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Surface protection method for zirconium hydride

A technology of zirconium hydride and zirconium oxychloride, applied in solid-state chemical plating, metal material coating process, coating and other directions, can solve problems such as unsatisfactory hydrogen blocking effect, achieve low raw material prices, ensure stability, and achieve outstanding results. The effect of thermal shock resistance

Active Publication Date: 2014-01-01
INNER MONGOLIA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

It can be seen that the hydrogen barrier coating prepared on the surface of zirconium hydride by the above method has a certain hydrogen barrier effect, but the hydrogen barrier effect is not ideal.

Method used

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  • Surface protection method for zirconium hydride
  • Surface protection method for zirconium hydride
  • Surface protection method for zirconium hydride

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Put the zirconium hydride into HF as 5% by volume, HNO 3 Is 45% by volume, H 2 Etch in O (the rest is water) polishing solution for 60 seconds, rinse with deionized water and dry. Put the polished zirconium hydride into a vacuum resistance furnace, evacuate, and then pass in a mixed gas of oxygen (V.5%) and helium (V.95%); then at a speed of 5℃ / min from room temperature The temperature is raised to 400°C, kept for 30 hours, and then cooled to 400°C at a cooling rate of 5°C / min, and then cooled to room temperature with the furnace to obtain an in-situ oxide film on the surface of zirconium hydride. A mixed solution of distilled water and absolute ethanol is used as a solvent, hydrogen peroxide is used as a catalyst, and zirconium oxychloride is used as a precursor to configure a precursor solution. The composition and content of the precursor solution are: V (anhydrous ethanol): V (H 2 O)=0.5:1, hydrogen peroxide 50mol / L, zirconium oxychloride 0.1mol / L. Add ammonia water...

Embodiment 2

[0037] Put zirconium hydride into HF at 15% by volume, HNO 3 15% by volume, H 2 Etch in O (the rest is water) polishing solution for 15s, rinse with deionized water and dry. Put the polished zirconium hydride into a vacuum resistance furnace, evacuate, and then pass in carbon dioxide gas; then at a rate of 1 ℃ / min from room temperature to 600 ℃, holding for 1 hour, and then at 1 ℃ / min The cooling rate is cooled to 400°C, and then cooled to room temperature with the furnace to obtain an in-situ oxide film layer on the surface of the zirconium hydride. A mixed solution of distilled water and absolute ethanol is used as a solvent, hydrogen peroxide is used as a catalyst, and zirconium oxychloride is used as a precursor to configure a precursor solution. The composition and content of the precursor solution are: V (anhydrous ethanol): V (H 2 O)=1:1, hydrogen peroxide 2.5mol / L, zirconium oxychloride 0.1mol / L. Add ammonia water dropwise to the prepared precursor solution to adju...

Embodiment 3

[0040] Put zirconium hydride into HF at 10% by volume, HNO 3 30% by volume, H 2 Etch in O (the rest is water) polishing solution for 30s, rinse with deionized water and dry. Put the polished zirconium hydride into a vacuum resistance furnace, evacuate, and then pass in oxygen; then increase from room temperature to 500°C at a rate of 3°C / min, keep it for 20 hours, and then decrease the temperature at 3°C / min The rate is cooled to 400°C, and then cooled to room temperature with the furnace to obtain an in-situ oxide film on the surface of the zirconium hydride. A mixed solution of distilled water and absolute ethanol is used as a solvent, hydrogen peroxide is used as a catalyst, and zirconium oxychloride is used as a precursor to configure a precursor solution. The composition and content of the precursor solution are: V (anhydrous ethanol): V (H 2 O)=0.8:1. Hydrogen peroxide 30mol / L, zirconium oxychloride 5mol / L. Add ammonia water dropwise to the prepared precursor solution to...

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Abstract

The invention relates to a method for preparing a hydrogen-permeation resistant coating on the surface of zirconium hydride. The method particularly adopts the technical scheme that an in situ oxidization method for the preparation of a bottom layer is adopted, a sol-gel method is adopted and a nanometer oxide coating is prepared on the bottom layer, and finally an oxide coating with a composite structure is obtained. The method includes the following steps: firstly, the zirconium hydride is subjected to in situ oxidization in an oxidizing gas, so as to prepare a zirconia bottom layer, then the zirconium hydride is placed in a zirconium oxychloride precursor sol, and the sol is solidified and sintered through adopting a segmented heat processing technology. Through the adoption of the method, the prepared composite coating on the surface of the zirconium hydride is tightly combined with a base body, and is proper in thickness, excellent in thermal shock resistance and better in high-temperature oxidation resistance.

Description

Technical field [0001] The invention relates to a method for protecting the surface of zirconium hydride, in particular to a method for preparing an anti-hydrogen permeation coating on the surface of zirconium hydride, and belongs to the technical field of material protection. technical background [0002] Zirconium hydride has high thermal stability, high hydrogen density, low neutron capture cross-section and high thermal conductivity, making it an ideal solid neutron slowing material. However, due to the high working temperature of zirconium hydride, within its working temperature range, the Zr-H reaction equilibrium shifts in the direction of hydrogen precipitation, causing the continuous precipitation of hydrogen, thereby reducing the neutron moderation efficiency of zirconium hydride. Therefore, controlling the hydrogen loss of zirconium hydride under high temperature conditions is an important issue that needs to be solved in the successful introduction of zirconium hydrid...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C23C20/08
Inventor 陈伟东闫淑芳闫国庆刘向东王志刚范秀娟张亚增车广东
Owner INNER MONGOLIA UNIV OF TECH
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