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Preparation method of P-phase VO2 nano-powder

A vanadium dioxide nano-powder technology, applied in the direction of vanadium oxide, nano-technology, etc., can solve the problems of increased cost and adverse environmental impact, and achieve the effects of small size, good dispersion, and simple preparation method

Active Publication Date: 2017-05-24
HEFEI INSTITUTES OF PHYSICAL SCIENCE - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although the hydrothermal method in this preparation method can obtain the vanadium dioxide powder of the orthorhombic phase P phase, there are also shortcomings. First, the oxalic acid in the raw material is easy to cause adverse effects on the environment; secondly, the obtained The subsequent annealing treatment of the orthorhombic phase P phase vanadium dioxide powder requires nitrogen protection, which increases the cost of production

Method used

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  • Preparation method of P-phase VO2 nano-powder
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  • Preparation method of P-phase VO2 nano-powder

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Embodiment 1

[0029] The concrete steps of preparation are:

[0030] Step 1, first according to the weight ratio of ammonium metavanadate, docusate sodium and water is 0.03:0.03:5, ammonium metavanadate and docusate sodium are added to water and stirred for 2h; wherein, water is deionized water (or distilled water) to obtain a mixed solution. Then according to the volume ratio of 80wt% formic acid solution and water in the mixed solution being 0.1:1, add the formic acid solution dropwise to the mixed solution under stirring to obtain a reaction precursor solution.

[0031] In step 2, first place the reaction precursor solution at 180° C. for a sealed reaction for 4 days to obtain a reaction solution. Carry out the processing of solid-liquid separation, washing and drying to reaction solution successively; Wherein, solid-liquid separation processing is centrifugal separation, and its rotating speed is 7000r / min, time is 10min, and washing processing is to use deionized water (or distilled w...

Embodiment 2

[0033] The concrete steps of preparation are:

[0034] Step 1, first according to the weight ratio of ammonium metavanadate, docusate sodium and water is 0.037:0.025:5, add ammonium metavanadate and docusate sodium to water and stir for 2.5h; wherein, water is deionized water (or distilled water) to obtain a mixed solution. Then, according to the volume ratio of 83wt% formic acid solution to water in the mixed solution of 0.085:1, the formic acid solution was added dropwise to the stirred mixed solution to obtain a reaction precursor solution.

[0035]In step 2, first place the reaction precursor solution at 198° C. for a closed reaction for 3 days to obtain a reaction solution. Carry out the treatment of solid-liquid separation, washing and drying to reaction solution successively; Wherein, solid-liquid separation process is centrifugation, and its rotating speed is 7750r / min, time is 9min, and washing process is to use deionized water (or distilled water) and ethanol The s...

Embodiment 3

[0037] The concrete steps of preparation are:

[0038] Step 1, first according to the weight ratio of ammonium metavanadate, docusate sodium and water is 0.044:0.02:5, ammonium metavanadate and docusate sodium are added to water and stirred for 3h; wherein, water is deionized water (or distilled water) to obtain a mixed solution. Then, according to the volume ratio of 85wt% formic acid solution to water in the mixed solution of 0.065:1, the formic acid solution was added dropwise to the stirred mixed solution to obtain a reaction precursor solution.

[0039] In step 2, first place the reaction precursor solution at 216° C. for a closed reaction for 3 days to obtain a reaction solution. Carry out the treatment of solid-liquid separation, washing and drying to reaction solution successively; Wherein, solid-liquid separation process is centrifugation, and its rotating speed is 8500r / min, time is 7min, and washing process is to use deionized water (or distilled water) and ethanol...

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Abstract

The invention discloses a preparation method of P-phase VO2 nano-powder. The method adopts a hydrothermal method and specifically comprises the following steps: firstly, ammonium metavanadate and docusate sodium are added to water and stirred, a mixed solution is obtained, a formic acid solution is added dropwise to the mixed solution under stirring, and a reaction precursor solution is obtained; then the reaction precursor solution is placed at 180-250 DEG C for closed reaction, a reaction liquid is obtained and subjected to solid-liquid separation, washing and drying, and a granular target product with particle size being 50-90 nm, namely, the P-phase VO2 nano-powder, is obtained. The preparation method has the characteristics that environmental protection is realized and nitrogen protection is not needed for follow-up annealing treatment of the target product, conversion of VO2(P) to VO2(M) can be realized easily through low temperature thermal treatment, and accordingly, the final product VO2(M) is applied to the fields of energy-saving windows, sensors, storage devices and the like commercially and widely quite easily.

Description

technical field [0001] The invention relates to a preparation method of nano powder, in particular to a preparation method of P-phase vanadium dioxide nano powder. Background technique [0002] As a transition metal element, vanadium ions have multiple valence states, and the structures and properties of vanadium oxides corresponding to different valence states are different. Studies have shown that in the tetravalent oxide vanadium dioxide (VO 2 ) various isomers - VO 2 (R), VO 2 (M), VO 2 (A), VO 2 (B), VO 2 (D) and VO 2 (P) etc., M-phase VO 2 (low-temperature semiconductor phase) can undergo reversible phase transition with R-phase (high-temperature metal phase) at the phase transition temperature Tc=68°C, and at the same time, its electrical and optical properties will undergo a sudden change. This feature makes it suitable for energy-saving windows, sensors and storage devices and other fields have broad application prospects. Currently, people are preparing M-...

Claims

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Application Information

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IPC IPC(8): C01G31/02B82Y40/00
CPCB82Y40/00C01G31/02C01P2002/72C01P2002/88C01P2004/03C01P2004/04C01P2004/64
Inventor 李广海钟莉罗媛媛
Owner HEFEI INSTITUTES OF PHYSICAL SCIENCE - CHINESE ACAD OF SCI
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