CN113461066A - Nano Li1.25Mn0.5V0.25O2Preparation method of positive electrode material - Google Patents
Nano Li1.25Mn0.5V0.25O2Preparation method of positive electrode material Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 7
- 239000007774 positive electrode material Substances 0.000 title claims description 5
- 239000000243 solution Substances 0.000 claims abstract description 42
- 239000011572 manganese Substances 0.000 claims abstract description 33
- 238000002360 preparation method Methods 0.000 claims abstract description 28
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 24
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000010405 anode material Substances 0.000 claims abstract description 21
- 239000011259 mixed solution Substances 0.000 claims abstract description 21
- 238000001354 calcination Methods 0.000 claims abstract description 15
- 238000010438 heat treatment Methods 0.000 claims abstract description 13
- 239000002243 precursor Substances 0.000 claims abstract description 13
- 238000000227 grinding Methods 0.000 claims abstract description 11
- XIXADJRWDQXREU-UHFFFAOYSA-M lithium acetate Chemical compound [Li+].CC([O-])=O XIXADJRWDQXREU-UHFFFAOYSA-M 0.000 claims abstract description 9
- FSJSYDFBTIVUFD-SUKNRPLKSA-N (z)-4-hydroxypent-3-en-2-one;oxovanadium Chemical compound [V]=O.C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O FSJSYDFBTIVUFD-SUKNRPLKSA-N 0.000 claims abstract description 8
- 229940071125 manganese acetate Drugs 0.000 claims abstract description 8
- UOGMEBQRZBEZQT-UHFFFAOYSA-L manganese(2+);diacetate Chemical compound [Mn+2].CC([O-])=O.CC([O-])=O UOGMEBQRZBEZQT-UHFFFAOYSA-L 0.000 claims abstract description 8
- 235000006408 oxalic acid Nutrition 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000001816 cooling Methods 0.000 claims abstract description 7
- 239000000843 powder Substances 0.000 claims abstract description 7
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 6
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 6
- 239000002904 solvent Substances 0.000 claims abstract description 6
- 238000001291 vacuum drying Methods 0.000 claims abstract description 3
- 238000001035 drying Methods 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 7
- 238000003760 magnetic stirring Methods 0.000 claims description 4
- 229910021645 metal ion Inorganic materials 0.000 claims description 2
- 238000003303 reheating Methods 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 6
- 239000010406 cathode material Substances 0.000 abstract description 4
- 238000003980 solgel method Methods 0.000 abstract description 4
- 230000015572 biosynthetic process Effects 0.000 abstract description 3
- 238000003786 synthesis reaction Methods 0.000 abstract description 3
- 238000002156 mixing Methods 0.000 abstract description 2
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 9
- 229910001416 lithium ion Inorganic materials 0.000 description 9
- 239000002245 particle Substances 0.000 description 6
- 238000005303 weighing Methods 0.000 description 5
- 238000001704 evaporation Methods 0.000 description 3
- 238000000975 co-precipitation Methods 0.000 description 2
- 238000001027 hydrothermal synthesis Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 238000010532 solid phase synthesis reaction Methods 0.000 description 2
- 238000001308 synthesis method Methods 0.000 description 2
- 229920000463 Poly(ethylene glycol)-block-poly(propylene glycol)-block-poly(ethylene glycol) Polymers 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 239000003945 anionic surfactant Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000002563 ionic surfactant Substances 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 230000003446 memory effect Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G45/00—Compounds of manganese
- C01G45/12—Manganates manganites or permanganates
- C01G45/1221—Manganates or manganites with a manganese oxidation state of Mn(III), Mn(IV) or mixtures thereof
- C01G45/1228—Manganates or manganites with a manganese oxidation state of Mn(III), Mn(IV) or mixtures thereof of the type [MnO2]n-, e.g. LiMnO2, Li[MxMn1-x]O2
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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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
- 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
- H01M4/485—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/50—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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/40—Electric properties
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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
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- 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
Abstract
The invention discloses a nano Li1.25Mn0.5V0.25O2The preparation method of the cathode material comprises the following steps: dissolving lithium acetate, manganese acetate and vanadyl acetylacetonate in ethanol to obtain a solution 1; dissolving oxalic acid in ethanol to obtain a solution 2; slowly adding the solution 2 into the solution 1 to obtain a mixed solution 3; will P123Adding the mixed solution into the mixed solution 3, and simultaneously dropwise adding ammonia water to enable the pH of the solution to be =7, so as to obtain a mixed solution 4; putting the mixed solution 4 into a water bath kettle, heating at constant temperature to evaporate the solvent to obtain sol; placing the sol inHeating again in a box furnace to obtain gel; carrying out vacuum drying on the gel to obtain a precursor; grinding the precursor, calcining, taking out the powder, cooling, grinding, and calcining again to obtain the anode material Li1.25Mn0.5V0.25O2. The invention adopts a sol-gel method, can achieve the uniform mixing of molecular or atomic level in the synthesis process, and improves the electrochemical performance of the material.
Description
Technical Field
The invention belongs to the technical field of lithium ion batteries, relates to a preparation method of a cathode material, and particularly relates to nano Li1.25Mn0.5V0.25O2A preparation method of the cathode material.
Background
The lithium ion battery as a novel secondary energy storage battery has the advantages of no memory effect, high specific capacity and the like. With the proposal of the national 'double-carbon' target, the lithium ion battery is environment-friendly, and has come to great development opportunities. In recent years, the application field of the lithium ion battery is continuously widened, and the shadow of the lithium ion battery can be seen everywhere from a miniature electronic product to a new energy automobile and a smart power grid, so that more severe requirements on the performance of the lithium ion battery are provided. The driving range of the electric automobile needs to be improved by the high-energy-density lithium ion battery, and the positive electrode material is taken as a key factor for restricting the performance of the lithium ion battery, so that a great deal of intensive research of researchers is attracted.
The synthesis methods of the lithium ion battery anode material are various, and the synthesis methods widely applied at present mainly comprise a hydrothermal method, a coprecipitation method, a sol-gel method, a high-temperature solid phase method and the like. Among the preparation methods, the hydrothermal method requires constant temperature and pressure, and has high requirements on equipment because the temperature and the pressure are high. The co-precipitation method requires strict control of the PH during the preparation process. The high-temperature solid phase method requires higher synthesis temperature, consumes large energy and increases production cost.
In view of the above, the present invention is particularly proposed.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a preparation method, and Li with stable performance and high capacity is obtained1.25Mn0.5V0.25O2And (3) a positive electrode material. The sol-gel method adopted by the invention can achieve the uniform mixing of molecular or atomic level in the synthesis process, and the purity of the synthesized product is high. With a surfactant PEO-PPO-PEO (P)123) As a template, particles with finer particle size are prepared, and high-capacity Li is obtained1.25Mn0.5V0.25O2The electrochemical performance of the anode material is improved.
In order to solve the technical problems, the invention adopts the following technical scheme:
nano Li1.25Mn0.5V0.25O2The preparation method of the anode material comprises the following specific steps:
(1) adding lithium acetate (CH)3COOLi), manganese acetate (Mn (CH)3COO)2·4H2O) and vanadyl acetylacetonate (C)10H14O5V) dissolving in ethanol, and recording as solution 1;
(2) weighing a certain amount of oxalic acid, dissolving in ethanol to form a transparent solution, and marking as a solution 2;
(3) slowly adding the solution 2 into the solution 1 through a constant-temperature magnetic stirrer, and marking as a mixed solution 3;
(4) weighing a certain amount of P under the action of a constant-temperature magnetic stirrer123Adding the mixed solution into the mixed solution 3, and simultaneously dropwise adding ammonia water to ensure that the solution has a pH =7, and marking as a mixed solution 4;
(5) putting the mixed solution 4 into a water bath kettle, heating at constant temperature to evaporate the solvent to obtain sol;
(6) placing the sol in a box type furnace for reheating to obtain gel;
(7) carrying out vacuum drying on the gel to obtain a precursor;
(8) grinding the precursor, and calcining in a tube furnace (air atmosphere);
(9) taking out the powder, cooling to room temperature, fully grinding again, and carrying out secondary calcination to finally obtain the anode material Li1.25Mn0.5V0.25O2 。
Further, in the step (1) of the preparation method, the molar ratio of lithium acetate, manganese acetate and vanadyl acetylacetonate is 5:2: 1.
Further, in the step (2) of the preparation method, the molar ratio of oxalic acid to metal ions is 1: 1.
Further, in the step (3) of the preparation method, the constant-temperature magnetic stirring is carried out for 10min at the temperature of 70-80 ℃.
Further, in the step (4) of the production method, P123The mass of (a) is 2g to 4 g.
Further, in the step (4) of the preparation method, the constant-temperature magnetic stirring is carried out for 20min to 30min at the temperature of (70 ℃ to 80 ℃).
Further, in the step (5) of the preparation method, the temperature of water bath heating is 80-100 ℃.
Further, in the preparation method, in the step (6), the heating temperature is 180-220 ℃, and the time is 10-14 hours.
Further, in the step (7), the drying temperature is 100-150 ℃ and the drying time is 4-6 h.
Further, in the step (8), the preferable calcining temperature is 480-550 ℃ and the time is 5-8 hours.
Further, in the step (9) of the preparation method, the calcination temperature is 760-900 ℃, and the calcination time is 10-15 hours.
The invention has the beneficial effects that: the invention adopts P123The anode material Li with uniform appearance is successfully prepared by a sol-gel method serving as a template1.25Mn0.5V0.25O2。P123Compared with an anionic surfactant, the ionic surfactant can effectively disperse the particle diameter to obtain a material with smaller and more uniform particle size, and meanwhile, because the material has smaller particles and larger specific surface area, the contact area between an active substance and an electrolyte is increased, so that the circulation stability of the material is remarkably improved.
Drawings
FIG. 1 shows Li prepared in example 1 of the present invention1.25Mn0.5V0.25O2SEM image of (d).
FIG. 2 shows Li prepared in example 1 of the present invention1.25Mn0.5V0.25O2Charge and discharge curves at a current density of 20 mA/g.
FIG. 3 shows Li prepared in example 1 of the present invention1.25Mn0.5V0.25O2Cycling performance plot at 100mA/g current density.
Detailed Description
To facilitate understanding of the present invention, a nano Li is described below with reference to specific examples1.25Mn0.5V0.25O2The preparation method of the cathode material is described in detail, and it should be understood by those skilled in the art that the examples are only for helping understanding the present invention and should not be construed as specifically limiting the present invention.
Example 1
Nano Li1.25Mn0.5V0.25O2The preparation method of the anode material comprises the following specific steps:
(1) 8.2487g (0.125 mol) of lithium acetate, 12.2543g (0.05 mol) of manganese acetate and 6.6287g (0.025 mol) of vanadyl acetylacetonate were dissolved in 100mL of ethanol and designated as solution 1.
(2) 18.0069g (0.2 mol) of oxalic acid was dissolved in 100mL of ethanol to give a clear solution, which was designated as solution 2.
(3) Stirring for 10min at 80 ℃ by a constant-temperature magnetic stirrer, slowly adding the solution 2 into the solution 1, and recording the mixed solution as 3.
(4) Weighing 4g of P123Adding into the above solution 3, stirring with a magnetic stirrer at a constant temperature of 80 ℃ for 20min, and adding dropwise ammonia water to obtain a solution with pH =7, and recording as solution 4.
(5) And (3) putting the mixed solution 4 into a water bath kettle, keeping the temperature constant at 90 ℃, heating and evaporating the solvent to obtain sol.
(6) And (3) placing the sol in a box furnace, and heating for 12h at 180 ℃ to obtain gel.
(7) And drying the gel at 120 ℃ for 6h in vacuum to obtain a precursor.
(8) After grinding, the precursor was calcined in a tube furnace (air atmosphere) at 500 ℃ for 8 h.
(9) Taking out the powder, cooling to room temperature, fully grinding again, carrying out secondary calcination for 12h at 800 ℃, and finally obtaining the anode material Li1.25Mn0.5V0.25O2 。
FIG. 1 shows Li prepared in example 1 of the present invention1.25Mn0.5V0.25O2The product is nano-particles, and no other impurities are generated on the surface of the particles in the SEM image.
FIG. 2 shows Li prepared in example 1 of the present invention1.25Mn0.5V0.25O2According to a charge-discharge curve chart under the current density of 20mA/g, the charge-discharge capacity of the material exceeds 350 mAh/g.
FIG. 3 shows Li prepared in example 1 of the present invention1.25Mn0.5V0.25O2According to a cycle performance diagram under the current density of 100mA/g, the initial discharge capacity can reach 313.5 mAh/g, and after 150 cycles, the material still has a high capacity retention rate.
Example 2
Nano Li1.25Mn0.5V0.25O2The preparation method of the anode material comprises the following specific steps:
(1) 4.1243g (0.0625 mol) of lithium acetate, 6.1468g (0.025 mol) of manganese acetate and 3.3144g (0.0125 mol) of vanadyl acetylacetonate were dissolved in 100mL of ethanol and the solution was designated as solution 1.
(2) 9.0035g (0.1 mol) of oxalic acid was dissolved in 100mL of ethanol to give a clear solution, which was designated as solution 2.
(3) Stirring for 10min at 70 ℃ by a constant-temperature magnetic stirrer, slowly adding the solution 2 into the solution 1, and recording the mixed solution as 3.
(4) Weighing 4g of P123Adding into the above solution 3, stirring with a magnetic stirrer at a constant temperature of 70 ℃ for 30min, and adding dropwise ammonia water to obtain a solution with pH =7, and recording as solution 4.
(5) And (3) putting the mixed solution 4 into a water bath kettle, keeping the temperature constant at 85 ℃, heating and evaporating the solvent to obtain sol.
(6) And (3) placing the sol in a box furnace, and heating for 12h at the temperature of 200 ℃ to obtain gel.
(7) And drying the gel at 130 ℃ for 5h in vacuum to obtain a precursor.
(8) After grinding, the precursor was calcined in a tube furnace (air atmosphere) at 480 ℃ for 8 h.
(9) Taking out the powder, cooling to room temperature, fully grinding again, carrying out secondary calcination for 12h at 780 ℃, and finally obtaining the anode material Li1.25Mn0.5V0.25O2 。
Example 3
Nano Li1.25Mn0.5V0.25O2The preparation method of the anode material comprises the following specific steps:
(1) 1.6497g (0.025 mol) of lithium acetate, 2.4508g (0.01 mol) of manganese acetate and 1.3258g (0.005 mol) of vanadyl acetylacetonate were dissolved in 100mL of ethanol and designated as solution 1.
(2) 3.6014g (0.04 mol) of oxalic acid was dissolved in 100mL of ethanol to give a clear solution, which was designated as solution 2.
(3) Stirring for 10min at 80 ℃ by a constant-temperature magnetic stirrer, slowly adding the solution 2 into the solution 1, and recording the mixed solution as 3.
(4) Weighing 2g of P123Adding into the above solution 3, stirring with a magnetic stirrer at a constant temperature of 70 ℃ for 30min, and adding dropwise ammonia water to obtain a solution with pH =7, and recording as solution 4.
(5) And (3) putting the mixed solution 4 into a water bath kettle, keeping the temperature constant at 80 ℃, heating and evaporating the solvent to obtain sol.
(6) And (3) putting the sol into a box furnace, and heating for 10 hours at the temperature of 200 ℃ to obtain gel.
(7) And drying the gel at 150 ℃ for 4h in vacuum to obtain a precursor.
(8) After grinding, the precursor was calcined in a tube furnace (air atmosphere) at 530 ℃ for 6 h.
(9) Taking out the powder, cooling to room temperature, and fully cooling againGrinding, and carrying out secondary calcination for 10h at 800 ℃ to finally obtain the anode material Li1.25Mn0.5V0.25O2 。
The above embodiments are merely examples of the present invention, and only have exemplary technical effects and implementations achieved by the present invention. Various alternatives, modifications, and variations are possible to those skilled in the art without departing from the spirit and scope of the invention and the appended claims. Therefore, the present invention should not be limited to the disclosure of the preferred embodiments and the accompanying drawings.
Claims (10)
1. Nano Li1.25Mn0.5V0.25O2The preparation method of the anode material is characterized by comprising the following steps:
(1) dissolving lithium acetate, manganese acetate and vanadyl acetylacetonate in ethanol, and recording as a solution 1;
(2) dissolving oxalic acid in ethanol to form a transparent solution, and marking as a solution 2;
(3) slowly adding the solution 2 into the solution 1 through a constant-temperature magnetic stirrer to obtain a mixed solution 3;
(4) under the action of a constant-temperature magnetic stirrer, P is stirred123Adding the mixed solution into the mixed solution 3, and simultaneously dropwise adding ammonia water to enable the pH of the solution to be =7, so as to obtain a mixed solution 4;
(5) putting the mixed solution 4 into a water bath kettle, heating at constant temperature to evaporate the solvent to obtain sol;
(6) placing the sol in a box type furnace for reheating to obtain gel;
(7) carrying out vacuum drying on the gel to obtain a precursor;
(8) grinding the precursor, and calcining the ground precursor in a tubular furnace in an air atmosphere to obtain powder;
(9) taking out the powder obtained in the step (8), cooling to room temperature, fully grinding again, and carrying out secondary calcination to obtain the nano Li1.25Mn0.5V0.25O2And (3) a positive electrode material.
2. Nano Li according to claim 11.25Mn0.5V0.25O2The preparation method of the anode material is characterized by comprising the following steps: in the step (1), the molar ratio of lithium acetate, manganese acetate and vanadyl acetylacetonate is 5:2: 1.
3. Nano Li according to claim 11.25Mn0.5V0.25O2The preparation method of the anode material is characterized by comprising the following steps: in the step (3), the molar ratio of oxalic acid to metal ions is 1: 1.
4. Nano Li according to claim 11.25Mn0.5V0.25O2The preparation method of the anode material is characterized by comprising the following steps: in the step (3), the constant-temperature magnetic stirring time is 10min, and the temperature is 70-80 ℃.
5. Nano Li according to claim 11.25Mn0.5V0.25O2The preparation method of the anode material is characterized by comprising the following steps: in the step (4), P123The mass of the stirring liquid is (2-4) g, the constant-temperature magnetic stirring time is 20-30 min, and the temperature is 70-80 ℃.
6. Nano Li according to claim 11.25Mn0.5V0.25O2The preparation method of the anode material is characterized by comprising the following steps: in the step (5), the water bath heating temperature is 80-100 ℃.
7. Nano Li according to claim 11.25Mn0.5V0.25O2The preparation method of the anode material is characterized by comprising the following steps: in the step (6), the heating temperature is 180-220 ℃, and the time is 10-14 h.
8. Nano Li according to claim 11.25Mn0.5V0.25O2Preparation method of positive electrode materialThe method is characterized in that: in the step (7), the drying temperature is 100-150 ℃, and the drying time is 4-6 h.
9. Nano Li according to claim 11.25Mn0.5V0.25O2The preparation method of the anode material is characterized by comprising the following steps: in the step (8), the calcining temperature is 480-550 ℃, and the time is 5-8 h.
10. Nano Li according to claim 11.25Mn0.5V0.25O2The preparation method of the anode material is characterized by comprising the following steps: in the step (9), the secondary calcination temperature is 760-900 ℃, and the secondary calcination time is 10-15 h.
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| US20120264018A1 (en) * | 2009-12-16 | 2012-10-18 | Lingyong Kong | Composite positive electrode material with core-shell structure for lithium ion batteries and preparing method thereof |
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