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Method for increasing hydrogen pre-charging speed of metal sample in hydrogen embrittlement test

A metal and sample technology, applied in the field of improving the pre-hydrogen charging speed of metal samples and hydrogen embrittlement test, can solve the problems of high hydrogen fugacity, long pre-charging time, and high heating temperature, so as to improve the pre-hydrogen charging speed and shorten the pre-charging temperature. The effect of hydrogen charging time

Pending Publication Date: 2022-04-12
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although electrolytic hydrogen charging is currently the simplest and most commonly used hydrogen charging method, this method only guarantees a certain concentration of hydrogen ions and cannot truly simulate the service state of materials in an actual high-pressure hydrogen environment.
In addition, the electrolytic hydrogen charging of aqueous solution will generate high hydrogen fugacity on the surface of the material, which will lead to cracking or phase change on the surface of the material.
[0006] (2) High-temperature gas-phase hydrogen filling: According to the gas state equation, increasing the temperature can cause the gas to expand to generate high-pressure hydrogen. However, only relying on increasing the temperature to increase the pressure requires a relatively high heating temperature. For example, if you want to increase the hydrogen pressure of 10MPa at 25°C to 40MPa, you need to heat the temperature to about 920°C, and when it is raised to 70MPa, you need to heat the temperature to 1820°C, which is difficult for traditional high-temperature and high-pressure hydrogen charging devices. this pressure
In addition, the high temperature environment may cause destructive effects on the material itself, such as thermal stress cracking, etc.
[0007] (3) Mechanical pressurized hydrogen charging: put the material in the hydrogen charging device, use a compressor to provide high-pressure hydrogen to the hydrogen charging device after sealing, and pre-charge hydrogen at room temperature or under mild conditions below 150 ° C. Although this method Basically, it will not cause damage to the material itself, but to achieve the high-pressure hydrogen environment when the material is actually in service, there is a shortcoming of long pre-filling time

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] The S304 stainless steel is processed into a sample having a diameter of 10 mm, thickness of 2 mm, and the mechanical processing contaminant of the sample surface is removed by sandpaper, and then acetone and ethanol are used for 20 min ultrasonic cleaning, and then the sample is dried, and the sample is placed after drying. The vacuum chamber of the magnetron sputtering system.

[0050] Preparation of Ceni by melting method 5 The hydrogen storage alloy is prepared, and the alloy target is prepared, and the target is placed in the target base.

[0051] High-purity argon with a volume fraction of 99.999% is a working atmosphere, and Ceni is deposited in the sample surface. 5 Hydrogen storage alloy film, deposition time is 30 min, Ceni 5 The hydrogen storage alloy film has a thickness of 12 nm to obtain a pre-charged sample.

[0052] The sample of the undumored hydrogen welded welding pleximin film is placed simultaneously in the hydrogen-hydrogen-hydrogen-hydrogen sample dep...

Embodiment 2

[0055] The S316 stainless steel was processed into a sample having a diameter of 10 mm and a thickness of 2 mm, and the mechanical processing contaminant of the sample surface was removed by sandpaper, and then acetone was used to dry the sample with ethanol, and the sample was dried.

[0056] The sample was placed in a vacuum chamber of the magnetron sputtering system, and the metal Ti and the metal Ni were used as the target, respectively, in two target bases, respectively.

[0057] High-purity argon with 99.99% by volume fraction is a working atmosphere, and a Tini hydrogen storage alloy film is deposited in the surface of the sample. The deposition time is 40 min, and the thickness of the Tini hydrogen storage alloy film is 15 nm to obtain a pre-charged sample.

[0058] Pre-charged hydrogen samples deposited in the hydrogen storage alloy film are placed in a hyperbine apparatus, and the seal is sealed and empty to 10 -2 PA, exclude impurity gases in the cavity of the hitting d...

Embodiment 3

[0061] S30408 ​​stainless steel was processed into a sample having a diameter of 10 mm and a thickness of 2 mm, and the mechanical processing contaminant of the sample was removed by sandpaper, and then acetone was used to dry the sample with ethanol, and then dried the sample.

[0062] Preparation of Ti by melting method 0.9 ZR 0.1 CR 1.2 Mn 0.8 Hydrogen storage alloy, then use a ball milling method to break the hydrogen storage alloy to make a powder, TI 0.9 ZR 0.1 CR 1.2 Mn 0.8 Hydrogen storage alloy powder is a raw material for hot plasma physical vapor deposition by ar-h 2 Tenic physical vapor deposition method 0.9 ZR 0.1 CR 1.2 Mn 0.8 The hydrogen storage alloy is deposited to the surface of the sample, the deposition time is 1 minute, Ti 0.9 ZR 0.1 CR 1.2 Mn 0.8 The hydrogen storage alloy has a thickness of 19 nm to obtain a pre-charged sample.

[0063] The sample of the undumored hydrogen welded welding pleximin film is placed simultaneously in the hydrogen-hydrogen-hydrog...

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Abstract

The invention belongs to the technical field of metal materials, and relates to a method for increasing the hydrogen pre-charging speed of a metal sample in a hydrogen embrittlement test, which comprises the following steps: forming a hydrogen storage alloy film on the surface of the metal sample to obtain a hydrogen pre-charging sample; and placing the hydrogen pre-filling sample in a hydrogen filling device for hydrogen pre-filling. According to the invention, the hydrogen storage alloy film has a catalytic effect of accelerating the dissociation of hydrogen molecules into hydrogen atoms, so that the concentration of hydrogen atoms on the surface of the pre-charged hydrogen sample is high, and meanwhile, the hydrogen storage alloy film has an effect of absorbing hydrogen atoms, and the diffusion speed of the hydrogen atoms in the hydrogen storage alloy film is extremely high. Therefore, high-pressure hydrogen introduced into the hydrogen charging device can be decomposed into hydrogen atoms more quickly under the action of the hydrogen storage alloy film, and the hydrogen atoms are diffused into a matrix of the metal sample through an interface between the hydrogen storage alloy film and the metal sample, so that the hydrogen pre-charging speed of the metal sample is effectively increased, and the hydrogen pre-charging time is shortened.

Description

Technical field [0001] The present invention relates to the technical field of metal materials, and in particular, to the method of improving the pre-charging speed of metal samples in a hydroxite test. Background technique [0002] The most important challenge in hydrogen energy development is the storage and transportation of hydrogen energy, find safe, economic, efficient, feasible storage and transportation model, is the key to hydrogen energy full life cycle application. At present, the high-pressure container is hydrogen storage method, and the hydrogen pressure level is generally 35 MPa or 70 MPa, but the high pressure container is exposed to a high pressure hydrogen environment in high pressure hydrogen environments, thereby causing the high pressure vessel cracking. [0003] Therefore, the material for the material for high pressure vessels is critical, and the most critical of the hydrogen crispy test is to provide the actual hydrogen service environment of the material...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N3/02
Inventor 王新华金宸吴宇浩严密
Owner ZHEJIANG UNIV