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Monoclinic phase vanadium dioxide thin film and preparation method thereof

A technology of vanadium oxide thin film and vanadium dioxide, which is applied in metal material coating process, vacuum evaporation plating, coating, etc., can solve the problems of harsh experimental conditions, high complexity, difficult control, etc., and save time and equipment The effect of cost of use

Active Publication Date: 2021-12-07
UNIV OF ELECTRONICS SCI & TECH OF CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] However, the vanadium-oxygen system shows high complexity due to the fact that the transition metal element vanadium can form a variety of oxides, including VO 2 (VO 2 (M), VO 2 (A), VO 2 (B)), V n o 2n-1 (VO, V 2 o 3 , V 4 o 7 , V 5 o 9 , V 7 o 13 , V 8 o 15 etc.) and V n o 2n+1 (V 2 o 5 , V 3 o 7 , V 4 o 9 , V 6 o 13 ), or part of V 4+ Ions are oxidized to give +4 / +5 mixed valence state of VO 2 / V 2 o 5 mixed product
In the preparation of VO by reactive magnetron sputtering 2 (M), V in the difficult-to-regulate product 4+ valence state, it is easy to get mixed valence state of vanadium oxide, and want to get pure monoclinic phase VO 2 , the experimental conditions will be relatively harsh, such as oxygen-enriched environment, etc.

Method used

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  • Monoclinic phase vanadium dioxide thin film and preparation method thereof
  • Monoclinic phase vanadium dioxide thin film and preparation method thereof
  • Monoclinic phase vanadium dioxide thin film and preparation method thereof

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preparation example Construction

[0037] The invention provides a method for preparing a monoclinic phase vanadium dioxide film, comprising the steps of:

[0038] (1) Deposit amorphous vanadium oxide film on the substrate by reactive magnetron sputtering in advance; step (1) use a metal vanadium target with a purity of 99.99% as the sputtering source, and deposit amorphous vanadium oxide film at room temperature by reactive magnetron sputtering method. In the crystal vanadium oxide film, the atomic percentage of vanadium in the amorphous vanadium oxide film is 30%-40%, and the rest is oxygen element.

[0039] Specifically include the following steps:

[0040] ①Place the quartz substrate at 2.5×10 -2 Pa-3.2×10 -3 Pa vacuum environment;

[0041]②Under the pure Ar working pressure of 6Pa-15Pa, pre-sputter the pure vanadium metal target at room temperature for 10-20 minutes to remove the surface oxide layer;

[0042] ③ Next, use an atmosphere with an oxygen / argon flow ratio of 1:40-1:65 and a working pressure ...

Embodiment 1

[0052] This embodiment provides a method for preparing a monoclinic phase vanadium dioxide film, comprising the following steps:

[0053] (1) clamp the cleaned quartz substrate with clean tweezers and dry it with 99.99% nitrogen gas and put it into the substrate holder; -2 After the basic vacuum pressure of Pa, turn on the substrate rotating power supply; open the argon gas valve, and after the gas pressure stabilizes, pre-sputter the metal V target with a purity of 99.99% at room temperature for 10 minutes at a pure Ar working pressure of 6Pa to remove surface oxide layer; then, using an atmosphere with an oxygen / argon flow ratio of 1:40 and a working pressure of 0.8Pa, deposit an amorphous vanadium oxide film with a thickness of 50nm on a quartz substrate at room temperature; after sputtering, wait for the target Cool down for 60 minutes, wait for the sputtering cathode to cool down naturally, and take out the deposited amorphous vanadium oxide film;

[0054] (2) The metal ...

Embodiment 2

[0058] This embodiment provides a method for preparing a monoclinic phase vanadium dioxide film, comprising the following steps:

[0059] (1) clamp the cleaned quartz substrate with clean tweezers and put it into the substrate rack with a purity of 99.99% nitrogen; -3 After the basic vacuum pressure of Pa, turn on the substrate rotating power supply; open the argon gas valve, and after the gas pressure stabilizes, pre-sputter the metal V target with a purity of 99.99% at room temperature for 10 minutes at a working pressure of pure Ar of 10 Pa to remove Surface oxide layer; then, using an atmosphere with an oxygen / argon flow ratio of 1:56 and a working pressure of 1.2Pa, deposit an amorphous vanadium oxide film with a thickness of 100nm on a quartz substrate at room temperature; after sputtering, wait for the target The temperature was lowered for 60 minutes, and the deposited amorphous vanadium oxide film was taken out after waiting for the sputtering cathode to cool naturall...

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Abstract

The invention provides a monoclinic phase vanadium dioxide thin film and a preparation method thereof. The preparation method comprises the following steps: (1) depositing an amorphous vanadium dioxide thin film on a substrate through reactive magnetron sputtering in advance; (2) depositing a hafnium oxide thin film on the amorphous vanadium oxide thin film obtained in the step (1) by utilizing reactive magnetron sputtering again to obtain a double-layer thin film; and (3) preparing the monoclinic phase vanadium dioxide thin film from the double-layer thin film obtained in the step (2) in a muffle furnace through a rapid annealing process. Raman spectrum Raman analysis proves that the material of the vanadium oxide thin film prepared by the method is in a monoclinic phase. The reactive magnetron sputtering method disclosed by the invention is easy to realize through the existing sputtering equipment and has low technological requirements on the equipment. According to the rapid annealing process, vacuum and other atmosphere environments do not need to be provided, rapid annealing is directly conducted in the air atmosphere, and compared with traditional vacuum pure atmosphere environment annealing, the annealing mode can save a large amount of time and equipment use cost.

Description

technical field [0001] The invention relates to the preparation of a monoclinic vanadium dioxide film, in particular to a method for rapidly preparing a monoclinic vanadium dioxide film and the obtained monoclinic vanadium dioxide film. Background technique [0002] Vanadyl oxide is a very important class of materials with intelligent properties. Changes in ambient temperature will cause changes in the crystal structure, electric domain structure, and magnetic structure of the material, resulting in large changes in physical properties. Especially monoclinic vanadium dioxide (VO 2 (M)) is subject to people's special attention. [0003] In 1959, F.J.Morin was the first to discover that the monoclinic phase vanadium dioxide was formed at 68°C (T MIT ) can undergo a reversible phase transition (IMT) phase transition between an insulator state and a metallic state, and its crystal structure has achieved a low-temperature monoclinic phase (M) structure to a high-temperature rut...

Claims

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Application Information

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IPC IPC(8): C23C14/08C23C14/35C23C14/58
CPCC23C14/083C23C14/352C23C14/5806C23C14/0036
Inventor 平依瑶顾德恩周鑫王涛高靖
Owner UNIV OF ELECTRONICS SCI & TECH OF CHINA