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A method for confinement synthesis of tungsten disulfide@c composite electrode material

A technology of tungsten disulfide and composite electrodes, which is applied in nanotechnology for materials and surface science, battery electrodes, secondary batteries, etc. It can solve the problem of strict temperature and time requirements, great influence on products, and difficulty in controlling morphology and other problems, to achieve the effect of low price, good product dispersibility, and easy control of process parameters

Active Publication Date: 2020-12-01
SHAANXI UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] However, when materials are used to construct nanostructures, their synthesis techniques are often limited: liquid phase conditions are harsh, with stricter requirements on temperature and time, which have a greater impact on the product; solid phase conditions are prone to agglomeration
At the same time, in the composite structure, it is difficult to control the morphology

Method used

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  • A method for confinement synthesis of tungsten disulfide@c composite electrode material
  • A method for confinement synthesis of tungsten disulfide@c composite electrode material
  • A method for confinement synthesis of tungsten disulfide@c composite electrode material

Examples

Experimental program
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Effect test

Embodiment 1

[0031] Step 1: At room temperature, add 0.618g of sodium tungstate dihydrate into 25mL of deionized water and stir until completely dissolved to form solution A. The stirring speed is 600r / min, and the stirring time is 0.1h;

[0032] Step 2: Add 0.168g glucose and 0.0168g PVP to solution A, stir until glucose and PVP are completely dissolved, and control the molar ratio of tungsten source and carbon source to 1:0.5. The stirring speed is 500r / min, and the stirring time is 30min;

[0033]Step 3: Dilute concentrated hydrochloric acid into a 2mol / L transparent solution B, add solution B dropwise to solution A until the pH value of the solution is 1.3, transfer the solution to a 100mL polytetrafluoroethylene reactor for homogeneous reaction, and react The temperature is 180°C, the reaction time is 12h, and it is naturally cooled to room temperature after the reaction;

[0034] Step 4: Open the reaction kettle, take out the product, wash it with absolute ethanol and deionized wate...

Embodiment 2

[0037] Step 1: At room temperature, add 1.28g of sodium tungstate dihydrate into 25mL of deionized water and stir until completely dissolved to form solution A. The stirring speed is 600r / min, and the stirring time is 0.1h;

[0038] Step 2: Add 0.349g glucose and 0.0349g PVP to solution A, stir until glucose and PVP are completely dissolved, and control the molar ratio of tungsten source and carbon source to 1:0.5. The stirring speed is 500r / min, and the stirring time is 30min;

[0039] Step 3: Dilute the concentrated hydrochloric acid into 4mol / L transparent solution B, add solution B dropwise to solution A until the pH value of the solution is about 1.7, transfer the solution to a 100mL polytetrafluoroethylene reactor for homogeneous reaction, The reaction temperature is 150° C., the reaction time is 24 hours, and the reaction is naturally cooled to room temperature after the reaction.

[0040] Step 4: Open the reaction kettle, take out the product, wash it with absolute et...

Embodiment 3

[0043] Step 1: At room temperature, add 0.825g of sodium tungstate dihydrate into 25mL of deionized water and stir until completely dissolved to form solution A. The stirring speed is 600r / min, and the stirring time is 1h;

[0044] Step 2: Add 0.225g glucose and 0.0225g PVP to solution A, stir until glucose and PVP are completely dissolved, and control the molar ratio of tungsten source and carbon source to 1:0.5. The stirring speed is 500r / min, and the stirring time is 30min;

[0045] Step 3: Dilute concentrated hydrochloric acid into a 2mol / L transparent solution B, add solution B dropwise to solution A until the pH value of the solution is 1.5, transfer the solution to a 100mL polytetrafluoroethylene reactor for homogeneous reaction, and react The temperature was 180° C., the reaction time was 12 hours, and the reaction was naturally cooled to room temperature after the reaction.

[0046] Step 4: Open the reaction kettle, take out the product, wash it with absolute ethanol...

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Abstract

The invention relates to a confined synthesis method for a tungsten disulfide@C composite electrode material. The method comprises the following steps: adding sodium tungstate dihydrate into deionizedwater, stirring until the sodium tungstate dihydrate is dissolved and solution A is formed, then adding glucose and PVP, mixing until solution is uniform, regulating a pH value to be 1.3-1.7, performing hydrothermal reaction for 12-24 hours at the temperature of 150-180 DEG C, washing, and drying, so that WO3@C powder is obtained; mixing WO3@C with thiourea, and calcining in an argon atmosphere,so that a WS2@C composite material is obtained. Process equipment for preparing the WS2@C composite material in the invention is simple, product dispersity is good, a hydrothermal process is utilizedfor uniformly compounding WO3 with a glucose carbon material grown in situ, and morphology is controllable; and then low temperature calcining sulfurization is utilized for rapidly preparing the WS2@Ccomposite material. The WS2@C composite material prepared by adopting the method provided by the invention has great research value and application value in the electrochemical field.

Description

technical field [0001] The present invention relates to WS 2 The technical field of nanomaterial preparation relates to a method for confinement synthesis of negative electrode materials using hydrothermal method and low-temperature calcination, and specifically relates to a method for confinement synthesis of tungsten disulfide@C composite electrode materials. Background technique [0002] Transition metal dichalcogenides (TMDs) are one of the anode materials for Na-ion batteries that have been widely studied as advanced energy storage materials, such as WS 2 , Sb 2 S 3 , GeS 2 , VS 2 Wait. At present, according to the reported literature, pure phase WS can be prepared by hydrothermal method, solid phase sintering method, chemical vapor deposition method, etc. 2 Material. But since WS 2 Poor crystallinity, unstable crystal structure, easy amorphization during charging and discharging, resulting in fast material capacity decay, and poor cycle stability make it imposs...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01M4/36H01M4/58H01M4/62H01M10/054B82Y30/00
CPCB82Y30/00H01M4/366H01M4/5815H01M4/625H01M10/054Y02E60/10
Inventor 黄剑锋罗晓敏曹丽云李嘉胤席乔郭玲王泽坤王芳敏
Owner SHAANXI UNIV OF SCI & TECH
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