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Liquid-phase preparation method of high-oriented vanadium dioxide film

A vanadium dioxide, high-orientation technology, applied in liquid chemical plating, metal material coating process, coating, etc., can solve the problems of no growth orientation of the film, complicated equipment and operation, increased production cost, etc., and achieve macro phase Significant variable characteristics, low cost of film production, and good growth orientation

Active Publication Date: 2014-09-24
ANHUI UNIVERSITY OF ARCHITECTURE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In view of the above goals, the current technology mainly has the following problems: (1) The sintering process requires gas protection, including reducing gas, inert gas, and the mixed gas of the two (CN201010126863.5); this requires additional gas sources, The gas circuit and gas mixing device make the equipment and operation more complicated, and also increase the production cost; (2) The vacuum requirement is too high during sintering in a vacuum environment, and the obtained VO 2 Lack of orientation; VO 2 The film is usually some vanadium oxide before sintering, and VO is prepared by vacuum sintering 2 Requires a vacuum greater than 10 -2 Pa (Surface & Coatings Technology, 201, 2007, 6772-6776), also reported as 1-2Pa (Applied Surface Science, 191, 2002, 176-180); overall, the prepared VO 2 The purity is generally not high, there are other phases of vanadium oxide in the X-ray diffraction spectrum, and the film has no growth orientation

Method used

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  • Liquid-phase preparation method of high-oriented vanadium dioxide film
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Examples

Experimental program
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Effect test

Embodiment 1

[0029] The vanadium dioxide film was prepared at a sintering temperature of 430° C., a heat preservation of 4 hours, and a vacuum of 5 Pa.

[0030] (1) Preparation of precursor solution:

[0031] Take 0.8 g of vanadyl triisopropoxide, dissolve it in 50 ml of isopropanol, add 1.3 g of glacial acetic acid dropwise to form a mixed solution, and stir with a glass rod for 10 minutes to obtain a vanadium dioxide film precursor.

[0032] (2) Clean the substrate:

[0033] Select the sapphire wafer as the substrate, place it in acetone, ethanol and deionized water for ultrasonic cleaning for 5 minutes, and finally dry it with nitrogen gas for later use.

[0034] (3) Precursor solution coating:

[0035] Select the precursor solution obtained in the above step (1), and use a homogenizer to spin coat the coating; the homogenization process is: first, the low speed is 200 rpm, and it is kept for 9 seconds; then the high speed is 2000 rpm, and it is kept for 20 seconds; then, the obtained...

Embodiment 2

[0041] The vanadium dioxide film was prepared at a sintering temperature of 530° C., a heat preservation of 7 hours, and a vacuum of 4 Pa.

[0042] (1) Preparation of precursor solution:

[0043] Take 1.9 g of vanadyl triisopropoxide, dissolve it in 50 ml of isopropanol, add 6.3 g of glacial acetic acid dropwise to form a mixed solution, and stir with a glass rod for 10 minutes to obtain a vanadium dioxide film precursor.

[0044] (2) Clean the substrate:

[0045] Select the sapphire wafer as the substrate, place it in acetone, ethanol and deionized water for ultrasonic cleaning for 5 minutes, and finally dry it with nitrogen gas for later use.

[0046] (3) Precursor solution coating:

[0047] Select the precursor solution obtained in the above step (1), and use a homogenizer to spin coat the coating; the homogenization process is: first, the low speed is 200 rpm, and it is kept for 9 seconds; Vanadium precursor films.

[0048] (4) Vanadium dioxide film sintering:

[0049] ...

Embodiment 3

[0053] The vanadium dioxide film was prepared at a sintering temperature of 590° C., a heat preservation time of 10 hours, and a vacuum degree of 8 Pa.

[0054] (1) Preparation of precursor solution:

[0055] Take 4.5 g of vanadyl triisopropoxide, dissolve it in 50 ml of isopropanol, add 25 g of glacial acetic acid dropwise to form a mixed solution, and stir with a glass rod for 10 minutes to obtain a vanadium dioxide film precursor.

[0056] (2) Clean the substrate:

[0057] Select the sapphire wafer as the substrate, place it in acetone, ethanol and deionized water for ultrasonic cleaning for 5 minutes, and finally dry it with nitrogen gas for later use.

[0058] (3) Precursor solution coating:

[0059] Select the precursor solution obtained in the above step (1), and use a homogenizer to spin-coat the coating; the homogenization process is: first at a low speed of 200 rpm, and hold for 9 seconds; then at a high speed of 2000 rpm, and hold for 20 seconds; then, the obtaine...

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Abstract

The invention discloses a liquid-phase preparation method of a high-oriented vanadium dioxide film, belonging to the field of chemical function materials. The preparation method comprises the following steps: preparing precursor liquid by taking triisopropoxyvanadium oxide as solute, coating a sapphire substrate with the obtained precursor liquid to prepare a precursor film, and finally sintering the precursor film in a vacuum environment. According to the preparation method, the vanadium dioxide film is prepared by controlling vacuum sintering conditions on the basis of a liquid-phase method, the obtained film is good in growth orientation, the phase change temperature of the film is about 60 DEG C, and the change of electrical resistivity before and after the phase change is more than three orders of magnitude; in addition, the preparation process is simple and suitable for large-range popularization.

Description

technical field [0001] The invention relates to a liquid-phase preparation method of a highly oriented vanadium dioxide film, which belongs to the field of chemical functional materials. Background technique [0002] Vanadium dioxide (VO 2 ) is a strongly correlated electronic material, the bulk VO 2 A structural mutation from a high-temperature metal phase (rutile R phase) to a low-temperature semiconductor phase (monoclinic M phase) occurs around 68 °C, accompanied by a huge change in its resistivity and infrared transmittance, and the phase transition process is reversible. Since the electrical, magnetic, and optical properties of this material have great changes before and after the phase transition, it has a wide range of application requirements in photoelectric switch materials, storage media, and smart window materials. [0003] VO 2 Thin films can undergo repeated phase-change cycles without breaking, so they have broader application prospects. High orientatio...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C23C18/12
Inventor 郭玉献徐海燕童彬
Owner ANHUI UNIVERSITY OF ARCHITECTURE
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