Preparation method of precursor of lithium iron phosphate-lithium vanadium phosphate composite

A technology of lithium vanadium phosphate and composite materials, which is applied in the direction of phosphorus compounds, iron compounds, chemical instruments and methods, etc., can solve the problems such as the electronic conductivity of lithium iron phosphate-lithium vanadium phosphate composite cathode materials needs to be improved, and achieve low cost, The process is simple and the product quality is good

Active Publication Date: 2014-06-04
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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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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  • Preparation method of precursor of lithium iron phosphate-lithium vanadium phosphate composite
  • Preparation method of precursor of lithium iron phosphate-lithium vanadium phosphate composite
  • Preparation method of precursor of lithium iron phosphate-lithium vanadium phosphate composite

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Embodiment 1

[0018] This embodiment includes the following steps:

[0019] (1) 85.5g of graphene oxide suspension with a mass fraction of 2% was placed in a 5L stirred reaction kettle with an ultrasonic device, and ultrasonically treated for 0.5h under the condition of 30KHz;

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

[0021] (3) Add 3.0g polyaniline to refine the particle size of iron vanadate particles, then stir at 200rpm for 0.5h, age for 3h, filter, wash, and blow dry at 100°C for 5h to o...

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 stirring reaction kettle with an ultrasonic device, and ultrasonically treated for 0.2h under the condition of 20KHz;

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

[0030] (3) 3.5g of polyaniline was added, then stirred at 200rpm for 0.5h, aged for 2h, filtered, washed, and freeze-dried at -50°C for 20h to obtain 30.36g of lithium iron p...

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 stirring reaction kettle with an ultrasonic device, and ultrasonically treated at 40KHz for 2h;

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

[0037] (3) 3.8g of polyaniline was added, then stirred at 200rpm for 0.5h, aged for 4h, filtered, washed, and dried at 90°C and -0.1MPa for 8h to obtain 45.34g of lithium iron phosphate-lithium vanadium phos...

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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 lithium iron phosphate-lithium vanadium phosphate composite material precursor. Background technique [0002] Existing cathode materials for lithium-ion batteries mainly include lithium cobalt oxide, lithium manganate, nickel-cobalt-manganese ternary system and lithium iron phosphate. Among them, lithium cobalt oxide, nickel-cobalt-manganese ternary system and lithium iron phosphate are the 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 spinel-type lithium manganate has a very low specific capacity, and the structural stability at high temperature needs to be strengthened. Lithium nickel cobalt manganate will decompose to produce oxygen when exposed to high temperature, which is unsafe. At the same time, Ni and Co are s...

Claims

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Application Information

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IPC IPC(8): C01G49/00C01B25/45
CPCY02E60/10
Inventor 张佳峰张宝李晖郑俊超王小玮袁新波
Owner CENT SOUTH UNIV
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