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Analysis method for nucleation of metal hydride containing surface oxide layer

A surface oxidation and analysis method technology, applied in the field of nuclear technology application, can solve the problems of interference measurement results, damage, inability to meet the requirements of metal hydride reaction measurement, etc., and achieve the effect of simple sample preparation and good statistics

Active Publication Date: 2020-08-14
INST OF NUCLEAR PHYSICS & CHEM CHINA ACADEMY OF
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Secondary ion mass spectrometry can obtain local hydrogen distribution, but it is a destructive test and cannot be dynamically observed
In addition, an oxide layer will inevitably form on the surface of actual metal materials, and the oxide will seriously interfere with the measurement results based on electron and X-ray probe techniques
[0004] Compared with pure metals, the hydrogenation reaction of metals with surface oxide layers is very complicated, which restricts the application of metal materials in hydrogen-containing atmospheres
However, the existing methods for observing the nucleation process of hydrides cannot meet the measurement requirements of metal hydride reactions that are close to the actual state (the surface contains oxide layers, damage, impurities, etc.), and new testing methods need to be developed

Method used

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  • Analysis method for nucleation of metal hydride containing surface oxide layer
  • Analysis method for nucleation of metal hydride containing surface oxide layer
  • Analysis method for nucleation of metal hydride containing surface oxide layer

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Experimental program
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Embodiment 1

[0043] The metal to be tested in this embodiment is a cerium metal sample, and the sample piece is polished on the same sandpaper for the same time, and stored at 200° C. in a 100KPa argon-oxygen mixture for about 10 hours to generate a certain thickness of oxide layer on the surface of the sample. The small-angle scattering test instrument is the Suanni neutron small-angle scattering spectrometer at the Mianyang Research Reactor in China.

[0044] The analytical method of the metal hydride nucleation that contains surface oxide layer in this embodiment, concrete steps are as follows:

[0045] a. Prepare a thin sheet-shaped cerium metal sample to be tested;

[0046] b. Place the cerium metal sample to be tested in the hydrogenation reaction chamber, continuously inject deuterium gas into the chamber, and carry out the small-angle neutron scattering test at the same time, and obtain the small-angle scattering of the metal sample to be tested at different time points during the ...

Embodiment 2

[0051] In this embodiment, the analysis method of metal hydride nucleation containing surface oxide layer, except for step (d), other operating steps are the same as in embodiment 1, wherein, step (d) is specifically:

[0052] Choose fixed scattering vector 0.41nm -1 , read the scattering intensity of the scattering vector for all the absolute intensity scattering curves, analyze the change of the scattering intensity with time, and the time when the scattering intensity starts to increase is the critical point of hydride nucleation.

[0053] In this embodiment, the scattering intensity of the small-angle scattering curve of the sample at different time points of the hydrogenation reaction is obtained at a fixed scattering vector, and the initial scattering intensity is deducted to obtain the scattering intensity increment in the hydrogenation reaction. image 3 The relationship of the scattering intensity increment with time is given. It can be seen that the scattering inten...

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Abstract

The invention discloses an analysis method for nucleation of metal hydride containing a surface oxide layer. The method comprises the steps of 1, firstly, loading a metal sample to be tested into a reaction cavity, then introducing hydrogen / deuterium gas into the cavity, carrying out a small-angle neutron scattering test in the process, processing small-angle scattering experimental data to obtainan absolute intensity scattering curve, and judging the critical point of hydride nucleation according to the time when the absolute scattering intensity is increased. The analysis method for nucleation of the metal hydride containing the surface oxide layer provides a sensitive initial hydride nucleation measurement method, and can be used for evaluating the surface hydrogenation reaction of a real metal material (the surface contains the oxide layer, damage, impurities and the like). The observed metal hydride nucleation containing the surface oxide layer is a key process of an actual metalhydrogenation reaction, and can be used for metal hydrogen corrosion resistance evaluation and hydrogen storage material activation process optimization.

Description

technical field [0001] The invention belongs to the application field of nuclear technology, and in particular relates to an analysis method for the nucleation of metal hydrides containing surface oxide layers. Background technique [0002] Interactions of metals with hydrogen are common in industry. Hydrogen embrittlement caused by hydrogen corrosion will affect the service life of metal pipelines and cause serious safety hazards. Some active metals are prone to surface corrosion during long-term storage, and the corrosion products will lead to a decrease in the mechanical properties of the material, and the corrosion products are flammable, which brings safety hazards to the processing and production of materials. The development of hydrogen storage alloys requires rapid hydrogen charging but is often limited by activation conditions. All the above problems are related to the generation and evolution of hydrides. The hydride nucleation process in the initial stage of the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N23/202
CPCG01N23/202
Inventor 汪小琳闫冠云纪和菲陈杰孙光爱夏元华邹林史鹏黄朝强龚建
Owner INST OF NUCLEAR PHYSICS & CHEM CHINA ACADEMY OF
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