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A method for preparing vanadium dioxide by dual temperature zone reduction method

A technology of vanadium dioxide and reduction method, which is applied in the direction of vanadium oxide, etc., can solve the problems of cumbersome preparation process, difficulty in controlling the stoichiometric ratio of vanadium dioxide powder, and limited preparation amount, so as to facilitate the collection of samples, crystal phases and particles The effect of controllable diameter and simple steps

Active Publication Date: 2015-08-19
SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The preparation process of these methods is relatively cumbersome, and some preparation methods also need to add organic solvents, and the stoichiometric ratio of the final vanadium dioxide powder is difficult to control and the preparation amount is limited.

Method used

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  • A method for preparing vanadium dioxide by dual temperature zone reduction method
  • A method for preparing vanadium dioxide by dual temperature zone reduction method
  • A method for preparing vanadium dioxide by dual temperature zone reduction method

Examples

Experimental program
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Effect test

Embodiment 1

[0032]Commercial vanadium pentoxide is used as raw material, and aluminum is a highly active reducing metal. They are placed in different heating zones in a closed tube furnace. After the whole system is evacuated to 0.1Pa, the aluminum and vanadium pentoxide are heated to 800 °C and 400 °C, turn off the heating power after 3 hours of reaction. After the sample is cooled, vanadium dioxide is obtained.

Embodiment 2

[0034] Using self-made vanadium pentoxide nanopowder as raw material (Ding SJ, Liu ZQ, Li DZ, Zhao W, Huang FQ, ACS Applied Materials & Interfaces. 2013, 5, 1630–1635), aluminum is a highly active reducing metal, put Put them into different heating zones in a closed tube furnace, vacuumize the whole system to 0.1Pa, heat the aluminum and vanadium pentoxide to 850°C and 200°C respectively, and turn off the heating power after 6 hours of reaction. After the sample is cooled, vanadium dioxide nanopowder is obtained. figure 2 and image 3 The TEM images of the vanadium pentoxide powder as the raw material and the vanadium dioxide powder obtained are shown respectively. It can be seen from the figure that the morphology of the vanadium dioxide powder can be kept consistent with the precursor vanadium pentoxide powder or Close, its particle size is 10-20nm.

Embodiment 3

[0036] Commercial vanadium pentoxide is used as raw material, and magnesium is a highly active reducing metal. They are placed in different heating zones in a closed tube furnace. After the whole system is evacuated to 0.1Pa, aluminum and vanadium pentoxide are heated to 750 °C and 450 °C, turn off the heating power after 5 hours of reaction. After the sample is cooled, vanadium dioxide is obtained.

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Abstract

The invention relates to a method of preparing vanadium dioxide by a double-temperature area reduction process. The method comprises the following steps: placing vanadium pentoxide and high-activity metal into a sealed system with negative pressure by spacing a certain distance; respectively heating vanadium pentoxide and the high-activity metal to different temperatures for thermally treating for determined time, so that oxygen partial pressure in the sealed system is lower than balanced oxygen partial pressure of vanadium pentoxide and vanadium pentoxide is reduced to obtain vanadium dioxide, wherein the high-activity metal is heated to a first temperature and vanadium pentoxide is heated to a second temperature lower than the first temperature; the heated high-activity metal reacts with oxygen gas in the sealed system to lower the oxygen partial pressure in the sealed system, so that the oxygen partial pressure of the sealed system is lower than the balanced oxygen partial pressure of vanadium pentoxide. The vanadium dioxide obtained by the method disclosed by the invention is controllable in crystalline phase and grain size, and has a morphology which is kept consistent or similar to that of a vanadium pentoxide precursor.

Description

technical field [0001] The invention relates to a method for preparing vanadium dioxide powder and film, in particular to a method for preparing vanadium dioxide powder and film with crystal phase and particle size controllable by assisting reduction of vanadium dioxide with dual-temperature zone high-activity metals. Background technique [0002] Facing the global energy crisis, energy-saving buildings are attracting more and more attention, but the current buildings are largely in the form of glass curtain walls, so how to control the heat exchange of glass windows is crucial to the overall energy saving. High-performance dimming film materials, such as low-e glass coatings and color-changing coatings, will shine in this field, because they can selectively transmit and reflect sunlight in a specific wavelength range, thereby Play the purpose of maintaining indoor temperature and energy saving. Among them, vanadium dioxide (VO 2 ) is a promising thermochromic material in ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G31/02
Inventor 黄富强刘战强汪宙
Owner SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI
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