In-situ hydrogen charging comprehensive test system and method

Abstract

The invention provides an in-situ hydrogen charging comprehensive test system, which comprises a solution pool, the top surface of the solution pool comprises an inclined plane area and a plane area, the inclined plane area is provided with a hydrogen charging hole, and the plane area is provided with a liquid charging port for charging a hydrogen charging solution; the inert electrode is inserted into the hydrogen filling solution through the liquid adding opening; the wedge-shaped sample to be tested comprises a matching inclined plane matched with the inclined plane area and a test observation surface; the positive electrode of the power supply is connected with the inert electrode, and the negative electrode is connected with the to-be-detected sample; the performance testing module is used for testing the sample to be tested; wherein the hydrogen charging solution can charge hydrogen into the to-be-tested sample through the hydrogen charging hole, and phase change, mechanical property change and acoustic property change of the to-be-tested sample in the hydrogen charging process can be observed in situ through the performance testing module, so that the diffusion condition of hydrogen in the to-be-tested sample in the hydrogen charging process and the damage condition of the to-be-tested sample are monitored.

Description

Technical Field

[0001] The present invention belongs to the technical field of hydrogen energy safety research, and specifically relates to an in-situ hydrogen charging comprehensive testing system and method, especially a system and method for studying hydrogen diffusion, phase change, hydrogen damage and material property changes during the hydrogen charging process of metal materials. Background Art

[0002] Hydrogen energy is a clean and efficient energy source, and an important way to transform and upgrade energy and achieve green development. When equipment / pipelines work in a hydrogen environment for a long time, the materials are prone to hydrogen damage, which leads to reduced material performance, usually resulting in reduced plasticity and strength, increased crack growth rate, and reduced fatigue life. It can also cause hydrogen-induced cracks, bulging, delamination, etc., causing failure under low stress conditions, seriously affecting the long-term safe operation of the equipment.

[0003] In the prior art, the test is conducted after hydrogen is pre-charged. However, due to the escape of hydrogen, there is a large difference between the test and the actual situation. Therefore, it is a better choice to conduct in-situ testing during the hydrogen charging process, and there is also some research on this in the prior art.

[0004] However, the existing in-situ hydrogen charging test technology still has some problems. For example, Chinese patent document CN110954586B provides an in-situ hydrogen display detection device and detection method, which generates white particles through the redox reaction of Ag+ and hydrogen, and then infers the distribution of hydrogen on the surface of the material through the distribution of white silver particles. This detection device and method are simple to implement, but are limited to studying the hydrogen distribution on the surface, and its detection results are not comprehensive and have poor reliability.

[0005] Chinese patent document CN111650093A provides a quantitative detection device for hydrogen permeation in metal micro-areas under in-situ loading conditions. In fact, during the in-situ loading process, electrochemical hydrogen charging is performed on a local micro-area with a controllable specific area, or multiple hydrogen charging and dehydrogenation tests are performed under various atmospheres and pH-adjustable corrosion environment conditions. However, it is mainly used to study the coupling effect of force and hydrogen diffusion, and does not involve the influence of hydrogen on material properties and microstructure.

[0006] Chinese patent document CN110133090A discloses an in-situ hydrogen charging experimental device, which realizes probe measurement under a thin liquid surface by using supporting nanoindentation, atomic force microscope, etc. The sample is immersed in the solution, which can only meet the equipment that can be inserted into the liquid for testing, and the solution easily corrodes the test probe. Similarly, only the surface of the sample is studied. However, hydrogen damage to the material is not always reflected on the surface. In the early and middle stages of the damage, it is generally concentrated inside the metal or in the subsurface position.

[0007] In addition, the prior art also has problems such as hydrogen bubbles gathering along the sample, affecting the experiment, samples immersed in hydrogen liquid being not conducive to testing, and samples having the same thickness, making changes caused by penetration into the sample surface difficult to capture.

[0008] Therefore, there is an urgent need for an in-situ hydrogen charging comprehensive testing system and method that can better study the entire process of hydrogen diffusion, enrichment and damage, and can measure changes in material properties during the entire process. Summary of the invention

[0009] In response to the technical problems mentioned above, the present invention aims to propose an in-situ hydrogen charging comprehensive testing system and method, which can study in situ the phase change, mechanical property changes, and acoustic property changes during the hydrogen charging process, and monitor the diffusion and damage of the material during the hydrogen charging process.

[0010] To this end, according to a first aspect of the present invention, there is provided an in-situ hydrogen charging comprehensive test system, comprising: a solution pool, wherein the top surface of the solution pool is configured to include an inclined surface area and a plane area, the inclined surface area is provided with a hydrogen charging hole, and the plane area is provided with a liquid filling port for filling a hydrogen charging solution; an inert electrode, which is inserted into the hydrogen charging solution through the liquid filling port; a wedge-shaped sample to be tested, which includes a matching inclined surface and a test observation surface for matching with the inclined surface area; a power supply, wherein the positive electrode of the power supply is connected to the inert electrode, and the negative electrode is connected to the sample to be tested; and a performance test module for testing the sample to be tested; wherein the hydrogen charging solution can charge the sample to be tested with hydrogen through the hydrogen charging hole, and the phase change, mechanical property change, and acoustic property change of the sample to be tested during the hydrogen charging process can be observed in situ through the performance test module, so as to monitor the diffusion of hydrogen in the sample to be tested during the hydrogen charging process, as well as the damage of the sample to be tested.

[0011] The present invention realizes simultaneous detection of multiple contents in one experimental process by combining surface morphology, internal damage acoustic emission detection and ultrasound, giving full play to the advantages of different research methods in different stages. In addition, by introducing acoustic emission monitoring and ultrasonic detection, a variety of monitoring and detection means are used for comprehensive characterization and mutual verification, thus realizing the monitoring and measurement of hydrogen diffusion and damage processes at the microscopic, mesoscopic and macroscopic scales, and significantly improving the reliability of the experimental results.

[0012] At the same time, by constructing the sample to be tested into a wedge shape so that its thickness changes continuously, it is convenient to capture the change process and study the influence of different types of tissues on hydrogen diffusion and the distribution of hydrogen among different tissues, which further improves the reliability of the experimental results.

[0013] In one embodiment, the matching inclined surface and the area corresponding to the hydrogen charging hole form a hydrogen charging surface area, and the hydrogen charging solution enters the interior of the sample to be tested through the hydrogen charging surface area and diffuses and enriches.

[0014] In one embodiment, the sample to be tested is a metal material.

[0015] In one embodiment, the test observation surface includes a horizontal observation surface, a vertical observation surface, and two symmetrical side observation surfaces.

[0016] The performance testing module performs performance testing and observation through the test observation surface, and the negative pole of the power supply is connected to the side observation surface.

[0017] In one embodiment, the performance testing module includes an ultrasonic detection unit, which is used to be set on the horizontal observation plane, the vertical observation plane or the side observation plane to carry out ordinary ultrasonic, phased array, ultrasonic diffraction time-of-flight detection or nonlinear ultrasonic detection.

[0018] In one embodiment, the performance testing module further includes an acoustic emission monitoring unit, which is arranged on the vertical observation surface or the side observation surface to perform acoustic emission monitoring during the test process.

[0019] In one embodiment, the performance testing module further includes a microscopic observation unit for performing metallographic structure observation on the horizontal observation plane during the hydrogen charging process.

[0020] In one embodiment, the performance testing module further includes an atomic force testing unit for performing an indentation test, a micro-area morphology test or a Kelvin probe scanning test on the horizontal observation surface during the hydrogen charging process.

[0021] In one embodiment, a plurality of first mounting holes are provided on the periphery of the hydrogen filling hole, mounting plates flush with the matching inclined surfaces are provided on both sides of the sample to be tested, and second mounting holes that can be matched with the first mounting holes are provided on the mounting plates.

[0022] The first mounting hole and the second mounting hole are fastened and connected by a fastener, so as to fasten the sample to be tested to the inclined surface area.

[0023] In one embodiment, a sealing member is installed at the hydrogen charging hole.

[0024] In one embodiment, a heating unit is disposed at the bottom of the solution pool.

[0025] According to a second aspect of the present invention, there is provided an in-situ hydrogen charging comprehensive test method, comprising the following steps:

[0026] Providing an in-situ hydrogen charging comprehensive test system as described above;

[0027] The sample to be tested is fixedly mounted on the inclined surface area, and the hydrogen charging solution is added into the solution pool through the liquid filling port;

[0028] Inserting the inert electrode into the hydrogen solution through the liquid filling port and connecting it to the positive electrode of the power supply, and connecting the negative electrode of the power supply to the sample to be tested;

[0029] Turn on the power switch and observe the phase change, mechanical property change and acoustic property change of the sample to be tested during the hydrogen charging process in situ through the performance testing module to monitor the diffusion of hydrogen in the sample to be tested during the hydrogen charging process and the damage of the sample to be tested.

[0030] In one embodiment, the horizontal viewing surface is subjected to grinding, polishing and etching processes.

[0031] In one embodiment, the liquid level of the hydrogen charging solution in the solution pool is higher than the upper edge of the hydrogen charging hole, so as to ensure that the hydrogen charging solution always covers the area corresponding to the matching inclined surface and the hydrogen charging hole.

[0032] Compared with the prior art, the advantages of this application are:

[0033] According to the in-situ hydrogen charging comprehensive test system and method of the present invention, by adopting wedge-shaped samples and single-sided hydrogen charging methods, and reserving metallographic observation, SKP scanning, indentation testing, acoustic emission detection and ultrasonic detection surfaces, it is possible to realize in-situ observation of the phase change, mechanical property change, and acoustic property change of the sample to be tested during the hydrogen charging process, monitor the diffusion of hydrogen in the sample to be tested during the hydrogen charging process, and the damage of the sample to be tested. By constructing the sample to be tested into a wedge shape so that it has a continuous change in thickness, it is convenient to capture the change process and study the influence of different types of tissues on hydrogen diffusion and the distribution of hydrogen among different tissues. By combining methods such as surface morphology, internal damage acoustic emission detection and ultrasound, it is possible to detect multiple contents simultaneously during one experiment, giving full play to the advantages of different research methods in studying different stages. In addition, by introducing acoustic emission monitoring and ultrasonic detection, a variety of monitoring and detection means are used for comprehensive characterization and mutual verification, and the monitoring and measurement of hydrogen diffusion and damage processes at the micro, meso and macro scales are realized, which significantly improves the reliability of the experimental results. In addition, compared with the prior art, the in-situ hydrogen charging comprehensive test system and method of the present invention solves the problems of hydrogen charging bubbles gathering along the sample, affecting the experiment, samples immersed in hydrogen charging liquid being not conducive to testing, and samples having the same thickness and changes caused by penetration into the sample surface being difficult to capture. BRIEF DESCRIPTION OF THE DRAWINGS

[0034] The present invention will be described below with reference to the accompanying drawings.

[0035] Figure 1 The structure of the in-situ hydrogen charging comprehensive test system according to the present invention is schematically shown;

[0036] Figure 2 Schematically shows Figure 1 The structure of the front view of the solution tank in the in-situ hydrogen charging comprehensive test system is shown;

[0037] Figure 3 Schematically shows Figure 2 A top view of the solution pool shown;

[0038] Figure 4 Schematically shows Figure 1 The structure of the front view of the sample to be tested in the in-situ hydrogen charging comprehensive test system shown;

[0039] Figure 5 Schematically shows Figure 4 A top view of the sample to be tested is shown;

[0040] Figure 6 Schematic diagram for calculating the hydrogen penetration depth of the sample to be tested;

[0041] Figure 7 FIG. 1 is a schematic diagram of calculating the hydrogen permeation thickness measured by an ultrasonic detection unit according to an embodiment of the present invention.

[0042] In the above figures, the meanings of the reference numerals are as follows:

[0043] 1-solution pool; 11-inclined surface area; 12-plane area; 13-hydrogen charging hole; 131-first mounting hole; 14-liquid filling port; 15-seal; 16-through-hole tube; 2-inert electrode; 3-sample to be tested; 31-matching inclined surface; 33-horizontal observation surface; 34-vertical observation surface; 35-side observation surface; 36-side observation surface; 37-mounting plate; 371-second mounting hole; 4-power supply; 5-ultrasonic detection unit; 51-ultrasonic detection probe; 6-acoustic emission monitoring unit; 61-acoustic emission sensor; 7-microscopic observation unit; 71-observation microscope; 8-atomic force test unit; 81-atomic force microscope; 100-in-situ hydrogen charging comprehensive test system.

[0044] In the present application, all drawings are schematic drawings, which are only used to illustrate the principles of the present invention, and are not necessarily drawn according to actual sizes and proportions. DETAILED DESCRIPTION

[0045] The present invention will be described below with reference to the accompanying drawings.

[0046] For ease of understanding, in this application, it should be noted that the directional terms or qualifiers "upper", "lower", etc. used in this application are all directed to the attached drawings to which they are referred. Figure 1The above description is only for the convenience of describing the present invention and simplifying the description, and does not indicate or imply that the device or element must have a specific orientation, be constructed and operate in a specific orientation, and therefore cannot be understood as limiting the present invention.

[0047] Figure 1 The structure of the in-situ hydrogen charging comprehensive test system 100 according to the present invention is schematically shown. Figure 1 As shown, a solution pool 1, an inert electrode 2, a wedge-shaped sample 3 to be tested, a power supply 4, and a performance test module for testing the sample 3 to be tested. Figure 2 As shown, the top surface of the solution pool 1 is constructed to include an inclined surface area 11 and a flat surface area 12. The inclined surface area 11 is provided with a hydrogen filling hole 13, and the flat surface area 12 is provided with a liquid filling port 14 for filling the hydrogen filling solution. The inert electrode 2 can be inserted into the hydrogen filling solution through the liquid filling port 14, and the inert electrode 2 is connected to the positive electrode of the power supply 4. The sample 3 to be tested includes a matching inclined surface 31 for matching with the inclined surface area 11 and a test observation surface (see Figure 4 and Figure 5 ), and the sample to be tested 3 is connected to the negative electrode of the power supply 4. The hydrogen-filling solution in the solution pool 1 can charge the sample to be tested 3 with hydrogen through the hydrogen-filling hole 13, and the phase change, mechanical property change, and acoustic property change of the sample to be tested 3 during the hydrogen-filling process can be observed in situ through the performance testing module to monitor the diffusion of hydrogen in the sample to be tested 3 during the hydrogen-filling process, as well as the damage of the sample to be tested 3.

[0048] According to the present invention, the matching slope 31 of the sample 3 to be tested and the area corresponding to the hydrogen charging hole 13 on the top surface of the solution pool 1 form a hydrogen charging surface area, and the hydrogen charging solution contacts the sample 3 to be tested through the hydrogen charging surface area and diffuses and enriches on the sample 3 to be tested.

[0049] In one embodiment, the solution pool 1 is configured as a substantially rectangular body, and its top surface is configured to include an inclined surface area 11 and a plane area 12. The solution pool 1 can be made of a non-metallic material or a metal material. The hydrogen charging hole 13 is disposed in the edge area of ​​the inclined surface area 11 close to the plane area 12, and is located in the middle of the junction of the inclined surface area 11 and the plane area 12. The hydrogen charging hole 13 can be configured as a square or a circle, and its specific size is set according to experimental requirements.

[0050] like Figure 3 As shown, a plurality of first mounting holes 131 are provided on the periphery of the hydrogen filling hole 13. Figure 3 In the embodiment shown, the hydrogen filling hole 13 is configured as a rectangular hole, and two first mounting holes 131 are respectively provided on both sides of the hydrogen filling hole 13, and the first mounting holes 131 on both sides of the hydrogen filling hole 13 are symmetrically distributed with each other. The function of the first mounting holes 131 will be described below.

[0051] Preferably, the liquid filling port 14 is arranged at a corner of the plane area 12 close to the solution pool 1, and a through-hole pipe 16 is arranged at the liquid filling port 14. The through-hole pipe 16 serves as a hydrogen filling port and a discharge port for the gas generated inside, and the inert electrode 2 is also inserted through the through-hole pipe 16.

[0052] According to the present invention, the sample 3 to be tested is a metal material to be studied. Before the detection test, the metal material to be studied is processed into a sample 3 to be tested in a specific shape according to the test requirements, that is, a wedge-shaped sample 3 to be tested. The specific wedge angle of the sample 3 to be tested is set according to the actual test requirements.

[0053] Figure 4 and Figure 5 The structure of the sample 3 to be tested is schematically shown. Figure 4 and Figure 5 As shown, the sample 3 to be tested is configured in a wedge shape, and the matching inclined surface 31 of the sample 3 to be tested is adapted to fit with the inclined surface area 11 of the solution pool 1. The test observation surface of the sample 3 to be tested includes a horizontal observation surface 33, a vertical observation surface 34, and two symmetrical side observation surfaces 35 and 36. The performance test module performs performance testing and observation through the test observation surface, and the negative pole of the power supply 4 can be connected to one of the side observation surfaces 35 and 36.

[0054] The present invention constructs the sample 3 to be tested into a wedge shape so that the thickness changes continuously, which facilitates the capture of the change process, the study of the influence of hydrogen diffusion on the tissue, and the distribution of hydrogen between different tissues. In addition, the inclined surface area 11 structure of the solution pool 1 can solve the problems of hydrogen bubbles gathering along the sample, affecting the experiment, the sample being immersed in the hydrogen filling liquid and not conducive to testing, and the sample thickness being the same, and the changes caused by penetration into the sample surface being difficult to capture. This is very helpful to improve the reliability of the experimental results.

[0055] The horizontal observation surface 33 is used for metallographic observation, indentation test, micro-area topography or Kelvin probe scanning (SKP) and other tests, and can also be used to place the ultrasonic detection probe 51 (see below) of the ultrasonic detection unit 5. The vertical observation surface 34 can be used to place the ultrasonic detection probe 51, and the side observation surfaces 35 and 36 can be used to place the acoustic emission sensor 61 (see below) of the acoustic emission monitoring unit 6 or the ultrasonic detection probe 51, which should be selected according to the actual needs of the experiment.

[0056] When conducting a test, the horizontal observation plane 33 is flush with or slightly higher than the plane area 12 of the solution pool 1 to facilitate observation and scanning / testing.

[0057] The angle between the vertical observation plane 34 and the horizontal observation plane 33 is determined according to experimental requirements, for example, it can be set to 90°. Of course, it can also be set to other angles as needed.

[0058] According to the present invention, Figure 1 As shown, the performance test module includes an ultrasonic detection unit 5, and the ultrasonic detection unit 5 includes a plurality of ultrasonic detection probes 51. The ultrasonic detection probes 51 can be set on the horizontal observation plane 33, the vertical observation plane 34 or the side observation planes 35 and 36 to carry out ordinary ultrasonic, phased array, ultrasonic diffraction time difference method or nonlinear ultrasonic detection.

[0059] According to the present invention, Figure 1 As shown, the performance test module further includes an acoustic emission monitoring unit 6, which includes a plurality of acoustic emission sensors 61. The acoustic emission sensors 61 can be arranged on the vertical observation surface 34 or the side observation surfaces 35, 36 to perform acoustic emission monitoring during the test process.

[0060] According to the present invention, Figure 1 As shown, the performance test module also includes a microscopic observation unit 7, which includes an observation microscope 71. The observation microscope 71 can be moved above the horizontal observation plane 33 to observe the metallographic structure of the horizontal observation plane 33 during the hydrogen charging process.

[0061] According to the present invention, Figure 1 As shown, the performance testing module also includes an atomic force testing unit 8, which includes an atomic force microscope 81. The atomic force microscope 81 can be moved above the horizontal observation plane 33 to perform indentation testing, micro-area morphology or Kelvin probe scanning testing on the horizontal observation plane 33 during the hydrogen charging process.

[0062] According to the present invention, Figure 5 As shown, on both sides of the sample 3 to be tested ( Figure 5 The upper and lower sides of the sample 3 to be tested are provided with mounting plates 37 flush with the matching inclined surfaces 31. The mounting plates 37 are arranged in a rectangular flat plate shape extending outward along both sides of the sample 3 to be tested. The mounting plates 37 are provided with second mounting holes 371 that can be matched with the first mounting holes 131 provided on the inclined surface area 11 of the solution pool 1. When installing the sample 3 to be tested, the first mounting hole 131 is aligned with the second mounting hole 371, and fasteners (not shown) are installed in sequence, and the sample 3 to be tested is fastened and installed to the inclined surface area 11 by the fasteners. The fasteners can be, for example, non-metallic or corrosion-resistant metal bolts.

[0063] In order to ensure the sealing between the sample 3 to be tested and the hydrogen filling hole 13 of the solution pool 1, a sealing member 15 may be provided in the hydrogen filling hole 13. The sealing member 15 may be, for example, a sealing ring. The sealing member 15 may be compressed by installing a fastener, thereby achieving the sealing between the sample 3 to be tested and the solution pool 1.

[0064] In order to further improve the hydrogen diffusion rate, in an embodiment not shown, a heating unit may be provided at the bottom of the solution pool 1 , and the temperature of the hydrogen-filled solution in the solution pool 1 may be controlled at about 70° C. by the heating unit.

[0065] When conducting the experiment, the required current value is calculated and set according to the area of ​​the hydrogen-filled surface area exposed by the sample and the required current density. The sample 3 to be tested is connected to the cathode of the power supply 4, and a hydrogen evolution reaction occurs. The hydrogen evolution process generates an acoustic emission signal, which is captured by the acoustic emission monitoring unit 6 and its acoustic characteristics are analyzed. Some of the precipitated hydrogen atoms are combined into hydrogen molecules. The sample 3 to be tested is set to a wedge shape, which has a matching inclined surface 31, which greatly reduces the number of bubbles adsorbed on the surface of the sample 3 to be tested, and ensures the stability of the hydrogen-filled area and the continuity of hydrogen-filled. The bubbles gather along the inclined surface area 11 to the upper part of the solution pool 1 and are discharged through the through-hole tube 16. The discharged gas needs to be connected to the ventilation system and discharged indoors to prevent aggregation at the top of the room. Another part of the hydrogen atoms enter the metal through the hydrogen-filled surface, and diffuse and enrich inside the metal. Due to the entry of hydrogen atoms, the lattice and defect positions are occupied, causing changes in material properties. The performance testing module can be used to observe in situ the phase change, mechanical property change, and acoustic property change of the test sample during the hydrogen charging process, so as to monitor the diffusion of hydrogen in the test sample 3 during the hydrogen charging process and the damage of the test sample 3.

[0066] The in-situ hydrogen charging comprehensive testing system 100 according to the present invention is introduced below according to specific experimental requirements.

[0067] Experimental requirement 1:

[0068] The metallographic structure changes and surface damage process of materials during hydrogen charging are studied.

[0069] The microscopic observation unit 7 uses a metallographic microscope to observe the metallographic structure during the hydrogen charging process on the horizontal observation surface 33, records the changes in the metallographic structure and morphology of the surface of the sample 3 to be tested during the hydrogen charging process, and sets an acoustic emission sensor 61 on the side observation surface 35 or the side observation surface 36 to monitor the hydrogen charging process and record the acoustic signal of the whole process. When the metallographic structure or morphology changes are found, the acoustic signal of the corresponding time period is analyzed, and the corresponding relationship between the morphology and tissue changes and the acoustic signal is established. The acquired acoustic signal is classified and marked according to the changes for subsequent signal feature extraction, and a signal recognition model is established through an intelligent algorithm. This is to facilitate the subsequent judgment of the tissue changes and hydrogen damage in the sample to be tested based only on the characteristics of the acoustic signal.

[0070] Experimental requirement 2:

[0071] Study the diffusion of hydrogen in materials and the changes in material properties.

[0072] The atomic force testing unit 8 uses an atomic force microscope to perform micro-area indentation and SKP testing on the horizontal observation surface 33 during the hydrogen charging process, and infers the depth of hydrogen diffusion through changes in the micro-area loading curve and changes in the SKP test results, and obtains the mechanical property parameters of the material after hydrogenation.

[0073] Experimental requirement three:

[0074] Ultrasonic detection probes 51 are set on the horizontal observation surface 33 and the vertical observation surface 34. Through the transmission and reception tests at multiple positions, a calculation equation is established according to the correspondence between the sound path change, the change of the hydrogen permeation layer and the corresponding sound propagation time, and the change of the diffusion depth and the sound velocity in the hydrogen permeation layer are obtained. The equations are compared and verified with the SKP or indentation test, and the change of material properties after hydrogen diffusion is inferred through the relationship between the sound velocity and the relevant test quantities.

[0075] Specifically, if Figure 7 As shown, in one embodiment of the present invention;

[0076] The angle between the horizontal observation plane 33 and the matching inclined plane 31 of the sample 3 to be tested is set to α. Ultrasonic detection probes 51 are arranged on both the horizontal observation plane 33 and the vertical observation plane 34. The calculation process of the diffusion depth change and the sound velocity in the hydrogen permeation layer is as follows:

[0077] Assume that the ultrasonic detection probe 51 disposed on the vertical observation plane 34 emits an acoustic signal, and the ultrasonic detection probe 51 disposed on the horizontal observation plane 33 receives an acoustic signal. Assume that the thickness of the hydrogen permeation layer in the sample 3 to be tested is h, and the propagation of the acoustic wave in the sample 3 to be tested goes through four stages: l1, l2, l3, and l4, wherein l1 and l4 are propagation distances of the acoustic wave in the portion of the sample 3 to be tested that is not permeated by hydrogen, and l2 and l3 are propagation distances of the acoustic wave in the portion of the sample 3 to be tested that is permeated by hydrogen. Assume that the total distance traveled by the acoustic wave is S, then:

[0078] S = l1 + l2 + l3 + l4;

[0079] exist Figure 7 In the figure, β is the refraction angle, c is the distance from the center of the ultrasonic detection probe 51 disposed on the vertical observation plane 34 to the lowermost end of the sample 3 to be tested, and d is the distance from the center of the ultrasonic detection probe 51 disposed on the horizontal observation plane 33 to the leftmost end of the test sample 3. It can be seen from the positional relationship in the figure that:

[0080]

[0081] Therefore, the time t it takes for the sound wave to reach the receiving end after refraction and reflection is:

[0082]

[0083] where vh is the sound velocity of the hydrogen-impregnated part of the sample 3 to be tested, and v is the sound velocity of the non-hydrogen-impregnated part of the sample 3 to be tested.

[0084] From the law of refraction of sound waves we know that:

[0085] Available

[0086] Further,

[0087] Substituting into equation 1, we get

[0088] In equation 2, v, t, c, d, and α are all known or can be directly measured.

[0089] v h The previously measured data can be substituted into equation 2 to test the thickness h of the hydrogen permeation layer in the sample 3 to be tested.

[0090] v h It is also possible to obtain multiple sets of data by moving the sensor probes 51 respectively located on the vertical observation plane 34 and the horizontal observation plane 33, and to bring them into equation 2 respectively, and then solve the equation group to obtain the thickness h of the hydrogen permeation layer.

[0091] It should be noted that the angle α between the horizontal observation plane 33 of the sample 3 to be tested and the matching inclined plane 31 can be replaced with different values ​​according to actual conditions, and can be substituted into the above equation 2 together with other known or measurable data that change accordingly to calculate the corresponding values.

[0092] like Figure 7 As shown, in a specific embodiment of the present invention, the angle α between the horizontal observation surface 33 of the sample 3 to be tested and the matching inclined surface 31 is 45°.

[0093] Experimental requirement 4:

[0094] Study the hydrogen damage process during the hydrogen charging process of materials.

[0095] The atomic force testing unit 8 uses an atomic force microscope to perform micro-area morphology and SKP tests during the hydrogen charging process on the horizontal observation surface 33 to track the depth of hydrogen diffusion. An acoustic emission sensor 61 is set on the vertical observation surface 34 to detect the damage signal generated during the hydrogen charging process and roughly determine the location of the damage. Ultrasonic detection units 5 are set on the side observation surfaces 35 and 36, such as: nonlinear ultrasound, ultrasonic phased array or TOFD detection probes, etc., to study the hidden damage generated during the hydrogen charging process of the material through nonlinear ultrasound, and to detect damage defects in the material whose size exceeds the detection limit through ultrasonic phased array or diffraction methods. Therefore, through multiple monitoring and detection methods on multiple surfaces, the microscopic, mesoscopic and macroscopic damage generated during the hydrogen charging process of the material is comprehensively studied.

[0096] According to the present invention, an in-situ hydrogen charging comprehensive test method is also provided, and the in-situ hydrogen charging comprehensive test method is implemented by the in-situ hydrogen charging comprehensive test system 100 of the present invention. The in-situ hydrogen charging comprehensive test method is described in detail below.

[0097] First, the material to be studied (metal material) is processed into the shape required for the experiment to prepare a wedge-shaped sample to be tested 3. In order to facilitate subsequent tissue observation, the horizontal observation surface 33 of the sample to be tested 3 can be polished and eroded.

[0098] Then, the sealing member 15 is installed around the hydrogen charging hole 13 of the inclined surface area 11 of the solution pool 1. After that, the first mounting hole 131 of the sample 3 to be tested is aligned with the second mounting hole 371 of the inclined surface area 11, and fasteners are installed in sequence, and the sample 3 to be tested is fastened and installed to the inclined surface area 11 by the fasteners. Thus, the installation of the sample 3 to be tested is achieved.

[0099] Afterwards, the hydrogen filling solution is injected into the solution pool 1 through the through-hole tube 16 , and the liquid level of the hydrogen filling solution is ensured to be higher than the upper edge of the hydrogen filling hole 13 , so as to keep the hydrogen filling solution always covering the hydrogen filling surface area of ​​the sample 3 to be tested.

[0100] After that, after checking that the seal is leak-free, the inert electrode 2 is placed in the through-hole tube 16 and connected to the positive pole of the power source 4. At the same time, the negative pole of the power source 4 is connected to the sample 3 to be tested, for example, it can be connected to the side observation surface 35 or the side observation surface 36 of the sample 3 to be tested.

[0101] A microscopic observation unit 7 is placed above the horizontal observation surface 33 for observing and recording the metallographic structure. An atomic force test unit 8 can also be placed above the horizontal observation surface 33 as needed for performing micro-area indentation testing or scanning Kelvin probe testing.

[0102] One or two acoustic emission sensors in the acoustic emission monitoring unit 6 are installed on the side observation surface 35, the side observation surface 36 or the vertical observation surface 34 of the sample to be tested 3 to monitor the acoustic emission during the test. At the same time, another acoustic emission sensor is installed on the control sample to monitor the environmental noise.

[0103] The ultrasonic detection probe 51 of the ultrasonic detection unit 5 is set on the horizontal observation plane 33, the vertical observation plane 34 or the side observation planes 35, 36 for carrying out ordinary ultrasonic, phased array, ultrasonic diffraction time difference method or nonlinear ultrasonic detection.

[0104] After all detection elements (ultrasonic detection probe 51, acoustic emission sensor 61, etc.) are connected and the original data before hydrogen filling is obtained, the power supply 4 is turned on, and the required current value is calculated and set according to the exposed area of ​​the hydrogen filling surface area of ​​the sample 3 to be tested and the required current density. The relevant calculation formula is: set current value = required current density × exposure area.

[0105] During the experiment, the sample to be tested 3 is connected to the cathode of the power supply 4, and a hydrogen evolution reaction occurs. The hydrogen evolution process generates an acoustic emission signal, which is captured by the acoustic emission monitoring unit 6 and analyzed for its acoustic characteristics. Some of the hydrogen atoms that are precipitated are combined into hydrogen molecules. Since the sample to be tested 3 is set in a wedge shape, by matching the structure of the inclined surface 31, the bubbles formed in the hydrogen evolution reaction will roll upward along the inclined surface 31, which greatly reduces the number of bubbles adsorbed on the surface of the sample to be tested 3, avoids the bubbles from gathering at the hydrogen filling surface area, and ensures the stability of the hydrogen filling area and the continuity of hydrogen filling. In addition, after the bubbles gather along the inclined surface area 11 of the solution pool 1 to the upper part of the solution pool 1, they can be discharged through the through-hole pipe 16 set at the liquid filling port 14. The discharged gas needs to be connected to the ventilation system to be discharged indoors to prevent gathering at the top of the room. Another part of the hydrogen atoms enter the metal interior (the interior of the sample to be tested 3) through the hydrogen filling surface area, and diffuse and enrich in the metal interior. Due to the entry of hydrogen atoms, the lattice and defect positions are occupied, causing changes in material properties. The changes in material properties within the hydrogen permeation layer will be reflected in the micro-area mechanical properties test results, SKP results and sound velocity measurement results.

[0106] In one embodiment, since the sample 3 to be tested is wedge-shaped and has a gradual change in thickness from thin to thick, the thickness of the hydrogen-filled layer can be directly reflected on the horizontal observation surface 33 of the sample 3 to be tested. Figure 6 As shown, the hydrogen penetration depth h=a·tanα can be calculated by measuring the length a from the point where the hardness or SKP test has a significant change to the tip, where α is the angle between the horizontal observation plane 33 and the matching inclined surface 31.

[0107] In another embodiment, ultrasonic detection probes 51 can be arranged on the horizontal observation plane 33 and the vertical observation plane 34, respectively. Since the probe position, the size of the sample to be tested, the angle of the inclined plane of the sample to be tested, and the sound velocity in the non-hydrogenated sample are known, the diffusion depth and the sound velocity in the hydrogen diffusion layer can also be estimated by measuring multiple positions according to the correspondence between the sound path change and the corresponding sound propagation time, using the above-mentioned equation 2. When the hydrogen diffusion layer is deep enough, the sound velocity in the hydrogen diffusion layer can be directly measured and substituted into equation 2, and the previously estimated hydrogen diffusion layer depth can be recalculated to reduce the error of the previous hydrogen diffusion layer estimation.

[0108] During the hydrogen diffusion process, the distribution and enrichment of hydrogen on the surface can be studied by the SKP test of the horizontal observation surface 33. During the hydrogen diffusion process, the acoustic emission monitoring unit 6 can also capture the acoustic emission signal, in which, in addition to the signal generated by the precipitation and collapse of hydrogen bubbles, the sound emitted by the dislocation inside the hydrogen-promoted material will also be captured. As the hydrogen filling continues, hydrogen is enriched inside the metal, and hydrogen molecules are formed at the defects, the volume expands, internal hydrogen pressure and local plastic deformation are generated, and even metal bonds are broken, forming tiny cracks, that is, irreversible damage is generated. This process will generate an acoustic emission signal, which can also be captured by the acoustic emission monitoring unit 6, and the time difference between the acquisition signal reaching different acoustic emission sensors 61 can be used to estimate the approximate location of the damage, which is used to reduce the scope of ultrasonic detection. When this irreversible damage is manifested on the surface, it is usually a phase change, bulge or crack, which can be captured and recorded by the microscopic observation unit 7 on the horizontal observation surface 33.

[0109] After irreversible damage occurs, the reflection and scattering of ultrasound are enhanced. Therefore, when the microcracks reach the detection limit of phased array or TOFD (time-of-flight diffraction), nonlinear ultrasound can be used as an effective detection method.

[0110] As hydrogen charging continues, the local hydrogen pressure rises and the crack gradually expands. When the detection limit of phased array and TOFD is reached, the phased array and TOFD methods can be selected. At the same time, the acoustic emission signal during the expansion process is collected by the acoustic emission monitoring unit 6, and the detection results of the phased array and TOFD are verified with the acoustic emission signal.

[0111] Therefore, through the above-mentioned in-situ hydrogen charging comprehensive test device and method, it is possible to realize the application of multiple analysis methods at different stages, and the mutual auxiliary verification of the results, to realize the study of the entire process of hydrogen diffusion, enrichment, crack generation and expansion in the material, and at the same time, it is possible to study the acoustic characteristics and material performance changes of each process. It provides convenience and a way for the research on the process and mechanism of hydrogen damage of materials, and the development of damage monitoring detection and evaluation technology.

[0112] According to the in-situ hydrogen charging comprehensive test system 100 and method of the present invention, by adopting wedge-shaped samples and single-sided hydrogen charging methods, and reserving metallographic observation, SKP scanning, indentation testing, acoustic emission detection and ultrasonic detection surfaces, it is possible to realize in-situ observation of phase change, mechanical property change, and acoustic property change of the sample to be tested during the hydrogen charging process, and monitor the diffusion and damage of the sample to be tested during the hydrogen charging process. By constructing the sample to be tested into a wedge shape, so that there is a continuous change in thickness, it is convenient to capture the change process and study the influence of tissue on hydrogen diffusion and the distribution of hydrogen among different tissues. By combining methods such as surface morphology, internal damage acoustic emission detection and ultrasound, it is possible to detect multiple contents simultaneously during an experiment, giving full play to the advantages of different research methods in studying different stages. In addition, by introducing acoustic emission monitoring and ultrasonic detection, a variety of monitoring and detection means are used for comprehensive characterization and mutual verification, and the microscopic, mesoscopic and macroscopic monitoring and measurement of hydrogen diffusion and damage processes are realized, which significantly improves the reliability of experimental results. In addition, compared with the prior art, the in-situ hydrogen charging comprehensive test system 100 and method of the present invention solves the problems of hydrogen charging bubbles gathering along the sample, affecting the experiment, samples immersed in hydrogen charging liquid being not conducive to testing, and samples having the same thickness and changes caused by penetration into the interior of the sample being difficult to capture.

[0113] The in-situ hydrogen charging comprehensive testing system and method of the present invention are introduced below through different application embodiments.

[0114] Application Example 1:

[0115] The changes of metallographic structure of 304L stainless steel during hydrogen charging were studied.

[0116] Since the hydrogen diffusion coefficient of 304L stainless steel is extremely low, a wedge-shaped sample with a small angle is preferably used. Therefore, the angle α between the horizontal observation surface 33 of the sample 3 to be tested and the matching inclined surface 31 is selected to be 10°.

[0117] The hydrogen filling holes 13 on the inclined surface area 11 of the solution pool 1 are square holes with a size of 10×10 mm. The hydrogen filling holes 13 are arranged at the uppermost portion of the inclined surface area 11 of the solution pool 1 .

[0118] First, the processed horizontal observation surface of the sample 3 to be tested is ground, polished and etched to facilitate subsequent microstructure observation.

[0119] Then, the sealing member 15 is installed around the hydrogen charging hole 13 of the inclined surface area 11 of the solution pool 1. After that, the first mounting hole 131 of the sample 3 to be tested is aligned with the second mounting hole 371 of the inclined surface area 11, and fasteners are installed in sequence, and the sample 3 to be tested is fastened and installed to the inclined surface area 11 by the fasteners. Thus, the installation of the sample 3 to be tested is achieved.

[0120] Afterwards, the hydrogen filling solution is injected into the solution pool 1 through the through-hole pipe 16, and the liquid level of the hydrogen filling solution is ensured to be higher than the upper edge of the hydrogen filling hole 13, so as to keep the hydrogen filling solution always covering the hydrogen filling surface area of ​​the sample to be tested 3. Specifically, the hydrogen filling solution is a mixed solution of 0.5 mol / L H2SO4 and 0.25 g / L As2O3.

[0121] In order to further increase the hydrogen diffusion rate, a heating unit (not shown) is provided at the bottom of the solution pool 1 to control the temperature of the hydrogen-filled solution in the solution pool 1 to be 70°C.

[0122] After that, after checking that the seal is leak-free, the inert electrode 2 is placed in the through-hole tube 16 to be inserted into the hydrogen-filled solution and connected to the positive electrode of the power source 4. At the same time, the negative electrode of the power source 4 is connected to the sample 3 to be tested, for example, it can be connected to the side observation surface 35 or the side observation surface 36 of the sample 3 to be tested.

[0123] Afterwards, a microscopic observation unit 7 is placed above the horizontal observation surface 33 of the sample 3 to be tested, so as to observe and record the metallographic structure.

[0124] After all detection elements (ultrasonic detection probe 51, acoustic emission sensor 61, etc.) are connected and the original data before hydrogen charging is obtained, the power supply 4 is turned on, and the required current value is calculated and set according to the area of ​​the hydrogen charging surface area exposed by the sample 3 to be tested and the required current density. Specifically, the hydrogen charging current is set to 100mA.

[0125] In this embodiment, since the tip of the sample is the thinnest, the metallographic observation starts from the thinnest part (tip) and gradually extends to the thick end as the hydrogen filling progresses. At the same time, an acoustic emission monitoring sensor is installed on the vertical observation surface 34, the side observation surface 35 or the side observation surface 36 of the sample 3 to be tested as an auxiliary, on the one hand to monitor the stage of hydrogen damage inside the metal, and on the other hand to capture the acoustic emission signal when the phase change occurs.

[0126] Application Example 2:

[0127] The hydrogen damage process and corresponding characteristic signals of 20 steel during hydrogen charging were studied.

[0128] The included angle α between the horizontal observation surface 33 of the sample 3 to be tested and the matching inclined surface 31 is selected to be 45°.

[0129] The hydrogen filling hole 13 on the inclined surface area 11 of the solution pool 1 is a rectangular hole of 20×80 mm, and the hydrogen filling hole 13 is arranged in the middle and upper part of the inclined surface area 11 of the solution pool 1 .

[0130] First, the processed horizontal observation surface of the sample 3 to be tested is ground, polished and etched to facilitate subsequent microstructure observation.

[0131] Then, the sealing member 15 is installed around the hydrogen charging hole 13 of the inclined surface area 11 of the solution pool 1. After that, the first mounting hole 131 of the sample 3 to be tested is aligned with the second mounting hole 371 of the inclined surface area 11, and fasteners are installed in sequence, and the sample 3 to be tested is fastened and installed to the inclined surface area 11 by the fasteners. Thus, the installation of the sample 3 to be tested is achieved.

[0132] Afterwards, the hydrogen filling solution is injected into the solution pool 1 through the through-hole tube 16, and the liquid level of the hydrogen filling solution is ensured to be higher than the upper edge of the hydrogen filling hole 13, so as to keep the hydrogen filling solution always covering the hydrogen filling surface area of ​​the sample 3 to be tested. Specifically, the hydrogen filling solution is a 0.1 mol / L NaOH solution.

[0133] After that, after checking that the seal is leak-free, the inert electrode 2 is placed in the through-hole tube 16 to be inserted into the hydrogen-filled solution and connected to the positive electrode of the power source 4. At the same time, the negative electrode of the power source 4 is connected to the sample 3 to be tested, for example, it can be connected to the side observation surface 35 or the side observation surface 36 of the sample 3 to be tested.

[0134] After all detection elements (ultrasonic detection probe 51, acoustic emission sensor 61, etc.) are connected and the original data before hydrogen charging is obtained, the power supply 4 is turned on, and the required current value is calculated and set according to the area of ​​the hydrogen charging surface area exposed by the sample 3 to be tested and the required current density. Specifically, the hydrogen charging current is set to 1A.

[0135] Specifically, an atomic force test unit 8 is placed above the horizontal observation surface 33 of the sample 3 to be tested, and micro-area morphology and SKP tests are performed during the hydrogen charging process to track the depth of hydrogen diffusion. An acoustic emission sensor 61 is set on the vertical observation surface 34 to detect the damage signal generated during the hydrogen charging process and roughly determine the location of the damage. Ultrasonic detection probes 51 are set on the vertical observation surface 34, the side observation surface 35 and the side observation surface 36 to study the hidden damage generated during the hydrogen charging process of the material through nonlinear ultrasound, and detect damage defects in the sample 3 to be tested that are larger than the detection limit through ultrasonic phased array or diffraction methods.

[0136] Therefore, in this embodiment, the above-mentioned in-situ hydrogen charging comprehensive test device and method are used to realize multiple monitoring and detection methods through multiple surfaces, comprehensively study the entire process of hydrogen diffusion, enrichment, crack generation and expansion in the material, and at the same time study the acoustic characteristics of each process.

[0137] Application Example 3:

[0138] The hydrogen diffusion process of Q345 steel and the influence of hydrogen on material properties were studied.

[0139] The angle α between the horizontal observation surface 33 of the sample 3 to be tested and the matching inclined surface 31 is selected to be 30°.

[0140] The hydrogen filling hole 13 on the inclined surface area 11 of the solution pool 1 is a rectangular hole of 30×100 mm, and the hydrogen filling hole 13 is arranged in the middle and upper part of the inclined surface area 11 of the solution pool 1 .

[0141] First, the processed horizontal observation surface of the sample 3 to be tested is ground, polished and etched to facilitate subsequent microstructure observation.

[0142] Then, the sealing member 15 is installed around the hydrogen charging hole 13 of the inclined surface area 11 of the solution pool 1. After that, the first mounting hole 131 of the sample 3 to be tested is aligned with the second mounting hole 371 of the inclined surface area 11, and fasteners are installed in sequence, and the sample 3 to be tested is fastened and installed to the inclined surface area 11 by the fasteners. Thus, the installation of the sample 3 to be tested is achieved.

[0143] Afterwards, the hydrogen charging solution is injected into the solution pool 1 through the through-hole tube 16, and the liquid level of the hydrogen charging solution is ensured to be higher than the upper edge of the hydrogen charging hole 13, so as to keep the hydrogen charging solution always covering the hydrogen charging surface area of ​​the sample to be tested 3. Specifically, the hydrogen charging solution uses a 0.1 mol / L NaOH solution, and the liquid level of the hydrogen charging solution is higher than the upper edge of the hydrogen charging hole 13, so as to keep the hydrogen charging solution always covering the hydrogen charging surface area of ​​the sample to be tested 3.

[0144] After that, after checking that the seal is leak-free, the inert electrode 2 is placed in the through-hole tube 16 to be inserted into the hydrogen-filled solution and connected to the positive electrode of the power source 4. At the same time, the negative electrode of the power source 4 is connected to the sample 3 to be tested, for example, it can be connected to the side observation surface 35 or the side observation surface 36 of the sample 3 to be tested.

[0145] After all detection elements (ultrasonic detection probe 51, acoustic emission sensor 61, etc.) are connected and the original data before hydrogen charging is obtained, the power supply 4 is turned on, and the required current value is calculated and set according to the area of ​​the hydrogen charging surface area exposed by the sample 3 to be tested and the required current density. Specifically, the hydrogen charging current is set to 1A.

[0146] Specifically, an atomic force testing unit 8 is placed above the horizontal observation surface 33 of the sample 3 to be tested, and micro-area indentation and SKP tests are performed during the hydrogen charging process. The depth of hydrogen diffusion is inferred through changes in the micro-area loading curve and changes in the SKP test results, and the mechanical properties of the material after hydrogen diffusion are obtained. Ultrasonic sensors are set on the horizontal observation surface 33 and the vertical observation surface 34, and through receiving and transmitting tests at multiple positions, according to the change in sound path, the change in hydrogen permeation layer and the corresponding sound propagation time, the above-mentioned equation 2 is used to obtain the change in diffusion depth and the sound velocity in the hydrogen permeation layer, and the results can be compared and verified with the SKP or indentation test results. Through the relationship between the sound velocity and the relevant test quantity, the change in material performance after hydrogen diffusion is inferred.

[0147] In the description of the present invention, it should be understood that the terms "first" and "second" are used for descriptive purposes only and should not be understood as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of the features. In the description of the present invention, the meaning of "plurality" is two or more, unless otherwise clearly and specifically defined.

[0148] In the present invention, unless otherwise clearly specified and limited, the terms "installed", "connected", "connected", "fixed" and the like should be understood in a broad sense, for example, it can be a fixed connection, a detachable connection, or an integral connection; it can be a mechanical connection or an electrical connection; it can be a direct connection, or it can be an indirect connection through an intermediate medium, or it can be the internal communication of two components. For ordinary technicians in this field, the specific meanings of the above terms in the present invention can be understood according to specific circumstances.

[0149] In addition, in the description of this specification, the description with reference to the terms "one embodiment", "some embodiments", "example", "specific example", or "some examples" means that the specific features, structures, materials or characteristics described in conjunction with the embodiment or example are included in at least one embodiment or example of the present invention. In this specification, the schematic representation of the above terms does not necessarily refer to the same embodiment or example. Moreover, the specific features, structures, materials or characteristics described may be combined in any one or more embodiments or examples in a suitable manner.

[0150] Finally, it should be noted that the above is only a preferred embodiment of the present invention and does not constitute any limitation to the present invention. Although the present invention has been described in detail with reference to the aforementioned embodiments, it is still possible for a person skilled in the art to modify the technical solutions described in the aforementioned embodiments or to replace some of the technical features therein by equivalents. Any modification, combination, improvement, equivalent replacement, etc. made within the spirit and principle of the present invention shall be included in the protection scope of the present invention.

Claims

1. An in-situ hydrogen charging comprehensive test system, comprising: A solution pool (1), the top surface of which is structured to include an inclined surface area (11) and a flat surface area (12), the inclined surface area (11) being provided with a hydrogen filling hole (13), and the flat surface area (12) being provided with a liquid filling port (14) for filling a hydrogen filling solution; An inert electrode (2) is inserted into the hydrogen solution through the liquid filling port (14); A sample to be tested (3) is constructed in a wedge shape, comprising a matching inclined surface (31) for matching with the inclined surface area (11) and a test observation surface; A power source (4), the positive electrode of which is connected to the inert electrode (2) and the negative electrode of which is connected to the sample to be tested (3); A performance testing module for testing a sample to be tested (3); The hydrogen-charging solution can charge the sample to be tested (3) with hydrogen through the hydrogen-charging hole (13), and the performance testing module can observe in situ the phase change, mechanical property change, and acoustic property change of the sample to be tested (3) during the hydrogen-charging process, so as to monitor the diffusion of hydrogen in the sample to be tested (3) during the hydrogen-charging process, as well as the damage of the sample to be tested (3).

2. The in-situ hydrogen charging comprehensive test system according to claim 1, characterized in that: The matching inclined surface (31) and the area corresponding to the hydrogen filling hole (13) form a hydrogen filling surface area, and the hydrogen filling solution enters the interior of the sample to be tested (3) through the hydrogen filling surface area and diffuses and enriches.

3. The in-situ hydrogen charging comprehensive test system according to claim 1, characterized in that: The sample to be tested (3) is a metal material.

4. The in-situ hydrogen charging comprehensive test system according to any one of claims 1 to 3, characterized in that: The test observation surface comprises a horizontal observation surface (33), a vertical observation surface (34), and two symmetrical side observation surfaces (35, 36). The performance testing module performs performance testing and observation through the test observation surface, and the negative pole of the power supply is connected to the side observation surface (35, 36).

5. The in-situ hydrogen charging comprehensive test system according to claim 4, characterized in that: The performance testing module comprises an ultrasonic detection unit (5) which is arranged on the horizontal observation plane (33), the vertical observation plane (34) or the side observation plane (35, 36) to carry out ordinary ultrasonic, phased array, ultrasonic diffraction time-of-flight detection or nonlinear ultrasonic detection.

6. The in-situ hydrogen charging comprehensive test system according to claim 4, characterized in that: The performance test module further comprises an acoustic emission monitoring unit (6) which is arranged on the vertical observation surface (34) or the side observation surfaces (35, 36) to perform acoustic emission monitoring during the test.

7. The in-situ hydrogen charging comprehensive test system according to claim 4, characterized in that: The performance testing module further comprises a microscopic observation unit (7) for observing the metallographic structure of the horizontal observation surface (33) during the hydrogen charging process.

8. The in-situ hydrogen charging comprehensive test system according to claim 4, characterized in that: The performance testing module also includes an atomic force testing unit (8) for performing an indentation test, a micro-area morphology test or a Kelvin probe scanning test on the horizontal observation surface (33) during the hydrogen charging process.

9. The in-situ hydrogen charging comprehensive test system according to any one of claims 1 to 3, characterized in that: A plurality of first mounting holes (131) are provided on the periphery of the hydrogen filling hole (13), mounting plates (37) flush with the matching inclined surfaces (31) are provided on both sides of the sample to be tested (3), and second mounting holes (371) that can be matched with the first mounting holes (131) are provided on the mounting plates (37). The first mounting hole (131) and the second mounting hole (371) are fastened together by a fastener, so as to fasten the sample to be tested (3) to the inclined surface area (11).

10. The in-situ hydrogen charging comprehensive test system according to claim 9, characterized in that: A sealing member (15) is installed at the hydrogen filling hole (13).

11. The in-situ hydrogen charging comprehensive test system according to any one of claims 1 to 3, characterized in that: A heating unit is arranged at the bottom of the solution pool (1).

12. A comprehensive in-situ hydrogen charging test method comprising the following steps: Providing an in-situ hydrogen charging comprehensive testing system according to any one of claims 1 to 11; The sample to be tested (3) is fixedly mounted on the inclined surface area (11), and the hydrogen filling solution is added into the solution pool (1) through the liquid filling port (14); Inserting the inert electrode (2) into the hydrogen solution through the liquid filling port (14), and connecting the positive electrode of the power supply (4), and connecting the negative electrode of the power supply (4) to the sample to be tested (3); The power source (4) is turned on, and the phase change, mechanical property change, and acoustic property change of the sample to be tested (3) during the hydrogen charging process are observed in situ by the performance testing module, so as to monitor the diffusion of hydrogen in the sample to be tested (3) during the hydrogen charging process, as well as the damage of the sample to be tested (3).

13. The in-situ hydrogen charging comprehensive test method according to claim 12, characterized in that: The horizontal observation surface (33) is subjected to grinding, polishing and erosion treatments.

14. The in-situ hydrogen charging comprehensive test method according to claim 12 or 13, characterized in that: The liquid level of the hydrogen-filling solution in the solution pool (1) is higher than the upper edge of the hydrogen-filling hole (13), so that the hydrogen-filling solution always covers the area corresponding to the matching inclined surface (31) and the hydrogen-filling hole (13).

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