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Method for preparing W-doped Li3V2(PO4)3 powder

A powder and conditional technology, applied in chemical instruments and methods, phosphorus compounds, inorganic chemistry, etc., can solve the problems of poor high-current discharge performance and low conductivity, and achieve good crystal phase development, high purity, and high efficiency. Effect

Inactive Publication Date: 2013-12-11
SHAANXI UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, Li 3 V 2 (PO 4 ) 3 The disadvantage is that the electronic conductivity is relatively low, and the high-current discharge performance is poor, so it needs to be carbon-coated or doped to improve the conductivity so that it can reach a practical level.

Method used

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  • Method for preparing W-doped Li3V2(PO4)3 powder
  • Method for preparing W-doped Li3V2(PO4)3 powder
  • Method for preparing W-doped Li3V2(PO4)3 powder

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] A preparation of W-doped Li 3 V 2 (PO 4 ) 3 The method of powder, comprises the steps:

[0020] Step 1: Add NH 4 VO 3 Dissolve in deionized water, heat and stir to dissolve, the concentration is 0.03mol / L;

[0021] Step 2: To NH 4 VO 3 Add (NH 4 ) 10 W 12 o 41 , LiOH·H 2 O, citric acid and H 3 PO 4 , under stirring conditions, all the raw materials were dissolved in turn, and mixed evenly, LiOH·H in the solution 2 O, NH 4 VO 3 , (NH 4 ) 10 W 12 o 41 、H 3 PO 4 The molar ratio with citric acid is 3:1.95:(0.05 / 12):3:1.5;

[0022] Step 3: Put the beaker containing the above mixed solution into a water bath at 80°C, and stir for 10 hours to obtain a dark blue gel;

[0023] Step 4: Put the dark blue gel-like product in an oven at 90°C, dry it completely and grind it into powder;

[0024] Step 5: Put the obtained powder in N 2 Calcined at 700 °C for 12 h under protected conditions to obtain W-doped Li 3 V 2 (PO 4 ) 3 Powder——Li 3 V 1.95 W 0.05 ...

Embodiment 2

[0029] A preparation of W-doped Li 3 V 2 (PO 4 ) 3 The method of powder, comprises the steps:

[0030] Step 1: Add NH 4 VO 3 Dissolve in deionized water, heat and stir to dissolve, and its concentration is 0.08mol / L;

[0031] Step 2: To NH 4 VO 3 Add (NH 4 ) 10 W 12 o 41 , LiOH·H 2 O, citric acid and H 3 PO 4 , under stirring conditions, all the raw materials were dissolved in turn, and mixed evenly, LiOH·H in the solution 2 O, NH 4 VO 3 , (NH 4 ) 10 W 12 o 41 、H 3 PO 4 The molar ratio with citric acid is 3:1.85:(0.15 / 12):3:1.5;

[0032] Step 3: Put the beaker containing the above mixed solution into a water bath at 90°C, and stir for 15 hours to obtain a dark blue gel;

[0033] Step 4: Put the dark blue gel-like product in an oven at 90°C, dry it completely and grind it into powder;

[0034] Step 5: Put the obtained powder in N 2 Calcined at 850 °C for 4 h under protected conditions to obtain W-doped Li 3 V 2 (PO 4 ) 3 Powder——Li 3 V 1.85 W 0....

Embodiment 3

[0036] A preparation of W-doped Li 3 V 2 (PO 4 ) 3 The method of powder, comprises the steps:

[0037] Step 1: Add NH 4 VO 3 Dissolve in deionized water, heat and stir to dissolve, the concentration is 0.06mol / L;

[0038] Step 2: To NH 4 VO 3 Add (NH 4 ) 10 W 12 o 41 , LiOH·H 2 O, citric acid and H 3 PO 4 , under stirring conditions, all the raw materials were dissolved in turn, and mixed evenly, LiOH·H in the solution 2 O, NH 4 VO 3 , (NH 4 ) 10 W 12 o 41 、H 3 PO 4 The molar ratio to citric acid is 3:1.99:(0.01 / 12):3:1.5;

[0039] Step 3: Put the beaker containing the above mixed solution into a water bath at 85°C, and stir for 12 hours to obtain a dark blue gel;

[0040] Step 4: Put the dark blue gel-like product in an oven at 90°C, dry it completely and grind it into powder;

[0041] Step 5: Put the obtained powder in N 2 Calcined at 800 °C for 8 h under protected conditions to obtain W-doped Li 3 V 2 (PO 4 ) 3 Powder——Li 3 V 1.99 W 0.01 (PO...

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PUM

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Abstract

The invention relates to a method for preparing W-doped Li3V2(PO4)3 powder, which comprises the steps that NH4VO3 is dissolved in deionized water; (NH4)10W12O41, LiOH.H2O, citric acid and H3PO4 are sequentially added to an NH4VO3 solution; all raw materials are sequentially dissolved and uniformly mixed by stirring, wherein a molar ratio of LiOH.H2O to NH4VO3 to (NH4)10W12O41 to H3PO4 to citric acid in the solution is 3:(2-x):(x / 12):3:1.5, and x is equal to 0.01-0.15; a beaker containing the mixed solution is placed in a water bath kettle at 80-90 DEG C; after the mixed solution is stirred for 10-15h, mazarine gel is formed; a mazarine gel-shaped product is dried, and ground into the powder; the powder is calcined under the condition of N2 protection; and the W-doped Li3V2(PO4)3 powder is formed. With the adoption of a sol-gel method, W-doped Li3V2(PO4)3 is formed; the method is simple in technology and high in efficiency; a crystal phase of the power grows well; the purity is high; W3<+> ions are doped in an Li3V2(PO4)3 lattice, and uniformly distributed in the Li3V2(PO4)3 powder; and obtained powder particles are fine and uniform.

Description

technical field [0001] The invention belongs to the technical field of functional materials, in particular to a method for preparing W-doped Li 3 V 2 (PO 4 ) 3 powder method. Background technique [0002] Lithium-ion batteries have become one of the ideal clean energy sources due to their high specific capacity, small self-discharge, long cycle life, light weight, and environmental friendliness, and are important candidate power sources for electric vehicles and hybrid electric vehicles. High energy density, high voltage, high rate and high safety are important conditions for lithium-ion batteries to become the power source of electric vehicles and hybrid electric vehicles. The positive electrode material based on phosphate polyanion is known as the third generation lithium ion battery positive electrode material after metal sulfide and metal oxide. In recent years, with the research and development of large-capacity and high-power lithium-ion batteries, the development...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/45H01M4/58
CPCY02E60/12Y02E60/10
Inventor 夏傲谈国强
Owner SHAANXI UNIV OF SCI & TECH
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