合し、十分に撹拌し均一に混合した後、正極スラリーを得て、正極スラリーをアルミニウム箔表面に塗布し、自然に乾燥した後、60℃で乾燥し、冷間プレスし、スライスして、正極板を得る。ここでは、正極活物質層の厚さは50μmであり、圧密密度は3g/cm3である。
グローブボックスにおいて、硫化物固体電解質Li3PS4と接着剤のスチレンブタジエンゴムを、99:1の重量比で、THF溶媒に混合し、電解質スラリーを調製し、電解質スラリーをガラス基材表面に塗布し、且つ60℃で乾燥してからスライスした後、硫化物固体電解質膜を得る。ここでは、硫化物固体電解質膜の厚さは50μmである。
正極板、硫化物固体電解質膜、リチウム金属負極を順に中心に合わせて積層し、室温(25℃)、250MPaで2min冷間プレスして積層ユニットを得て、10個の積層ユニットを積層し且つ冷間プレスした後、外装に入れてパッケージし、成形して固体リチウム金属電池を得る。
上記リチウム金属負極、硫化物固体電解質膜、リチウム金属シートを順に中心に合わせて積層し、室温、250MPaで2min冷間プレスして積層ユニットを得て、そして外装に入れてパッケージし、成形して固体対称リチウム金属電池を得る。
製造方法は実施例1と類似し、異なるのはリチウム金属負極の製造ステップにおける関連するパラメータを調節し、対応するリチウム金属電池を得ることであり、詳細は表1に示される。
1、Li/Li対称電池のテスト
定電流充放電の方式を採用してサイクルテストを行い、ここでは、堆積と溶出容量を6mAh/cm2に限定し、テスト電流密度は約0.39mA/cm2であり、テスト温度は25℃である。
1)25℃で、実施例と比較例で製造して得た固体リチウム金属電池に対して、定電流充放電方式を採用してテストを行い、具体的には、0.1C(電流密度は約0.13mA/cm2)の定電流で電圧が4.2Vになるまで充電し、その後、定電圧で電流が0.05Cになるまで充電し、1サイクル目の充電比容量を記録し、5min静置し、次に0.1Cの定電流恒で電圧が2.8Vになるまで放電し、1サイクル目の放電比容量を記録する。電池に対して上記方法でサイクル充放電テストを行い、200サイクル目のサイクルの放電比容量を記録する。
Claims (23)
- リチウム金属負極であって、
負極集電体と、
前記負極集電体の少なくとも一つの表面に設置される少なくとも一つのリチウム系金属層と、
イオン伝導性のポリマー修飾層であって、前記ポリマー修飾層は少なくとも一つの前記リチウム系金属層の表面に位置し、且つ少なくとも触媒量のルイス酸を含み、前記ルイス酸はリチウムと合金系活物質を形成可能な金属のカチオンを含むイオン伝導性のポリマー修飾層とを含む、リチウム金属負極。 - 前記ポリマー修飾層の厚さは100nm~10μmである、請求項1に記載のリチウム金属負極。
- 前記ルイス酸は、式(1)に示される化合物から選択される一つ又は複数であり、
AnLm(1)
ただし、AはAl、Zn、Mg、Pb、Ge、Sn又はSbのカチオンを表し、
LはF-、Cl-、Br-、I-又は式(2)に示されるアニオンを独立して表し、
ただし、XとYは、それぞれF、Cl、Br、I、炭素原子数が1~4であるアルキル基、又は炭素原子数が1~4であるハロゲン化アルキル基を独立して表し、
zは0、1、2、3又は4であり、
nとmは、Aの価数×n=Lの価数×mを満たす、請求項1又は2に記載のリチウム金属負極。 - 前記LはF-、Cl-、Br-、I-、[(FSO2)2N]-、[(CF3SO2)2N]-、[(FSO2)(CF3SO2)N]-、[(FSO2)(C2F5SO2)N]-、又は[(FSO2)(C4F9SO2)N]-を表す、請求項3に記載のリチウム金属負極。
- 前記ルイス酸は、AlCl3、ZnCl2、Al[(FSO2)2N]3とZn[(FSO2)2N]2から選択される一つ又は複数である、請求項1又は2に記載のリチウム金属負極。
- 前記ポリマー修飾層の圧縮弾性率は0.01MPa~1MPaである、請求項1~5のいずれか一項に記載のリチウム金属負極。
- 前記ポリマーは、ポリエーテル、ポリエステルとポリイミンのうちの一つ又は複数を含む、請求項1~6のいずれか一項に記載のリチウム金属負極。
- 前記ポリマーは、ポリ炭酸エステル、ポリ硫酸エステル、ポリ亜硫酸エステルとポリスルホン酸エステルのうちの一つ又は複数を含む、請求項7に記載のリチウム金属負極。
- 前記ポリマー修飾層は、リチウム塩をさらに含み、前記ポリマー修飾層における前記リチウム塩の重量比率は≦60%である、請求項1~8のいずれか一項に記載のリチウム金属負極。
- 前記リチウム塩は、LiPF6、LiBF4、LiClO4、LiAsF6、LiBOB、LiDFOB、LiTFOP、LiN(SO2RF)2とLiN(SO2F)(SO2RF)のうちの一つ又は複数を含み、RFは、CnF2n+1を表し、nは0~10の整数である、請求項9に記載のリチウム金属負極。
- 前記ポリマー修飾層は、無機フィラーをさらに含み、前記ポリマー修飾層における前記無機フィラーの重量比率は≦10%である、請求項1~10のいずれか一項に記載のリチウム金属負極。
- 前記無機フィラーは、二酸化ケイ素(SiO2)、酸化チタン(TiO2)、アルミナ(Al2O3)、酸化マグネシウム(MgO)、酸化ジルコニウム(ZrO2)、酸化亜鉛(ZnO)、酸化鉄(Fe3O4)、チタン酸バリウム(BaTiO3)、チタン酸鉛(PbTiO3)、窒化リチウム(Li3N)、アルミン酸リチウム(LiAlO2)、モンモリロナイトとモレキュラーシーブのうちの一つ又は複数を含み、及び/又は、
前記無機フィラーの体積平均粒径Dv50は、50nm~1000nmである、請求項11に記載のリチウム金属負極。 - リチウム金属負極の製造方法であって、
負極集電体及び前記負極集電体の少なくとも一つの表面に設置されるリチウム系金属層を含む被修飾リチウム金属負極を提供するステップと、
リチウムと合金系活物質を形成可能な金属のカチオンを含むルイス酸とモノマーとを含む混合溶液を提供するステップと、
前記混合溶液を少なくとも一つの前記リチウム系金属層の表面に被覆し、前記ルイス酸は前記モノマーを触媒して重合させて、イオン伝導性のポリマー修飾層を形成し、リチウム金属負極を得るステップとを含む、リチウム金属負極の製造方法。 - 100重量部の前記モノマーに対して、前記ルイス酸の重量部は1~35である、請求項13に記載の製造方法。
- 前記混合溶液は、反応緩和剤をさらに含み、100重量部の前記モノマーに対して、前記反応緩和剤の重量部は0より大きく800以下である、請求項13又は14に記載の製造方法。
- 前記反応緩和剤は、炭酸ジメチル、炭酸ジエチル、炭酸ジプロピル、メチルエチルカーボネート、ギ酸メチル、ギ酸エチル、プロピオン酸エチル、プロピオン酸プロピル、酪酸メチル、酢酸エチル、N-メチルピロリドン、N-メチルホルムアミド、N-メチルアセトアミド、アセトニトリル、スルホラン、ジメチルスルホキシド、メチルスルフィド、亜硫酸ジエチル、亜硫酸ジメチル、テトラヒドロフラン、式(I)に示される環状エステルのうちの一つ又は複数を含み、
ただし、QはO又はSを表し、R1とR2はH、F、又は炭素原子数が1~4であるフルオロアルキル基を独立して表し、R3は炭素原子数が1~3であるフルオロアルキレン基を表す、請求項15に記載の製造方法。 - 前記混合溶液は、リチウム塩をさらに含み、前記リチウム塩の含有量は、100重量部の前記モノマーに対して、200重量部以下であり、及び/又は、
前記混合溶液は、無機フィラーをさらに含み、前記無機フィラーの含有量は、100重量部の前記モノマーに対して、30重量部以下である、請求項13~16のいずれか一項に記載の製造方法。 - 前記モノマーは、環状炭酸エステル、環状スルホン酸エステル、環状硫酸エステル、環状亜硫酸エステル及びそのハロゲン化誘導体のうちの一つ又は複数を含む、請求項13に記載の製造方法。
- 前記モノマーは、エチレンカーボネート、プロピレンカーボネート及びそれらのハロゲン化誘導体のうちの一つ又は複数を含む、請求項13に記載の製造方法。
- 正極板と負極板とを含み、前記負極板は、請求項1~12のいずれか一項に記載のリチウム金属負極である、リチウム金属電池。
- 前記正極板は、正極集電体及び前記正極集電体の少なくとも一つの表面に設置され且つ正極活物質を含む正極膜層を含み、前記正極活物質は、オリビン構造のリチウム含有リン酸塩、リチウム遷移金属酸化物及びそれぞれの変性化合物のうちの一つ又は複数を含む、請求項20に記載のリチウム金属電池。
- 前記リチウム金属電池は、前記負極板と正極板との間に設置される固体電解質膜をさらに含む、請求項20又は21に記載のリチウム金属電池。
- 請求項20~22のいずれか一項に記載のリチウム金属電池を含む、装置。
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