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Tin-tungsten co-doped vanadium dioxide powder and preparation method thereof

A vanadium dioxide and co-doping technology, which is applied in the field of nanomaterials and nanometers, can solve the problems of cumbersome process, low efficiency, and high energy consumption, and achieve the effects of high controllability, simple and easy operation of the process, and mild reaction conditions

Inactive Publication Date: 2016-01-27
UNIV OF SCI & TECH BEIJING
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] In view of the above-mentioned deficiencies in the prior art, the object of the present invention is to provide a preparation method of tin-tungsten co-doped vanadium dioxide powder, aiming at reducing the phase transition temperature of vanadium dioxide and solving the problem of existing doped vanadium dioxide There are many problems in powder preparation, such as cumbersome process, low efficiency, and high energy consumption. It has the advantages of simple process, high efficiency and energy saving, and high degree of controllability.

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  • Tin-tungsten co-doped vanadium dioxide powder and preparation method thereof

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preparation example Construction

[0024] A kind of preparation method of tin-tungsten co-doped vanadium dioxide powder, the preparation method of described tin-tungsten co-doped vanadium dioxide powder comprises the following steps:

[0025] Step 1): dissolving the soluble vanadium salt, dissolving the soluble vanadium salt in deionized water, stirring evenly at room temperature to obtain a stable solution, the soluble vanadium salt is one or more of the water-soluble vanadium salts, including: vanadyl sulfate , vanadyl oxalate, etc.;

[0026] Step 2): Prepare the precipitation dispersion of the solution in step 1), react the vanadium-containing solution prepared in step 1) with the precipitating agent in deionized water to obtain a suspension, centrifuge and wash to remove impurities, and disperse the obtained precipitate in deionized water ionized water. The precipitating agent is one or more of water-soluble alkaline reagents, including: ammonia water, sodium hydroxide, potassium hydroxide, sodium bicarbon...

Embodiment 1

[0030] like figure 1 , 2 As shown, weigh 1.14g of vanadyl sulfate powder and dissolve it in 60mL of deionized water, stir evenly at room temperature, and prepare a blue transparent solution. Will pre-prepared VOSO 4 Solution and ammonia water were prepared by co-titration method to obtain VO(OH) 2 Precipitation, washing with deionized water and centrifugation were repeated three times, and the resulting precipitate was dispersed in 60 mL of deionized water.

[0031] According to the molar ratio, add 0.63g oxalic acid, 0.5mL hydrogen peroxide, 0.0304g ammonium tungstate and 0.0859g stannous sulfate to VO(OH) 2 Stir evenly in the dispersion liquid, transfer to a hydrothermal kettle, and conduct a hydrothermal reaction at 280°C for 36 hours. After the hydrothermal kettle was naturally cooled to room temperature, the obtained crude product was repeatedly washed and centrifuged with deionized water and absolute ethanol, and then dried in a vacuum oven at 60°C for 6 hours to obt...

Embodiment 2

[0033] like figure 1 , 3 As shown, weigh 1.14g of vanadyl sulfate powder and dissolve it in 60mL of deionized water, stir evenly at room temperature, and prepare a blue transparent solution. Will pre-prepared VOSO 4 Solution and ammonia water were prepared by co-titration method to obtain VO(OH) 2 Precipitation, washing with deionized water and centrifugation were repeated three times, and the resulting precipitate was dispersed in 60 mL of deionized water.

[0034] Add 0.63g oxalic acid, 0.5mL hydrogen peroxide and 0.0859g stannous sulfate to VO(OH) according to the molar ratio 2 Stir evenly in the dispersion liquid, transfer to a hydrothermal kettle, and conduct a hydrothermal reaction at 280°C for 36 hours. After the hydrothermal kettle was naturally cooled to room temperature, the obtained crude product was repeatedly washed and centrifuged with deionized water and absolute ethanol, and then dried in a vacuum oven at 60°C for 6 hours to obtain blue-black 1at%Sn-doped V...

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Abstract

The invention provides a preparation method of tin-tungsten co-doped vanadium dioxide powder. The preparation method includes the steps that firstly, soluble vandic salt is dissolved and then reacts with precipitant to obtain a vanadium-sediment-containing intermediate, centrifugation, washing and diffusion are conducted, and vanadium-containing dispersion liquid is obtained; secondly, a tungsten source, a tin source, a needed oxidizing agent and a needed reducing agent are added to the dispersion liquid and evenly stirred, and the mixture is transferred into a hydrothermal kettle; the hydrothermal kettle is arranged at the temperature of 200-300 DEG C for a hydrothermal reaction for 6-72 h; after the hydrothermal reaction is completed, the product is centrifuged, washed and dried, and then the tin-tungsten co-doped vanadium dioxide powder is obtained. The preparation process is simple, cost is low, reproducibility is good, the controllable degree is high, the co-doped vanadium dioxide powder is directly prepared through a one-step hydrothermal method, and heat treatment or crystallization is not needed. The phase-transition temperature of VO2(M / R) nano-powder can be regulated through tin-tungsten co-doping.

Description

technical field [0001] The invention belongs to the field of nanomaterials and nanotechnology, in particular to a tin-tungsten co-doped vanadium dioxide powder and a preparation method thereof. Background technique [0002] Vanadium dioxide (VO 2 ) is a high-quality phase change material, which can undergo a reversible phase change between a low-temperature monoclinic semiconductor phase (M phase) and a high-temperature rutile phase (R phase) near 68 ° C, accompanied by infrared light transmittance, resistivity , magnetic susceptibility and other properties, so it has broad application prospects in the fields of intelligent temperature control films and thermistor materials. However, different industries have different requirements for the phase transition temperature of vanadium dioxide. If the VO can be properly reduced 2 The phase transition temperature of (M) can break its application limit, so how to reduce VO 2 (M) The phase transition temperature has become a rese...

Claims

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Application Information

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IPC IPC(8): C01G31/02C01G41/02
Inventor 曹文斌李尧匡健磊张瑞
Owner UNIV OF SCI & TECH BEIJING
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