Transmission electron microscope sample rod and sample testing method

Abstract

A transmission electron microscope sample rod (100) and a sample testing method. The transmission electron microscope sample rod (100) comprises a heating element (10) and a testing mechanism (20), wherein the heating element (10) is configured to heat a sample, the testing mechanism (20) is constructed with a plurality of connecting arms (21) which are arranged at intervals in a circumferential direction of the testing mechanism (20), an accommodating space (23) is defined by means of the plurality of connecting arms (21), one side of each connecting arm (21) facing the accommodating space is defined as an output end (202), the plurality of output ends (202) jointly clamp the sample, each connecting arm (21) can extend and retract in an extension direction of the output end (202), and each connecting arm (21) is connected to the heating element (10).

Description

Transmission electron microscope sample holder and sample testing method

[0001] Related applications

[0002] This application claims priority to Chinese patent application number 202311085300.X, filed on August 25, 2023, entitled “Transmission electron microscope sample rod and sample testing method”, the entire contents of which are incorporated by reference into this application. Technical Field

[0003] The present application relates to the technical field of transmission electron microscope accessories and nanomaterial in-situ research, and in particular to a transmission electron microscope sample rod and a sample testing method. Background Art

[0004] Transmission electron microscopy (TEM), a device with ultra-high resolution that uses an electron beam as its light source, is widely used to study the microstructure, physical, and chemical properties of materials at the nanoscale and atomic scale. With the development of in-situ TEM technology, researchers can apply various physical effects to samples to replicate the material's actual service environment. Simultaneously, they can observe changes in the material's microstructure, physical, and chemical properties during the application of these effects under TEM. This allows for direct study of the performance of materials or devices during actual use, which is of great significance for improving material performance and optimizing material processing techniques.

[0005] Materials subjected to long-term high-temperature operation not only withstand thermal loads but also face a complex stress state caused by the combined effects of multiple mechanical loads. However, currently available transmission electron microscope (TEM) in-situ high-temperature mechanical specimen holders cannot reflect the microstructural evolution of materials subjected to complex stresses during actual service. This makes it difficult to provide an accurate and reliable scientific basis for improving material performance, hindering the research and development of these materials.

[0006] Summary of the Invention

[0007] According to various embodiments of the present application, a transmission electron microscope sample holder and a sample testing method are provided.

[0008] A transmission electron microscope sample holder, comprising a heating element and a testing mechanism; the heating element is used to heat the sample; the testing mechanism is constructed with a plurality of connecting arms arranged at intervals along the circumference of the testing mechanism, the plurality of connecting arms are arranged to form an accommodating space, and the side of each connecting arm facing the accommodating space is defined as an output end, the plurality of output ends jointly clamp the sample, and each connecting arm can be extended and retracted along the extension direction of the output end; each connecting arm is connected to the heating element.

[0009] In one embodiment, the testing mechanism is provided with connecting arms on both sides along the first direction and on both sides along the second direction, respectively, and the transmission electron microscope sample rod includes a plurality of driving members arranged at intervals, and the end of the connecting arm away from the accommodating space is defined as the input end, and each of the driving members is connected to the input end; wherein, the first direction and the second direction are arranged at an angle.

[0010] In one embodiment, the driving member is configured as a piezoelectric driver, the connecting arm is configured as a flexible hinge, the input end and the output end of each flexible hinge are configured at an angle, and the input end is attached to the piezoelectric driver.

[0011] In one embodiment, the testing mechanism further includes a fixing portion, and along the circumference of the testing mechanism, the fixing portion is connected between the input ends of any two adjacent flexible hinges, and the fixing portion is connected to the heating element.

[0012] In one embodiment, the transmission electron microscope sample holder further includes a thermal insulation member connected between the piezoelectric driver and the input end of the flexible hinge.

[0013] In one embodiment, the heating element is provided with a plurality of gaps arranged at intervals, and the piezoelectric driver and the thermal insulation element are installed at the gaps.

[0014] In one embodiment, the transmission electron microscope sample holder further includes a mounting frame, the mounting frame is provided with a mounting groove, the heating element is mounted at the bottom of the mounting groove, and the flexible hinge is located on the side of the heating element away from the bottom of the mounting groove.

[0015] In one embodiment, the mounting frame is constructed with a connecting portion, and the connecting portion is spaced apart from the mounting groove; the transmission electron microscope sample rod also includes a mounting seat and a rod body, and the mounting seat is connected between the rod body and the connecting portion.

[0016] In one embodiment, the mounting seat includes a seat body and a cover body, one of the seat body and the connecting part is configured with a positioning protrusion, and the other is configured with a positioning hole, the positioning protrusion is passed through the positioning hole, and the cover body is pressed onto the connecting part and connected to the seat body.

[0017] In one embodiment, the transmission electron microscope sample holder further includes a temperature measuring component, and a detection end of the temperature measuring component extends into the accommodating space.

[0018] In one embodiment, the temperature measuring element includes an optical fiber, the mounting frame is provided with a limiting groove and a guide hole connected to the limiting groove, the optical fiber extends into the limiting groove and passes through the guide hole; along the third direction, the heating element is provided with a through hole opposite to the accommodating space, the optical fiber passes through the through hole, and the end of the optical fiber faces the accommodating space.

[0019] The present application also provides a sample testing method, which is applied to the above-mentioned transmission electron microscope sample rod; the sample testing method includes: multiple connecting arms jointly clamping the sample; heating the sample to a first temperature; and each of the connecting arms extending or contracting along the extension direction of the output end.

[0020] In one embodiment, the extension or contraction of each of the connecting arms along the extension direction of the output end includes: applying a positive or negative voltage to the piezoelectric driver in the transmission electron microscope sample rod; the piezoelectric driver undergoes positive deformation according to the positive voltage or negative deformation according to the negative voltage; the connecting arm amplifies the deformation of the piezoelectric driver and transmits the amplified deformation to the sample.

[0021] In one embodiment, applying a positive or negative voltage to the piezoelectric actuator of the transmission electron microscope sample holder includes: applying the positive voltage to one of the piezoelectric actuators located on both sides of the test mechanism along the first direction, and applying the negative voltage to the other; and / or, applying the positive voltage to one of the piezoelectric actuators located on both sides of the test mechanism along the second direction, and applying the negative voltage to the other.

[0022] In one embodiment, the piezoelectric driver generates positive deformation according to the positive voltage or negative deformation according to the negative voltage, including: applying a positive voltage to one of the piezoelectric drivers located on both sides of the test mechanism along the first direction and applying a negative voltage to the other, the piezoelectric drivers on both sides generate relative or opposite deformations along the first direction; applying a positive voltage to one of the piezoelectric drivers located on both sides of the test mechanism along the second direction and applying a negative voltage to the other, the piezoelectric drivers on both sides generate relative or opposite deformations along the second direction.

[0023] In one embodiment, the connecting arm amplifies the deformation of the piezoelectric driver and transmits the amplified deformation to the sample, including: when the piezoelectric drivers located on both sides of the testing mechanism along the first direction are relatively deformed along the first direction, the sample is compressed along the first direction; when the piezoelectric drivers located on both sides of the testing mechanism along the first direction are deformed in opposite directions along the first direction, the sample is stretched along the first direction; when the piezoelectric drivers located on both sides of the testing mechanism along the second direction are relatively deformed along the second direction, the sample is compressed along the second direction; when the piezoelectric drivers located on both sides of the testing mechanism along the second direction are deformed in opposite directions along the second direction, the sample is stretched along the second direction.

[0024] The details of one or more embodiments of the present application are set forth in the accompanying drawings and the description below. Other features, objects, and advantages of the present application will become apparent from the description, drawings, and claims. BRIEF DESCRIPTION OF THE DRAWINGS

[0025] In order to more clearly illustrate the embodiments of the present application or the technical solutions in the conventional technology, the following briefly introduces the drawings required for use in the embodiments or the conventional technology descriptions. Obviously, the drawings described below are only some embodiments of the present application. For ordinary technicians in this field, other drawings can be obtained based on these drawings without creative work.

[0026] FIG1 is a schematic diagram of a sample holder structure of a transmission electron microscope according to some embodiments.

[0027] FIG2 is a cross-sectional view of a transmission electron microscope sample holder according to some embodiments.

[0028] FIG3 is a partial enlarged view of point A in FIG2 .

[0029] FIG. 4 is a schematic structural diagram of a mounting frame in a transmission electron microscope sample holder according to some embodiments.

[0030] 5 is a top view of a mounting frame in a transmission electron microscope sample holder according to some embodiments.

[0031] 6 is a bottom view of a mounting frame in a transmission electron microscope sample holder according to some embodiments.

[0032] FIG. 7 is a schematic structural diagram of a base body in a transmission electron microscope sample holder according to some embodiments.

[0033] FIG8 is a schematic diagram of the structure of a heater in a transmission electron microscope sample holder according to some embodiments.

[0034] Reference numerals: 100, TEM sample rod; 101, rod body; 1011, groove; 10, heating element; 11, notch; 12, through hole; 20, testing mechanism; 21, connecting arm; 211, flexible hinge; 22, fixing portion; 23, accommodating space; 201, input end; 202, output end; 203, stage; 300, driving element; 30, piezoelectric driver; 40, thermal insulation element; 50, mounting frame Frame; 51, mounting groove; 52, connecting part; 521, positioning hole; 53, limiting groove; 54, guide hole; 60, mounting seat; 61, seat body; 611, positioning protrusion; 612, boss; 613, assembly platform; 614, assembly protrusion; 615, line groove; 62, cover body; 700, temperature measuring component; 70, optical fiber; 701, detection end; 81, first cover plate; 82, second cover plate; 90, electrical connector. DETAILED DESCRIPTION

[0035] To make the above-mentioned objects, features, and advantages of the present application more clearly understood, the specific embodiments of the present application are described in detail below with reference to the accompanying drawings. The following description sets forth many specific details to facilitate a full understanding of the present application. However, the present application can be implemented in many other ways than those described herein, and those skilled in the art can make similar improvements without violating the scope of the present application. Therefore, the present application is not limited to the specific embodiments disclosed below.

[0036] It should be noted that when a component is referred to as being "fixed to" or "disposed on" another component, it may be directly on the other component or there may be a central component. When a component is considered to be "connected to" another component, it may be directly connected to the other component or there may be a central component at the same time. The terms "vertical", "horizontal", "upper", "lower", "left", "right" and similar expressions used in the specification of this application are for illustrative purposes only and do not represent the only implementation method.

[0037] Furthermore, the terms "first" and "second" are used for descriptive purposes only and should not be construed as indicating or implying relative importance or implicitly specifying the number of the technical features being referred to. Thus, a feature defined as "first" or "second" may explicitly or implicitly include at least one of such features. Throughout the description of this application, "plurality" means at least two, for example, two, three, etc., unless otherwise specifically defined.

[0038] In this application, unless otherwise expressly specified or limited, when a first feature is "above" or "below" a second feature, it can mean that the first feature is directly in contact with the second feature, or the first feature and the second feature are indirectly in contact through an intermediary. Furthermore, when a first feature is "above," "above," or "above" a second feature, it can mean that the first feature is directly above or diagonally above the second feature, or simply means that the first feature is higher in level than the second feature. When a first feature is "below," "below," or "below" a second feature, it can mean that the first feature is directly below or diagonally below the second feature, or simply means that the first feature is lower in level than the second feature.

[0039] Unless otherwise defined, all technical and scientific terms used in the specification of this application have the same meaning as commonly understood by those skilled in the art to which this application belongs. The terms used in the specification of this application are only for the purpose of describing specific embodiments and are not intended to limit this application. The term "and / or" used in the specification of this application includes any and all combinations of one or more of the relevant listed items.

[0040] Please refer to Figures 1 to 8. The present application provides a transmission electron microscope sample holder 100, which includes a heating element 10 and a testing mechanism 20; the heating element 10 is used to heat the sample; the testing mechanism 20 is constructed with a plurality of connecting arms 21 arranged at intervals along the circumference of the testing mechanism 20, and the plurality of connecting arms 21 are arranged to form an accommodating space 23. The side of each connecting arm 21 facing the accommodating space 23 is defined as an output end 202, and the plurality of output ends 202 jointly clamp the sample, and each connecting arm 21 can be extended and retracted along the extension direction of the output end 202; each connecting arm 21 is connected to the heating element 10.

[0041] In this way, multiple connecting arms 21 jointly clamp the sample to achieve sample fixation, which is conducive to performing mechanical loading experiments on the sample. For example, the output end 202 of each connecting arm 21 is constructed with a stage 203. The sample is placed on the stage 203, and then a first locking member is passed through the sample and the stage 203. The first locking member and the stage 203 can be connected by a thread to achieve locking. During the mechanical loading experiment, the heating element 10 can provide heat to the sample. The end of the connecting arm 21 away from the accommodating space 23 is defined as the input end 201. The input end 201 of the connecting arm 21 contacts the heating element 10 and can transfer heat from the heating element 10 to the output end 202, and then from the output end 202 to the sample, so that the sample is in a high-temperature environment. In a specific embodiment, the heating element 10 can be configured as a heating plate to increase the contact area with the connecting arm 21. The heating plate can be made of a heating film or a heating ceramic plate; the connecting arm 21 can be made of a copper alloy with a high thermal conductivity coefficient to achieve efficient heat conduction. Furthermore, multiple connecting arms can collectively secure the sample. Each of the multiple connecting arms 21 can extend and retract along the extension direction of the output end 202 to exert tensile or compressive forces on the sample, achieving a dual-purpose effect. Because the multiple connecting arms 21 are distributed in different directions, different tensile or compressive forces can be exerted on the same sample in different directions. This allows for the analysis of microstructural changes in the sample under high temperature and complex stresses, enabling real-time characterization of the material's microstructural evolution under complex stresses and providing a more accurate and reliable scientific basis for the sample's service performance.

[0042] For ease of explanation, the embodiment of the present application installs the connecting arm 21 and the heating plate through the mounting frame 50, and regards the outline of the mounting frame 50 as a rectangular parallelepiped, defines the length direction of the rod body 101 of the transmission electron microscope sample rod 100 and the length direction of the mounting frame 50 as the second direction, and takes the second direction as the x-axis, defines the width direction of the mounting frame 50 as the first direction, and takes the first direction as the y-axis, and defines the thickness direction of the mounting frame 50 as the third direction, and takes the third direction as the z-axis.

[0043] As shown in Figures 4 and 5, in a further embodiment, the testing mechanism 20 is provided with connecting arms 21 on both sides along the first direction and on both sides along the second direction, respectively. The transmission electron microscope sample holder 100 includes multiple spaced apart drive members 300, each connected to an input end 201; the first and second directions are arranged at an angle. In this way, the drive members 300 provide a power source for the extension and retraction of the connecting arms 21. Specifically, the drive members 300 transmit power to the input end 201 of the connecting arm 21, which is then transmitted from the input end 201 of the connecting arm 21 to the output end 202 of the connecting arm 21, thereby stretching or compressing the sample. Simultaneously, the connecting arms 21 are provided on both sides of the first direction and on both sides of the second direction, respectively, to enable stretching or compressing the sample in the first and second directions, facilitating various biaxial mechanical loading tests on the sample.

[0044] As shown in Figures 4 and 5, in an optional embodiment, the driving member 300 is configured as a piezoelectric driver 30, and the connecting arm 21 is configured as a flexible hinge 211. The input end 201 and the output end 202 of each flexible hinge 211 are arranged at an angle, and the input end 201 is attached to the piezoelectric driver 30. In this way, the piezoelectric driver 30 can produce different deformations depending on the input voltage. Configuring the connecting arm 21 as a flexible hinge 211 can amplify the deformation of the piezoelectric driver 30 and transmit it to the sample, thereby achieving tension and compression of the sample.

[0045] As shown in Figures 4 and 5, in a further embodiment, the testing mechanism 20 further includes a fixing portion 22. Along the circumference of the testing mechanism 20, a fixing portion 22 is connected between the input ends 201 of any two adjacent flexible hinges 211. The fixing portion 22 is connected to the heating element 10. In this way, the flexible hinge 211 can be fixed on both sides along the extension direction of the input end 201 by the fixing portion 22, preventing the flexible hinge 211 from shifting when transmitting deformation, thereby ensuring the accuracy of the force applied to the sample. At the same time, heat from the heating element 10 can be transferred to the input end 201 through the fixing portion 22, and then from the input end 201 to the output end 202.

[0046] As shown in Figures 4 and 5 , in a specific embodiment, each flexible hinge 211 is a hollow "T"-shaped structure with an axis of symmetry. The output end 202 extends in a direction aligned with the axis of symmetry of the T-shaped structure, while the input end 201 extends perpendicularly or nearly perpendicularly to the axis of symmetry of the T-shaped structure. This allows the input end 201 to have a larger area for connection with the piezoelectric actuator 30, allowing the flexible hinge 211 to amplify micro-deformations of the piezoelectric actuator 30.

[0047] As shown in Figures 4 and 5, in an optional embodiment, the transmission electron microscope sample rod 100 further includes a thermal insulation member 40, which is connected between the piezoelectric driver 30 and the input end 201 of the flexible hinge 211. In this way, the heat of the heating element 10 can be isolated to a certain extent, reducing the outward diffusion of heat from the heating element 10, which is beneficial to reducing heat loss and improving the heating efficiency of the heating element 10. At the same time, it can also reduce the heat transfer to the piezoelectric driver 30, avoiding the heat from affecting the piezoelectric driver 30, and facilitating the normal operation of the piezoelectric driver 30. Specifically, the thermal insulation member 40 is configured as a thermal insulation sheet, which is attached between the piezoelectric driver 30 and the flexible hinge 211. At the same time, the thermal insulation sheet can be made of a high-temperature resistant ceramic material.

[0048] As shown in Figures 5 and 8 , in a further embodiment, the heating element 10 is provided with a plurality of spaced-apart notches 11, and the piezoelectric driver 30 and the thermal insulation member 40 are mounted in the notches 11. Thus, the notches are arranged so that the heating element is positioned away from the piezoelectric driver and the thermal insulation member. Preventing contact between the heating element 10 and the piezoelectric driver 30 can reduce the impact of the heating element 10 on the piezoelectric driver 30, further facilitating the normal operation of the piezoelectric driver 30.

[0049] Next, the installation structure involved in assembling the testing mechanism 20 and the driving member 300 will be described.

[0050] As shown in Figures 4 and 5, in an optional embodiment, the mounting frame 50 is provided with a mounting slot 51. The heater 10 is mounted at the bottom of the mounting slot 51, and the flexible hinge 211 is located on the side of the heater 10 facing away from the bottom of the mounting slot 51. Thus, the mounting frame 50 facilitates the integrated installation of components such as the driver 300, the heater 10, and the testing mechanism 20. The mounting slot 51 facilitates assembly and positioning, and can limit the position of the heater 10, the driver 300, and the flexible hinge 211, thereby ensuring stable installation.

[0051] As shown in Figures 1 to 5 , in a further embodiment, the mounting frame 50 is configured with a connecting portion 52 spaced apart from the mounting slot 51. The TEM sample holder 100 also includes a mounting base 60 and a rod body 101, with the mounting base 60 connected between the rod body 101 and the connecting portion 52. This arrangement allows the mounting frame 50 to be connected to the mounting base 60 via the connecting portion 52. The connection between the mounting base 60 and the rod body 101 further establishes the connection between the mounting frame 50 and the rod body 101, with the mounting base 60 providing support for the mounting frame 50. Specifically, the rod body 101 can be made of aluminum alloy to reduce weight.

[0052] As shown in Figures 3, 5, and 7, in a further embodiment, the mounting base 60 includes a base 61 and a cover 62. One of the base 61 and the connecting portion 52 is configured with a positioning protrusion 611, and the other is configured with a positioning hole 521. The positioning protrusion 611 is inserted into the positioning hole 521. The cover 62 is pressed against the connecting portion 52 and connected to the base 61. It will be understood that the base 61 can support the mounting frame 50. The provision of the positioning protrusion 611 and the positioning hole 521 facilitates the positioning of the connecting portion 52 during assembly and the limiting of the position of the connecting portion 52 after assembly. The provision of the cover 62 facilitates the fixing of the connecting portion 52 between the base 61 and the cover 62, thereby achieving the assembly of the mounting frame 50 and the mounting base 60. In this way, the hole wall of the positioning hole 521 can produce a limiting effect on the positioning protrusion 611 along the radial direction of the positioning hole 521, which is beneficial to the positioning of the mounting frame 50. By pressing the cover body 62 onto the connecting portion 52, a limiting effect is produced on the connecting portion 52 along the axial direction of the positioning hole 521, and then the connecting portion 52 is fixed between the cover body 62 and the base body 61, thereby achieving the fixation of the mounting frame 50. Exemplarily, the base body 61 is constructed with a positioning protrusion 611, and the connecting portion 52 is constructed with a positioning hole 521. Of course, the connecting portion 52 can also be constructed with a positioning protrusion 611, and the base body 61 is constructed with a positioning hole 521. In addition, the base body 61 can be made of ceramic material to facilitate heat insulation, promote the heating of the sample, and also facilitate line laying.

[0053] As shown in Figures 3 and 7, in a specific embodiment, the seat 61 is partially inserted into the rod 101. The inner wall of the rod 101 is formed with an annular groove 1011. The seat 61 is correspondingly formed with a boss 612. The boss 612 extends into the groove 1011 to limit the position of the seat 61. Furthermore, a nut is provided between the seat 61 and the rod 101. The nut can be threadedly engaged with the rod 101 to secure the seat 61 within the rod 101. The portion of the seat 61 extending outside the rod 101 is formed with an assembly platform 613 and an assembly protrusion 614. There is space between the assembly platform 613 and the assembly protrusion 614 for placing the connecting portion 52. The positioning protrusion 611 is provided on the assembly platform 613. The cover 62 presses the connecting portion 52 against the assembly platform 613 and is connected to the seat 61 via the assembly protrusion 614. More specifically, the second locking member passes through the cover body 62 and the assembly protrusion 614 , and is threadedly connected to the cover body 62 and the assembly protrusion 614 respectively, thereby achieving locking of the cover body 62 and the base body 61 .

[0054] In an optional embodiment, the TEM sample holder 100 further includes a temperature measuring element 700. A detection end 701 of the temperature measuring element 700 extends into the accommodating space 23 to accurately obtain the sample temperature during testing, monitor the sample temperature in real time, and ensure that the sample temperature remains stable during testing. It will be appreciated that the temperature measuring element 700 is configured to detect sample temperature data in real time, thereby enabling timely adjustment of the sample's test temperature.

[0055] As shown in Figures 2 and 6, in a specific embodiment, the temperature measuring element 700 includes an optical fiber 70. The mounting frame 50 is provided with a limiting groove 53 and a guide hole 54 connected to the limiting groove 53. The optical fiber 70 extends into the limiting groove 53 and passes through the guide hole 54. Along the third direction, the heating element 10 is provided with a through hole 12 directly opposite the accommodating space 23. The optical fiber 70 passes through the through hole 12, with the end of the optical fiber 70 facing the accommodating space 23. In this way, the provision of the limiting groove 53 and the guide hole 54 facilitates the positioning of the optical fiber 70. The limiting groove 53 can limit the optical fiber 70 so that the optical fiber 70 is arranged along a predetermined path. The provision of the guide hole 54 facilitates guiding the optical fiber 70 to the accommodating space 23 where the sample is located. The heating element 10 is provided with the through hole 12 to facilitate the passage of the optical fiber 70, thereby allowing the end of the optical fiber to face the sample, ensuring that the detection position of the optical fiber 70 is accurate, thereby achieving precise detection.

[0056] Furthermore, the end of the optical fiber 70 away from the sample is connected to a spectrometer. After calibrating the input signal of the spectrometer and fitting the blackbody radiation curve and the blackbody radiation formula, the temperature of the sample can be obtained, so as to facilitate real-time temperature detection of the sample.

[0057] As shown in FIG2 , in a specific embodiment, the transmission electron microscope sample holder 100 further includes a first cover plate 81 . The rod body 101 is hollow along its own axial direction. The first cover plate 81 is sealed on the side of the rod body 101 away from the mounting frame 50 along its own axial direction. The optical fiber 70 passes through the first cover plate 81 and the rod body 101 along the axial direction of the rod body 101, thereby achieving the assembly of the optical fiber 70.

[0058] More specifically, a seal is provided between the first cover plate 81 and the rod body 101 to ensure a tight connection. A fiber optic connector is also connected to the first cover plate 81. The optical fiber 70 is routed through the rod body 101 and connected to an external spectrometer via the connector. The connector is sealed to the first cover plate 81 and the optical fiber 70 to the connector using high-vacuum adhesive to maintain the vacuum environment within the rod body 101.

[0059] As shown in FIG2 , in some embodiments, a mounting hole is defined in the sidewall of the rod body 101. The TEM sample holder 100 further includes an electrical connector 90 and a second cover plate 82. The electrical connector 90 is mounted in the mounting hole and passes through the second cover plate 82. The second cover plate 82 is pressed against the electrical connector 90 and the sidewall of the rod body 101. The piezoelectric driver 30 and the heater 10 are each electrically connected to the electrical connector 90. In this manner, both the piezoelectric driver 30 and the heater 10 can be electrically connected to an external source via the electrical connector 90, achieving electrical conduction. Specifically, the provision of the second cover plate 82 facilitates positioning of the electrical connector 90, and a seal is provided between the second cover plate 82 and the rod body 101 to achieve a seal.

[0060] In a specific embodiment, a terminal is further provided at the bottom of the mounting groove 51 of the mounting frame 50, and the terminal is located at the notch 11 of the heating plate, and each piezoelectric driver 30 has a lead connected to the terminal. At the same time, the mounting frame 50 is also installed with a wiring circuit, and the lead is connected to the wiring circuit through the terminal. Furthermore, the mounting frame 50 is also connected to an electrode at the connection portion 52, and the electrode is connected to the wiring circuit. The cover body 62 is installed with an electrode contact pin, and the cover body 62 can achieve close contact between the electrode contact pin and the electrode while pressing the connection portion 52. The electrode contact pin is connected to the electrical connector 90 through a wire. Among them, the ground lead of the piezoelectric driver 30 is directly connected to the electrical connector 90 through a wire. In this way, the conduction of current is achieved, so that different voltages can be input to control the piezoelectric driver 30. Specifically, the cover body 62 can be made of polyetheretherketone material to ensure the insulation of the electrode connection. 7 , the portion of the base 61 within the rod 101 is configured with a line groove 615 , so that the line connected to the electrode contact pin enters the hollow rod 101 and connects to the electrical connector 90 , thereby protecting the line.

[0061] The present application also provides a sample testing method, applicable to the transmission electron microscope sample holder 100 described above. The sample testing method includes: a plurality of connecting arms 21 jointly clamping a sample; heating the sample to a first temperature; and extending or retracting each connecting arm 21 along the extension direction of the output end 202. In this manner, the connecting arms 21 can provide support for the sample and apply a compressive or tensile force to the sample. The force applied to the sample by the multiple connecting arms 21 and the extension or retraction of the multiple connecting arms 21 produce tension or compression in different directions on the sample, thereby simulating the microstructural evolution of the sample under high temperature and complex stress conditions.

[0062] In some embodiments, the extension or contraction of each connecting arm 21 along the extension direction of the output end 202 includes: applying a positive voltage or a negative voltage to the piezoelectric actuator 30 in the transmission electron microscope sample holder 100; the piezoelectric actuator 30 deforms positively in response to the positive voltage or negatively in response to the negative voltage; and the connecting arm 21 amplifies the deformation of the piezoelectric actuator 30 and transmits the amplified deformation to the sample. Thus, by applying a voltage to the piezoelectric actuator 30, the piezoelectric actuator 30 deforms, and the deformation of the piezoelectric actuator 30 is amplified by the connecting arm 21, thereby facilitating the stretching or compression of the sample.

[0063] In some embodiments, applying a positive or negative voltage to the piezoelectric actuator 30 of the transmission electron microscope sample holder 100 includes: applying a positive voltage to one of the piezoelectric actuators 30 located on opposite sides of the test mechanism 20 along a first direction, and applying a negative voltage to the other; and / or applying a positive voltage to one of the piezoelectric actuators 30 located on opposite sides of the test mechanism 20 along a second direction, and applying a negative voltage to the other. In this manner, different voltages can be applied to the piezoelectric actuator 30 to meet different experimental conditions, thereby causing the piezoelectric actuator 30 to deform accordingly. It is understood that applying opposite voltages to the piezoelectric actuators 30 on opposite sides of the first or second direction can meet the requirements of high-temperature biaxial mechanical loading experiments.

[0064] In some embodiments, the piezoelectric driver 30 undergoes positive deformation according to a positive voltage or negative deformation according to a negative voltage, including: as shown in Figure 5, when a positive voltage is applied to one of the piezoelectric drivers 30 located on both sides of the testing mechanism 20 along the first direction and a negative voltage is applied to the other, the piezoelectric drivers 30 on both sides produce relative or opposite deformations along the first direction. For example, along the first direction, a positive voltage is applied to the piezoelectric driver 30 close to the negative direction of the y-axis, and the piezoelectric driver 30 deforms toward the positive direction of the y-axis; a negative voltage is applied to the piezoelectric driver 30 away from the negative direction of the y-axis, and the piezoelectric driver 30 deforms toward the negative direction of the y-axis. The piezoelectric drivers 30 on both sides are relatively deformed. Conversely, along the first direction, a negative voltage is applied to the piezoelectric driver 30 close to the negative direction of the y-axis, and the piezoelectric driver 30 deforms toward the negative direction of the y-axis; a positive voltage is applied to the piezoelectric driver 30 away from the negative direction of the y-axis, and the piezoelectric driver 30 deforms toward the positive direction of the y-axis. The piezoelectric drivers 30 on both sides are deformed opposite to each other. When a positive voltage is applied to one of the piezoelectric drivers 30 located on both sides of the testing mechanism 20 along the second direction and a negative voltage is applied to the other, the piezoelectric drivers 30 on both sides will produce relative or opposite deformations along the second direction. For details, please refer to the voltage settings of the piezoelectric drivers 30 on both sides of the first direction, which will not be repeated here.

[0065] It can be understood that the corresponding deformation generated by the piezoelectric actuator 30 in response to the voltage signal causes the sample to be stretched or compressed on both sides along the first or second direction. In other words, by applying opposite voltages to the piezoelectric actuators 30 on both sides of the first and second directions, the piezoelectric actuators 30 on both sides of the first direction deform toward or away from each other, and the piezoelectric actuators 30 on both sides of the second direction deform toward or away from each other. By combining these two methods of applying voltages to the piezoelectric actuators 30, different deformation modes can be achieved to meet the requirements of high-temperature biaxial mechanical loading experiments.

[0066] The sample is stretched or compressed accordingly to the combined deformation of different piezoelectric actuators 30. Specifically, when the piezoelectric actuators 30 on either side of the testing mechanism 20 along a first direction deform relative to each other in the first direction, the sample is compressed in the first direction. When the piezoelectric actuators 30 on either side of the testing mechanism 20 along the first direction deform in opposite directions in the first direction, the sample is stretched in the first direction. When the piezoelectric actuators 30 on either side of the testing mechanism 20 along a second direction deform relative to each other in the second direction, the sample is compressed in the second direction. When the piezoelectric actuators 30 on either side of the testing mechanism 20 along the second direction deform in opposite directions in the second direction, the sample is stretched in the second direction.

[0067] As shown in Figure 5, in actual use, the deformation of the piezoelectric actuator 30 is often used to implement different mechanical loading experiments. In some embodiments, a high-temperature biaxial compression test is performed on a sample: the temperature of the sample is first maintained at a first temperature, that is, a preset temperature. Then, along the first direction, a positive voltage is applied to the piezoelectric driver 30 close to the negative direction of the y-axis, and the piezoelectric driver 30 deforms toward the positive direction of the y-axis. A negative voltage is applied to the piezoelectric driver 30 away from the negative direction of the y-axis, and the piezoelectric driver 30 deforms toward the negative direction of the y-axis, so that the piezoelectric drivers 30 on both sides are relatively deformed. After amplification, the deformation is transferred to the sample, and the sample is subjected to relative forces along the first direction, thereby achieving synchronous compression of the sample on both sides along the first direction; further, along the second direction, a positive voltage is applied to the piezoelectric driver 30 close to the negative direction of the x-axis, and the piezoelectric driver 30 deforms toward the positive direction of the x-axis. A negative voltage is applied to the piezoelectric driver 30 away from the negative direction of the x-axis, and the piezoelectric driver 30 deforms toward the negative direction of the x-axis, so that the piezoelectric drivers 30 on both sides are relatively deformed. After amplification, the deformation is transferred to the sample, and the sample is subjected to relative forces along the second direction, thereby achieving synchronous compression of the sample on both sides along the second direction.

[0068] In other embodiments, the sample can also be subjected to high-temperature biaxial tension tests, high-temperature x-axis tension and y-axis compression tests, and high-temperature x-axis compression and y-axis tension tests. All of these can refer to the high-temperature biaxial compression test embodiment, differing only in the voltages applied to the piezoelectric actuator 30 in different directions. In each of the above experiments, maintaining a constant voltage across the piezoelectric actuator 30 on the four sides allows for creep testing under the corresponding experiment, such as the high-temperature biaxial compression creep test.

[0069] Based on the high-temperature biaxial compression test, when the voltage reaches a certain value, the voltage of the piezoelectric actuators 30 on these four sides is simultaneously reduced. At this time, the deformation of the corresponding piezoelectric actuators 30 continues to decrease until they return to their original position. Furthermore, by applying the reverse voltage to the piezoelectric actuators 30 on these four sides, the corresponding biaxial compression is transformed into biaxial tension. This cycle is repeated to complete the biaxial fatigue loading test under high-temperature conditions.

[0070] The technical features of the above-mentioned embodiments can be combined arbitrarily. In order to make the description concise, not all possible combinations of the technical features in the above-mentioned embodiments are described. However, as long as there is no contradiction in the combination of these technical features, they should be considered to be within the scope of this specification.

[0071] The above-described embodiments merely represent several implementation methods of the present application. While the descriptions are relatively specific and detailed, they should not be construed as limiting the scope of the patent application. It should be noted that a person of ordinary skill in the art may make various modifications and improvements without departing from the spirit of the present application, all of which fall within the scope of protection of the present application. Therefore, the scope of patent protection for the present application shall be determined by the appended claims.

Claims

1. A transmission electron microscope sample holder, characterized in that: The transmission electron microscope sample holder comprises: A heating element, used for heating the sample; The testing mechanism is constructed with a plurality of connecting arms arranged at intervals along the circumference of the testing mechanism, the plurality of connecting arms are arranged to form a containing space, a side of each connecting arm facing the containing space is defined as an output end, the plurality of output ends jointly clamp the sample, and each connecting arm can be extended and retracted along the extension direction of the output end; each connecting arm is connected to the heating element.

2. The transmission electron microscope sample holder according to claim 1, wherein: The testing mechanism is provided with connecting arms on both sides along the first direction and on both sides along the second direction, respectively; the transmission electron microscope sample rod comprises a plurality of driving members arranged at intervals; an end of the connecting arm away from the accommodating space is defined as an input end, and each of the driving members is connected to the input end; wherein the first direction and the second direction are arranged at an angle.

3. The transmission electron microscope sample holder according to claim 2, wherein: The driving member is configured as a piezoelectric driver, the connecting arm is configured as a flexible hinge, the input end and the output end of each flexible hinge are configured at an angle, and the input end is attached to the piezoelectric driver.

4. The transmission electron microscope sample holder according to claim 3, wherein: The testing mechanism further comprises a fixing portion, and along the circumference of the testing mechanism, the fixing portion is connected between the input ends of any two adjacent flexible hinges, and the fixing portion is connected to the heating element.

5. The transmission electron microscope sample holder according to claim 3, wherein: The transmission electron microscope sample holder also includes a heat insulating member connected between the piezoelectric driver and an input end of the flexible hinge.

6. The transmission electron microscope sample holder according to claim 5, wherein: The heating element is provided with a plurality of gaps arranged at intervals, and the piezoelectric driver and the heat insulating element are installed at the gaps.

7. The transmission electron microscope sample holder according to claim 3, wherein: The transmission electron microscope sample holder also includes a mounting frame, which is provided with a mounting groove. The heating element is mounted at the bottom of the mounting groove, and the flexible hinge is located on a side of the heating element away from the bottom of the mounting groove.

8. The transmission electron microscope sample holder according to claim 7, wherein: The mounting frame is structured with a connecting portion, and the connecting portion is spaced apart from the mounting groove; the transmission electron microscope sample rod also includes a mounting seat and a rod body, and the mounting seat is connected between the rod body and the connecting portion.

9. The transmission electron microscope sample holder according to claim 8, wherein: The mounting seat includes a seat body and a cover body, one of the seat body and the connecting portion is configured with a positioning protrusion, and the other is configured with a positioning hole, the positioning protrusion is passed through the positioning hole, and the cover body is pressed on the connecting portion and connected to the seat body.

10. The transmission electron microscope sample holder according to claim 7, wherein: The transmission electron microscope sample holder also includes a temperature measuring component, and a detection end of the temperature measuring component extends into the accommodating space.

11. The transmission electron microscope sample holder according to claim 10, wherein: The temperature measuring element includes an optical fiber, the mounting frame is provided with a limiting groove and a guide hole connected to the limiting groove, and the optical fiber extends into the limiting groove and passes through the guide hole; Along the third direction, the heating element is provided with a through hole directly facing the accommodating space, the optical fiber passes through the through hole, and the end of the optical fiber faces the accommodating space.

12. A sample testing method, characterized in that: A transmission electron microscope sample holder as claimed in any one of claims 1 to 11; The sample testing method includes: Multiple connecting arms jointly clamp the sample; heating the sample to a first temperature; Each of the connecting arms extends or contracts along the extension direction of the output end.

13. The sample testing method according to claim 12, wherein: Each of the connecting arms extending or contracting along the extension direction of the output end includes: Applying a positive voltage or a negative voltage to the piezoelectric actuator in the transmission electron microscope sample holder; The piezoelectric driver is positively deformed according to the positive voltage or negatively deformed according to the negative voltage; The connecting arm amplifies the deformation of the piezoelectric driver and transmits the amplified deformation to the sample.

14. The sample testing method according to claim 13, wherein: The applying a positive voltage or a negative voltage to the piezoelectric driver of the transmission electron microscope sample holder comprises: Applying the positive voltage to one of the piezoelectric drivers located on both sides of the test mechanism along the first direction, and applying the negative voltage to the other piezoelectric driver; and / or, The positive voltage is applied to one of the piezoelectric drivers located at two sides of the test mechanism along the second direction, and the negative voltage is applied to the other piezoelectric driver.

15. The sample testing method according to claim 14, wherein: The piezoelectric driver positively deforms according to the positive voltage or negatively deforms according to the negative voltage, including: When a positive voltage is applied to one of the piezoelectric drivers located on both sides of the test mechanism along the first direction and a negative voltage is applied to the other one, the piezoelectric drivers on the two sides deform relative to each other or deform in opposite directions along the first direction; A forward voltage is applied to one of the piezoelectric actuators located on both sides of the test mechanism along the second direction, and a forward voltage is applied to the other piezoelectric actuator When a negative voltage is applied, the piezoelectric drivers on both sides deform relative to or opposite to each other along the second direction; The connecting arm amplifies the deformation of the piezoelectric driver and transmits the amplified deformation to the sample, including: When the piezoelectric drivers located at two sides of the testing mechanism along the first direction are relatively deformed along the first direction respectively, the sample is compressed along the first direction; When the piezoelectric drivers located at two sides of the testing mechanism along the first direction are deformed in opposite directions along the first direction respectively, the sample is stretched along the first direction; When the piezoelectric drivers located at two sides of the testing mechanism along the second direction are relatively deformed along the second direction respectively, the sample is compressed along the second direction; When the piezoelectric drivers located at two sides of the testing mechanism along the second direction are deformed in opposite directions respectively along the second direction, the sample is stretched along the second direction.

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