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Preparation method of monoclinic phase vanadium dioxide nanometer powder

A technology of vanadium dioxide nanometer and vanadium dioxide, which is applied in the field of ball milling to prepare VO2 powder, which can solve the problems of affecting product performance, not being easy to powder, increasing production costs, etc., achieving high production efficiency, short time, and energy saving Effect

Active Publication Date: 2019-10-18
蒋绪川
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, its process parameters are too many, and the prepared products are often accompanied by other heterogeneous phases and agglomeration, so it is not easy to directly obtain nanoscale VO 2 (M) Powder
VO is currently made by phase transition 2 Transformation of heterophase to monoclinic vanadium dioxide VO 2 (M), mainly achieved by high-temperature annealing under vacuum or inert atmosphere, but this method requires high-temperature heating and high energy consumption, which undoubtedly increases production costs. On the other hand, the product is easy to reunite after high-temperature annealing, which will also affect product performance. For example: the article (Inorg.Chem.Front., 2016, 3, 1035–1042|1039) mentions that VO prepared by hydrothermal annealing at 550°C under vacuum conditions 2 (D) Powder for 3 hours to obtain VO with a particle size above 500nm and serious agglomeration 2 (M) Powder

Method used

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  • Preparation method of monoclinic phase vanadium dioxide nanometer powder
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  • Preparation method of monoclinic phase vanadium dioxide nanometer powder

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Embodiment 1

[0037] A preparation method of monoclinic phase vanadium dioxide nanopowder, comprising the following steps:

[0038] (1) Hydrothermal preparation:

[0039] will V 2 o 5(1.001g) was added to 20mL of deionized water, then 1.5ml of concentrated sulfuric acid was added, stirred with a magnetic stirrer at 60-70°C for 10min, and then 0.520g of N 2 h 4 ·HO 2 Adjust the pH to 3-4 using sodium hydroxide and transfer to a Teflon-lined stainless steel autoclave. The autoclave was sealed and reacted at 230°C for 24 hours. Subsequently, the autoclave was slowly cooled to room temperature to obtain the product, which was washed twice with deionized water and once with ethanol to remove the residue, and dried at 80°C for 10 hours to obtain a powder Body, carry out X-ray diffraction (XRD) test, and with VO 2 (A) Standard card comparison, such as figure 1 As shown, the obtained powder is VO 2 (A) Powder.

[0040] (2) Ball milling treatment:

[0041] 1) 3.000g VO obtained by heating ...

Embodiment 2

[0046] A preparation method of monoclinic phase vanadium dioxide nanopowder, comprising the following steps:

[0047] (1) Hydrothermal preparation:

[0048] will V 2 o 5 Add 0.600g and 0.790g of oxalic acid into 40mL of deionized water. Stir for 1 h with a magnetic stirrer to obtain a blue transparent liquid, which is transferred to a polytetrafluoroethylene-lined stainless steel autoclave. The autoclave was sealed and reacted at 210° C. for 24 h, and then the autoclave was slowly cooled to room temperature. The product was obtained, washed three times by centrifugation with absolute ethanol, and the residue was removed, and vacuum-dried at 55°C for 12h to obtain a powder, which was tested by X-ray diffraction (XRD), and compared with VO 2 (B) Standard card comparison, such as figure 2 As shown, the obtained powder is VO 2 (B) Powder.

[0049] (2) Ball milling treatment:

[0050] 1) 1.123g VO obtained by heating step (1) multiple times 2 (B) The powder was mixed wit...

Embodiment 3

[0055] A preparation method of monoclinic phase vanadium dioxide nanopowder, comprising the following steps:

[0056] (1) Hydrothermal preparation:

[0057] will V 2 o 5 (0.8014g) was added to 20mL deionized water, stirred with a magnetic stirrer at 60-70°C for 10min, then added 0.5200gN 2 h 4 ·HO 2 Adjust the pH to 7-8 using sodium hydroxide and transfer to a Teflon-lined stainless steel autoclave. The autoclave was sealed and reacted at 260° C. for 24 h, and then the autoclave was slowly cooled to room temperature. Obtain the product, wash twice with deionized water, wash once with ethanol, remove the residue, dry at 80°C for 10h, obtain powder, carry out X-ray diffraction (XRD) test, and compare with VO 2 (D) Standard card comparison, such as image 3 As shown, the obtained powder is VO 2 (D) Powder.

[0058] (2) Ball milling treatment:

[0059] 1) 2.023g VO obtained by heating step (1) multiple times 2 (D) Powder, mixed with 2.345 g of butyric acid.

[0060] 2)...

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Abstract

The invention provides a preparation method of monoclinic phase vanadium dioxide nanometer powder, and belongs to the field of preparation of VO2 powder by a ball-milling method. The preparation method comprises the following steps that (1) vanadium dioxide powder is prepared by a hydrothermal method; (2) the vanadium dioxide powder prepared in the step (1) is mixed and stirred with a grinding aid; (3) the ingredients obtained by mixing in the step (2) are added to a grinding device, and grinding balls are added to perform grinding; and (4) abrasive obtained in the step (3) is washed and driedto obtain the monoclinic phase vanadium dioxide. According to the preparation method of the monoclinic phase vanadium dioxide nanometer powder, the monoclinic phase VO2 is prepared by the ball-milling method, phase transition of an impurity phase of the VO2 is promoted by mechanical force, and the particle size of materials is continuously reduced due to the grinding action in the continuous ball-milling process. The preparation method does not require heating, and energy consumption is reduced; and the phase transition can occur in a short time, the time is short, and the production efficiency is high.

Description

technical field [0001] The invention belongs to ball milling method for preparing VO 2 In the powder field, it specifically relates to a method for preparing monoclinic vanadium dioxide nanometer powder. Background technique [0002] In recent years, in order to reduce the energy consumption of indoor air conditioning in modern buildings, "smart windows" have received widespread attention. Smart windows can intelligently adjust the transmittance of light and heat through stimuli such as light, heat, and electricity. Therefore, they can be divided into photochromic smart windows, thermochromic smart windows, and electrochromic smart windows. [0003] Monoclinic vanadium dioxide VO 2 (M) It has excellent thermal discoloration performance. When the ambient temperature is higher than the phase transition temperature, it is in a metallic state, reflecting near-infrared light; when it is lower than the phase transition temperature, it is in an insulating state, allowing light to...

Claims

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Application Information

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IPC IPC(8): C01G31/02B82Y30/00
CPCB82Y30/00C01G31/02C01P2002/72
Inventor 蒋绪川王驰元徐慧妍聂永王程
Owner 蒋绪川
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