CN111342017A - Multi-component silicon-oxygen negative electrode material for lithium ion battery and preparation method thereof - Google Patents
Multi-component silicon-oxygen negative electrode material for lithium ion battery and preparation method thereof Download PDFInfo
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- CN111342017A CN111342017A CN202010156329.2A CN202010156329A CN111342017A CN 111342017 A CN111342017 A CN 111342017A CN 202010156329 A CN202010156329 A CN 202010156329A CN 111342017 A CN111342017 A CN 111342017A
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- negative electrode
- silicon
- electrode material
- lithium ion
- powder
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- 239000007773 negative electrode material Substances 0.000 title claims abstract description 40
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 title claims abstract description 39
- 229910001416 lithium ion Inorganic materials 0.000 title claims abstract description 39
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- OBNDGIHQAIXEAO-UHFFFAOYSA-N [O].[Si] Chemical compound [O].[Si] OBNDGIHQAIXEAO-UHFFFAOYSA-N 0.000 title claims description 25
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 38
- 229910052744 lithium Inorganic materials 0.000 claims abstract description 33
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 31
- 239000002131 composite material Substances 0.000 claims abstract description 31
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims abstract description 23
- 239000007784 solid electrolyte Substances 0.000 claims abstract description 21
- 239000000463 material Substances 0.000 claims abstract description 18
- 239000002245 particle Substances 0.000 claims abstract description 18
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 14
- 229910052726 zirconium Inorganic materials 0.000 claims abstract description 13
- 229910052746 lanthanum Inorganic materials 0.000 claims abstract description 12
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 11
- 239000010406 cathode material Substances 0.000 claims abstract description 9
- 239000011258 core-shell material Substances 0.000 claims abstract description 7
- 239000000843 powder Substances 0.000 claims description 66
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 34
- 239000000203 mixture Substances 0.000 claims description 32
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Chemical compound [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 claims description 28
- 238000010438 heat treatment Methods 0.000 claims description 23
- 238000001816 cooling Methods 0.000 claims description 19
- 238000000034 method Methods 0.000 claims description 17
- 238000002156 mixing Methods 0.000 claims description 16
- 229910052814 silicon oxide Inorganic materials 0.000 claims description 11
- 239000011247 coating layer Substances 0.000 claims description 10
- IDBFBDSKYCUNPW-UHFFFAOYSA-N lithium nitride Chemical compound [Li]N([Li])[Li] IDBFBDSKYCUNPW-UHFFFAOYSA-N 0.000 claims description 8
- 238000012216 screening Methods 0.000 claims description 8
- 239000003792 electrolyte Substances 0.000 claims description 7
- 238000004519 manufacturing process Methods 0.000 claims description 7
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 6
- 239000012298 atmosphere Substances 0.000 claims description 6
- 239000011248 coating agent Substances 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- 230000001590 oxidative effect Effects 0.000 claims description 6
- 238000000576 coating method Methods 0.000 claims description 5
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 claims description 5
- 239000007791 liquid phase Substances 0.000 claims description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 4
- 239000001301 oxygen Substances 0.000 claims description 4
- 239000002994 raw material Substances 0.000 claims description 4
- 239000007790 solid phase Substances 0.000 claims description 4
- 239000012535 impurity Substances 0.000 claims description 3
- 239000010416 ion conductor Substances 0.000 claims description 3
- 230000000737 periodic effect Effects 0.000 claims description 3
- 238000004321 preservation Methods 0.000 claims description 3
- 150000002500 ions Chemical class 0.000 claims 1
- 239000000377 silicon dioxide Substances 0.000 abstract description 10
- 238000006243 chemical reaction Methods 0.000 abstract description 6
- 239000011244 liquid electrolyte Substances 0.000 abstract description 3
- 239000012528 membrane Substances 0.000 abstract description 3
- 230000003313 weakening effect Effects 0.000 abstract 1
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 16
- 239000012300 argon atmosphere Substances 0.000 description 10
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 description 9
- 229910052786 argon Inorganic materials 0.000 description 8
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 7
- 239000010703 silicon Substances 0.000 description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 6
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 6
- 239000006185 dispersion Substances 0.000 description 6
- 238000003756 stirring Methods 0.000 description 6
- 239000002904 solvent Substances 0.000 description 5
- 239000010936 titanium Substances 0.000 description 5
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 4
- JLRJWBUSTKIQQH-UHFFFAOYSA-K lanthanum(3+);triacetate Chemical compound [La+3].CC([O-])=O.CC([O-])=O.CC([O-])=O JLRJWBUSTKIQQH-UHFFFAOYSA-K 0.000 description 4
- 239000003960 organic solvent Substances 0.000 description 4
- -1 polyethylene Polymers 0.000 description 4
- IVORCBKUUYGUOL-UHFFFAOYSA-N 1-ethynyl-2,4-dimethoxybenzene Chemical compound COC1=CC=C(C#C)C(OC)=C1 IVORCBKUUYGUOL-UHFFFAOYSA-N 0.000 description 3
- NCOYDQIWSSMOEW-UHFFFAOYSA-K 2-hydroxypropane-1,2,3-tricarboxylate;lanthanum(3+) Chemical compound [La+3].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NCOYDQIWSSMOEW-UHFFFAOYSA-K 0.000 description 3
- DUFCMRCMPHIFTR-UHFFFAOYSA-N 5-(dimethylsulfamoyl)-2-methylfuran-3-carboxylic acid Chemical compound CN(C)S(=O)(=O)C1=CC(C(O)=O)=C(C)O1 DUFCMRCMPHIFTR-UHFFFAOYSA-N 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- BSDOQSMQCZQLDV-UHFFFAOYSA-N butan-1-olate;zirconium(4+) Chemical compound [Zr+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] BSDOQSMQCZQLDV-UHFFFAOYSA-N 0.000 description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 238000007599 discharging Methods 0.000 description 3
- 238000001704 evaporation Methods 0.000 description 3
- 239000010439 graphite Substances 0.000 description 3
- 229910002804 graphite Inorganic materials 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- XIXADJRWDQXREU-UHFFFAOYSA-M lithium acetate Chemical compound [Li+].CC([O-])=O XIXADJRWDQXREU-UHFFFAOYSA-M 0.000 description 3
- 229940071264 lithium citrate Drugs 0.000 description 3
- WJSIUCDMWSDDCE-UHFFFAOYSA-K lithium citrate (anhydrous) Chemical compound [Li+].[Li+].[Li+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O WJSIUCDMWSDDCE-UHFFFAOYSA-K 0.000 description 3
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 2
- 239000004698 Polyethylene Substances 0.000 description 2
- 239000004743 Polypropylene Substances 0.000 description 2
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 239000013543 active substance Substances 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 239000010426 asphalt Substances 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 2
- 239000006258 conductive agent Substances 0.000 description 2
- YXEUGTSPQFTXTR-UHFFFAOYSA-K lanthanum(3+);trihydroxide Chemical compound [OH-].[OH-].[OH-].[La+3] YXEUGTSPQFTXTR-UHFFFAOYSA-K 0.000 description 2
- 239000007774 positive electrode material Substances 0.000 description 2
- 239000002153 silicon-carbon composite material Substances 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 229910052719 titanium Inorganic materials 0.000 description 2
- ZFQCFWRSIBGRFL-UHFFFAOYSA-B 2-hydroxypropane-1,2,3-tricarboxylate;zirconium(4+) Chemical compound [Zr+4].[Zr+4].[Zr+4].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O.[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O.[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O.[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O ZFQCFWRSIBGRFL-UHFFFAOYSA-B 0.000 description 1
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 description 1
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 1
- 229910017569 La2(CO3)3 Inorganic materials 0.000 description 1
- 229910001290 LiPF6 Inorganic materials 0.000 description 1
- 229910014604 LixSiOy Inorganic materials 0.000 description 1
- 239000004793 Polystyrene Substances 0.000 description 1
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 description 1
- 229930006000 Sucrose Natural products 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 239000011149 active material Substances 0.000 description 1
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 description 1
- 239000010405 anode material Substances 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 description 1
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 230000008602 contraction Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 1
- 125000002534 ethynyl group Chemical group [H]C#C* 0.000 description 1
- XPFVYQJUAUNWIW-UHFFFAOYSA-N furfuryl alcohol Chemical compound OCC1=CC=CO1 XPFVYQJUAUNWIW-UHFFFAOYSA-N 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000011245 gel electrolyte Substances 0.000 description 1
- 239000008103 glucose Substances 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 238000002354 inductively-coupled plasma atomic emission spectroscopy Methods 0.000 description 1
- NZPIUJUFIFZSPW-UHFFFAOYSA-H lanthanum carbonate Chemical compound [La+3].[La+3].[O-]C([O-])=O.[O-]C([O-])=O.[O-]C([O-])=O NZPIUJUFIFZSPW-UHFFFAOYSA-H 0.000 description 1
- 229960001633 lanthanum carbonate Drugs 0.000 description 1
- NCRUJFPNHKQCJG-UHFFFAOYSA-K lanthanum(3+);propanoate Chemical compound [La+3].CCC([O-])=O.CCC([O-])=O.CCC([O-])=O NCRUJFPNHKQCJG-UHFFFAOYSA-K 0.000 description 1
- PLOSEKHZRPLNLO-UHFFFAOYSA-K lanthanum(3+);triformate Chemical compound [La+3].[O-]C=O.[O-]C=O.[O-]C=O PLOSEKHZRPLNLO-UHFFFAOYSA-K 0.000 description 1
- 239000010410 layer Substances 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
- XKPJKVVZOOEMPK-UHFFFAOYSA-M lithium;formate Chemical compound [Li+].[O-]C=O XKPJKVVZOOEMPK-UHFFFAOYSA-M 0.000 description 1
- AXMOZGKEVIBBCF-UHFFFAOYSA-M lithium;propanoate Chemical compound [Li+].CCC([O-])=O AXMOZGKEVIBBCF-UHFFFAOYSA-M 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- YQCIWBXEVYWRCW-UHFFFAOYSA-N methane;sulfane Chemical compound C.S YQCIWBXEVYWRCW-UHFFFAOYSA-N 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 238000003801 milling Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000011255 nonaqueous electrolyte Substances 0.000 description 1
- 125000004430 oxygen atom Chemical group O* 0.000 description 1
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 229920001568 phenolic resin Polymers 0.000 description 1
- 239000005011 phenolic resin Substances 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 229920002223 polystyrene Polymers 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 1
- XPGAWFIWCWKDDL-UHFFFAOYSA-N propan-1-olate;zirconium(4+) Chemical compound [Zr+4].CCC[O-].CCC[O-].CCC[O-].CCC[O-] XPGAWFIWCWKDDL-UHFFFAOYSA-N 0.000 description 1
- 239000001294 propane Substances 0.000 description 1
- TVCBSVKTTHLKQC-UHFFFAOYSA-M propanoate;zirconium(4+) Chemical compound [Zr+4].CCC([O-])=O TVCBSVKTTHLKQC-UHFFFAOYSA-M 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 238000010532 solid phase synthesis reaction Methods 0.000 description 1
- 239000011232 storage material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000005720 sucrose Substances 0.000 description 1
- JMXKSZRRTHPKDL-UHFFFAOYSA-N titanium ethoxide Chemical compound [Ti+4].CC[O-].CC[O-].CC[O-].CC[O-] JMXKSZRRTHPKDL-UHFFFAOYSA-N 0.000 description 1
- XJUNLJFOHNHSAR-UHFFFAOYSA-J zirconium(4+);dicarbonate Chemical compound [Zr+4].[O-]C([O-])=O.[O-]C([O-])=O XJUNLJFOHNHSAR-UHFFFAOYSA-J 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
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
- H01M4/366—Composites as layered products
-
- 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
- H01M10/0561—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of inorganic materials only
- H01M10/0562—Solid materials
-
- 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
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- 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
-
- 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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
-
- 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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
-
- 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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
-
- 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
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Landscapes
- Chemical & Material Sciences (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Engineering & Computer Science (AREA)
- Inorganic Chemistry (AREA)
- Composite Materials (AREA)
- Manufacturing & Machinery (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Materials Engineering (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention relates to a multi-element composite silica negative electrode material for a lithium ion battery and a preparation method thereof, and relates to the technical field of new materials, wherein the negative electrode material comprises six elements of Si, O, Li, C, La and Zr, the negative electrode material comprises a plurality of particle units, and each particle unit is of a core-shell structure; weakening the reaction of the cathode material and the liquid electrolyte to generate the solid electrolyte after the battery is manufactured, and reducing the lithium consumption for forming the solid electrolyte membrane due to the reaction; as a result, the purpose of improving the first efficiency and the cycle life can be achieved.
Description
Technical Field
The invention relates to the technical field of new materials, in particular to a multi-component composite silica negative electrode material and a preparation method thereof, and particularly relates to a multi-component composite silica negative electrode material for a lithium ion battery and a preparation method thereof.
Background
It is known that as portable electric appliances such as mobile phones, notebook computers, tablet computers, etc. are rapidly popularized, the market demand for rechargeable batteries with high energy density is also increased, and thus the demand for lithium ion secondary batteries is explosively increased. Meanwhile, with the rapid development of electric vehicles, especially electric automobiles in recent years, the demand for lithium ion secondary batteries has further increased. In practical applications, the application end requires that the lithium ion secondary battery has the characteristics of high energy density, long cycle life and the like.
The energy density of a lithium ion secondary battery is directly related to the lithium storage capacity of the positive electrode material and the negative electrode material. Taking the negative electrode material as an example, the negative electrode material is usually graphite, the theoretical energy density of the graphite is 372mAh/g, the current development and application are mature, and the requirements of market application ends are difficult to meet. The necessity and urgency for the development of higher capacity anode materials are particularly prominent.
It was found that silicon can also be used as a negative electrode active material, and the theoretical energy density was 4200 mAh/g. The silicon has large lithium storage capacity, large volume expansion and contraction change during charge and discharge cycles, and easy pulverization. Silicon reacts with electrolyte during charge and discharge cycles, resulting in electrolyte consumption, low cycle life of the battery, and the like.
The silicon monoxide is also a negative electrode active substance, the theoretical energy density of the silicon monoxide reaches 2000mAh/g, is lower than that of simple substance silicon, the volume expansion and shrinkage change is reduced during corresponding charge-discharge circulation, the reaction active liquid with the electrolyte is reduced, the cycle life is prolonged, and the silicon monoxide is a lithium ion secondary battery negative electrode material with practical prospect. As a negative electrode lithium storage material, during charging and discharging of a battery, lithium coming from a positive electrode material penetrates through the surface and enters into the interior of the silicon protoxide, only a part of the lithium can return to the positive electrode to play a role in circulation, and the rest part of the lithium is respectively consumed on the surface and the interior of the silicon protoxide, so that the first charging and discharging efficiency of the battery is low, and the problem which needs to be solved by application is solved.
Through search, Chinese patent, patent application number is: 97120801.8, publication number: CN1188335A, filed as follows: on the day 28 of 11/1997, the patent names: a non-aqueous electrolyte secondary battery and a method for manufacturing the same, which are primarily improved by introducing lithium into silicon oxide at a material preparation stage to form a lithium-containing silicon oxide expressed as LixSiOy (0< x,0< y <2) c. Chinese patent, patent application number is: 02112180.X, publication no: CN1402366A, filed as follows: day 21, 06/2002, with patent names: the silicon-carbon composite material with high specific capacity for the lithium ion battery negative electrode and the preparation method thereof realize the coating of a layer of carbon on the surface of negative electrode active materials such as silicon monoxide and the like by a method of compounding the silicon-carbon composite material with a carbon material, and further improve the performance. Although the industry's efforts to improve have continued, the problems affecting the utility of the material still remain, the first time the efficiency is low and the cycle life is not long enough.
Therefore, how to provide the multi-component silicon-oxygen cathode material for the lithium ion battery and the preparation method thereof become a long-term technical demand of the technical personnel in the field.
Disclosure of Invention
The invention provides a multi-element composite silica cathode material for a lithium ion battery and a preparation method thereof, aiming at overcoming the defects in the background technology.
In order to achieve the above purpose, the invention adopts the following technical scheme:
the multi-component composite silica negative electrode material for the lithium ion battery comprises the following components in percentage by weight:
the multi-component composite silica negative electrode material for the lithium ion battery comprises a plurality of particle units, and each particle unit is of a core-shell structure.
The multi-element composite silicon-oxygen negative electrode material for the lithium ion battery is a crystalline and amorphous mixed structure formed by four elements including Si, O, Li and C in a core part of each particle unit, and an amorphous structure mixture formed by O, Li, C, La and Zr in a core part of each particle unit.
According to the multielement composite silicon-oxygen negative electrode material for the lithium ion battery, the core-shell part forms a solid electrolyte LixLayZr2O12 with 9< x +3y <16 by using O, Li, La and Zr elements, and then forms a composite shell mainly comprising electron-conductive C and ion-conductive solid electrolyte.
The Zr element can be replaced by a same group element Ti in the periodic table, the electrolyte formed after the Ti element is replaced is LixLayTi2O6, 3< x +3y <4, and then the composite shell is mainly composed of an electron-conductive C and ion-conductive solid electrolyte LixLayTi2O6, 3< x +3y < 4.
The preparation method of the multi-component silicon-oxygen negative electrode material for the lithium ion battery specifically comprises the following steps:
firstly, adopting silicon monoxide powder with a carbon coating layer on the surface, uniformly mixing the silicon monoxide powder with lithium source powder under the protection of a non-oxidizing atmosphere, heating the mixed material to 350-750 ℃, preserving heat for 2-24 hours, and cooling to room temperature to obtain base powder;
secondly, uniformly mixing the basic powder obtained in the previous step with a solid electrolyte LixLayZr2O12, 9< x +3y <16 or LixLayTi2O6, 3< x +3y <4 material by a solid-phase or liquid-phase mixing method, drying, heating to 100-600 ℃ under a non-oxidizing atmosphere, carrying out heat preservation treatment for 1-6 hours, and cooling to room temperature to obtain target powder;
and thirdly, scattering, removing impurities and screening the target powder obtained in the last step to obtain the required multi-element composite silicon-oxygen cathode material.
According to the preparation method of the multi-component composite silicon-oxygen cathode material for the lithium ion battery, the silicon oxide powder with the carbon coating layer on the surface is composite powder obtained by codeposition of silicon oxide and carbon or powder obtained by carbon coating after the silicon oxide powder is prepared.
According to the preparation method of the multi-component composite silica negative electrode material for the lithium ion battery, the particle size of the silicon monoxide powder with the carbon coating layer on the surface is 1-20 microns.
According to the preparation method of the multi-component composite silicon-oxygen cathode material for the lithium ion battery, the lithium source powder is one or a mixture of Li3N or LiH.
According to the preparation method of the multi-element composite silica negative electrode material for the lithium ion battery, the solid electrolyte LixLayZr2O12, 9< x +3y <16 material is a lithium ion conductor which is synthesized by reacting various raw materials respectively containing a lithium source, a lanthanum source, a zirconium source and an oxygen source in the manufacturing process.
By adopting the technical scheme, the invention has the following advantages:
according to the invention, according to the working principle of the lithium ion secondary battery, the process of inefficiently consuming the lithium material by the negative electrode material after the battery is formed is advanced to be pre-completed in the material manufacturing process, so that the requirement characteristic of high efficiency and long cycle life of the negative electrode material for the first time is achieved; the lithium ion solid electrolyte membrane is formed on the surface of the negative electrode material particles in advance, so that the reaction of the negative electrode material and the liquid electrolyte to generate the solid electrolyte after the battery is manufactured is weakened, and the lithium consumption for forming the solid electrolyte membrane due to the reaction is reduced; as a result, the purposes of improving the first efficiency and prolonging the cycle life can be achieved, and the method is suitable for large-scale popularization and application.
Detailed Description
The present invention will be explained in more detail by the following examples, which are not intended to limit the invention;
the multi-component composite silica negative electrode material for the lithium ion battery comprises the following components in percentage by weight:
the multi-component silicon-oxygen negative electrode material comprises a plurality of particle units, and each particle unit is of a core-shell structure. The core part in each particle unit is a crystalline and amorphous mixed structure composed of four elements of Si, O, Li and C, and the core part in each particle unit is an amorphous structure mixture composed of O, Li, C, La and Zr.
Further, the core-shell portion forms a solid electrolyte LixLayZr2O12, 9< x +3y <16, from O, Li, La and Zr elements, and then a composite shell composed mainly of an electron-conductive C and an ion-conductive solid electrolyte.
In specific implementation, the Zr element can be replaced by Ti element in the same group of the periodic table, the electrolyte formed after the Ti element is replaced is LixLayTi2O6, 3< x +3y <4, and then the composite shell is mainly composed of an electron-conductive C and ion-conductive solid electrolyte LixLayTi2O6, 3< x +3y < 4.
The preparation method of the multi-component silicon-oxygen negative electrode material for the lithium ion battery specifically comprises the following steps:
firstly, adopting silicon monoxide powder with a carbon coating layer on the surface, uniformly mixing the silicon monoxide powder with lithium source powder under the protection of a non-oxidizing atmosphere, heating the mixed material to 350-750 ℃, preserving heat for 2-24 hours, and cooling to room temperature to obtain base powder; the silicon oxide powder with the carbon coating layer on the surface is composite powder obtained by codeposition of silicon oxide and carbon or powder obtained by carbon coating after the silicon oxide powder is prepared; the carbon source for coating carbon can be any one or a combination of two or more of sucrose, glucose, citric acid, asphalt, furfuryl alcohol resin, phenolic resin, polyethylene, polystyrene, polypropylene, methane, propane and acetylene, and the method is not limited to be a gas phase method, a liquid phase method or a solid phase method; the particle size of the silicon monoxide powder with the carbon coating layer on the surface is 1-20 microns, preferably 1-10 microns, and further preferably 3-8 microns; the lithium source powder is any one or a mixture of two of Li3N or LiH;
secondly, uniformly mixing the basic powder obtained in the previous step with a solid electrolyte LixLayZr2O12, 9< x +3y <16 or LixLayTi2O6, 3< x +3y <4 material by a solid-phase or liquid-phase mixing method, drying, heating to 100-600 ℃ under a non-oxidizing atmosphere, carrying out heat preservation treatment for 1-6 hours, and cooling to room temperature to obtain target powder; the solid electrolyte LixLayZr2O12, 9< x +3y <16 material is a lithium ion conductor which is synthesized by reacting various raw materials respectively containing a lithium source, a lanthanum source, a zirconium source and an oxygen source in the manufacturing process;
and thirdly, scattering, removing impurities and screening the target powder obtained in the last step to obtain the required multi-element composite silicon-oxygen cathode material.
In the practice of the invention, the lithium source is any one or a combination of two or more of lithium formate, lithium acetate, lithium propionate, lithium citrate, lithium carbonate and lithium hydroxide.
Further, the lanthanum source is any one or a combination of two or more of lanthanum formate, lanthanum acetate, lanthanum propionate, lanthanum citrate, lanthanum carbonate and lanthanum hydroxide.
The zirconium source is any one or a combination of two or more of zirconium acid, zirconium acetate, zirconium propionate, zirconium citrate, zirconium carbonate, zirconium hydroxide, methyl zirconate, ethyl zirconate, propyl zirconate and butyl zirconate.
Further, the titanium source is any one or a combination of two or more of nano titanium dioxide, metatitanic acid, methyl titanate, ethyl titanate, propyl titanate and butyl titanate.
Further, the oxygen source has been included in lithium sources, lanthanum sources, zirconium sources.
Further, the solid phase mixing means any one or a combination of two or more of fusion, mixing and milling, mechanical mixing, high-speed mechanical mixing and ball milling.
Further, the liquid phase mixing refers to a method of adding the raw materials into a liquid solvent to perform dispersion, mixing and reaction respectively. The liquid solvent is any one or a combination of two or more of organic solvents of ethanol, propanol, isopropanol, butanol, ethyl acetate, acetone and toluene.
The invention has the characteristics of high charging and discharging efficiency, long cycle life, simple equipment and easy commercial production.
The specific embodiment of the invention is as follows:
the invention adopts ICP-AES as an analysis means of material components and adopts a high-frequency induction carbon-sulfur analyzer as an analysis means of carbon content. The materials obtained in examples and comparative examples were used to fabricate button-type secondary batteries, and the use properties of the materials were evaluated.
First, a silicon monoxide powder having a carbon coating layer is prepared. Taking commercially available silica powder with the molar ratio of silicon to oxygen atoms of 1:1 and the granularity D50 of 6 microns, taking high-temperature petroleum asphalt powder as a carbon coating agent, mechanically mixing the two kinds of powder according to a proper proportion by using a high-speed mixer, putting the mixture into a vacuum heating furnace, heating to 800 ℃, preserving heat for 2 hours, cooling to room temperature, scattering and screening for later use. By adopting the method, three basic powders with carbon contents of 2.5%, 5.2% and 7.6% are respectively obtained.
Example 1
100g of basic powder with the carbon content of 2.5 percent and 10g of Li3N powder are taken and mixed evenly in an argon protection box; then placing the mixture in an argon atmosphere for heat treatment at 500 ℃ for 12h, and naturally cooling the mixture to room temperature. Adding 0.2g of lithium hydroxide, 0.7g of lanthanum hydroxide and 0.9g of zirconium acetate into 100g of the powder, and uniformly fusing by high-speed dispersion; and then placing the mixture in an argon atmosphere for heat treatment at 600 ℃ for 1h, naturally cooling the mixture to room temperature, and scattering and screening the mixture to obtain a finished product.
Example 2
100g of basic powder with the carbon content of 5.2 percent and 10g of LiH powder are taken and mixed evenly in an argon protection box; then placing the mixture in an argon atmosphere for heat treatment at 600 ℃ for 6h, and naturally cooling the mixture to room temperature. Adding 1g of lithium citrate, 3g of lanthanum citrate and 1g of zirconium hydroxide into 100g of the powder, and uniformly fusing by high-speed dispersion; and then placing the mixture in an argon atmosphere for heat treatment at 550 ℃ for 2h, naturally cooling the mixture to room temperature, and scattering and screening the mixture to obtain a finished product.
Example 3
100g of basic powder with the carbon content of 7.6 percent and 20g of Li3N powder are taken and mixed evenly in an argon protection box; then placing the mixture in an argon atmosphere for heat treatment at 400 ℃ for 24 hours, and naturally cooling the mixture to room temperature. 1g of lithium acetate, 4.5g of lanthanum acetate and 2g of zirconium hydroxide are added into 100g of the powder, and the powder is uniformly dispersed and fused at a high speed; and then placing the mixture in an argon atmosphere for heat treatment at 550 ℃ for 6 hours, naturally cooling the mixture to room temperature, and scattering and screening the mixture to obtain a finished product.
Example 4
100g of basic powder with the carbon content of 2.5 percent and 5g of LiH powder are taken and mixed evenly in an argon protection box; then placing the mixture in an argon atmosphere for heat treatment at 500 ℃ for 12h, and naturally cooling the mixture to room temperature. Adding 100g of organic solvent ethyl acetate into a stirring dispersion machine, then respectively adding 100g of the basic powder, 1g of lithium acetate, 3.5g of lanthanum acetate and 3g of butyl zirconate, uniformly dispersing and stirring, heating to 100 ℃, evaporating, drying to remove the solvent, then preserving heat at 300 ℃ for 6 hours for heat treatment,
example 5
100g of basic powder with the carbon content of 5.2 percent and 13g of Li3N powder are taken and mixed evenly in an argon protection box; then placing the mixture in an argon atmosphere for heat treatment at 600 ℃ for 6h, and naturally cooling the mixture to room temperature. Adding 100g of isopropanol serving as an organic solvent into a stirring dispersion machine, then respectively adding 100g of the basic powder, 0.2g of lithium hydroxide, 2.4g of lanthanum citrate and 2g of butyl zirconate, uniformly dispersing and stirring, heating to 100 ℃, evaporating, drying and removing the solvent, then carrying out heat treatment at 400 ℃ for 4 hours, and cooling to obtain the required finished product.
Example 6
100g of basic powder with the carbon content of 7.6 percent and 20g of Li3N powder are taken and mixed evenly in an argon protection box; then placing the mixture in an argon atmosphere for heat treatment at 400 ℃ for 24 hours, and naturally cooling the mixture to room temperature. Adding 100g of organic solvent ethanol into a stirring dispersion machine, then respectively adding 100g of the basic powder, 1g of lithium citrate, 4g of lanthanum acetate and 3g of zirconium acetate, uniformly dispersing and stirring, heating to 100 ℃, evaporating, drying and removing the solvent, then preserving heat at 500 ℃ for 6h, and cooling to obtain the required finished product.
Comparative example 1
The base powder with 5.2% carbon content coated by carbon is directly used as a finished product.
Comparative example 2
100g of basic powder with the carbon content of 5.2 percent and 13g of Li3N powder are taken and mixed evenly in an argon protection box; and then placing the mixture in an argon atmosphere for heat treatment at 600 ℃ for 6h, naturally cooling the mixture to room temperature, and scattering and screening the mixture to obtain a finished product.
The composition of samples of the finished products of examples and comparative examples was analyzed, and the results are shown in the following table:
the lithium ion battery negative electrode materials prepared in the examples and the comparative examples are respectively used as active materials for manufacturing button batteries with metal lithium sheets as counter electrodes. The slurry adopts the proportion of active substances, conductive agents and binders in a ratio of 75:15:10, wherein the conductive agents are conductive carbon black SP and conductive graphite KS-6/SFG-6, and the binders are CMC + SBR. LiPF6/DEC + DMC + EC + FEC electrolyte and PE/PP diaphragm are adopted. The battery is manufactured in an argon protection glove box, the charge and discharge test adopts the charge and discharge rate of 0.005V-1.5V and the voltage of 0.1C, and the test results are shown in the following table:
it can be seen from the results of battery tests of examples and comparative examples that the effective capacity, first efficiency and cycle performance of the battery were significantly improved by using the negative active material of the present invention.
The invention can be used for solid electrolyte batteries, gel electrolyte batteries and liquid electrolyte batteries.
The present invention is not described in detail in the prior art.
The embodiments selected for the purpose of disclosing the invention, are presently considered to be suitable, it being understood, however, that the invention is intended to cover all variations and modifications of the embodiments which fall within the spirit and scope of the invention.
Claims (10)
1. The multi-component silicon-oxygen cathode material for the lithium ion battery is characterized in that: the multielement composite silicon-oxygen negative electrode material comprises the following components in percentage by weight:
2. the multi-component silicon-oxygen negative electrode material for the lithium ion battery as claimed in claim 1, wherein: the multi-component composite silicon-oxygen negative electrode material comprises a plurality of particle units, and each particle unit is of a core-shell structure.
3. The multi-component silicon-oxygen negative electrode material for the lithium ion battery as claimed in claim 2, wherein: the core part in each particle unit is a crystalline and amorphous mixed structure composed of four elements of Si, O, Li and C, and the core part in each particle unit is an amorphous structure mixture composed of O, Li, C, La and Zr.
4. The multi-component silicon-oxygen negative electrode material for the lithium ion battery as claimed in claim 3, wherein: the core-shell part forms a solid electrolyte LixLayZr2O12 with 9< x +3y <16 by O, Li, La and Zr elements, and then is a composite shell mainly composed of electron conductive C and ion conductive solid electrolyte.
5. The multi-component silicon-oxygen negative electrode material for the lithium ion battery as claimed in claim 1, wherein: the Zr element can be replaced by a same group element Ti in the periodic table, an electrolyte formed by replacing the Ti element is LixLayTi2O6, 3< x +3y <4, and then a composite shell is formed by taking an electron-conductive C and ion-conductive solid electrolyte LixLayTi2O6, 3< x +3y <4 as a main body.
6. The method for preparing the multi-component silicon-oxygen negative electrode material for the lithium ion battery according to any one of claims 1 to 5, which is characterized by comprising the following steps: the preparation method specifically comprises the following steps:
firstly, adopting silicon monoxide powder with a carbon coating layer on the surface, uniformly mixing the silicon monoxide powder with lithium source powder under the protection of a non-oxidizing atmosphere, heating the mixed material to 350-750 ℃, preserving heat for 2-24 hours, and cooling to room temperature to obtain base powder;
secondly, uniformly mixing the basic powder obtained in the previous step with a solid electrolyte LixLayZr2O12, 9< x +3y <16 or LixLayTi2O6, 3< x +3y <4 material by a solid-phase or liquid-phase mixing method, drying, heating to 100-600 ℃ under a non-oxidizing atmosphere, carrying out heat preservation treatment for 1-6 hours, and cooling to room temperature to obtain target powder;
and thirdly, scattering, removing impurities and screening the target powder obtained in the last step to obtain the required multi-element composite silicon-oxygen cathode material.
7. The method for preparing the multi-element composite silicon-oxygen negative electrode material for the lithium ion battery according to claim 6, which is characterized by comprising the following steps of: the silicon oxide powder with the carbon coating layer on the surface is composite powder obtained by codeposition of silicon oxide and carbon or powder obtained by carbon coating after the silicon oxide powder is prepared.
8. The method for preparing the multi-element composite silicon-oxygen negative electrode material for the lithium ion battery according to claim 6, which is characterized by comprising the following steps of: the particle size of the silicon monoxide powder with the carbon coating layer on the surface is 1-20 microns.
9. The method for preparing the multi-element composite silicon-oxygen negative electrode material for the lithium ion battery according to claim 6, which is characterized by comprising the following steps of: the lithium source powder is any one or a mixture of Li3N or LiH.
10. The method for preparing the multi-element composite silicon-oxygen negative electrode material for the lithium ion battery according to claim 6, which is characterized by comprising the following steps of: the solid electrolyte LixLayZr2O12, 9< x +3y <16 material is a lithium ion conductor which is synthesized by reacting various raw materials respectively containing a lithium source, a lanthanum source, a zirconium source and an oxygen source in the manufacturing process.
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