A heating device for mechanical and thermal coupling of scanning electron microscope

Abstract

The present invention discloses a heating device for mechanical and thermal coupling of a scanning electron microscope, and relates to the field of in-situ heating test technology of a scanning electron microscope, comprising a fixed part, the cross section of the fixed part is a circular ring structure, and a first power terminal is arranged on the inner side wall of the fixed part, and the first power terminal is connected to an external power source; a rotating part is movably sleeved in the fixed part, and the bottom of the rotating part is arranged on the rotating sample stage of the scanning electron microscope; a second power terminal is arranged on the outer side wall of the rotating part, and the second power terminal is in contact with and connected to the first power terminal; a heating part is fixedly arranged in the rotating part and is electrically connected to the second power terminal, and a sample placement device is arranged on the top of the heating part, and the heating part can heat the sample in the sample placement device. The present invention can drive the sample to rotate in real time, so that the state of the material can be dynamically observed at different viewing angles, thereby improving the experimental effect.

Description

Technical Field

[0001] The invention relates to the technical field of in-situ heating testing of a scanning electron microscope, in particular to a heating device for mechanical and thermal coupling of a scanning electron microscope. Background Art

[0002] Micro-nano materials are subjected to repeated mechanical vibrations and thermal cycles in integrated circuit chips and micro-electromechanical systems, and their fatigue behavior directly affects the long-term structural integrity and functional stability of the system. Therefore, in-depth research on the fatigue performance of micro-nano materials under mechanical and thermal coupling will help improve the reliability of the system and extend its service life. In the technical solutions known to the inventors, the high-temperature working conditions of the material are often simulated in a scanning electron microscope, and the microstructural changes of the material are in situ detected and analyzed. However, the heating device under the existing scanning electron microscope can only move in a single direction and cannot drive the material sample to rotate in real time, so that the state of the material cannot be dynamically observed at different viewing angles, which reduces the experimental effect. Summary of the invention

[0003] The purpose of the present invention is to provide a heating device for thermal coupling of a scanning electron microscope to solve the problems existing in the above-mentioned prior art, which can drive the sample to rotate in real time, thereby dynamically observing the state of the material at different viewing angles and improving the experimental effect.

[0004] To achieve the above object, the present invention provides the following solutions:

[0005] The present invention provides a heating device for mechanical and thermal coupling of a scanning electron microscope, comprising:

[0006] A fixing part, wherein the cross section of the fixing part is a circular ring structure, and a first power terminal is provided on the inner side wall of the fixing part, and the first power terminal is connected to an external power source;

[0007] A rotating part, which is movably sleeved in the fixed part, and the bottom of the rotating part is arranged on the rotating sample stage of the scanning electron microscope; a second electrical terminal is arranged on the outer wall of the rotating part, and the second electrical terminal is in contact with and connected to the first electrical terminal;

[0008] The heating part is fixedly arranged in the rotating part and is electrically connected to the second electrical terminal. A sample placement device is arranged on the top of the heating part, and the heating part can heat the sample in the sample placement device.

[0009] Optionally, the fixed part includes at least two arc-shaped metal shells spliced ​​in sequence along the circumferential direction, and the two adjacent metal shells are fixedly connected by a shell connecting flange; the first power terminal ring is arranged on the inner wall of the metal shell; a heating power supply wire is passed through the outer wall of the fixed part, and the first power terminal is externally connected to a power source through the heating power supply wire.

[0010] Optionally, a first temperature measuring electrical terminal is arranged on the inner wall of the fixed part, which is spaced apart from the first electrical terminal and not connected to it; a second temperature measuring electrical terminal is arranged on the outer wall of the rotating part, which is spaced apart from the second electrical terminal and not connected to it; a thermocouple is arranged at the heating part, the working end of the thermocouple is located in the heating part and is connected to the second temperature measuring electrical terminal, a non-working end of the thermocouple is fixedly arranged on the outer wall of the fixed part, one end of the non-working end of the thermocouple is externally connected to a display instrument, and the other end is connected to the first temperature measuring electrical terminal, and the second temperature measuring electrical terminal is in contact with and connected to the first temperature measuring electrical terminal.

[0011] Optionally, the rotating part includes a cylindrical rotating seat, a positioning device is fixedly provided at the bottom of the rotating seat, and the positioning device is connected to the rotating sample stage of the scanning electron microscope; a heat insulation sleeve is fixedly provided at the top of the rotating seat, and the heating part is fixed in the heat insulation sleeve; the second power terminal ring is arranged on the outer side wall of the rotating seat.

[0012] Optionally, the thermal insulation sleeve comprises a rigid ceramic thermal insulation sleeve fixedly mounted on the rotating seat, an inorganic thermal insulation coating layer is disposed on the inner side of the rigid ceramic thermal insulation sleeve, and the heating part is disposed on the inner side of the inorganic thermal insulation coating layer.

[0013] Optionally, the heating part includes a support seat fixed in the rotating part, a heating core column is provided on the support seat, an electric heating wire is surrounded by the outer side of the heating core column, the electric heating wire is electrically connected to the second power terminal, and the sample placement device is provided on the top of the heating core column.

[0014] Optionally, the sample placement device includes a metal shell top cover, a sample port is provided at a center position of the metal shell top cover, a heating boss is provided at the top of the heating core column, and the sample port is located at the position of the heating boss.

[0015] Optionally, a cover edge is arranged at the outer edge of the lower side of the top cover of the metal shell, an electrode interface is opened on the cover edge, the top edge position of the heating core column is arranged on a pedestal, an electrode is arranged on the pedestal, the cover edge is buckled on the pedestal, and the electrode is connected to the electrode interface, the electrode interface is connected to a retractable electrode through a wire, the retractable electrode is located below the sample port, and the retractable electrode is electrically connected to the piezoelectric ceramic sheet in the sample port, and the piezoelectric ceramic sheet is provided with the sample; a first excitation power terminal is arranged on the inner wall of the fixed part, which is spaced apart from the first power terminal and is not connected; a second excitation power terminal is arranged on the outer wall of the rotating part, which is spaced apart from the second power terminal and is not connected, the electrode is connected to the second excitation power terminal, a piezoelectric ceramic excitation power supply wire is passed through the outer wall of the fixed part, one end of the piezoelectric ceramic excitation power supply wire is connected to the first excitation power terminal, and the other end is externally connected to a piezoelectric ceramic excitation power supply.

[0016] Optionally, the sample port is a square sample port or a circular sample port.

[0017] Optionally, the first power terminal and the second power terminal each include a positive terminal and a negative terminal, respectively; the positive terminal and the negative terminal of the first power terminal are both annular concave structures, and the positive terminal and the negative terminal of the second power terminal are both annular convex structures; the second power terminal is movably nested in the first power terminal; the structures of the first temperature measuring power terminal and the first excitation power terminal are the same as those of the first power terminal, and the structures of the second temperature measuring power terminal and the second excitation power terminal are the same as those of the second power terminal.

[0018] Compared with the prior art, the present invention has achieved the following technical effects:

[0019] The present invention adopts a coaxially nested fixed part and a rotating part, the electrode terminal on the inner wall of the fixed part is connected to an external power supply, the rotating part is arranged on the sample stage, and can follow the sample stage to drive the heating device and the sample to rotate, the electrode terminal on the side wall of the rotating part is always in a sliding contact state with the electrode terminal of the fixed part, so that during the relative rotation of the fixed part and the rotating part, the power required by the heating part can be maintained continuously, ensuring the continuity of the heating process; the heating device of the present invention can realize the functions of self-rotation and self-movement under micro-nanoscale, in-situ force-thermal coupling fatigue mechanics experiments, the sample can be carried on the sample port on the top of the heating device, and the evolution of the internal microstructure of the sample during high-cycle fatigue (such as the generation and expansion of cracks) can be dynamically observed from all directions and different viewing angles, thereby more accurately capturing the micro-fracture mechanism. BRIEF DESCRIPTION OF THE DRAWINGS

[0020] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings required for use in the embodiments will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying creative work.

[0021] Figure 1 It is a schematic diagram of the overall structure of the present invention;

[0022] Figure 2 is a schematic diagram of a metal housing of the present invention;

[0023] Figure 3 This is a schematic diagram of the internal structure of the present invention after the metal shell is removed;

[0024] Figure 4 It is a structural schematic diagram of the heating part in the present invention;

[0025] Figure 5 It is a schematic diagram of the structure of the metal housing top cover with a circular sample port in the present invention;

[0026] Figure 6 It is a schematic diagram of the structure of the metal housing top cover with a square sample port in the present invention.

[0027] In the figure: 1-metal shell top cover, 2-metal shell, 3-shell connecting flange, 4-piezoelectric ceramic excitation power supply wire, 5-heating power supply wire, 6-thermocouple, 7-positioning device, 8-positive terminal, 9-negative terminal, 10-heating part, 11-electrode, 12-inorganic thermal insulation coating layer, 13-rigid ceramic thermal insulation sleeve, 14-heating boss, 15-heating core column, 16-electric heating wire, 17-support seat, 18-retractable electrode, 19-electrode interface, 20-circular sample port, 21-square sample port. DETAILED DESCRIPTION

[0028] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0029] The purpose of the present invention is to provide a heating device for thermal coupling of a scanning electron microscope to solve the problems existing in the above-mentioned prior art, which can drive the sample to rotate in real time, thereby dynamically observing the state of the material at different viewing angles and improving the experimental effect.

[0030] In order to make the above-mentioned objects, features and advantages of the present invention more obvious and easy to understand, the present invention is further described in detail below with reference to the accompanying drawings and specific embodiments.

[0031] The present invention provides a heating device for mechanical and thermal coupling of a scanning electron microscope. The scanning electron microscope is a scanning electron microscope, which is a high-resolution microscope that uses an electron beam to scan the surface of a sample and forms an image by detecting the signal generated by the interaction between the electron and the sample. The scanning electron microscope includes a sample stage that can move and rotate. Mechanical and thermal coupling refers to the interaction and influence between mechanical stress and temperature change in a material or structure. This coupling effect is very important in many engineering applications and natural phenomena, especially in the fields of material behavior, thermal stress analysis, thermal deformation, and thermal fatigue under high temperature environments. In a thermal-mechanical coupling experiment under a scanning electron microscope, a device that can heat a sample needs to be placed on the sample stage, and the sample is placed on the heating device to achieve heating of the sample. The heating device needs to use an external power supply with a wire, so the heating device placed on the sample stage can only move in a single direction with the sample stage and cannot rotate. Otherwise, problems such as wire winding may occur, and the state of the material cannot be dynamically observed at different viewing angles.

[0032] refer to Figure 1 to Figure 6 As shown, in order to solve this problem, the structure of the present invention is designed to include a fixed part, a rotating part and a heating part 10, the cross section of the fixed part is a circular ring structure, and a first power terminal is arranged on the inner wall of the fixed part, and the first power terminal is connected to an external power supply through a heating power supply wire 5; the rotating part is movably sleeved in the fixed part, and the bottom of the rotating part is arranged on the rotating sample stage of the scanning electron microscope; a second power terminal is arranged on the outer wall of the rotating part, and the second power terminal is in contact with and connected to the first power terminal; the heating part 10 is fixedly arranged in the rotating part and is electrically connected to the second power terminal, and a sample placement device is arranged on the top of the heating part 10, and the heating part 10 can heat the sample in the sample placement device. Since the heating part 10 is connected to the annular second power terminal, the fixed part is connected to the annular first power terminal, and the first power terminal is externally connected to a power source, when the sample stage drives the heating part 10 and the rotating part to rotate, the second power terminal rotates relative to the first power terminal, and the contact is always maintained during the rotation process to achieve current conduction, and the first power terminal is fixed and does not cause the problem of wire entanglement, thereby achieving the rotation of the sample during the mechanical and thermal coupling experiment.

[0033] Furthermore, in a specific embodiment, the fixed part adopts at least two arc-shaped metal shells 2 spliced ​​in sequence along the circumferential direction to be spliced ​​into a cylindrical structure, and the two adjacent metal shells 2 are fixedly connected by the shell connecting flange 3, thereby forming a complete cylindrical structure; the first power terminal ring is arranged on the inner wall of the metal shell 2; the outer wall of the fixed part is penetrated by the non-working end of the heating power supply wire 5 and the thermocouple 6, the first power terminal is externally connected to the power supply through the heating power supply wire 5, one end of the non-working end of the thermocouple 6 is externally connected to the display, and the other end is connected to the first power terminal, the working end of the thermocouple 6 is arranged in the heating part, the working end of the thermocouple 6 is connected to the second temperature measuring power terminal, and the second temperature measuring power terminal is in contact with the first temperature measuring power terminal, thereby realizing the temperature measurement function of the thermocouple 6. The rotating part of this embodiment includes a cylindrical rotating seat, a positioning device 7 is fixedly provided at the bottom of the rotating seat, and the positioning device 7 is connected to the rotating sample stage of the scanning electron microscope; a rigid ceramic insulation sleeve 13 is fixedly provided at the top of the rotating seat, and an inorganic insulation coating layer 12 is provided on the inner side of the rigid ceramic insulation sleeve 13; the heating part 10 includes a supporting seat 17, a heating core column 15 is provided on the supporting seat 17, and an electric heating wire 16 is surrounded on the outer side of the heating core column 15, and the electric heating wire 16 is electrically connected to the second power terminal; a sample placement device is provided on the top of the heating core column 15, and the heating core column 15 is arranged on the inner side of the inorganic insulation coating layer 12, and the inorganic insulation coating layer 12 has a heat preservation effect; the second power terminal ring is arranged on the outer wall of the rotating seat.

[0034] In order to make the power supply of the heating device conduct more smoothly, the first power terminal and the second power terminal of this embodiment respectively include a positive terminal 8 and a negative terminal 9; the positive terminal 8 and the negative terminal 9 of the first power terminal are both annular concave structures, and the positive terminal 8 and the negative terminal 9 of the second power terminal are both annular convex structures; the second power terminal is movably nested in the first power terminal, and the positive pole is opposite to the positive pole, and the negative pole is opposite to the negative pole, and the two are nested with each other to realize the transmission of current, and the current can still be kept unobstructed when rotating relative to each other.

[0035] In order to improve the heating effect of the sample, a heating boss 14 is provided on the top of the heating core column 15. The sample placement device includes a metal shell top cover 1. A sample port is provided at the center of the metal shell top cover 1. The sample port is located at the upper part of the heating boss 14. The heating core column 15 is heated by the heating wire 16 wrapped around its outside, and then the heat is transferred to the heating boss 14, and the sample is heated by the heating boss 14.

[0036] In order to enable force to be applied to the sample during the thermal coupling experiment, a cover edge is provided at the outer edge of the lower side of the top cover 1 of the metal shell of the present embodiment, and an electrode interface 19 is provided on the cover edge. The top edge of the heating core column 15 is provided on a pedestal, and an electrode 11 is provided on the pedestal. The cover edge is buckled on the pedestal, and the electrode 11 is communicated with the electrode interface 19. The electrode interface 19 is connected with a retractable electrode 18 through a wire. The retractable electrode 18 is located below the sample port, and the retractable electrode 18 is electrically connected to the piezoelectric ceramic sheet in the sample port. The sample is provided on the piezoelectric ceramic sheet, and the retractable electrode 18 is retracted to be in contact with the piezoelectric ceramic sheet of a corresponding shape in the sample port. The positive and negative poles of the ceramic piece are connected to make it vibrate. A first excitation power terminal is arranged on the inner wall of the fixed part, which is spaced from the first power terminal and is not connected. A second excitation power terminal is arranged on the outer wall of the rotating part, which is spaced from the second power terminal and is not connected. The electrode 11 is connected to the second excitation power terminal. A piezoelectric ceramic excitation power supply wire 4 is passed through the outer wall of the fixed part. One end of the piezoelectric ceramic excitation power supply wire 4 is connected to the first excitation power terminal, and the other end is externally connected to the piezoelectric ceramic excitation power supply. It is set separately from the power supply required for heating, and does not interfere with each other. The respective power terminals are spaced apart, and there will be no leakage and interference between each other. Therefore, the present invention can realize the self-rotation of the heating device, changing the original status that it can only move alone. By rotating the piezoelectric ceramic piece, the sample can be carried at any position of the piezoelectric ceramic piece. During the experiment, the evolution of the internal microstructure of the sample during high-cycle fatigue (such as the generation and expansion of cracks) can be dynamically observed in all directions and from different perspectives, so as to more accurately capture the microscopic fracture mechanism.

[0037] like Figure 5 and Figure 6 As shown, in order to make the device of the present invention have a wider range of applications, a replaceable metal shell top cover 1 is designed. Different metal shell top covers 1 have different sample port shapes. By replacing different metal shell top covers 1, a square sample port 21 or a circular sample port 20 can be used for experiments, and then piezoelectric ceramic sheets of different shapes can be selected to study the overall fatigue behavior of the sample and the influence of stress concentration on the fatigue behavior, respectively.

[0038] The present invention uses specific examples to illustrate the principles and implementation methods of the present invention. The above examples are only used to help understand the method and core ideas of the present invention. At the same time, for those skilled in the art, according to the ideas of the present invention, there will be changes in the specific implementation methods and application scope. In summary, the content of this specification should not be understood as limiting the present invention.

Claims

1. A heating device for thermal coupling of a scanning electron microscope, characterized in that: include: A fixing part, wherein the cross section of the fixing part is a circular ring structure, and a first power terminal is provided on the inner side wall of the fixing part, and the first power terminal is connected to an external power source; A rotating part, which is movably sleeved in the fixed part, and the bottom of the rotating part is arranged on the rotating sample stage of the scanning electron microscope; a second electrical terminal is arranged on the outer wall of the rotating part, and the second electrical terminal is in contact with and connected to the first electrical terminal; The heating part is fixedly arranged in the rotating part and is electrically connected to the second power terminal. A sample placement device is provided on the top of the heating part, and the heating part can heat the sample in the sample placement device. The heating part is connected to the annular second power terminal, and the fixed part is connected to the annular first power terminal. When the heating part and the rotating part rotate, the second power terminal rotates relative to the first power terminal, and the contact is always maintained during the rotation process.

2. The heating device for thermal coupling of a scanning electron microscope according to claim 1, characterized in that: The fixing part comprises at least two arc-shaped metal shells spliced ​​in sequence along the circumferential direction, and two adjacent metal shells are fixedly connected by a shell connecting flange; the first power terminal ring is arranged on the inner wall of the metal shell; a heating power supply wire is passed through the outer wall of the fixing part, and the first power terminal is externally connected to a power source through the heating power supply wire.

3. The heating device for thermal coupling of a scanning electron microscope according to claim 1, characterized in that: A first temperature measuring electrical terminal is arranged on the inner wall of the fixed part, which is spaced apart from the first electrical terminal and is not connected; a second temperature measuring electrical terminal is arranged on the outer wall of the rotating part, which is spaced apart from the second electrical terminal and is not connected; a thermocouple is arranged at the heating part, the working end of the thermocouple is located in the heating part and is connected to the second temperature measuring electrical terminal, a non-working end of the thermocouple is fixedly arranged on the outer wall of the fixed part, one end of the non-working end of the thermocouple is externally connected to a display instrument, and the other end is connected to the first temperature measuring electrical terminal, and the second temperature measuring electrical terminal is in contact with and connected to the first temperature measuring electrical terminal.

4. The heating device for thermal coupling of a scanning electron microscope according to claim 1, characterized in that: The rotating part includes a cylindrical rotating seat, a positioning device is fixedly provided at the bottom of the rotating seat, and the positioning device is connected to the rotating sample stage of the scanning electron microscope; a heat insulation sleeve is fixedly provided at the top of the rotating seat, and the heating part is fixedly provided in the heat insulation sleeve; the second power terminal ring is arranged on the outer side wall of the rotating seat.

5. The heating device for thermal coupling of a scanning electron microscope according to claim 4, characterized in that: The heat-insulating sleeve comprises a rigid ceramic heat-insulating sleeve fixedly arranged on the rotating seat, an inorganic heat-insulating coating layer is arranged on the inner side of the rigid ceramic heat-insulating sleeve, and the heating part is arranged on the inner side of the inorganic heat-insulating coating layer.

6. The heating device for thermal coupling of a scanning electron microscope according to claim 3, characterized in that: The heating part includes a support seat fixed in the rotating part, a heating core column is arranged on the support seat, a heating wire is surrounded by the outer side of the heating core column, the thermocouple is arranged in the heating core column, the heating wire is electrically connected to the second power terminal, and the sample placement device is arranged on the top of the heating core column.

7. The heating device for thermal coupling of a scanning electron microscope according to claim 6, characterized in that: The sample placement device comprises a metal shell top cover, a sample port is arranged at the center of the metal shell top cover, a heating boss is arranged at the top of the heating core column, and the sample port is located at the position of the heating boss.

8. The heating device for mechanical and thermal coupling of a scanning electron microscope according to claim 7, characterized in that: A cover edge is arranged at the outer edge of the lower side of the top cover of the metal shell, an electrode interface is opened on the cover edge, the top edge position of the heating core column is arranged on a pedestal, an electrode is arranged on the pedestal, the cover edge is buckled on the pedestal, and the electrode is connected to the electrode interface, the electrode interface is connected with a retractable electrode through a wire, the retractable electrode is located below the sample port, and the retractable electrode is electrically connected to the piezoelectric ceramic sheet in the sample port, and the sample is arranged on the piezoelectric ceramic sheet; a first excitation power terminal is arranged on the inner wall of the fixed part, which is spaced apart from the first power terminal and is not connected; a second excitation power terminal is arranged on the outer wall of the rotating part, which is spaced apart from the second power terminal and is not connected, the electrode is connected to the second excitation power terminal, a piezoelectric ceramic excitation power supply wire is passed through the outer wall of the fixed part, one end of the piezoelectric ceramic excitation power supply wire is connected to the first excitation power terminal, and the other end is externally connected to a piezoelectric ceramic excitation power supply.

9. The heating device for thermal coupling of a scanning electron microscope according to claim 7, characterized in that: The sample port is a square sample port or a circular sample port.

10. The heating device for thermal coupling of a scanning electron microscope according to claim 8, characterized in that: The first power terminal and the second power terminal each include a positive terminal and a negative terminal, respectively; the positive terminal and the negative terminal of the first power terminal are both annular concave structures, and the positive terminal and the negative terminal of the second power terminal are both annular convex structures; the second power terminal is movably nested in the first power terminal; the structures of the first temperature measuring power terminal and the first excitation power terminal are the same as those of the first power terminal, and the structures of the second temperature measuring power terminal and the second excitation power terminal are the same as those of the second power terminal.

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