CN114551843A - Positive electrode material and preparation method and application thereof - Google Patents
Positive electrode material and preparation method and application thereof Download PDFInfo
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- CN114551843A CN114551843A CN202210189239.2A CN202210189239A CN114551843A CN 114551843 A CN114551843 A CN 114551843A CN 202210189239 A CN202210189239 A CN 202210189239A CN 114551843 A CN114551843 A CN 114551843A
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- positive electrode
- manganese oxide
- lithium nickel
- nickel manganese
- electrode material
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- 239000007774 positive electrode material Substances 0.000 title claims abstract description 48
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- FRMOHNDAXZZWQI-UHFFFAOYSA-N lithium manganese(2+) nickel(2+) oxygen(2-) Chemical compound [O-2].[Mn+2].[Ni+2].[Li+] FRMOHNDAXZZWQI-UHFFFAOYSA-N 0.000 claims abstract description 88
- 239000010406 cathode material Substances 0.000 claims abstract description 44
- 238000003756 stirring Methods 0.000 claims abstract description 40
- 238000010438 heat treatment Methods 0.000 claims abstract description 36
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 34
- 238000001354 calcination Methods 0.000 claims abstract description 31
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 23
- 238000002156 mixing Methods 0.000 claims abstract description 22
- 239000000413 hydrolysate Substances 0.000 claims abstract description 16
- 239000003960 organic solvent Substances 0.000 claims abstract description 16
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229910001416 lithium ion Inorganic materials 0.000 claims abstract description 12
- ZYXUQEDFWHDILZ-UHFFFAOYSA-N [Ni].[Mn].[Li] Chemical compound [Ni].[Mn].[Li] ZYXUQEDFWHDILZ-UHFFFAOYSA-N 0.000 claims abstract description 3
- 239000002245 particle Substances 0.000 claims description 30
- 239000000463 material Substances 0.000 claims description 28
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 23
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 19
- 239000011572 manganese Substances 0.000 claims description 18
- 238000000034 method Methods 0.000 claims description 18
- VZGDMQKNWNREIO-UHFFFAOYSA-N tetrachloromethane Chemical group ClC(Cl)(Cl)Cl VZGDMQKNWNREIO-UHFFFAOYSA-N 0.000 claims description 18
- 229910052744 lithium Inorganic materials 0.000 claims description 14
- 239000000377 silicon dioxide Substances 0.000 claims description 13
- 238000001291 vacuum drying Methods 0.000 claims description 12
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 11
- AMWRITDGCCNYAT-UHFFFAOYSA-L hydroxy(oxo)manganese;manganese Chemical group [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 claims description 11
- 229910052748 manganese Inorganic materials 0.000 claims description 11
- 229910052759 nickel Inorganic materials 0.000 claims description 11
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical group [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 claims description 9
- 229910052808 lithium carbonate Inorganic materials 0.000 claims description 9
- 229910000480 nickel oxide Inorganic materials 0.000 claims description 9
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical group [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 claims description 9
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 claims description 8
- 238000001914 filtration Methods 0.000 claims description 8
- 235000012239 silicon dioxide Nutrition 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 4
- 229910052751 metal Inorganic materials 0.000 claims description 3
- 229910052596 spinel Inorganic materials 0.000 claims description 3
- 239000011029 spinel Substances 0.000 claims description 3
- 238000006243 chemical reaction Methods 0.000 claims description 2
- 239000002184 metal Substances 0.000 claims description 2
- 238000004321 preservation Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 4
- 239000003792 electrolyte Substances 0.000 abstract description 10
- 238000007086 side reaction Methods 0.000 abstract description 4
- 238000000576 coating method Methods 0.000 description 19
- 230000000052 comparative effect Effects 0.000 description 15
- 239000011248 coating agent Substances 0.000 description 14
- 239000007787 solid Substances 0.000 description 12
- 239000010410 layer Substances 0.000 description 10
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Chemical compound [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 10
- 239000002904 solvent Substances 0.000 description 10
- 238000001816 cooling Methods 0.000 description 7
- LQKOJSSIKZIEJC-UHFFFAOYSA-N manganese(2+) oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[Mn+2].[Mn+2].[Mn+2].[Mn+2] LQKOJSSIKZIEJC-UHFFFAOYSA-N 0.000 description 7
- 239000011259 mixed solution Substances 0.000 description 7
- 238000010992 reflux Methods 0.000 description 6
- 239000003513 alkali Substances 0.000 description 5
- 239000012153 distilled water Substances 0.000 description 5
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 4
- 229910052681 coesite Inorganic materials 0.000 description 4
- 229910052906 cristobalite Inorganic materials 0.000 description 4
- 230000014759 maintenance of location Effects 0.000 description 4
- 229910052682 stishovite Inorganic materials 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 229910052905 tridymite Inorganic materials 0.000 description 4
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 239000007790 solid phase Substances 0.000 description 3
- OIFBSDVPJOWBCH-UHFFFAOYSA-N Diethyl carbonate Chemical compound CCOC(=O)OCC OIFBSDVPJOWBCH-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- KMTRUDSVKNLOMY-UHFFFAOYSA-N Ethylene carbonate Chemical compound O=C1OCCO1 KMTRUDSVKNLOMY-UHFFFAOYSA-N 0.000 description 2
- 229910000572 Lithium Nickel Cobalt Manganese Oxide (NCM) Inorganic materials 0.000 description 2
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 2
- 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 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 238000005253 cladding Methods 0.000 description 2
- 229910017052 cobalt Inorganic materials 0.000 description 2
- 239000010941 cobalt Substances 0.000 description 2
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 2
- 230000001351 cycling effect Effects 0.000 description 2
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 description 2
- 239000011888 foil Substances 0.000 description 2
- BDKWOJYFHXPPPT-UHFFFAOYSA-N lithium dioxido(dioxo)manganese nickel(2+) Chemical compound [Mn](=O)(=O)([O-])[O-].[Ni+2].[Li+] BDKWOJYFHXPPPT-UHFFFAOYSA-N 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- QPJSUIGXIBEQAC-UHFFFAOYSA-N n-(2,4-dichloro-5-propan-2-yloxyphenyl)acetamide Chemical compound CC(C)OC1=CC(NC(C)=O)=C(Cl)C=C1Cl QPJSUIGXIBEQAC-UHFFFAOYSA-N 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 description 1
- XDLMVUHYZWKMMD-UHFFFAOYSA-N 3-trimethoxysilylpropyl 2-methylprop-2-enoate Chemical compound CO[Si](OC)(OC)CCCOC(=O)C(C)=C XDLMVUHYZWKMMD-UHFFFAOYSA-N 0.000 description 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229910001290 LiPF6 Inorganic materials 0.000 description 1
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 1
- 239000002033 PVDF binder Substances 0.000 description 1
- 108010009736 Protein Hydrolysates Proteins 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 239000010405 anode material Substances 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
- 239000011247 coating layer Substances 0.000 description 1
- 230000002860 competitive effect Effects 0.000 description 1
- 239000006258 conductive agent Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- QHGJSLXSVXVKHZ-UHFFFAOYSA-N dilithium;dioxido(dioxo)manganese Chemical compound [Li+].[Li+].[O-][Mn]([O-])(=O)=O QHGJSLXSVXVKHZ-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 229910052809 inorganic oxide Inorganic materials 0.000 description 1
- GELKBWJHTRAYNV-UHFFFAOYSA-K lithium iron phosphate Chemical compound [Li+].[Fe+2].[O-]P([O-])([O-])=O GELKBWJHTRAYNV-UHFFFAOYSA-K 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Natural products C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 125000000956 methoxy group Chemical group [H]C([H])([H])O* 0.000 description 1
- 239000002052 molecular layer Substances 0.000 description 1
- 238000004537 pulping Methods 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- BPSIOYPQMFLKFR-UHFFFAOYSA-N trimethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CO[Si](OC)(OC)CCCOCC1CO1 BPSIOYPQMFLKFR-UHFFFAOYSA-N 0.000 description 1
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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
- H01M10/42—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
- H01M4/36—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
- H01M4/50—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
- 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
- H01M4/52—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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- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/628—Inhibitors, e.g. gassing inhibitors, corrosion inhibitors
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- 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
- H01M2004/028—Positive electrodes
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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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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract
The invention relates to the technical field of lithium ion batteries, in particular to a positive electrode material and a preparation method and application thereof. The preparation method of the cathode material provided by the invention comprises the following steps: mixing a lithium nickel manganese oxide positive electrode material, a silane coupling agent, an organic solvent and water, heating and stirring to obtain lithium nickel manganese oxide coated with a silane coupling agent hydrolysate; and calcining the lithium nickel manganese coated by the silane coupling agent hydrolysate to obtain the cathode material. The positive electrode material prepared by the preparation method provided by the invention can greatly reduce the contact surface of the lithium nickel manganese oxide and the electrolyte, so that the occurrence of side reactions of the lithium nickel manganese oxide battery under high temperature and high pressure is greatly reduced, and the cycle performance of the battery under the harsh conditions of high temperature and high pressure is improved.
Description
Technical Field
The invention relates to the technical field of lithium ion batteries, in particular to a positive electrode material and a preparation method and application thereof.
Background
With the development of the electric automobile industry, the requirements of automobile enterprises on battery enterprises are increasing, and positive electrode materials with high specific energy, long service life and low cost and batteries thereof are urgently needed. Among them, the lithium ion battery is favored by battery enterprises due to its advantages of high working voltage, large specific energy, long cycle life, little pollution, etc.
Currently, commonly used lithium ion battery positive electrode materials are lithium cobaltate, lithium manganate, lithium nickel cobalt manganese oxide, lithium iron phosphate, high-voltage lithium nickel manganese oxide and the like. Because cobalt is expensive, and lithium cobaltate and lithium nickel cobalt manganese oxide have great potential safety hazards when used for power batteries. Therefore, compared with a cobalt-containing positive electrode material, the lithium nickel manganese oxide is an ideal positive electrode material for a lithium ion power battery, but the lithium nickel manganese oxide material is different from other positive electrode materials, the discharge voltage plateau of the lithium nickel manganese oxide material is as high as 4.7V, and the cycle performance under the conditions of high pressure and high temperature is not ideal.
In order to improve the cycle performance of the lithium nickel manganese oxide material under the conditions of high temperature and high pressure, two methods of doping and coating are mainly used at present, wherein the doping method is to dope some metal elements in the process of preparing the lithium nickel manganese oxide so as to improve the conductivity and the structural stability of the lithium nickel manganese oxide; the coating method is a solid-phase mixed coating method, in which metal oxide or inorganic oxide is directly mixed with lithium nickel manganese oxide, the obtained coated surface is in a particle dotted state, the surface of the lithium nickel manganese oxide still contacts with electrolyte in a large area, a large amount of side reactions still occur with the electrolyte under the conditions of high temperature and high pressure, gas generation is serious, and the cycle performance is poor.
Disclosure of Invention
The invention aims to solve the problems that the existing coating method is difficult to isolate electrolyte and prevent side reactions under high temperature and high pressure when coating the lithium nickel manganese oxide, and further the defect of limiting the cycle performance of the lithium nickel manganese oxide material under the condition of high temperature and high pressure is overcome, and further the invention provides the positive electrode material and the preparation method and the application thereof.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of a positive electrode material comprises the following steps:
1) mixing a lithium nickel manganese oxide positive electrode material, a silane coupling agent, an organic solvent and water, heating and stirring to obtain lithium nickel manganese oxide coated with a silane coupling agent hydrolysate;
2) and calcining the lithium nickel manganese coated by the silane coupling agent hydrolysate to obtain the cathode material.
Preferably, the mass ratio of the lithium nickel manganese oxide positive electrode material, the silane coupling agent, the organic solvent and the water is 100: (5-7): (750-850): (1-1.5).
Preferably, the silane coupling agent is selected from at least one of KH570, KH560 and KH 550;
the organic solvent is carbon tetrachloride.
Wherein KH570 is gamma-methacryloxypropyltrimethoxysilane with molecular formula C10H20O5Si; KH560 is gamma-glycidoxypropyltrimethoxysilane; KH550 is gamma-aminopropyl triethoxysilane. In the invention, KH570 is taken as an example, KH570(R-Si- (OCH3)3) is hydrolyzed to form siloxane (R-Si- (OH)3) and CH3OH, carbon chain R in the siloxane is dissolved in an organic solvent by a similar compatibility principle, and-OH hydroxyl is adsorbed on the surface of lithium nickel manganese oxide to form a coating state, so that the lithium nickel manganese oxide coated with a silane coupling agent hydrolysate can be obtained.
Preferably, the heating and stirring temperature in the step 1) is 70-90 ℃, and the heating and stirring time is 3-6 h;
the calcination temperature in the step 2) is 700-750 ℃, the calcination time is 3-5h, and the calcination step is carried out in the air atmosphere.
Preferably, in the step 1), the lithium nickel manganese oxide positive electrode material is mixed with an organic solvent, then a silane coupling agent and water are added, and heating and stirring are carried out, so that the lithium nickel manganese oxide coated with a silane coupling agent hydrolysate is obtained.
In the invention, alkali liquor is not added in the step 1), and the alkali liquor comprises inorganic alkali such as sodium hydroxide and potassium hydroxide, and organic alkali such as amine.
Preferably, the step 1) of filtering and drying the reaction solution after the heating and stirring are finished, and preferably, the drying step is vacuum drying, the vacuum drying temperature is 50-70 ℃, and the vacuum drying time is 20-40 h;
the core of the positive electrode material is a lithium nickel manganese oxide positive electrode material, and the surface of the core is coated with a silicon dioxide layer;
the lithium nickel manganese oxide positive electrode material is a spinel lithium nickel manganese oxide positive electrode material.
Preferably, the preparation method of the lithium nickel manganese oxide cathode material comprises the following steps:
and mixing a manganese source, a nickel source and a lithium source, and then calcining the mixed material to obtain the lithium nickel manganese oxide cathode material.
Preferably, the manganese source is trimanganese tetroxide, the nickel source is nickel oxide, and the lithium source is lithium carbonate;
the molar ratio of metal atoms Li, Ni and Mn in the mixed material is (1.01-1.05): (0.4-0.475): 1.525-1.6); it is understood that the manganese source, the nickel source and the lithium source are added in atomic molar ratios of (1.01-1.05): (0.4-0.475): (1.525-1.6) in terms of Li, Ni and Mn, respectively;
in the preparation method of the lithium nickel manganese oxide positive electrode material, the calcination temperature is 800-950 ℃, the heat preservation time is 10-12 h, the calcination step is carried out in the air atmosphere, and the air introduction flow is 18-22L/min;
the particle diameter D50 of manganese source is 2-4um, the particle diameter D50 of nickel source is 8-10um, the particle diameter D50 of lithium source is 8-10 um.
Preferably, in the preparation method of the lithium nickel manganese oxide cathode material, the manganese source, the nickel source and the lithium source are stirred at 1500-; the heating rate in the calcining step is 2-4 ℃/min.
The invention also provides a battery anode, which comprises the anode material prepared by the preparation method.
The invention also provides a lithium ion battery, and the positive electrode of the lithium ion battery is the battery positive electrode.
The invention has the beneficial effects that:
1. the preparation method of the cathode material provided by the invention comprises the steps of mixing the lithium nickel manganese oxide cathode material, the silane coupling agent, the organic solvent and water, heating and stirring to obtain the lithium nickel manganese oxide coated by the silane coupling agent hydrolysate, and sintering to obtain the silicon dioxide coated lithium nickel manganese oxide. According to the invention, organic solvent and water are used as solvents, alkali liquor is not added in the preparation process, the silane coupling agent is adsorbed on the surface of an inorganic material under a high-temperature condition to form a molecular silane coupling agent coating by heating and stirring, and a layer of uniform and compact SiO is formed on the surface of lithium nickel manganese oxide after calcination2The coating film can greatly reduce the contact surface of the lithium nickel manganese oxide and the electrolyte, so that the occurrence of side reactions of the lithium nickel manganese oxide battery is greatly reduced at high temperature and high pressure, and the cycle performance of the battery under the harsh conditions of high temperature and high pressure is improved. While the SiO2The coating film can also conduct lithium ions efficiently to improve the capacity and rate capability of the battery, and SiO2The layer can also react with hydrofluoric acid (HF) generated in the electrolyte, so that the surface of the lithium nickel manganese oxide electrode material is prevented from being etched by the HF.
Compared with the existing solid-phase mixed coating method or the method of coating after forming silicon dioxide through hydrolysis, the silicon dioxide coated film obtained by the preparation method disclosed by the invention can be used for coating the surface of the lithium nickel manganese oxide more uniformly and compactly, and meanwhile, the conduction of lithium ions between the surface of the lithium nickel manganese oxide and an electrolyte is not hindered, so that the cycle performance of the lithium nickel manganese oxide material under high temperature and high pressure can be greatly improved.
2) The preparation method of the cathode material provided by the invention further comprises the following steps of mixing the lithium nickel manganese oxide cathode material, the silane coupling agent, the organic solvent and the water according to the mass ratio of 100: (5-7): (750-850): (1-1.5). The invention is mainlyThe method is characterized in that an organic solvent is used as a solvent, a very small amount of water is added to enable a silane coupling agent to be adsorbed on the surface of the lithium nickel manganese oxide, the organic solvent and the water in a specific ratio are matched with a lithium nickel manganese oxide positive electrode material and the silane coupling agent in a specific ratio, so that the surface of the lithium nickel manganese oxide positive electrode material is more beneficial to forming a molecular layer of silane coupling agent coating, and a layer of uniform and compact SiO is formed on the surface of the lithium nickel manganese oxide after calcination2The coated film obviously improves the cycle performance of the battery under the harsh conditions of high temperature and high pressure.
3) The preparation method of the cathode material provided by the invention further comprises the steps that the silane coupling agent is selected from at least one of KH570, KH560 and KH550, and the organic solvent is carbon tetrachloride; according to the invention, at least one of KH570, KH560 and KH550 is selected as the silane coupling agent for coating, carbon tetrachloride is used as a solvent, so that the silane coupling agent coating is formed on the surface of the lithium nickel manganese oxide positive electrode material, and a layer of uniform and compact SiO is formed on the surface of the lithium nickel manganese oxide after calcination2And the film is coated, so that the cycle performance of the battery under the harsh conditions of high temperature and high pressure is improved.
4) The preparation method of the cathode material provided by the invention further comprises the step 1) that the heating and stirring temperature is 70-90 ℃ and the heating and stirring time is 3-6h, wherein the heating and stirring temperature is controlled to be 70-90 ℃, so that the silane coupling agent is more favorably coated on the surface of the lithium nickel manganese oxide under the high-temperature condition, a silane coupling agent coating layer is formed on the surface of the lithium nickel manganese oxide cathode material, then the lithium nickel manganese oxide cathode material is calcined at the temperature of 700-750 ℃, and a layer of uniform and compact SiO is further formed on the surface of the lithium nickel manganese oxide2The coated film can obviously improve the cycle performance of the battery under the harsh conditions of high temperature and high pressure.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and other drawings can be obtained by those skilled in the art without creative efforts.
Fig. 1 is an electron microscope scanning image of the cathode material prepared in example 1 of the present invention.
FIG. 2 is a SEM-EDS elemental map of Si in the cathode material prepared in example 1 of the present invention.
Fig. 3 is a graph of the cycling performance at 45 ℃ of R2032 button cells prepared using the positive electrode materials of example 1 and comparative example 1 of the invention.
Fig. 4 is an electron microscope scanning image of the cathode material prepared in comparative example 1 provided by the present invention.
Fig. 5 is a schematic view of a preparation method of the cathode material of example 1 provided by the present invention.
Detailed Description
The following examples are provided to further understand the present invention, not to limit the scope of the present invention, but to provide the best mode, not to limit the content and the protection scope of the present invention, and any product similar or similar to the present invention, which is obtained by combining the present invention with other prior art features, falls within the protection scope of the present invention.
The examples do not show the specific experimental steps or conditions, and can be performed according to the conventional experimental steps described in the literature in the field. The reagents or instruments used are not indicated by manufacturers, and are all conventional reagent products which can be obtained commercially.
Example 1
The embodiment provides a preparation method of a cathode material, which comprises the following steps:
1) manganese tetraoxide Mn3O4(particle size D50 ═ 3um), nickel oxide NiO (particle size D50 ═ 9um), and Li2CO3(particle diameter D50 ═ 9um) according to Li: ni: mixing Mn atoms in a molar ratio of 1.01:0.4:1.6, stirring for 20min by using a mixing stirrer at 2000 rpm, heating the mixed material to 900 ℃ at a heating rate of 2 ℃/min under the air atmosphere (the air introduction flow is 20L/min), calcining, keeping the temperature for 10h, naturally cooling, and collecting to obtain the lithium nickel manganese oxide cathode material;
2) adding 100g of the lithium nickel manganese oxide prepared in the step 1) into 800g of carbon tetrachloride solvent, uniformly stirring, adding 5.364g of KH570 and 1.341g of distilled water, uniformly stirring, heating and stirring the mixed solution at 80 ℃ under the condition of water bath reflux for 4h, filtering to obtain a solid, and performing vacuum drying on the obtained solid at 60 ℃ for 24h to obtain KH570 hydrolysate-coated lithium nickel manganese oxide (recorded as KH570@ LNMO);
3) calcining the KH570 hydrolysate-coated lithium nickel manganese oxide obtained in the step 2) at 720 ℃ for 4h in an air atmosphere to obtain the cathode material (marked as SiO)2@ LNMO), the cathode material kernel is nickel lithium manganate, and the kernel surface cladding has the silica layer. As can be seen from FIG. 1, the surface of the prepared lithium nickel manganese oxide cathode material is a layer of dense and smooth SiO2Coating film, SiO from FIG. 22Uniformly coating the surface of the spinel lithium nickel manganese oxide.
Example 2
The embodiment provides a preparation method of a cathode material, which comprises the following steps:
1) manganese tetraoxide Mn3O4(particle diameter D50 ═ 2um), nickel oxide NiO (particle diameter D50 ═ 10um), and Li2CO3(particle diameter D50 ═ 8um) according to Li: ni: mixing Mn atoms according to the molar ratio of 1.02:0.41:1.59, stirring for 20min by using a mixing stirrer at 2000 rpm, heating the mixed material to 950 ℃ at the heating rate of 3 ℃/min in the air atmosphere (the air introduction flow is 18L/min), calcining, keeping the temperature for 12h, naturally cooling, and collecting materials to obtain the lithium nickel manganese oxide positive electrode material;
2) adding 100g of the lithium nickel manganese oxide prepared in the step 1) into 750g of carbon tetrachloride solvent, uniformly stirring, adding 5g of KH570 and 1g of distilled water, uniformly stirring, heating and stirring the mixed solution at 70 ℃ under the condition of water bath reflux for 6h, filtering to obtain a solid, and performing vacuum drying on the obtained solid at 50 ℃ for 40h to obtain KH570 hydrolysate-coated lithium nickel manganese oxide (recorded as KH570@ LNMO);
3) calcining the KH570 hydrolysate-coated lithium nickel manganese oxide obtained in the step 2) at 700 ℃ for 5h in air atmosphere to obtain the cathode material (marked as SiO)2@ LNMO), the core of the positive electrode material is lithium nickel manganese oxide, and the surface of the coreIs coated with a silicon dioxide layer.
Example 3
The embodiment provides a preparation method of a cathode material, which comprises the following steps:
1) manganese tetraoxide Mn3O4(particle size D50 ═ 4um), nickel oxide NiO (particle size D50 ═ 8um), and Li2CO3(particle diameter D50 ═ 10um) according to Li: ni: mixing Mn atoms in a molar ratio of 1.03:0.42:1.58, stirring for 20min by using a mixing stirrer at 2000 rpm, heating the mixed material to 800 ℃ at a heating rate of 2 ℃/min under an air atmosphere (air introduction flow is 22L/min), calcining, keeping the temperature for 10h, naturally cooling, and collecting to obtain a lithium nickel manganese oxide positive electrode material;
2) adding 100g of the lithium nickel manganese oxide prepared in the step 1) into 850g of carbon tetrachloride solvent, uniformly stirring, adding 7g of KH570 and 1.5g of distilled water, uniformly stirring, heating and stirring the mixed solution at 90 ℃ under the condition of water bath reflux for 3h, filtering to obtain a solid, and performing vacuum drying on the obtained solid at 70 ℃ for 20h to obtain KH570 hydrolysate-coated lithium nickel manganese oxide (recorded as KH570@ LNMO);
3) calcining the KH570 hydrolysate-coated lithium nickel manganese oxide obtained in the step 2) at 750 ℃ for 3h in air atmosphere to obtain the cathode material (marked as SiO)2@ LNMO), the cathode material kernel is nickel lithium manganate, and the kernel surface cladding has the silica layer.
Example 4
This example provides a method for preparing a positive electrode material, which is different from example 1 in that the silane coupling agent used in step 2) is KH 560.
Example 5
This example provides a method for preparing a positive electrode material, which is different from example 1 in that the silane coupling agent used in step 2) is KH 550.
Example 6
The embodiment provides a preparation method of a cathode material, which comprises the following steps:
1) manganese tetraoxide Mn3O4(particle size D50 ═ 3um), nickel oxide NiO (particle size D50 ═ 9um), and Li2CO3(particle diameter D50 ═ 9um) according to Li: ni: mixing Mn atoms in a molar ratio of 1.01:0.4:1.6, stirring for 20min by using a mixing stirrer at 2000 rpm, heating the mixed material to 900 ℃ at a heating rate of 2 ℃/min under the air atmosphere (the air introduction flow is 20L/min), calcining, keeping the temperature for 10h, naturally cooling, and collecting to obtain the lithium nickel manganese oxide cathode material;
2) adding 100g of the lithium nickel manganese oxide prepared in the step 1) into 400g of carbon tetrachloride solvent, uniformly stirring, adding 5.364g of KH570 and 401.341g of distilled water, uniformly stirring, heating and stirring the mixed solution at 80 ℃ under the condition of water bath reflux for 4h, filtering to obtain a solid, vacuum-drying the obtained solid at 60 ℃ for 24h, and calcining the obtained material at 720 ℃ under an air atmosphere for 4h to obtain the cathode material.
Comparative example 1
The comparative example provides a method for preparing a positive electrode material, comprising the steps of:
1) manganese tetraoxide Mn3O4(particle size D50 ═ 3um), nickel oxide NiO (particle size D50 ═ 9um), and Li2CO3(particle diameter D50 ═ 9um) according to Li: ni: mixing Mn atoms in a molar ratio of 1.01:0.4:1.6, stirring for 20min by using a mixing stirrer at 2000 rpm, heating the mixed material to 900 ℃ at a heating rate of 2 ℃/min under the air atmosphere (the air introduction flow is 20L/min), calcining, keeping the temperature for 10h, naturally cooling, and collecting to obtain the lithium nickel manganese oxide cathode material;
2) 100g of the lithium nickel manganese oxide prepared in step 1) and 5.364g of SiO2Uniformly mixing particles (the particle size is 20nm), and calcining for 4 hours at the temperature of 720 ℃ in an air atmosphere to obtain the cathode material (marked as SiO)2@ LNMO). As shown in fig. 4, the surface of the silicon dioxide coating is dotted, and the material in this state can expose a large area of the surface of the lithium nickel manganese oxide and contact the electrolyte.
Comparative example 2
The comparative example provides a method for preparing a positive electrode material, comprising the steps of:
1) manganese tetraoxide Mn3O4(particle diameter D50 ═ 3)um), nickel oxide NiO (particle size D50 ═ 9um), and Li2CO3(particle diameter D50 ═ 9um) according to Li: ni: mixing Mn atoms in a molar ratio of 1.01:0.4:1.6, stirring for 20min by using a mixing stirrer at 2000 rpm, heating the mixed material to 900 ℃ at a heating rate of 2 ℃/min under the air atmosphere (the air introduction flow is 20L/min), calcining, keeping the temperature for 10h, naturally cooling, and collecting to obtain the lithium nickel manganese oxide cathode material;
2) adding 100g of the lithium nickel manganese oxide prepared in the step 1) into 800g of ethanol, uniformly stirring, adding 5.364g of KH570 and 100ml of ammonia water (the concentration is 15mol/L), heating and stirring the mixed solution at 80 ℃ under the condition of water bath reflux for 4h, filtering to obtain a solid, and vacuum-drying the obtained solid at 60 ℃ for 24h to obtain the cathode material.
Comparative example 3
The comparative example provides a method for preparing a positive electrode material, comprising the steps of:
1) manganese tetraoxide Mn3O4(particle size D50 ═ 3um), nickel oxide NiO (particle size D50 ═ 9um), and Li2CO3(particle diameter D50 ═ 9um) according to Li: ni: mixing Mn atoms in a molar ratio of 1.01:0.4:1.6, stirring for 20min by using a mixing stirrer at 2000 rpm, heating the mixed material to 900 ℃ at a heating rate of 2 ℃/min under the air atmosphere (the air introduction flow is 20L/min), calcining, keeping the temperature for 10h, naturally cooling, and collecting to obtain the lithium nickel manganese oxide cathode material;
2) adding 100g of the lithium nickel manganese oxide prepared in the step 1) into 800g of carbon tetrachloride solvent, uniformly stirring, adding 5.364g of KH570 and 1.341g of distilled water, uniformly stirring, heating and stirring the mixed solution at 80 ℃ under the water bath reflux condition for 4h, filtering to obtain a solid, and performing vacuum drying on the obtained solid at 60 ℃ for 24h to obtain the KH570 hydrolysate-coated lithium nickel manganese oxide (recorded as KH570@ LNMO), namely the cathode material.
Test example
The positive electrode materials prepared in the above examples and comparative examples were prepared into lithium ion batteries, and electrochemical performance tests were performed, specifically as follows:
the positive electrodes prepared in examples and comparative examples were respectivelyThe material was mixed with SP (carbon black conductive agent), PVDF (polyvinylidene fluoride) in a ratio of 92: 4: 4, then NMP (N-methyl pyrrolidone) is used as a solvent for pulping and stirring, the mixture is evenly mixed and then coated on an aluminum foil (the thickness of the aluminum foil is 20um), and the mixture is dried to obtain a positive plate (the surface density is 8.28 mg/cm)2) The diaphragm made of PE material is adopted, and electrolyte is dripped (the electrolyte adopts 1mol/L LiPF6As a solute, a mixed solution of ethylene carbonate and diethyl carbonate is adopted as a solvent, the volume ratio of the ethylene carbonate to the diethyl carbonate is 3:7), 80uL is adopted, a lithium sheet is used as a negative electrode, and the button battery case of R2032 is used for carrying out button electricity assembly.
1C cycle performance test at 45 ℃: the button battery prepared by the method is tested by using a blue tester, and specifically comprises the following steps: and (3) placing the prepared button battery in a high-temperature oven at 45 ℃ for charge and discharge tests, wherein the voltage range is 3.4V-5.0V, the charge and discharge are carried out for one circle at 0.1C, then the constant current and the constant voltage are charged at 0.5C, the cut-off current is 0.05C, the constant current discharge is carried out at 1C, and the cycle is carried out for 100 circles, so that the relevant data of parameters such as the first discharge capacity, the first coulomb efficiency, the 100 th circle discharge specific capacity retention rate and the like are obtained. The test results are shown in table 1.
TABLE 1 high temperature cycling performance of the cells
As can be seen from Table 1, the first discharge capacity of example 1 was 135.5mAh/g, and SiO prepared by the method was compared to the solid phase hybrid coating method of comparative example 12The first effect of the coated lithium nickel manganese oxide material is improved from 91.14% to 91.99%, meanwhile, the material can improve the capacity retention rate after 100 cycles from 48.83% to 98.08% in a high-temperature environment of 45 ℃, and the discharge capacity after 100 cycles is improved from 66.8mAh/g to 132.9 mAh/g. Compared with the method that the silane coupling agent is firstly hydrolyzed into silicon oxide under the alkaline condition and then coated in the comparative example 2, the material provided by the invention can improve the capacity retention rate from 60.67% to 98.08% after 100 cycles under the high-temperature environment of 45 ℃, and improve the specific discharge capacity from 81.66mAh/g after 100 cyclesTo 132.9 mAh/g. Compared with the comparative example 3 (without sintering treatment), the material provided by the invention can improve the capacity retention rate after 100 cycles from 50.20% to 98.08% under the high-temperature environment of 45 ℃, and improve the specific discharge capacity after 100 cycles from 58.0mAh/g to 132.9 mAh/g.
Further, the test results of 1C cycle performance at 45 ℃ of the R2032 button cell prepared by using the positive electrode materials of the invention in example 1 and the comparative example 1 are shown in fig. 3, and it can be seen from fig. 3 that the high temperature cycle performance of the material prepared in example 1 is far better than that of the comparative example. Therefore, the material obtained by the method provided by the invention has excellent cycle performance under high-temperature and high-pressure conditions, and can be normally used under high-temperature and high-pressure conditions, so that the lithium nickel manganese oxide material has market competitive advantages.
It should be understood that the above examples are only for clarity of illustration and are not intended to limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications therefrom are within the scope of the invention.
Claims (10)
1. The preparation method of the cathode material is characterized by comprising the following steps of:
1) mixing a lithium nickel manganese oxide positive electrode material, a silane coupling agent, an organic solvent and water, heating and stirring to obtain lithium nickel manganese oxide coated with a silane coupling agent hydrolysate;
2) and calcining the lithium nickel manganese coated by the silane coupling agent hydrolysate to obtain the cathode material.
2. The preparation method of the cathode material according to claim 1, wherein the mass ratio of the lithium nickel manganese oxide cathode material to the silane coupling agent to the organic solvent to the water is 100: (5-7): (750-850): (1-1.5).
3. The method for producing the cathode material according to claim 1 or 2, characterized in that the silane coupling agent is at least one selected from the group consisting of KH570, KH560 and KH 550;
the organic solvent is carbon tetrachloride.
4. The method for producing a positive electrode material according to any one of claims 1 to 3, wherein the heating and stirring temperature in step 1) is 70 to 90 ℃ and the heating and stirring time is 3 to 6 hours;
the calcination temperature in the step 2) is 700-750 ℃, the calcination time is 3-5h, and the calcination step is carried out in the air atmosphere.
5. The method for preparing the positive electrode material according to any one of claims 1 to 4, wherein the lithium nickel manganese oxide positive electrode material is mixed with an organic solvent in the step 1), and then the silane coupling agent and water are added, heated and stirred to obtain the silane coupling agent hydrolysate-coated lithium nickel manganese oxide.
6. The method for preparing the cathode material according to any one of claims 1 to 5, wherein the step 1) of filtering and drying the reaction solution after the heating and stirring is finished is further included, preferably, the drying step is vacuum drying, the temperature of the vacuum drying is 50 to 70 ℃, and the time of the vacuum drying is 20 to 40 hours;
the core of the positive electrode material is a lithium nickel manganese oxide positive electrode material, and the surface of the core is coated with a silicon dioxide layer;
the lithium nickel manganese oxide positive electrode material is a spinel lithium nickel manganese oxide positive electrode material.
7. The method for preparing the positive electrode material according to any one of claims 1 to 6, wherein the method for preparing the lithium nickel manganese oxide positive electrode material comprises the following steps:
and mixing a manganese source, a nickel source and a lithium source, and then calcining the mixed material to obtain the lithium nickel manganese oxide cathode material.
8. The method for producing a positive electrode material according to claim 7, wherein the manganese source is trimanganese tetroxide, the nickel source is nickel oxide, and the lithium source is lithium carbonate;
the molar ratio of metal atoms Li, Ni and Mn in the mixed material is (1.01-1.05): (0.4-0.475): 1.525-1.6);
in the preparation method of the lithium nickel manganese oxide positive electrode material, the calcination temperature is 800-950 ℃, the heat preservation time is 10-12 h, the calcination step is carried out in the air atmosphere, and the air introduction flow is 18-22L/min;
the particle diameter D50 of manganese source is 2-4um, the particle diameter D50 of nickel source is 8-10um, the particle diameter D50 of lithium source is 8-10 um.
9. A positive electrode for a battery, comprising the positive electrode material produced by the production method according to any one of claims 1 to 8.
10. A lithium ion battery, wherein a positive electrode of the lithium ion battery is the battery positive electrode according to claim 9.
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