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A liquid phase preparation method of highly oriented vanadium dioxide film

A vanadium dioxide, high-orientation technology, applied in liquid chemical plating, metal material coating process, coating and other directions, can solve the problems of no growth orientation of the film, complicated equipment and operation, increase production cost, etc., and achieve a macroscopic phase. The effect of remarkable change characteristics, low film production cost and good growth orientation

Active Publication Date: 2017-01-25
ANHUI UNIVERSITY OF ARCHITECTURE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

For 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 (CN201010126663.5); this requires increasing the gas source, 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 1-2 Pa (Applied Surface Science, 191, 2002, 176-160); 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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  • A liquid phase preparation method of highly oriented vanadium dioxide film
  • A liquid phase preparation method of highly oriented vanadium dioxide film
  • A liquid phase preparation method of highly oriented vanadium dioxide film

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] 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.

[0025] (1) Preparation of precursor solution:

[0026] Take 0.6 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.

[0027] (2) Clean the substrate:

[0028] 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.

[0029] (3) Precursor solution coating:

[0030] Select the precursor solution obtained in the above step (1), and use a homogenizer to spin coat the film; the homogenization process is: first at a low speed of 200 revolutions / minute, and keep for 9 seconds; then at a high speed of 2000 revolutions / second, and keep for 20 seconds; th...

Embodiment 2

[0036] 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.

[0037] (1) Preparation of precursor solution:

[0038] 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.

[0039] (2) Clean the substrate:

[0040]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.

[0041] (3) Precursor solution coating:

[0042] 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, for 9 seconds; then at a high speed of 2000 rpm, for 20 seconds, to obtain the Vanadium precursor films.

[004...

Embodiment 3

[0048] 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 6 Pa.

[0049] (1) Preparation of precursor solution:

[0050] 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.

[0051] (2) Clean the substrate:

[0052] 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.

[0053] (3) Precursor solution coating:

[0054] Select the precursor solution obtained in the above step (1), and use a homogenizer to spin coat the film; the homogenization process is: first at a low speed of 200 revolutions / minute, and keep for 9 seconds; then at a high speed of 2000 revolutions / second, and keep for 20...

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Abstract

The invention discloses a liquid-phase preparation method of a highly oriented vanadium dioxide film, which belongs to the field of chemical functional materials. In the preparation method, vanadyl triisopropoxide is used as a solute to prepare a precursor solution, the obtained precursor solution is coated on a sapphire substrate to prepare a precursor film, and finally the precursor film is fired in a vacuum environment. The present invention prepares vanadium dioxide films by controlling vacuum sintering conditions on the basis of the liquid phase method. The obtained films all have good growth orientation, the phase transition temperature is about 60°C, and the resistivity changes before and after the phase transition within three above the order of magnitude; and the preparation process is simple, which is suitable for large-scale promotion.

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, and 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 66 °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 orientat...

Claims

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Application Information

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