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Three-phase system molybdenum oxide MoO3/Mo4O11/MoO2 nano electrode material and preparation method thereof

A technology of molybdenum oxide and three-phase system, which is applied in the direction of molybdenum oxide/molybdenum hydroxide, battery electrodes, circuits, etc., can solve the problems of nanometer electrode materials that have not been reported, and achieve high yield, environmental friendliness and low cost. Effect

Active Publication Date: 2018-02-27
SHAANXI UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] At present, on the synthesis of three-phase system molybdenum oxide MoO 3 / Mo 4 o 11 / MoO 2 The method of nanometer electrode material has not been reported yet

Method used

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  • Three-phase system molybdenum oxide MoO3/Mo4O11/MoO2 nano electrode material and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] (1) Weigh 1g ammonium molybdate tetrahydrate ((NH 4 ) 6 Mo 7 o 24 4H 2 O), dissolved in a mixed solvent with a volume of 60 ml (volume ratio water: absolute ethanol = 11:1), stirred for 20 min, and then adjusted to pH = 1 with 3mol / L HCl while stirring to obtain a uniform solution A ;

[0030] (2) Pour the stirred solution A into a polytetrafluoroethylene-lined hydrothermal kettle, seal it, and then place it in a homogeneous reactor for solvothermal reaction at a temperature of 150°C for 15 hours;

[0031] (3) After the reaction, the reaction kettle was cooled at room temperature, and the product was alternately washed 6 times with deionized water and organic solvent absolute ethanol, and vacuum-dried to obtain product B;

[0032] (4) Weigh 0.5g of vacuum-dried product B, place it in a porcelain boat and heat-treat it in Ar. The heat-treatment temperature is 450°C, the time is 2h, and the heating rate is 10°C / min to obtain the target product MoO 3 / Mo 4 o 11 / Mo...

Embodiment 2

[0036] (1) Weigh 1g ammonium molybdate tetrahydrate ((NH4 ) 6 Mo 7 o 24 4H 2 O), dissolved in a mixed solvent with a volume of 60 ml (volume ratio water: absolute ethanol = 11:1), stirred for 20 min, and then adjusted to pH = 1 with 12mol / L HCl while stirring to obtain a uniform solution A ;

[0037] (2) Pour the stirred solution A into a polytetrafluoroethylene-lined hydrothermal kettle, seal it, and then place it in a homogeneous reactor for solvothermal reaction at a reaction temperature of 150°C for 24 hours;

[0038] (3) After the reaction, the reaction kettle was cooled at room temperature, and the product was alternately washed 6 times with deionized water and organic solvent absolute ethanol, and vacuum-dried to obtain product B;

[0039] (4) Weigh 0.5g of the vacuum-dried product B, put it in a porcelain boat and heat-treat it in Ar. The heat-treatment temperature is 300°C, the time is 4h, and the heating rate is 10°C / min to obtain the target product MoO 3 / Mo 4...

Embodiment 3

[0041] (1) Weigh 2g ammonium molybdate tetrahydrate ((NH 4 ) 6 Mo 7 o 24 4H 2 O), dissolved in a mixed solvent with a volume of 60 ml (volume ratio water: absolute ethanol = 5:1), stirred for 20 min, and then adjusted to pH = 1 with 3mol / L HCl while stirring to obtain a uniform solution A ;

[0042] (2) Pour the stirred solution A into a polytetrafluoroethylene-lined hydrothermal kettle, seal it, and then place it in a homogeneous reactor for solvothermal reaction at a reaction temperature of 150°C for 6 hours;

[0043] (3) After the reaction, the reaction kettle was cooled at room temperature, and the product was alternately washed 6 times with deionized water and organic solvent acetone, and dried in vacuum to obtain product B;

[0044] (4) Weigh 0.5g of the vacuum-dried product B, put it in a porcelain boat and heat-treat it in Ar. The heat-treatment temperature is 500°C, the time is 2h, and the heating rate is 10°C / min to obtain the target product MoO 3 / Mo 4 o 11 ...

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Abstract

The invention discloses a synthesis method of a three-phase system molybdenum oxide MoO3 / Mo4O11 / MoO2 lithium-ion battery negative electrode material. The synthesis method comprises the following steps: 1) dissolving a molybdenum source into an enough ethanol-water mixed solvent according to a formula amount; sufficiently stirring and regulating the pH (Potential of Hydrogen) to 1 to 5 by utilizinghydrogen acid; 2) carrying out solvothermal reaction on a product, wherein the reaction temperature is 60 DEG C to 150 DEG C and the time is 3h to 24h; 3) after finishing reaction, cooling a product,and washing and drying; 4) carrying out heat treatment on the product for 2h to 4h in an inert atmosphere at 300 DEG C to 500 DEG C, so as to obtain a target product MoO3 / Mo4O11 / MoO2. The invention discloses the MoO3 / Mo4O11 / MoO2 material; MoO2 and Mo4O11 have metal-like conductivity; on the basis, a relatively high theoretical capacity and a unique lamellar structure of the MoO3 also have extremely great advantages.

Description

technical field [0001] The invention belongs to the technical field of battery materials, and relates to a method for preparing a lithium-ion battery negative electrode material, in particular to a three-phase system molybdenum oxide MoO 3 / Mo 4 o 11 / MoO 2 Nano electrode material and its preparation method. Background technique [0002] Lithium-ion batteries have the characteristics of high energy density, high voltage platform, long cycle life, and environmental friendliness, and are widely used in the fields of consumer electronics and power batteries. The current commercial lithium-ion battery system is mainly based on graphite-based carbon anode materials, but its theoretical specific capacity is only 372 mAh g -1 , the development of new anode materials has become a top priority. [0003] Metal molybdenum has a variety of binary oxides, among which the most studied ones are MoO 3 、Mo 4 o 11 、MoO 2 Wait. Because molybdenum oxide has a high theoretical specific...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G39/02H01M4/48H01M10/0525
CPCC01G39/02C01P2002/72C01P2004/82C01P2006/40H01M4/48H01M10/0525Y02E60/10
Inventor 曹丽云贺菊菊李嘉胤黄剑锋齐樱张宁仵婉晨李倩颖
Owner SHAANXI UNIV OF SCI & TECH
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