Preparation method of tungsten disulfide/CFC@C multiphase 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 problems of inability to prevent direct contact of tungsten disulfide, poor cycle stability, fast capacity decay, etc. problems, to achieve the effect of facilitating the transmission of electrons, reducing the cost of raw materials, and alleviating side reactions

Active Publication Date: 2019-02-05
SHAANXI UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] Commonly used preparation methods include: hydrothermal method, Jing Ren et al. reported that sodium tungstate dihydrate was selected as the tungsten source, and thiourea was used as the sulfur source to synthesize WS in one step. 2 and their composite products (Ren J, Wang Z, Yang F, et al. Freestanding 3D single-wall carbon nanotubes / WS 2 , nanosheets foams asultra-long-life anodes for rechargeable lithium ion batteries[J].ElectrochimicaActa,2018.), but its synthesis temperature is higher, at 250℃
Due to the large volume expansion of tungsten disulfide in the process of charging and discharging, its capacity decays quickly and its cycle stability is poor. At present, a kind of method to solve the collective expansion is to compound it with a high-conductivity carbon material to alleviate its infiltration. Structural damage caused by volume expansion to improve capacity drop
However, this combination often cannot prevent the direct contact of tungsten disulfide with the electrolyte during the charge and discharge process, resulting in side reactions

Method used

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  • Preparation method of tungsten disulfide/CFC@C multiphase composite electrode material
  • Preparation method of tungsten disulfide/CFC@C multiphase composite electrode material
  • Preparation method of tungsten disulfide/CFC@C multiphase composite electrode material

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Experimental program
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Effect test

Embodiment 1

[0035] Step 1: Cut the carbon cloth (CFC) into a square with a size of 3cm×3cm, soak it in concentrated nitric acid solution for 1 hour for activation treatment, rinse the activated carbon cloth with deionized water and ethanol repeatedly until it becomes neutral, Dry in an oven at 60°C for 8 hours for later use;

[0036] Step 2: 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 600r / min and the stirring time is 10min. Control solution concentration is 0.025mol / L;

[0037] Step 3: add thioacetamide in solution A, control molar ratio n(WCl6):n(CH 3 CSNH 2 )=10:1, stirred for 2h to form a uniform mixed solution;

[0038] Step 4: Put the activated carbon cloth into the above solution, put it into an ultrasonic cleaner with a power of 500W, and shake it for 8 minutes;

[0039]Step 5: Transfer the above solution and carbon cloth to a 100mL polytetrafluoroet...

Embodiment 2

[0045] Step 1: Cut the carbon cloth (CFC) into a 3cm×3cm square, soak it in concentrated nitric acid solution for 3 hours for activation treatment, and rinse the activated carbon cloth with deionized water and absolute ethanol repeatedly until neutral , placed in a 60°C oven to dry for 8 hours for later use;

[0046] Step 2: Add 0.5625g of tungsten hexachloride into 45mL of ethanol solution and magnetically stir until completely dissolved to form a yellow clear solution A. The stirring speed is 600r / min, and the stirring time is 10min. Control solution concentration is 0.0315mol / L;

[0047] Step 3: add thioacetamide in solution A, control molar ratio n(WCl6):n(CH 3 CSNH 2 )=4:1, stirred for 2h to form a uniform mixed solution;

[0048] Step 4: Put the activated carbon cloth into the above solution, put it into an ultrasonic cleaner with a power of 500W, and shake it for 8 minutes;

[0049] Step 5: Transfer the above solution and carbon cloth to a 100mL polytetrafluoroethyl...

Embodiment 3

[0055] Step 1: Cut the carbon cloth (CFC) into a 3cm×3cm square, soak it in concentrated nitric acid solution for 0.5h for activation treatment, and rinse the activated carbon cloth with deionized water and absolute ethanol repeatedly until neutral Afterwards, put into the oven of 60 ℃ and dry for 8 hours for subsequent use;

[0056] Step 2: Add 1.386g of tungsten hexachloride into 50mL of ethanol solution and magnetically stir until completely dissolved to form a yellow clear solution A. The stirring speed is 600r / min and the stirring time is 10min. Control solution concentration is 0.07mol / L;

[0057] Step 3: add thioacetamide in solution A, control molar ratio n(WCl6):n(CH 3 CSNH 2 )=9:2, stirred for 2h to form a uniform mixed solution;

[0058] Step 4: Put the activated carbon cloth into the above solution, put it into an ultrasonic cleaner with a power of 500W, and shake it for 8 minutes;

[0059] Step 5: Transfer the above solution and carbon cloth to a 100mL polytet...

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Abstract

The invention relates to a preparation method of a tungsten disulfide/CFC@C multiphase composite electrode material. The preparation method comprises the steps of adding tungsten hexachloride in alcohol, mixing uniformly and then adding thioacetamide, so as to obtain a mixed solution, soaking activated carbon cloth in the mixed solution, performing homogenous reaction so as to obtain a WS2/CFC composite material; adding maltose and PVP to deionized water, mixing uniformly, so as to obtain a transparent solution; putting the WS2/CFC composite material in the transparent solution, performing ultrasonic reaction and then homogeneous reaction, so as to obtain the tungsten disulfide/CFC@C multiphase composite electrode material. According to the preparation method disclosed by the invention, the tungsten disulfide is grown on a carbon cloth substrate and then is wrapped, so that the tungsten disulfide as sodium ion battery anode material does not expand in charging and discharging and is more stable in structure, and electrochemical stability of batteries is improved. Through adoption of the preparation method, the multiphase composite material is prepared through a hydrothermal method;the process is simple; the cost of raw materials is low; the reaction temperature is easy to control; the reaction time is short.

Description

technical field [0001] The present invention relates to WS 2 The technical field of nanomaterial preparation, in particular to a method for preparing a tungsten disulfide / CFC@C multiphase composite electrode material. Background technique [0002] Transition metal dichalcogenides, especially group VI transition metal sulfides of W, are hot materials in recent academic research due to their two-dimensional ordered layered structure and unique physical and chemical functional properties. Its structure is similar to that of graphene, where transition metal chalcogenides are held together by strong inner-layer covalent M–S bonds and weaker van der Waals interlayer interactions. Its anisotropic layered structure has excellent optical, electronic and mechanical properties, so it is widely used in biomedicine, energy storage, mechanical lubrication, catalysis, sensors, optoelectronic devices and other fields. [0003] Commonly used preparation methods include: hydrothermal method...

Claims

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Application Information

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Patent Type & Authority Applications(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王蓉徐培光席乔王芳敏
Owner SHAANXI UNIV OF SCI & TECH
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