Method used for preparing lithium ion battery positive pole material fluophosphate vanadium lithium

A lithium-ion battery, lithium vanadium phosphate technology, applied in the direction of battery electrodes, circuits, electrical components, etc., can solve the problems of uneven distribution of material components, unstable electrochemical performance, harsh control conditions, etc., to achieve excellent electrochemical performance , Excellent electrochemical performance and short synthesis cycle

Active Publication Date: 2012-02-15
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method has harsh control conditions, high energy consumption, high production costs, uneven distribution of components, large particles, and unstable electrochemical properties of the prepared materials.

Method used

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  • Method used for preparing lithium ion battery positive pole material fluophosphate vanadium lithium
  • Method used for preparing lithium ion battery positive pole material fluophosphate vanadium lithium
  • Method used for preparing lithium ion battery positive pole material fluophosphate vanadium lithium

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Using lithium fluoride, vanadium pentoxide and ammonium dihydrogen phosphate as raw materials, press LiVPO 4 According to the stoichiometric ratio of F, add oxalic acid (1.5 times the theoretical amount), mechanically activate for 20 hours until the pentavalent vanadium is completely reduced to trivalent vanadium, and then the resulting powder is stored at 600°C in an argon atmosphere. 650°C, 700°C, 750°C and 800°C for 12 hours to obtain the positive electrode material LiVPO 4 F, the resulting product was assembled into a button battery to measure its charge and discharge capacity and rate performance. Charge and discharge at different rates, the first discharge specific capacity is shown in Table 1.

[0029] Table 1 Experimental conditions and results of Example 1

[0030]

Embodiment 2

[0032] Using lithium carbonate, vanadium trifluoride, ammonium metavanadate and diammonium hydrogen phosphate as raw materials, according to the stoichiometric ratio of LiVPO4F, add ascorbic acid (adding 5 times the theoretical amount), and mechanically activate for 0.5 hours until the pentavalent vanadium is completely It is reduced to trivalent vanadium, and then the resulting powder is kept at 650°C in a nitrogen atmosphere for 0.5, 2, 6, and 12 hours to obtain the positive electrode material LiVPO 4 F, the obtained product was assembled into a button battery to measure its charge and discharge capacity and rate performance, and the charge and discharge were carried out at different rates, and the specific capacity of the first discharge is shown in Table 2.

[0033] Table 2 Experimental conditions and results of Example 2

[0034]

Embodiment 3

[0036] Using lithium hydrogen fluoride, vanadium dioxide and triammonium phosphate as raw materials, press LiVPO 4 According to the stoichiometric proportion of F, add hydrazine hydrate (according to 1 times the theoretical amount), mechanically activate for 6 hours until the pentavalent vanadium is completely reduced to trivalent vanadium, and then the obtained powder is kept at 600°C for 10 hours in a nitrogen atmosphere. Hours, the positive electrode material LiVPO 4 F, the obtained product was assembled into a button battery to measure its charge and discharge capacity and rate performance, and the charge and discharge were carried out at different rates, and the first discharge specific capacity at 0.1C, 0.5C, 2C, 5C and 10C rates was 150.7 respectively mAh·g -1 , 148.5mAh·g -1 , 141.3 mAh·g -1 , 120.3 mAh·g -1 and 101.3 mAh·g -1 .

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Abstract

The invention discloses a method used for preparing lithium ion battery positive pole material fluophosphate vanadium lithium. The method is characterized in that a normal temperature reduction-heat treating method is adopted to prepare a lithium ion battery positive pole material LiVPO4F; the method comprises the following steps: mixing a lithium source, a vanadium source, a fluorine source and a phosphorus source according to the mol ratio of a lithium element, a vanadium element, a fluorine element, and a phosphorus element of 1:1:1:1, adding a reducer, wherein the dosage of the reducer is 1-5 times of that of the theory dosage; carrying out mechanical activation for 0.5-20 hours under the normal temperature condition, and reducing a high-price vanadium to a trivalence vanadium so as to prepare tiny amorphism LiVPO4F of small grains; and heating to 600-800 DEG C in non-oxidizing atmosphere and keeping constant temperature for 0.5-20 hours, thereby obtaining the positive pole material fluophosphate vanadium lithium. The electrochemistry performance of the prepared fluophosphate vanadium lithium is excellent. The fluophosphate vanadium lithium provided by the invention has the advantages of short flow, simple process, lower energy consumption and small production cost, and is easy to realize large scale production and the like.

Description

technical field [0001] The invention belongs to the field of lithium-ion battery materials and preparation methods thereof, and relates to a method for preparing lithium-ion battery cathode material LiVPO 4 F's method. Background technique [0002] Lithium vanadium fluorophosphate (LiVPO 4 F) is a new type of polyanion material, its structure is a PO 4 Tetrahedron and VO 4 f 2 A three-dimensional framework network constructed by octahedra, where PO 4 Tetrahedron and VO 4 f 2 Octahedrons share one oxygen vertex, and VO 4 f 2 The octahedra are connected by fluorine vertices. In this three-dimensional structure, lithium ions occupy two different positions. As the cathode material, LiVPO 4 F has a very high potential platform (4.2V v.s.Li), a theoretical specific capacity of 156mAh / g, good lithium ion transport reversibility, high energy density, good electrochemical performance, high thermal stability and safety performance. J.Barker et al first synthesized LiVPO wit...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/58
CPCY02E60/10
Inventor 王志兴王接喜李新海郭华军彭文杰胡启阳张云河
Owner CENT SOUTH UNIV
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