Chromium oxide and zirconium oxide composite coating and preparation method thereof

A composite coating and zirconia technology, applied in the coating, metal material coating process, liquid chemical plating, etc., can solve the problem of lack of composite hydrogen/deuterium/tritium penetration coating, inability to completely cover complex shape parts, Insufficient permeation barrier ability and other problems, to achieve excellent hydrogen/deuterium/tritium permeation resistance, improve thermal compatibility, and increase service life

Active Publication Date: 2022-07-01
HUAZHONG UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Most of the researches on hydrogen permeation barrier coatings that have been carried out so far are single-layer or multi-layer coating material systems with a single component, such as a single Cr 2 o 3 、Al 2 o 3 、Er 2 o 3 Coating and Al 2 o 3 / FeAl, Al 2 o 3 / Cr 2 o 3 、Er 2 o 3 / SiC and other composite coatings, the traditional single coating has insufficient permeation barrier ability to structural materials, poor film-base bonding, and the composite coating has better hydrogen permeation resistance performance, which is the main development direction of hydrogen permeation barrier coatings in the future.
[0004] CN104708863A discloses a kind of Al prepared by organic chemical vapor deposition or magnetron sputtering 2 o 3 / Cr 2 o 3 Composite coating, which combines the hydrogen permeation resistance properties of chromium oxide layer and aluminum oxide layer, but still has the problem of complex preparation process and inability to completely cover parts with complex shapes
[0005] In summary, the current technology still lacks a composite hydrogen / deuterium / tritium permeable coating that is composed of two phases, has a simple preparation process, and meets the needs of complex components.

Method used

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  • Chromium oxide and zirconium oxide composite coating and preparation method thereof
  • Chromium oxide and zirconium oxide composite coating and preparation method thereof
  • Chromium oxide and zirconium oxide composite coating and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] A pure ZrO 2 Hydrogen / deuterium / tritium permeation barrier coating, prepared by:

[0030] 1. Polish the 321L stainless steel to a mirror surface, deionize it with ethanol for 15 minutes, and clean it with acetone.

[0031] 2. Weigh 3 g of zirconium acetate, add 50 ml of absolute ethanol, 2.5 ml of acetone, and 50 μL of glacial acetic acid, place it on a magnetic stirrer and stir for about 10 hours until it is fully dissolved and become clear and transparent, and stand for 24 hours to obtain a zirconium sol.

[0032] 3. The dipping and pulling process is completed with a pulling machine. The pulling speed is uniform throughout the process. The pulling speed is set to 400 μm / s. After pulling, the wet sol and the substrate are placed together at 80 °C for drying for 1 hour, and kept at 400 °C for 30 minutes. , after cooling, the second layer is pulled up, and the previous operation is repeated for a total of three times, and finally heat treatment is performed, and the te...

Embodiment 2

[0034] A Cr with a Cr and Zr molar ratio of 1:1 2 O 3 / ZrO 2 The composite hydrogen / deuterium / tritium permeation barrier coating is prepared by the following methods:

[0035] 1. Polish the 321L stainless steel to a mirror surface, deionize it with ethanol for 15 minutes, and clean it with acetone.

[0036] 2. Weigh 3g of zirconium acetate, add 50ml of absolute ethanol, 2.5ml of acetone, and 50μl of glacial acetic acid, place it on a magnetic stirrer and stir for about 10h until it is fully dissolved and become clear and transparent, and stand for 24h to obtain a zirconium sol; then add to it 1.23g of chromium acetate, ultrasonic for 0.5h or magnetic stirring for about 1h, to obtain a mixed sol.

[0037] 3. The dipping and pulling process is completed with a pulling machine. The pulling speed is uniform throughout the process. The pulling speed is set to 400 μm / s. After pulling, the wet sol and the substrate are placed together at 80 °C for drying for 1 hour, and kept at 40...

Embodiment 3

[0039] A Cr with a Cr and Zr molar ratio of 2:1 2 O 3 / ZrO 2 The composite hydrogen / deuterium / tritium permeation barrier coating is prepared by the following methods:

[0040] 1. Polish the 321L stainless steel to a mirror surface, deionize it with ethanol for 15 minutes, and clean it with acetone.

[0041] 2. Weigh 3 g of zirconium acetate, add 50 ml of absolute ethanol, 2.5 ml of acetone, and 50 μl of glacial acetic acid, place it on a magnetic stirrer and stir for about 10 hours until it is fully dissolved and become clear and transparent, and stand still for 24 hours to obtain a zirconium sol; 2.46 g of chromium acetate was added, and the mixture was ultrasonicated for 0.5 h or magnetically stirred for about 1 h to obtain a mixed sol.

[0042] 3. The dipping and pulling process is completed with a pulling machine. The pulling speed is uniform throughout the process. The pulling speed is set to 400 μm / s. After pulling, the wet sol and the substrate are placed at 80 °C fo...

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Abstract

The invention provides a chromium oxide and zirconium oxide composite coating and a preparation method thereof. The chromium oxide and zirconium oxide composite coating can be suitable for resisting hydrogen and permeation of isotopes thereof in various hydrogen related fields such as fusion reactor cladding module structure materials and hydrogen storage devices. The composite coating is a single-layer composite coating or a multi-layer gradient composite coating, each layer is formed by compounding Cr2O3 and ZrO2, the composite coating combines the hydrogen / deuterium / tritium permeation resistance characteristics of zirconium oxide and chromium oxide, on the basis that the hydrogen / deuterium / tritium resistance performance of the single-phase zirconium oxide coating is improved, the good toughness of the zirconium oxide coating is reserved, and the service life of the zirconium oxide coating is prolonged. The preparation process combining sol-gel with dip-coating can be suitable for coating the surface of a material with a complex structure, and the practical value of the composite coating is greatly improved. The whole process method is simple, healthy, environmentally friendly and suitable for large-scale production.

Description

technical field [0001] The invention relates to the technical field of material surface protection, in particular to a chromium oxide and zirconium oxide composite coating and a preparation method thereof. Background technique [0002] Hydrogen and hydrogen isotopes such as tritium and deuterium can easily penetrate into metal structural materials, causing the strength and plasticity of structural materials to decrease, performance deterioration, shortening the service period of structural materials, and endangering service safety. At present, the cladding module structural materials of fusion reactors, the collector tubes for solar thermal power generation, the pump barrels of oil pumps, oil pipelines and other hydrogen-related devices all have serious hydrogen and its isotope permeation problems. Therefore, it is urgent to prepare a surface of the structural materials. A layer of coating material that blocks hydrogen permeation, ie, a hydrogen / deuterium / tritium permeation ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C23C18/12
CPCC23C18/1216C23C18/1241C23C18/1254C23C18/1291
Inventor 李和平郑立雨周俊严有为
Owner HUAZHONG UNIV OF SCI & TECH
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