CN113690442A - Fast ion conductor coated positive electrode material, preparation method thereof and lithium ion battery - Google Patents
Fast ion conductor coated positive electrode material, preparation method thereof and lithium ion battery Download PDFInfo
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- CN113690442A CN113690442A CN202110961271.3A CN202110961271A CN113690442A CN 113690442 A CN113690442 A CN 113690442A CN 202110961271 A CN202110961271 A CN 202110961271A CN 113690442 A CN113690442 A CN 113690442A
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- 239000010416 ion conductor Substances 0.000 title claims abstract description 95
- 239000007774 positive electrode material Substances 0.000 title claims abstract description 68
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 title claims abstract description 19
- 229910001416 lithium ion Inorganic materials 0.000 title claims abstract description 18
- 238000000576 coating method Methods 0.000 claims abstract description 92
- 239000011248 coating agent Substances 0.000 claims abstract description 87
- 239000007788 liquid Substances 0.000 claims abstract description 36
- 238000006243 chemical reaction Methods 0.000 claims abstract description 34
- 239000013543 active substance Substances 0.000 claims abstract description 33
- 239000000463 material Substances 0.000 claims abstract description 27
- 238000000034 method Methods 0.000 claims abstract description 27
- 238000002156 mixing Methods 0.000 claims abstract description 17
- 238000005507 spraying Methods 0.000 claims abstract description 8
- 239000010405 anode material Substances 0.000 claims description 38
- 238000010438 heat treatment Methods 0.000 claims description 35
- 239000010936 titanium Substances 0.000 claims description 32
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 24
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 24
- 239000001301 oxygen Substances 0.000 claims description 24
- 229910052760 oxygen Inorganic materials 0.000 claims description 24
- 229910052719 titanium Inorganic materials 0.000 claims description 23
- 239000010955 niobium Substances 0.000 claims description 15
- 239000012298 atmosphere Substances 0.000 claims description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- 229910052758 niobium Inorganic materials 0.000 claims description 7
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 claims description 6
- ZTILUDNICMILKJ-UHFFFAOYSA-N niobium(v) ethoxide Chemical compound CCO[Nb](OCC)(OCC)(OCC)OCC ZTILUDNICMILKJ-UHFFFAOYSA-N 0.000 claims description 6
- 239000002994 raw material Substances 0.000 claims description 6
- 238000012216 screening Methods 0.000 claims description 6
- VXUYXOFXAQZZMF-UHFFFAOYSA-N titanium(IV) isopropoxide Chemical compound CC(C)O[Ti](OC(C)C)(OC(C)C)OC(C)C VXUYXOFXAQZZMF-UHFFFAOYSA-N 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 239000002904 solvent Substances 0.000 claims description 5
- QUVMSYUGOKEMPX-UHFFFAOYSA-N 2-methylpropan-1-olate;titanium(4+) Chemical compound [Ti+4].CC(C)C[O-].CC(C)C[O-].CC(C)C[O-].CC(C)C[O-] QUVMSYUGOKEMPX-UHFFFAOYSA-N 0.000 claims description 4
- 239000007789 gas Substances 0.000 claims description 4
- XNHGKSMNCCTMFO-UHFFFAOYSA-D niobium(5+);oxalate Chemical compound [Nb+5].[Nb+5].[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O XNHGKSMNCCTMFO-UHFFFAOYSA-D 0.000 claims description 3
- LZRGWUCHXWALGY-UHFFFAOYSA-N niobium(5+);propan-2-olate Chemical compound [Nb+5].CC(C)[O-].CC(C)[O-].CC(C)[O-].CC(C)[O-].CC(C)[O-] LZRGWUCHXWALGY-UHFFFAOYSA-N 0.000 claims description 2
- 239000011247 coating layer Substances 0.000 abstract description 19
- 239000002103 nanocoating Substances 0.000 abstract description 7
- 238000012546 transfer Methods 0.000 abstract description 5
- 239000010410 layer Substances 0.000 description 20
- 239000000843 powder Substances 0.000 description 14
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 13
- 239000011572 manganese Substances 0.000 description 12
- 230000000052 comparative effect Effects 0.000 description 11
- 150000002500 ions Chemical class 0.000 description 10
- 229910052759 nickel Inorganic materials 0.000 description 10
- 239000000243 solution Substances 0.000 description 10
- 229910013716 LiNi Inorganic materials 0.000 description 9
- 239000012467 final product Substances 0.000 description 9
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 7
- 229910052744 lithium Inorganic materials 0.000 description 7
- 238000007873 sieving Methods 0.000 description 6
- 239000007787 solid Substances 0.000 description 6
- 238000005303 weighing Methods 0.000 description 6
- 239000010406 cathode material Substances 0.000 description 5
- 239000003792 electrolyte Substances 0.000 description 5
- 238000000635 electron micrograph Methods 0.000 description 5
- 239000002243 precursor Substances 0.000 description 5
- 239000002245 particle Substances 0.000 description 4
- 239000007784 solid electrolyte Substances 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- 229910015872 LiNi0.8Co0.1Mn0.1O2 Inorganic materials 0.000 description 3
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 3
- 239000000084 colloidal system Substances 0.000 description 3
- 239000011163 secondary particle Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- LSGOVYNHVSXFFJ-UHFFFAOYSA-N vanadate(3-) Chemical compound [O-][V]([O-])([O-])=O LSGOVYNHVSXFFJ-UHFFFAOYSA-N 0.000 description 3
- 239000000654 additive Substances 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 229920001940 conductive polymer Polymers 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000007599 discharging Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- FRMOHNDAXZZWQI-UHFFFAOYSA-N lithium manganese(2+) nickel(2+) oxygen(2-) Chemical compound [O-2].[Mn+2].[Ni+2].[Li+] FRMOHNDAXZZWQI-UHFFFAOYSA-N 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 229920000767 polyaniline Polymers 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 229910052720 vanadium Inorganic materials 0.000 description 2
- 102000004310 Ion Channels Human genes 0.000 description 1
- 229910014248 MzO2 Inorganic materials 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- MQRWBMAEBQOWAF-UHFFFAOYSA-N acetic acid;nickel Chemical compound [Ni].CC(O)=O.CC(O)=O MQRWBMAEBQOWAF-UHFFFAOYSA-N 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
- 238000000498 ball milling Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 238000005253 cladding Methods 0.000 description 1
- 230000001427 coherent effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000000755 effect on ion Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000012983 electrochemical energy storage Methods 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- XIXADJRWDQXREU-UHFFFAOYSA-M lithium acetate Chemical compound [Li+].CC([O-])=O XIXADJRWDQXREU-UHFFFAOYSA-M 0.000 description 1
- 229910003002 lithium salt Inorganic materials 0.000 description 1
- 159000000002 lithium salts Chemical class 0.000 description 1
- AZVCGYPLLBEUNV-UHFFFAOYSA-N lithium;ethanolate Chemical compound [Li+].CC[O-] AZVCGYPLLBEUNV-UHFFFAOYSA-N 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 229940071125 manganese acetate Drugs 0.000 description 1
- UOGMEBQRZBEZQT-UHFFFAOYSA-L manganese(2+);diacetate Chemical compound [Mn+2].CC([O-])=O.CC([O-])=O UOGMEBQRZBEZQT-UHFFFAOYSA-L 0.000 description 1
- 230000003446 memory effect Effects 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 229940078494 nickel acetate Drugs 0.000 description 1
- 125000004433 nitrogen atom Chemical group N* 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 239000011164 primary particle Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229910052707 ruthenium Inorganic materials 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 229910052712 strontium Inorganic materials 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- 239000011135 tin Substances 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- GPPXJZIENCGNKB-UHFFFAOYSA-N vanadium Chemical compound [V]#[V] GPPXJZIENCGNKB-UHFFFAOYSA-N 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
Images
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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
- 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
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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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M2004/021—Physical characteristics, e.g. porosity, surface area
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/028—Positive electrodes
-
- 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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Abstract
The invention provides a fast ion conductor coated positive electrode material, a preparation method thereof and a lithium ion battery, wherein the preparation method comprises the following steps: and spraying the fast ion conductor coating liquid into the fluidized bed reaction device, and mixing and coating the positive active substance and the fast ion conductor coating liquid in the fluidized bed reaction device to obtain a coating material. The invention provides a fluidized bed nano coating process, and the positive electrode material prepared by the method has a thin and uniform coating layer and an accurate and controllable thickness, can reduce the charge transfer resistance of a battery in the charge and discharge processes, and obviously improves the high rate performance and the cycle stability of the positive electrode material.
Description
Technical Field
The invention belongs to the technical field of lithium ion batteries, and relates to a fast ion conductor coated positive electrode material, a preparation method thereof and a lithium ion battery.
Background
The lithium ion battery is widely applied to portable electronic product markets such as mobile phones, digital cameras, personal computers and the like due to the characteristics of high energy density, high voltage, long service life, no memory effect, no pollution and the like, and has good development prospects in the fields of power batteries and large-scale energy storage in the future.
The lithium ion battery anode material is a key factor for restricting the capacity and the service life of the lithium battery, so the lithium ion battery anode material has great significance for the research of the anode material. Aiming at market demands, the lithium ion battery anode material mainly adopts doping, cladding, optimized synthesis process and the like to improve the performance. The coating technology is one of the methods which are most widely applied and have the best effect at present, namely, the specific capacity, the cycle performance, the rate capability and the like of the anode material are improved by coating a layer of oxide or other salt substances on the surface of the anode material. The surface coating modification can prevent the direct contact of the anode material and the electrolyte, inhibit the occurrence of side reactions and improve the cycle performance of the anode material; and secondly, the high-conductivity material can increase the electronic conductivity or ionic conductivity of the positive electrode material, and improve the rate capability of the material. At present, most of common coating agents of the positive electrode material are metal oxides, phosphate conductive polymers and the like, the ion conduction capability of the coating agents is weak, and the rate performance of the battery can be influenced when the coating agents are coated on the surface of the positive electrode material. Furthermore, a coating layer without ion conductivity is not suitable for a solid-state battery system, but rather increases the interfacial resistance between the positive electrode material and the electrolyte.
The fast ion conductor has wide application prospect in the fields of high-energy high-density batteries, electrochemical energy storage and the like. Taking lithium vanadate as an example, the lithium vanadate has a layered structure and high specific capacity, and can effectively improve the cycle performance of the ternary material. However, vanadium contains a plurality of valence states, and it is difficult to identify a synthesized component, and the coating tends to be nonuniform. Therefore, the modification of the ternary cathode material by using lithium vanadate needs to be further improved. The conductive polymer is a kind of polymer which is transformed into a conductor by chemical or electrochemical doping from a polymer with conjugated pi-pi bonds, and is an ideal electrode material of a secondary battery. Taking polyaniline as an example, the main chain of the ternary positive electrode material contains alternate benzene rings and nitrogen atoms, so that the ternary positive electrode material has the characteristics of easiness in synthesis, easiness in processing, good conductivity and the like, and the rate capability of the ternary positive electrode material can be improved to a certain extent by using the conductive polyaniline.
CN108023077A discloses a fast ion conductor coated modified high nickel positive electrode material and a preparation method thereof, the high nickel positive electrode material includes: the substrate is a compound LiNi shown as a formula I1-x-yCoxMnyMzO2(ii) a In the formula I, x is more than 0 and less than or equal to 0.20, y is more than 0 and less than or equal to 0.20, and z is more than 0 and less than or equal to 0.1; m is any one or more of Al, Mg, Ti, Zr, Mn, Ni, Sn, Co, Zn, W, Mo, Ru, Ca, Sr, Ba, B, Y, V and Nb; the preparation method comprises the following steps: and washing and drying the high-nickel anode material, then uniformly mixing with a proper amount of coating agent, sintering and sieving to obtain the fast ion conductor coated modified high-nickel anode material.
CN110690435A discloses a fast ion conductor coated high-nickel ternary positive electrode material and a preparation method thereof, wherein the high-nickel ternary positive electrode material is spherical or quasi-spherical secondary particles consisting of primary particles, the diameter of the secondary particles is 1-30 mu m, and the chemical formula of the secondary particles is LiNi0.8Co0.1Mn0.1O2. The preparation method comprises the following steps: weighing raw materials for synthesizing the fast ionic conductor according to a proportion, and uniformly dispersing the raw materials in a solvent to obtain a mixed solution; adding the high-nickel ternary precursor into the mixed solution, and then stirring, drying and grinding to obtain high-nickel ternary precursor powder coated by the fast ion conductor; and uniformly mixing the obtained precursor powder with lithium salt, and sintering to obtain the fast ion conductor coated high-nickel ternary cathode material.
CN105938899A discloses a preparation method of a fast ionic conductor coated modified lithium ion battery anode material, which comprises the steps of ball-milling and mixing nano-scale aluminum powder and the anode material, and stirring and reacting the mixture with a lithium-containing solution at the temperature of 40-80 ℃ to obtain an aluminum hydroxide colloid coated anode material precursor; and calcining the precursor of the aluminum hydroxide colloid-coated positive electrode material at the temperature of 500-900 ℃ to obtain the aluminum hydroxide colloid-coated positive electrode material.
For the coating of the fast ion conductor, the prior art is mostly dry coating, the dry coating has strict limitation on the particle size of the coating additive, and the nano-scale coating additive needs to be selected for uniform coating, so that the cost is high and the types are few. The dry-method coated anode material is mostly point-shaped coated, the contact between the anode material and the electrolyte cannot be effectively avoided, and the point-shaped coated anode material applied to a solid system cannot establish a continuous ion channel, so that the improvement effect on ion conduction is limited.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a fast ion conductor coated positive electrode material, a preparation method thereof and a lithium ion battery.
In order to achieve the purpose, the invention adopts the following technical scheme:
in a first aspect, the present invention provides a method for preparing a fast ion conductor coated positive electrode material, wherein the method comprises:
and atomizing the fast ion conductor coating liquid, spraying the atomized fast ion conductor coating liquid into a fluidized bed reaction device, and mixing and coating the positive active substance and the atomized fast ion conductor coating liquid in the fluidized bed reaction device to obtain a coating material.
The invention is different from the common dry coating process, and provides a fluidized bed nano coating process, the coating layer of the anode material prepared by the method is thin and uniform, the thickness is accurate and controllable, the charge transfer resistance of the battery in the charging and discharging process can be reduced, the high rate performance and the cycle stability of the anode material are obviously improved, the interface film impedance and the charge transfer impedance of electrolyte and the anode material are effectively improved, the cycle and the rate performance are obviously improved, meanwhile, the fast ion conductor can also be used as the solid electrolyte of a lithium ion battery, and the ion conduction capability of the anode material is effectively improved by coating the fast ion conductor on the surface of the anode material, so that the anode material has wide application prospect in a solid battery system.
As a preferred technical solution of the present invention, the preparation method further comprises: the coating material is subjected to heat treatment to obtain the anode material.
Preferably, the heat treatment temperature is 600 to 800 ℃, for example, 600 ℃, 620 ℃, 640 ℃, 660 ℃, 680 ℃, 700 ℃, 720 ℃, 740 ℃, 760 ℃, 780 ℃ or 800 ℃, but is not limited to the recited values, and other values not recited in the range of the values are also applicable.
Preferably, the heat treatment time is 4 to 8 hours, for example, 4.0 hours, 4.2 hours, 4.4 hours, 4.6 hours, 4.8 hours, 5.0 hours, 5.2 hours, 5.4 hours, 5.6 hours, 5.8 hours, 6.0 hours, 6.2 hours, 6.4 hours, 6.6 hours, 6.8 hours, 7.0 hours, 7.2 hours, 7.4 hours, 7.6 hours, 7.8 hours or 8.0 hours, but is not limited to the enumerated values, and other non-enumerated values in the numerical range are also applicable.
Preferably, the heat treatment process is performed in an oxygen-containing atmosphere.
Preferably, the oxygen-containing atmosphere has a volume concentration of 20 to 100% of oxygen, for example, 20%, 25%, 30%, 35%, 40%, 45%, 50%, 55%, 60%, 65%, 70%, 75%, 80%, 85%, 90%, 95% or 100%, but not limited to the recited values, and other values not recited in the range of values are also applicable.
As a preferable technical scheme, the anode material is screened to obtain a product.
Preferably, the screening process uses a 300-400 mesh screen, such as 300 mesh, 310 mesh, 320 mesh, 330 mesh, 340 mesh, 350 mesh, 360 mesh, 370 mesh, 380 mesh, 390 mesh or 400 mesh, but not limited to the values listed, and other values not listed in the range of the values are also applicable.
As a preferable technical solution of the present invention, the fast ion conductor coating liquid includes a coating raw material and a solvent.
As a preferable technical scheme of the invention, the coating raw material comprises a niobium source and a titanium source.
Preferably, the niobium source comprises niobium ethoxide.
Preferably, the titanium source comprises isopropyl titanate.
Preferably, the niobium source and the titanium source are mixed in a mass ratio of Nb to Ti of 2 to 1.
Preferably, the solvent comprises ethanol and/or water.
As a preferable technical scheme of the invention, the fast ion conductor coating liquid is sprayed into the fluidized bed reaction device under the action of gas flow.
Preferably, the gas flow is preheated and then sprayed into the fluidized bed reaction device with the fast ion conductor coating liquid;
preferably, the preheating temperature is 100 to 300 ℃, for example, 100 ℃, 120 ℃, 140 ℃, 160 ℃, 180 ℃, 200 ℃, 220 ℃, 240 ℃, 260 ℃, 280 ℃ or 300 ℃, but is not limited to the recited values, and other values not recited in the range of the values are also applicable.
In a second aspect, the invention provides a positive electrode material prepared by the preparation method of the first aspect, where the positive electrode material includes a positive electrode active material and a fast ion conductor layer coated on the surface of the positive electrode active material.
In a preferred embodiment of the present invention, the thickness of the fast ion conductor layer is 1 to 20nm, and may be, for example, 1nm, 2nm, 3nm, 4nm, 5nm, 6nm, 7nm, 8nm, 9nm, 10nm, 11nm, 12nm, 13nm, 14nm, 15nm, 16nm, 17nm, 18nm, 19nm or 20nm, but the present invention is not limited to the above-mentioned values, and other values not listed in the above-mentioned value range are also applicable.
As a preferable technical solution of the present invention, the fast ion conductor in the fast ion conductor layer includes titanium niobate.
In a third aspect, the invention provides a lithium ion battery, which includes a positive electrode, a diaphragm and a negative electrode that are sequentially stacked, wherein a positive electrode material adopted by the positive electrode is the positive electrode material of the second aspect.
The lithium ion battery prepared from the anode material prepared by the invention can increase the ion conductivity of the surface after being coated on the surface of the anode material, can effectively improve the multiplying power performance of the battery in a liquid lithium ion battery system, can construct a good ion conduction passage between the anode material and a solid electrolyte in a solid lithium ion battery system, and effectively reduces the interface impedance, and meanwhile, the coating layer prepared by the fluidized bed nano coating process is thin and uniform, and a coherent ion passage is formed on the surface of the anode material, so that the multiplying power and the cycle performance of the battery are effectively improved.
Compared with the prior art, the invention has the beneficial effects that:
the invention is different from the common dry coating process, and provides a fluidized bed nano coating process, the coating layer of the anode material prepared by the method is thin and uniform, the thickness is accurate and controllable, the charge transfer resistance of the battery in the charging and discharging process can be reduced, the high rate performance and the cycle stability of the anode material are obviously improved, the interface film impedance and the charge transfer impedance of electrolyte and the anode material are effectively improved, the cycle and the rate performance are obviously improved, meanwhile, the fast ion conductor can also be used as the solid electrolyte of a lithium ion battery, and the ion conduction capability of the anode material is effectively improved by coating the fast ion conductor on the surface of the anode material, so that the anode material has wide application prospect in a solid battery system.
Drawings
FIG. 1 is an electron micrograph of a positive electrode material prepared in example 1 of the present invention;
FIG. 2 is an electron micrograph of a positive electrode material prepared in comparative example 1 of the present invention;
FIG. 3 is an electron micrograph of a positive electrode material prepared in comparative example 2 of the present invention;
fig. 4 is a cycle diagram of the liquid half-cell prepared in example 1, comparative example 1 and comparative example 2 of the present invention.
Detailed Description
The technical scheme of the invention is further explained by the specific implementation mode in combination with the attached drawings.
Example 1
The embodiment provides a preparation method of a fast ion conductor coated positive electrode material, which specifically comprises the following steps:
(1) 500g of LiNi as a positive electrode active material was taken0.8Co0.1Mn0.1O2Introducing the powder into a fluidized bed reaction device and preheating to 200 ℃;
(2) calculating and weighing 5.2g of isopropyl titanate and 11.64g of niobium ethoxide according to the molar ratio of Ti to Nb of 1:2, adding 120g of ethanol, uniformly mixing, preparing to obtain a fast ionic conductor coating solution, preheating airflow to 200 ℃, spraying the fast ionic conductor coating solution into a fluidized bed reaction device, mixing and coating an anode active substance with the fast ionic conductor coating solution in the fluidized bed reaction device to form a uniform coating layer, and obtaining a coating material;
(3) and (3) carrying out heat treatment on the coating material at 750 ℃ for 5h, wherein the heat treatment process is carried out in an oxygen-containing atmosphere (the volume concentration of oxygen is 97%), and after the heat treatment is finished, sieving by a 400-mesh sieve to obtain a final product.
The prepared positive electrode material comprises a positive electrode active substance and a titanium niobate fast ion conductor layer coated on the surface of the positive electrode active substance, the thickness of the titanium niobate fast ion conductor layer is 5nm, and a finished electron microscope photo of the evidence material is shown in figure 1.
Example 2
The embodiment provides a preparation method of a fast ion conductor coated positive electrode material, which specifically comprises the following steps:
(1) 500g of LiNi as a positive electrode active material was taken0.8Co0.1Mn0.1O2Introducing the powder into a fluidized bed reaction device and preheating to 100 ℃;
(2) calculating and weighing 1.25g of isobutyl titanate and 2.328g of pentaethoxy niobium according to the molar ratio of Ti to Nb of 1:2, adding 100g of water, uniformly mixing, preparing to obtain a fast ionic conductor coating liquid, preheating airflow to 100 ℃, spraying the fast ionic conductor coating liquid into a fluidized bed reaction device, mixing and coating an anode active substance with the fast ionic conductor coating liquid in the fluidized bed reaction device to form a uniform coating layer, and obtaining a coating material;
(3) and (3) carrying out heat treatment on the coating material at 600 ℃ for 8h, carrying out the heat treatment process in an oxygen-containing atmosphere (the volume concentration of oxygen is 20%), and carrying out 300-mesh sieving after the heat treatment is finished to obtain a final product.
The prepared positive electrode material comprises a positive electrode active substance and a titanium niobate fast ion conductor layer coated on the surface of the positive electrode active substance, and the thickness of the titanium niobate fast ion conductor layer is 1 nm.
Example 3
The embodiment provides a preparation method of a fast ion conductor coated positive electrode material, which specifically comprises the following steps:
(1) 500g of LiNi as a positive electrode active material was taken0.8Co0.1Mn0.1O2Introducing the powder into a fluidized bed reaction device and preheating to 150 ℃;
(2) 5.2g of isopropyl titanate and 11.93g of niobium pentaisopropoxide are calculated and weighed according to the molar ratio of Ti to Nb of 1:2.05, 110g of ethanol is added and uniformly mixed to prepare a fast ionic conductor coating liquid, airflow is preheated to 150 ℃ and then sprayed into a fluidized bed reaction device with the fast ionic conductor coating liquid, and an anode active substance is mixed and coated with the fast ionic conductor coating liquid in the fluidized bed reaction device to form a uniform coating layer to obtain a coating material;
(3) and (3) carrying out heat treatment on the coating material at 650 ℃ for 7h, wherein the heat treatment process is carried out in an oxygen-containing atmosphere (the volume concentration of oxygen is 40%), and after the heat treatment is finished, carrying out 320-mesh screening to obtain a final product.
The prepared positive electrode material comprises a positive electrode active substance and a titanium niobate fast ion conductor layer coated on the surface of the positive electrode active substance, the thickness of the titanium niobate fast ion conductor layer is 5nm, and the mass of the fast ion conductor coating layer accounts for 12750ppm of the mass of the positive electrode active substance.
Example 4
The embodiment provides a preparation method of a fast ion conductor coated positive electrode material, which specifically comprises the following steps:
(1) 500g of LiNi as a positive electrode active material was taken0.8Co0.1Mn0.1O2Introducing the powder into a fluidized bed reaction device and preheating to 200 ℃;
(2) calculating and weighing 12.5g of isobutyl titanate and 24.44g of niobium oxalate according to the molar ratio of Ti to Nb of 1:2.1, adding 130g of water, uniformly mixing, preparing to obtain a fast ionic conductor coating liquid, preheating airflow to 200 ℃, spraying the fast ionic conductor coating liquid into a fluidized bed reaction device, mixing and coating an anode active substance with the fast ionic conductor coating liquid in the fluidized bed reaction device to form a uniform coating layer, and obtaining a coating material;
(3) and (3) carrying out heat treatment on the coating material at 700 ℃ for 6h, carrying out the heat treatment process in an oxygen-containing atmosphere (the volume concentration of oxygen is 60%), and carrying out 350-mesh screening after the heat treatment is finished to obtain a final product.
The prepared positive electrode material comprises a positive electrode active substance and a titanium niobate fast ion conductor layer coated on the surface of the positive electrode active substance, the thickness of the titanium niobate fast ion conductor layer is 10nm, and the mass of a fast ion conductor coating layer accounts for 25500ppm of the mass of the positive electrode active substance.
Example 5
The embodiment provides a preparation method of a fast ion conductor coated positive electrode material, which specifically comprises the following steps:
(1) 500g of LiNi as a positive electrode active material was taken0.8Co0.1Mn0.1O2Introducing the powder into a fluidized bed reaction device and preheating to 250 ℃;
(2) calculating and weighing 15.6g of isopropyl titanate and 37.54g of niobium ethoxide according to the molar ratio of Ti to Nb of 1:2.15, adding 140g of ethanol, uniformly mixing, preparing to obtain a fast ionic conductor coating solution, preheating airflow to 250 ℃, spraying the fast ionic conductor coating solution into a fluidized bed reaction device along with the airflow, and mixing and coating the positive active substance and the fast ionic conductor coating solution in the fluidized bed reaction device to form a uniform coating layer to obtain a coating material;
(3) and (3) carrying out heat treatment on the coating material at 750 ℃ for 5h, wherein the heat treatment process is carried out in an oxygen-containing atmosphere (the volume concentration of oxygen is 80%), and after the heat treatment is finished, carrying out 380-mesh screening to obtain a final product.
The prepared positive electrode material comprises a positive electrode active substance and a titanium niobate fast ion conductor layer coated on the surface of the positive electrode active substance, the thickness of the titanium niobate fast ion conductor layer is 15nm, and the mass of the fast ion conductor coating layer accounts for 38250ppm of the mass of the positive electrode active substance.
Example 6
The embodiment provides a preparation method of a fast ion conductor coated positive electrode material, which specifically comprises the following steps:
(1) 500g of LiNi as a positive electrode active material was taken0.8Co0.1Mn0.1O2Introducing the powder into a fluidized bed reaction device and preheating to 300 ℃;
(2) calculating and weighing 20.8g of isobutyl titanate and 51.22g of niobium oxalate according to the molar ratio of Ti to Nb of 1:2.2, adding 150g of water, uniformly mixing, preparing to obtain a fast ionic conductor coating liquid, preheating airflow to 300 ℃, spraying the fast ionic conductor coating liquid into a fluidized bed reaction device, mixing and coating an anode active substance with the fast ionic conductor coating liquid in the fluidized bed reaction device to form a uniform coating layer, and obtaining a coating material;
(3) and (3) carrying out heat treatment on the coating material at 800 ℃ for 4h, carrying out the heat treatment process in an oxygen-containing atmosphere (the volume concentration of oxygen is 100%), and carrying out 400-mesh screening after the heat treatment is finished to obtain a final product.
The prepared positive electrode material comprises a positive electrode active substance and a titanium niobate fast ion conductor layer coated on the surface of the positive electrode active substance, the thickness of the titanium niobate fast ion conductor layer is 20nm, and the mass of the fast ion conductor coating layer accounts for 51000ppm of the mass of the positive electrode active substance.
Example 7
The embodiment provides a preparation method of a fast ion conductor coated positive electrode material, which specifically comprises the following steps:
(1) 500g of a positive electrode active material L was takeniNi0.8Co0.1Mn0.1O2Introducing the powder into a fluidized bed reaction device and preheating to 200 ℃;
(2) 8.264g of lithium ethoxide and 56.4636g of isopropyl titanate are calculated and weighed according to the molar ratio of Li to Ti being 4:5, 120g of ethanol is added and mixed uniformly to obtain fast ionic conductor coating liquid, airflow is preheated to 200 ℃ and then is sprayed into a fluidized bed reaction device with the fast ionic conductor coating liquid, and an anode active substance is mixed and coated with the fast ionic conductor coating liquid in the fluidized bed reaction device to form a uniform coating layer to obtain a coating material;
(3) and (3) carrying out heat treatment on the coating material at 750 ℃ for 5h, wherein the heat treatment process is carried out in an oxygen-containing atmosphere (the volume concentration of oxygen is 97%), and after the heat treatment is finished, sieving by a 400-mesh sieve to obtain a final product.
The prepared positive electrode material comprises a positive electrode active substance and a lithium titanate fast ion conductor layer coated on the surface of the positive electrode active substance, wherein the thickness of the lithium titanate fast ion conductor layer is 5 nm.
Example 8
The embodiment provides a preparation method of a fast ion conductor coated positive electrode material, which specifically comprises the following steps:
(1) 500g of LiNi as a positive electrode active material was taken0.8Co0.1Mn0.1O2Introducing the powder into a fluidized bed reaction device and preheating to 200 ℃;
(2) 1.9844g of lithium acetate, 2.9932g of nickel acetate and 11.7923g of manganese acetate are calculated and weighed according to the molar ratio of Li to Ni to Mn of 1:0.4:1.6, 120g of pure water is added and uniformly mixed to prepare fast ionic conductor coating liquid, the fast ionic conductor coating liquid is carried after the airflow is preheated to 200 ℃ and is sprayed into a fluidized bed reaction device, and the positive active substance is mixed and coated with the fast ionic conductor coating liquid in the fluidized bed reaction device to form a uniform coating layer to obtain a coating material;
(3) and (3) carrying out heat treatment on the coating material at 750 ℃ for 5h, wherein the heat treatment process is carried out in an oxygen-containing atmosphere (the volume concentration of oxygen is 97%), and after the heat treatment is finished, sieving by a 400-mesh sieve to obtain a final product.
The prepared positive electrode material comprises a positive electrode active substance and a lithium nickel manganese oxide fast ion conductor layer coated on the surface of the positive electrode active substance, wherein the thickness of the lithium nickel manganese oxide fast ion conductor layer is 5 nm.
Comparative example 1
This example provides a positive electrode active material LiNi0.8Co0.1Mn0.1O2Powder, uncoated LiNi0.8Co0.1Mn0.1O2An electron micrograph of the powder particles is shown in FIG. 2.
Comparative example 2
The embodiment provides a preparation method of a fast ion conductor coated positive electrode material, which specifically comprises the following steps:
(1) 100g of LiNi as a positive electrode active material was taken0.8Co0.1Mn0.1O2Adding the powder and 1.275g of titanium niobate powder into a mixing device, and stirring for 10min at the stirring speed of 2500rpm to obtain a coating material;
(2) and (3) carrying out heat treatment on the coating material at 750 ℃ for 5 hours, wherein the heat treatment process is carried out in an oxygen-containing atmosphere (the volume concentration of oxygen is 97 percent), and after the heat treatment is finished, sieving by a 400-mesh sieve to obtain a final product.
As can be seen from the electron micrographs of the positive electrode material particles shown in fig. 1, fig. 2, and fig. 3, the coating layer on the surface of the positive electrode material particle in fig. 1 (example 1) is more uniform.
The positive electrode materials prepared in examples 1 to 6 and comparative examples 1 and 2 were used to prepare liquid half cells and solid half cells, which were subjected to electrochemical performance tests, respectively, and the test results of the liquid half cells are shown in table 1, and the cycle diagrams of the liquid half cells of example 1, comparative example 1 and comparative example 2 are shown in fig. 4. The test results of the solid-state half-cell are shown in table 2.
TABLE 1
TABLE 2
As can be seen from the data in table 1, the test results of example 1 are higher than those of comparative example 1 and comparative example 2, which shows that the cathode material using the fluidized bed nano coating process provided by the present application is superior to the uncoated cathode material and the cathode material using the dry coating process in rate and cycle performance. The reason is that titanium niobate is used as a fast ion conductor, can increase the ion conductivity of the surface after coating the surface of the anode material, can effectively improve the rate capability of the battery in a liquid system, can construct a good ion conduction path between the anode material and the interface of the solid electrolyte in a solid system, and effectively reduces the interface impedance, and meanwhile, the coating layer prepared by the fluidized bed nano coating process is thin and uniform, and forms a continuous ion path on the surface of the anode material, thereby effectively improving the rate and the cycle performance of the battery.
The applicant declares that the above description is only a specific embodiment of the present invention, but the scope of the present invention is not limited thereto, and it should be understood by those skilled in the art that any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are within the scope and disclosure of the present invention.
Claims (10)
1. A preparation method of a fast ion conductor coated positive electrode material is characterized by comprising the following steps:
and spraying the fast ion conductor coating liquid into the fluidized bed reaction device, and mixing and coating the positive active substance and the fast ion conductor coating liquid in the fluidized bed reaction device to obtain a coating material.
2. The method of claim 1, further comprising: the coating material is subjected to heat treatment to obtain the anode material;
preferably, the heat treatment temperature is 600-800 ℃;
preferably, the heat treatment time is 4-8 h;
preferably, the heat treatment process is carried out in an oxygen-containing atmosphere;
preferably, in the oxygen-containing atmosphere, the volume concentration of oxygen is 20-100%.
3. The preparation method according to claim 1 or 2, wherein the positive electrode material is sieved to obtain a product;
preferably, the screening process adopts a screen of 300-400 meshes.
4. The method according to any one of claims 1-3, wherein the fast ion conductor coating solution comprises a coating raw material and a solvent.
5. The method of claim 4, wherein the clad raw material comprises a niobium source and a titanium source;
preferably, the niobium source comprises any one or a combination of at least two of niobium ethoxide, niobium pentaethoxide, niobium pentaisopropoxide or niobium oxalate;
preferably, the titanium source comprises isopropyl titanate or isobutyl titanate;
preferably, the niobium source and the titanium source are mixed according to a molar ratio of Ti to Nb being 1 (2-2.2);
preferably, the solvent comprises ethanol and/or water.
6. The preparation method according to any one of claims 1 to 5, wherein the fast ion conductor coating liquid is sprayed into a fluidized bed reaction device under the action of a gas flow;
preferably, the gas flow is preheated and then sprayed into the fluidized bed reaction device with the fast ion conductor coating liquid;
preferably, the preheating temperature is 100-300 ℃.
7. The positive electrode material prepared by the preparation method of any one of claims 1 to 6, wherein the positive electrode material comprises a positive electrode active substance and a fast ion conductor layer coated on the surface of the positive electrode active substance.
8. The positive electrode material according to claim 7, wherein the fast ion conductor layer has a thickness of 1 to 20 nm.
9. The positive electrode material as claimed in claim 7 or 8, wherein the fast ion conductor in the fast ion conductor layer comprises titanium niobate.
10. A lithium ion battery, characterized in that, the lithium ion battery comprises a positive electrode, a diaphragm and a negative electrode which are sequentially laminated, wherein the positive electrode material adopted by the positive electrode is the positive electrode material of any one of claims 7 to 9.
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