High tungsten doping content nanometer VO2 powder material and preparation method thereof

A tungsten-doped, high-content technology, applied in nanotechnology, nanotechnology, nanotechnology and other directions for materials and surface science, can solve the problems of inability to dope atomic doping, affecting the application effect of VO2, and single preparation process. , to achieve the effect of increasing the amount of doping

Active Publication Date: 2014-05-21
深圳清研皓隆科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the low activity of the doping metal source, the existing preparation process is single and ca

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0062] Example 1

[0063] Preparation of scheelite:

[0064] 15wt% sodium tungstate (Na 2 WO 4 ·2H 2 O) 100mL of solution is added dropwise to 0.5mol·L -1 HNO 3 In 150 mL of the solution, a yellowish precipitate was generated. After the dripping is completed, let stand for 2h, filter the formed precipitate, and use 100mL of 0.05mol·L for the precipitate. -1 HNO 3 , 100mL of 95% ethanol and 100mL of ether for three times. Dry it at 80℃ for 10h to obtain white or slightly yellow powdery scheelite.

Example Embodiment

[0065] Example 2

[0066] A preparation method of nano vanadium dioxide powder doped with high content of tungsten, including the following steps:

[0067] (1) First doping

[0068] ①Add 91g (0.5mol) V 2 O 5 Add deionized water to adjust the slurry, then add an aqueous solution of oxalic acid with a concentration of 0.1g / mL at a dropping rate of 10mL / min to adjust the pH to 7, and stir at 40°C for 1 hour; where, V 2 O 5 The ratio of mass to deionized water is 1:2;

[0069] ②To the solution obtained in step ①, add 100 mL of concentrated hydrochloric acid dropwise in 3 times, boil slightly for 5 minutes, and then add 10 mL of N with a concentration of 1 g / mL at a dropping rate of 0.5 mL / min. 2 H 4 ·2HCl aqueous solution is fully reacted to obtain VOCl 2 Solution; then dilute to 1mol / L with deionized water;

[0070] ③Next, add carbon dioxide to the solution obtained in step ② to drive oxygen for 10 minutes, while continuing to add carbon dioxide, add 0.1 mol / L of NH dropwise under the act...

Example Embodiment

[0077] Example 3

[0078] A preparation method of nano vanadium dioxide powder doped with high content of tungsten, including the following steps:

[0079] (1) First doping

[0080] ①Add 91g (0.5mol) V 2 O 5 Add deionized water to adjust the slurry, then add an aqueous solution of oxalic acid with a concentration of 0.3g / mL at a dropping rate of 15mL / min to adjust the pH to 6, and stir at 50°C for 1.5 hours; where, V 2 O 5 The ratio of mass to deionized water is 1:3;

[0081] ②To the solution obtained in step ①, add 200 mL of concentrated hydrochloric acid dropwise in 4 times, boil slightly for 5 minutes, and then add 15 mL of N with a concentration of 1 g / mL at a dropping rate of 0.5 mL / min. 2 H 4 ·2HCl aqueous solution is fully reacted to obtain VOCl 2 Solution; dilute to 1.5mol / L with deionized water;

[0082] ③Then add carbon dioxide to the solution obtained in step ② to drive oxygen for 20 minutes, while continuing to add carbon dioxide, add 0.5mol / L of NH dropwise at the same tim...

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Abstract

The present invention provides a high tungsten doping content nanometer VO2 powder material and a preparation method thereof. According to the preparation method, a hydrothermal synthesis doping method and a sol-gel doping method are organically combined so as to improve the tungsten atom doping amount; and the chemical activity of the used raw material white tungstic acid is much higher than the chemical activity of other compounds of tungsten, such that the amount of the tungsten doped in the VO2 lattice is substantially increased. With the method, the VO2 phase-transition temperature can be effectively reduced, and wide applications can be achieved.

Description

technical field [0001] The invention belongs to the field of production and preparation of inorganic functional materials, and relates to a tungsten-doped nano vanadium dioxide powder material with high doping content and a preparation method thereof. Background technique [0002] Vanadium dioxide (VO 2 ) is a metal oxide with phase transition properties. Since Morin F.J. of Bell Laboratories in the United States discovered vanadium dioxide (VO 2 ) Since the thermally induced phase transition, VO 2 It has become one of the most concerned phase-change metal compounds. Vanadium dioxide (VO 2 ) As a functional material, there will be a reversible phase transition from low-temperature monoclinic phase (M phase) to high-temperature tetragonal rutile phase (R phase) at about 68 ° C. With this structural change, its electrical conductivity, magnetic susceptibility, and light transmission The physical properties such as pass rate, resistivity and reflectivity will change sudden...

Claims

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Application Information

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IPC IPC(8): C01G41/00C01G31/00B82Y30/00
Inventor 刘畅刘英博乔东才
Owner 深圳清研皓隆科技有限公司
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