Preparation method of tungsten diselenide nanosheet

A technology of tungsten diselenide nanometer and tungsten diselenide, which is applied in the direction of binary selenium/tellurium compound, nanotechnology, metal selenide/telluride, etc., which can solve the application limitation of WSe2, unfavorable large-scale industrial production, and reaction atmosphere Require high-level issues to achieve the effect of green raw materials, fewer layers, and low cost

Inactive Publication Date: 2016-07-20
UNIV OF ELECTRONICS SCI & TECH OF CHINA
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  • Description
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Problems solved by technology

This method adopts two-step method, and preparation steps are loaded down with trivial details, and in WO 2 The selenization process also needs to be carried out under the protection of high-purity argon, and the reaction temperature is high, ranging from 600°C to 900°C
[0007] Because with graphite, M O S 2 Unlike natural minerals, WSe 2 It can only be prepared by artificial synthesis. Because the soluble selenium salt used in

Method used

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  • Preparation method of tungsten diselenide nanosheet
  • Preparation method of tungsten diselenide nanosheet
  • Preparation method of tungsten diselenide nanosheet

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Step 1: Dissolve 0.1513g of sodium borohydride in 50ml of N,N-dimethylformamide and mix evenly, add 0.3632g of selenium powder and stir until completely dissolved, then add 0.6597g of sodium tungstate to prepare a mixed solution;

[0028] Step 2: transfer the mixed solution obtained in step 1 to a polytetrafluoroethylene reactor, and react at a temperature of 200° C. for 48 hours;

[0029] Step 3: After the temperature of the reaction kettle in step 2 was naturally cooled to room temperature, the black product was collected by suction filtration, washed with deionized water and ethanol respectively, and freeze-dried for 24 hours to obtain tungsten diselenide nanosheets.

[0030] figure 1 It is the Raman spectrogram of the product after reacting the reactant of Example 1 at 200°C for 48 hours. As can be seen from the figure, at 249cm -1 WSe 2 Obvious Raman characteristic peak E 1 2g .

Embodiment 2

[0032] Step 1: Dissolve 0.1135g of sodium borohydride in 50ml of N,N-dimethylformamide and mix evenly, add 0.3395g of selenium powder and stir until completely dissolved, then add 0.6597g of sodium tungstate to prepare a mixed solution;

[0033] Step 2: transfer the mixed solution obtained in step 1 to a polytetrafluoroethylene reactor, and react at a temperature of 220° C. for 36 hours;

[0034] Step 3: After the temperature of the reaction kettle in step 2 was naturally cooled to room temperature, the black product was collected by suction filtration, washed with deionized water and ethanol respectively, and freeze-dried for 24 hours to obtain tungsten diselenide nanosheets.

[0035] figure 2 In order to implement the X-ray diffraction (XRD) pattern of the product after the reaction of the 2 reactants for 36 hours at 220°C, it can be seen from the figure that the product is a tungsten diselenide nanosheet (WSe) with better crystallization. 2 ), without any impurity.

[0036...

Embodiment 3

[0038] Step 1: Dissolve 0.1135g of sodium borohydride in 80ml of N,N-dimethylformamide and mix evenly, add 0.6317g of selenium powder and stir until completely dissolved, then add 1.3194g of sodium tungstate to prepare a mixed solution;

[0039] Step 2: transfer the mixed solution obtained in step 1 to a polytetrafluoroethylene reactor, and react at a temperature of 240° C. for 24 hours;

[0040] Step 3: After the temperature of the reaction kettle in step 2 was naturally cooled to room temperature, the black product was collected by suction filtration, washed with deionized water and ethanol respectively, and freeze-dried for 24 hours to obtain tungsten diselenide nanosheets.

[0041] Figure 4 It is a transmission electron microscope (TEM) figure of the product after reacting the reactant of Example 3 under the condition of 240° C. for 24 hours. As can be seen from the figure, the product is WSe similar to graphene 2 nanoflakes.

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Abstract

The invention discloses a preparation method of a tungsten diselenide nanosheet, and belongs to the technical field of nanometer material preparation. The preparation method comprises the following steps of dissolving sodium borohydride into an organic solvent, and successively adding selenium powder and sodium tungstate to prepare a mixed solution; transferring the mixed solution to a reaction kettle, and performing reaction for 6 to 48 hours at 200 DEG C to 240 DEG C; after the temperature of the reaction kettle is naturally cooled to the room temperature, collecting black products through suction filtration; washing the product by deionized water and ethyl alcohol; freezing and drying the washed product to obtain the tungsten diselenide nanosheet. The invention provides the method for synthesizing the tungsten diselenide nanosheet in one step by a solvothermal method for the first time. The preparation method has the advantages that the raw materials are green and environment-friendly; the cost is low; the yield is high; the reaction condition is mild; the scale production can be realized. The high-crystallization tungsten diselenide nanosheet prepared by the method has the advantages that the size is great; the layer number is small; the distribution is uniform; the specific surface area is high; high application prospects are realized in the fields of catalysis, energy storage and the like.

Description

technical field [0001] The invention belongs to the technical field of nanomaterial preparation, in particular to a tungsten diselenide (WSe 2 ) Preparation method of nanosheets. Background technique [0002] In recent years, people have mostly studied transition metal sulfides and achieved great results. Judging from the current public literature, the main reason is that sulfur sources are wide and most of them have low toxicity, while water-soluble selenides are toxic. Therefore for transition metal sulfide MS 2 (M=Mo, W, Nb, Ta, Zr, Hf, Re, Pt) There are also many reports on the preparation method and performance research, while involving transition metal selenide MSe 2 (M=Mo, W, Nb, Ta, Zr, Hf, Re, Pt) There are few related studies, especially its morphology control and application research. Therefore, many scholars have turned their attention to transition metal selenides. [0003] Tungsten diselenide (WSe 2 ), as the main transition metal selenide, is a kind of en...

Claims

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Application Information

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IPC IPC(8): C01B19/04B82Y40/00
CPCC01B19/007C01P2002/01C01P2002/72C01P2002/82C01P2004/03C01P2004/04C01P2004/24
Inventor 陈远富王新强戚飞郑斌杰贺加瑞周金浩张万里
Owner UNIV OF ELECTRONICS SCI & TECH OF CHINA
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