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High-temperature self-transformation amorphous/nanocrystalline high-entropy oxide film, preparation method and application

An oxide film and nanocrystal technology, applied in the field of protective coatings, achieves the effects of rich structure-activity relationship regulation space, excellent mechanical properties, and good oxygen barrier effect.

Active Publication Date: 2021-05-25
ZHENGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The crystallization process of amorphous oxides at higher temperatures is also affected by the high-entropy effect, but no one has reported high-entropy nanocrystalline materials grown in amorphous confinement

Method used

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  • High-temperature self-transformation amorphous/nanocrystalline high-entropy oxide film, preparation method and application
  • High-temperature self-transformation amorphous/nanocrystalline high-entropy oxide film, preparation method and application
  • High-temperature self-transformation amorphous/nanocrystalline high-entropy oxide film, preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] The preparation of Zr-Cr-Nb-Al-Fe(O) oxide film, the steps are as follows:

[0035] (1) Cut and combine Zr-Cr-Nb into a new sputtering target, Al-Fe into another new sputtering target, and use the two combined targets as sputtering targets; use single crystal The silicon wafer was used as the coating substrate, and the substrate was ultrasonically treated with acetone, alcohol, and deionized water for 20 minutes, and then dried with a high-purity nitrogen air gun for later use; when the vacuum degree of the chamber reached 5×10 -4 Start to deposit at around mbar;

[0036] (2) Pre-sputtering: The sputtering target material cut and combined by Zr-Cr-Nb is connected to the target position connected to the direct current (DC) power supply. The sputtering target material cut and assembled by Al-Fe is connected to the target position connected to the radio frequency (RF) power supply, and the air pressure in the chamber reaches 5×10 -4 When it is below Pa, open the process...

Embodiment 2

[0040] The preparation of Zr-Cr-Nb-Al-Fe-Si(O) amorphous nanocrystalline oxide film, the steps are as follows:

[0041] (1) Combine Zr-Cr-Nb cutting into a new sputtering target, Al-Fe-Si cutting into another new sputtering target, and the two combined targets as sputtering targets; The crystalline silicon wafer was used as the coating substrate, and the substrate was ultrasonically treated with acetone, alcohol, and deionized water for 20 minutes, and then dried with a high-purity nitrogen air gun for later use; when the vacuum degree of the chamber reached 5×10 -4 Start to deposit at around mbar;

[0042] (2) Connect the sputtering target formed by Zr-Cr-Nb cutting and combination to the target position connected to the direct current (DC) power supply. The sputtering target material cut and combined by Al-Fe-Si is connected to the target position connected to the radio frequency (RF) power supply. The air pressure in the chamber reaches 5×10 -4 When it is below Pa, open ...

Embodiment 3

[0046] The preparation of Zr-Cr-Nb-Al-Fe-Si(O) amorphous nanocrystalline oxide film, the steps are as follows:

[0047] (1) Combine Zr-Cr-Nb cutting into a new sputtering target, Al-Fe-Si cutting into another new sputtering target, and the two combined targets as sputtering targets; The crystalline silicon wafer was used as the coating substrate, and the substrate was ultrasonically treated with acetone, alcohol, and deionized water for 20 minutes, and then dried with a high-purity nitrogen air gun for later use; when the vacuum degree of the chamber reached 5×10 -4 Start to deposit at around mbar;

[0048] (2) Pre-sputtering: The sputtering target material cut and combined by Zr-Cr-Nb is connected to the target position connected to the direct current (DC) power supply. The sputtering target material cut and combined by Al-Fe-Si is connected to the target position connected to the radio frequency (RF) power supply. The air pressure in the chamber reaches 5×10 -4 When it i...

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Abstract

The invention provides a high-temperature self-transformation amorphous / nanocrystalline high-entropy oxide thin film, a preparation method and application. The preparation method comprises the following steps that (1) a zirconium-based multi-element target material is cut and combined into a sputtering target material A, an Al-based multi-element target material is cut and combined into a sputtering target material B, the sputtering target material A is connected with a direct-current power source, the sputtering target material B is connected with a radio-frequency power source, and a high-entropy metal glass film is deposited by adopting a co-sputtering method after pre-sputtering; and (2) the obtained high-entropy metal glass film is placed in a muffle furnace, and calcining is carried out to obtain the amorphous / nanocrystalline high-entropy oxide film. The high-entropy thin film prepared through the method gradually achieves in-situ transformation at the high temperature, uniform and compact high-entropy oxide is formed, and cracks and coating failure are avoided. The high mixing entropy enhances the intersolubility among the elements and inhibits the formation of a single compound. Meanwhile, due to high interface energy and dynamic obstacles (slow kinetics) of atomic diffusion in the crystallization process, an amorphous / nanocrystalline system can stably exist.

Description

technical field [0001] The invention relates to the field of protective coatings, in particular to a high-temperature self-transformation amorphous / nanocrystalline high-entropy oxide film, a preparation method and an application. Background technique [0002] For the special environment of zirconium alloy cladding materials, neutron economy, stability, compactness and radiation resistance should be considered. The structural characteristics of the coating itself and the coordination of physicochemical properties between the coating and the substrate are crucial. The coatings currently researched and designed are mainly metal Cr coatings, MAX phase coatings, etc. Coatings of elements such as Cr, Fe, Al, Si, etc. are facing (critical state) oxide aerogelation due to the weak bonding nature of local bonds inside the coating and the large diffusion coefficient of metal atoms in zirconium and zirconia. , loose oxide film, surface damage caused by selective oxidation, excessive ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C23C14/14C23C14/34C23C14/58
CPCC23C14/14C23C14/3464C23C14/5853
Inventor 曹国钦裴书博胡俊华邵国胜田佳佳姚航航
Owner ZHENGZHOU UNIV
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