Clamp assembly for clamping a transmission electron microscope sample for a thermal vacuum volatilization test and a method for testing thermal vacuum volatilization properties of a material

Abstract

The application relates to the technical field of testing the chemical or physical properties of materials, in particular to a clamp assembly for clamping a transmission electron microscope sample to perform a hot vacuum volatilization test and a material hot vacuum volatilization characteristic test method. The clamp assembly comprises a first clamp, a second clamp and a sample positioning piece. The first clamp and the second clamp are connected to form a containing cavity, the first clamp is formed with a detection hole communicating with the containing cavity, and the size of the detection hole is smaller than that of the transmission electron microscope sample. The sample positioning piece is at least partially arranged in the containing cavity and is used for positioning the transmission electron microscope sample so that the transmission electron microscope sample can be kept in a position facing the detection hole. According to the embodiment of the application, the transmission electron microscope sample is kept in the position facing the detection hole through cooperation of the first clamp, the second clamp and the sample positioning piece, so that the material to be tested for the hot vacuum volatilization characteristic can be made into the shape of the transmission electron microscope sample, and the hot vacuum volatilization test is performed under the clamping of the clamp assembly.

Description

Technical Field

[0001] The embodiments of this application relate to the technical field of testing the chemical or physical properties of materials, and in particular to a clamping assembly for holding transmission electron microscope samples for thermal vacuum volatilization testing and a method for testing the thermal vacuum volatilization characteristics of materials. Background Technology

[0002] This section is only intended to provide background information relevant to this application and does not necessarily constitute prior art.

[0003] The principle of nuclear power is to extract the fission energy from the reactor core and generate electricity through a thermoelectric conversion device. When used for deep space exploration, nuclear power sources need to withstand high temperatures (exceeding 800°C) and ultra-high vacuum (less than 1×10⁻⁶). -5 The thermal vacuum environment (Pa) necessitates thermal vacuum volatilization tests on materials used in nuclear power sources. However, current methods for testing the thermal vacuum volatilization characteristics of materials suffer from inaccurate results. Summary of the Invention

[0004] A brief overview of this application is provided below to offer a basic understanding of certain aspects thereof. It should be understood that this overview is not an exhaustive summary of the application. It is not intended to identify key or essential parts of the application, nor is it intended to limit its scope. Its purpose is merely to present certain concepts in a simplified form as a prelude to the more detailed description that follows.

[0005] In a first aspect, embodiments of this application provide a clamping assembly for holding a transmission electron microscope (TEM) sample for a thermal vacuum volatilization test. The clamping assembly includes a first clamp, a second clamp, and a sample positioning element. The first clamp and the second clamp are connected to form a receiving cavity. The first clamp has a detection hole communicating with the receiving cavity, the size of which is smaller than the size of the TEM sample. The sample positioning element is at least partially disposed in the receiving cavity for positioning the TEM sample so that the TEM sample can be held in a position facing the detection hole.

[0006] In this embodiment, the first clamp, the second clamp, and the sample positioning component work together to hold the transmission electron microscope (TEM) sample in a position facing the detection hole, thus preventing damage, movement, and detachment of the TEM sample during testing and observation. This facilitates the observation and transportation of the TEM sample, enabling the material to be tested for thermal vacuum volatilization characteristics to be shaped into a TEM sample and subjected to thermal vacuum volatilization testing under the clamping of the clamp assembly.

[0007] Secondly, embodiments of this application provide a method for testing the thermal vacuum volatilization characteristics of materials, comprising: S1, preparing a transmission electron microscope (TEM) sample; S2, detecting the surface morphology of the TEM sample using a TEM; S3, clamping the TEM sample using a fixture assembly provided in the first aspect of this application; S4, placing the fixture assembly holding the TEM sample into a thermal vacuum volatilization characteristic testing device for a thermal vacuum volatilization test; S5, removing the fixture assembly holding the TEM sample from the thermal vacuum volatilization characteristic testing device, electrically bonding the fixture assembly to the stage of a scanning electron microscope (SEM), and detecting the surface morphology of the TEM sample after the thermal vacuum volatilization test using an SEM.

[0008] These and other advantages of this application will become more apparent from the following detailed description of preferred embodiments in conjunction with the accompanying drawings. Attached Figure Description

[0009] To further illustrate the above and other advantages and features of this application, the specific embodiments of this application will be described in more detail below with reference to the accompanying drawings. The drawings, together with the following detailed description, are included in and form a part of this specification. Elements having the same function and structure are indicated by the same reference numerals. It should be understood that these drawings only depict typical examples of this application and should not be considered as limiting the scope of this application.

[0010] Figure 1 This is a schematic diagram of a clamp assembly according to one embodiment of the present application;

[0011] Figure 2 This is a cross-sectional schematic diagram of a clamp assembly according to an embodiment of this application;

[0012] Figure 3 This is an exploded view of a clamp assembly according to an embodiment of this application.

[0013] It should be noted that the accompanying drawings are not necessarily drawn to scale, but are shown only in a schematic manner without affecting the reader's understanding.

[0014] Explanation of reference numerals in the attached figures:

[0015] 1. Fixture assembly;

[0016] 10. First clamp; 11. Receiving cavity; 12. Cover; 121. Inspection hole; 13. Ring-shaped part; 131. Clamping hole;

[0017] 20. Second clamp; 21. Rotating part; 22. Protrusion; 221. Second mating part;

[0018] 30. Sample positioning component; 31. Body; 311. Positioning groove; 32. First mating part;

[0019] 40. Anchoring components;

[0020] 50. Sample. Detailed Implementation

[0021] Exemplary embodiments of this application will be described below with reference to the accompanying drawings. For clarity and brevity, not all features of actual implementations are described in the specification. However, it should be understood that many implementation-specific decisions must be made in the development of any such actual embodiment to achieve the developer's specific goals, such as complying with constraints related to the system and business, and these constraints may vary depending on the implementation. Furthermore, it should be understood that while development work can be very complex and time-consuming, such development work is merely a routine task for those skilled in the art who benefit from the content of this application.

[0022] It should also be noted that, in order to avoid obscuring this application with unnecessary details, only the equipment structure and / or processing steps closely related to the solution according to this application are shown in the accompanying drawings, while other details that are not closely related to this application are omitted.

[0023] It should be noted that, unless otherwise defined, the technical or scientific terms used in this application shall have the ordinary meaning as understood by a person with ordinary skills in the field to which this application pertains.

[0024] In the description of the embodiments of this application, "multiple" means at least two, such as two, three, etc., unless otherwise explicitly specified.

[0025] Before and after conducting thermal vacuum volatilization tests on materials, it is necessary to observe the microstructure of the samples using transmission electron microscopy (TEM) and scanning electron microscopy (SEM). In related techniques, to meet the testing requirements of TEM, the samples need to be cut and processed into TEM samples after the test. TEM samples are typically circular discs with a diameter of approximately 3 mm. A through-hole is formed in the center of the disc, surrounded by a thin region of 100-200 nm thick, used for TEM observation.

[0026] The inventors of this application discovered that cutting or other processing of the samples after the test can lead to inaccurate test results. Using an in-situ heating rod for thermal vacuum volatilization under a transmission electron microscope can avoid this problem, but such a test would be very expensive.

[0027] In order to reduce testing costs, the inventors of this application have discovered that before conducting the thermal vacuum volatilization test, the sample can be made into a transmission electron microscope (TEM) sample, and then the TEM sample can be clamped by a clamping assembly and placed into a high-temperature, high-vacuum thermal vacuum volatilization test device to conduct the TEM sample volatilization test.

[0028] Based on this, embodiments of this application provide a clamping assembly for holding transmission electron microscope samples for thermal vacuum volatilization tests. Figure 1 This is a schematic diagram of a clamp assembly according to one embodiment of the present application. Figure 2 This is a cross-sectional schematic diagram of a clamp assembly according to an embodiment of this application. Figure 1 and Figure 2 As shown, the clamp assembly 1 includes a first clamp 10, a second clamp 20, and a sample positioning element 30. The first clamp 10 and the second clamp 20 are connected to form a receiving cavity 11. The first clamp 10 has a detection hole 121 communicating with the receiving cavity 11. The size of the detection hole 121 is smaller than the size of the transmission electron microscope sample 50. The sample positioning element 30 is at least partially disposed in the receiving cavity 11 for positioning the transmission electron microscope sample 50 so that the transmission electron microscope sample 50 can be held in a position facing the detection hole 121.

[0029] The clamp assembly 1 of this application sets the sample positioning member 30 in the receiving cavity 11, so that the transmission electron microscope sample 50 is kept in a position facing the detection hole 121, avoiding damage, movement and fall off of the transmission electron microscope sample 50 during the test, and facilitating the transfer and transportation of the transmission electron microscope sample 50. Thus, it is possible to make the material to be tested for thermal vacuum volatilization characteristics into the shape of a transmission electron microscope sample and perform thermal vacuum volatilization test under the clamping of the clamp assembly 1.

[0030] Thus, before the experiment begins, the transmission electron microscope (TEM) sample 50 can be placed on the TEM stage, and the surface morphology of the TEM sample 50 before the thermal vacuum volatilization test can be detected using the TEM. Then, the TEM sample 50 is assembled with the clamp assembly 1 (the clamp assembly 1 can be conductively bonded to the TEM stage, and the surface morphology of the TEM sample 50 before the thermal vacuum volatilization test can be detected using the TEM), and the clamp assembly 1 holds the TEM sample 50 for the experiment. After the experiment, the TEM sample 50 can be separated from the clamp assembly 1, and the TEM sample 50 can be placed on the TEM stage, and the surface morphology of the TEM sample 50 after the thermal vacuum volatilization test can be detected using the TEM. Alternatively, the clamp assembly 1 can be directly conductively bonded to the TEM stage, and the surface morphology of the TEM sample 50 after the thermal vacuum volatilization test can be detected using the TEM. Since no processing of the sample is required after the experiment, the true morphology of the sample before and after the experiment can be obtained more accurately, making the test results more accurate.

[0031] Figure 3 This is an exploded view of a clamp assembly 1 according to an embodiment of this application. Figure 3 As shown, in some embodiments, the sample positioning element 30 includes a positioning groove 311, the depth of which is less than or equal to the thickness of the transmission electron microscope (TEM) sample 50. When the first clamp 10 and the second clamp 20 are connected, the TEM sample 50 can abut against the periphery of the detection hole 121. By placing the TEM sample 50 in the positioning groove 311 and having the periphery of the detection hole 121 abut against the TEM sample 50, the TEM sample 50 is fixed in the center of the positioning groove 311, preventing the TEM sample 50 from moving during testing and observation.

[0032] In some embodiments, the diameter of the transmission electron microscope (TEM) sample is 3 mm. In some embodiments, the peripheral thickness of the TEM sample 50 can be greater than 0.2 mm and less than or equal to 0.3 mm, and the groove depth of the positioning groove 311 can be 0.2 mm.

[0033] In some embodiments, the positioning groove 311 can be a circular groove, and the inner diameter of the positioning groove 311 can be slightly larger than the outer diameter of the transmission electron microscope sample 50, which is beneficial for fixing the transmission electron microscope sample 50 with the positioning groove 311. For example, the inner diameter of the positioning groove 311 can be 0.1-0.5 mm larger than the outer diameter of the transmission electron microscope sample 50.

[0034] like Figure 2 and Figure 3 As shown, in some embodiments, the sample positioning member 30 includes a body 31 and a first mating part 32. A positioning groove 311 is formed in the body 31, the body 31 is located in the receiving cavity 11, and the first mating part 32 is connected to the body 31. The second clamp 20 forms a second mating part 221, and through the cooperation of the first mating part 32 and the second mating part 221, the sample positioning member 30 faces the detection hole 121.

[0035] like Figure 3 As shown, in some embodiments, the first clamp 10 includes an annular member 13 and a cover 12 disposed at one end of the annular member 13, with a detection hole 121 formed in the cover 12. The annular member 13 and the cover 12 together with the second clamp 20 form a receiving cavity 11.

[0036] In some embodiments, the cover 12 is connected to the radially inner edge of the annular member 13, and the end face of the cover 12 and the annular member 13 away from the second clamp 20 is flush. The detection hole 121 may be formed at the center of the cover 12.

[0037] In some embodiments, the overall size of the clamp assembly is less than 350 mm, so that the clamp assembly 1 can hold the transmission electron microscope (TEM) sample 50 for observation under a scanning electron microscope (SEM). Since the TEM sample 50 undergoes a thermal vacuum volatilization test while held by the clamp assembly 1, and can be directly observed under the SEM while held by the clamp, the testing efficiency is improved. Furthermore, it avoids the influence of the test sample during the subsequent preparation of the SEM sample, thus improving the accuracy of the thermal vacuum volatilization test results.

[0038] When performing scanning electron microscopy (SEM) observations, the closer the SEM objective lens is to the sample surface, the clearer the observation of the sample surface morphology. In some embodiments, the thickness of the cover 12 is 0.1-0.2 mm. Setting a thinner cover 12 can reduce the distance between the sample 50 surface and the cover 12 surface, thereby facilitating a closer distance between the SEM objective lens and the sample surface, thus ensuring that observation can be performed at an appropriate magnification.

[0039] In some embodiments, the distance between the detection hole 121 and the annular member 13 is 1-1.5 mm. This ensures the overall mechanical strength of the first clamp 10 when the cover member 12 is relatively thin, and ensures the stability of the clamp assembly 1 during the material thermal vacuum volatilization test.

[0040] like Figure 3 As shown, in some embodiments, the first clamp 10, the second clamp 20, and the sample positioning member 30 are made of tantalum, and the cover 12 is welded to the annular member 13. Tantalum is ductile and easy to weld. Using tantalum, the cover 12 can be made with a thickness as thin as 0.1-0.2 mm, and the cover 12 can be welded to the annular member 13 using a welding process, ensuring the machining accuracy and mechanical strength of the cover 12. In particular, when the sample 50 is placed in the tantalum clamp assembly 1 for a thermal vacuum volatilization characteristic test apparatus for a thermal vacuum volatilization test, the thermal deformation of the tantalum is small, which helps to maintain the stability of the sample 50.

[0041] like Figure 2 and Figure 3 As shown, in some embodiments, the second clamp 20 includes a rotating portion 21 and a protrusion 22 connected to the rotating portion 21, the protrusion 22 being threadedly connected to the annular member 13; a second mating portion 221 is formed on the protrusion 22. The protrusion 22 is able to enter the radially inner side of the annular member 13 so that the second mating portion 221 faces the detection hole 121.

[0042] The embodiments of this application achieve a tight connection between the first clamp 10 and the second clamp 20 by threading the protrusion 22 and the annular part 13. At the same time, the distance between the detection hole 121 and the positioning groove 311 can be adjusted according to the thickness of the sample 50 to achieve observation of samples 50 with different thicknesses.

[0043] Specifically, when assembling fixture assembly 1, the sample positioning component 30 is first placed in the second fixture 20, the sample 50 is placed in the positioning groove 311 of the sample positioning component 30, and the annular component 13 of the first fixture 10 is placed on the protrusion 22. When the second fixture 20 rotates relative to the first fixture 10, the sample positioning component 30 drives the sample 50 to rotate together and continuously move towards the cover component 12. When the sample 50 or the sample positioning component 30 contacts the cover component 12 of the first fixture 10, as the second fixture 20 continues to rotate relative to the first fixture 10, the sample 50 or the sample positioning component 30 will no longer rotate relative to the first fixture 10 under the action of friction, thereby avoiding wear on the sample 50 and causing inaccurate testing of the sample 50.

[0044] In some embodiments, the outer surface of the protrusion 22 may be an M5 thread, and the inner surface of the annular member 13 may be an M5 thread that matches the outer surface of the protrusion 22.

[0045] In some embodiments, the rotating part 21 may be a circular plate structure that is flush with the radial outer surface of the annular part 13.

[0046] In some embodiments, the radially outer surface of the annular member 13 may also form two opposing and parallel tangential surfaces, so that when assembling the clamping assembly 1, the annular member 13 is kept relatively stationary by clamping the tangential surfaces, thereby driving the rotating part 21 to rotate and tightening the first clamp 10 and the second clamp 20.

[0047] like Figure 2 and Figure 3 As shown, in some embodiments, the second mating part 221 is a mating groove formed on the protrusion 22; the first mating part 32 enters the mating groove and is in clearance fit with the mating groove.

[0048] In some embodiments, the size of the body 31 is larger than the size of the mating groove, and the body 31 contacts the protrusion 22 above the mating groove. In some embodiments, the mating groove passes through the rotating part 21 and the protrusion 22, and the length of the first mating part 32 is equal to the sum of the heights of the protrusion 22 and the rotating part 21.

[0049] Specifically, when assembling the fixture assembly 1, the first mating part 32 is inserted into the mating groove, and the sample 50 is placed in the positioning groove 311. When the rotating part 21 rotates, the friction between the first mating part 32 and the mating groove, and between the body 31 and the protrusion 22, causes the sample positioning member 30 to drive the sample 50 to rotate together and continuously move towards the cover 12. When the sample 50 or the sample positioning member 30 contacts the cover 12 of the first fixture 10, as the second fixture 20 continues to rotate relative to the first fixture 10, the friction between the sample 50 or the sample positioning member 30 and the cover 12 is greater than the sum of the friction between the first mating part 32 and the mating groove, and between the body 31 and the protrusion 22. The sample positioning member 30 and the sample 50 will no longer rotate relative to the first fixture 10, thereby avoiding wear on the sample 50 and causing inaccurate testing of the sample 50.

[0050] In some embodiments, the protrusion 22 is disposed at the center of the rotating part 21, and the first mating part 32 is located at the center of the annular part 13, thereby fixing the sample 50 at the center of the clamp assembly 1.

[0051] like Figure 2 and Figure 3 As shown, in some embodiments, the inner diameter of the annular member 13 is larger than the outer diameter of the body 31 of the sample positioning member 30, so that there is a gap between the radially inner surface of the annular member 13 and the body 31. This arrangement prevents the sample positioning member 30 from contacting the radially inner surface of the first clamp 10 during the rotation of the second clamp 20 relative to the first clamp 10 when the second clamp 20 is threadedly engaged with the first clamp 10, thus preventing friction caused by the contact between the sample positioning member 30 and the first clamp 10 from interfering with the threaded engagement between the second clamp 20 and the first clamp 10.

[0052] like Figure 1 and Figure 2 As shown, in some embodiments, the first clamp 10 further forms a clamping hole 131 communicating with the receiving cavity 11. The clamp assembly 1 also includes a clamping member 40, which enters the clamping hole 131 to clamp the second clamp 20, thereby fixing the relative positions of the first clamp 10 and the second clamp 20. By setting the clamping member 40 to cooperate with the clamping hole 131, the relative positions of the first clamp 10 and the second clamp 20 can be further fixed, ensuring that the sample 50 remains in the same position in the clamp assembly 1 during transportation and transfer.

[0053] In some embodiments, a clamping hole 131 is formed on a cross-section of the annular member 13 so that the clamping member 40 enters the clamping hole 131 to clamp the second clamp 20.

[0054] In some embodiments, the clamping member 40 and the clamping hole 131 can be threadedly connected, wherein the clamping member 40 can fix a set screw, such as an M3 set screw, and the clamping hole 131 is a threaded hole that matches the size of the fixed set screw.

[0055] The embodiments of this application also provide a method for testing the thermal vacuum volatilization characteristics of materials, including: S1, preparing a transmission electron microscope (TEM) sample 50 from the sample to be tested; S2, detecting the surface morphology of the TEM sample using a TEM; S3, clamping the TEM sample 50 using a clamp assembly 1 provided in any embodiment of this application; S4, placing the clamp assembly 1 holding the TEM sample 50 into a thermal vacuum volatilization characteristic testing device for a thermal vacuum volatilization test; S5, removing the clamp assembly 1 holding the TEM sample 50 from the thermal vacuum volatilization characteristic testing device, conductively bonding the clamp assembly 1 to the stage of a scanning electron microscope (SEM), and detecting the surface morphology of the TEM sample 50 after the thermal vacuum volatilization test using an SEM.

[0056] The clamp assembly 1 of this application, by placing the sample positioning member 30 in the receiving cavity 11, keeps the transmission electron microscope (TEM) sample 50 in a position facing the detection hole 121, preventing damage, movement, and detachment of the TEM sample 50 during the test, and facilitating the transfer and transportation of the TEM sample 50. This allows the material to be tested for thermal vacuum volatilization characteristics to be shaped into a TEM sample and subjected to thermal vacuum volatilization testing under the clamping of the clamp assembly 1. Since no sample processing is required after the thermal vacuum volatilization characteristic test, the true morphology of the sample before and after the test can be obtained more accurately, resulting in more accurate test results.

[0057] Since the transmission electron microscope sample 50 is held by the fixture assembly 1 for the thermal vacuum volatilization test, and can be directly observed by the scanning electron microscope while held by the fixture, the testing efficiency is improved. It can also avoid the influence of the test sample on the test sample during the later process of making the test sample into a scanning electron microscope sample, thereby improving the accuracy of the thermal vacuum volatilization test results.

[0058] In some embodiments, the transmission electron microscope (TEM) sample 50 is a circular disc with a diameter of 3 mm. A through-hole is formed in the center of the disc, and a thin region with a thickness of 100-200 nm is formed around the through-hole for TEM observation. In S1, the through-hole in the center of the 3 mm diameter circular disc sample and the thin region with a thickness of 100-200 nm around the through-hole can be formed using an electrolyte etching process.

[0059] In some embodiments, after step S3 and before step S4, the method may further include: electrically attaching the fixture assembly 1 to the stage of the scanning electron microscope, and using the scanning electron microscope to detect the surface morphology of the transmission electron microscope sample 50 before conducting the thermal vacuum volatilization test.

[0060] In some embodiments, after step S5, the transmission electron microscope sample 50 can be separated from the fixture assembly 1, and the transmission electron microscope sample 50 can be placed on the stage of the transmission electron microscope to detect the surface morphology of the transmission electron microscope sample 50 after the thermal vacuum volatilization test.

[0061] Regarding the embodiments of this application, it should also be noted that, without conflict, the embodiments of this application and the features in the embodiments can be combined with each other to obtain new embodiments.

[0062] The above description is merely a specific embodiment of this application, but the scope of protection of this application is not limited thereto. The scope of protection of this application shall be determined by the scope of the claims.

Claims

1. A clamping assembly for holding transmission electron microscope samples for thermal vacuum volatilization testing, characterized in that, The clamp assembly includes: A first clamp and a second clamp are connected to form a receiving cavity. The first clamp has a detection hole communicating with the receiving cavity. The size of the detection hole is smaller than the size of the transmission electron microscope sample. A sample positioning element, at least partially disposed in the receiving cavity, is used to position the transmission electron microscope sample so that the transmission electron microscope sample can be held in a position facing the detection aperture; The sample positioning component includes a positioning groove, the depth of which is less than or equal to the thickness of the transmission electron microscope sample. When the first clamp and the second clamp are connected, the transmission electron microscope sample can abut against the periphery of the detection hole. The sample positioning element includes: The body, wherein the positioning groove is formed in the body, and the body is located in the receiving cavity; The first mating part is connected to the main body; The second fixture forms a second mating part, and through the cooperation of the first mating part and the second mating part, the sample positioning element faces the detection hole. The first clamp includes an annular component and a cover component disposed at one end of the annular component, and the detection hole is formed in the cover component; The second clamp includes a rotating part and a protrusion connected to the rotating part, the protrusion and the annular part being threadedly connected; The second mating portion is formed on the protrusion; The protrusion can enter the radially inner side of the annular part so that the second mating part faces the detection hole.

2. The clamping assembly according to claim 1, characterized in that, The overall size of the clamping assembly is less than or equal to 35 mm, so that the clamping assembly can hold the transmission electron microscope sample for observation under a scanning electron microscope; The thickness of the cover is 0.1-0.2 mm, and the distance between the detection hole and the annular part is 1-1.5 mm.

3. The clamping assembly according to claim 1, characterized in that, The first clamp, the second clamp, and the sample positioning element are made of tantalum; The cover is welded to the annular component.

4. The clamping assembly according to claim 1, characterized in that, The second mating part is a mating groove formed on the protrusion; The first mating part enters the mating groove and is in clearance fit with the mating groove.

5. The clamping assembly according to claim 1, characterized in that, The inner diameter of the annular component is larger than the outer diameter of the sample positioning component, so that there is a gap between the radial inner surface of the annular component and the body.

6. The clamping assembly according to any one of claims 1-5, characterized in that, The first clamp also has a mating hole communicating with the receiving cavity; The clamping assembly further includes a clamping member that enters the clamping hole to clamp the second clamp, thereby fixing the relative positions of the first clamp and the second clamp.

7. A method for testing the thermal vacuum volatilization characteristics of materials, characterized in that, include: S1. Prepare the sample to be tested into a transmission electron microscope sample; S2. The surface morphology of the transmission electron microscope sample is detected using a transmission electron microscope; S3. Clamp the transmission electron microscope sample using the clamping assembly; S4. Place the clamp assembly holding the transmission electron microscope sample into the thermal vacuum volatilization characteristic test device for thermal vacuum volatilization test; S5. Remove the clamping assembly holding the transmission electron microscope sample from the thermal vacuum volatilization characteristic test device, and electrically attach the clamping assembly to the stage of the scanning electron microscope. Use the scanning electron microscope to detect the surface morphology of the transmission electron microscope sample after the thermal vacuum volatilization test. The clamp assembly includes: A first clamp and a second clamp are connected to form a receiving cavity. The first clamp has a detection hole communicating with the receiving cavity. The size of the detection hole is smaller than the size of the transmission electron microscope sample. A sample positioning element, at least partially disposed in the receiving cavity, is used to position the transmission electron microscope sample so that the transmission electron microscope sample can be held in a position facing the detection aperture; The sample positioning component includes a positioning groove, the depth of which is less than or equal to the thickness of the transmission electron microscope sample. When the first clamp and the second clamp are connected, the transmission electron microscope sample can abut against the periphery of the detection hole. The sample positioning element includes: The body, wherein the positioning groove is formed in the body, and the body is located in the receiving cavity; The first mating part is connected to the main body; The second fixture forms a second mating part, and through the cooperation of the first mating part and the second mating part, the sample positioning element faces the detection hole. The first clamp includes an annular component and a cover component disposed at one end of the annular component, and the detection hole is formed in the cover component; The second clamp includes a rotating part and a protrusion connected to the rotating part, the protrusion and the annular part being threadedly connected; The second mating portion is formed on the protrusion; The protrusion can enter the radially inner side of the annular part so that the second mating part faces the detection hole.

8. The test method according to claim 7, characterized in that, The overall size of the clamping assembly is less than or equal to 35 mm, so that the clamping assembly can hold the transmission electron microscope sample for observation under a scanning electron microscope; The thickness of the cover is 0.1-0.2 mm, and the distance between the detection hole and the annular part is 1-1.5 mm.

9. The test method according to claim 7, characterized in that, The first clamp, the second clamp, and the sample positioning element are made of tantalum; The cover is welded to the annular component.

10. The test method according to claim 7, characterized in that, The second mating part is a mating groove formed on the protrusion; The first mating part enters the mating groove and is in clearance fit with the mating groove.

11. The test method according to claim 7, characterized in that, The inner diameter of the annular component is larger than the outer diameter of the sample positioning component, so that there is a gap between the radial inner surface of the annular component and the body.

12. The test method according to any one of claims 7-11, characterized in that, The first clamp also has a mating hole communicating with the receiving cavity; The clamping assembly further includes a clamping member that enters the clamping hole to clamp the second clamp, thereby fixing the relative positions of the first clamp and the second clamp.

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