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Method for preparing zirconium hydride

A zirconium hydride, oxidizing technology, applied in the direction of transition element hydride, etc., can solve the problems of micro-cracks in the matrix, easy cracking and peeling of the film layer, and difficulty in the hydrogen barrier film layer. Effects of the hydrogen problem

Active Publication Date: 2009-10-21
有研资源环境技术研究院(北京)有限公司
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  • Abstract
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  • Claims
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AI Technical Summary

Problems solved by technology

[0005] The hydrogen barrier films prepared by various methods have a certain hydrogen barrier effect, but the hydrogen barrier effect is not ideal, mainly because the thermal cycle performance of the film layer is low, and the film layer is easy to crack and peel off, thus losing the protection of the substrate. effect
In addition, due to the high brittleness of zirconium hydride, there are many defects such as microcracks in the substrate itself, which brings great difficulties to prepare a uniform and dense hydrogen barrier film on the surface of zirconium hydride.
Therefore, it is difficult to solve the problem of hydrogen loss of zirconium hydride under high temperature conditions by simply relying on the method of preparing a hydrogen barrier film layer on the surface of zirconium hydride, and it is also difficult to meet the requirements for the use of zirconium hydride moderator materials

Method used

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  • Method for preparing zirconium hydride
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  • Method for preparing zirconium hydride

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Cut zirconium hydride with a hydrogen-zirconium atomic ratio of about 1.8 into a Φ20mm×10mm cylindrical sample. The samples were ultrasonically cleaned with acetone for 15 minutes and then dried.

[0030] The pretreated zirconium hydride sample is placed in a vacuum tube resistance furnace for high-temperature thermal oxidation treatment, so that a zirconium oxide hydrogen barrier film layer is formed on the surface of the zirconium hydride. The specific steps are as follows: put the zirconium hydride sample into a stainless steel crucible, then put it into a vacuum tube resistance furnace, start the mechanical pump, vacuumize, extract the air in the crucible, and then inject CO into the crucible. 2 To 0.1MPa, start heating. The heating rate during the heating process is 1°C / min. When the temperature reaches 350°C, keep it warm for 60 hours, then cut off the power supply, and cool down with the furnace to form a zirconia hydrogen barrier film layer.

[0031] The oxidi...

Embodiment 2

[0033] Cut zirconium hydride with a hydrogen-zirconium atomic ratio of about 1.8 into a Φ20mm×10mm cylindrical sample. The samples were ultrasonically cleaned with acetone for 20 minutes and then dried.

[0034] The pretreated zirconium hydride sample is placed in a vacuum tube resistance furnace for high-temperature thermal oxidation treatment, so that a zirconium oxide hydrogen barrier film layer is formed on the surface of the zirconium hydride. The specific steps are as follows: put the zirconium hydride sample into a stainless steel crucible, then put it into a vacuum tube resistance furnace, start the mechanical pump, vacuumize, extract the air in the crucible, and then inject CO into the crucible. 2 To 0.1MPa, start heating. The heating rate during the heating process is 5°C / min. When the temperature reaches 600°C, keep it warm for 30 hours, then cut off the power supply, and cool down with the furnace to form a zirconia hydrogen barrier film layer.

[0035] The oxidi...

Embodiment 3

[0037] Cut zirconium hydride with a hydrogen-zirconium atomic ratio of about 1.8 into a Φ20mm×10mm cylindrical sample. The samples were ultrasonically cleaned with acetone for 20 minutes and then dried.

[0038] The pretreated zirconium hydride sample is placed in a vacuum tube resistance furnace for high-temperature thermal oxidation treatment, so that a zirconium oxide hydrogen barrier film layer is formed on the surface of the zirconium hydride. The specific steps are as follows: put the zirconium hydride sample into a stainless steel crucible, then put it into a vacuum tube resistance furnace, start the mechanical pump, vacuumize, extract the air in the crucible, and then inject CO into the crucible. 2 To 0.1MPa, start heating. The heating rate during the heating process is 2°C / min. When the temperature reaches 500°C, keep it warm for 40 hours, then cut off the power supply, and cool down with the furnace to form a zirconia hydrogen barrier film layer.

[0039] The oxidi...

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Abstract

The invention relates to a method for preparing zirconium hydride, comprising the following steps: (1) ultrasonically washing the zirconium hydride for 15 minutes to 20 minutes by acetone and drying the zirconium hydride; (2) placing the zirconium hydride obtained in the step (1) into a stainless steel crucible and then into a vacuum tube type resistance furnace for pumping vacuum, charging carbon dioxide into the crucible, heating the zirconium hydride to 350 DEG C to 600 DEG C from room temperature at the speed of 1 DEG C to 5 DEG C / min and insulating the zirconium hydride for 30 hours to 60 hours in the temperature range; and (3) cooling the zirconium hydride to the room temperature and forming a zirconium hydride film layer with a certain hydrogen permeation resistant function on the zirconium hydride surface. The zirconium hydride is arranged in the mixture atmosphere of oxidizing gas and inert gas to be heated, and a hydrogen evolution phenomenon of the zirconium hydride under the condition of high temperature can be effectively prevented by heating the zirconium hydride to 500 DEG C to 900 DEG C from the room temperature.

Description

technical field [0001] The invention relates to a preparation method of zirconium hydride, which belongs to the technical field of material protection. technical background [0002] Zirconium hydride has become an ideal solid neutron moderator material for space stacks due to its high thermal stability, high hydrogen density, low neutron capture cross section and good thermal conductivity. However, within the working temperature range of zirconium hydride, hydrogen will be continuously precipitated from zirconium hydride, which will reduce the neutron moderation efficiency. Therefore, controlling the hydrogen loss of zirconium hydride under high temperature conditions is an important problem that urgently needs to be solved when the zirconium hydride moderator is used in space reactors. [0003] Under the premise of not affecting the performance of the matrix material, a thin layer of ceramic coating with low hydrogen diffusion coefficient and low surface recombination cons...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B6/02
Inventor 王力军陈伟东黄永章张力陈松王建伟吴延科
Owner 有研资源环境技术研究院(北京)有限公司
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