Method for preparing tungsten diselenide nanoflower

A technology of tungsten diselenide and nanoflowers, which is applied in the direction of binary selenium/tellurium compounds, metal selenides/tellurides, etc., can solve the problems of high requirements for reaction atmosphere, high reaction temperature, and high preparation temperature, and achieve easy-to-obtain raw materials The effect of low cost, mild reaction conditions and uniform scale distribution

Active Publication Date: 2016-09-28
UNIV OF ELECTRONICS SCI & TECH OF CHINA
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  • Abstract
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  • Claims
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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
[0005] Because with graphite, M O S 2 Unlike natural minerals, WSe 2 It can only be prepared by artificial synthesis. The existing processes generally need to be carried out in CVD tube furnaces. The equipment is expensive, the preparation temperature is high, and the requirements for the reaction atmosphere are high, which is not conducive to large-scale industrial production.
Therefore, WSe 2 The application of the

Method used

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  • Method for preparing tungsten diselenide nanoflower
  • Method for preparing tungsten diselenide nanoflower
  • Method for preparing tungsten diselenide nanoflower

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Step 1: Add 0.3869g H 2 SeO 3 Dissolve in 50ml of N,N-dimethylformamide (DMF), add 0.3299g Na while stirring 2 WO 4 2H 2 After O, a mixed solution is obtained;

[0023] Step 2: Transfer the mixed solution in step 1 to a 100ml polytetrafluoroethylene reactor, and react at a temperature of 200°C for 48 hours;

[0024] Step 3: after the temperature in the reaction kettle of step 2 is naturally cooled to room temperature, the black product is collected by suction filtration, and the product is washed with deionized water and ethanol respectively, and after vacuum drying, tungsten diselenide (WSe 2 ) nanoflowers.

[0025] like figure 1 Shown: the reactant of embodiment 1 is the X-ray diffraction (XRD) pattern of the final product after reacting under the condition of 200 ℃ for 48 hours at a temperature, as can be seen from the figure that the product is WSe with better crystallization 2 , and there is no impurity.

Embodiment 2

[0027] Step 1: Add 0.3869g H 2 SeO 3 Dissolve in 50ml of N,N-dimethylformamide (DMF), add 0.3299g Na while stirring 2 WO 4 2H 2 After O, a mixed solution is obtained;

[0028] Step 2: Transfer the mixed solution in step 1 to a 100ml polytetrafluoroethylene reactor, and react at a temperature of 220°C for 36 hours;

[0029] Step 3: after the temperature in the reaction kettle of step 2 is naturally cooled to room temperature, the black product is collected by suction filtration, and the product is washed with deionized water and ethanol respectively, and after vacuum drying, tungsten diselenide (WSe 2 ) nanoflowers.

[0030] like figure 2 Shown: the Raman spectrogram of the final product after the reaction of the reactant in Example 2 was reacted at 220°C for 36 hours, as can be seen from the figure, at 247cm -1 WSe 2 Obvious Raman characteristic peak E 1 2g .

Embodiment 3

[0032] Step 1: Add 0.6449g H 2 SeO 3 Dissolve in 50ml of N,N-dimethylformamide (DMF), add 0.3299g Na while stirring 2 WO 4 2H 2 After O, a mixed solution is obtained;

[0033] Step 2: Transfer the mixed solution in step 1 to a 100ml polytetrafluoroethylene reactor, and react at a temperature of 220°C for 24 hours;

[0034]Step 3: after the temperature in the reaction kettle of step 2 is naturally cooled to room temperature, the black product is collected by suction filtration, and the product is washed with deionized water and ethanol respectively, and after vacuum drying, tungsten diselenide (WSe 2 ) nanoflowers.

[0035] like image 3 As shown, the scanning electron microscope (SEM) figure of the final product after the reaction of the reactant in Example 3 was reacted for 24 hours under the condition of 220 ° C, it can be seen from the figure that the product is uniform in size and evenly distributed. 2 composed of nanoflowers.

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Abstract

The invention discloses a method for preparing a tungsten diselenide nanoflower, and belongs to the technical field of nanometer material preparation. The method comprises the following steps: dissolving H2SeO3 in an organic solvent and mixing uniformly, and adding Na2WO4 2H2O to prepare a mixed solution while stirring; transferring the mixed solution into a reaction kettle and reacting at a temperature in the range of 180-240 DEG C for 12 hours to 48 hours; after the temperature of the reaction kettle is naturally cooled to room temperature, collecting a black product by suction filtration, washing the product with deionized water and ethanol respectively, and drying in vacuum to obtain tungsten diselenide nanoflower. The method for synthesizing the tungsten diselenide nanoflower by one step through a solvothermal method is firstly provided. The preparation method provided by the invention has the advantages of simple process, easy obtaining of raw materials, low cost, mild reaction conditions 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 ) The preparation method of nano flower. 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 ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B19/04
CPCC01B19/007C01P2002/72C01P2002/82C01P2004/03C01P2004/04C01P2004/30
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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