CN114079051A - 负极活性材料、负极以及电池 - Google Patents
负极活性材料、负极以及电池 Download PDFInfo
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- CN114079051A CN114079051A CN202110947477.0A CN202110947477A CN114079051A CN 114079051 A CN114079051 A CN 114079051A CN 202110947477 A CN202110947477 A CN 202110947477A CN 114079051 A CN114079051 A CN 114079051A
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- negative electrode
- active material
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- 239000007773 negative electrode material Substances 0.000 title claims abstract description 38
- 239000002245 particle Substances 0.000 claims abstract description 44
- 239000007822 coupling agent Substances 0.000 claims abstract description 30
- 150000002736 metal compounds Chemical class 0.000 claims abstract description 30
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 16
- 230000004048 modification Effects 0.000 claims abstract description 14
- 238000012986 modification Methods 0.000 claims abstract description 14
- 229910052751 metal Inorganic materials 0.000 claims abstract description 10
- 239000002184 metal Substances 0.000 claims abstract description 10
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 10
- 239000010703 silicon Substances 0.000 claims abstract description 8
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 7
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 claims description 34
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Chemical class [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 claims description 16
- 125000001424 substituent group Chemical group 0.000 claims description 15
- -1 silane compound Chemical class 0.000 claims description 11
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 10
- 229910052814 silicon oxide Inorganic materials 0.000 claims description 10
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 9
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 9
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- 239000011149 active material Substances 0.000 claims description 8
- 125000003277 amino group Chemical group 0.000 claims description 7
- 239000003575 carbonaceous material Substances 0.000 claims description 7
- 239000002482 conductive additive Substances 0.000 claims description 7
- 125000003700 epoxy group Chemical group 0.000 claims description 7
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 7
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 claims description 6
- 125000003396 thiol group Chemical group [H]S* 0.000 claims description 6
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 5
- 239000006183 anode active material Substances 0.000 claims description 5
- 239000011230 binding agent Substances 0.000 claims description 5
- 239000003792 electrolyte Substances 0.000 claims description 5
- 229910052744 lithium Inorganic materials 0.000 claims description 5
- 229910000000 metal hydroxide Inorganic materials 0.000 claims description 5
- 150000004692 metal hydroxides Chemical class 0.000 claims description 5
- 239000007774 positive electrode material Substances 0.000 claims description 5
- 229910000077 silane Inorganic materials 0.000 claims description 5
- 239000011734 sodium Substances 0.000 claims description 5
- 229920002125 Sokalan® Polymers 0.000 claims description 4
- 229910002804 graphite Inorganic materials 0.000 claims description 4
- 239000010439 graphite Substances 0.000 claims description 4
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 4
- UUEWCQRISZBELL-UHFFFAOYSA-N 3-trimethoxysilylpropane-1-thiol Chemical compound CO[Si](OC)(OC)CCCS UUEWCQRISZBELL-UHFFFAOYSA-N 0.000 claims description 3
- 229920002134 Carboxymethyl cellulose Polymers 0.000 claims description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 3
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 3
- 239000002033 PVDF binder Substances 0.000 claims description 3
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 3
- 239000002202 Polyethylene glycol Substances 0.000 claims description 3
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 3
- HMDDXIMCDZRSNE-UHFFFAOYSA-N [C].[Si] Chemical compound [C].[Si] HMDDXIMCDZRSNE-UHFFFAOYSA-N 0.000 claims description 3
- 239000006229 carbon black Substances 0.000 claims description 3
- 239000002041 carbon nanotube Substances 0.000 claims description 3
- 229910052802 copper Inorganic materials 0.000 claims description 3
- 239000010949 copper Substances 0.000 claims description 3
- 229910021389 graphene Inorganic materials 0.000 claims description 3
- 229910000625 lithium cobalt oxide Inorganic materials 0.000 claims description 3
- 150000002642 lithium compounds Chemical class 0.000 claims description 3
- BFZPBUKRYWOWDV-UHFFFAOYSA-N lithium;oxido(oxo)cobalt Chemical compound [Li+].[O-][Co]=O BFZPBUKRYWOWDV-UHFFFAOYSA-N 0.000 claims description 3
- 239000004584 polyacrylic acid Substances 0.000 claims description 3
- 229920002239 polyacrylonitrile Polymers 0.000 claims description 3
- 229920001223 polyethylene glycol Polymers 0.000 claims description 3
- 229920002981 polyvinylidene fluoride Polymers 0.000 claims description 3
- 229910052700 potassium Inorganic materials 0.000 claims description 3
- 239000011591 potassium Substances 0.000 claims description 3
- 229910052708 sodium Inorganic materials 0.000 claims description 3
- 229920003048 styrene butadiene rubber Polymers 0.000 claims description 3
- IKYAJDOSWUATPI-UHFFFAOYSA-N 3-[dimethoxy(methyl)silyl]propane-1-thiol Chemical compound CO[Si](C)(OC)CCCS IKYAJDOSWUATPI-UHFFFAOYSA-N 0.000 claims description 2
- SJECZPVISLOESU-UHFFFAOYSA-N 3-trimethoxysilylpropan-1-amine Chemical compound CO[Si](OC)(OC)CCCN SJECZPVISLOESU-UHFFFAOYSA-N 0.000 claims description 2
- 229920000049 Carbon (fiber) Polymers 0.000 claims description 2
- PFYQFCKUASLJLL-UHFFFAOYSA-N [Co].[Ni].[Li] Chemical compound [Co].[Ni].[Li] PFYQFCKUASLJLL-UHFFFAOYSA-N 0.000 claims description 2
- 125000003545 alkoxy group Chemical group 0.000 claims description 2
- 239000004917 carbon fiber Substances 0.000 claims description 2
- 229910021393 carbon nanotube Inorganic materials 0.000 claims description 2
- 239000001768 carboxy methyl cellulose Substances 0.000 claims description 2
- 235000010948 carboxy methyl cellulose Nutrition 0.000 claims description 2
- 239000008112 carboxymethyl-cellulose Substances 0.000 claims description 2
- GELKBWJHTRAYNV-UHFFFAOYSA-K lithium iron phosphate Chemical compound [Li+].[Fe+2].[O-]P([O-])([O-])=O GELKBWJHTRAYNV-UHFFFAOYSA-K 0.000 claims description 2
- BPSIOYPQMFLKFR-UHFFFAOYSA-N trimethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CO[Si](OC)(OC)CCCOCC1CO1 BPSIOYPQMFLKFR-UHFFFAOYSA-N 0.000 claims description 2
- 229910000572 Lithium Nickel Cobalt Manganese Oxide (NCM) Inorganic materials 0.000 claims 1
- 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 1
- 239000000203 mixture Substances 0.000 description 17
- 239000002002 slurry Substances 0.000 description 15
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 11
- 229910001416 lithium ion Inorganic materials 0.000 description 11
- 230000000052 comparative effect Effects 0.000 description 10
- 239000007787 solid Substances 0.000 description 9
- 239000007864 aqueous solution Substances 0.000 description 8
- 125000004429 atom Chemical group 0.000 description 5
- 238000002360 preparation method Methods 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
- 239000002904 solvent Substances 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- 230000036571 hydration Effects 0.000 description 3
- 238000006703 hydration reaction Methods 0.000 description 3
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 3
- 230000014759 maintenance of location Effects 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- KMTRUDSVKNLOMY-UHFFFAOYSA-N Ethylene carbonate Chemical compound O=C1OCCO1 KMTRUDSVKNLOMY-UHFFFAOYSA-N 0.000 description 2
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 2
- 239000004698 Polyethylene Substances 0.000 description 2
- 239000004743 Polypropylene Substances 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 125000002947 alkylene group Chemical group 0.000 description 2
- 238000006482 condensation reaction Methods 0.000 description 2
- 230000018044 dehydration Effects 0.000 description 2
- 238000006297 dehydration reaction Methods 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 238000006460 hydrolysis reaction Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- SNKMVYBWZDHJHE-UHFFFAOYSA-M lithium;dihydrogen phosphate Chemical compound [Li+].OP(O)([O-])=O SNKMVYBWZDHJHE-UHFFFAOYSA-M 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 229920000573 polyethylene Polymers 0.000 description 2
- 229920001155 polypropylene Polymers 0.000 description 2
- 239000002210 silicon-based material Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- PXQLVRUNWNTZOS-UHFFFAOYSA-N sulfanyl Chemical class [SH] PXQLVRUNWNTZOS-UHFFFAOYSA-N 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- OIFBSDVPJOWBCH-UHFFFAOYSA-N Diethyl carbonate Chemical compound CCOC(=O)OCC OIFBSDVPJOWBCH-UHFFFAOYSA-N 0.000 description 1
- 239000004593 Epoxy Substances 0.000 description 1
- 229910010710 LiFePO Inorganic materials 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 239000002174 Styrene-butadiene Substances 0.000 description 1
- SOXUFMZTHZXOGC-UHFFFAOYSA-N [Li].[Mn].[Co].[Ni] Chemical compound [Li].[Mn].[Co].[Ni] SOXUFMZTHZXOGC-UHFFFAOYSA-N 0.000 description 1
- NJSVDVPGINTNGX-UHFFFAOYSA-N [dimethoxy(propyl)silyl]oxymethanamine Chemical compound CCC[Si](OC)(OC)OCN NJSVDVPGINTNGX-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 125000000217 alkyl group Chemical group 0.000 description 1
- 238000005275 alloying Methods 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 239000004760 aramid Substances 0.000 description 1
- 229920003235 aromatic polyamide Polymers 0.000 description 1
- 229910021383 artificial graphite Inorganic materials 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 230000001351 cycling effect Effects 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- TXLQIRALKZAWHN-UHFFFAOYSA-N dilithium carbanide Chemical compound [Li+].[Li+].[CH3-].[CH3-] TXLQIRALKZAWHN-UHFFFAOYSA-N 0.000 description 1
- IEJIGPNLZYLLBP-UHFFFAOYSA-N dimethyl carbonate Chemical compound COC(=O)OC IEJIGPNLZYLLBP-UHFFFAOYSA-N 0.000 description 1
- 239000008151 electrolyte solution Substances 0.000 description 1
- 125000001301 ethoxy group Chemical group [H]C([H])([H])C([H])([H])O* 0.000 description 1
- JBTWLSYIZRCDFO-UHFFFAOYSA-N ethyl methyl carbonate Chemical compound CCOC(=O)OC JBTWLSYIZRCDFO-UHFFFAOYSA-N 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 239000007770 graphite material Substances 0.000 description 1
- 239000011357 graphitized carbon fiber Substances 0.000 description 1
- 229910021385 hard carbon Inorganic materials 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 230000002687 intercalation Effects 0.000 description 1
- 238000009830 intercalation Methods 0.000 description 1
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 description 1
- 229910052808 lithium carbonate Inorganic materials 0.000 description 1
- 229910000032 lithium hydrogen carbonate Inorganic materials 0.000 description 1
- 229910003002 lithium salt Inorganic materials 0.000 description 1
- 159000000002 lithium salts Chemical class 0.000 description 1
- GLNWILHOFOBOFD-UHFFFAOYSA-N lithium sulfide Chemical compound [Li+].[Li+].[S-2] GLNWILHOFOBOFD-UHFFFAOYSA-N 0.000 description 1
- HQRPHMAXFVUBJX-UHFFFAOYSA-M lithium;hydrogen carbonate Chemical compound [Li+].OC([O-])=O HQRPHMAXFVUBJX-UHFFFAOYSA-M 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 125000000956 methoxy group Chemical group [H]C([H])([H])O* 0.000 description 1
- 239000002071 nanotube Substances 0.000 description 1
- 229910021382 natural graphite Inorganic materials 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- RUOJZAUFBMNUDX-UHFFFAOYSA-N propylene carbonate Chemical compound CC1COC(=O)O1 RUOJZAUFBMNUDX-UHFFFAOYSA-N 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229910021384 soft carbon Inorganic materials 0.000 description 1
- 239000007784 solid electrolyte Substances 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
Classifications
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- H—ELECTRICITY
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- 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
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- H01M4/36—Selection of substances as active materials, active masses, active liquids
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- H01M4/366—Composites as layered products
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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
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
- H01M4/386—Silicon or alloys based on silicon
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- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/483—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides for non-aqueous cells
-
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- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/50—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
- H01M4/505—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese of mixed oxides or hydroxides containing manganese for inserting or intercalating light metals, e.g. LiMn2O4 or LiMn2OxFy
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- 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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- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
- H01M4/587—Carbonaceous material, e.g. graphite-intercalation compounds or CFx for inserting or intercalating light metals
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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/64—Carriers or collectors
- H01M4/66—Selection of materials
- H01M4/661—Metal or alloys, e.g. alloy coatings
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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
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/027—Negative electrodes
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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
- H01M2220/00—Batteries for particular applications
- H01M2220/20—Batteries in motive systems, e.g. vehicle, ship, plane
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- H—ELECTRICITY
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- H01M4/134—Electrodes based on metals, Si or alloys
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- 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
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Abstract
本发明涉及负极活性材料、负极以及电池。负极活性材料包含活性粒子以及修饰层。活性粒子含有硅元素、碳元素、或其组合。修饰层披覆于活性粒子的表面。修饰层包含偶合剂的残基与金属化合物的残基。偶合剂的残基键合在活性粒子与金属化合物的残基之间。金属化合物的残基含有金属原子。
Description
技术领域
本发明涉及负极活性材料、负极以及电池。
背景技术
随着锂离子电池能量密度的不断提升,传统的石墨材料已经无法满足高比能电池的设计需求。硅(Si)基材料凭借着高达4200mAh/g的容量,以及与石墨接近的嵌锂平台,成为了最有希望的下一代高容量负极材料。然而,硅材料在与锂(Li)进行合金化的过程中体积膨胀可达300%以上,从而导致颗粒的粉化和破碎,以及固体电解质界面膜(SolidElectrolyte Interphase;SEI)的破坏,严重影响锂离子电池的循环寿命。
硅氧化物(SiOx)材料的出现让高容量硅基负极的应用出现了转机。然而,硅氧化物首次库伦效率远低于石墨和硅碳材料。这成为了硅氧化物材料应用的一大障碍。
发明内容
本发明涉及负极活性材料、负极以及电池。
根据本发明的一方面,提出负极活性材料,其包含活性粒子以及修饰层;活性粒子含有硅元素、碳元素、或其组合;修饰层披覆于活性粒子的表面;修饰层包含偶合剂的残基与金属化合物的残基;偶合剂的残基键合在活性粒子与金属化合物的残基之间;金属化合物的残基含有金属原子。
根据本发明的另一方面,提出负极,其包含集电层以及活性材料层;活性材料层在集电层上;活性材料层包含如上所述的负极活性材料、导电添加剂及粘着剂。
根据本发明的又一方面,提出电池,其包含正极、如上所述的负极、隔离膜以及电解液;隔离膜在正极与负极之间;电解液在正极与负极之间。
为了对本发明的上述及其他方面有更佳的了解,下文特举实施方式,详细说明如下。
实施方式
根据本公开内容的实施方式提供负极活性材料,以及应用此负极活性材料的负极与电池。电池具有较长的循环寿命,以及较佳的库伦效率。
根据本公开内容的实施方式,负极活性材料可包含活性粒子以及修饰层。
所述活性粒子(负极活性粒子)含有硅元素、碳元素、或其组合。活性粒子可包含硅(Si)、硅氧化物(SiOx)、碳修饰的氧化硅、硅碳(SiC)、碳材(碳材料)、或其组合。碳材例如包括天然石墨、人造石墨、软碳、硬碳、石墨烯或石墨化碳纤维等。
所述修饰层披覆于活性粒子的表面,修饰层包含偶合剂的残基与金属化合物的残基。根据本公开内容的实施方式,修饰层与活性粒子表面之间具有化学键合,其中,偶合剂的残基键合在活性粒子与金属化合物的残基之间。金属化合物的残基含有金属原子,例如包含锂(Li)、钠(Na)、钾(K)、或其组合。
所述偶合剂可为硅烷化合物。在硅烷化合物的化学结构中,硅原子上的取代基(例如第一反应取代基)为可水解基团或甲基,另一取代基(例如第二反应取代基)为含有巯基(-SH)、环氧基、乙烯基、或胺基的基团。
硅烷化合物可以式(1)表示:
QmH3-mSiA式(1)
其中,Q(后称为第一反应取代基)各自独立为可水解基团或甲基;m=1~3;A(后称为第二反应取代基)为末端含有巯基(-SH)、环氧基、乙烯基、或胺基的基团。前述可水解基团可为烷氧基,能以-OR表示,R表示碳数为1至5的烷基。在一些实施方式中,前述可水解基团包含甲氧基(-OCH3)或乙氧基(-OCH2CH3)。在一些实施方式中,前述末端含有巯基(-SH)、环氧基、乙烯基、或胺基的基团可包含含有碳数为1至8的伸烷基(alkylene),举例来说,含有巯基(-SH)的基团可为-(CH2)n-SH,n=1~8。
前述偶合剂可包含3-硫醇基丙基三甲氧基硅烷((3-mercaptopropyl)trimethoxysilane;MPTMS)、3-硫醇基丙基甲基二甲氧基硅烷(3-mercaptopropylmethyldimethoxysilane;MPDMS)、3-缩水甘油基氧基丙基三甲氧基硅烷(3-glycidoxypropyltrimethoxysilane;GPTMS)、3-氨基丙基三甲氧基硅烷(3-Aminopropyltrimethoxysilane;APTMS)、3-氨基丙基三乙氧基硅烷(3-Aminopropyltriethoxysilane;APTES)、或其组合。
在一些实施方式中,前述金属化合物可包含金属氢氧化物或锂化合物。金属氢氧化物的金属原子可包含锂(Li)、钠(Na)、钾(K)、或其组合。金属氢氧化物包含氢氧化钠(NaOH)、氢氧化锂(LiOH)、氢氧化钾(KOH)、或其组合。锂化合物包含碳酸锂(Li2CO3)、碳酸氢锂(LiHCO3)、硫化锂(Li2S)、碳化锂(Li2C2)、磷酸二氢锂(LiH2PO4)、或其组合。
在一些实施方式中,前述负极活性材料的制备方法可包括以下步骤。首先,混合前述的偶合剂以及前述的活性粒子以得到第一混合物。偶合剂的第一反应取代基(可水解基团)可与活性粒子形成键合。例如,硅氧化物(活性粒子)可能含有羟基。偶合剂的可水解基团可与活性粒子的表面上的羟基(-OH)进行水解反应后形成键合。例如,偶合剂的可水解基团可与活性粒子的表面上的羟基进行脱水缩合反应后形成键合。第一混合物中偶合剂经与活性粒子反应后留下的残基可含有第二反应取代基(包含巯基、环氧基、乙烯基、或胺基的基团),亦即第二反应取代基可不与活性粒子反应而保留在残基中。在一些实施例中,偶合剂的重量为活性粒子的重量的0.1%至2%。
然后,将第一混合物与前述的金属化合物进行混合,以得到第二混合物。第一混合物中偶合剂的残基所含的第二反应取代基(包含巯基、环氧基、乙烯基、或胺基的基团)能与金属化合物形成键合。例如,偶合剂的第二反应取代基能与金属化合物形成氢键。例如,偶合剂的第二反应取代基能与金属化合物进行水解反应后形成键合。例如,偶合剂的第二反应取代基能与金属化合物进行脱水缩合反应后形成键合。金属化合物与偶合剂残基反应形成键合后留下来的金属化合物残基含有金属原子。在一些实施方式中,偶合剂的重量:金属化合物重量为1:1至1:10。上述反应完成后可得到前述的负极活性材料,即,负极活性材料包含活性粒子以及修饰层,修饰层披覆于活性粒子的表面;修饰层包含偶合剂的残基与金属化合物的残基,且偶合剂的残基键合在活性粒子与金属化合物的残基之间,金属化合物的残基含有金属原子。实施方式中,可将第一混合物与金属化合物的溶液进行混合,以得到第二混合物。金属化合物的溶液包括金属化合物以及溶剂。溶剂可包括水(例如去离子水)。金属化合物的溶液可为含有金属化合物的水溶液。
在一些实施方式中,前述负极活性材料可应用于作为电池的负极
本公开内容提供的电池包含负极、正极、隔离膜以及电解液,隔离膜设置在正极与负极之间以分隔正极与负极;正极与负极之间定义出容置空间,电解液设置在容置空间中,并在正极与负极之间。
电池的负极包含集电层以及活性材料层。活性材料层设置在集电层上,活性材料层包含负极活性材料、导电添加剂以及粘着剂。活性材料层可由负极活性材料浆料(或负极活性材料浆料组合物)形成。负极活性材料浆料包含负极活性材料、导电添加剂以及粘着剂。导电添加剂可包含碳黑、导电石墨、碳纳米管、碳纤维、石墨烯、或其组合。粘着剂可包含聚偏氟乙烯(poly(vinylidene fluoride);PVDF)、丁苯橡胶(styrene-butadiene rubber;SBR)、聚丙烯酸(Poly(acrylic acid);PAA)、或聚丙烯腈(Polyacrylonitrile;PAN)、聚乙二醇(PEG)、羧甲基纤维素(carboxymethyl cellulose;CMC)、聚环氧乙烷(PEO)、或其组合。集电层可包含金属,例如铜片。
前述电池的正极包含正极活性材料。正极活性材料包含锂钴氧化物(LCO)、镍钴锰酸锂(NMC)、镍钴铝酸锂(NCA)、磷酸铁锂(例如LiFePO4,简称为LFP)、或其组合。
前述的隔离膜可包含聚乙烯(polyethylene;PE)、聚丙烯(polypropylene;PP)、芳纶、陶瓷、或其组合。
前述的电解液可包含锂盐、溶剂、及压克力树脂。溶剂可为碳酸丙烯酯、碳酸乙烯酯、碳酸甲乙酯、碳酸二甲酯、碳酸二乙酯、碳酸氟化乙烯酯、或其组合。
为让本公开内容的上述目的、特征、和优点能更明显易懂,下文特举具体实施例,作详细说明如下:
<实施例1>
以负极活性材料浆料的固含量的重量为基准,将0.2重量%(wt%)作为偶合剂的3-硫醇基丙基三甲氧基硅烷,以及96.05重量%的活性粒子SiO/C(氧化硅与碳材的混合物,厂牌为贝特瑞BTR-SiO550-1A),以及0.30重量%的导电添加剂Super-p(碳黑)均匀混合以得到第一混合物。然后,在第一混合物中加入浓度为5重量%~10重量%的LiOH水溶液,LiOH水溶液中LiOH的量为活性粒子(SiO/C)的0.2重量%,以得到第二混合物,并以水合法在45℃条件下搅拌混合120分钟进行预反应处理。如此,制备的第二混合物中含有负极活性材料:经表面改质的SiO/C粒子。随后将负极活性材料(含经表面改质的SiO/C粒子),以及,以负极活性材料浆料的固含量的重量为基准,固含量占0.495重量%的导电碳液CNT(厂牌为TUBALLTM,含碳纳米管,购自OCSiAl)、固含量占1.28重量%的电极粘着剂CMC、固含量占1.48重量%的SBR等分散于去离子水中,形成均一结构的负极活性材料浆料(固含量约占43重量%)涂布于金属铜片集电层,制得负极极板。
以正极活性材料浆料的固含量的重量为基准,将97.3重量%的NMC811、1重量%的Super-p、1.4重量%的PVDF5130、以及0.3重量%的CNT均匀分散于N-甲基砒喀烷酮(NMP)溶剂中,形成均一结构的正极活性材料浆料(固含量约占70重量%)涂布于金属铝片集电层,制得正极极板。
将负极极板、正极极板与隔离膜等组装成标准电池芯(Jelly Roll),尺寸为65mm(高)x 60mm(宽)x 70mm(长),即656070标准型电池芯,灌入16.5克的液态标准电解液,封装后得锂离子二次电池。
<实施例2>
实施例2的锂离子二次电池的制造方法类似实施例1,差异在于负极活性材料浆料的制备过程中,LiOH水溶液中LiOH的量为活性粒子SiO/C的0.3重量%。
<实施例3>
实施例3的锂离子二次电池的制造方法类似实施例1,差异在于负极活性材料浆料的制备过程中,LiOH水溶液中LiOH的量为活性粒子SiO/C的0.4重量%。
<实施例4>
实施例4的锂离子二次电池的制造方法类似实施例2,差异在于负极活性材料浆料的制备过程中,LiOH水溶液是以KOH水溶液取代,KOH水溶液中KOH的量为活性粒子SiO/C的0.3重量%,并且第二混合物是以水合法在45℃条件下搅拌混合60分钟进行预反应处理。
<实施例5>
实施例5的锂离子二次电池的制造方法类似实施例1,差异在于负极活性材料浆料的制备过程中,活性粒子SiO/C(氧化硅与碳材的混合物,厂牌为贝特瑞BTR-SiO550-1A)的添加量为96.29重量%(以负极活性材料浆料的固含量的重量为基准);LiOH水溶液中LiOH的量为活性粒子SiO/C的1重量%;并且第二混合物是以水合法在45℃条件下搅拌混合60分钟进行预反应处理。
<实施例6>
实施例6的锂离子二次电池的制造方法类似实施例5,差异在于负极活性材料浆料的制备过程中,偶合剂使用3-胺丙基三乙氧基硅烷(APTES);且LiOH水溶液中LiOH的量为活性粒子SiO/C的0.2重量%。
<对比例1>
对比例1的锂离子二次电池的制造方法类似实施例1,差异在于负极活性材料是使用未经表面改质的SiO/C粒子。
<对比例2>
对比例2的锂离子二次电池的制造方法类似对比例1,差异在于对比例2使用浓度为0.2重量%的LiOH水溶液,且未使用任何偶合剂。
<评价>
表1列示实施例1~6与对比例1~2的锂离子二次电池,以0.1C充电与0.1C放电的循环方式量测出的库伦效率;以及以0.5C充电与0.5C放电的循环方式,在充电放电循环测试圈次第400、800次时的容量保持率(以最大储存电容为基准算出的百分比率)。表1
从测试数据可知,跟对比例的不具有经表面改质的SiO/C粒子的电池相比,实施例的具有经表面改质的SiO/C粒子的电池具有较长的循环寿命,以及较佳的库伦效率,包括较佳的首次(第一次)库伦效率。此外,实施例1与实施例2在第800次循环的容量保持率分别为87.6%、87.2%,皆明显优于对比例1与对比例2于第400次循环的容量保持率78.4%、74.5%。
综上所述,虽然本发明已以实施方式公开如上,然其并非用以限定本发明。本发明所属技术领域的技术人员,在不脱离本发明的精神和范围内,当可作各种更动与润饰。因此,本发明的保护范围当视所附的权利要求所界定者为准。
Claims (15)
1.负极活性材料,包含:
活性粒子,其含有硅元素、碳元素、或其组合;以及
修饰层,其披覆于所述活性粒子的表面,其中所述修饰层包含偶合剂的残基与金属化合物的残基,所述偶合剂的残基键合在所述活性粒子与所述金属化合物的残基之间,所述金属化合物的残基含有金属原子。
2.如权利要求1所述的负极活性材料,其中所述活性粒子包含硅、硅氧化物、碳修饰的氧化硅、硅碳、碳材、或其组合。
3.如权利要求1所述的负极活性材料,其中所述偶合剂为硅烷化合物,其中在所述硅烷化合物中,硅原子上的取代基为可水解基团或甲基,另一取代基为含有巯基、环氧基、乙烯基、或胺基的基团。
4.如权利要求1所述的负极活性材料,其中所述偶合剂为硅烷化合物,以式(1)表示,
QmH3-mSiA 式(1)
其中,m=1~3,
Q各自独立为可水解基团或甲基,
A为末端含有巯基(-SH)、环氧基、乙烯基、或胺基的基团。
5.如权利要求3或4所述的负极活性材料,其中所述可水解基团为烷氧基。
6.如权利要求1所述的负极活性材料,其中所述偶合剂包含3-硫醇基丙基三甲氧基硅烷、3-硫醇基丙基甲基二甲氧基硅烷、3-缩水甘油基氧基丙基三甲氧基硅烷、3-氨基丙基三甲氧基硅烷、3-氨基丙基三乙氧基硅烷、或其组合。
7.如权利要求1所述的负极活性材料,其中所述金属原子包含锂、钠、钾、或其组合。
8.如权利要求1所述的负极活性材料,其中所述金属化合物包含金属氢氧化物或锂化合物。
9.如权利要求8所述的负极活性材料,其中所述金属氢氧化物包含氢氧化钠、氢氧化锂、氢氧化钾、或其组合。
10.负极,包含:
集电层;以及
活性材料层,其在所述集电层上,并包含如权利要求1所述的负极活性材料、导电添加剂、和粘着剂。
11.如权利要求10所述的负极,其中所述导电添加剂包含碳黑、导电石墨、碳纳米管、碳纤维、石墨烯、或其组合。
12.如权利要求10所述的负极,其中所述粘着剂包含聚偏氟乙烯、丁苯橡胶、聚丙烯酸、聚丙烯腈、聚乙二醇、羧甲基纤维素、聚环氧乙烷、或其组合。
13.如权利要求10所述的负极,其中所述集电层包含铜片。
14.电池,包含:
正极;
如权利要求10所述的负极;
隔离膜,其在所述正极与所述负极之间;以及
电解液,其在所述正极与所述负极之间。
15.如权利要求14所述的电池,其中所述正极包含正极活性材料,所述正极活性材料包含锂钴氧化物、镍钴锰酸锂、镍钴铝酸锂、磷酸铁锂、或其组合。
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