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Method for preparing anode material doped with LiVPO4F for lithium ion battery

A lithium-ion battery and cathode material technology, applied in battery electrodes, secondary batteries, circuits, etc., can solve problems such as poor cycle stability, achieve the effects of improving conductivity, shortening the process flow, and excellent charge and discharge performance

Active Publication Date: 2017-04-26
HUNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] To achieve the above object, the present invention provides a one-step rapid chemical reduction preparation of doped modified LiVPO 4 The method of F lithium-ion battery positive electrode material, solves LiVPO 4 F material has problems such as poor cycle stability. At the same time, the particle size distribution of the doped sample is uniform and the conductivity is higher, which improves the electrochemical performance of the material, simplifies the production process, and is easier for industrial production.

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  • Method for preparing anode material doped with LiVPO4F for lithium ion battery
  • Method for preparing anode material doped with LiVPO4F for lithium ion battery
  • Method for preparing anode material doped with LiVPO4F for lithium ion battery

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Embodiment 1

[0041]Lithium fluoride, vanadium pentoxide, ammonium dihydrogen phosphate, titanium trifluoride, citric acid, and phenolic resin are used as raw materials (titanium trifluoride is used as the fluorine source and metal compound), and the ingredients are stoichiometrically proportioned. Titanium trifluoride The doping amount is 1%, the molar ratio of citric acid and vanadium is 1:1, and the carbon source accounts for 5% of the total weight. Distilled water is used as a solvent to prepare a solution with a concentration of 0.15mol / l, and it is formed by rapid magnetic stirring at 85°C. After the thick solution was dried in vacuum, the drying temperature was 90°C, and the temperature was kept for 16h. After grinding and sieving, the powder obtained was calcined at 650°C, 700°C, 750°C, 800°C and 850°C for 4h in an argon atmosphere to obtain LiVPO 4 F powder, the resulting sample is assembled into a button cell for electrochemical performance testing. Charge and discharge at differe...

Embodiment 2

[0045] Lithium carbonate, vanadium dioxide, diammonium hydrogen phosphate, lithium fluoride, chromium trifluoride, oxalic acid, sucrose as raw materials, lithium, vanadium, phosphorus, fluorine molar ratio 1:1:1:1, chromium trifluoride The doping amount is 5%; the oxalic acid: vanadium molar ratio is 2:1, the carbon source accounts for 15% of the total proportion, and distilled water is used as a solvent to configure a solution with a concentration of 0.25mol / l, which is formed by rapid magnetic stirring at 50°C. After drying the solution, the drying temperature is 100°C, and the temperature is kept for 10h. After grinding and sieving, the powder obtained is calcined at 800°C for 2, 4, 6, 10, 14h in an argon atmosphere to obtain LiVPO 4 F powder, the resulting sample is assembled into a button cell for electrochemical performance testing. Charge and discharge at different rates, the specific capacity of the first charge and discharge is shown in Table 2.

[0046] Experimental...

Embodiment 3

[0049] Lithium acetate, ammonium metavanadate, triammonium phosphate, ammonium trifluoride, aluminum fluoride, malic acid, and polyvinylidene fluoride are used as raw materials, and the molar ratio of lithium, vanadium, phosphorus, and fluorine is 1:1:1:1 , the doping amount of aluminum fluoride is 1%, 2%, 3%, 4%, 5% respectively, malic acid: vanadium molar ratio is 1.5:1, carbon source accounts for 10% of total proportion, is configured with distilled water as solvent A solution with a concentration of 0.2 mol / l is stirred rapidly at 90°C to form a viscous solution, then vacuum-dried at a drying temperature of 95°C and kept for 12 hours. After grinding and sieving, the powder obtained is calcined at 800°C for 4 hours in an argon atmosphere. Get LiVPO 4 F powder, the resulting sample is assembled into a button cell for electrochemical performance testing. Charge and discharge at different rates, the specific capacity of the first charge and discharge is shown in Table 3 and ...

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Abstract

The invention discloses a method for preparing an anode material doped with LiVPO4F for a lithium ion battery. The method comprises the following steps: weighing a lithium source, a vanadium source, a phosphorus source, a fluorine source, doping elements and a reducing agent according to a certain stoichiometric ratio, quickly and completely reducing V5 + into to V3 + to form a green porous material, performing grinding and sieving, placing the material in a vacuum tube furnace, heating the material to 650-850 DEG C in an inert atmosphere, performing heat preservation for 2-14 h, and performing natural cooling to obtain a modified LiVPO4F composite material. The problems of poor circulatory stability of the LiVPO4F material and the like are solved, meanwhile the particle size distribution of the sample is uniform after being doped, the electrical conductivity is higher, the electrochemical performance of the material is improved, the production process is simplified, and industrialized production is easy to realize.

Description

technical field [0001] The invention belongs to the technical field of lithium ion battery manufacturing, and relates to the preparation of doped modified LiVPO by one-step rapid chemical reduction 4 F Lithium-ion battery cathode material method. Background technique [0002] Lithium-ion batteries have the advantages of high working voltage, high energy density, small self-discharge rate, no memory effect and good cycle performance, so they have achieved vigorous development and replaced the original nickel in many industries. Cadmium, lead acid and nickel metal hydride batteries. [0003] Lithium vanadium fluorophosphate (LiVPO 4 F) is a new type of polyanion cathode material, and LiAlPO 4 F and LiFePO 4 Natural minerals such as OH have the same crystal structure, which belongs to the triclinic system, and its interior is composed of [PO 4 ] tetrahedra and [VO 4 f 2 ] A three-dimensional structure composed of octahedrons, in which lithium ions occupy two different po...

Claims

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Application Information

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IPC IPC(8): H01M4/36H01M4/58H01M4/62H01M10/0525
CPCH01M4/362H01M4/5825H01M4/62H01M10/0525Y02E60/10
Inventor 范长岭曾滔滔文政李奇愿韩绍昌
Owner HUNAN UNIV
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