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A kind of zirconium hydride surface protection method

A technology of zirconium hydride and zirconium oxychloride, which is applied in the direction of solid-state chemical plating, metal material coating process, coating, etc., can solve the problem of unsatisfactory hydrogen blocking effect, achieve good hydrogen blocking effect, and highlight thermal shock resistance The effect of moderate power and thickness

Active Publication Date: 2015-11-18
INNER MONGOLIA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

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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  • A kind of zirconium hydride surface protection method
  • A kind of zirconium hydride surface protection method
  • A kind of zirconium hydride surface protection method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Put zirconium hydride into HF at 5% by volume, HNO 3 45% by volume, H 2 O (the rest is water) polishing solution was etched for 60s, rinsed with deionized water and dried. Put the polished zirconium hydride into a vacuum resistance furnace, vacuumize, and then feed a mixed gas of oxygen (V.5%) and helium (V.95%); Raise to 400°C, keep it warm for 30 hours, then cool to 400°C at a cooling rate of 5°C / min, and then cool to room temperature with the furnace to obtain an in-situ oxide film layer 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 (absolute ethanol): V (H 2 O)=0.5:1, hydrogen peroxide 50mol / L, zirconium oxychloride 0.1mol / L. Add ammonia water dropwise to the configured precursor solution to adjust the pH value...

Embodiment 2

[0037]Put zirconium hydride into HF at 15% by volume, HNO 3 15% by volume, H 2 O (the rest is water) polishing solution was etched for 15s, rinsed with deionized water and dried. Put the polished zirconium hydride into a vacuum resistance furnace, vacuumize, and then introduce carbon dioxide gas; then raise it from room temperature to 600°C at a rate of 1°C / min, keep it warm for 1 hour, and then increase it at a rate of 1°C / min Cool down to 400°C at a cooling rate, and then cool down to room temperature with the furnace to obtain an in-situ oxide film layer 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 (absolute ethanol): V (H 2 O)=1:1, hydrogen peroxide 2.5mol / L, zirconium oxychloride 0.1mol / L. Add ammonia water dropwise...

Embodiment 3

[0040] Put zirconium hydride into HF to 10 volume%, HNO 3 30% by volume, H 2 O (the rest is water) polishing solution was etched for 30s, rinsed with deionized water and dried. Put the polished zirconium hydride into a vacuum resistance furnace, vacuumize, and then introduce oxygen; then rise from room temperature to 500°C at a rate of 3°C / min, keep it warm for 20 hours, and then cool down at a rate of 3°C / min Speed ​​cooling to 400°C, and then cooling to room temperature with the furnace, to obtain an in-situ oxide film layer 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 (absolute ethanol): V (H 2 O)=0.8:1, hydrogen peroxide 30mol / L, zirconium oxychloride 5mol / L. Add ammonia water dropwise to the prepared precursor solut...

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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 a hydrogen permeation-proof 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, and is an ideal solid neutron moderator material. However, due to the high working temperature of zirconium hydride, the Zr-H reaction equilibrium shifts to the direction of hydrogen precipitation within its working temperature range, resulting in continuous hydrogen precipitation, which in turn reduces the neutron moderation efficiency of zirconium hydride. Therefore, controlling the hydrogen loss of zirconium hydride at high temperature is an important problem to be solved for the successful introduction of zirconium hydride moderator. ...

Claims

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Application Information

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Patent Type & Authority Patents(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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