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Preparation method for WS2-in situ biological carbon composite anode material

A negative electrode material and bio-carbon technology, which is applied in the field of preparing high-magnification WS2-in-situ bio-carbon composite materials, can solve the problems of difficult control of material microstructure, difficult control of reactant ratio, and easy powder agglomeration process conditions, etc., to achieve Harmless structure control and composite modification, excellent high-current charge and discharge performance, and simple process equipment

Active Publication Date: 2015-11-11
珠海东杰科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Precipitation reduction method, thermal decomposition method and solid phase vulcanization method all synthesize WS under high temperature atmosphere conditions. 2 , the powder is easy to agglomerate and the process conditions are difficult to control, which is very important for the preparation of WS 2 The utilization rate of the required raw materials is very small; and the sintering or vulcanization reaction of the solid-phase method under reducing atmosphere conditions will also cause the agglomeration of nanocrystals, the grains grow abnormally, and the microstructure of the material is difficult to control
At the same time, the in-situ evaporation method and chemical vapor deposition method require high equipment and the ratio of reactants is difficult to control. In addition, the prepared WS 2 It is easy to introduce impurities into nanomaterials, and the powder is easy to agglomerate

Method used

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  • Preparation method for WS2-in situ biological carbon composite anode material
  • Preparation method for WS2-in situ biological carbon composite anode material
  • Preparation method for WS2-in situ biological carbon composite anode material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Step 1: Add analytically pure sodium tungstate dihydrate (Na 2 WO 4 ·2H 2 O) and thiourea (CH 4 N 2 S) Add deionized water to control the ratio of the amount of tungsten and sulfur to n W : N S =1:3, keep stirring until the sodium tungstate dihydrate and thiourea dissolve, then put them into an ultrasonic cleaner with a power of 300W and ultrasonically vibrate for 60 minutes to make the sodium tungstate dihydrate and thiourea fully dissolved and control the dihydrate in the mixed solution The total concentration of sodium tungstate and thiourea is 0.005mol·L -1 , This mixed solution is marked as solution A;

[0026] Step 2: Add a mixture of analytically pure β-cyclodextrin and commercially available raffinose (produced by Henan Tianrun Biotechnology Co., Ltd., with a purity of 99.3%), β-cyclodextrin and cotton seed to solution A The mass ratio of sugar is m β-cyclodextrin : M Raffinose =1:2, control the total added amount of β-cyclodextrin and raffinose to wt%=5%, and he...

Embodiment 2

[0034] Step 1: Add analytically pure sodium tungstate dihydrate (Na 2 WO 4 ·2H 2 O) and thiourea (CH 4 N 2 S) Add deionized water separately to control the ratio of the amount of tungsten and sulfur to n W : N S =2:1, keep stirring until the sodium tungstate dihydrate and thiourea dissolve, then put them into an ultrasonic cleaner with a power of 1000W and ultrasonically vibrate for 20 minutes, so that the sodium tungstate dihydrate and thiourea are fully dissolved and control the dihydrate in the mixed solution The total concentration of sodium tungstate and thiourea is 0.015mol·L -1 , This mixed solution is marked as solution A;

[0035] Step 2: Add a mixture of analytically pure β-cyclodextrin and commercially available raffinose (produced by Henan Tianrun Biotechnology Co., Ltd., with a purity of 99.3%), β-cyclodextrin and cotton seed to solution A The mass ratio of sugar is m β-cyclodextrin : M Raffinose =5:3, control the total added amount of β-cyclodextrin and raffinose ...

Embodiment 3

[0041] Step 1: Add analytically pure sodium tungstate dihydrate (Na 2 WO 4 ·2H 2 O) and thiourea (CH 4 N 2 S) Add deionized water to control the ratio of the amount of tungsten and sulfur to n W : N S =1:1, keep stirring until the sodium tungstate dihydrate and thiourea dissolve, then put it into an ultrasonic cleaner with a power of 800W and ultrasonically oscillate for 30 minutes to make the sodium tungstate dihydrate and thiourea fully dissolved, and control the dihydrate in the mixed solution The total concentration of sodium tungstate and thiourea is 0.02mol·L -1 , This mixed solution is marked as solution A;

[0042] Step 2: Add a mixture of analytically pure β-cyclodextrin and commercially available raffinose (produced by Henan Tianrun Biotechnology Co., Ltd., with a purity of 99.3%), β-cyclodextrin and cotton seed to solution A The mass ratio of sugar is m β-cyclodextrin : M Raffinose =3:7, control the total added amount of β-cyclodextrin and raffinose to wt%=20%, and h...

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Abstract

The invention provides a preparation method for a WS2-in situ biological carbon composite anode material. The preparation method comprises the following steps of: adding sodium tungstate dihydrate, thiourea, Beta-cyclodextrin and raffinose into deionized water and carrying out ultrasonic oscillation for full dissolving; adjusting pH to be 3-7 by using hydrochloric acid; carrying out ultrasonic oscillation to obtain a suspension liquid; placing the suspension liquid in a high-throughput ultrahigh-pressure microwave digestion device for reaction; and taking out a product, and sequentially washing, freezing and drying the product to obtain the WS2-in situ biological carbon composite anode material. The preparation method is a simple and green method by which the morphology and the constituent of the product can be controlled through controlling the proportion of a precursor solution and the like; compared with the normal hydrothermal method and a solvothermal method, the preparation method has the advantages of high efficiency, rapidness and high nucleation rate; and the prepared WS2-in situ biological carbon composite anode material is high in purity and dispensability, is uniform in size and morphology, and is simultaneously endowed with high rate capability.

Description

Technical field [0001] The invention relates to a method for preparing high-rate WS 2 -Method of in-situ bio-carbon composite material, especially relates to an ultrasonic-assisted microwave hydrothermal method for preparing WS 2 -A method for in-situ biological carbon composite sodium ion battery anode material. Background technique [0002] WS 2 Crystal structure and MoS 2 Similarly, it is also a closely packed hexagonal layered structure. There are strong chemical bonds between tungsten atoms and sulfur atoms, while the interlayer sulfur atoms and sulfur atoms are connected by weak molecular bonds. The bonding force between layers is still van der Waals force, which is similar to MoS 2 Compared to WS 2 The layer spacing is larger and the friction coefficient is lower, between 0.03 and 0.05. [0003] WS 2 It is insoluble in almost all media, including water, oil, alkali and almost all acids. But it is more sensitive to free gaseous fluorine, hot sulfuric acid and hydrofluoric a...

Claims

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Application Information

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IPC IPC(8): H01M4/36H01M4/58H01M4/587B82Y30/00
CPCB82Y30/00H01M4/362H01M4/5815H01M4/587H01M10/0525Y02E60/10
Inventor 黄剑锋王鑫曹丽云李嘉胤程娅伊殷立雄许占位费杰郝巍
Owner 珠海东杰科技有限公司
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