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A preparation method of a metal hydride surface hydrogen permeation resistance layer

A hydride and permeable layer technology, applied in the direction of metal material coating process, coating, solid diffusion coating, etc., can solve the problems of difficult to prepare coatings, complex shapes, etc., to achieve improved hydrogen permeation resistance and adaptability Strong, prevent hydrogen release effect

Active Publication Date: 2019-03-22
有研资源环境技术研究院(北京)有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Metal hydride functional components such as zirconium hydride generally have complex shapes, and it is difficult to prepare uniform coatings on various parts by methods such as physical vapor deposition; high temperature or rapid thermal shock are used in the process of preparing barrier layers on the surface of metal hydrides such as zirconium hydride method is also not suitable
There is no report on the method of preparing nitrogen-oxygen, carbon-oxygen or carbon-nitrogen-oxygen coatings on metal hydride substrates such as zirconium hydride

Method used

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  • A preparation method of a metal hydride surface hydrogen permeation resistance layer
  • A preparation method of a metal hydride surface hydrogen permeation resistance layer
  • A preparation method of a metal hydride surface hydrogen permeation resistance layer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] The preparation device of the hydrogen barrier permeable layer adopted in this embodiment is as follows: figure 1 shown.

[0029] 1. Degrease, clean and polish the surface of Φ20mm×20mm zirconium hydride, zirconium hydride H / Zr=1.0.

[0030] 2. Put zirconium hydride in a sealed and ventilated stainless steel vacuum reaction vessel 1, put the reaction vessel 1 into the first temperature-controlled heating furnace 2, and vacuumize the reaction vessel 1 to 2.0×10 -4 Pa.

[0031] 3. In situ reaction:

[0032] (1) In terms of volume percentage, according to CO:CO 2 :H 2 =5:80:15 ratio gas distribution, the mixed gas is distributed into water vapor through the water scrubbing device 3, and the gas flow rate is 0.2 liters / minute;

[0033] (2) The solid mixture of calcium carbonate, magnesium carbonate, and ammonium carbonate each 10kg is packed into decomposition reaction bed 5, and decomposition reaction bed 5 is inserted in the second temperature-control type heating fu...

Embodiment 2

[0039] 1. Degrease, clean and polish the surface of Φ20mm×20mm zirconium hydride, zirconium hydride H / Zr=1.6.

[0040] 2. Put zirconium hydride in a sealed and ventilated stainless steel vacuum reaction vessel, put the reaction vessel into a heating furnace, and vacuumize to 1.0×10 -4 Pa.

[0041] 3. In situ reaction:

[0042] (1) In terms of volume percentage, according to CO:CO 2 :NH 3 :N 2 :H 2 =20:35:35:5:5 ratio gas distribution;

[0043] (2) Connect the inlet valve, pass the mixed gas in (1) into the reaction vessel at a speed of 0.2 liters / minute, and open the reaction vessel outlet valve until the reaction vessel pressure reaches 0.1MPa;

[0044] (3) At the same time of constant ventilation, first raise the heating furnace from room temperature to 500°C at a rate of 300°C / hour, and keep it warm for 100 hours; then cool it down to room temperature at a rate of 10°C / hour, and the carbon-nitrogen-containing Oxygen barrier to hydrogen permeation.

Embodiment 3

[0046] 1. Degrease, clean and polish the surface of Φ20mm×20mm zirconium hydride, zirconium hydride H / Zr=1.80.

[0047] 2. Put zirconium hydride in a sealed and ventilated high-temperature-resistant glass vacuum reaction vessel, put the reaction vessel into a heating furnace, and vacuumize to 2.0×10 -4 Pa.

[0048] 3. In situ reaction:

[0049] (1) In terms of volume percentage, according to CO:CO 2 :H 2 =80:10:10 ratio gas distribution, the mixed gas is mixed with water vapor through the water scrubbing device, and the gas flow rate is 0.2 liters / minute;

[0050] (2) Calcium carbonate, magnesium carbonate, sodium carbonate each 10kg are packed into decomposition reaction bed, and reaction bed is heated up to 700 ℃ and decomposes and produces the gas containing carbon, oxygen, gas flow rate 0.1 liter / minute;

[0051] (3) the gas obtained in (1) is passed into the reaction vessel with a speed of 0.2 liters / minute; simultaneously the gas in (2) is passed into the reaction ve...

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Abstract

The invention relates to a preparation method for a hydrogen-resistance permeation layer on the surface of metal hydride. According to the preparation method, a metal hydride matrix subjected to surface treatment is sealed in a vacuum reaction vessel; gas containing carbon oxygen or nitrogen oxygen or carbon-nitrogen oxygen is injected into the reaction vessel at constant flow; an in-situ reaction is conducted between the gas containing the carbon oxygen or the nitrogen oxygen or the carbon-nitrogen oxygen and metal elements of the matrix at the temperature of 400-900 DEG C; and the dense and complete hydrogen-resistance permeation layer containing the carbon oxygen or the nitrogen oxygen or the carbon-nitrogen oxygen is obtained after cooling. The preparation method for the hydrogen-resistance permeation layer on the surface of the metal hydride solves the problems of interlayer defects and untight interlayer combination of a carbide film overlaying with an oxide film, a nitride film overlaying with the oxide film, and the nitride film overlaying with the carbide film and the oxide film, restrains / retards precipitation of hydrogen from the metal hydride matrix effectively, and has a high hydrogen-resistance permeation capacity.

Description

technical field [0001] The invention belongs to the technical field of metal hydride material protection, in particular to a method for preparing a hydrogen permeation-resistant layer on the surface of a metal hydride. Background technique [0002] Metal hydrides have the functions of hydrogen storage and fixation, and are often used as hydrogen-carrying materials. Keeping hydrogen from being lost at high temperatures is a key factor in material performance; layers are important. [0003] There are many research reports on hydrogen permeation resistance, most of which are hydrogen permeation barrier layers prepared on the surface of stainless steel or carbon steel. The stainless steel substrate is essentially different from the metal hydride substrate. Stainless steel has good plasticity and a series of other metal properties, and its shape is relatively simple. It is suitable for physical vapor deposition process, embedded aluminizing process, etc. Metal hydride functiona...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C23C8/28
CPCC23C8/28
Inventor 陈洋王力军闫国庆张顺利张建东车小奎吴明彭家庆
Owner 有研资源环境技术研究院(北京)有限公司
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