CN113390011B - Pressurization and hydrogen filling method for metal hydrogen embrittlement test in high-pressure hydrogen environment - Google Patents
Pressurization and hydrogen filling method for metal hydrogen embrittlement test in high-pressure hydrogen environment Download PDFInfo
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Abstract
The invention relates to a pressurization and hydrogen filling method for a metal hydrogen embrittlement test in a high-pressure hydrogen environment, which comprises the following steps: providing a hydrogen charging device, wherein the hydrogen charging device is provided with an inner cavity; placing a hydrogen storage alloy and a metal sample in an inner cavity of a hydrogen charging device together, and filling hydrogen into the inner cavity of the hydrogen charging device to ensure that the hydrogen storage alloy is saturated by absorbing hydrogen; and heating the hydrogen charging device to ensure that the hydrogen storage alloy saturated by hydrogen absorption releases high-pressure hydrogen, so that the inner cavity environment of the hydrogen charging device becomes a high-pressure hydrogen environment, and charging the metal sample. The method can change the inner cavity environment of the hydrogen charging device into a high-pressure hydrogen environment only by small temperature rise, has less consumption, low cost and relatively higher safety, and can directly charge the hydrogen for the metal sample and improve the hydrogen charging speed.
Description
Technical Field
The invention relates to the technical field of metal materials, in particular to a pressurization and hydrogen filling method for a metal hydrogen embrittlement test in a high-pressure hydrogen environment.
Background
Safe and efficient storage and transportation are the key points of hydrogen energy application, at present, high-pressure container hydrogen storage is the main hydrogen storage mode, the pressure grade of hydrogen is generally 350bar or 700bar, but the high-pressure container and the hydrogen charging and discharging pipelines are exposed to the high-pressure hydrogen environment for a long time and hydrogen embrittlement occurs, so that the durability and the performance are reduced. Therefore, it is important to study hydrogen embrittlement of materials for high-pressure vessels. The most key to hydrogen embrittlement research is to provide the actual hydrogen service environment of the material, so that the material needs to be charged with hydrogen and a high-pressure hydrogen environment when the material is actually in service is achieved. The conventional hydrogen filling method for the hydrogen embrittlement test is roughly divided into three types:
(1) Electrochemical hydrogen charging: the material is used as a cathode and is charged with hydrogen under the condition of electrolysis, and the content of the hydrogen in the material is mainly determined by the magnitude of current density. The method is simple to operate, has small potential safety hazard, and can obtain higher hydrogen concentration, but the method is only suitable for the conditions of normal temperature and normal pressure, and has larger difference with the high-pressure hydrogen environment actually serving as the material. Therefore, the electrolysis method only ensures a certain hydrogen ion concentration, and cannot simulate a real high-pressure hydrogen service environment, and in addition, the electrolysis method may also have an influence on the performance of the material.
(2) Filling hydrogen in a gas phase at room temperature: the material is placed in a container with room temperature and high pressure for hydrogen charging, wherein the high pressure hydrogen environment in actual service of the material can be achieved by using a compressor for supplying high pressure hydrogen, but the compressor capable of supplying more than 400bar is expensive.
(3) And (3) charging the material by using high-pressure hydrogen generated by gas expansion: the principle of this method is to generate high pressure hydrogen by expanding low pressure hydrogen gas at elevated temperature according to the gaseous equation, and this method only increases the pressure by raising the temperature, which is very inefficient. For example, if a hydrogen pressure of 100bar at 25 ℃ is to be raised to 400bar, the temperature needs to be heated to about 920 ℃, and when the hydrogen pressure is raised to 700bar, the temperature needs to be heated to 1820 ℃, and the traditional high-temperature and high-pressure hydrogen charging device cannot bear the high-temperature condition.
Disclosure of Invention
In view of the above, there is a need to provide a pressurization and hydrogen charging method for a metal hydrogen embrittlement test in a high-pressure hydrogen environment, which only needs a small temperature rise to enable an inner cavity environment of a hydrogen charging device to be a high-pressure hydrogen environment, has low consumption, low cost and relatively high safety, and can directly charge hydrogen to a metal sample to increase the hydrogen charging speed.
A pressurization and hydrogen charging method for a metal hydrogen embrittlement test in a high-pressure hydrogen environment comprises the following steps:
providing a hydrogen charging device, wherein the hydrogen charging device is provided with an inner cavity;
placing a hydrogen storage alloy and a metal sample in an inner cavity of a hydrogen charging device together, and filling hydrogen into the inner cavity of the hydrogen charging device to ensure that the hydrogen storage alloy is saturated by absorbing hydrogen; and
and heating the hydrogen charging device to ensure that the hydrogen storage alloy saturated in hydrogen absorption releases high-pressure hydrogen, so that the inner cavity environment of the hydrogen charging device becomes a high-pressure hydrogen environment, and charging the metal sample.
In one embodiment, the hydrogen storage alloy is selected from AB2Hydrogen-absorbing alloy, AB5At least one of type hydrogen storage alloy and AB type hydrogen storage alloy.
In one embodiment, the hydrogen storage alloy is selected from the AB2Type AB hydrogen storage alloy2The general formula of the hydrogen storage alloy is RxT2Wherein R is selected from at least one of Ti, zr and Ca, T is selected from at least one of V, cr, fe, mn, mo, cu and Ni, and x is more than or equal to 0.9 and less than or equal to 1.3.
In one embodiment, the volume of the inner cavity of the hydrogen charging device is V1The volume of the metal sample is V2The AB2The mass of the hydrogen storage alloy in the inner cavity of the hydrogen charging device is W1，V1、V2And W1The following formula is satisfied: 2 × (V)1-V2)≤W1≤4×(V1-V2) Wherein, V1In units of ml, V2Unit of (2) is milliliter, W1The unit of (c) is g.
In one embodiment, the hydrogen charging device is charged with hydrogen to enable the AB to be charged2In the step of hydrogen absorption saturation of the hydrogen storage alloy, the temperature is 0-30 ℃, and the pressure is 50-120 bar.
In one embodiment, the hydrogen storage alloy is selected from the group consisting of the AB5Type AB hydrogen storage alloy5The general formula of the hydrogen storage alloy is MDyWherein M is selected from at least one of rare earth elements, D is selected from at least one of Ni, mn, al, co and Fe, and y is more than or equal to 4.7 and less than or equal to 5.2.
In one embodiment, the volume of the inner cavity of the hydrogen charging device is V1The volume of the metal sample is V2The AB2The mass of the hydrogen storage alloy in the inner cavity of the hydrogen charging device is W2，V1、V2And W2The following formula is satisfied: 2 × (V)1-V2)≤W2≤4×(V1-V2) Wherein, V1In units of ml, V2Unit of (2) is milliliter, W2The unit of (c) is g.
In one embodiment, the hydrogen charging device is charged with hydrogen to enable the AB to be charged5In the step of hydrogen absorption saturation of the hydrogen storage alloy, the temperature is 0-30 ℃, and the hydrogen absorption pressure is 20-50 bar.
In one embodiment, the hydrogen storage alloy is selected from the AB type hydrogen storage alloys, the AB type hydrogen storage alloy comprises a TiFe multi-element alloy, and the volume of the inner cavity of the hydrogen charging device is V1The volume of the metal sample is V2The mass of the AB type hydrogen storage alloy in the inner cavity of the hydrogen charging device is W3，V1、V2And W3The following formula is satisfied: 2X (V)1-V2)≤W3≤4×(V1-V2) Wherein V is1In units of ml, V2Unit of (2) is milliliter, W3The unit of (c) is g.
In one embodiment, the hydrogen filling device is filled with hydrogen, and the AB type hydrogen storage alloy is saturated by absorbing hydrogen at 0-30 ℃ and under 20-50 bar.
During the hydrogen absorption process of the hydrogen storage alloy, hydrogen is firstly absorbed on the surface of the hydrogen storage alloy and decomposed into hydrogen atoms, and the hydrogen atoms are gradually diffused into the hydrogen storage alloy from the surface to form MHxSolid solution (alpha phase), finally MHxThe solid solution is saturated and then reacts with hydrogen to generate metal hydride MHy(beta phase), the hydrogen pressure P of the metal hydride at the hydrogen release equilibrium is exponential to 1000/T (T is temperature, and the unit is K). Therefore, the hydrogen storage alloy is added into the hydrogen charging device, after the hydrogen storage alloy absorbs hydrogen at low temperature and is saturated to form metal hydride, the metal hydride can be decomposed and release high-pressure hydrogen only by raising the temperature by a small margin, and further the inner cavity environment of the hydrogen charging device becomes the high-pressure hydrogen environment.
In addition, during the process of charging the metal sample, hydrogen molecules are decomposed into hydrogen atoms before entering the metal sample, so the speed of decomposing the hydrogen molecules into the hydrogen atoms affects the charging speed. The hydrogen storage alloy has the catalytic action of decomposing hydrogen molecules into hydrogen atoms, so that the metal sample and the hydrogen storage alloy are simultaneously placed in the inner cavity of the hydrogen charging device, the metal sample can be directly charged with hydrogen when the inner cavity environment of the hydrogen charging device becomes a high-pressure hydrogen environment, and meanwhile, the hydrogen storage alloy can accelerate the decomposition of the hydrogen molecules into the hydrogen atoms, so that the hydrogen charging speed is increased. Therefore, in the method, the pressurization and the hydrogen charging are integrated, and the hydrogen charging device has simple structure and high hydrogen charging efficiency.
Drawings
FIG. 1 is a schematic diagram of a pressurization and hydrogen charging method for a metal hydrogen embrittlement test in a high-pressure hydrogen environment according to the present invention;
FIG. 2 is a schematic diagram of the pressurization and hydrogen charging method of the high pressure hydrogen environment metal hydrogen embrittlement test of comparative example 1.
In the figure: 11. a hydrogen charging device; 110. an inner cavity; 12. a hydrogen storage alloy; 13. a metal sample; 14. a hydrogen source device; 15. high-temperature high-pressure hydrogen charging device.
Detailed Description
The pressurizing and hydrogen charging method for the metal hydrogen embrittlement test in the high-pressure hydrogen environment provided by the invention is further explained below.
As shown in fig. 1, the pressurization and hydrogen charging method for the metal hydrogen embrittlement test in the high-pressure hydrogen environment provided by the invention comprises the following steps:
s1, providing a hydrogen charging device 11, wherein the hydrogen charging device 11 is provided with an inner cavity 110;
s2, placing the hydrogen storage alloy 12 and the metal sample 13 together in the inner cavity 110 of the hydrogen charging device 11, and charging hydrogen into the inner cavity 110 of the hydrogen charging device 11 to ensure that the hydrogen storage alloy 12 is saturated by absorbing hydrogen;
and S3, heating the hydrogen charging device 11 to enable the hydrogen storage alloy 12 saturated in hydrogen absorption to release high-pressure hydrogen, enabling the environment of the inner cavity 110 of the hydrogen charging device 11 to be a high-pressure hydrogen environment, and charging the metal sample 13.
In the step S1, the hydrogen charging device 11 may be a reaction kettle capable of heating, so that the hydrogen charging device 11 is directly heated in the step S3.
In order to obtain a high pressure hydrogen environment of 350bar or more at a lower temperature, particularly at 200 ℃, and to reduce the hydrogen absorption saturation conditions of the hydrogen storage alloy 2, so that the hydrogen storage alloy 12 can be saturated by absorbing hydrogen at room temperature, in step S2, the hydrogen storage alloy 12 is selected from AB2Hydrogen-absorbing alloy, AB5At least one of type hydrogen storage alloy and AB type hydrogen storage alloy.
In one embodiment, the hydrogen storage alloy 12 is selected from the AB2When the hydrogen storage alloy is of the type AB2The general formula of the hydrogen storage alloy is RxT2Wherein R is selected from at least one of Ti, zr and Ca, T is selected from at least one of V, cr, fe, mn, mo, cu and Ni, and x is more than or equal to 0.9 and less than or equal to 1.3. Further, R is selected from at least one of Ti and Zr, and T is selected from at least one of Cr, fe and Mn.
The volume of the inner cavity 110 of the hydrogen charging device 11 is V1The volume of the metal sample 13 is V2When said hydrogen storage alloy 12 is selected from said AB2When the hydrogen storage alloy is formed, the AB is2The mass of the hydrogen storage alloy in the inner cavity of the hydrogen charging device is W1，V1、V2And W1The following formula is satisfied: 2X (V)1-V2)≤W1≤4×(V1-V2) Wherein V is1In units of ml, V2Unit of (2) is milliliter, W1Has the unit of g, preferably, W1＝3×(V1-V2)。
At this time, hydrogen gas is charged into the hydrogen charging device 11 to charge the AB2In the step of hydrogen absorption saturation of the hydrogen storage alloy, the temperature is 0-30 ℃, and the pressure is 50-120 bar.
In one embodiment, the hydrogen storage alloy 12 is selected from the AB5Type AB hydrogen storage alloy5The general formula of the hydrogen storage alloy is MDyWherein M is at least one of rare earth elements, further at least one of La, pr, ce, ho, nd, pm, sm, eu and Gd, D is at least one of Ni, mn, al, co and Fe,y is more than or equal to 4.7 and less than or equal to 5.2. Further, M is selected from at least one of La, ce and Ho, and D is selected from at least one of Ni, mn and Al.
When the hydrogen storage alloy 12 is selected from the AB5When the hydrogen storage alloy is formed, the AB is5The mass of the hydrogen storage alloy in the inner cavity of the hydrogen charging device is W2，V1、V2And W2The following formula is satisfied: 2 × (V)1-V2)≤W2≤4×(V1-V2) Wherein, W2Has the unit of g, preferably, W2＝3×(V1-V2)。
At this time, hydrogen gas is charged into the hydrogen charging device 11 to charge the AB5In the step of hydrogen absorption saturation of the hydrogen storage alloy, the temperature is 0-30 ℃, and the hydrogen absorption pressure is 20-50 bar.
In one embodiment, the hydrogen storage alloy 12 is selected from the group consisting of the AB type hydrogen storage alloys, including the TiFe multi-element alloys.
When the hydrogen storage alloy 12 is selected from the AB type hydrogen storage alloy, the mass of the AB type hydrogen storage alloy in the inner cavity of the hydrogen charging device is W3，V1、V2And W3The following formula is satisfied: 2 × (V)1-V2)≤W3≤4×(V1-V2) Wherein W is3Has the unit of g, preferably, W3＝3×(V1-V2)。
At this time, in the step of filling hydrogen into the hydrogen filling device 11 to ensure that the AB type hydrogen storage alloy absorbs hydrogen and is saturated, the temperature is 0-30 ℃, and the hydrogen absorption pressure is 20-50 bar.
In one embodiment, the hydrogen storage alloy 12 is AB2Hydrogen-absorbing alloy, AB5A mixture of at least two of the type AB hydrogen storage alloy and the type B hydrogen storage alloy.
Specifically, during the hydrogen absorption saturation process of the hydrogen storage alloy 12, hydrogen gas is firstly absorbed on the surface of the hydrogen storage alloy 12 and decomposes hydrogen atoms, and the hydrogen atoms gradually diffuse into the hydrogen storage alloy 12 from the surface to form MHxSolid solution (alpha phase), finally MHxThe solid solution is saturatedLater reacted with hydrogen to produce metal hydride MHy(beta phase).
It should be noted that, before filling the inner cavity 110 of the charging device 11 with hydrogen gas to saturate the hydrogen storage alloy 12 with hydrogen, the hydrogen storage alloy 12 needs to be activated, and in actual operation, the activated hydrogen storage alloy 12 and the metal sample 13 may be placed together in the inner cavity 110 of the charging device 11.
In step S3, the hydrogen storage alloy 12 may be directly filled in the inner cavity 110 of the hydrogen charging device 11, the metal sample 13 may be fixedly disposed in the inner cavity 110 of the hydrogen charging device 11, the fixing may be erected, disposed on a fixed platform, or the like, and of course, the metal sample 13 may also be directly filled in the inner cavity 110 of the hydrogen charging device 11.
The hydrogen-releasing equilibrium hydrogen pressure P of the metal hydride is exponential to 1000/T (T is temperature, and the unit is K), and the metal hydride in the hydrogen storage alloy 12 decomposes and releases high-pressure hydrogen gas during the temperature increase. Therefore, in step S3, if the hydrogen storage alloy 12 saturated with hydrogen is AB when the charging device 11 is heated2When the hydrogen storage alloy is used, 400bar of hydrogen can be released when the heating temperature is about 60 ℃, and 700bar of hydrogen can be released when the heating temperature is about 90 ℃; the hydrogen occluding alloy 12 is AB if saturated with hydrogen absorption5The hydrogen storage alloy can release 400bar of hydrogen when the heating temperature is about 150 ℃; if the hydrogen storage alloy 12 which is saturated by absorbing hydrogen is AB type hydrogen storage alloy, 400bar of hydrogen can be released when the heating temperature is about 160 ℃.
Therefore, the hydrogen storage alloy 12 is added into the hydrogen charging device 11, when the hydrogen storage alloy 12 is saturated with hydrogen at a low temperature to form metal hydride, the metal hydride can be decomposed and high-pressure hydrogen can be released only by raising the temperature by a small margin, and further the environment of the inner cavity 110 of the hydrogen charging device 11 becomes a high-pressure hydrogen environment, and the pressure value can be flexibly adjusted. The method does not need a high-pressure hydrogen compressor or the high temperature of a gas expansion method, and has the advantages of low consumption, low cost and relatively high safety.
In practice, high pressure hydrogen of less than 400bar is requiredContext, AB can be selected2Hydrogen-absorbing alloy, AB5At least one of the AB type hydrogen storage alloy or the type hydrogen storage alloy can obtain a high-pressure hydrogen environment of more than 350bar under the heating condition of not more than 165 ℃; if a high pressure hydrogen environment of above 400bar is required, such as a high pressure hydrogen environment of 400bar to 700bar, AB is preferred2The hydrogen storage alloy can obtain a high-pressure hydrogen environment of 700bar under the heating condition of not more than 90 ℃.
On the other hand, the charging device 11 of the present invention integrates pressurization and charging. In the invention, the metal sample 13 and the hydrogen storage alloy 12 are simultaneously arranged in the inner cavity 110 of the hydrogen charging device 11, and when the environment of the inner cavity 110 of the hydrogen charging device 11 becomes a high-pressure hydrogen environment, the metal sample 13 can be directly charged with hydrogen. Meanwhile, in the process of charging the metal sample 13, hydrogen molecules are decomposed into hydrogen atoms and then enter the metal sample 13, so that the speed of decomposing the hydrogen molecules into the hydrogen atoms affects the charging speed, and the hydrogen storage alloy 12 has the catalytic action of decomposing the hydrogen molecules into the hydrogen atoms, so that when the metal sample 13 and the hydrogen storage alloy 12 are simultaneously placed in the inner cavity 110 of the charging device 11, the charging speed of the metal sample 13 can be improved.
Hereinafter, the pressurizing and hydrogen charging method for the high-pressure hydrogen environment metal hydrogen embrittlement test will be further described by the following specific examples.
Example 1:
AB adopted2Type Ti alloy containing TiZr as a component0.02Cr1.1Fe0.5Mn0.4. Weighing Ti, zr, cr, fe and Mn metals according to a specific ratio, wherein the purity of Ti, zr, cr, fe and Mn raw materials used by the alloy is more than 99 percent, and the TiZr0.02Cr1.1Fe0.5Mn0.4The total mass of the alloy is 650g; then putting the alloy components weighed according to the proportion into a water-cooled copper crucible according to the sequence of melting points, vacuumizing for 3 times, and then filling a proper amount of argon for smelting, in order to ensure the uniformity of the alloy components, completely smelting other metals except Mn, adding Mn for repeatedly smelting for 3 times to reach the target weight, and washing the copper crucible for 3 times before each smeltingAnd evacuation operations to minimize contamination with impurities.
Fully smelted TiZr0.02Cr1.1Fe0.5Mn0.4Mechanically pulverizing the alloy into alloy powder with diameter less than 1mm after polishing off oxide skin on the surface of the alloy, activating, adding into an inner cavity of a hydrogen charging device together with a metal sample, charging 120bar hydrogen at room temperature, maintaining the pressure for 30min, and allowing TiZr to pass0.02Cr1.1Fe0.5Mn0.4The alloy is saturated with hydrogen.
Then, the hydrogen charging device is heated to make TiZr0.02Cr1.1Fe0.5Mn0.4The temperature of the alloy is raised to 58 ℃ to make TiZr0.02Cr1.1Fe0.5Mn0.4High-pressure hydrogen is discharged from the alloy, and the pressure reaches 400bar; continuously adding TiZr0.02Cr1.1Fe0.5Mn0.4The alloy temperature was raised to 87 ℃ and the pressure reached 700bar.
Example 2:
AB adopted5The hydrogen storage alloy comprises MmNi5Wherein Mm is a mixture of La, pr and Ce, and the atomic ratio is 30. La, pr, ce and Ni are weighed according to a specific proportion, the purity of La, pr, ce and Ni raw materials used by the alloy is more than 99 percent, and MmNi5The total mass of the alloy is 650g; then putting the alloy components weighed according to the proportion into a water-cooled copper crucible according to the sequence of melting points, vacuumizing for 3 times, and then filling a proper amount of argon for smelting, repeatedly smelting for 3 times in order to ensure the uniformity of the alloy components, and performing gas washing and vacuumizing operations on the copper crucible 3 times before each smelting to reduce impurity pollution as much as possible.
MmNi completely smelted5Mechanically pulverizing alloy powder with diameter less than 1mm after removing oxide skin on the surface of the alloy, activating, adding into the inner cavity of a hydrogen charging device together with metal sample, charging 50bar hydrogen at room temperature, maintaining the pressure for 30min, and allowing MmNi to exist5The alloy is saturated with hydrogen.
Then, the hydrogen charging device is heated to make MmNi5The temperature of the alloy is raised to 158 ℃ so thatMmNi5The alloy releases high pressure hydrogen, and the pressure reaches 400bar.
Example 3:
the AB type hydrogen storage alloy is Ti0.95La0.05Fe0.9Mn0.1The Ti, la, fe and Mn metals are weighed according to the component proportion, the purity of the Ti, la, fe and Mn raw materials used by the alloy is more than 99 percent, and the Ti0.95La0.05Fe0.9Mn0.1The total mass of the alloy is 650g; then putting the alloy components weighed according to the proportion into a water-cooled copper crucible according to the sequence of melting points, vacuumizing for 3 times, and then filling a proper amount of argon for smelting, repeatedly smelting for 3 times in order to ensure the uniformity of the alloy components, and performing gas washing and vacuumizing operations on the copper crucible 3 times before each smelting to reduce impurity pollution as much as possible.
Melting-through Ti0.95La0.05Fe0.9Mn0.1Mechanically pulverizing the alloy into alloy powder with diameter less than 1mm after polishing off oxide skin on the surface, activating, adding into the inner cavity of a hydrogen charging device together with the test sample, charging 50bar hydrogen at room temperature and maintaining the pressure for 30min to allow Ti to pass through0.95La0.05Fe0.9Mn0.1The alloy is saturated with hydrogen.
Then, the hydrogen charging device is heated to make Ti0.95La0.05Fe0.9Mn0.1The temperature of the alloy is raised to 161 ℃ to make Ti0.95La0.05Fe0.9Mn0.1The alloy releases high pressure hydrogen, and the pressure reaches 400bar.
Comparative example 1:
as shown in fig. 2, the comparative example 1 includes a hydrogen source device 14 and a high-temperature and high-pressure hydrogen charging device 15, the hydrogen source device 14 and the high-temperature and high-pressure hydrogen charging device 15 are connected by a pipeline, and a control valve is arranged on the pipeline. Comparative example 1 differs from example 2 only in that the LaNi after activation5The alloy is arranged in the inner cavity of the hydrogen source device 14, and the metal sample 13 is arranged in the high-temperature high-pressure hydrogen charging device 15.
50bar of hydrogen gas is filled into the inner cavity of the hydrogen source device 14 at room temperature and the pressure is keptForce for 30min, let LaNi5The alloy absorbs hydrogen to be saturated, then the hydrogen source device 14 is heated, and a valve is opened to charge hydrogen into the high-temperature high-pressure hydrogen charging device 15, so that LaNi is charged5The temperature of the alloy is raised to 285 ℃, laNi5The alloy releases high-pressure hydrogen, and the pressure of the high-temperature high-pressure hydrogen charging device 15 reaches 400bar; continuing to mix LaNi5The temperature of the alloy is raised to 330 ℃, and the pressure of the high-temperature high-pressure hydrogen charging device 15 reaches 700bar.
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent should be subject to the appended claims.
Claims (9)
1. A pressurization and hydrogen charging method for a metal hydrogen embrittlement test in a high-pressure hydrogen environment is characterized by comprising the following steps:
providing a hydrogen charging device, wherein the hydrogen charging device is provided with an inner cavity;
placing a hydrogen storage alloy and a metal sample in an inner cavity of the hydrogen charging device together, and filling hydrogen into the inner cavity of the hydrogen charging device to ensure that the hydrogen storage alloy absorbs hydrogen and is saturated, wherein the hydrogen storage alloy is selected from AB2Hydrogen-absorbing alloy, AB5At least one of a type-AB hydrogen storage alloy and a type-AB hydrogen storage alloy; and
and heating the hydrogen charging device to ensure that the hydrogen storage alloy saturated by hydrogen absorption releases high-pressure hydrogen, so that the inner cavity environment of the hydrogen charging device becomes a high-pressure hydrogen environment, and charging the metal sample.
2. The method for increasing pressure and charging hydrogen for high pressure hydrogen environment metal hydrogen embrittlement test of claim 1, wherein the hydrogen storage alloy is selected from the group consisting of AB2Type AB hydrogen storage alloy2The general formula of the hydrogen storage alloy is RxT2Wherein R is selected from at least one of Ti, zr and Ca, T is selected from at least one of V, cr, fe, mn, mo, cu and Ni, and x is more than or equal to 0.9 and less than or equal to 1.3.
3. The method for increasing the pressure and charging hydrogen for the metal hydrogen embrittlement test in the high-pressure hydrogen environment according to claim 2, wherein the volume of the inner cavity of the charging device is V1The volume of the metal sample is V2The AB2The mass of the hydrogen storage alloy in the inner cavity of the hydrogen charging device is W1，V1、V2And W1The following formula is satisfied: 2 × (V)1-V2)≤W1≤4×(V1-V2) Wherein V is1In units of ml, V2Unit of (2) is milliliter, W1The unit of (c) is g.
4. The method for increasing the pressure and charging hydrogen for the metal hydrogen embrittlement test in the high-pressure hydrogen environment according to claim 2, wherein the hydrogen gas is charged into the charging device to enable the AB to be used2In the step of hydrogen absorption saturation of the hydrogen storage alloy, the temperature is 0-30 ℃, and the pressure is 50-120 bar.
5. The method for increasing pressure and charging hydrogen for high pressure hydrogen environment metal hydrogen embrittlement test of claim 1, wherein the hydrogen storage alloy is selected from the group consisting of AB5Type AB hydrogen storage alloy5The general formula of the hydrogen storage alloy is MDyWherein M is selected from at least one of rare earth elements, D is selected from at least one of Ni, mn, al, co and Fe, and y is more than or equal to 4.7 and less than or equal to 5.2.
6. The method for increasing pressure and charging hydrogen for high-pressure hydrogen environment metal hydrogen embrittlement test according to claim 5, wherein the method comprisesCharacterized in that the volume of the inner cavity of the hydrogen charging device is V1The volume of the metal sample is V2The AB2The mass of the hydrogen storage alloy in the inner cavity of the hydrogen charging device is W2，V1、V2And W2The following formula is satisfied: 2 × (V)1-V2)≤W2≤4×(V1-V2) Wherein, V1In units of ml, V2Unit of (2) is milliliter, W2The unit of (c) is g.
7. The method for increasing the pressure and charging hydrogen for the metal hydrogen embrittlement test in the high-pressure hydrogen environment according to claim 5, wherein the AB is caused to be in contact with hydrogen gas charged into the charging device5In the step of hydrogen absorption saturation of the hydrogen storage alloy, the temperature is 0-30 ℃, and the hydrogen absorption pressure is 20-50 bar.
8. The method for increasing pressure and charging hydrogen for metal hydrogen embrittlement test in high-pressure hydrogen environment according to claim 1, wherein the hydrogen storage alloy is selected from AB type hydrogen storage alloys, the AB type hydrogen storage alloy comprises TiFe multi-element alloy, and the volume of the inner cavity of the charging device is V1The volume of the metal sample is V2The mass of the AB type hydrogen storage alloy in the inner cavity of the hydrogen charging device is W3，V1、V2And W3The following formula is satisfied: 2 × (V)1-V2)≤W3≤4×(V1-V2) Wherein V is1In units of ml, V2Unit of (2) is milliliter, W3The unit of (c) is g.
9. The method for increasing the pressure and charging hydrogen for the metal hydrogen embrittlement test in the high-pressure hydrogen environment according to claim 8, wherein in the step of charging hydrogen into the charging device to saturate the AB type hydrogen storage alloy in hydrogen absorption, the temperature is 0 ℃ to 30 ℃ and the pressure is 20bar to 50bar.
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