CN112708514B - 一种锂和有机溶液预锂后极片用清洗液及其应用 - Google Patents
一种锂和有机溶液预锂后极片用清洗液及其应用 Download PDFInfo
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- 229910052744 lithium Inorganic materials 0.000 title claims abstract description 95
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims abstract description 94
- 238000004140 cleaning Methods 0.000 title claims abstract description 58
- 239000000654 additive Substances 0.000 claims abstract description 16
- 230000000996 additive effect Effects 0.000 claims abstract description 15
- 239000000243 solution Substances 0.000 claims description 66
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 15
- 238000012360 testing method Methods 0.000 claims description 10
- 239000002153 silicon-carbon composite material Substances 0.000 claims description 6
- 238000002791 soaking Methods 0.000 claims description 6
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 6
- 239000003960 organic solvent Substances 0.000 claims description 5
- OXMIDRBAFOEOQT-UHFFFAOYSA-N 2,5-dimethyloxolane Chemical compound CC1CCC(C)O1 OXMIDRBAFOEOQT-UHFFFAOYSA-N 0.000 claims description 4
- 238000005507 spraying Methods 0.000 claims description 4
- LZDKZFUFMNSQCJ-UHFFFAOYSA-N 1,2-diethoxyethane Chemical compound CCOCCOCC LZDKZFUFMNSQCJ-UHFFFAOYSA-N 0.000 claims description 2
- GDXHBFHOEYVPED-UHFFFAOYSA-N 1-(2-butoxyethoxy)butane Chemical compound CCCCOCCOCCCC GDXHBFHOEYVPED-UHFFFAOYSA-N 0.000 claims description 2
- JWUJQDFVADABEY-UHFFFAOYSA-N 2-methyltetrahydrofuran Chemical compound CC1CCCO1 JWUJQDFVADABEY-UHFFFAOYSA-N 0.000 claims description 2
- LJPCNSSTRWGCMZ-UHFFFAOYSA-N 3-methyloxolane Chemical compound CC1CCOC1 LJPCNSSTRWGCMZ-UHFFFAOYSA-N 0.000 claims description 2
- YZYKZHPNRDIPFA-UHFFFAOYSA-N tris(trimethylsilyl) borate Chemical group C[Si](C)(C)OB(O[Si](C)(C)C)O[Si](C)(C)C YZYKZHPNRDIPFA-UHFFFAOYSA-N 0.000 claims description 2
- 239000012530 fluid Substances 0.000 claims 3
- XTHFKEDIFFGKHM-UHFFFAOYSA-N Dimethoxyethane Chemical compound COCCOC XTHFKEDIFFGKHM-UHFFFAOYSA-N 0.000 claims 2
- 239000007772 electrode material Substances 0.000 abstract description 10
- 238000000926 separation method Methods 0.000 abstract description 8
- 239000012535 impurity Substances 0.000 abstract description 5
- 238000006138 lithiation reaction Methods 0.000 abstract description 5
- 150000001491 aromatic compounds Chemical class 0.000 abstract description 4
- 239000007795 chemical reaction product Substances 0.000 abstract description 4
- 230000016507 interphase Effects 0.000 abstract description 2
- 238000012545 processing Methods 0.000 abstract description 2
- 239000007784 solid electrolyte Substances 0.000 abstract description 2
- 239000012300 argon atmosphere Substances 0.000 description 7
- 230000007613 environmental effect Effects 0.000 description 7
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 6
- IJDNQMDRQITEOD-UHFFFAOYSA-N n-butane Chemical compound CCCC IJDNQMDRQITEOD-UHFFFAOYSA-N 0.000 description 6
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 5
- 229910052710 silicon Inorganic materials 0.000 description 5
- 239000010703 silicon Substances 0.000 description 5
- VAYTZRYEBVHVLE-UHFFFAOYSA-N 1,3-dioxol-2-one Chemical compound O=C1OC=CO1 VAYTZRYEBVHVLE-UHFFFAOYSA-N 0.000 description 4
- ZUOUZKKEUPVFJK-UHFFFAOYSA-N diphenyl Chemical compound C1=CC=CC=C1C1=CC=CC=C1 ZUOUZKKEUPVFJK-UHFFFAOYSA-N 0.000 description 4
- 238000007599 discharging Methods 0.000 description 4
- 238000004090 dissolution Methods 0.000 description 4
- 238000001035 drying Methods 0.000 description 4
- 239000007773 negative electrode material Substances 0.000 description 4
- SBLRHMKNNHXPHG-UHFFFAOYSA-N 4-fluoro-1,3-dioxolan-2-one Chemical compound FC1COC(=O)O1 SBLRHMKNNHXPHG-UHFFFAOYSA-N 0.000 description 3
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- VEWLDLAARDMXSB-UHFFFAOYSA-N ethenyl sulfate;hydron Chemical compound OS(=O)(=O)OC=C VEWLDLAARDMXSB-UHFFFAOYSA-N 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- HMDDXIMCDZRSNE-UHFFFAOYSA-N [C].[Si] Chemical compound [C].[Si] HMDDXIMCDZRSNE-UHFFFAOYSA-N 0.000 description 2
- 235000010290 biphenyl Nutrition 0.000 description 2
- 239000004305 biphenyl Substances 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Chemical compound [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 2
- 239000002210 silicon-based material Substances 0.000 description 2
- 230000001502 supplementing effect Effects 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- ZUHZGEOKBKGPSW-UHFFFAOYSA-N tetraglyme Chemical compound COCCOCCOCCOCCOC ZUHZGEOKBKGPSW-UHFFFAOYSA-N 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- OKIYQFLILPKULA-UHFFFAOYSA-N 1,1,1,2,2,3,3,4,4-nonafluoro-4-methoxybutane Chemical compound COC(F)(F)C(F)(F)C(F)(F)C(F)(F)F OKIYQFLILPKULA-UHFFFAOYSA-N 0.000 description 1
- WDXYVJKNSMILOQ-UHFFFAOYSA-N 1,3,2-dioxathiolane 2-oxide Chemical compound O=S1OCCO1 WDXYVJKNSMILOQ-UHFFFAOYSA-N 0.000 description 1
- FSSPGSAQUIYDCN-UHFFFAOYSA-N 1,3-Propane sultone Chemical compound O=S1(=O)CCCO1 FSSPGSAQUIYDCN-UHFFFAOYSA-N 0.000 description 1
- HYLLZXPMJRMUHH-UHFFFAOYSA-N 1-[2-(2-methoxyethoxy)ethoxy]butane Chemical compound CCCCOCCOCCOC HYLLZXPMJRMUHH-UHFFFAOYSA-N 0.000 description 1
- PZHIWRCQKBBTOW-UHFFFAOYSA-N 1-ethoxybutane Chemical compound CCCCOCC PZHIWRCQKBBTOW-UHFFFAOYSA-N 0.000 description 1
- NVJUHMXYKCUMQA-UHFFFAOYSA-N 1-ethoxypropane Chemical compound CCCOCC NVJUHMXYKCUMQA-UHFFFAOYSA-N 0.000 description 1
- -1 1-methoxybutylane Chemical compound 0.000 description 1
- JPSKCQCQZUGWNM-UHFFFAOYSA-N 2,7-Oxepanedione Chemical compound O=C1CCCCC(=O)O1 JPSKCQCQZUGWNM-UHFFFAOYSA-N 0.000 description 1
- FALRKNHUBBKYCC-UHFFFAOYSA-N 2-(chloromethyl)pyridine-3-carbonitrile Chemical compound ClCC1=NC=CC=C1C#N FALRKNHUBBKYCC-UHFFFAOYSA-N 0.000 description 1
- DSMUTQTWFHVVGQ-UHFFFAOYSA-N 4,5-difluoro-1,3-dioxolan-2-one Chemical compound FC1OC(=O)OC1F DSMUTQTWFHVVGQ-UHFFFAOYSA-N 0.000 description 1
- OQXNUCOGMMHHNA-UHFFFAOYSA-N 4-methyl-1,3,2-dioxathiolane 2,2-dioxide Chemical compound CC1COS(=O)(=O)O1 OQXNUCOGMMHHNA-UHFFFAOYSA-N 0.000 description 1
- NEILRVQRJBVMSK-UHFFFAOYSA-N B(O)(O)O.C[SiH](C)C.C[SiH](C)C.C[SiH](C)C Chemical compound B(O)(O)O.C[SiH](C)C.C[SiH](C)C.C[SiH](C)C NEILRVQRJBVMSK-UHFFFAOYSA-N 0.000 description 1
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- AUEPDNOBDJYBBK-UHFFFAOYSA-N [Si].[C-]#[O+] Chemical compound [Si].[C-]#[O+] AUEPDNOBDJYBBK-UHFFFAOYSA-N 0.000 description 1
- 150000008065 acid anhydrides Chemical class 0.000 description 1
- BTGRAWJCKBQKAO-UHFFFAOYSA-N adiponitrile Chemical compound N#CCCCCC#N BTGRAWJCKBQKAO-UHFFFAOYSA-N 0.000 description 1
- 229910021383 artificial graphite Inorganic materials 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- LXQJDZXMYIZZMQ-UHFFFAOYSA-N but-1-en-3-yne;carbonic acid Chemical compound C=CC#C.OC(O)=O LXQJDZXMYIZZMQ-UHFFFAOYSA-N 0.000 description 1
- 239000006258 conductive agent Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- SBZXBUIDTXKZTM-UHFFFAOYSA-N diglyme Chemical compound COCCOCCOC SBZXBUIDTXKZTM-UHFFFAOYSA-N 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 125000001033 ether group Chemical group 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- VANNPISTIUFMLH-UHFFFAOYSA-N glutaric anhydride Chemical compound O=C1CCCC(=O)O1 VANNPISTIUFMLH-UHFFFAOYSA-N 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 229910021385 hard carbon Inorganic materials 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000002931 mesocarbon microbead Substances 0.000 description 1
- VNKYTQGIUYNRMY-UHFFFAOYSA-N methoxypropane Chemical compound CCCOC VNKYTQGIUYNRMY-UHFFFAOYSA-N 0.000 description 1
- GBPVMEKUJUKTBA-UHFFFAOYSA-N methyl 2,2,2-trifluoroethyl carbonate Chemical compound COC(=O)OCC(F)(F)F GBPVMEKUJUKTBA-UHFFFAOYSA-N 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 239000005543 nano-size silicon particle Substances 0.000 description 1
- 229910021382 natural graphite Inorganic materials 0.000 description 1
- 150000002825 nitriles Chemical class 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 229910021384 soft carbon Inorganic materials 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229940014800 succinic anhydride Drugs 0.000 description 1
- IAHFWCOBPZCAEA-UHFFFAOYSA-N succinonitrile Chemical compound N#CCCC#N IAHFWCOBPZCAEA-UHFFFAOYSA-N 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- 229910000314 transition metal oxide Inorganic materials 0.000 description 1
- QJMMCGKXBZVAEI-UHFFFAOYSA-N tris(trimethylsilyl) phosphate Chemical compound C[Si](C)(C)OP(=O)(O[Si](C)(C)C)O[Si](C)(C)C QJMMCGKXBZVAEI-UHFFFAOYSA-N 0.000 description 1
- VMZOBROUFBEGAR-UHFFFAOYSA-N tris(trimethylsilyl) phosphite Chemical compound C[Si](C)(C)OP(O[Si](C)(C)C)O[Si](C)(C)C VMZOBROUFBEGAR-UHFFFAOYSA-N 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
- C11D7/22—Organic compounds
- C11D7/26—Organic compounds containing oxygen
- C11D7/267—Heterocyclic compounds
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
- C11D7/22—Organic compounds
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
- C11D7/22—Organic compounds
- C11D7/28—Organic compounds containing halogen
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
- C11D7/22—Organic compounds
- C11D7/34—Organic compounds containing sulfur
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
- C11D7/50—Solvents
- C11D7/5004—Organic solvents
- C11D7/5022—Organic solvents containing oxygen
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
- C11D7/50—Solvents
- C11D7/5004—Organic solvents
- C11D7/5027—Hydrocarbons
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- 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
- H01M4/139—Processes of manufacture
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D2111/00—Cleaning compositions characterised by the objects to be cleaned; Cleaning compositions characterised by non-standard cleaning or washing processes
- C11D2111/10—Objects to be cleaned
- C11D2111/14—Hard surfaces
- C11D2111/22—Electronic devices, e.g. PCBs or semiconductors
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract
本发明涉及一种锂和有机溶液预锂后极片用清洗液及其应用,属于电极材料加工技术领域。本发明的锂和有机溶液预锂后极片用清洗液,对用锂‑有机溶液预锂后的极片进行清洗时,首先可以清除极片上预锂后的反应产物芳香族化合物,其次添加剂可以和极片表面未反应的预锂溶液反应,不仅可以消除多余的预锂溶液还可以在电极材料上形成一层SEI膜,优化电极性能;更重要的是添加剂可以和因不均匀预锂造成部分地方微量析锂的锂负极反应,消除电极析锂的隐患,通过清除极片上的杂质并同时在负极形成SEI膜,优化预锂后电极材料的克容量发挥和电性能,具有广阔的应用前景。
Description
技术领域
本发明涉及一种锂和有机溶液预锂后极片用清洗液及其应用,属于电极材料加工技术领域。
背景技术
目前,硅材料作为一种高克容量负极,理论容量达到4200mAh/g,成为下一代负极研究的重点,但巨大的充放电体积变化成为其产业化应用的障碍。为解决硅负极充放电体积变化巨大的问题,人们开发出了各种硅负极,包括纳米化硅、氧化亚硅、氧化亚硅石墨复合负极、硅碳负极等。但不管哪一种硅负极,都有首次充放电库伦效率低的问题,其严重影响了电池能量密度的提升。为解决这个问题,人们开发出了预锂化技术。通过提前给硅负极材料补锂来提高其首次库伦效率和体系能量密度。锂-有机溶液预锂作为一种补锂技术,可以对负极进行定量补锂,成为一种潜在的预锂方法。但溶液预锂化后极片电性能劣化明显,如何提高溶液预锂化后极片电性能成为关键。
有鉴于上述的缺陷,本设计人,积极加以研究创新,以期创设一种锂和有机溶液预锂后极片用清洗液及其应用,使其更具有产业上的利用价值。
发明内容
为解决上述技术问题,本发明的目的是提供一种锂和有机溶液预锂后极片用清洗液及其应用。本发明的锂和有机溶液预锂后极片用清洗液,对用锂-有机溶液预锂后的极片进行清洗时,首先可以清除极片上预锂后的反应产物芳香族化合物,其次添加剂可以和极片表面未反应的预锂溶液反应,不仅可以消除多余的预锂溶液还可以在电极材料上形成一层SEI膜,优化电极性能;更重要的是添加剂可以和因不均匀预锂造成部分地方微量析锂的锂负极反应,消除电极析锂的隐患,通过清除极片上的杂质并同时在负极形成SEI膜,优化预锂后电极材料的克容量发挥和电性能,具有广阔的应用前景。
本发明的一种锂和有机溶液预锂后极片用清洗液,所述清洗液成分包括有机溶剂和添加剂。
进一步的,所述有机溶剂为醚类溶剂。
进一步的,所述有机溶剂为1-甲氧基丙烷,1-甲氧基丁基烷,1-乙氧基丙烷,1-乙氧基丁烷,乙醚,四氢呋喃,2-甲基四氢呋喃,3-甲基四氢呋喃,2,5-二甲基四氢呋喃,2,2,5,5-四甲基四氢呋喃,1,2-二甲基乙烷,1,2-二乙氧基乙烷,1,2-二丁氧基乙烷,1,2-二甲氧基甲烷,1,2-二乙氧基甲烷,二乙二醇二甲醚,二乙二醇丁基甲醚,四乙二醇二甲醚中的一种或多种。
进一步的,所述添加剂为含氟、含硫、含磷、含硼、酸酐类、腈类、醚类及含碳酸酯类添加剂中的一种或多种。
进一步的,所述添加剂为碳酸亚乙烯酯、乙烯基碳酸亚乙烯酯、氟代碳酸乙烯酯、1,2-二氟代碳酸乙烯酯、三氟乙基甲基碳酸酯、1,1,2,2-四氟乙基-2,2,3,3-四氟丙基醚、八氟戊基-四氟乙基醚、甲基九氟正丁醚、亚硫酸乙烯酯、1,3-丙磺酸内酯、1-丙烯基-1,3-磺酸内酯,硫酸乙烯酯、硫酸丙烯酯、1-氟-1,3-丙磺酸内酯、甲基二磺酸亚甲酯、乙腈、丁二腈、己二腈、丁二酸酐、戊二酸酐、己二酸酐、马来酸酐、三(三甲基硅基)磷酸酯、三(三甲基硅基)亚磷酸酯、三(三甲基硅基)硼酸酯中的一种或多种。
进一步的,所述清洗液中添加剂的添加量为清洗液总质量的0.01%~10%。
一种锂和有机溶液预锂后极片用清洗液的应用,利用所述锂和有机溶液预锂后极片用清洗液对锂和有机溶液预锂后极片进行清洗。
进一步的,所述清洗的方式为喷淋或者浸泡。
进一步的,所述喷淋或浸泡清洗包括一次清洗或多次清洗,多次清洗包括相同浓度清洗液清洗或不同浓度清洗液梯度清洗。
进一步的,所述极片为负极材料,具体为天然石墨、人造石墨,中间相碳微球、软炭、硬炭,钛酸锂,硅,氧化亚硅,硅碳复合材料,氧化亚硅碳复合材料,锡或过渡金属氧化物中的任意一种。
借由上述方案,本发明至少具有以下优点:
本发明的锂和有机溶液预锂后极片用清洗液,对用锂-有机溶液预锂后的极片进行清洗时,首先可以清除极片上预锂后的反应产物芳香族化合物,其次添加剂可以和极片表面未反应的预锂溶液反应,不仅可以消除多余的预锂溶液还可以在电极材料上形成一层SEI膜,优化电极性能;更重要的是添加剂可以和因不均匀预锂造成部分地方微量析锂的锂负极反应,消除电极析锂的隐患,通过清除极片上的杂质并同时在负极形成SEI膜,优化预锂后电极材料的克容量发挥和电性能,具有广阔的应用前景。
上述说明仅是本发明技术方案的概述,为了能够更清楚了解本发明的技术手段,并可依照说明书的内容予以实施,以下以本发明的较佳实施例详细说明如后。
具体实施方式
下面结合实施例,对本发明的具体实施方式作进一步详细描述。以下实施例用于说明本发明,但不用来限制本发明的范围。
1、锂电池极片的制备:
选取硅碳复合材料为负极材料,负极克容量(500mAh/g),将负极、导电剂、粘结剂按照93:3:4的比例混合均匀,制得负极片;
2、锂电池性能测试:
硅碳复合负极扣式电池充放电条件:0.1C恒流放电至5mV;0.02C恒流放电至5mV;0.1C充电至1.5V;
3、电池极片预锂:
在氩气氛围,环境指标为H2O≤0.5ppm,O2≤2.0ppm的手套箱中,称取7.71g联苯,将其溶解到100ml的THF溶液中,然后将0.425g锂粉加入到联苯-THF溶液中,搅拌一夜,制得预锂溶液;将制得的硅碳极片浸入预锂溶液中进行预锂,浸泡时间为30min,溶液温度25℃。
实例1
在氩气氛围,环境指标为H2O≤0.5ppm,O2≤2.0ppm的手套箱中,称取1g碳酸亚乙烯酯,将其溶解到49g的四氢呋喃中,溶解均匀后,制得清洗液1,将具体实施方式中预锂结束后的极片用清洗液1对极片进行浸泡清洗,清洗时间分别为5min、10min,然后在50℃条件下烘干,制得预锂极片,将预锂极片进行扣电组装测试。
实例2
在氩气氛围,环境指标为H2O≤0.5ppm,O2≤2.0ppm的手套箱中,称取1g三(三甲基硅烷)硼酸酯,将其溶解到49g的四氢呋喃中,溶解均匀后,制得清洗液2,将基体实施方式中预锂结束后的极片用清洗液2对极片进行浸泡清洗,清洗时间为10min,然后在50℃条件下烘干,制得预锂极片,将预锂极片进行扣电组装测试。
实例3
在氩气氛围,环境指标为H2O≤0.5ppm,O2≤2.0ppm的手套箱中,称取:2g氟代碳酸乙烯酯,将其溶解到48g的1,2-二甲基乙烷中,溶解均匀后,制得清洗液3,将具体实施方式中预锂结束后的极片用清洗液3对极片进行浸泡清洗,清洗时间为10min,然后在50℃条件下烘干,制得预锂极片,将预锂极片进行扣电组装测试。
实例4
在氩气氛围,环境指标为H2O≤0.5ppm,O2≤2.0ppm的手套箱中,称取0.5g碳酸亚乙烯酯、0.5g硫酸乙烯酯,将其溶解到49g的四氢呋喃中,溶解均匀后,制得清洗液4,将具体实施方式中预锂结束后的极片用清洗液4对极片进行浸泡清洗,清洗时间分为10min,然后在50℃条件下烘干,制得预锂极片,将预锂极片进行扣电组装测试。
实例5
在氩气氛围,环境指标为H2O≤0.5ppm,O2≤2.0ppm的手套箱中,称取0.5g碳酸亚乙烯酯、0.5g硫酸乙烯酯,将其溶解到24.5g四氢呋喃和24.5g 1,2-二甲基乙烷中,溶解均匀后,制得清洗液5,将具体实施方式中预锂结束后的极片用清洗液5对极片进行浸泡清洗,清洗时间为10min,然后在50℃条件下烘干,制得预锂极片,将预锂极片进行扣电组装测试。
对比例1:
在氩气氛围,环境指标为H2O≤0.5ppm,O2≤2.0ppm的手套箱中,将具体实施方式中的预锂极片在50℃条件下烘干,制得预锂极片,将预锂极片进行扣电组装测试。
性能检测试验
分别对实例1~5和对比例1中最终得到的预锂极片进行扣电组装测试,测试结果如表1所示;
检测方法/试验方法
测试方法:硅碳复合负极扣式电池充放电条件:0.1C恒流放电至5mV;0.02C恒流放电至5mV;0.1C充电至1.5V,并在此条件下进行循环。
表1性能检测结果
从表1数据可以看出,预锂极片经过清洗溶液清洗后,相比预锂后未处理的极片,材料的克容量发挥和循环性能都有明显的提升,说明本发明的清洗液通过对预锂后极片上的杂质物质清除,可以提高材料预锂后的克容量发挥,并优化其电性能,证实了本发明的锂和有机溶液预锂后极片用清洗液,对用锂-有机溶液预锂后的极片进行清洗时,首先可以清除极片上预锂后的反应产物芳香族化合物,其次添加剂可以和极片表面未反应的预锂溶液反应,不仅可以消除多余的预锂溶液还可以在电极材料上形成一层SEI膜,优化电极性能;更重要的是添加剂可以和因不均匀预锂造成部分地方微量析锂的锂负极反应,消除电极析锂的隐患,通过清除极片上的杂质并同时在负极形成SEI膜,优化预锂后电极材料的克容量发挥和电性能。
以上所述仅是本发明的优选实施方式,并不用于限制本发明,应当指出,对于本技术领域的普通技术人员来说,在不脱离本发明技术原理的前提下,还可以做出若干改进和变型,这些改进和变型也应视为本发明的保护范围。
Claims (4)
1.一种锂和有机溶液预锂后极片用清洗液,其特征在于:所述清洗液成分由有机溶剂和添加剂组成;
所述有机溶剂为四氢呋喃,2-甲基四氢呋喃,3-甲基四氢呋喃,2,5-二甲基四氢呋喃,2,2,5,5-四甲基四氢呋喃,1,2-二甲氧基乙烷,1,2-二乙氧基乙烷,1,2-二丁氧基乙烷,1,2-二甲氧基甲烷,1,2-二乙氧基甲烷中的一种或多种;
所述添加剂为三(三甲基硅基)硼酸酯;
所述清洗液中添加剂的添加量为清洗液总质量的0.01%~10%;
所述极片为负极极片,极片材料为硅碳复合材料;所述极片经所述清洗液清洗后的硅碳复合负极扣式电池测试前电压为0.283V-0.3095V。
2.权利要求1所述的一种锂和有机溶液预锂后极片用清洗液的应用,其特征在于:利用所述锂和有机溶液预锂后极片用清洗液对锂和有机溶液预锂后极片进行清洗。
3.根据权利要求2所述的一种锂和有机溶液预锂后极片用清洗液的应用,其特征在于:所述清洗的方式为喷淋或者浸泡。
4.根据权利要求3所述的一种锂和有机溶液预锂后极片用清洗液的应用,其特征在于:所述喷淋或浸泡清洗包括一次清洗或多次清洗,多次清洗包括相同浓度清洗液清洗或不同浓度清洗液梯度清洗。
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CN105199874A (zh) * | 2014-06-20 | 2015-12-30 | 惠州Tcl金能电池有限公司 | 电池表面清洗剂及其制备方法 |
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