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Inorganic sol-gel preparation method of vanadium dioxide film

A technology of vanadium dioxide and inorganic sol, which is applied in the field of material chemistry, can solve the problems of high equipment requirements and temperature exceeding the heat resistance limit of ordinary glass, and achieve the effects of low cost investment, excellent optical control performance, and reduced energy consumption

Inactive Publication Date: 2015-12-30
WUHAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Y.Long et al. used high vacuum (1.0×10 -4 pa), thermal decomposition at a high temperature of 750°C, but this method requires too much equipment, and the temperature exceeds the heat resistance limit of ordinary glass

Method used

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  • Inorganic sol-gel preparation method of vanadium dioxide film
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  • Inorganic sol-gel preparation method of vanadium dioxide film

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] (1) Preparation of vanadium sol: take 0.3g vanadium pentoxide, dissolve in 30ml mass fraction of 30% hydrogen peroxide, fully stir and react for 40min, let stand for 1h, then seal with plastic wrap and store at room temperature for 24h. That is, a stable pentavalent vanadium sol is obtained.

[0045] (2) Substrate cleaning: Quartz glass was selected as the substrate, and deionized water, acetone and ethanol were used to ultrasonically clean for 20 minutes in sequence, and then placed in an oven at 80°C to dry in order to prepare for coating.

[0046] (3) Spin coating film formation: select the sol obtained in the above step (1), and use a spin coater to coat the film. First low speed 500r / min, keep 9s, then high speed 3000r / min, keep 30s. The spin-coated film was dried in an oven at 80°C for 10 min, and spin-coated only once.

[0047] (4) Annealing: put the dried film into a tube furnace, and first evacuate to 2.0×10 3 pa, and then feed ammonia and argon respectively...

Embodiment 2

[0056] (1) The preparation of vanadium sol: take by weighing 0.6g metal vanadium powder, be dissolved in 30ml mass fraction and be 15% hydrogen peroxide, after fully stirring and reacting for 60min, let stand for 2h, then seal with plastic wrap and store at room temperature for 20h, namely A stable pentavalent vanadium sol was obtained.

[0057] (2) Substrate cleaning: select soda-lime-silica glass as the substrate, ultrasonically clean it with deionized water, acetone and ethanol in sequence for 20 minutes, and put it in an oven at 80°C to dry in order to prepare for coating.

[0058] (3) Spin coating film formation: select the sol obtained in the above step (1), and use a spin coater to coat the film. First low speed 500r / min, keep 9s, then high speed 3000r / min, keep 30s. The spin-coated film was dried in an oven at 60°C for 20 min, and spin-coated only once.

[0059] (4) Annealing: put the dried film into a tube furnace, and first evacuate to 1.0×10 2 pa, and then feed a...

Embodiment 3

[0062] (1) The preparation of vanadium sol: take by weighing 0.5g vanadium pentoxide, be dissolved in 30ml mass fraction and be 6% hydrogen peroxide, after fully stirring and reacting for 50min, leave standstill for 1h, then seal with plastic wrap and store at room temperature for 12h, That is, a stable pentavalent vanadium sol is obtained.

[0063] (2) Substrate cleaning: Quartz glass was selected as the substrate, and deionized water, acetone and ethanol were used to ultrasonically clean for 20 minutes in sequence, and then placed in an oven at 80°C to dry in order to prepare for coating.

[0064] (3) Spin coating film formation: select the sol obtained in the above step (1), and use a spin coater to coat the film. First low speed 500r / min, keep 9s, then high speed 3000r / min, keep 30s. The spin-coated film was dried in an oven at 70°C for 15 minutes, and spin-coated only once.

[0065] (4) Annealing: put the dried film into the tube furnace, first vacuum to 3.0×10 3 pa, a...

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Abstract

The invention belongs to the technical field of material chemistry and relates to an inorganic sol-gel preparation method of a vanadium dioxide film. The inorganic sol-gel preparation method comprises 1, dissolving vanadium powder or vanadic anhydride powder in hydrogen peroxide, carrying out stirring, carrying out standing, and carrying out room temperature preservation to obtain pentavalent vanadium sol, and 2, coating a substrate with the sol obtained by the step 1 and carrying out weak-reduction one-step annealing in an inert gas protective atmosphere to obtain the vanadium dioxide film. The one-step annealing method solves the problem that the existing pentavalent vanadium sol film preparation method needs hydrogen pre-reduction and a complicated two-step annealing process or harsh conditions of high-vacuum and high-temperature thermal decomposition, has an annealing temperature in a common glass bearing range, has low requirements on an annealing furnace and further reduces a cost. The vanadium dioxide film has excellent optical regulation and control performances, the highest visible light transmittance rate of 70%, the highest infrared adjusting performance of 60% and a wide application prospect in the field of a photoelectric functional material.

Description

technical field [0001] The invention belongs to the technical field of material chemistry, and in particular relates to an inorganic sol-gel preparation method for preparing a vanadium dioxide film with an adjustable phase transition temperature by annealing in a mixed atmosphere. Background technique [0002] Since Morin FJ discovered vanadium dioxide has metal-semiconductor phase transition properties in 1959, research based on this substance has always been a hot spot in the material science community. Specifically, vanadium dioxide will undergo a phase transition when the normal temperature rises to around 68°C, from a low-temperature monoclinic phase to a high-temperature tetragonal rutile phase. The phase transition process is accompanied by 4-5 orders of magnitude changes in resistivity and Optical transmittance mutation, and can be completed in nanoseconds, phase change is reversible, etc. This series of excellent characteristics makes it widely used, and one of the...

Claims

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Application Information

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IPC IPC(8): C03C17/23C01G31/02
Inventor 赵修建张文元陶海征万美南
Owner WUHAN UNIV OF TECH
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