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Preparation method of 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 preparation temperature, and high reaction temperature, and achieve easy-to-obtain raw materials The effect of low cost, uniform scale distribution, and mild reaction conditions

Active Publication Date: 2018-04-13
UNIV OF ELECTRONICS SCI & TECH OF CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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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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  • Preparation method of tungsten diselenide nanoflower
  • Preparation method of tungsten diselenide nanoflower
  • Preparation method of 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] Such as 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] Such as 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] Such as 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 preparation method of tungsten diselenide nano-flowers, belonging to the technical field of nano-material preparation. The invention comprises the following steps: dissolving H2SeO3 in an organic solvent and mixing evenly, adding Na2WO4·2H2O while stirring to prepare a mixed solution; transferring the obtained mixed solution to a reaction kettle, and keeping the temperature range of 180°C to 240°C React for 12 hours to 48 hours; after the temperature of the reaction kettle is naturally cooled to room temperature, collect the black product by suction filtration, wash the product with deionized water and ethanol respectively, and dry it in vacuum to obtain tungsten diselenide nanoflowers . The present invention proposes a method for synthesizing tungsten diselenide nanoflowers in one step through a solvothermal method for the first time; the present invention has the advantages of simple process, readily available 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 Patents(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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