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A metal hydride surface hydrogen permeation resistance layer and its preparation method

A permeable layer and hydride technology, applied in metal material coating process, coating, solid-state diffusion coating, etc., can solve the problem of weak bonding between the coating and the hydride substrate, difficulty in implementing a hydrogen barrier film, and incompact film layer Integrity and other issues, to achieve excellent hydrogen barrier performance, moderate thickness, dense film effect

Active Publication Date: 2019-05-21
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

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Problems solved by technology

Metal hydride functional components such as zirconium hydride generally have complex shapes. The use of physical vapor deposition, ion implantation and other methods to prepare hydrogen barrier films on hydride special-shaped components has problems such as difficulty in implementation and uneven film formation in parts such as channels; The embedding aluminizing method is difficult to ensure that metal hydrides such as zirconium hydride do not lose hydrogen; the electroplating method has weak bonding force between the coating and the hydride substrate, the film layer is not dense and complete, and the film layer falls off. There is no report on the preparation of composite hydrogen barrier layer containing carbon, nitrogen and oxygen on the surface of isohydride

Method used

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  • A metal hydride surface hydrogen permeation resistance layer and its preparation method
  • A metal hydride surface hydrogen permeation resistance layer and its preparation method
  • A metal hydride surface hydrogen permeation resistance layer and its preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] 1. Degrease, clean and polish the surface of Φ30mm×30mm zirconium hydride, and the H / Zr of zirconium hydride is 1.65.

[0034] 2. Loading and heat-resistant glass packaging

[0035] ① Weigh 1.5g urea with a balance;

[0036] ② Put urea and zirconium hydride in a high-temperature-resistant glass tube, vacuum seal, and the pressure inside the high-temperature-resistant glass tube is 1×10 - 5 Pa.

[0037] 3. Preparation of hydrogen-resistant permeable layer containing carbon, nitrogen and oxygen

[0038] Put the encapsulated glass tube in a temperature-controlled tube furnace, raise it from room temperature to 500°C at a rate of 300°C / h, keep it at 500°C for 100 hours, then cool it down to 300°C at a rate of 600°C / h, and then cool it naturally to room temperature to obtain a hydrogen permeable barrier layer containing carbon, nitrogen and oxygen.

[0039] The surface AES analysis of the hydrogen barrier permeation layer adopts the PHI-700 nanometer scanning Auger syst...

Embodiment 2

[0042] 1. Degrease, clean and polish the surface of Φ30mm×30mm zirconium hydride, the H / Zr of zirconium hydride=1.85.

[0043] 2. Loading and quartz tube packaging

[0044] ① Use a balance to weigh 5g of acrylamide;

[0045] ②Place acrylamide and zirconium hydride in a quartz tube for vacuum packaging, the pressure inside the quartz tube is 1×10 -3 Pa.

[0046] 3. Preparation of hydrogen-resistant permeable layer containing carbon, nitrogen and oxygen

[0047] Put the packaged quartz tube in a temperature-controlled tube furnace, raise it from room temperature to 400°C at a rate of 600°C / h, keep it at 400°C for 200h, and then raise it from room temperature to 500°C at a rate of 300°C / h , kept at 500° C. for 100 h, and finally cooled naturally in the furnace to room temperature to obtain a hydrogen-resistant permeable layer containing carbon, nitrogen and oxygen, and its hydrogen permeability level is equivalent to that of the carbon, nitrogen and oxygen-containing coating i...

Embodiment 3

[0049] 1. Degrease, clean and polish the surface of Φ20mm×20mm zirconium hydride, and the H / Zr of zirconium hydride is 1.9.

[0050] 2. Loading and stainless steel pipe welding and sealing

[0051] ① Take 5g of ammonium carbonate with a balance;

[0052] ②Put the ammonium carbonate and zirconium hydride in the stainless steel tube, argon arc welding, the pressure inside the stainless steel tube is 101kPa.

[0053] 3. Preparation of hydrogen-resistant permeable layer containing carbon, nitrogen and oxygen

[0054] The stainless steel tube is placed in a temperature-controlled tube furnace, raised from room temperature to 200°C at a rate of 300°C / h, and kept at 200°C for 1 hour; then raised to 500°C at a rate of 100°C / h, and kept at 500°C for 50 hours ; After that, the temperature was raised to 600°C at a rate of 10°C / h, and kept at 600°C for 200h; then the temperature was lowered to 300°C at a rate of 600°C / h, and then naturally cooled to room temperature to obtain a hydrogen...

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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 for the hydrogen-resistance permeation layer on the surface of the metal hydride, source materials containing carbon oxygen or nitrogen oxygen or carbon-nitrogen oxygen are sealed in a reaction vessel with metal hydride matrices, the pressure is controlled between 1.010<5> Pa-101 kPa, and the temperature is controlled to rise from the room temperature to 200-900 DEG C; the carbon oxygen or the nitrogen oxygen or the carbon-nitrogen oxygen is diffused to the surfaces of the metal hydride matrices and conducted in-situ reactions with metal elements of the matrices; and the dense and continuous composite hydrogen-resistance permeation layer which contains the carbon oxygen or the nitrogen oxygen or the carbon-nitrogen oxygen can be obtained after cooling. The hydrogen-resistance permeation layer is tightly combined with the matrices, is moderate in thickness, has an excellent hydrogen-resistance performance and can effectively prevent the hydrogen desorption of the metal hydride when used at the temperature of 200-900 DEG C. The hydrogen-resistance permeation layer on the surface of the metal hydride and the preparation method thereof are simple in operation, high in adaptability, and are not restricted by shapes and structures of complex matrices.

Description

technical field [0001] The invention belongs to the technical field of metal hydride material protection, in particular to a metal hydride surface hydrogen permeation resistance layer and a preparation method thereof. Background technique [0002] Metal hydride has the function of storing and fixing hydrogen, and is often used as a hydrogen storage material. However, at a certain temperature, hydrogen will be released from the metal hydride due to thermodynamic equilibrium, thereby reducing the hydrogen content of the metal hydride and ensuring that the hydrogen content does not decrease. Or to make the reduction rate very low, a common method is to prepare a hydrogen permeable barrier coating on the metal hydride surface. [0003] The permeability of hydrogen in ceramic materials is low, and theoretically very thin ceramic materials can reduce the permeability of metal sheets by 6 orders of magnitude. The currently reported hydrogen permeable ceramic materials mainly inclu...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C23C8/72
CPCC23C8/72
Inventor 王力军陈洋张顺利闫国庆张建东彭家庆吴明吴延科
Owner 有研资源环境技术研究院(北京)有限公司
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