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A kind of preparation method of vanadium disulfide micro-nano structure material

A vanadium disulfide micro-nano and structural material technology, applied in the field of nano-materials and new energy materials, can solve the problems of unstable structure and performance, easy collapse of the structure, complicated preparation method and operation, etc. Structural stability, cheap and easily available raw materials

Active Publication Date: 2018-04-06
NANKAI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Because vanadium has multiple valence states (II, III, IV, V, etc.), vanadium disulfide is difficult to be directly combined with elements, and is mostly synthesized in organic solvents. The preparation method is complicated and difficult to control the valence state of vanadium, and it is difficult to obtain VS. 2 Pure phase and controllable preparation, resulting in instability of structure and properties
For example, in the field of electrochemistry, VS 2 As an electrode material for lithium-ion batteries, due to the large material particles, the material stability is poor, and the structure is easy to collapse, resulting in serious capacity attenuation; in the study of hydrogen evolution, the irregular vanadium disulfide particles cannot expose more active sites. lead to poor catalytic performance

Method used

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  • A kind of preparation method of vanadium disulfide micro-nano structure material
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  • A kind of preparation method of vanadium disulfide micro-nano structure material

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Embodiment 1

[0021] A preparation method of vanadium disulfide micro-nano structure material, comprising the following steps:

[0022] 1) At room temperature, measure 15mL of ultrapure water in a 50mL beaker, put 0.5g of polyvinylpyrrolidone K30 (PVP-K30) in the beaker, and stir with an electromagnetic stirrer at 800r / min for 30 minutes until completely dissolved;

[0023] 2) Add 0.2mmol of ammonium metavanadate and 0.1mmol of thioacetamide to the above solution and continue to stir until it is completely dissolved. After it is completely dissolved and the color of the solution turns dark brown, add ammonia water with a concentration of 12mol / L dropwise to adjust the pH value is 9;

[0024] 3) Put the mixed solution in a 25ml polytetrafluoroethylene liner, and place the liner in a high-pressure hydrothermal kettle. Cool to room temperature naturally after reacting at 160°C for 15 hours;

[0025] 4) Take out the black suspension and put it in a 50ml centrifuge tube, use a centrifuge to wa...

Embodiment 2

[0028] A preparation method of vanadium disulfide micro-nano structure material, comprising the following steps:

[0029] 1) At room temperature, measure 15mL of ultrapure water in a 50mL beaker, put 0.5g of polyvinylpyrrolidone K60 (PVP-K60) in the beaker, and stir at 800r / min for 30 minutes with an electromagnetic stirrer until completely dissolved;

[0030] 2) Add 0.2mmol of ammonium metavanadate and 0.1mmol of thioacetamide to the above solution and continue to stir until it is completely dissolved. After it is completely dissolved and the color of the solution turns dark brown, add ammonia water with a concentration of 12mol / L dropwise to adjust the pH value is 9;

[0031] 3) Put the mixed solution in a 25mL polytetrafluoroethylene liner, and place the liner in a high-pressure hydrothermal kettle. Cool to room temperature naturally after reacting at 160°C for 20 hours;

[0032] 4) Take out the black suspension and put it in a 50m centrifuge tube, wash it 6 times with ul...

Embodiment 3

[0035] This example does not add polyvinylpyrrolidone, as a comparative example, the flower-shaped vanadium disulfide particles have been synthesized, and the steps are as follows:

[0036] 1) At room temperature, take 15mL of ultrapure water in a 50mL beaker, add 0.2mmol ammonium metavanadate and 0.1mmol thioacetamide, stir until completely dissolved, wait until completely dissolved and the dissolved color reaches dark brown, add the concentration dropwise The ammonia water of 12mol / L is adjusted to a pH value of 9;

[0037] 2) Put the mixed solution in a 25mL polytetrafluoroethylene liner, and place the liner in a high-pressure hydrothermal kettle. Cool to room temperature naturally after reacting at 160°C for 20 hours;

[0038] 3) Take out the black suspension and put it in a 50mL centrifuge tube, wash it with ultrapure water and absolute ethanol for 6 times at the speed of 9800r / min in a centrifuge, take the precipitated substance, and put it in a vacuum oven at 110°C and...

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Abstract

The invention relates to a preparation method for a vanadium dioxide micro-nanometer structure material. According to the invention, by adopting polyvinylpyrrolidone (PVP) as a surfactant, a pure-phase vanadium dioxide micro-nanometer structure is hydrothermally prepared. The invention has the following advantages: VS2 lamellas prepared by using the method provided by the invention have regular sizes and uniform stacking thickness, so controllable preparation of vanadium dioxide is successfully realized; the preparation method has the advantages of simple operation, strong controllability, cheap and easily-available raw materials, and facilitation to mass production; and the vanadium dioxide prepared by using the method provided by the invention can reinforce structure stability and exposes more active sites, thereby facilitating to application in a plurality of fields like electrochemistry, oxygen reduction and hydrogen evolution.

Description

technical field [0001] The invention relates to nanometer material and new energy material technology, in particular to a preparation method of vanadium disulfide micronano structure material. Background technique [0002] Environmental pollution and energy shortage have become one of the most serious problems faced by human beings, and finding renewable energy and safe and reliable energy storage technology has become a very important issue. Lithium-ion batteries have the advantages of high voltage, large capacity, no memory effect and long life, and are widely used in electronic products such as mobile phones, digital cameras and notebooks, and have become the focus of the development of the battery industry. One of the keys to the development of lithium-ion batteries is to find suitable electrode materials, so that the battery has a sufficiently high lithium intercalation capacity and good lithium intercalation and deintercalation capabilities, so as to ensure the large s...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G31/02
CPCC01G31/02C01P2002/72C01P2004/03C01P2004/50C01P2004/61
Inventor 陶占良李攀孙维祎陈军李海霞
Owner NANKAI UNIV