Preparation method of vanadium dioxide film

A vanadium dioxide and thin film technology, applied in metal material coating process, vacuum evaporation coating, coating and other directions, can solve the problems of high cost, complex method, complex preparation process, etc., to ensure crystallinity, high infrared mutation Amplitude, easy operation effect

Active Publication Date: 2022-02-18
JILIN UNIV
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Problems solved by technology

In general, there are more than a dozen different vanadium-molybdenum oxides within a narrow vanadium-to-oxygen ratio range, so the parameters need to be controlled very precisely. The current preparation methods of vanadium dioxide thin films mainly include hydrothermal method, sol Gel method or pulsed laser deposition method, etc., and these methods are difficult to achieve a balance between cost and quality, either the cost is too high and the method is complicated, or the quality of film formation cannot be guaranteed, and if you want to achieve a relatively good optical performance, often need to carry out The design of composite films such as buffer layer and anti-reflection layer, and common substrates generally need to choose such as Si 3 N 4 , ZnO, TiO 2 Or sapphire substrate, etc., for example, the prior art "The effect of TiO 2 buffer layer thickness on the thermochromic properties of VO 2 thin-film fabricated by high density plasma source[Japanese Journal of Applied Physics 60, SAAB04(2021)]”reported that the optical properties of vanadium dioxide films were improved by introducing a titanium dioxide buffer layer, although it was different from that deposited under the same conditions The optical performance of the film in the infrared band has been improved by about 10%
However, due to the setting of the buffer layer in this method, the preparation cost is greatly increased to a certain extent, and the preparation process is also relatively complicated.

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preparation example Construction

[0033] The invention provides a kind of preparation method of vanadium dioxide film, comprises the following steps:

[0034] In a vacuum reaction chamber, radio frequency magnetron sputtering is used to sputter vanadium dioxide on the surface of the substrate, and the temperature of the substrate is increased to perform in-situ annealing to obtain a vanadium dioxide film; there is no gap between the substrate and the vanadium dioxide film. set the buffer layer;

[0035] The conditions of the radio frequency magnetron sputtering are: the temperature of the substrate is 250-300° C.; the flow rate of argon into the reaction chamber is 0.8 sccm; the flow rate of oxygen into the reaction chamber is 40 sccm; the pressure of the reaction chamber is 0.8 Pa; sputtering time is 15-20min; sputtering power is 95W;

[0036] The temperature of the in-situ annealing is 460-520°C, and the holding time is 200s;

[0037] The time for heating up to the temperature of the in-situ annealing is ≤...

Embodiment 1

[0059] The sapphire substrate was ultrasonically cleaned with acetone, absolute ethanol and high-purity deionized water for 15 minutes, then dried with a nitrogen gun and placed in a sputtering chamber;

[0060] Pump the pressure in the sputtering chamber to 8×10 through a mechanical pump -4 Pa, raise the substrate temperature to 270°C, control oxygen and argon to flow into the reaction chamber at a flow rate of 0.8sccm and 40sccm through the gas flow meter, and control the sputtering pressure to 0.8Pa through the gate valve; use the baffle Put on the target, turn on the sputtering power supply for pre-sputtering (sputtering power is 95W), to remove impurities on the surface of the target; remove the baffle, set the distance between the target and the substrate to 80mm, the substrate speed to 25rad / s, radio frequency The power is 95W, after deposition for 16min, turn off the gas flowmeter, heat the substrate temperature to 490°C for 7s, keep it warm for 200s, and cool it to ro...

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Abstract

The invention relates to the technical field of phase change materials, in particular to a preparation method of a vanadium dioxide film. The preparation method provided by the invention comprises the following steps: sputtering vanadium dioxide on the surface of a substrate in a vacuum reaction chamber by adopting a radio frequency magnetron sputtering method, raising the temperature of the substrate, and carrying out in-situ annealing to obtain a vanadium dioxide film; wherein no buffer layer is arranged between the substrate and the vanadium dioxide film; the conditions of the radio frequency magnetron sputtering are as follows: the temperature of the substrate is 250-300 DEG C; the flow rate of argon introduced into the reaction chamber is 0.8 sccm; the flow rate of oxygen introduced into the reaction chamber is 40 sccm; the air pressure of the reaction chamber is 0.8 Pa; the sputtering time is 15 to 20 minutes; the sputtering power is 95W; the in-situ annealing temperature is 460-520 DEG C, and the heat preservation time is 200 s; and the time for raising the temperature to the in-situ annealing temperature is less than or equal to 7s. According to the preparation method, the vanadium dioxide thin film with good optical performance can be obtained on the premise that a buffer layer is not arranged.

Description

technical field [0001] The invention relates to the technical field of phase change materials, in particular to a method for preparing a vanadium dioxide thin film. Background technique [0002] In 1959, F.J.Morin (MorinF.J.Oxides which show ametal-to-insulatortransition at the Neel temperature[J].Physical Review Letters,1959,3(1):34.) first discovered and studied the phase change material dioxide MIT (metal-semiconductor) phase transition properties of vanadium. In the following decades, as a typical phase change material, vanadium dioxide has been studied in depth by a large number of scholars. Vanadium dioxide is a metal oxide with phase change properties. Under normal circumstances, its phase transition temperature is around 68°C. And the vanadium dioxide in the film state can realize the phase transition from the low-temperature monoclinic rutile structure to the high-temperature tetragonal rutile structure before and after the phase transition temperature. This proce...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C23C14/35C23C14/02C23C14/08C23C14/54C23C14/58
CPCC23C14/0036C23C14/083C23C14/5806C23C14/021C23C14/54C23C14/548
Inventor 田宏伟刘鸿旭杨俊于陕升
Owner JILIN UNIV
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