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Preparing method for vanadium oxide film

A technology of vanadium oxide and film layer, which is applied in the direction of coating, metal material coating process, ion implantation plating, etc., can solve the problem of limited improvement of phase transition temperature or thermal hysteresis curve shape, long preparation time of vanadium oxide film layer, film Layer structure design is limited and other issues, to shorten the heating annealing time, improve annealing production efficiency, shorten the effect of cooling time

Active Publication Date: 2016-08-17
GUANGZHOU INST OF ENERGY CONVERSION - CHINESE ACAD OF SCI
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  • Application Information

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Problems solved by technology

[0006] Through the research and analysis of the existing technology, the vanadium oxide film layer of the prior art generally has technical problems such as long preparation time, complicated production process, high cost and limited structure design of the film layer.
For this reason, the present invention provides a kind of preparation method of vanadium oxide film layer, to solve the problems existing in the prior art: annealing efficiency is low, phase change temperature or thermal hysteresis curve shape improvement is limited, process atmosphere cost is high

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  • Preparing method for vanadium oxide film
  • Preparing method for vanadium oxide film
  • Preparing method for vanadium oxide film

Examples

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Embodiment 1

[0039] A method for preparing a vanadium oxide film: provide a cleaned tempered glass substrate (G) with a thickness of 3 mm, enter a magnetron sputtering coating vacuum chamber to sputter to form a film at room temperature, and pass through relevant targets in sequence to form G / SiNx / VOx / SiNx film layer structure, send the coated substrate into the vacuum annealing furnace cavity, turn on the vacuum pump group to evacuate to 0.5Pa, fill in Ar gas, make the annealing protection atmosphere in the furnace vacuum to 150Pa, turn on the infrared The radiation lamp is heated, the annealing temperature is 500°C, and it is turned off after heating for 190s. When the temperature of the glass substrate in the vacuum annealing furnace drops to 50°C, the glass substrate is taken out. The obtained phase transition temperature characteristic curve of the vanadium oxide film is shown in figure 1 . Wherein the phase transition temperature is 49.5°C, the definition of the phase transition tem...

Embodiment 2

[0041] A kind of preparation method of vanadium oxide film layer, present embodiment is compared with embodiment 1, difference is: after coating film substrate is sent into vacuum annealing furnace, background vacuum degree is pumped to 10Pa, is filled with N 2 Atmosphere to annealing protection atmosphere vacuum to 150Pa, turn on the infrared radiation lamp to heat, the annealing temperature is 500°C, turn off after heating for 150s, take out the glass substrate in the vacuum annealing furnace when the temperature drops to 200°C, the obtained vanadium oxide film layer Phase transition temperature characteristic curve see figure 2 , wherein the phase transition temperature is 46°C, the thermal hysteresis curve is steeper than that of Example 1, and the temperature change during the heating phase transition process is about 25°C. At the same time, compared with Example 1 (annealing in an oxygen-free atmosphere), the annealing time of Example 2 is significantly shortened by 40s...

Embodiment 3

[0043] A method for preparing a vanadium oxide film layer. Compared with Example 2, this example differs in that: the background vacuum is evacuated to 300Pa and then annealed directly, the annealing temperature is 400°C, and the heating time is 480s. The phase transition temperature characteristic curve of the vanadium oxide film layer is shown in image 3 . Wherein the phase transition temperature is 55°C, the thermal hysteresis curve is steeper compared to Example 2, and the temperature change during the heating phase transition process is about 10°C. Compared with Example 2, the adjustment difference of the phase transition temperature reaches 9°C . Compared with Examples 2 and 3, for the same precursor film layer, the adjustment of the annealing process atmosphere and related parameters can achieve a relatively large adjustment of the phase transition temperature, and the shape of the thermal hysteresis curve also changes significantly.

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Abstract

The invention provides a preparing method for a vanadium oxide film. The preparing method comprises the steps that a vanadium oxide layer or a composite layer containing a vanadium oxide layer is deposited on the surface of a clean substrate; then, the substrate plated with a film is fed into a vacuum annealing furnace with a radiation modulator tube heating source for annealing treatment, wherein an annealing protection atmosphere in the vacuum annealing furnace is made of dualistic or polybasic mixed gas containing oxygen, the annealing protection atmosphere vacuum degree of the annealing environment protection atmosphere is larger than or equal to 10 Pa and smaller than or equal to 1000 Pa, the annealing temperature ranges from 400 DEG C to 700 DEG C, and the annealing time ranges from 30 s to 480 s; after annealing is finished, when the temperature of the substrate plated with the film is not lower than 200 DEG C, the substrate plated with the film is exposed in the atmospheric environment to be cooled. By regulating and controlling the preparing technology, the crystal grain size, the microstructure and other aspects of the vanadium oxide film in the annealing process are regulated and controlled, and finally the single-layer vanadium oxide film with the phase-change feature in a wider range is finally obtained.

Description

technical field [0001] The present invention relates to the field of energy-saving and environment-friendly materials, in particular to a vanadium oxide film with phase change characteristics, and in particular to a method for significantly improving film preparation efficiency through annealing process setting and regulation, obtaining films with different phase change characteristic curves and reducing process costs method. Background technique [0002] VO 2 As a new type of energy-saving material, its phase transition temperature is 68°C. When the ambient temperature is higher than its phase transition temperature, VO 2 It has a tetragonal crystal structure, has metal phase characteristics, and can reflect infrared rays; when the ambient temperature is lower than its phase transition temperature, VO 2 It has a monoclinic crystal structure, has semiconductor phase characteristics, and can pass through infrared rays. VO 2 The film layer can undergo a phase change under...

Claims

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Application Information

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IPC IPC(8): C23C14/08C23C14/58C23C14/34C23C14/24
CPCC23C14/0021C23C14/0036C23C14/08C23C14/5806
Inventor 詹勇军徐刚肖秀娣程浩亮
Owner GUANGZHOU INST OF ENERGY CONVERSION - CHINESE ACAD OF SCI
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