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A kind of preparation method of lithium iron phosphate-lithium vanadium phosphate composite material precursor

A technology of lithium vanadium phosphate and composite materials, which is applied in the direction of electrical components, battery electrodes, circuits, etc., can solve the problems of lithium iron phosphate-lithium vanadium phosphate composite positive electrode material that the electronic conductivity needs to be improved, and achieve low cost and good product quality , The effect of stable product quality

Active Publication Date: 2015-08-12
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the electronic conductivity of lithium iron phosphate-lithium vanadium phosphate composite cathode materials still needs to be improved.

Method used

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  • A kind of preparation method of lithium iron phosphate-lithium vanadium phosphate composite material precursor
  • A kind of preparation method of lithium iron phosphate-lithium vanadium phosphate composite material precursor
  • A kind of preparation method of lithium iron phosphate-lithium vanadium phosphate composite material precursor

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Experimental program
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Embodiment 1

[0018] This embodiment includes the following steps:

[0019] (1) Put 85.5g of graphene oxide suspension with a mass fraction of 2% in a 5L stirred reactor with an ultrasonic device, and ultrasonically treat it at 30KHz for 0.5h;

[0020] (2) Add 39.9g of ferric sulfate to 1L of deionized water to make a ferric sulfate solution with a concentration of 0.1mol / L, and add 36.8g of sodium orthovanadate to 1L of deionized water to make a solution with a concentration of 0.2mol / L. Sodium vanadate solution; then simultaneously add ferric sulfate solution and sodium orthovanadate solution to the stirring reaction kettle at a speed of 400mL / h, control the stirring speed to 200rpm, adjust the pH to 6 with ammonia water, and react for 1.0h;

[0021] (3) Add 3.0g of polyaniline to refine the particle size of ferric vanadate particles, then stir at 200rpm for 0.5h, age for 3h, filter, wash, and blow dry at 100°C for 5h to obtain 38.4g Precursor Fe of lithium iron phosphate-lithium vanadiu...

Embodiment 2

[0027] This embodiment includes the following steps:

[0028] (1) 136.8g of graphene oxide suspension with a mass fraction of 2% was placed in a 5L stirred reactor with an ultrasonic device, and ultrasonically treated at 20KHz for 0.2h;

[0029] (2) Add 31.99g of ferric sulfate to 1L of deionized water to make a ferric sulfate solution with a concentration of 0.08mol / L, and add 29.44g of sodium orthovanadate to 1L of deionized water to make a solution with a concentration of 0.16mol / L. Sodium vanadate solution; then simultaneously add ferric sulfate solution and sodium orthovanadate solution into the stirred reactor at a speed of 200mL / h, control the stirring speed to 50rpm, adjust the pH to 2 with ammonia water, and react for 1h;

[0030] (3) Add 3.5g of polyaniline, then stir at 200rpm for 0.5h, age for 2h, filter, wash, and freeze-dry at -50°C for 20h to obtain 30.36g of lithium iron phosphate-lithium vanadium phosphate composite material precursor Fe 4 (VO 4 ) 4 · x h...

Embodiment 3

[0034] This embodiment includes the following steps:

[0035] (1) 90.8g of graphene oxide suspension with a mass fraction of 2% was placed in a 5L stirred reactor with an ultrasonic device, and ultrasonically treated at 40KHz for 2h;

[0036] (2) Add 47.98g of ferric sulfate to 1L of deionized water to make a ferric sulfate solution with a concentration of 0.12mol / L, and add 44.16g of sodium orthovanadate to 1L of deionized water to make a solution with a concentration of 0.24mol / L. Sodium vanadate solution; then simultaneously add ferric sulfate solution and sodium orthovanadate solution into the reaction kettle at a rate of 600mL / h, control the stirring speed to 400rpm, adjust the pH to 8 with ammonia water, and react for 4h;

[0037] (3) Add 3.8g of polyaniline, then stir at 200rpm for 0.5h, age for 4h, filter, wash, and dry at 90°C and -0.1MPa for 8h to obtain 45.34g of lithium iron phosphate-lithium vanadium phosphate composite material Precursor Fe 4 (VO 4 ) 4 · x h ...

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Abstract

The invention relates to a preparation method of a precursor of a lithium iron phosphate-lithium vanadium phosphate composite. The preparation method comprises the following steps of (1) placing graphene oxide turbid liquid with the mass percentage of 1-3% into a stirring reaction kettle with an ultrasonic device to carry out ultrasonic treatment for 0.2-2.0h; (2) simultaneously adding 0.08-0.12mol / L ferric sulfate solution and 0.16-0.24mol / L sodium orthovanadate into the stirring reaction kettle at the speed of 200-600mL / h, controlling the stirring speed at 50-400rpm, regulating the pH value of the solution to 2-8 by using ammonium hydroxide, and reacting for 0.5-4.0h; (3) adding polyaniline, stirring, ageing, filtering, cleaning and drying to obtain the precursor. According to the invention, the precursor of the lithium iron phosphate-lithium vanadium phosphate composite, which is synthesized through the in-situ growing of ferric vanadate on graphene oxide, is fine and uniform in particle; the electrochemical properties of the synthesized lithium iron phosphate-lithium vanadium phosphate composite cathode material are excellent.

Description

technical field [0001] The invention relates to a preparation method of a precursor of a lithium iron phosphate-lithium vanadium phosphate composite material. Background technique [0002] The existing lithium-ion battery positive electrode materials mainly include lithium cobaltate, lithium manganate, nickel-cobalt-manganese ternary system and lithium iron phosphate. Among them, lithium cobaltate, nickel-cobalt-manganese ternary system and lithium iron phosphate are mainstream materials, but cobalt is highly toxic, and cobalt resources are seriously scarce and expensive. Although the layered lithium manganate has a specific capacity of 285mAh / g, its structural stability is very poor, while the specific capacity of the spinel lithium manganate is very low, and the structural stability at high temperature needs to be strengthened. Lithium nickel cobalt manganese oxide will decompose and produce oxygen when exposed to high temperature, which poses a hidden danger of safety. A...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01M4/1397
CPCY02E60/10
Inventor 张佳峰张宝李晖郑俊超王小玮袁新波
Owner CENT SOUTH UNIV