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One-step hydrothermal method for preparing molybdenum-doped VO2 (M) powder by aid of tartaric acid used as reducing agent

A technology of tartaric acid and reducing agent, applied in vanadium oxide and other directions, can solve the problems of affecting thermally induced phase change performance, powder agglomeration, complex process and other problems, and achieve the effects of good crystallinity, low cost and simple operation.

Inactive Publication Date: 2018-02-02
SICHUAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, VO prepared by hydrothermal method 2 The final product is usually metastable VO 2 (B), if you want to get VO 2 (M), also need to VO 2 (B) The powder is subjected to further heat treatment, which will inevitably lead to the agglomeration of the powder, thereby affecting its thermally induced phase change performance, and the energy consumption is large, and the process is more complicated

Method used

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  • One-step hydrothermal method for preparing molybdenum-doped VO2 (M) powder by aid of tartaric acid used as reducing agent
  • One-step hydrothermal method for preparing molybdenum-doped VO2 (M) powder by aid of tartaric acid used as reducing agent
  • One-step hydrothermal method for preparing molybdenum-doped VO2 (M) powder by aid of tartaric acid used as reducing agent

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] (1) Put 1.092 g V 2 o 5 , 0.18 g of tartaric acid, 1.5 at % ammonium molybdate, and 70 ml of deionized water were put into a beaker, and magnetically stirred at room temperature for 1 hour.

[0025] (2) Transfer the mixed solution to a 100 ml polytetrafluoroethylene autoclave and react at 240 °C for 48 hours.

[0026] (3) Synthesized by hydrothermal reaction, after naturally cooling to room temperature, the precipitate obtained from the reaction was centrifuged and washed three times with deionized water and absolute ethanol respectively.

[0027] (4) Put the washings in an oven and dry at 60 °C for 12 h to obtain the final product.

Embodiment 2

[0029] (1) Put 1.092 g V 2 o 5 , 0.36 g of tartaric acid, 1 at % ammonium molybdate, and 70 ml of deionized water were put into a beaker, and magnetically stirred at room temperature for 2 hours.

[0030] (2) Transfer the mixed solution to a 100 ml polytetrafluoroethylene autoclave and react at 220 °C for 72 hours.

[0031] (3) Synthesized by hydrothermal reaction, after naturally cooling to room temperature, the precipitate obtained from the reaction was washed by centrifugation twice with deionized water and absolute ethanol respectively.

[0032] (4) Put the washings into an oven and dry at 80°C for 10 hours to obtain the final product.

Embodiment 3

[0034] (1) Put 1.092 g V 2 o 5 , 0.36 g of tartaric acid, 2 at % ammonium molybdate, and 80 ml of deionized water were put into a beaker, and magnetically stirred at room temperature for one hour.

[0035] (2) Transfer the mixed solution to a 100 ml polytetrafluoroethylene autoclave and react at 240 °C for 48 hours.

[0036] (3) Synthesized by hydrothermal reaction, after naturally cooling to room temperature, the precipitate obtained from the reaction was centrifuged and washed three times with deionized water and absolute ethanol respectively.

[0037] (4) Put the washings into an oven and dry at 70°C for 10 hours to obtain the final product.

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Abstract

The invention relates to a one-step hydrothermal method for preparing molybdenum-doped VO2 (M) powder by the aid of tartaric acid used as a reducing agent. The one-step hydrothermal method mainly includes steps of uniformly stirring certain quantities of vanadium pentoxide, the tartaric acid, doping agents and deionized water at the room temperature to obtain mixtures, then transferring the mixtures into a high-pressure reaction kettle and carrying out hydrothermal reaction in the temperature ranges of 180-240 DEG C for the reaction time of 24-72 hours; naturally cooling reaction products until the temperatures of the reaction products reach the room temperature, repeatedly centrifugally washing obtained precipitates and ultimately drying the precipitates to obtain the molybdenum-doped VO2(M) powder. The one-step hydrothermal method has the advantages that the pure-phase molybdenum-doped VO2 (M) powder can be prepared by the aid of one-step hydrothermal processes at the low reaction temperatures for the short reaction time, and accordingly the problems of particle aggregation and influence on the thermochromism performance due to VO2 (M) powder prepared by the aid of hydrothermalprocesses and annealing heat treatment processes can be solved; the molybdenum-doped VO2 (M) powder prepared by the aid of the one-step hydrothermal method is high in purity and good in crystallinity,and the phase change temperatures can be controlled.

Description

technical field [0001] The invention relates to a one-step hydrothermal preparation of molybdenum-doped VO using tartaric acid as a reducing agent 2 (M) The powder method belongs to the field of material synthesis. Background technique [0002] As an important transition metal oxide, vanadium dioxide (VO 2 ) has always attracted the attention of scholars at home and abroad. VO 2 Has a variety of crystal structures, so far, more than 10 kinds of VO 2 Crystalline phases (B, M, R, A, C, etc.) are reported. However, in these crystal forms, VO 2 (M) has the most research significance and application value, because only VO 2 (M) can be at the temperature closest to room temperature ( T c =68 ℃) a reversible phase transition (Metal-Semiconductor Transition, referred to as MST phase transition) occurs from a low-temperature monoclinic semiconductor phase (M phase) to a high-temperature tetragonal rutile metal phase (R phase). And in the process of phase transition, it is...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G31/02
CPCC01G31/02C01P2002/72C01P2002/85C01P2004/03
Inventor 黄婉霞梁珊施奇武
Owner SICHUAN UNIV
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