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CN-122016533-A - Test device and method for three-electrode in-situ electrochemical hydrogen charging micro-nano mechanical test

CN122016533ACN 122016533 ACN122016533 ACN 122016533ACN-122016533-A

Abstract

The invention discloses a test device and a test method for three-electrode in-situ electrochemical hydrogen charging micro-nano mechanical test, and belongs to the technical field of hydrogen energy. The device prevents hydrogen from overflowing or generating bubbles by a three-electrode system electrochemical in-situ hydrogen charging test method, and ensures that a sample is kept completely immersed in a hydrogen charging solution in the long-time test process of hardness, hydrogen diffusion coefficient, fatigue performance and the like. The device is characterized in that a sample placing table is connected with a container assembly, a sample is immersed in hydrogen charging solution, and mechanical property characterization, hydrogen diffusion coefficient measurement and the like are performed on the sample through a nano indentation instrument. The invention effectively solves the problem that hydrogen in the material overflows and hydrogen bubbles are generated by in-situ hydrogen filling in the process from the completion of hydrogen filling to the beginning of the test in the traditional ex-situ hydrogen filling method to interfere with micro-nano mechanical test, and can effectively inhibit the bubbles generated during hydrogen filling by carrying out three-electrode controllable constant potential hydrogen filling on the electrode, the reference electrode and the sample so as to solve the influence of the bubbles on the micro-nano mechanical test.

Inventors

  • WU WEIJIE
  • Xia Chenwei
  • YE FEI
  • WANG XIAOWEI
  • PENG YAWEI
  • GONG JIANMING

Assignees

  • 南京工业大学

Dates

Publication Date
20260512
Application Date
20260312

Claims (9)

  1. 1. The test device for the three-electrode in-situ electrochemical hydrogen charging micro-nano mechanical test comprises an electrochemical workstation (4) and a nano indentation instrument and is characterized by comprising a container assembly and a lofting assembly, wherein the container assembly is internally used for accommodating the lofting assembly, and hydrogen charging solution (5) is filled in the container assembly; The lofting component is used for placing a sample (3), The platinum wire electrode (6) and the calomel reference electrode (9) are respectively and electrically connected with the electrochemical workstation (4); the sample (3) is electrically connected with an electrochemical workstation (4); The container assembly was positioned on a nanoindentation instrument for testing experiments.
  2. 2. The test device for the three-electrode in-situ electrochemical hydrogen charging micro-nano mechanical test according to claim 1, wherein the container assembly comprises a base (10) and a containing cavity (13); The base (10) is provided with a containing cavity (13), and the horizontal end surface of the base (10) is larger than the end surface of the containing cavity (13); a boss (14) for fixing the lofting component is arranged in the accommodating cavity (13); the side wall of the containing cavity (13) is provided with a left connecting port (12) and a right connecting port (15) for fixing the platinum wire electrode (6) and the calomel reference electrode (9).
  3. 3. The test device for the three-electrode in-situ electrochemical hydrogen charging micro-nano mechanical test according to claim 2 is characterized in that the left connecting port (12) is used for fixing a platinum wire electrode (6) and is positioned at the center of the side wall of the containing cavity (13); The right connecting port (15) is used for fixing the calomel reference electrode (9), is positioned on the side wall of the accommodating cavity (13) at the other side of the left connecting port (12), and is close to the upper edge part of the side wall of the accommodating cavity (13); The calomel reference electrode (9) is close to the sample (3) of the lofting component.
  4. 4. The test device for the three-electrode in-situ electrochemical hydrogen charging micro-nano mechanical test according to claim 1 or 2, wherein the lofting assembly comprises a lofting table (7) and a fixing bolt, and the shape of the lofting table (7) is matched with that of a boss (14); The sample stage (7) is provided with a sample stage (18) and screw holes (19) are uniformly distributed; the boss (14) is provided with a first screw hole (16) which is matched with the second screw hole (19) of the sample placing table (7), and the first screw hole (16) and the second screw hole (19) between the sample placing table (7) and the boss (14) are mutually fixed through bolts; The horizontal plane at the upper end of the sample placing table (7) is used for placing a sample (3).
  5. 5. The test device for the three-electrode in-situ electrochemical hydrogen charging micro-nano mechanical test according to claim 4, wherein the sample stage (7) and the inner wall of the containing cavity (13) of the container assembly are in non-contact arrangement; The combined height of the sample stage (7), the sample (3) and the boss (14) is lower than the top level of the accommodating cavity (13).
  6. 6. The test device for the three-electrode in-situ electrochemical hydrogen charging micro-nano mechanical test according to claim 3, wherein a silica gel seal is adopted between the left connecting port (12) and the platinum wire electrode (6); And a silica gel seal is adopted between the right connecting port (15) and the calomel reference electrode (9).
  7. 7. A test method using the three-electrode in-situ electrochemical hydrogen-charging micro-nano mechanical test device according to any one of claims 1 to 6, characterized by the following steps: Step 1, adhering a sample (3) connected with a lead to a sample stage (7), and fixing the sample stage (7) with a boss (14) in a cavity (13); Step 2, a platinum wire electrode (6) and a calomel reference electrode (9) are respectively counted on a left connecting port (12) and a right connecting port (15) corresponding to the containing cavity (13), and the interfaces are sealed through silica gel; Step 3, mounting the accommodating cavity (13) on a test bed of a nano indentation instrument, and fixing through the base (10); step 4, injecting the electrolyte (5) into the accommodating cavity (13), and keeping the liquid level of the electrolyte (5) lower than the top level of the accommodating cavity (13); step 5, presetting test current density in an electrochemical workstation (4); And 6, operating the submerged pressure head (2) of the nano indentation instrument to test the sample (3) and recording test data.
  8. 8. The method of the three-electrode in-situ electrochemical hydrogen-charging micro-nano mechanical test device according to claim 7, wherein the hydrogen-charging solution (5) in the step 4 contains an electrolyte.
  9. 9. The method of the three-electrode in-situ electrochemical hydrogen-charging micro-nano mechanical test device according to claim 7, wherein the reference voltage of the saturated calomel reference electrode (9) in step 5 is controlled to be E corr – 0.8 V ~ E corr +0.5v, wherein E corr is the corrosion potential.

Description

Test device and method for three-electrode in-situ electrochemical hydrogen charging micro-nano mechanical test Technical Field The invention belongs to the technical field of hydrogen energy, and particularly relates to a test device and a test method for a three-electrode in-situ electrochemical hydrogen charging micro-nano mechanical test. Background Along with the increasing exhaustion of fossil energy, the development of new energy has become a goal pursued by global scientists, and hydrogen energy has the advantages of high efficiency, cleanliness, large reserves and the like compared with other energy sources. There are a number of problems associated with this, such as the flammability and explosiveness of hydrogen, the need for great care during storage and transportation, and the hydrogen contact with the metal may also cause hydrogen embrittlement. Therefore, in the context of hydrogen economy, high requirements are put on the hydrogen embrittlement resistance of the metal materials. The hydrogen embrittlement phenomenon refers to a phenomenon that after hydrogen atoms penetrate into a metal material, toughness or bearing capacity of the metal material is reduced, and low-stress brittle fracture is initiated. This phenomenon is called "metal plague", and constitutes a serious threat to the safety of critical materials in the fields of aerospace, energy transportation, chemical equipment and the like. In order to study the effect of hydrogen on metallic materials, it is necessary to subject the metallic materials to a hydrogen charging process and then test the mechanical properties thereof and observe the microstructure. Common hydrogen charging methods include aqueous solution electrolytic charging, gas phase charging and molten salt electrolytic charging, wherein the application of the aqueous solution electrolytic charging is the most widely used. Benefiting from the advantages of environmental protection, lower cost and the like. Most of the research is currently macroscopic in which the effect of hydrogen on metallic materials is reflected. However, with further research, the influence of hydrogen on metal materials on a microscopic scale is becoming more and more important, and thus research is required by using precise instruments such as nanoindentation. The conventional hydrogen filling method can combine hydrogen in the material into hydrogen to overflow in the process from the completion of hydrogen filling to the beginning of the test, thereby affecting the accuracy of the test. The in-situ hydrogen charging method can ensure that the metal material always maintains higher hydrogen concentration and no hydrogen overflows. However, the method of using in-situ charging in the nanoindentation test needs to consider that bubbles generated by charging have an influence on the nanoindentation test result. It is important to suppress the generation of bubbles during the hydrogen filling process. In summary, the effect of hydrogen on the microscopic aspect of the metal material can be studied by using the nanoindentation apparatus, but there is no test apparatus capable of performing nanoindentation test while charging hydrogen, so that the microscopic aspect of the study is very difficult. Disclosure of Invention The invention provides an in-situ constant potential electrochemical hydrogen charging micro-nano mechanical testing device and method, solves the problem that the research on the influence of hydrogen on a metal material is difficult in the microscopic field, effectively solves the problem that hydrogen is combined into hydrogen to overflow and cannot be subjected to long experiments, and can be used for carrying out long-time tests on the metal material in a hydrogen environment, such as a mechanical property test, a hydrogen diffusion coefficient test and a fatigue test, so that the influence of hydrogen on the metal material on the microscopic scale is further researched. The invention adopts the following technical scheme: The invention relates to a test device for a three-electrode in-situ electrochemical hydrogen charging micro-nano mechanical test, which consists of two parts, including a container assembly and a sample stage. The container assembly is used to provide a hydrogen environment for hydrogen to fully enter the metallic material. The container assembly is filled with hydrogen charging solution, the container assembly is provided with a platinum wire electrode and a calomel reference electrode which are in contact with the hydrogen charging solution, the platinum wire electrode and the calomel reference electrode are respectively and electrically connected with an electrochemical workstation, a sample is electrically connected with the electrochemical workstation, and a sample placing table is used for placing the sample, and the sample is connected with a wire and is in contact with a nano indentation needle. The sample stage is rectangular and has special arc not