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Preparation method for vanadium dioxide and doped powder thereof

A technology of vanadium dioxide and vanadium pentoxide, applied in the direction of vanadium oxide, etc., can solve the problems of uneven dispersion of dopants, unfavorable large-scale growth, long reaction time, etc., and achieve simple process, excellent phase change performance, low cost effect

Active Publication Date: 2012-06-20
张家港楚人新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

So far, there are only two reports on the preparation of doped VO2 by hydrothermal method: Li, J. reported [1] using ammonium metavanadate and tungstic acid ammonium, and then adjust the pH to 2-3 with acetic acid, first prepare the doped powder of VO2(B), and then convert it into VO2(M) Doped powder, this method has very high requirements for pH, is not conducive to large-scale growth, and has poor repeatability; Cao, C. X. and Whittaker, L. have reported [2-3] using Preparation of doped monoclinic VO2(M) by high temperature hydrothermal reaction of V2O5, oxalic acid and tungstic acid for 7 days , this method has shortcomings such as long reaction time, strict requirements on hydrothermal kettle, and uneven dispersion of dopant in the product.

Method used

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  • Preparation method for vanadium dioxide and doped powder thereof
  • Preparation method for vanadium dioxide and doped powder thereof
  • Preparation method for vanadium dioxide and doped powder thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] Add 0.45 g of vanadium pentoxide to 23.00 g of distilled water, and add 2.22 g of hydrogen peroxide to prepare V 5+ 4.08 g reductant ethanol was added to the complex solution, and a magnetic stirrer was used to stir for 0.5 h to obtain a clear solution; the obtained clear solution was transferred to a hydrothermal reaction kettle and heated at 180 After reacting at ℃ for 24 h, the material was naturally cooled to room temperature and discharged, centrifuged, washed with deionized water, and dried in vacuum to obtain undoped VO 2 , figure 1 a is the obtained VO 2 The XRD spectrum of the figure, it can be seen from the figure that VO 2 VO 2 (B). Finally, the resulting VO 2 (B) Calcined in a high-purity argon atmosphere at 700 °C for 2 h to obtain the final product VO with phase transition properties 2 , figure 2 a shows the XRD pattern of the final product, as can be seen from the figure, the final product is monoclinic VO 2 (M); Adopting differential scanning ca...

Embodiment 2

[0044] Add 0.15 g of vanadium pentoxide to 27.00 g of distilled water, and add 2.85 g of hydrogen peroxide to prepare V 5+ 12.00 g reducing agent ethanol was added to the complex solution, and a magnetic stirrer was used to stir for 0.5 h to obtain a clear solution; the obtained clear solution was transferred to a hydrothermal reaction kettle and heated at 140 After reacting at ℃ for 168 h, the material was naturally cooled to room temperature and discharged, centrifuged, washed with deionized water, and dried in vacuum to obtain undoped VO 2 (B); Finally, the obtained VO 2 (B) Calcined at 700 °C for 10 min in a high-purity argon atmosphere to obtain the final product VO with phase transition properties 2 (M).

Embodiment 3

[0046] Add 3.64 g of vanadium pentoxide to 25.48 g of distilled water, and add 7.28 g of hydrogen peroxide to prepare V 5+ 1.82 g reducing agent ethanol and 1.82 g surfactant sodium dodecyl sulfate (SDS) were added to the complex solution, and stirred with a magnetic stirrer for 2 h to obtain a clear solution; The obtained clear solution was transferred to a hydrothermal reaction kettle, reacted at 220 °C for 72 h, cooled down to room temperature naturally, and discharged, centrifuged, washed with deionized water, and dried in vacuum to obtain undoped VO 2 (B); Finally, the obtained VO 2 (B) Calcined at 400 °C for 720 min in a high-purity argon atmosphere to obtain the final product VO with phase transition properties 2 (M).

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Abstract

The invention discloses a preparation method for vanadium dioxide and doped powder thereof. The method comprises the following steps: 1, weighing vanadium pentoxide, hydrogen peroxide and distilled water, preparing the materials into a V<5+>-containing complex aqueous solution; 2, adding a reducing agent, a surfactant and a dopant to the complex aqueous solution, and stirring to form a clear solution; 3, transferring the resulting solution from the step 2 to a hydrothermal reaction kettle, and carrying out a reaction for 1-168 hours at a temperature of 140-220 DEG C to obtain the doped powderof the VO2(B); 4, placing the resulting doped powder of the VO2(B) from the step 3 in high pure argon atmosphere or nitrogen atmosphere, and annealing for 10-720 minutes at the temperature of 400-700DEG C to obtain the doped powder of the VO2(M). The method of the present invention has characteristics of low cost, simple process and easy control, and is suitable for the large-scale industrial production. With the method of the present invention, the doping of the VO2 powder material can be realized, and the doped atoms can be uniformly dispersed in the VO2.

Description

[0001] technical field [0002] The invention belongs to the field of preparation of inorganic functional materials, in particular to a preparation method of vanadium dioxide and its doped powder. Background technique [0003] Vanadium dioxide (VO 2 ) is a typical metal oxide with phase transition properties, which can undergo a reversible phase transition between a low-temperature monoclinic phase (M) and a high-temperature tetragonal rutile phase (R) around 68 °C, VO 2 The phase transition temperature of is the closest to room temperature among the compounds known to have such phase transition properties. VO 2 Before and after the phase transition, its conductivity, resistivity, magnetic susceptibility, light transmittance, and reflectance will change abruptly. For example, its conductivity will have a sudden change of 5 orders of magnitude before and after the phase transition; 2 This phase transition characteristic of VO 2 It has broad application prospects in thermi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G31/02
Inventor 黄驰张依福刘兴海樊美娟
Owner 张家港楚人新材料科技有限公司
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