Solvothermal method for preparing three-dimensional nanometer layered structure WS2 and electrochemical application thereof

A layered structure, three-dimensional nanotechnology, applied in inorganic chemistry, nanotechnology, structural parts, etc., can solve the problems of ultra-high temperature hydrothermal danger, high reaction energy consumption, harsh conditions, etc., to achieve uniform morphology and no phase. Impurities, effects of mild reaction conditions

Active Publication Date: 2015-08-12
SOUTHWEST UNIVERSITY
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The CVD method uses chemical vapor deposition equipment, which has high cost, harsh conditions and low yield; both chemical stripping and physical stripping methods require the preparation of commercial WS 2 The sample is subjected to long-term low-power ultrasonic treatment, which has low efficiency and extremely low yield; while in the solid-phase method, the tungsten source and the sulfur source are placed in an inert environment for a high temperature and long-term reaction to obtain flake WS 2 , but the reaction has high energy consumption and may have sulfur vapor and SO 2 gas generation; in addition, hydrothermal methods typically use tungsten hexachloride (WCl 6 ) and thioacetamide (TAA), the reaction temperature is usually 265 ° C, the reaction time is 24h or even longer, the reaction process has SO 2 Generated, and ultra-high temperature water heat has a certain risk

Method used

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  • Solvothermal method for preparing three-dimensional nanometer layered structure WS2 and electrochemical application thereof
  • Solvothermal method for preparing three-dimensional nanometer layered structure WS2 and electrochemical application thereof
  • Solvothermal method for preparing three-dimensional nanometer layered structure WS2 and electrochemical application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Example 1 Preparation of three-dimensional nano-layered structure WS 2

[0030] The three-dimensional nanolayer structure prepared by solvothermal synthesis is as follows:

[0031] (1) Weigh 125mg of tungstic acid and 70mg of S powder and disperse in the mixed solution of octylamine and n-hexanol, stir vigorously at room temperature for 30min, and the mixing ratio of octylamine and n-hexanol is 7:1;

[0032] (2) Transfer the above solution into the liner of a polytetrafluoroethylene reactor, put it into a stainless steel shell, tighten it, and react in a constant temperature oven at 200°C for 24 hours;

[0033] (3) After cooling to room temperature, the product was collected by filtration, washed three times with ethanol and deionized water, and the obtained powder was vacuum-dried at 80°C for 12 hours;

[0034] (4) The dried samples were heat-treated at 400°C and 750°C for 2 hours in a nitrogen atmosphere, and cooled to obtain a three-dimensional nano-layered structu...

Embodiment 2 3

[0037] Example 2 Three-dimensional nano-layered structure WS 2 Applied to Li-ion battery and performance testing

[0038] Li-ion battery assembly and performance testing:

[0039] (1) Positive electrode preparation: The resulting product is mixed with conductive acetylene black and binder PVDF (polyvinylidene fluoride) in a mass ratio (70:20:10), and a certain amount of 1-methyl-2-pyrrolidone ( NMP), fully ground into a paste, evenly spread it on a copper foil with a diameter of 14 mm and a thickness of about 9 μm, then vacuum-dry at 120 ° C for 12 hours, after cooling, take it out for use;

[0040] (2) Battery assembly: Transfer the electrode sheet from the previous step to a glove box filled with argon gas, use a CR2025 button battery case, a metal lithium sheet with a diameter of 16mm as the negative electrode of the counter electrode, and a Celgard 2325 polypropylene film as a diaphragm, dissolve the 1mol / LLiPF 6 A mixture of ethylene carbonate (EC) and diethyl carbonat...

Embodiment 3

[0044] Example 3 Three-dimensional nano-layered structure WS 2 Application in electrocatalytic hydrogen evolution reaction

[0045] Electrode preparation and performance test for electrocatalytic hydrogen evolution reaction:

[0046] (1) Electrode preparation: take 1 mg of WS obtained in Example 1 2 The product, 0.5mg conductive carbon black, and 5ug Nafion aqueous solution (5wt%) are dispersed in 0.2ml water and ethanol mixture (volume ratio 1:1), and ultrasonicated for at least 30min until dispersed into a homogeneous solution. Then, 5 μg of the above solution was dropped on a glassy carbon electrode with a diameter of 3 mm, and dried in the air for measurement.

[0047] Hydrogen evolution reaction test: the polarization curve was carried out on the electrochemical workstation (CHI) test system using a three-electrode system. Step (1) prepare electrode, saturated calomel electrode and platinum wire as working electrode, reference electrode and counter electrode respective...

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Abstract

The invention relates to a solvothermal method for preparing a three-dimensional nanometer layered structure WS2 and an electrochemical application thereof. The method comprises the following steps: adding tungstic acid and S powder into a mixed solution of octylamine and n-hexyl alcohol, and rapidly stirring at room temperature, so that the components are fully mixed; transferring the fully stirred mixed solution into a hydro-thermal synthesis reactor, reacting under the constant temperature of 180-240 DEG C for 24 hours, filtering and collecting the reaction solution after the reaction solution is cooled to room temperature, cleaning by using ethanol and deionized water, drying, and performing heat treatment on the obtained solid products in a nitrogen atmosphere under the condition of 400-750 DEG C for 2 hours, thereby obtaining the three-dimensional nanometer layered structure WS2. The three-dimensional nanometer layered structure WS2 is applied to lithium ion battery and electro-catalysis hydrogen evolution reaction, good electrochemical performance can be obtained under the condition that mixing and coating are absent, and when the current density is 20mA/g, the discharge capacity of the lithium battery is 468mAh/g; and moreover, a hydrogen evolution initial potential more correct than WS2 in the prior art is obtained under the scanning speed of 10mV/s.

Description

technical field [0001] The invention belongs to the field of new energy materials and their applications, and relates to the preparation of three-dimensional nano-layered structure WS by solvothermal method 2 and its electrochemical applications. Background technique [0002] The inorganic layered material tungsten disulfide has been widely used in solid lubricants or lubricating oil additives due to its special microstructure and composition. In addition, tungsten disulfide also has broad application prospects in catalysts, lithium batteries, hydrogen storage, and electrochemistry. [0003] Lithium-ion batteries are a new generation of chemical power sources. Compared with traditional carbon batteries, alkaline batteries and lead-acid batteries, lithium-ion batteries have obvious advantages, such as high voltage, high specific energy, low self-discharge rate, cycle performance so wait. Moreover, as the best mobile energy storage device in the consumer electronics market ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G41/00H01M4/136C25B11/06B82Y40/00
CPCY02E60/10
Inventor 徐茂文刘三贵于亚楠
Owner SOUTHWEST UNIVERSITY
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