CN116505089A - 一种低界面阻抗的电解液及锂离子电池的制备方法 - Google Patents
一种低界面阻抗的电解液及锂离子电池的制备方法 Download PDFInfo
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- 239000003792 electrolyte Substances 0.000 title claims abstract description 59
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 title claims abstract description 38
- 229910001416 lithium ion Inorganic materials 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- IIPYXGDZVMZOAP-UHFFFAOYSA-N lithium nitrate Chemical compound [Li+].[O-][N+]([O-])=O IIPYXGDZVMZOAP-UHFFFAOYSA-N 0.000 claims abstract description 46
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 38
- 238000000034 method Methods 0.000 claims abstract description 30
- 239000011248 coating agent Substances 0.000 claims abstract description 18
- 238000000576 coating method Methods 0.000 claims abstract description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 18
- AVQQQNCBBIEMEU-UHFFFAOYSA-N 1,1,3,3-tetramethylurea Chemical compound CN(C)C(=O)N(C)C AVQQQNCBBIEMEU-UHFFFAOYSA-N 0.000 claims abstract description 17
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 16
- 239000010439 graphite Substances 0.000 claims abstract description 16
- 230000008569 process Effects 0.000 claims abstract description 15
- 239000008367 deionised water Substances 0.000 claims abstract description 14
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 14
- 238000001704 evaporation Methods 0.000 claims abstract description 4
- 239000006258 conductive agent Substances 0.000 claims description 25
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 22
- 239000000654 additive Substances 0.000 claims description 19
- 230000000996 additive effect Effects 0.000 claims description 18
- 239000002002 slurry Substances 0.000 claims description 16
- 239000007787 solid Substances 0.000 claims description 15
- 229920000049 Carbon (fiber) Polymers 0.000 claims description 14
- 239000004917 carbon fiber Substances 0.000 claims description 14
- 239000011230 binding agent Substances 0.000 claims description 13
- 229910003002 lithium salt Inorganic materials 0.000 claims description 13
- 159000000002 lithium salts Chemical class 0.000 claims description 13
- 239000002041 carbon nanotube Substances 0.000 claims description 11
- 229910021393 carbon nanotube Inorganic materials 0.000 claims description 11
- 238000003756 stirring Methods 0.000 claims description 11
- DPXJVFZANSGRMM-UHFFFAOYSA-N acetic acid;2,3,4,5,6-pentahydroxyhexanal;sodium Chemical compound [Na].CC(O)=O.OCC(O)C(O)C(O)C(O)C=O DPXJVFZANSGRMM-UHFFFAOYSA-N 0.000 claims description 10
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 10
- 229910052782 aluminium Inorganic materials 0.000 claims description 10
- 239000001768 carboxy methyl cellulose Substances 0.000 claims description 10
- 235000019812 sodium carboxymethyl cellulose Nutrition 0.000 claims description 10
- 229920001027 sodium carboxymethylcellulose Polymers 0.000 claims description 10
- KMTRUDSVKNLOMY-UHFFFAOYSA-N Ethylene carbonate Chemical compound O=C1OCCO1 KMTRUDSVKNLOMY-UHFFFAOYSA-N 0.000 claims description 9
- 229910013553 LiNO Inorganic materials 0.000 claims description 9
- GELKBWJHTRAYNV-UHFFFAOYSA-K lithium iron phosphate Chemical compound [Li+].[Fe+2].[O-]P([O-])([O-])=O GELKBWJHTRAYNV-UHFFFAOYSA-K 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 9
- 238000005520 cutting process Methods 0.000 claims description 8
- JBTWLSYIZRCDFO-UHFFFAOYSA-N ethyl methyl carbonate Chemical compound CCOC(=O)OC JBTWLSYIZRCDFO-UHFFFAOYSA-N 0.000 claims description 8
- 229910021389 graphene Inorganic materials 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 8
- 238000005096 rolling process Methods 0.000 claims description 8
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 7
- 229910021383 artificial graphite Inorganic materials 0.000 claims description 7
- VONWDASPFIQPDY-UHFFFAOYSA-N dimethyl methylphosphonate Chemical compound COP(C)(=O)OC VONWDASPFIQPDY-UHFFFAOYSA-N 0.000 claims description 7
- 229920003048 styrene butadiene rubber Polymers 0.000 claims description 7
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 claims description 6
- 239000003063 flame retardant Substances 0.000 claims description 6
- XZZNDPSIHUTMOC-UHFFFAOYSA-N triphenyl phosphate Chemical compound C=1C=CC=CC=1OP(OC=1C=CC=CC=1)(=O)OC1=CC=CC=C1 XZZNDPSIHUTMOC-UHFFFAOYSA-N 0.000 claims description 6
- 239000006183 anode active material Substances 0.000 claims description 5
- 239000010410 layer Substances 0.000 claims description 5
- 239000002904 solvent Substances 0.000 claims description 5
- SBLRHMKNNHXPHG-UHFFFAOYSA-N 4-fluoro-1,3-dioxolan-2-one Chemical compound FC1COC(=O)O1 SBLRHMKNNHXPHG-UHFFFAOYSA-N 0.000 claims description 4
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 4
- 229910013870 LiPF 6 Inorganic materials 0.000 claims description 4
- 229910000572 Lithium Nickel Cobalt Manganese Oxide (NCM) Inorganic materials 0.000 claims description 4
- FBDMTTNVIIVBKI-UHFFFAOYSA-N [O-2].[Mn+2].[Co+2].[Ni+2].[Li+] Chemical compound [O-2].[Mn+2].[Co+2].[Ni+2].[Li+] FBDMTTNVIIVBKI-UHFFFAOYSA-N 0.000 claims description 4
- 239000011889 copper foil Substances 0.000 claims description 4
- ASMQGLCHMVWBQR-UHFFFAOYSA-M diphenyl phosphate Chemical compound C=1C=CC=CC=1OP(=O)([O-])OC1=CC=CC=C1 ASMQGLCHMVWBQR-UHFFFAOYSA-M 0.000 claims description 4
- 239000011888 foil Substances 0.000 claims description 4
- 238000003475 lamination Methods 0.000 claims description 4
- 229910000625 lithium cobalt oxide Inorganic materials 0.000 claims description 4
- 229910002102 lithium manganese oxide Inorganic materials 0.000 claims description 4
- BFZPBUKRYWOWDV-UHFFFAOYSA-N lithium;oxido(oxo)cobalt Chemical compound [Li+].[O-][Co]=O BFZPBUKRYWOWDV-UHFFFAOYSA-N 0.000 claims description 4
- VLXXBCXTUVRROQ-UHFFFAOYSA-N lithium;oxido-oxo-(oxomanganiooxy)manganese Chemical compound [Li+].[O-][Mn](=O)O[Mn]=O VLXXBCXTUVRROQ-UHFFFAOYSA-N 0.000 claims description 4
- 229910021382 natural graphite Inorganic materials 0.000 claims description 4
- 239000007774 positive electrode material Substances 0.000 claims description 4
- 238000007789 sealing Methods 0.000 claims description 4
- 239000002344 surface layer Substances 0.000 claims description 4
- 238000004804 winding Methods 0.000 claims description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 3
- 239000002808 molecular sieve Substances 0.000 claims description 3
- 239000001301 oxygen Substances 0.000 claims description 3
- 229910052760 oxygen Inorganic materials 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
- 239000002253 acid Substances 0.000 claims description 2
- 238000007873 sieving Methods 0.000 claims description 2
- FWWFVQIMBNWUGL-UHFFFAOYSA-N CCOP1N=PN=P[N]1 Chemical compound CCOP1N=PN=P[N]1 FWWFVQIMBNWUGL-UHFFFAOYSA-N 0.000 claims 1
- 239000007788 liquid Substances 0.000 claims 1
- RSNHXDVSISOZOB-UHFFFAOYSA-N lithium nickel Chemical compound [Li].[Ni] RSNHXDVSISOZOB-UHFFFAOYSA-N 0.000 claims 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 abstract description 8
- 229910052744 lithium Inorganic materials 0.000 abstract description 8
- 230000004913 activation Effects 0.000 abstract description 2
- 230000015572 biosynthetic process Effects 0.000 abstract description 2
- 239000006184 cosolvent Substances 0.000 abstract description 2
- 230000008020 evaporation Effects 0.000 abstract description 2
- 239000007773 negative electrode material Substances 0.000 abstract description 2
- 230000001681 protective effect Effects 0.000 abstract description 2
- 239000013589 supplement Substances 0.000 abstract description 2
- 239000011267 electrode slurry Substances 0.000 abstract 1
- 239000003292 glue Substances 0.000 description 12
- 239000000243 solution Substances 0.000 description 11
- 239000003960 organic solvent Substances 0.000 description 6
- 239000002131 composite material Substances 0.000 description 5
- 229910013872 LiPF Inorganic materials 0.000 description 4
- 101150058243 Lipf gene Proteins 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 description 4
- CBTAIOOTRCAMBD-UHFFFAOYSA-N 2-ethoxy-2,4,4,6,6-pentafluoro-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound CCOP1(F)=NP(F)(F)=NP(F)(F)=N1 CBTAIOOTRCAMBD-UHFFFAOYSA-N 0.000 description 3
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 3
- 239000002000 Electrolyte additive Substances 0.000 description 3
- 239000002174 Styrene-butadiene Substances 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- IEJIGPNLZYLLBP-UHFFFAOYSA-N dimethyl carbonate Chemical compound COC(=O)OC IEJIGPNLZYLLBP-UHFFFAOYSA-N 0.000 description 3
- 229920003222 semicrystalline poly(phosphazene) Polymers 0.000 description 3
- 229910002651 NO3 Inorganic materials 0.000 description 2
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 2
- 239000002033 PVDF binder Substances 0.000 description 2
- 239000010406 cathode material Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- FYDKNKUEBJQCCN-UHFFFAOYSA-N lanthanum(3+);trinitrate Chemical compound [La+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O FYDKNKUEBJQCCN-UHFFFAOYSA-N 0.000 description 2
- -1 lithium hexafluorophosphate Chemical compound 0.000 description 2
- 230000014759 maintenance of location Effects 0.000 description 2
- 230000010287 polarization Effects 0.000 description 2
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 2
- 235000010344 sodium nitrate Nutrition 0.000 description 2
- 239000004317 sodium nitrate Substances 0.000 description 2
- HJGJHDZQLWWMRT-UHFFFAOYSA-N 2,2,2-trifluoroethyl hydrogen carbonate Chemical compound OC(=O)OCC(F)(F)F HJGJHDZQLWWMRT-UHFFFAOYSA-N 0.000 description 1
- 239000002841 Lewis acid Substances 0.000 description 1
- 229910012851 LiCoO 2 Inorganic materials 0.000 description 1
- 229910010707 LiFePO 4 Inorganic materials 0.000 description 1
- 229910015643 LiMn 2 O 4 Inorganic materials 0.000 description 1
- 229910013290 LiNiO 2 Inorganic materials 0.000 description 1
- 208000012868 Overgrowth Diseases 0.000 description 1
- 239000004793 Polystyrene Substances 0.000 description 1
- 239000010405 anode material Substances 0.000 description 1
- 239000006256 anode slurry Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-N carbonic acid Chemical compound OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000009831 deintercalation Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 239000013538 functional additive Substances 0.000 description 1
- 239000007770 graphite material Substances 0.000 description 1
- 238000009830 intercalation Methods 0.000 description 1
- 230000002687 intercalation Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 230000002427 irreversible effect Effects 0.000 description 1
- 150000007517 lewis acids Chemical class 0.000 description 1
- 239000011572 manganese Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
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- 238000013508 migration Methods 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 1
- 229920002223 polystyrene Polymers 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000012047 saturated solution Substances 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 239000002210 silicon-based material Substances 0.000 description 1
- 239000007784 solid electrolyte Substances 0.000 description 1
- 229910052596 spinel Inorganic materials 0.000 description 1
- 239000011029 spinel Substances 0.000 description 1
- 238000010025 steaming Methods 0.000 description 1
- 239000011366 tin-based material Substances 0.000 description 1
- ITMCEJHCFYSIIV-UHFFFAOYSA-N triflic acid Chemical compound OS(=O)(=O)C(F)(F)F ITMCEJHCFYSIIV-UHFFFAOYSA-N 0.000 description 1
Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/058—Construction or manufacture
- H01M10/0583—Construction or manufacture of accumulators with folded construction elements except wound ones, i.e. folded positive or negative electrodes or separators, e.g. with "Z"-shaped electrodes or separators
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/056—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
- H01M10/0564—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of organic materials only
- H01M10/0566—Liquid materials
- H01M10/0567—Liquid materials characterised by the additives
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/058—Construction or manufacture
- H01M10/0587—Construction or manufacture of accumulators having only wound construction elements, i.e. wound positive electrodes, wound negative electrodes and wound separators
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/42—Methods or arrangements for servicing or maintenance of secondary cells or secondary half-cells
- H01M10/4235—Safety or regulating additives or arrangements in electrodes, separators or electrolyte
-
- 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
- H01M4/04—Processes of manufacture in general
- H01M4/0402—Methods of deposition of the material
- H01M4/0407—Methods of deposition of the material by coating on an electrolyte layer
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- H01M4/04—Processes of manufacture in general
- H01M4/0471—Processes of manufacture in general involving thermal treatment, e.g. firing, sintering, backing particulate active material, thermal decomposition, pyrolysis
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- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/133—Electrodes based on carbonaceous material, e.g. graphite-intercalation compounds or CFx
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- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
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- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/027—Negative electrodes
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Abstract
本发明公开了一种低界面阻抗的电解液及锂离子电池的制备方法,涉及二次锂离子电池技术领域。本发明利用负极材料匀浆过程,将硝酸锂溶解在负极浆料的去离子水中,并在涂布烘烤过程中,硝酸锂随着去离子水的蒸发偏析到极片表面;并利用四甲基脲作为硝酸锂的助溶剂,将部分硝酸锂溶解在电解液中;同时负极表面的硝酸锂在制片的时候附着在负极表面;锂电池经过化成,完成激活后,电解液中的四甲基脲溶解的硝酸锂会优先在石墨负极表面被还原,形成一层无机保护膜层;四甲基脲也会持续溶解负极表面的硝酸锂;形成硝酸锂的持续补充,提高电池的低温性能和长循环性能。
Description
技术领域
本发明涉及二次锂离子电池技术领域,特别涉及一种低界面阻抗的电解液及锂离子电池的制备方法。
背景技术
锂离子电池已经在储能领域和新能源交通运输等领域得到了广泛应用,但在更加严苛(例如高温、低温)的工作环境下,锂离子电池的容量和功率急剧下降,导致锂离子电池的性能下降。锂离子电池的电化学性能主要取决于电极材料和电解液;商业化的锂离子电池正极材料主要有层状结构的LiCoO2,LiNiO2,Li(NixCoyMnz)O2;尖晶石结构的LiMn2O4和橄榄石型的LiFePO4。负极材料主要有碳材料石墨,硅基材料、锡基材料;石墨材料导电性好,结晶度较高,具有良好的层状结构,适合锂离子的嵌入和脱出,其工作电位与金属锂负极接近,充放电比容量可以达到350 mAh/g,充放电效率在90%以上。是目前商业化应用最广泛的锂离子电池负极材料;
锂离子电池电解液主要由有机溶剂、电解质锂盐及各类功能添加剂组成,六氟磷酸锂(LiPF6)是目前常见的商业化锂离子电池的电解质,当温度高于 55 ℃时,电解液中LiPF6易受热分解产生的 PF5 是一种很强的路易斯酸,能够与痕量水分发生不可逆反应产生HF,腐蚀负极材料表面的SEI(Solid electrolyte interface)膜,造成电池容量损失。当环境温度低于0 ℃时,电解液电导率明显下降,离子迁移速率变缓,导致更高的电化学极化,电池的容量和功率急剧下降,锂离子电池在充放电过程中SEI膜的破裂与过度生长是石墨负极电化学性能失效的重要原因,SEI膜阻止了负极石墨与电解液接触界面的副反应持续进行,对石墨负极的锂离子电池性能具有极其重要的作用,但是石墨负极在充放电过程中的体积膨胀与收缩和电池高温循环,都会导致SEI膜局部破裂,破裂的SEI膜也会重新生长,会持续消耗活性锂离子,造成电池容量损失,过渡生长的SEI膜也会导致电池的内阻和极化增大,影响电池的循环稳定性、安全性,因此构建一种稳定的低界面阻抗的SEI膜,对改善锂离子电池循环寿命非常有意义;
申请公布号CN113651839A的专利公开了一种改善锂电池高低温性能的电解液添加剂及其制备方法、电解液及电化学装置,其将四氯硼酸锂和三氟甲磺酸溶于二氯甲烷中,然后向其中加入NaHCO3饱和溶液,在0~10℃下搅拌6h~20h,然后将得到的混合液在35℃~50℃旋蒸,得到所述电解液添加剂;将制备的电解液添加剂与电解液混合;制备得到电化学装置。其不足之处在于,该添加剂制备工艺复杂,对环境不友好,且成本昂贵;电解液与石墨负极的相容性差,会影响石墨电化学性能的发挥;
申请公布号 CN101841061A的专利公开了一种磷酸铁锂动力电池低温电解液及其制备方法,该磷酸铁锂动力电池低温电解液是由0.7-1.4mol/L的锂盐,65-95%的有机溶剂和3-15% 的添加剂配制而成。其不足之处在于,该电解液只是通过添加剂(聚苯乙烯、碳酸乙烯酯、羟基羧酸中的任意一种或一种以上的混合物)来调节电解液中锂盐LiPF6的浓度,该电解液虽然提升了低温条件下LiPF6的浓度,但是低温条件下锂离子电池电解液的粘度会随电解质锂盐浓度的增大而增大,因此该电解液中的电荷转移速度依然较低,也就是该电解液的低温性能依然较差,没有实质性提高。
发明内容
本发明的主要目的在于提供一种低界面阻抗的电解液及锂离子电池的制备方法,可以有效改善现有的锂离子电池受环境温度影响大,低温性能差,安全性能差等固有缺陷,同时解决LiNO3在常规碳酸酯类电解液溶解性差的问题。
为实现上述目的,本发明采取的技术方案为:一种低界面阻抗的锂离子电池的制备方法,包括正极片的制备和负极片的制备;
所述正极片的制备方法,包括如下步骤:
S1:将正极活性材料、粘结剂、导电剂按照质量份为94:3:3的比例均匀混合,并按照固含量为45%-60%溶于N-甲基吡咯烷酮(NMP)中,形成稳定的浆料;
S2:将上述形成的稳定的浆料,以均匀的面密度涂覆在洁净的铝箔上,并辊压、分切、模切制片,得到用于组装电池的正极极片;
所述负极片的制备,包括如下步骤:
S3:将负极石墨,粘结剂CMC(羧甲基纤维素钠)和SBR(丁苯橡胶)、导电剂,按照质量份为96:1.5:1.5:1的比例均匀混合,并按照固含量为40%-55%均匀分散在去离子水中,形成稳定的浆料,并添加固体质量分数2%的锂盐添加剂LiNO3,搅拌均匀;
S4:将上述形成的稳定的浆料,以均匀的面密度涂覆在洁净的铜箔上,在涂布烘箱烘烤过程中,硝酸锂依靠去离子水蒸发,在涂布膜层表面和近表层偏析,后经辊压、分切、模切制片,得到用于组装电池的负极极片;
S5:将上述制得的正负极极片用商用隔离膜,按负极-隔离膜-正极的“Z”字型叠片或卷绕工艺,组装成待注液电池。
一种低界面阻抗的电解液的制备方法,基于上述方法制备的锂离子电池,电解液的制备方法包括如下步骤:
S6:将75mL四甲基脲(1,1,3,3-Tetramethylurea,TMU)用分子筛过筛,除去微量水分,然后放置于手套箱中(手套箱中水、氧含量都要求小于10ppm),备用;
S7:将18g LiNO3溶解在上述干燥的四甲基脲,搅拌均匀;
S8:电解液采用锂离子电解液,锂盐LiPF6,1mol/L;溶剂EC(碳酸乙烯酯)/DMC(1,2-二甲基碳酸酯)/EMC(碳酸甲乙酯),体积比为1/1/1;成膜添加剂2 wt%FEC(氟代碳酸乙烯酯);阻燃添加剂1 wt%,甲基膦酸二甲酯(DMMP)、磷酸三苯酯(TPP)、磷酸二苯酯(CDP)、烯丙基二(2,2, 2-三氟乙基)碳酸酯(ATFEC)、乙氧基(五氟)环三磷腈(PFPN)当中的一种或多种;
取上述溶解有LiNO3的75mL TMU与配制好的锂离子电池电解液500ml,搅拌混合均匀,得到目标电解液。
由上述步骤进一步得到的一种低界面阻抗的电解液制备的锂电池,还包括S9:将上述得到的目标电解液注入到S5步骤中待注液电池,电池经密封、静置、化成、分容后得到目标电池。
所述S1中正极主材可以是磷酸铁锂、镍钴锰酸锂、镍酸锂、锰酸锂、钴酸锂等,优选为磷酸铁锂;导电剂可以是导电炭黑、碳纳米管、导电碳纤维、导电石墨烯一种或多种组合;优选为碳纳米管和导电碳纤维质量为1:1比例的复合导电剂。
所述S3中负极石墨可以是人造石墨、天然石墨等,优选为人造石墨;导电剂可以是导电炭黑、碳纳米管、导电碳纤维、导电石墨烯一种或多种组合;优选为导电炭黑和导电碳纤维质量比为1:1复合导电剂;锂盐添加剂可以是硝酸锂、硝酸钠、硝酸镧等硝酸盐,本发明优选硝酸锂,添加量为1 wt%~20 wt%。
所述S5中电芯(待注液电池)组装可以是方形铝壳电池,也可以是圆柱形电池,也可以是软包电池;优选方形铝壳电池。
本发明具有如下有益效果:
本发明创造性的利用负极材料匀浆过程,将硝酸锂溶解在负极浆料的去离子水中,并在涂布烘烤过程中,硝酸锂随着去离子水的蒸发偏析到极片表面;
利用四甲基脲作为硝酸锂的助溶剂,将部分硝酸锂溶解在电解液中;同时负极表面的硝酸锂在制片的时候附着在负极表面;锂电池经过化成,完成激活后,电解液中的四甲基脲溶解的硝酸锂会优先在石墨负极表面被还原,形成一层无机保护膜层;四甲基脲也会持续溶解负极表面的硝酸锂;形成硝酸锂的持续补充,提高电池的低温性能和长循环性能。
本发明工艺简单,易宏量化生产。
当然,实施本发明的任一产品并不一定需要同时达到以上所述的所有优点。
附图说明
为了更清楚地说明本发明实施例的技术方案,下面将对实施例描述所需要使用的附图作简单地介绍,显而易见地,下面描述中的附图仅仅是本发明的一些实施例,对于本领域普通技术人员来讲,在不付出创造性劳动的前提下,还可以根据这些附图获得其他的附图。
图1为本发明低界面阻抗的电解液及锂离子电池的制备流程架构图。
实施方式
下面将对本实用发明例中的技术方案进行清楚、完整地描述,显然,所描述的实施例仅仅是本发明一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有作出创造性劳动前提下所获得的所有其它实施例,都属于本发明保护的范围。
实施例1
如图1所示,一种低界面阻抗的锂离子电池的制备方法,包括正极片的制备和负极片的制备,其中,
1、正极片的制备
步骤1:正极制胶,将正极用的粘结剂PVDF,溶解在有机溶剂NMP中,搅拌形成稳定的胶液;胶液固含量4%~10%;
步骤2:将正极活性材料,粘结剂,导电剂按照质量份为94:3:3的比例均匀混合,并按照固含量为45%~60%,溶于有机溶剂NMP中,形成稳定的浆料;正极活性材料可以是磷酸铁锂、镍钴锰酸锂、镍酸锂、锰酸锂、钴酸锂等,优选为磷酸铁锂;导电剂可以是导电炭黑、碳纳米管、导电碳纤维、导电石墨烯一种或多种组合;优选为碳纳米管和导电碳纤维质量为1:1比例的复合导电剂;
步骤3:将上述形成的稳定的浆料,以合适的面密度涂覆在洁净的铝箔上,并辊压、分切、模切制片,得到能用于组装电池的正极极片。
2、负极片的制备
步骤4:负极制胶,将负极用的粘结剂CMC(羧甲基纤维素钠),溶解在去离子水中,搅拌形成稳定的胶液,胶液固含量0.8%~2%;
步骤5:将负极石墨,粘结剂CMC(羧甲基纤维素钠)和SBR(丁苯橡胶),导电剂,按照质量份为96:1.5:1.5:1的比例均匀混合,并按照固含量为40%~55%,均匀分散在去离子水中,形成稳定的浆料,并添加固体质量分数2%的锂盐添加剂LiNO3,搅拌均匀;负极主材可以是人造石墨、天然石墨等,优选为人造石墨;导电剂可以是导电炭黑、碳纳米管、导电碳纤维、导电石墨烯一种或多种组合;优选为导电炭黑和导电碳纤维质量比为1:1复合导电剂;锂盐添加剂可以是硝酸锂、硝酸钠、硝酸镧等硝酸盐,本发明优选硝酸锂;
步骤6:将上述形成的稳定的浆料,以合适的面密度涂布在洁净的铜箔上,在涂布烘箱烘烤过程中,硝酸锂会依靠去离子水蒸发,在涂布膜层表面和近表层偏析;经辊压、分切、模切制片,得到能用于组装电池的负极极片;
步骤7:将上述制得的正负极极片用商用隔离膜,按负极-隔离膜-正极的“Z”字型叠片或卷绕工艺,组装成待注液电池;电芯组装可以是方形铝壳电池,也可以是圆柱形电池,也可以是软包电池;优选方形铝壳电池。
一种低界面阻抗的电解液的制备方法,包括,
3、电解液的制备
步骤8:将75mL四甲基脲(1,1,3,3-Tetramethylurea,TMU)用分子筛过筛,除去微量水分;然后放置于手套箱中(手套箱中水、氧含量都要求小于10ppm),备用;
步骤9:将18g LiNO3溶解在上述干燥的四甲基脲,搅拌均匀;
步骤10:电解液采用锂离子电解液,锂盐LiPF6,1mol/L;溶剂EC(碳酸乙烯酯)/DMC(1,2-二甲基碳酸酯)/EMC(碳酸甲乙酯), 体积比为1/1/1;成膜添加剂2 wt%FEC(氟代碳酸乙烯酯);阻燃添加剂1 wt%,甲基膦酸二甲酯(DMMP)、磷酸三苯酯(TPP)、磷酸二苯酯(CDP)、烯丙基二(2, 2, 2-三氟乙基) 碳酸酯(ATFEC)、乙氧基(五氟) 环三磷腈(PFPN)当中的一种或多种,优选阻燃添加剂为磷酸三苯酯(TPP);取上述溶解有LiNO3的75mL TMU与配制好的锂离子电池电解液500ml,搅拌混合均匀,得到目标电解液;
步骤11:将上述得到的目标电解液注入到步骤7步骤中待注液电池,电池经密封,静置,化成,分容后得到目标电池。
对比例1
一种低界面阻抗的电解液以及使用该电解液制备的锂离子电池,包括:
1、正极片的制备
步骤1:正极制胶,将正极用的粘结剂PVDF,溶解在NMP有机溶剂中,搅拌形成稳定的胶液;胶液固含量4%~10%;
步骤2:将正极活性材料,粘结剂,导电剂按照质量份为94:3:3的比例均匀混合,并按照固含量为45%~60%,溶于有机溶剂NMP中,形成稳定的浆料;正极活性材料可以是磷酸铁锂、镍钴锰酸锂、镍酸锂、锰酸锂、钴酸锂等,优选为磷酸铁锂;导电剂可以是导电炭黑、碳纳米管、导电碳纤维、导电石墨烯一种或多种组合;优选为碳纳米管和导电碳纤维质量为1:1比例的复合导电剂;
步骤3:将上述形成的稳定的浆料,以合适的面密度涂布在洁净的铝箔上,并辊压、分切、模切制片,得到能用于组装电池的正极极片;
2、负极片的制备
步骤4:负极制胶,将负极用的粘结剂CMC,溶解在去离子水中,搅拌形成稳定的胶液,胶液固含量0.8%~2%;
步骤5:将负极石墨,粘结剂CMC(羧甲基纤维素钠)和SBR(丁苯橡胶),导电剂,按照质量份为96:1.5:1.5:1的比例均匀混合,并按照固含量为40%~55%,均匀分散在去离子水中,形成稳定的浆料;负极石墨可以是人造石墨、天然石墨等,优选为人造石墨;导电剂可以是导电炭黑、碳纳米管、导电碳纤维、导电石墨烯一种或多种组合;优选为导电炭黑和导电碳纤维质量比为1:1复合导电剂;
步骤6:将上述形成的稳定的浆料,以合适的面密度涂布在洁净的铜箔上,在涂布烘箱烘烤过程中,硝酸锂会依靠去离子水蒸发,在涂布膜层表面和近表层偏析;经辊压、分切、模切制片,得到能用于组装电池的负极极片;
步骤7:将上述制得的正负极极片用商用隔离膜,按负极-隔离膜-正极的“Z”字型叠片或卷绕工艺,组装成待注液电池;待注液电池组装可以是方形铝壳电池,也可以是圆柱形电池,也可以是软包电池;优选方形铝壳电池;
3、电解液的制备
步骤8:电解液采用锂离子电解液,锂盐LiPF6,1mol/L;溶剂EC(碳酸乙烯酯)/DMC(1,2-二甲基碳酸酯)/EMC(碳酸甲乙酯), 体积比为1/1/1;成膜添加剂2 wt%FEC(氟代碳酸乙烯酯);阻燃添加剂1 wt%,甲基膦酸二甲酯(DMMP)、磷酸三苯酯(TPP)、磷酸二苯酯(CDP)、烯丙基二(2,2,2-三氟乙基)碳酸酯(ATFEC)、乙氧基(五氟) 环三磷腈(PFPN)当中的一种或多种,优选阻燃添加剂为磷酸三苯酯(TPP);
步骤9:将上述得到的目标电解液注入到步骤7步骤中待注液电池,电池经密封,静置,化成,分容后得到目标电池。
将实施例1、对比例1制得的容量为75 Ah的电池分别在-10℃、-20℃条件下0.5C充放电循环100次后,电池的容量保持率及电池内阻如下表所示:
表1为电池的容量保持率及电池内阻比较图:
在本说明书的描述中,参考术语“一个实施例”、“示例”、“具体示例”等的描述意指结合该实施例或示例描述的具体特征、结构、材料或者特点包含于本发明的至少一个实施例或示例中。在本说明书中,对上述术语的示意性表述不一定指的是相同的实施例或示例。而且,描述的具体特征、结构、材料或者特点可以在任何的一个或多个实施例或示例中以合适的方式结合。
以上公开的本发明优选实施例只是用于帮助阐述本发明。优选实施例并没有详尽叙述所有的细节,也不限制该发明仅为所述的具体实施方式。显然,根据本说明书的内容,可作很多的修改和变化。本说明书选取并具体描述这些实施例,是为了更好地解释本发明的原理和实际应用,从而使所属技术领域技术人员能很好地理解和利用本发明。本发明仅受权利要求书及其全部范围和等效物的限制。
Claims (7)
1.一种低界面阻抗的锂离子电池的制备方法,其特征在于:包括正极片的制备和负极片的制备;
所述正极片的制备方法,包括如下步骤:
S1:将正极活性材料、粘结剂、导电剂按照质量份为94:3:3的比例均匀混合,并按照固含量为45%-60%溶于N-甲基吡咯烷酮中,形成稳定的浆料;
S2:将上述形成的稳定的浆料,以均匀的面密度涂覆在铝箔上,并辊压、分切、模切制片,得到用于组装电池的正极极片;
所述负极片的制备方法,包括如下步骤:
S3:将负极石墨,粘结剂羧甲基纤维素钠和丁苯橡胶、导电剂,按照质量份为96:1.5:1.5:1的比例均匀混合,并按照固含量为40%-55%均匀分散在去离子水中,形成稳定的浆料,并添加固体质量分数2%的硝酸锂,搅拌均匀;
S4:将上述形成的稳定的浆料,以均匀的面密度涂覆在铜箔上,在涂布烘箱烘烤过程中,硝酸锂依靠去离子水蒸发,在涂布膜层表面和近表层偏析,后经辊压、分切、模切制片,得到用于组装电池的负极极片;
S5:将上述制得的正负极极片用隔离膜,按负极-隔离膜-正极的“Z”字型叠片或卷绕工艺,组装成待注液电池。
2.一种低界面阻抗的电解液的制备方法,基于权利要求1制备的低界面阻抗的锂离子电池,其特征在于:包括如下步骤:
S6:将75mL四甲基脲用分子筛过筛,除去水分,然后放置于手套箱中,备用;
S7:将18g 锂盐添加剂LiNO3溶解在上述干燥的四甲基脲,搅拌均匀;
S8:电解液采用锂离子电解液,包括锂盐LiPF6,1mol/L;溶剂碳酸乙烯酯/1,2-二甲基碳酸酯/碳酸甲乙酯;成膜添加剂2 wt%氟代碳酸乙烯酯;阻燃添加剂1 wt%,甲基膦酸二甲酯、磷酸三苯酯、磷酸二苯酯、烯丙基二(2,2,2-三氟乙基)碳酸酯、乙氧基环三磷腈当中的一种或多种;
取上述溶解有LiNO3的75mL 四甲基脲与配制好的锂离子电池电解液500ml,搅拌混合均匀,得到目标电解液;
S9:将上述得到的目标电解液注入到S5步骤中待注液电池,电池经密封、静置、化成、分容后得到目标电池。
3.根据权利要求1所述的一种低界面阻抗的锂离子电池的制备方法,其特征在于:所述S1中正极活性材料包括磷酸铁锂或镍钴锰酸锂或镍酸锂或锰酸锂或钴酸锂,导电剂包括导电炭黑或碳纳米管或导电碳纤维或导电石墨烯中的一种或多种组合。
4.根据权利要求1所述的一种低界面阻抗的锂离子电池的制备方法,其特征在于:所述S3中负极石墨包括人造石墨或天然石墨,导电剂包括导电炭黑或碳纳米管或导电碳纤维或导电石墨烯中的一种或多种组合。
5.根据权利要求1所述的一种低界面阻抗的锂离子电池的制备方法,其特征在于:所述S5中组装的待注液电池包括方形铝壳电池或圆柱形电池或软包电池。
6.根据权利要求2所述的一种低界面阻抗的电解液的制备方法,其特征在于:所述S6中手套箱中水、氧含量都小于10ppm。
7.根据权利要求2所述的一种低界面阻抗的电解液的制备方法,其特征在于:所述S8中溶剂碳酸乙烯酯/1,2-二甲基碳酸酯/碳酸甲乙酯的体积比为1/1/1。
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