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Method of preparing intelligent energy-saving vanadium dioxide by hydrothermal method

A vanadium dioxide, hydrothermal technology, applied in vanadium oxide, chemical industry, climate sustainability and other directions, can solve the problems of difficult to obtain VO2 pure phase, difficult to control vanadium valence state, difficult to large-scale production and so on , to achieve the effect of superior intelligent energy-saving cycle performance, easy to scale up mass production, and low cost

Inactive Publication Date: 2010-05-05
UNIV OF SCI & TECH OF CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method requires expensive cost and it is difficult to control the valence state of vanadium in it, and it is difficult to obtain VO 2 pure phase
This makes the monoclinic and tetragonal rutile vanadium dioxide (VO2(M) and VO 2 (R)) The preparation cost of the powder is greatly increased, and it is difficult to achieve large-scale production

Method used

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  • Method of preparing intelligent energy-saving vanadium dioxide by hydrothermal method
  • Method of preparing intelligent energy-saving vanadium dioxide by hydrothermal method
  • Method of preparing intelligent energy-saving vanadium dioxide by hydrothermal method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Monoclinic VO 2 (VO 2 (M)) Realization of uniform ultra-long nanowires: add 2mmol ammonium metavanadate (NH 4 VO 3 ), and add 45ml of water, and then add 1ml of 1mol / L ammonia water to completely dissolve the ammonium metavanadate in the alkaline aqueous solution, then add 1ml of hydrazine hydrate, and stir for 10min. After sealing the hydrothermal autoclave, place it in an oven at 200° C. for 30 h. After natural cooling, the obtained product was washed with deionized water and absolute ethanol to remove possible impurities. Such as figure 1 As shown, all X-ray powder diffraction peaks can be indexed as VO 2 (M) powder, and no other impurity peaks occur, so what is synthesized in Example 1 is high-purity VO 2 (M) Powder material. figure 2 According to the test results of the intelligent energy-saving performance of the product obtained according to the embodiment of the present invention, the test chart is the actual measurement curve of 20 cycles. It can be see...

Embodiment 2

[0033] Nano-sized monoclinic VO 2 (VO 2 (M)) The realization of the smooth nanobelt of powder material: add 2mmol acetylacetonate vanadyl complex in 50ml polytetrafluoroethylene liner, and add 45ml water, add the hydrochloric acid of 0.5ml 1mol / L finally to make acetylacetonate vanadyl complex Completely dissolved in acidic aqueous solution, then stirred in the air for 30min. After sealing the hydrothermal autoclave, place it in an oven at 200° C. for 30 h. After natural cooling, the obtained product was washed with deionized water and absolute ethanol to remove possible impurities. Figure 4 It is the FE-SEM picture of the smooth nanobelt obtained according to the embodiment. This solution is also applicable to the following combinations: 2mmol vanadium acetylacetonate complex+45ml water+0.5ml 1mol / L sulfuric acid; 2mmol o-vanadyl vanillic acid complex+45ml water+0.5ml 1mol / L hydrochloric acid or sulfuric acid; 2mmol VCl4+45ml Water+0.5ml 1mol / L hydrochloric acid; 2mmol V...

Embodiment 3

[0035] Nano-sized monoclinic VO 2 (VO 2 (M)) Realization of powder material nano-hexagonal flower: add 2mmol VOOH to 50ml polytetrafluoroethylene liner, add 45ml water, then add 1ml 1mol / L hydrochloric acid to completely dissolve VOOH in the aqueous solution, then add 3ml 0.1mol / L nitric acid, and stirred in the air for 10min. After sealing the hydrothermal autoclave, place it in an oven at 200° C. for 30 h. After natural cooling, the obtained product was washed with deionized water and absolute ethanol to remove possible impurities. Figure 5 It is the FE-SEM photograph of the hexagonal flower shape of the product obtained according to this embodiment. This experimental protocol is also applicable to the following combinations: 2mmol V(OH)2NH2+45ml water+2ml 0.1mol / L nitric acid or hydrogen peroxide; 2mmol V2O3+1ml nitric acid+45ml water+2ml 0.1mol / L hydrogen peroxide; 2mmol vanadium acetylacetonate complex +45ml water+2ml0.1mol / L nitric acid. This figure shows that diff...

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Abstract

The invention relates to a method of preparing vanadium dioxide by hydrothermal method. The method comprises the following steps: adding oxidant, reducing agent or acidity and alkalinity adjusting agent in a hydrothermal kettle containing proper amount of aqueous solution of the source of vanadium, then placing the hydrothermal kettle in a 40-300 DEG C of oven to perform heat preservation for 30 minutes to 5 days, and centrifuging to collect vanadium dioxide after the reaction is completely finished. The preparation method provided by the invention has simple process, low cost and high yield, the mass production can be realized and the purity of the obtained intelligent energy-saving vanadium dioxide nano-powder is high. Vanadium dioxide doped powder can further be obtained by adding proper amount of compound containing tungsten, molybdenum, manganese, chromium or titanium in the aqueous solution of the source of vanadium to realize wider industrial applications. The control of different appearances of vanadium dioxide nano-powder can be realized by controlling the categories of the source of vanadium and the dosage of oxidant, reducing agent or acidity and alkalinity adjusting agent.

Description

technical field [0001] The invention relates to the preparation of monoclinic phase and tetragonal rutile phase vanadium dioxide nanometer powder, in particular to a method for preparing the nanometer powder and doped powder based on a hydrothermal method. Background technique [0002] Vanadyl oxide is a very important class of materials with intelligent properties. Changes in ambient temperature will cause changes in the crystal structure, electric domain structure, and magnetic structure of the material, resulting in large changes in optical properties. Especially vanadium dioxide (VO 2 ) has received special attention. [0003] Monoclinic VO 2 (VO 2 (M)) and tetragonal rutile phase VO 2 (VO 2 (R)) powder can be intelligently regulated to the outside world, such as the infrared part of sunlight, through phase change to achieve intelligent energy saving. Single crystal VO 2 The metal-insulator phase transition temperature is about 68 °C. At this temperature, VO 2 T...

Claims

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Application Information

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IPC IPC(8): C01G31/02
CPCY02P20/10
Inventor 吴长征张晓东谢毅
Owner UNIV OF SCI & TECH OF CHINA
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