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Preparation method of nitrogen and sulfur co-doped tungsten disulfide sodium ion battery negative electrode material

A sodium-ion battery, tungsten disulfide technology, applied in battery electrodes, circuits, electrical components, etc., can solve the problems of poor structural stability, large volume expansion, poor conductivity, etc., to achieve reaction temperature control, easy reaction temperature, and operation process. simple effect

Active Publication Date: 2019-03-08
SHAANXI UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Tungsten disulfide is a good electrode material due to its unique layered structure and large interlayer spacing, which is conducive to the deintercalation of ions during the electrochemical charge and discharge process of the battery. There is a large volume expansion in the material, resulting in poor structural stability of the material
However, the tungsten disulfide material still has the problem of poor electrical conductivity. Doping can often solve this problem. The introduction of defects in the material effectively improves the active sites in contact with the electrolyte and controls the number of carriers to improve the material. The electrical conductivity, thereby accelerating the transport of electrons and improving the electrochemical performance of the material

Method used

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  • Preparation method of nitrogen and sulfur co-doped tungsten disulfide sodium ion battery negative electrode material
  • Preparation method of nitrogen and sulfur co-doped tungsten disulfide sodium ion battery negative electrode material
  • Preparation method of nitrogen and sulfur co-doped tungsten disulfide sodium ion battery negative electrode material

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Step 1: Add 0.2975g of tungsten hexachloride into 30mL of ethanol solution and magnetically stir until completely dissolved to form a yellow clear solution A. The stirring speed is 700r / min, and the stirring time is 8min. Control solution concentration is 0.025mol / L;

[0027] Step 2: in solution A, add 0.5625g thioacetamide, control molar ratio n( WCl6 ):n(CH 3 CSNH 2 )=10:1, add melamine and thiocyanate again, control mass ratio m( WCl6 ):m(C 3 h 6 N 6 ):m(C 3 h 3 N 3 S 3 )=10:1:1, stirred for 0.5h to form a uniform mixed solution;

[0028] Step 3: Transfer the above solution to a 100mL polytetrafluoroethylene reactor for homogeneous reaction, the reaction temperature is 200°C, the reaction time is 12h, and naturally cool to room temperature after the reaction.

[0029] Step 4: Open the reaction kettle, take out the product, wash it with absolute ethanol and deionized water in turn, and centrifuge it, repeat the washing 4 times, and dry it in a freeze dryer ...

Embodiment 2

[0032] Step 1: Add 0.595g of tungsten hexachloride into 40mL of ethanol solution and magnetically stir until completely dissolved to form a yellow clear solution A. The stirring speed is 800r / min, and the stirring time is 5min. Control solution concentration is 0.0375mol / L;

[0033] Step 2: in solution A, add 1.127g thioacetamide, control molar ratio n ( WCl6 ):n(CH 3 CSNH 2 )=10:1, add melamine and thiocyanate again, control mass ratio m( WCl6 ):m(C 3 h 6 N 6 ):m(C 3 h 3 N 3 S 3 )=7:0.5:1, stirred for 1.5h to form a uniform mixed solution;

[0034] Step 3: Transfer the above solution to a 100mL polytetrafluoroethylene reactor for homogeneous reaction. The reaction temperature is 210° C., and the reaction time is 4 hours. After the reaction is completed, it is naturally cooled to room temperature.

[0035] Step 4: Open the reaction kettle, take out the product, wash it with absolute ethanol and deionized water in turn, and centrifuge it, repeat the washing 6 times, ...

Embodiment 3

[0038] Step 1: Add 1.19g of tungsten hexachloride into 60mL of ethanol solution and magnetically stir until completely dissolved to form a yellow clear solution A. The stirring speed is 700r / min and the stirring time is 8min. Control solution concentration is 0.05mol / L;

[0039] Step 2: in solution A, add 2.25g thioacetamide, control molar ratio n( WCl6 ):n(CH 3 CSNH 2 )=10:1, add melamine and thiocyanate again, control mass ratio m( WCl6 ):m(C 3 h 6 N 6 ):m(C 3 h 3 N 3 S 3 )=9:2:1, stirred for 3h to form a uniform mixed solution;

[0040] Step 3: Transfer the above solution to a 100mL polytetrafluoroethylene reactor for homogeneous reaction. The reaction temperature is 200°C and the reaction time is 24h. After the reaction is completed, it is naturally cooled to room temperature.

[0041] Step 4: Open the reaction kettle, take out the product, wash it with absolute ethanol and deionized water in turn, and centrifuge it. After repeated washing for 5 times, put it in...

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Abstract

A preparation method of a nitrogen and sulfur co-doped tungsten disulfide sodium ion battery negative electrode material comprises the steps of adding tungsten hexachloride into ethyl alcohol for magnetic stirring until the tungsten hexachloride is completely dissolved to form a clear solution, adding thioacetamide, melamine and trithiocyanuric acid, and performing homogeneous reaction for 4-48 hours at 200-240 DEG C to obtain black powder; and performing calcination on the black powder under protection of an argon atmosphere to obtain the nitrogen and sulfur co-doped tungsten disulfide sodiumion battery negative electrode material. The tungsten hexachloride, the thioacetamide and a carbon fabric are used as raw materials, and the nitrogen and sulfur co-doped WS2 electrdoe material is successfully prepared by methods such as assisted solvent thermal and thermal treatment of the melamine and the trithiocyanuric acid. The preparation method is simple in operation process, and the reaction temperature is also easy to control. More active sites are provided for the electrode materials by nitrogen and sulfur co-doping, ion and electron transmission is facilitated, so that the electrochemical performance of the battery is improved.

Description

technical field [0001] The present invention relates to WS 2 The technical field of nanomaterial preparation, in particular to a preparation method of nitrogen and sulfur co-doped tungsten disulfide sodium ion battery negative electrode material. Background technique [0002] WS 2 Because of the unique two-dimensional nanostructure of nanomaterials, conventional sheet-like tungsten disulfide crystals are composed of unit layers composed of S=W=S. In the unit layer, each W atom is combined with two S by strong covalent bonds. The atoms in the crystal are arranged to form a network planar structure, and the planes are combined by weak van der Waals force. Insoluble in acids, alkalis, alcohols, has certain reducing properties, and can react with strong oxidizing substances such as aqua regia, nitric acid and hot concentrated sulfuric acid. At the same time, it has high specific surface area, surface effect, quantum size effect and small size effect, and is widely used in man...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/36H01M4/38H01M4/58
CPCH01M4/364H01M4/38H01M4/5815Y02E60/10
Inventor 黄剑锋罗晓敏曹丽云李嘉胤王蓉徐培光王泽坤王芳敏
Owner SHAANXI UNIV OF SCI & TECH
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