Vanadium dioxide powders and preparation method thereof

A technology for vanadium dioxide and powder, applied in the field of vanadium dioxide powder and its preparation, can solve the problems of high toxicity, low solubility, high price and the like, and achieve the effects of low toxicity, simple preparation method and low price

Active Publication Date: 2012-07-25
SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, these raw materials are highly toxic,

Method used

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  • Vanadium dioxide powders and preparation method thereof
  • Vanadium dioxide powders and preparation method thereof
  • Vanadium dioxide powders and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Add 2.10 grams of citric acid to 50 milliliters of hydrogen peroxide with a mass fraction of 30%, adjust the pH value to 10 with ammonia water, place the above solution in an ice-water bath, slowly add 1.63 grams of vanadyl sulfate, stir for 2 hours, add 50 Milliliter of ethanol and let it stand for 4 hours, the resulting precipitate was separated by filtration to obtain the peroxo complex of vanadium.

[0036] The Raman spectrum of the product obtained in this embodiment is as follows figure 1 Shown: at 885cm -1 、608cm -1 、526cm -1 The peak at is the characteristic peak of peroxy group, shows that contains peroxy group in the product. 971cm -1 The peak at is the characteristic peak of the V=O bond.

[0037] The infrared spectrum of the product obtained in this embodiment is as follows figure 2 Shown: at 870cm -1 、610cm -1 、523cm -1 The peak at is the characteristic peak of the peroxy group, 950cm -1 The peak at is the characteristic peak of the V=O bond.

...

Embodiment 2

[0045] Dissolve 20 ml of hydrogen peroxide with a mass fraction of 30% in 80 ml of water, add 1.08 g of tartaric acid, adjust the pH value to 12 with ammonia water, place the above solution in an ice-water bath, slowly add 0.78 g of vanadyl sulfate, and stir After 4 hours, 120 ml of isopropanol was added and allowed to stand for 8 hours, and the resulting precipitate was separated by filtration to obtain a vanadium peroxy complex.

[0046] Using Raman and infrared spectroscopy to analyze the functional groups contained in the product obtained in this example, the results are similar to those in Example 1, indicating that it contains peroxy groups.

Embodiment 3

[0048] In 50 milliliters of hydrogen peroxide with a mass fraction of 30%, add 2.40 grams of malic acid, adjust the pH value to 14 with ammonia water, place the above solution in an ice-water bath, slowly add 1.96 grams of vanadyl sulfate, and stir for 4 hours. After adding 80 milliliters of acetone, the mixture was allowed to stand for 6 hours, and the resulting precipitate was separated by filtration to obtain a peroxo complex of vanadium.

[0049] Using Raman and infrared spectroscopy to analyze the functional groups contained in the product obtained in this example, the results are similar to those in Example 1, indicating that it contains peroxy groups.

[0050] The obtained product of embodiment 2 and 3 is through elemental analysis, and its obtained product composition meets general formula V 2 N 3±x h 14±y o 11±z , where the values ​​of x, y, and z are all between 0-1.

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Abstract

The invention discloses a preparation method of vanadium dioxide powders. The preparation method comprises the following steps: 1) dissolving carboxylic acid with hydroxyl in hydrogen peroxide, regulating pH value of the solution with ammonia water to be more than 7; adding vanadyl sulfate in the solution to obtain a reaction solution; after the completion of the reaction, adding an organic solvent in the solution, standing to generate precipitate, separating the precipitate from the solution to obtain peroxide complex of vanadium; 2) adding the peroxide complex of vanadium obtained in the step 1) and a reducing agent in water to form a water solution, and carrying out hydrothermal treatment to obtain vanadium dioxide powders. According to the invention, the preparation process is simple; the phase of product is adjustable; the powders of vanadium dioxide containing phase A are prepared, so that the material is provided for studying vanadium dioxide powders with phase A, and therefore, the preparation method is potentially significant for the scientific study.

Description

technical field [0001] The invention relates to a vanadium dioxide powder and a preparation method thereof, belonging to the field of preparation and application of functional materials. Background technique [0002] Vanadium dioxide (VO 2 ) has a variety of phases, among which the most stable phases are R phase and M phase, and the two can transform into each other around 68°C: when the temperature is higher than 68°C, VO 2 It is the R phase of rutile structure, and it is the M phase of monoclinic structure when it is lower than 68°C. In addition to R phase, M phase, VO 2 There are also some unstable phases, such as phase A and phase B. Among them, phase B can be obtained at low temperature or short reaction time, but the preparation and performance of phase A are rarely studied. During the mutual transition between R phase and M phase, VO 2 Physical properties such as optical transmittance, resistivity, and magnetic susceptibility will also change suddenly. Based on th...

Claims

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Application Information

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IPC IPC(8): C01G31/02B82Y40/00
Inventor 高彦峰刘新玲罗宏杰
Owner SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI
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