In-situ tensile hydrogen desorption testing device and testing method

Abstract

The invention discloses an in-situ tensile hydrogen desorption testing device and method, the device comprises a vacuum chamber, two tensile transmission rods movably penetrate through the chamber wall of the vacuum chamber to form a vacuum chamber, one end of each tensile transmission rod is located in the vacuum chamber, the other end of each tensile transmission rod is located outside the vacuum chamber, and the other end of each tensile transmission rod is located outside the vacuum chamber; an in-situ hydrogen desorption sample to be tested is fixed in the vacuum chamber through the stretching transmission rod and is stretched through the stretching transmission rod; a movable heating probe is also arranged, so that the in-situ hydrogen desorption sample can be heated; in the hydrogen desorption testing process, the mass spectrometer is used for detecting the hydrogen content in real time, the hydrogen content is transmitted to the electronic equipment to be recorded, a hydrogen desorption spectral line is formed, a rule between stress-strain and hydrogen desorption behaviors is established, and the problem of hydrogen desorption spectral line collection in the in-situ stretching process is effectively solved; meanwhile, the defect that a traditional hydrogen desorption technology cannot explore the influence rule of stress strain on the hydrogen trap capacity is overcome, and theoretical and experimental basis is provided for the hydrogen embrittlement mechanism of the metal material.

Description

Technical Field

[0001] This application relates to the field of metallic hydrogen desorption technology, specifically to an in-situ tensile hydrogen desorption testing device and method. Background Technology

[0002] With the rapid development of the hydrogen economy, the demand for high-performance metallic materials for facilities such as high-pressure hydrogen storage tanks, hydrogen pipelines, and fuel cells has surged. High-strength steel, titanium alloys, and aluminum alloys are susceptible to hydrogen intrusion during service, leading to reduced plasticity. This hydrogen embrittlement problem poses a fatal threat to the safe operation of equipment. Therefore, deepening our understanding of the interaction between hydrogen and the microstructure of materials, and deciphering the microscopic mechanisms of hydrogen embrittlement, is of great significance for energy transition and the development of high-end manufacturing.

[0003] Hydrogen desorption technology, as an important method for exploring the trapping properties of hydrogen in the microstructure of materials, is widely used in the study of hydrogen embrittlement mechanisms. Thermal desorption technology causes hydrogen to desorb from materials through heating, obtaining characteristic parameters such as the hydrogen content and hydrogen trap types in the materials, thus providing strong evidence for the study of hydrogen embrittlement mechanisms.

[0004] However, traditional hydrogen desorption techniques can only rely on thermal energy to induce hydrogen desorption and can only study hydrogen trapping behavior in materials under static conditions. Hydrogen embrittlement often occurs with deformation, and during the elastoplastic process, hydrogen and defects such as dislocations will continue to interact, and the hydrogen trapping behavior will also change. Therefore, obtaining information on hydrogen desorption behavior driven by mechanical energy such as tensile stress at room temperature and exploring the changes in hydrogen trapping characteristics under specific stress and strain are crucial for revealing the intrinsic mechanism of hydrogen embrittlement. Summary of the Invention

[0005] This application provides an in-situ tensile hydrogen desorption testing device and method to address the current situation where traditional hydrogen desorption relies solely on thermal energy and is limited to observing hydrogen traps under static conditions.

[0006] The first aspect of this application provides an in-situ tensile hydrogen desorption testing apparatus, comprising: A vacuum chamber provides a vacuum environment; The tensile transmission rod assembly includes two tensile transmission rods, each of which is configured to movably pass through the wall of the vacuum chamber to form one end located inside the vacuum chamber as a sample fixing end and the other end located outside the vacuum chamber as a tensile force receiving end. An in-situ hydrogen desorption sample to be tested is fixed between the two sample fixing ends, and the tensile force receiving end stretches and deforms the in-situ hydrogen desorption sample under the action of external force. The heating assembly includes a heating probe and a movement control device. The heating probe is fixed to one end of the movement control device, and the distance between the heating probe and the in-situ hydrogen desorption sample is adjustable under the action of the movement control device. A vacuum pumping device acts within the vacuum chamber and adjusts the vacuum level within the vacuum chamber; A mass spectrometer is used to detect the hydrogen content within the vacuum chamber; An electronic device having a computer program running on it, the computer program controlling the external force applied to the tensile transmission rod to stretch the in-situ hydrogen desorption sample at a set strain rate, recording hydrogen desorption data in real time after the stretching begins, and obtaining the relationship between the hydrogen desorption data and the strain rate after the stretching ends; and... The device is configured to control the movement of the mobile control unit to bring the heating probe into contact with the in-situ hydrogen desorption sample and to control the heating probe to heat the in-situ hydrogen desorption sample at a set heating rate. It also records hydrogen desorption data in real time after heating begins and obtains the relationship between the hydrogen desorption data and the heating rate after heating ends. The device controls the external force on the tension transmission rod to make the in-situ hydrogen desorption sample obtain a set stress or strain. Based on this, it controls the movement control device to drive the heating probe to contact the in-situ hydrogen desorption sample and controls the heating probe to heat the in-situ hydrogen desorption sample at a set heating rate. After heating, it obtains the relationship between stress or strain, hydrogen desorption data and heating rate.

[0007] Furthermore, the in-situ hydrogen desorption sample has a plate-like structure.

[0008] Furthermore, the tensile end is connected to a stress-strain testing machine.

[0009] Furthermore, the movement control device is a pneumatic valve, the main body of which is fixed outside the vacuum chamber, and the telescopic end of which is configured to pass through the wall of the vacuum chamber and be fixedly connected to the heating probe.

[0010] Furthermore, the telescopic end of the pneumatic valve is sealed to the wall of the vacuum chamber using a bellows.

[0011] A second aspect of this application provides a method of using the in-situ tensile hydrogen desorption testing device based on any one of claims 1-5, comprising: The in-situ hydrogen desorption sample is fixed between the two ends of the tensile transmission rod assembly located inside the vacuum chamber. Adjust the vacuum level in the vacuum chamber to 3×10 -4 Pa; In-situ tensile hydrogen desorption tests, hydrogen thermal desorption tests, and hydrogen thermal desorption tests were conducted on in-situ hydrogen desorption samples under certain stress or strain, as required. The relationships between different strain rates and hydrogen content, different heating rates and hydrogen content, and different heating rates and hydrogen content under certain stress or strain were obtained during the test.

[0012] Furthermore, the in-situ hydrogen desorption sample is subjected to a hydrogen thermal desorption test under a certain stress or strain, including: After controlling the external force on the tensile transmission rod to make the in-situ hydrogen desorption sample obtain the set stress or strain, the tensile deformation is stopped. The movement control device is activated to move the heating probe to contact the surface of the in-situ hydrogen desorption sample. The heating rate of the heating probe is set to heat the in-situ hydrogen desorption sample, and the hydrogen desorption data during the heating process is recorded.

[0013] Furthermore, methods for obtaining the relationship between different strain rates and hydrogen content include: Plot the time and concentration in the in-situ stretching hydrogen desorption data, with time on the X-axis and concentration on the Y-axis, to obtain the first relationship graph between the change in hydrogen desorption concentration and time. Convert the time axis in the first relationship graph to the nominal strain axis, where nominal strain = time × strain rate, to obtain a second relationship graph between the change in hydrogen desorption concentration and strain. Preferably, the curve of the first relationship graph is differentiated once, and the additional hydrogen desorption caused by the deformation process is analyzed based on the differentiation.

[0014] Furthermore, methods for obtaining the relationship between different heating rates and hydrogen content include: Plot the time and concentration in the hydrogen thermal desorption test data, with time on the X-axis and concentration on the Y-axis, to obtain a third relationship graph between the change in hydrogen desorption concentration and time. The time axis in the third relationship graph is converted to a temperature axis, where temperature = room temperature + time × heating rate, to obtain a fourth relationship graph between the change in hydrogen desorption concentration and temperature.

[0015] Furthermore, the relationship between different heating rates and hydrogen content under certain stress or strain is obtained, including: Plot the time and concentration of hydrogen thermal desorption test data under each stress or strain, with time on the X-axis and concentration on the Y-axis, to obtain the fifth relationship graph between the change of hydrogen desorption concentration and time under each stress or strain. Convert the time axis in the fifth relationship graph to a temperature axis, where temperature = room temperature + time × heating rate, to obtain a sixth relationship graph between the change in hydrogen desorption concentration and temperature under each stress or strain.

[0016] Beneficial effects: This invention provides an in-situ tensile hydrogen desorption testing device and method, which is simple in structure and easy to use. By changing the strain rate, stress-strain magnitude and heating rate, it can realize the real-time measurement of hydrogen desorption spectra at different stages during the tensile process of in-situ hydrogen desorption samples, establish the law between stress-strain and hydrogen desorption behavior, effectively solve the problem of hydrogen desorption spectrum acquisition during in-situ tensile process, and overcome the shortcomings of traditional hydrogen desorption technology in exploring the influence of stress-strain on hydrogen trapping ability, thus providing a theoretical and experimental basis for the hydrogen embrittlement mechanism of metallic materials. Attached Figure Description

[0017] The accompanying drawings, which form part of this application, are used to provide a further understanding of this application. The illustrative embodiments and descriptions of this application are used to explain this application and do not constitute an undue limitation of this application. In the drawings: Figure 1 This is a schematic diagram of the structure of an in-situ tensile hydrogen desorption test device according to an embodiment of the present invention; Figure 2 This is a schematic diagram showing the changes in hydrogen desorption concentration obtained from in-situ stretching hydrogen desorption tests according to an embodiment of the present invention. Figure 3 This is a schematic diagram showing the change in hydrogen desorption concentration obtained from a hydrogen thermal desorption test according to an embodiment of the present invention.

[0018] The meanings of the various reference numerals in the figure are as follows: 1. Vacuum chamber; 2. Tensile transmission rod; 3. In-situ hydrogen desorption sample; 4. Vacuum sealing cover; 5. Vacuum chamber support rod; 6. Vacuum pump; 7. Mass spectrometer; 8. Electronic equipment; 9. Motion control device; 10. Bellows; 11. Heating probe; 12. Vacuum gauge. Detailed Implementation

[0019] It should be noted that, unless otherwise specified, the embodiments and features described in this application can be combined with each other. This application will now be described in detail with reference to the accompanying drawings and embodiments.

[0020] In the description of this application, it should be understood that the terms "center," "longitudinal," "lateral," "length," "width," "thickness," "upper," "lower," "front," "rear," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," "outer," "clockwise," and "counterclockwise," etc., indicating orientation or positional relationships based on the orientation or positional relationships shown in the accompanying drawings, are only for the convenience of describing this application and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, or be constructed and operated in a specific orientation, and therefore should not be construed as a limitation of this application. Furthermore, the terms "first" and "second" are used for descriptive purposes only and should not be construed as indicating or implying relative importance or implicitly specifying the number of indicated technical features. Thus, features defined with "first" and "second" may explicitly or implicitly include one or more of the stated features. In the description of this application, "a plurality of" means two or more, unless otherwise explicitly specified.

[0021] In the description of this application, it should be noted that, unless otherwise expressly specified and limited, the terms "installation," "connection," and "linking" should be interpreted broadly. For example, they can refer to a fixed connection, a detachable connection, or an integral connection; they can refer to a mechanical connection, an electrical connection, or a connection that allows communication between them; they can refer to a direct connection or an indirect connection through an intermediate medium; they can refer to the internal communication between two components or the interaction between two components. Those skilled in the art can understand the specific meaning of the above terms in this application according to the specific circumstances.

[0022] like Figure 1 The diagram shown is a structural schematic of an in-situ tensile hydrogen desorption testing device provided in an embodiment of this application. Figure 1 It can be seen that the in-situ tensile hydrogen desorption testing device includes: Vacuum chamber 1 provides a vacuum environment. In this embodiment, vacuum chamber 1 is a cuboid cavity constructed from 1 cm thick 316L stainless steel plates, with an internal volume of 0.1 cubic meters. Vacuum chamber 1 is supported on the ground or platform by vacuum chamber support rods 5. To achieve a vacuum environment, vacuum chamber 1 is equipped with a vacuum pumping device, which includes a vacuum pump 6 and a vacuum gauge 12 connected by stainless steel pipes. The vacuum pump 6 consists of a mechanical pump and a turbomolecular pump, used to adjust the vacuum level within the cavity and detect the vacuum level using the vacuum gauge 12, thereby constructing a suitable testing environment.

[0023] The tensile transmission rod assembly includes two tensile transmission rods 2, each of which is a cylinder with a diameter of 20 mm. A through hole is provided on each opposite side of the vacuum chamber 1 for the tensile transmission rod 2 to pass through. Each tensile transmission rod 2 is configured to movably pass through the wall of the vacuum chamber 1, forming a sample fixing end inside the vacuum chamber 1 and a tensile force-bearing end outside the vacuum chamber 1. To ensure the airtightness of the vacuum chamber 1, a vacuum sealing cover 4 is provided around the through hole. An in-situ hydrogen desorption sample 3 to be tested is fixed between the two sample fixing ends. The in-situ hydrogen desorption sample 3 has a plate-like structure with a hydrogen gauge length of 15 mm and a thickness of 1.5 mm. The two ends of the plate-like structure along its length are connected and fixed to the fixing ends of the tensile transmission rods 2 by bolts. The tensile stress end can be connected to a stress-strain testing machine. In this embodiment, the Xi'an Licheng NL-50 stress-strain testing machine is selected. This equipment can realize the predetermined stress-strain rate change, and the tensile mechanical properties of the sample can be measured in advance. When a tensile hydrogen desorption test is required, the stress-strain testing machine provides tensile force to cause the in-situ hydrogen desorption sample 3 to undergo tensile deformation, and controls the stress and strain on the in-situ hydrogen desorption sample 3 to change in a preset manner.

[0024] The heating assembly includes a heating probe 11 and a movement control device 9. The heating probe 11 is fixed to one end of the movement control device 9. The heating probe 11 has a rectangular cross-section and is made of copper alloy. A thermocouple and a heating resistance wire are installed inside the probe, and the maximum heating temperature is 500 degrees Celsius. The movement control device 9 is a pneumatic valve. The main body of the pneumatic valve is fixed outside the vacuum chamber 1. The telescopic end of the pneumatic valve is configured to pass through the wall of the vacuum chamber 1 and then be fixedly connected to the heating probe 11. A bellows 10 seals the telescopic end of the pneumatic valve with the wall of the vacuum chamber 1. The distance between the heating probe 11 and the in-situ hydrogen desorption sample 3 is adjustable under the action of the movement control device 9. When hydrogen thermal desorption is required, the heating probe 11 is moved to contact and heat the plate surface of the in-situ hydrogen desorption sample 3. The heating temperature and heating rate of the heating probe 11 are adjustable, and the hydrogen desorption can be observed by setting different heating rates.

[0025] Mass spectrometer 7, optionally a quadrupole mass spectrometer, is fixed on the vacuum chamber 1 and used to detect the hydrogen content in the vacuum chamber 1 to generate hydrogen desorption data.

[0026] Electronic device 8 includes a memory, a processor, and a computer program stored in the memory and executable on the processor. The stress-strain testing machine, heating probe 11, motion control device 9, mass spectrometer 7, vacuum pump 6, and vacuum gauge 12 are all electrically connected to and controlled by electronic device 8. They perform tests according to the test steps and parameters set by the computer program and feed back the collected data to electronic device 8.

[0027] Specifically, the computer program controls the external force applied to the tensile transmission rod 2, causing the in-situ hydrogen desorption sample 3 to be stretched at a set strain rate. After the stretching begins, it records the hydrogen desorption data collected from the mass spectrometer 7 in real time. After the stretching is completed, it processes the hydrogen desorption data and strain rate data to obtain the relationship between the hydrogen desorption data and the strain rate; and... The device is used to control the movement of the mobile control unit 9 to bring the heating probe 11 into contact with the in-situ hydrogen desorption sample 3 and to control the heating probe 11 to heat the in-situ hydrogen desorption sample 3 at a set heating rate. After heating begins, it records hydrogen desorption data collected by the mass spectrometer 7 in real time. After heating ends, it processes the hydrogen desorption data and heating rate data to obtain the relationship between the hydrogen desorption data and the heating rate. The device controls the external force on the tensile transmission rod 2 to make the in-situ hydrogen desorption sample 3 obtain a set stress or strain. Based on this, it controls the movement control device 9 to drive the heating probe 11 to contact the in-situ hydrogen desorption sample 3 and controls the heating probe 11 to heat the in-situ hydrogen desorption sample 3 at a set heating rate. After heating, it processes the stress or strain data, hydrogen desorption data, and heating rate data to obtain the relationship between stress or strain, hydrogen desorption data, and heating rate.

[0028] The aforementioned in-situ tensile hydrogen desorption testing device can independently perform tensile hydrogen desorption tests, hydrothermal desorption tests, and hydrothermal desorption tests on in-situ hydrogen desorption sample 3 after it has been stretched to a certain stress or strain. It has a wide range of applications. It can achieve real-time measurement of hydrogen desorption spectra at different stages during the tensile process of the in-situ hydrogen desorption sample 3, establish the relationship between stress and strain and hydrogen desorption behavior, effectively solve the problem of hydrogen desorption spectrum acquisition during in-situ tensile testing, and overcome the limitation of traditional hydrogen desorption techniques in being unable to explore the influence of stress and strain on hydrogen trapping ability.

[0029] In this embodiment, the in-situ hydrogen desorption sample 3 needs to be pretreated before testing, specifically including the following steps: Step S101: Select medium carbon martensitic steel as the test material, process it into the size of in-situ hydrogen desorption sample 3, and polish the hydrogen-filled surface of the in-situ hydrogen desorption sample 3 to 2000 mesh using sandpaper. Step S102: Wrap the non-test surface of the in-situ hydrogen desorption sample 3 with waterproof tape, and prepare an electrochemical hydrogen charging solution of 3% NaCl + 0.3% NH4SCN; Step S103: Electrochemical hydrogen charging of in-situ hydrogen desorption sample 3 is performed using a DC power supply, with a charging parameter of 5 mA / cm. 2 The hydrogen charging time is 12 hours; Step S104: The in-situ hydrogen desorption sample 3 after hydrogen charging is cleaned with anhydrous ethanol and dried with compressed gas.

[0030] In this embodiment, before conducting the test, an airtightness test is required on the in-situ tensile hydrogen desorption testing device to confirm its normal sealing performance. The specific process of the airtightness test involves adjusting the vacuum level in vacuum chamber 1 to 3 × 10⁻⁶ without placing a sample. -4 Pa, when a stress-strain testing machine is used to perform tensile testing under no-load conditions, if the vacuum level does not decrease during the tensile process, the sealing performance is normal.

[0031] After completing the preparation of in-situ hydrogen desorption sample 3 and passing the airtightness test, the pre-test environment preparation was carried out according to the following method: Step S201: Fix the in-situ hydrogen desorption sample 3 between the two ends of the tensile transmission rod 2 assembly located inside the vacuum chamber 1; Step S202: Adjust the vacuum level in the vacuum chamber 1 to 3×10⁻⁶. -4 Pa.

[0032] Subsequently, in-situ tensile hydrogen desorption tests, hydrogen thermal desorption tests, and hydrogen thermal desorption tests can be performed as needed, and the in-situ hydrogen desorption sample 3 can be subjected to hydrogen thermal desorption tests under certain stress or strain. The relationships between different strain rates and hydrogen content, different heating rates and hydrogen content, and different heating rates and hydrogen content under certain stress or strain can be obtained during the test.

[0033] Test 1: Conduct in-situ tensile hydrogen desorption test, the specific method is as follows: Step S301: Connect the tensile force-bearing end of the tensile transmission rod 2 to the stress-strain testing machine, set the required strain rate, and control the stress-strain testing machine to perform tensile deformation on the in-situ hydrogen desorption sample 3. For example, set the strain rate to 1×10⁻⁶. -5 s -1 , 2×10 -5 s -1 3×10 -5 s-1 5×10 -5 s -1 Four in-situ hydrogen desorption samples 3 were subjected to tensile deformation. Step S302: After the in-situ hydrogen desorption sample 3 begins to stretch and deform, the mass spectrometer 7 is turned on to detect the hydrogen content, i.e. the concentration of hydrogen in the vacuum chamber 1, and transmits it to the memory of the electronic device 8 in real time. The memory records the hydrogen content and the corresponding time, thus forming the hydrogen desorption data during the stretching process. Step S303: After the tensile deformation is completed, control the stress-strain testing machine to unload the tensile transmission rod 2, remove the stress on the in-situ hydrogen desorption sample 3, turn off the vacuum pump 6, and after the vacuum gauge 12 shows atmospheric pressure, take out the in-situ hydrogen desorption sample 3, save the experimental data, and complete the experiment.

[0034] The experimental data were processed as follows: The computer program plotted the time and concentration in the in-situ stretching hydrogen desorption data, with time as the X-axis and concentration as the Y-axis, to obtain the first relationship graph between the change in hydrogen desorption concentration and time. Convert the time axis in the first relationship graph to the nominal strain axis, where nominal strain = time × strain rate, to obtain a second relationship graph between the change in hydrogen desorption concentration and strain. In some preferred embodiments, the curve of the first relationship graph is differentiated once, and the additional hydrogen desorption caused by the deformation process is analyzed based on the differentiation.

[0035] like Figure 2 As shown, the curve after differentiation and the second relationship graph are combined. Figure 2 It can be seen that the hydrogen desorption rate is initially small as strain begins, but increases when the strain reaches about 0.05, indicating that deformation promotes hydrogen desorption. As the strain continues to increase, hydrogen desorption gradually increases, and the higher the strain rate, the higher the hydrogen desorption rate, indicating that dislocation motion accelerates the surface desorption of hydrogen.

[0036] Test 2: Conduct a hydrogen thermal desorption test. The specific method is as follows: Step S401: Connect the tensile force-bearing end of the tensile transmission rod 2 to the stress-strain testing machine, set the stress-strain testing machine to not apply force, or the stress-strain testing machine can be disconnected, start the pneumatic valve of the movement control device 9, extend the heating probe 11, and contact it with the in-situ hydrogen desorption sample 3. Step S402: Set the heating rate, such as 100℃ / h, to heat the in-situ hydrogen desorption sample 3. At the same time, turn on the mass spectrometer 7 to detect the hydrogen content, i.e. the concentration of hydrogen in the vacuum chamber 1, and transmit it to the memory of the electronic device 8 in real time. The memory records the hydrogen content and the corresponding time, i.e., the hydrogen desorption data during the heating process. Step S403: After heating to the specified temperature, turn off the heating probe 11 and start the pneumatic valve to retract the heating probe 11; control the strain testing machine to unload the tensile transmission rod 2, turn off the vacuum pump 6, and after the vacuum gauge 12 shows atmospheric pressure, take out the in-situ hydrogen desorption sample 33, save the experimental data, and complete the experiment.

[0037] The experimental data were processed as follows: the time and concentration in the hydrogen thermal desorption test data were plotted, with time on the X-axis and concentration on the Y-axis, to obtain a third relationship graph between the change in hydrogen desorption concentration and time; Converting the time axis in the third graph to a temperature axis, where temperature = room temperature + time × heating rate, yields a fourth graph relating hydrogen desorption concentration to temperature. Figure 3 The 0MPa curve.

[0038] Test 3: In-situ hydrogen desorption of sample 3 under certain stress or strain conditions was performed using a hydrogen thermal desorption test. The specific method is as follows: Step S401: Connect the tensile force-bearing end of the tensile transmission rod 2 to the stress-strain testing machine, and control the stress-strain testing machine to perform tensile deformation on the in-situ hydrogen desorption sample 3. After the in-situ hydrogen desorption sample 3 is deformed to the required stress or strain, stop the tensile deformation. For example, in this embodiment, two different stresses are selected, namely 100MPa and 500MPa, and the three hydrogen thermal desorption samples are stretched to the corresponding stresses respectively (the strain scheme is similar to the stress scheme, and will not be specifically illustrated here); start the pneumatic valve of the movement control device 9 to extend the heating probe 11 and contact it with the in-situ hydrogen desorption sample 3. Step S402: Set the heating rate, for example, set the heating rate to 100℃ / h, heat the in-situ hydrogen desorption sample 3, and at the same time turn on the mass spectrometer 7 to detect the hydrogen content, that is, the concentration of hydrogen in the vacuum chamber 1, and transmit it to the memory of the electronic device 8 in real time. The memory records the hydrogen content and the corresponding time, that is, to form hydrogen desorption data during the heating process. Step S404: After heating to the specified temperature, turn off the heating probe 11 and start the pneumatic valve to retract the heating probe 11; control the strain testing machine to unload the tensile transmission rod 2 to remove the stress on the in-situ hydrogen desorption sample 3, turn off the vacuum pump 6, and after the vacuum gauge 12 shows atmospheric pressure, take out the in-situ hydrogen desorption sample 33, save the experimental data, and complete the experiment.

[0039] The experimental data were processed as follows: a graph was plotted on the time and concentration of the hydrogen thermal desorption test data under each stress, with time on the X-axis and concentration on the Y-axis, to obtain the fifth relationship graph between the change of hydrogen desorption concentration and time under each stress. Convert the time axis in the fifth relationship graph to a temperature axis, where temperature = room temperature + time × heating rate, to obtain a sixth relationship graph between the change in hydrogen desorption concentration and temperature under each stress or strain, as shown below. Figure 3 As shown, by Figure 3 It can be seen that the application of uniaxial stress will cause the peak position of the desorption peak to change. Further comparison of the hydrogen desorption curves under no stress (0 MPa) and tensile stress of 100 MPa and 500 MPa shows that the application of tensile stress increases the peak temperature of hydrogen desorption, but when the stress is further increased to 500 MPa, the peak temperature of hydrogen desorption remains basically unchanged.

[0040] The above are merely embodiments of this application and are not intended to limit the scope of this application. Various modifications and variations can be made to this application by those skilled in the art. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of this application should be included within the scope of the claims of this application.

Claims

1. An in-situ tensile hydrogen desorption testing device, characterized in that, include: A vacuum chamber provides a vacuum environment; The tensile transmission rod assembly includes two tensile transmission rods, each of which is configured to movably pass through the wall of the vacuum chamber to form one end located inside the vacuum chamber as a sample fixing end and the other end located outside the vacuum chamber as a tensile force receiving end. An in-situ hydrogen desorption sample to be tested is fixed between the two sample fixing ends, and the tensile force receiving end stretches and deforms the in-situ hydrogen desorption sample under the action of external force. The heating assembly includes a heating probe and a movement control device. The heating probe is fixed to one end of the movement control device, and the distance between the heating probe and the in-situ hydrogen desorption sample is adjustable under the action of the movement control device. A vacuum pumping device acts within the vacuum chamber and adjusts the vacuum level within the vacuum chamber; A mass spectrometer is used to detect the hydrogen content within the vacuum chamber; An electronic device having a computer program running on it, the computer program controlling the external force applied to the tensile transmission rod to stretch the in-situ hydrogen desorption sample at a set strain rate, recording hydrogen desorption data in real time after the stretching begins, and obtaining the relationship between the hydrogen desorption data and the strain rate after the stretching ends; and... The device is configured to control the movement of the mobile control unit to bring the heating probe into contact with the in-situ hydrogen desorption sample and to control the heating probe to heat the in-situ hydrogen desorption sample at a set heating rate. It also records hydrogen desorption data in real time after heating begins and obtains the relationship between the hydrogen desorption data and the heating rate after heating ends. The device controls the external force on the tension transmission rod to make the in-situ hydrogen desorption sample obtain a set stress or strain. Based on this, it controls the movement control device to drive the heating probe to contact the in-situ hydrogen desorption sample and controls the heating probe to heat the in-situ hydrogen desorption sample at a set heating rate. After heating, it obtains the relationship between stress or strain, hydrogen desorption data and heating rate.

2. The apparatus according to claim 1, characterized in that, The in-situ hydrogen desorption sample has a plate-like structure.

3. The apparatus according to claim 1, characterized in that, The tensile stress end is connected to the stress-strain testing machine.

4. The apparatus according to claim 1, characterized in that, The movement control device is a pneumatic valve. The main body of the pneumatic valve is fixed outside the vacuum chamber, and the telescopic end of the pneumatic valve is configured to pass through the chamber wall of the vacuum chamber and then be fixedly connected to the heating probe.

5. The apparatus according to claim 4, characterized in that, The telescopic end of the pneumatic valve is sealed to the wall of the vacuum chamber using a bellows.

6. A method of using the in-situ tensile hydrogen desorption testing device based on any one of claims 1-5, characterized in that, include: The in-situ hydrogen desorption sample is fixed between the two ends of the tensile transmission rod assembly located inside the vacuum chamber. Adjust the vacuum level in the vacuum chamber to 3×10 -4 Pa; In-situ tensile hydrogen desorption tests, hydrogen thermal desorption tests, and hydrogen thermal desorption tests were conducted on in-situ hydrogen desorption samples under certain stress or strain, as required. The relationships between different strain rates and hydrogen content, different heating rates and hydrogen content, and different heating rates and hydrogen content under certain stress or strain were obtained during the test.

7. The method according to claim 6, characterized in that, The hydrogen thermal desorption test performed on the in-situ hydrogen desorption sample under a certain stress or strain includes: After controlling the external force on the tensile transmission rod to make the in-situ hydrogen desorption sample obtain the set stress or strain, the tensile deformation is stopped. The movement control device is activated to move the heating probe to contact the surface of the in-situ hydrogen desorption sample. The heating rate of the heating probe is set to heat the in-situ hydrogen desorption sample, and the hydrogen desorption data during the heating process is recorded.

8. The method according to claim 6, characterized in that, Methods for obtaining the relationship between different strain rates and hydrogen content include: Plot the time and concentration in the in-situ stretching hydrogen desorption data, with time on the X-axis and concentration on the Y-axis, to obtain the first relationship graph between the change in hydrogen desorption concentration and time. Convert the time axis in the first relationship graph to the nominal strain axis, where nominal strain = time × strain rate, to obtain a second relationship graph between the change in hydrogen desorption concentration and strain. Preferably, the curve of the first relationship graph is differentiated once, and the additional hydrogen desorption caused by the deformation process is analyzed based on the differentiation.

9. The method according to claim 6, characterized in that, Methods for obtaining the relationship between different heating rates and hydrogen content include: Plot the time and concentration in the hydrogen thermal desorption test data, with time on the X-axis and concentration on the Y-axis, to obtain a third relationship graph between the change in hydrogen desorption concentration and time. The time axis in the third relationship graph is converted to a temperature axis, where temperature = room temperature + time × heating rate, to obtain a fourth relationship graph between the change in hydrogen desorption concentration and temperature.

10. The method according to claim 7, characterized in that, To obtain the relationship between different heating rates and hydrogen content under certain stress or strain, including: Plot the time and concentration of hydrogen thermal desorption test data under each stress or strain, with time on the X-axis and concentration on the Y-axis, to obtain the fifth relationship graph between the change of hydrogen desorption concentration and time under each stress or strain. Convert the time axis in the fifth relationship graph to a temperature axis, where temperature = room temperature + time × heating rate, to obtain a sixth relationship graph between the change in hydrogen desorption concentration and temperature under each stress or strain.

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