CN108987683A - A kind of preparation method of carbon coating tertiary cathode material - Google Patents
A kind of preparation method of carbon coating tertiary cathode material Download PDFInfo
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- CN108987683A CN108987683A CN201810536846.5A CN201810536846A CN108987683A CN 108987683 A CN108987683 A CN 108987683A CN 201810536846 A CN201810536846 A CN 201810536846A CN 108987683 A CN108987683 A CN 108987683A
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- cathode material
- tertiary cathode
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- carbon
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 88
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 88
- 239000010406 cathode material Substances 0.000 title claims abstract description 50
- 238000000576 coating method Methods 0.000 title claims abstract description 45
- 239000011248 coating agent Substances 0.000 title claims abstract description 44
- 238000002360 preparation method Methods 0.000 title claims abstract description 29
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 95
- 239000000463 material Substances 0.000 claims abstract description 54
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 46
- 239000012670 alkaline solution Substances 0.000 claims abstract description 9
- 239000002243 precursor Substances 0.000 claims abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000005253 cladding Methods 0.000 claims abstract description 8
- 238000001354 calcination Methods 0.000 claims abstract description 7
- 230000009977 dual effect Effects 0.000 claims abstract description 6
- 239000002904 solvent Substances 0.000 claims abstract description 6
- 239000008367 deionised water Substances 0.000 claims abstract description 5
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 5
- 239000002270 dispersing agent Substances 0.000 claims abstract description 4
- 239000003960 organic solvent Substances 0.000 claims abstract description 4
- 239000000725 suspension Substances 0.000 claims abstract description 3
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 9
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 4
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 4
- KFDQGLPGKXUTMZ-UHFFFAOYSA-N [Mn].[Co].[Ni] Chemical compound [Mn].[Co].[Ni] KFDQGLPGKXUTMZ-UHFFFAOYSA-N 0.000 claims description 4
- 238000005245 sintering Methods 0.000 claims description 4
- VXEGSRKPIUDPQT-UHFFFAOYSA-N 4-[4-(4-methoxyphenyl)piperazin-1-yl]aniline Chemical compound C1=CC(OC)=CC=C1N1CCN(C=2C=CC(N)=CC=2)CC1 VXEGSRKPIUDPQT-UHFFFAOYSA-N 0.000 claims description 3
- 239000005049 silicon tetrachloride Substances 0.000 claims description 3
- 239000000126 substance Substances 0.000 claims description 3
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 2
- 229910004455 Li(Ni1-x-yCoxMny)O2 Inorganic materials 0.000 claims description 2
- UIIMBOGNXHQVGW-DEQYMQKBSA-M Sodium bicarbonate-14C Chemical compound [Na+].O[14C]([O-])=O UIIMBOGNXHQVGW-DEQYMQKBSA-M 0.000 claims description 2
- 239000000908 ammonium hydroxide Substances 0.000 claims description 2
- UBHZUDXTHNMNLD-UHFFFAOYSA-N dimethylsilane Chemical compound C[SiH2]C UBHZUDXTHNMNLD-UHFFFAOYSA-N 0.000 claims description 2
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 claims 1
- 239000002245 particle Substances 0.000 claims 1
- 229910052814 silicon oxide Inorganic materials 0.000 claims 1
- 239000011734 sodium Substances 0.000 claims 1
- 229910052708 sodium Inorganic materials 0.000 claims 1
- 239000010410 layer Substances 0.000 abstract description 5
- 239000011241 protective layer Substances 0.000 abstract description 4
- 230000009467 reduction Effects 0.000 abstract description 4
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 abstract description 3
- 230000015572 biosynthetic process Effects 0.000 abstract description 3
- 238000007599 discharging Methods 0.000 abstract description 3
- 229910001416 lithium ion Inorganic materials 0.000 abstract description 3
- 235000012239 silicon dioxide Nutrition 0.000 abstract description 3
- 239000010405 anode material Substances 0.000 description 30
- 230000000052 comparative effect Effects 0.000 description 11
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 10
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 9
- 230000004087 circulation Effects 0.000 description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 8
- 239000000243 solution Substances 0.000 description 7
- 238000003756 stirring Methods 0.000 description 7
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 6
- 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 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- 238000002474 experimental method Methods 0.000 description 6
- 239000008103 glucose Substances 0.000 description 6
- 238000000034 method Methods 0.000 description 6
- 229910052681 coesite Inorganic materials 0.000 description 5
- 229910052906 cristobalite Inorganic materials 0.000 description 5
- 238000001035 drying Methods 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 5
- 229910052757 nitrogen Inorganic materials 0.000 description 5
- 229910052682 stishovite Inorganic materials 0.000 description 5
- 229910052905 tridymite Inorganic materials 0.000 description 5
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- 235000019441 ethanol Nutrition 0.000 description 4
- 230000014759 maintenance of location Effects 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 3
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 3
- 238000001914 filtration Methods 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 239000008187 granular material Substances 0.000 description 3
- 229910052744 lithium Inorganic materials 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 238000010792 warming Methods 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 229910052493 LiFePO4 Inorganic materials 0.000 description 2
- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 2
- 229920002472 Starch Polymers 0.000 description 2
- QXZUUHYBWMWJHK-UHFFFAOYSA-N [Co].[Ni] Chemical compound [Co].[Ni] QXZUUHYBWMWJHK-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 238000003763 carbonization Methods 0.000 description 2
- 239000011247 coating layer Substances 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 238000002242 deionisation method Methods 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- VYFYYTLLBUKUHU-UHFFFAOYSA-N dopamine Chemical compound NCCC1=CC=C(O)C(O)=C1 VYFYYTLLBUKUHU-UHFFFAOYSA-N 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 238000007654 immersion Methods 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 229910052748 manganese Inorganic materials 0.000 description 2
- 239000011572 manganese Substances 0.000 description 2
- 230000001681 protective effect Effects 0.000 description 2
- 239000008107 starch Substances 0.000 description 2
- 235000019698 starch Nutrition 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 101100373011 Drosophila melanogaster wapl gene Proteins 0.000 description 1
- 229910004403 Li(Ni0.6Co0.2Mn0.2)O2 Inorganic materials 0.000 description 1
- 229910015118 LiMO Inorganic materials 0.000 description 1
- 229910002097 Lithium manganese(III,IV) oxide Inorganic materials 0.000 description 1
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
- 239000002033 PVDF binder Substances 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- 240000000111 Saccharum officinarum Species 0.000 description 1
- 235000007201 Saccharum officinarum Nutrition 0.000 description 1
- 229920002125 Sokalan® Polymers 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
- QSNQXZYQEIKDPU-UHFFFAOYSA-N [Li].[Fe] Chemical compound [Li].[Fe] QSNQXZYQEIKDPU-UHFFFAOYSA-N 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 229910052786 argon Inorganic materials 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
- 239000011230 binding agent Substances 0.000 description 1
- 150000001868 cobalt Chemical class 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 229960003638 dopamine Drugs 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 125000004494 ethyl ester group Chemical group 0.000 description 1
- 238000007306 functionalization reaction Methods 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 150000002642 lithium compounds Chemical class 0.000 description 1
- 229910021450 lithium metal oxide Inorganic materials 0.000 description 1
- 150000002696 manganese Chemical class 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 150000002815 nickel Chemical class 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 1
- 229910052609 olivine Inorganic materials 0.000 description 1
- 239000010450 olivine Substances 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- VDGJOQCBCPGFFD-UHFFFAOYSA-N oxygen(2-) silicon(4+) titanium(4+) Chemical compound [Si+4].[O-2].[O-2].[Ti+4] VDGJOQCBCPGFFD-UHFFFAOYSA-N 0.000 description 1
- 210000004483 pasc Anatomy 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 239000004584 polyacrylic acid Substances 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 150000004040 pyrrolidinones Chemical class 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 1
- 229910052596 spinel Inorganic materials 0.000 description 1
- 239000011029 spinel Substances 0.000 description 1
- 239000005720 sucrose Substances 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
Classifications
-
- 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
- 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
-
- 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
-
- 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
-
- 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
- H01M4/628—Inhibitors, e.g. gassing inhibitors, corrosion inhibitors
-
- 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
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Inorganic Chemistry (AREA)
- Composite Materials (AREA)
- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention discloses a kind of preparation methods of carbon coating tertiary cathode material, belong to technical field of lithium ion.The preparation method includes: that (1) tertiary cathode material and silica precursor are added in organic solvent, is uniformly mixed, then deionized water is added dropwise, is stirred to react, and is then evaporated all solvents, and calcining obtains the tertiary cathode material of coated with silica；(2) tertiary cathode material of coated with silica and organic carbon source are added in dispersing agent, obtain suspension, the tertiary cathode material that silica and carbon dual cladding is made is sintered after being evaporated；(3) tertiary cathode material of silica and carbon dual cladding is soaked in alkaline solution, obtains carbon coating tertiary cathode material.The present invention is using silicon dioxide layer as intermediate protective layer; prevent carbon source from discharging reducibility gas reduction material of main part during high temperature cabonization; the carbon coating of formation gives full play to its electric conductivity, improves the high current charge-discharge ability of battery, and then improve high rate performance.
Description
Technical field
The present invention relates to technical field of lithium ion, and in particular to a kind of preparation side of carbon coating tertiary cathode material
Method.
Background technique
Current commercialized anode material for lithium-ion batteries is probably divided into three classes according to its structure: the first kind is that have
The lithium metal oxide LiMO of six side's layer structures2(M=Co, Ni, Mn), represent material be mainly cobalt acid lithium, ternary just
Pole material (NCM, NCA), rich lithium material.Second class is the material of spinel structure, represents material mainly and have 4V grades of mangaic acid
Lithium (LiMn2O4).Third class is the compound with polyanionic structure, and representing material is mainly the phosphorus for having olivine structural
Sour iron lithium (LiFePO4)。
Wherein tertiary cathode material energy density with higher, it is environmental-friendly the features such as, this makes ternary material gradually
First choice as power battery anode material.But the material also has its defect, such as cycle performance decline, high rate performance is poor,
This is also the reason of limitation ternary material rapidly develops.
For above problem, the surface of ternary material is modified to can solve certain problem, the modified packet in general surface
Include doping and surface cladding.Wherein cladding means can reduce side reaction of material during circulating battery, carry out to material
Protection, and the covering material of some functionalization can further promote the cycle performance and high rate performance of material.
Carbon coating is to improve the important means of material conductivity, and low cost, advantages of environment protection make carbon coating gradually
The Critical policies modified as positive electrode.Such as the various carbon coating means of LiFePO4, it has obtained on the market at present
It is widely applied.
Mostly using organic matter sugarcane sugar and starch as carbon source in document, heating carbonization in an inert atmosphere.Carbon coating is as anode
The protective layer of material reduces charge transfer impedance, can inhibit the dissolution of metal ion, in addition, carbon coating can also be improved material
The surface electronic conductivity of material improves the electrical contact between material granule, and then improves the chemical property of material.
The patent document of Publication No. CN103474628A discloses a kind of preparation method of carbon coating tertiary cathode material,
The following steps are included: S1, using nickel salt, cobalt salt and manganese salt as raw material, prepare ternary anode material precursor；S2, preparation conductive carbon
Dispersion: it disperses conductive carbon in the water containing organic carbon source；S3, ternary anode material precursor and lithium compound are added
Enter into conductive carbon dispersion, be uniformly mixed, obtains mixture；S4, mixture is dried under vacuum conditions；S5, will be through
The mixture of drying is in confined conditions or the atmosphere high temperature of inert gas shielding is handled, and obtains carbon coating tertiary cathode material
Material.
But for oxide-based tertiary cathode material, promotion and improvement of the carbon coating of commonsense method for performance
It is also extremely limited.Reason is common carbon coating means during carbonization, and carbon source will form the CO with reproducibility
Or the reducibility gas such as H2, it has a certain impact to tertiary cathode material, the valence state of various metals generates variation, so that brilliant
The decline of lattice structure.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation methods of carbon coating tertiary cathode material, to overcome existing carbon packet
The problem of tertiary cathode material is easily restored by carbon under the high temperature conditions in coating method.
To achieve the above object, the present invention adopts the following technical scheme:
A kind of preparation method of carbon coating tertiary cathode material, comprising the following steps:
(1) tertiary cathode material and silica precursor are added in organic solvent, are uniformly mixed, then deionization is added dropwise
Water is stirred to react, and is then evaporated all solvents, and calcining obtains the tertiary cathode material of coated with silica；
(2) tertiary cathode material of coated with silica and organic carbon source are added in dispersing agent, obtain suspension, is evaporated
It is sintered the tertiary cathode material that silica and carbon dual cladding is made afterwards；
(3) tertiary cathode material of silica and carbon dual cladding is soaked in alkaline solution, obtains carbon coating three
First positive electrode.
In preparation method of the invention, step (1) formed coated with silica layer step (2) high temperature cabonization process
In serve as protective layer, to inhibit carbon at high temperature to the reduction of tertiary cathode material, also just solve at present tradition it is carbon-coated
One drawback.After the carbon coating layer that step (2) are formed, silica loses original effect, by step (3) in alkali
Property solution in etching to form single clad.
The tertiary cathode material can be nickel-cobalt-manganternary ternary anode material (NCM), nickel cobalt aluminium tertiary cathode material
(NCA)。
Preferably, the tertiary cathode material is nickel-cobalt-manganternary ternary anode material, chemical molecular formula in step (1)
For Li (Ni1-x-yCoxMny)O2, wherein 0 < x < 0.4,0 < y < 1.The molar ratio of nickel cobalt manganese is 6:2:2,5:2:3,4:4:2 or 1:1:
1。
Preferably, the silica precursor is silica dioxide granule, silicon tetrachloride, positive silicic acid in step (1)
One of ethyl ester, dimethylsilane are a variety of.
Preferably, the silica precursor is with the mass ratio of tertiary cathode material in terms of silica
0.005-0.2:1。
More preferably, ethyl orthosilicate is 0.01:1 with the mass ratio of tertiary cathode material in terms of silica.
Preferably, in step (1), the organic solvent be one of methanol, ethyl alcohol, isopropanol, ethylene glycol or
It is a variety of.
Preferably, the temperature being stirred to react is 20-80 DEG C, revolving speed 800-1000r/min in step (1), when
Between be 2-7h.Deionized water is added dropwise according to stoichiometric ratio, while stirring Si (OH) x for guaranteeing tetraethyl orthosilicate and hydrolyzing
It uniformly adequately covers on the surface of the material.
More preferably, the temperature being stirred to react is 60 DEG C, revolving speed 800r/min, time 3h.
The calcining carries out in air atmosphere, preferably, the temperature of the calcining is 200-700 in step (1)
DEG C, time 2-8h.
More preferably, the temperature of the calcining is 500 DEG C, time 5h.
In step (2), the organic carbon source can be high-molecular organic material or glucide, preferably, described
Organic carbon source be one of sucrose, glucose, polyacrylic acid, starch, polyethylene glycol, dopamine or a variety of.
Preferably, the tertiary cathode material of coated with silica and the mass ratio of organic carbon source are 1 in step (2):
0.01-0.1。
More preferably, the tertiary cathode material of coated with silica and the mass ratio of glucose are 0.05:1.
Preferably, the dispersing agent is water, ethyl alcohol, ethylene glycol, methylene chloride, methanol, isopropanol in step (2)
One of or it is a variety of.
The sintering carries out in protective atmosphere, and the protective atmosphere can be nitrogen.Preferably, in step (2), institute
The temperature for the sintering stated is 100-1000 DEG C, time 1-20h.
More preferably, the temperature of the sintering is 800 DEG C, time 3h.
In step (3), alkaline solution falls the silica coated in ternary material and remaining pasc reaction.As excellent
Choosing, in step (3), the alkaline solution be one of sodium hydroxide, potassium hydroxide, ammonium hydroxide, sodium bicarbonate, sodium carbonate or
It is a variety of.
Preferably, the concentration of the alkaline solution is 0.1mol/L-2mol/L in step (3).
More preferably, the alkaline solution concentration is 0.5mol/L.
Preferably, the time impregnated is 1-2h.
It is that the present invention has the utility model has the advantages that
In carbon coating tertiary cathode material preparation method provided by the invention, using silicon dioxide layer as intermediate protection
Layer prevents carbon source from discharging reducibility gas reduction material of main part during high temperature cabonization, and the carbon coating of formation, which gives full play to, to be led
The excellent electric conductivity of electrical carbon improves the high current charge-discharge ability of battery, and then improves high rate performance.
Detailed description of the invention
Fig. 1 is the SEM figure of carbon coating nickel-cobalt-manganternary ternary anode material made from embodiment 1.
Fig. 2 is the SEM figure of carbon coating nickel-cobalt-manganternary ternary anode material made from embodiment 2.
Fig. 3 is the SEM figure of carbon coating nickel-cobalt-manganternary ternary anode material made from comparative example 1.
Fig. 4 is the SEM figure of the uncoated nickel-cobalt-manganternary ternary anode material of comparative example 2.
Fig. 5 is the TEM figure of carbon coating nickel-cobalt-manganternary ternary anode material made from embodiment 1.
Fig. 6 is the TEM figure of carbon coating nickel-cobalt-manganternary ternary anode material made from embodiment 2.
Fig. 7 is the TEM figure of carbon coating nickel-cobalt-manganternary ternary anode material made from comparative example 1.
Fig. 8 is the TEM figure of the uncoated nickel-cobalt-manganternary ternary anode material of comparative example 2.
Fig. 9 is the XRD diagram of 2 sample of carbon coating nickel-cobalt-manganternary ternary anode material and comparative example made from embodiment 1-3.
Figure 10 is the forthright again of carbon coating nickel-cobalt-manganternary ternary anode material and comparative example 1-2 sample made from embodiment 2-3
It can figure.
Figure 11 is the cycle performance of 1 sample of carbon coating nickel-cobalt-manganternary ternary anode material and comparative example made from embodiment 1-3
Figure.
Specific embodiment
The present invention will be further described below with reference to examples.Following embodiment is only intended to clearly illustrate this
The performance of invention, and the following examples cannot be limited only to.
Embodiment 1
A kind of novel carbon coating nickel-cobalt-manganternary ternary anode material, preparation method are as follows:
Step 1, the NCM622 prepared, i.e. Li (Ni0.6Co0.2Mn0.2)O2For basis material, naked ternary material and
Ethyl orthosilicate (being converted to silica) 1:0.01 in mass ratio is blended in ethyl alcohol phase, 60 DEG C of stirring 3h, is counted according to chemistry
Amount is warming up to 100 DEG C after 800r/min reaction 3h and distributes all solvents, scrape powder than a certain amount of deionized water is slowly added dropwise
It is placed in 500 DEG C of air and is sintered 5h, then cooled down, therefrom obtain the ternary material of coated with silica, be denoted as
SiO2@NCM。
Step 2 is added to 5% glucose solution using the coated with silica ternary material in experimental procedure one
Middle heating stirring, is evaporated to dryness, and is then placed in tube furnace 800 DEG C and is sintered 3h under the atmosphere of nitrogen, silica and carbon
Ternary material is covered in double-contracting, is denoted as C/SiO2@NCM。
Step 3 is put into immersion 1h in the NaOH solution of 0.5mol/L using the material in experimental procedure two and etches away, obtains
To simple carbon encapsulated material, then filtering drying, completes the preparation of carbon-coated positive electrode, is named as #1.
As shown in Figure 1, the SEM for carbon coating nickel-cobalt-manganternary ternary anode material schemes；As shown in figure 5, being carbon coating nickel cobalt manganese
The TEM of tertiary cathode material schemes.
Embodiment 2
A kind of novel carbon coating nickel-cobalt-manganternary ternary anode material, preparation method are as follows:
Step 1 is basis material the NCM622 prepared, naked ternary material and silicon tetrachloride (is converted to titanium dioxide
Silicon) 1:0.005 in mass ratio is blended in ethyl alcohol phase, and 20 DEG C are stirred, 7h, and a certain amount of deionization is being added dropwise according to stoichiometric ratio
Water is warming up to 100 DEG C and distributes all solvents after 800r/min reaction 3h, scrapes powder and is placed in 200 DEG C of air and is sintered 8h,
Then it is cooled down, therefrom obtains the ternary material of coated with silica, be denoted as SiO2@NCM。
Step 2 coats ternary material using the silica in experimental procedure one, is added in 1% glucose solution
Heating stirring is evaporated to dryness, and is then placed in tube furnace and is sintered 20h, pair of silica and carbon under the atmosphere of nitrogen for 100 DEG C
Ternary material is coated, C/SiO is denoted as2@NCM。
Step 3 is put into immersion 1h in the ammonia spirit of 0.1mol/L using the material in experimental procedure two and etches away, obtains
To simple carbon encapsulated material, then filtering drying, completes the preparation of carbon-coated positive electrode, is named as #2.
As shown in Fig. 2, the SEM for carbon coating nickel-cobalt-manganternary ternary anode material schemes；As shown in fig. 6, being carbon coating nickel cobalt manganese
The TEM of tertiary cathode material schemes.
Embodiment 3
A kind of novel carbon coating nickel-cobalt-manganternary ternary anode material, preparation method are as follows:
Step 1: being basis material the NCM622 prepared, in mass ratio naked ternary material and silica dioxide granule
1:0.02 is blended in methanol phase, 80 DEG C of stirring 2h, and a certain amount of deionized water, 800r/min is being added dropwise according to stoichiometric ratio
It is warming up to 100 DEG C after reaction 3h and distributes all solvents, scrape powder and be placed in 700 DEG C of air and be sintered 2h, then carry out cold
But, the ternary material for therefrom obtaining coated with silica, is denoted as SiO2@NCM。
Step 2: coating ternary material using the silica in experimental procedure one, it is added to 10% glucose solution
Middle heating stirring, is evaporated to dryness, and is then placed in tube furnace 1000 DEG C and is sintered 1h under the atmosphere of nitrogen, silica and carbon
Ternary material is covered in double-contracting, is denoted as C/SiO2@NCM。
It is etched away Step 3: being put into the KOH solution of 2mol/L using the material in experimental procedure two and impregnating 1h, obtains list
Pure carbon encapsulated material, then filtering drying, completes the preparation of carbon-coated positive electrode, is named as #3.
Comparative example 1
A kind of common carbon coating nickel-cobalt-manganternary ternary anode material, preparation method are as follows:
It is basis material the NCM622 prepared, is added to heating stirring in 10% glucose solution, is evaporated to
It is dry.It is then placed in tube furnace and is sintered 3h under the atmosphere of nitrogen for 800 DEG C.Carbon-coated nickel-cobalt-manganternary ternary anode material is obtained,
It is named as #4.
As shown in figure 3, the SEM for common carbon coating nickel-cobalt-manganternary ternary anode material schemes；As shown in fig. 7, being common carbon packet
Cover the TEM figure of nickel-cobalt-manganternary ternary anode material.
Comparative example 2
Using NCM622 as uncoated nickel-cobalt-manganternary ternary anode material, it is named as #.As shown in figure 4, being uncoated nickel cobalt
The SEM of manganese tertiary cathode material schemes；As shown in figure 8, the TEM for uncoated nickel-cobalt-manganternary ternary anode material schemes.
Application examples
1, apparent analysis
As can be seen from Figure 9: there is no variations for the main structure of the nickel-cobalt-manganternary ternary anode material of embodiment 1-3 carbon coated.
2, performance test:
Assembled battery method: by the embodiment 1-3 and comparative example 1-2 positive electrode powder prepared and conductive black super
P and binder Kynoar (PVDF) are uniform according to mass ratio 85:10:5 hand lapping.A certain amount of 1- methyl -2- is added
Pyrrolidones (NMP) is stirred evenly with homogenate flesh.Then it is scratched with plate coating machine, blade coating thickness is set as 0.02mm
(before drying).It is put into 80 DEG C to dry five hours, places into 100 DEG C of vacuum oven overnights.It is cut to the electrode that diameter is 11.7mm
Piece is put into argon air box assembled battery in order later.It is tested after standing one day after being completed.
Test method: battery is tested on blue electricity 5V-5mA or 5V-10mA battery test system, and test method is with electric current
Density is to carry out charge-discharge test in the electrochemical window of 2.8-4.3V subject to 1C=180mA/g；And with 0.2C, 0.5C, 1C,
The circulation of charge and discharge is completed under 2C, 5C different multiplying powers.
It was found from Figure 10 and Figure 11: embodiment 1 prepares the tertiary cathode material of carbon at voltage 4.3V, for the first time discharge capacity
For 179.5mAh/g, capacity is in 173.8mAh/g, capacity retention ratio 96.8% after 50 circulations.Ternary material it is forthright again
Can, the specific discharge capacity under the multiplying power of 0.2C, 0.5C, 1C, 2C, 5C be respectively 181mAh/g, 176mAh/g, 167mAh/g,
150mAh/g,138mAh/g.It recycles its specific capacity under 0.2C again after circulation and is still maintained at 178mAh/g.
Embodiment 2 prepares the tertiary cathode material of carbon at voltage 4.3V, and discharge capacity is 172.2mAh/g for the first time, through 50
Capacity is in 153mAh/g, capacity retention ratio 88.9% after secondary circulation.The high rate performance of ternary material, 0.2C, 0.5C, 1C,
Specific discharge capacity under the multiplying power of 2C, 5C is respectively 179mAh/g, 173mAh/g, 167mAh/g, 158mAh/g, 139mAh/g.
It recycles its specific capacity under 0.2C again after circulation and is still maintained at 172mAh/g.
Embodiment 3 prepares the tertiary cathode material of carbon at voltage 4.3V, and discharge capacity is 163mAh/g for the first time, through 50 times
Capacity is in 154mAh/g, capacity retention ratio 94.5% after circulation.The high rate performance of ternary material, 0.2C, 0.5C, 1C, 2C,
Specific discharge capacity under the multiplying power of 5C is respectively 176mAh/g, 165mAh/g, 156mAh/g, 146mAh/g, 121mAh/g.By
Again its specific capacity is recycled after circulation under 0.2C and is still maintained at 173mAh/g.
Comparative example 1 prepares common carbon-coated tertiary cathode material at voltage 4.3V, and discharge capacity is 176mAh/ for the first time
G, capacity is in 143mAh/g, capacity retention ratio 81.3% after 50 circulations.The high rate performance of ternary material, 0.2C,
Specific discharge capacity under the multiplying power of 0.5C, 1C, 2C, 5C be respectively 178mAh/g, 153mAh/g, 143mAh/g, 132mAh/g,
108mAh/g.Recycling its specific capacity under 0.2C again after circulation is 168mAh/g.
In the method for the preparation carbon coating nickel-cobalt-manganternary ternary anode material of above-described embodiment, using silica as intermediate
Protective layer, prevent carbon source discharged during high temperature cabonization reducibility gas reduction material of main part.The carbon coating layer of formation is bright
The aobvious electric conductivity for showing that conductive carbon is excellent improves the big electricity of battery compared with common carbon-coated tertiary cathode material
Charging and discharging capabilities are flowed, to improve high rate performance.
The above statement is only preferred embodiment of the invention, it is noted that those skilled in the art, not
Under the premise of being detached from the invention design, various modifications and improvements can be made, these also should be regarded as protection of the invention
Within the scope of.
Claims (10)
1. a kind of preparation method of carbon coating tertiary cathode material, which comprises the following steps:
(1) tertiary cathode material and silica precursor are added in organic solvent, are uniformly mixed, then deionized water is added dropwise,
It is stirred to react, is then evaporated all solvents, calcining obtains the tertiary cathode material of coated with silica；
(2) tertiary cathode material of coated with silica and organic carbon source are added in dispersing agent, obtain suspension, is burnt after being evaporated
Tie the tertiary cathode material that silica and carbon dual cladding is made；
(3) tertiary cathode material of silica and carbon dual cladding is soaked in alkaline solution, is obtaining carbon coating ternary just
Pole material.
2. preparation method as described in claim 1, which is characterized in that in step (1), the tertiary cathode material is nickel cobalt
Manganese tertiary cathode material, chemical molecular formula are Li (Ni1-x-yCoxMny)O2, wherein 0 < x < 0.4,0 < y < 1.
3. preparation method as described in claim 1, which is characterized in that in step (1), the silica precursor is two
One of silicon oxide particle, silicon tetrachloride, ethyl orthosilicate, dimethylsilane are a variety of.
4. preparation method as claimed in claim 3, which is characterized in that the silica precursor in terms of silica with
The mass ratio of tertiary cathode material is 0.005-0.2:1.
5. preparation method as described in claim 1, which is characterized in that in step (1), the temperature being stirred to react is
20-80 DEG C, revolving speed 800-1000r/min, time 2-7h.
6. preparation method as described in claim 1, which is characterized in that in step (1), the temperature of the calcining is 200-
700 DEG C, time 2-8h.
7. preparation method as described in claim 1, which is characterized in that in step (2), the tertiary cathode material of coated with silica
The mass ratio of material and organic carbon source is 1:0.01-0.1.
8. preparation method as described in claim 1, which is characterized in that in step (2), the temperature of the sintering is 100-
1000 DEG C, time 1-20h.
9. preparation method as described in claim 1, which is characterized in that in step (3), the alkaline solution is hydroxide
One of sodium, potassium hydroxide, ammonium hydroxide, sodium bicarbonate, sodium carbonate are a variety of.
10. preparation method as described in claim 1, which is characterized in that in step (3), the concentration of the alkaline solution is
0.1mol/L-2mol/L。
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| CN109994725A (en) * | 2018-12-12 | 2019-07-09 | 彩虹集团新能源股份有限公司 | A kind of manufacturing method of the nickelic tertiary cathode material of hydrophobic type |
| CN111490236A (en) * | 2020-03-20 | 2020-08-04 | 广东墨睿科技有限公司 | Preparation method of carbon nanotube/amorphous carbon double-layer carbon-coated ternary cathode material |
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| CN111490236A (en) * | 2020-03-20 | 2020-08-04 | 广东墨睿科技有限公司 | Preparation method of carbon nanotube/amorphous carbon double-layer carbon-coated ternary cathode material |
| CN111689527A (en) * | 2020-06-22 | 2020-09-22 | 湖南金富力新能源股份有限公司 | Preparation method of one-pot double-coated lithium ion battery NCM ternary cathode material |
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| CN114314691A (en) * | 2021-12-27 | 2022-04-12 | 材料科学姑苏实验室 | Impurity ion doped and regenerated ternary cathode material and preparation method and application thereof |
| CN114335500A (en) * | 2021-12-29 | 2022-04-12 | 湖北融通高科先进材料有限公司 | Nano-porous SiO 2-coated ternary cathode material and preparation method and application thereof |
| CN114335500B (en) * | 2021-12-29 | 2024-07-02 | 湖北融通高科先进材料集团股份有限公司 | SiO2 coated ternary positive electrode material with nano porous structure, and preparation method and application thereof |
| CN114551843A (en) * | 2022-02-28 | 2022-05-27 | 蜂巢能源科技股份有限公司 | Positive electrode material and preparation method and application thereof |
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| CN114551843B (en) * | 2022-02-28 | 2024-02-13 | 蜂巢能源科技股份有限公司 | Positive electrode material and preparation method and application thereof |
| CN114566641B (en) * | 2022-02-28 | 2024-02-23 | 蜂巢能源科技股份有限公司 | Positive electrode material and preparation method and application thereof |
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