An in-situ compression device for a transmission electron microscope

Abstract

The present invention provides an in-situ compression device for a transmission electron microscope, comprising: a transmission electron microscope sample rod, a sample rod sample stage and a control system. The input end of the sample rod sample stage is connected to the control system through a power line, and the output end of the sample rod sample stage is connected to the transmission electron microscope sample rod. The transmission electron microscope sample rod is used to place the sample material to be compressed; the sample rod sample stage is used to perform an electrochemical reaction on the sample material placed on the transmission electron microscope sample rod. Through synthesis and preparation, a core-shell structure is formed by coating the sample material to be compressed with a battery negative electrode material. Then, through an electrochemical reaction, ions are controlled to be embedded in the negative electrode material of the coating layer, causing the volume of the coating layer to expand, thereby realizing the inward compression of the coated sample material.

Description

Technical Field

[0001] The present invention relates to the technical field of mechanical properties and microstructure characterization of nanomaterials in transmission electron microscopes, and particularly to an in-situ compression device for a transmission electron microscope. Background Art

[0002] As a fundamental physical parameter, pressure can not only significantly change the structure and various physical and chemical properties of materials, but also manipulate materials to cross traditional physical property interfaces such as insulator-conductor-even superconductor, amorphous-crystalline, ionic bonding-covalent bonding, active-inert, etc. High-pressure technologies represented by diamond anvil techniques have promoted the synthesis of a series of new materials and discovered many special physical and chemical phenomena and properties that do not exist under normal temperature and pressure. Currently, its spatial resolution remains at the micron scale. Exploring the microstructure and properties of materials under high pressure is an inevitable requirement for more comprehensively and deeply understanding the origin and essence of various special physical and chemical phenomena and properties induced by high pressure. Therefore, the development of high-pressure science requires combining macroscopic and microscopic research to comprehensively characterize and deeply analyze the structure and physical properties of materials at multiple scales.

[0003] Microstructure research, especially at the nanometer and atomic scales, cannot do without advanced transmission electron microscopy analysis techniques with high spatial and high energy resolutions. In the past decade or so, with the progress of technologies such as spherical aberration correction and energy filtering, (scanning) transmission electron microscopes have achieved a spatial resolution of 40 pm and an energy resolution of the order of 10 meV. At the same time, by combining new detectors and advanced analysis methods, researchers have realized various in-situ electron microscopy analysis techniques that simulate external environmental conditions (such as temperature, mechanical mechanics, electric field, and atmosphere, etc.) in transmission electron microscopes. As the only powerful research means that can directly image and observe at the nanometer and atomic scales and integrate various spectroscopy analyses, electron microscopes have been widely used in advanced frontier scientific research such as materials, geology, biology, and medicine, leading to major innovations and discoveries in the field of microscopic research.

[0004] However, for a long time, high-pressure generating devices represented by diamond anvil cells, due to their fully enclosed pressure chamber design and the limitation of the thickness of the chamber material (micrometer level), have excluded the possibility of studying high-pressure samples using electron beams with relatively weak penetration ability (~200 nanometers).

[0005] It is extremely challenging to achieve the high-pressure conditions (tens of thousands of times atmospheric pressure or higher) required for experimental observations in the electron microscope vacuum environment. There are relatively few in-situ high-pressure transmission electron microscope experimental studies, and the progress is also relatively slow. Currently, coating or indentation techniques are mainly used to create a local high-pressure environment.

[0006] In 2005-2006, researchers such as Li et al. and Sun et al. from the University of Mainz, Germany successively reported an experimental method for generating high pressure in situ in an electron microscope by using a graphite (Li and F. Banhart, The Deformation of Single, Nanometer-Sized Metal Crystals in Graphitic Shells, Advanced Materials, 2005, 17, 1539-1542.) or carbon nanotube (L. Sun, F. Banhart, A. Krasheninnikov, J. Rodriguez-Manzo, M. Terrones and P. Ajayan, Carbon Nanotubes as High-Pressure Cylinders and Nanoextruders, Science, 2006, 312, 1199-1202. L. Sun, J. Rodriguez-Manzo and F. Banhart, Elastic deformation of nanometer-sized metal crystals in graphitic shells, Applied Physics Letters, 2006, 89, 263104.) cavity to coat nanoparticles. The basic principle of this method is to generate a certain concentration of point defects (carbon vacancies) in the coating layer by using high-energy electron beam irradiation. The coating layer containing point defects undergoes volume shrinkage through structural reorganization at high temperature (500-600 °C), thereby achieving the effect of generating pressure on the cavity nanoparticle sample. Using this method, the research group of Litao Sun from Southeast University in China and Wu and Buseck from Arizona State University in the United States have achieved certain results in the high-temperature and high-pressure research of nanomaterials. However, there are some technical problems that are difficult to overcome in the practical application of this method, including sample size limitation (fine spherical nanoparticles), preparation of uniformly carbon-coated electron microscope samples, experimental temperature range limitation (500-600 °C), poor controllability of pressure intensity, and electron beam irradiation damage. Therefore, it has not been further promoted so far.

[0007] Nanoindentation technology is a widely used transmission electron microscopy experimental method for studying the mechanical properties of materials through in-situ mechanical pressurization. Research institutions such as Xi'an Jiaotong University, Zhejiang University, and Beijing University of Technology in China, as well as Lawrence Berkeley National Laboratory, the University of California, and the Massachusetts Institute of Technology in the United States, have all done a lot of research work on the application and development of nanoindentation technology. However, this experimental method often produces a complex stress state with a local high-pressure stress gradient distribution. In brittle materials (such as inorganic ceramics and glass phases), this local stress distribution will easily cause defect aggregation and ultimately lead to crack generation and stress release.

[0008] All in all, there is currently no mature electron microscopy technology at home and abroad that can achieve in-situ high-pressure research at the microscale. There is an urgent need to intensify the development of a transmission electron microscopy technology method that can achieve in-situ research on the microstructures of materials at the atomic scale under high-pressure environments. Summary of the Invention

[0009] The present invention provides a transmission electron microscopy in-situ compression device with a simple process, which can be used under uniaxial or biaxial tilting conditions, and can realize in-situ or non-in-situ research on pressure-induced microstructures, behaviors, phenomena, and properties of materials at the nano, atomic, and sub-angstrom scales.

[0010] The present invention provides a transmission electron microscopy in-situ compression device, including: a transmission electron microscopy sample rod, a sample rod sample stage, and a control system. The input end of the sample rod sample stage is connected to the control system through a power cord, the output end of the sample rod sample stage is connected to the transmission electron microscopy sample rod, the transmission electron microscopy sample rod is used to place the sample stage, and the transmission electron microscopy sample rod sample stage is used to place the sample material to be compressed and perform an electrochemical reaction on the sample material.

[0011] Preferably, the electrochemical reaction is to control the ion intercalation into the coated anode material, so that the coated anode material compresses inward and coats the sample material to be compressed.

[0012] Preferably, the control system includes: a CPU, an ammeter, an electrochemical test and control unit 5, a control switch, and a power supply. The output end of the CPU is connected to the transmission electron microscopy sample rod, the input end of the CPU is sequentially connected to the ammeter and the electrochemical test and control unit 5, and one end of the electrochemical test and control unit 5 away from the ammeter is connected to the power supply through the control switch.

[0013] Preferably, the transmission electron microscopy sample rod includes a MEMS microelectrical chip structure and a scanning probe control structure; the MEMS microelectrical chip structure is a transmission electron microscopy sample rod with a microelectrical measurement chip made by MEMS technology; the scanning probe control structure is a transmission electron microscopy sample rod with a scanning probe control unit.

[0014] Preferably, the MEMS micro electrical chip structure is arranged on the sample rod loading platform through a transmission electron microscope sample rod and connected to a power supply through a control system; the MEMS micro electrical chip structure includes: a battery negative electrode material, a coated negative electrode material, a battery electrolyte material, a battery positive electrode material, and a first metal electrode material. The coated negative electrode material, the battery electrolyte material, and the battery positive electrode material are connected together in sequence. On one side of the coated negative electrode material away from the battery electrolyte material and on one side of the battery positive electrode material away from the battery electrolyte material, first metal electrode materials are respectively provided. The first metal electrode materials are respectively connected to the positive and negative electrodes of the power supply; the battery negative electrode material is coated inside the coated negative electrode material, and a sample is embedded in the battery negative electrode material.

[0015] Preferably, the scanning probe control structure includes: a battery electrolyte material, a battery positive electrode material, a conductive sample stage, a second metal electrode material, and a driving device. One end of the driving device is connected to a power supply and a control system, and the other end of the driving device is sequentially connected to the second metal electrode material, the battery positive electrode material, and the battery electrolyte material to form a whole. On one side of the battery electrolyte material away from the battery positive electrode material, a conductive sample stage is provided at intervals. On one side of the conductive sample stage away from the battery electrolyte material, a circuit is formed with the control system, the power supply, and the driving device through a power line; on one side of the conductive sample stage close to the battery electrolyte material, a battery negative electrode material is provided, and the battery negative electrode material is used to coat the sample.

[0016] Preferably, the second metal electrode material is a pure metal or alloy material such as a tungsten tip, and the battery positive electrode material and the battery electrolyte material adhere to the tip of the second metal electrode material.

[0017] Preferably, the second metal electrode material is a pure metal or alloy material such as a tungsten tip, and the battery positive electrode material and the battery electrolyte material are deposited on the tip of the second metal electrode material by coating.

[0018] Preferably, the battery electrolyte material is set as a colloidal electrolyte, and the battery positive electrode material and the second metal electrode material are combined into a whole and connected to the colloidal electrolyte.

[0019] The beneficial effects of the present invention are as follows:

[0020] The present invention provides a transmission electron microscope in-situ compression device, including: a transmission electron microscope sample rod, a sample rod loading platform, and a control system. The input end of the sample rod loading platform is connected to the control system through a power line, and the output end of the sample rod loading platform is connected to the transmission electron microscope sample rod. The transmission electron microscope sample rod is used to place the loading platform, and the transmission electron microscope sample rod loading platform is used to place the sample material to be compressed and perform an electrochemical reaction on the sample material.

[0021] The transmission electron microscope compression device of the present invention is provided with a battery positive electrode, an electrolyte, a negative electrode, a sample material to be compressed, a metal electrode, a power supply, an ammeter, a switch, etc. Its principle is based on controlling the volume expansion induced by ion intercalation into the coating material, so as to realize the function of compressing and controlling the coated sample particles.

[0022] This device can conduct in-situ compression experiments on the sample material under the conditions of single-axis tilting or double-axis tilting. At the same time, it can couple environmental variables such as temperature and electric field to realize in-situ or ex-situ research on pressure-induced microstructure, behavior, phenomena, and properties, etc. at the nano, atomic, and sub-angstrom scales. Through techniques such as diffraction and high-resolution imaging of the transmission electron microscope, in-situ dynamic comprehensive characterization of the crystal structure, chemical composition, element valence state, etc. of the sample is carried out. Specifically, first, a core-shell structure is obtained by synthesizing and preparing the sample material to be compressed coated with the battery negative electrode material, and then the ion intercalation into the coated negative electrode material is controlled through an electrochemical reaction, causing the volume expansion of the coating layer, and further realizing the inward compression of the coated sample material.

[0023] The in-situ compression device for transmission electron microscope provided by the present invention can be placed in a micro electrical measurement chip made by MEMS technology, installed in the sample holder of the transmission electron microscope, and comprehensively characterized the crystal structure, chemical composition, element valence state, etc. of the sample in-situ dynamically and with high resolution.

[0024] The in-situ compression device for transmission electron microscope provided by the present invention can also be placed in the sample holder of the transmission electron microscope and equipped with a scanning probe control unit. The single nanostructure is manipulated by the probe, and the crystal structure, chemical composition, element valence state, etc. of the sample are comprehensively characterized in-situ dynamically and with high resolution. The driving mode of the compression experiment can adopt various methods such as piezoelectric ceramics, electromagnetism, and shape memory alloy.

[0025] Taking the compression device placed in the chip as an example: the metal electrode, battery positive electrode material, battery electrolyte material, and battery negative electrode material (coating the sample material to be compressed) form a secondary battery unit. An ultra-thin micro-battery device unit suitable for transmission electron microscope observation is prepared by focused ion beam or other techniques and fixed on the stage of the micro electrical measurement chip of the transmission electron microscope sample holder. The transmission electron microscope sample holder is externally connected to a power supply control and electrochemical cycling test device, etc., to form a complete battery charging circuit. On this basis, by adjusting the ion intercalation amount, the pressure regulation is realized.

[0026] Taking the probe-type compression device as an example: The sample material to be compressed coated with the negative electrode material of the battery is placed on the conductive sample stage, the positive electrode material of the battery and the electrolyte material are respectively placed at the tips of metal electrode materials such as tungsten needle tips, and the metal electrode materials are connected to driving devices such as piezoelectric ceramics. By using driving devices such as piezoelectric ceramics to control the movement of the metal electrode materials until they contact the negative electrode material, the transmission electron microscope sample rod is externally connected to a power supply control and an electrochemical cycling test device, etc., to form a complete battery charging circuit. On this basis, by adjusting the ion insertion amount, the pressure adjustment can be further realized.

[0027] The advantages of the present invention are as follows:

[0028] 1. The principle and process are simple, and the compression function can be realized by using the principle of a simple secondary battery.

[0029] 2. It can perform in-situ compression experiments on the sample material under uniaxial tilting or biaxial tilting conditions, and study the deformation process and microstructure of the material in-situ or ex-situ under high-pressure environments (millions of atmospheres).

[0030] 3. The device can better achieve precise control of pressure, and at the same time can greatly reduce the sample damage problem caused by long-term electron beam irradiation, and effectively solve the problem of high-temperature experimental condition limitations in traditional high-voltage electron microscope methods.

[0031] 4. It can not only be widely applied to the microscopic research of various types of high-pressure materials, expand the high-pressure scientific experimental research from the micron scale to the nano, atomic, and sub-angstrom scales (from the average effect of hundreds or thousands of unit cells to single-atom resolution), but also enable direct experimental observation and research on high-pressure induction and the coupling of high pressure with other mature in-situ environmental electron microscope techniques (such as temperature, atmosphere, and electric field), making it possible to conduct experimental research on high-pressure thermodynamics, kinetics, mechanics, electricity, and environmental science based on the control of two or more environmental variables, and study the microscopic nature of the interface effect, defect behavior, nano-size effect, structural order-disorder, stress field, phase transformation, etc. of materials. At the same time, it is expected to lead to the formation of multiple new research fields and research directions in high-pressure science and the innovative development of related theories.

[0032] Other features and advantages of the present invention will be described in the subsequent specification, and some of them will be obvious from the specification or understood by implementing the present invention. The objectives and other advantages of the present invention can be achieved and obtained through the structures specifically pointed out in the written specification and the drawings.

[0033] The technical solutions of the present invention will be further described in detail below through the drawings and embodiments. Description of the Drawings

[0034] The accompanying drawings are used to provide a further understanding of the present invention and form a part of the specification. They are used together with the embodiments of the present invention to explain the present invention, but do not constitute a limitation to the present invention. In the accompanying drawings:

[0035] Figure 1 Schematic diagram of an in-situ high-pressure sample stage for a transmission electron microscope according to the present invention;

[0036] Figure 2 Schematic diagram of a chip-type high-pressure sample stage for a transmission electron microscope, with the coated negative electrode material being a single layer;

[0037] Figure 3 Schematic diagram of a chip-type high-pressure sample stage for a transmission electron microscope, with the coated negative electrode material being a core-shell structure;

[0038] Figure 4 Schematic diagram of a probe-type high-pressure sample stage for a transmission electron microscope;

[0039] Figure 5 Schematic diagram of another embodiment of a probe-type high-pressure sample stage for a transmission electron microscope;

[0040] Among them, 1 - transmission electron microscope sample rod, 2 - sample rod sample stage, 3 - CPU, 4 - ammeter, 5 - electrochemical test and control unit 5, 6 - power supply, 7 - control switch, 8 - control system, 9 - sample, 10 - battery negative electrode material, 11 - coated layer negative electrode material, 12 - battery electrolyte material, 13 - battery positive electrode material, 14 - first metal electrode material, 15 - conductive sample stage, 16 - second metal electrode material, 17 - driving device. Detailed implementation manners

[0041] The following describes the preferred embodiments of the present invention with reference to the accompanying drawings. It should be understood that the preferred embodiments described herein are only used to illustrate and explain the present invention and are not used to limit the present invention.

[0042] According to Figures 1-5 As shown, an in-situ compression device for a transmission electron microscope provided by an embodiment of the present invention is characterized by including: a transmission electron microscope sample rod 1, a sample rod sample stage 2, and a control system 8. The input end of the sample rod sample stage 2 is connected to the control system 8 through a power supply 6 wire, and the output end of the sample rod sample stage 2 is connected to the transmission electron microscope sample rod 1. The transmission electron microscope sample rod 1 is used to place the sample stage, and the sample rod sample stage 2 is used to place the sample material 9 to be compressed and perform an electrochemical reaction on the sample material 9.

[0043] The electrochemical reaction is to control the ion intercalation into the coated layer negative electrode material 11, so that the coated layer negative electrode material 11 compresses inward and coats the sample material 9 to be compressed.

[0044] The control system 8 includes: a CPU 3, an ammeter 4, an electrochemical test and control unit 5, a control switch 7, and a power supply 6. The output end of the CPU 3 is connected to the TEM sample holder 1. The input end of the CPU 3 is sequentially connected to the ammeter 4 and the electrochemical test and control unit 5. One end of the electrochemical test and control unit 5 away from the ammeter 4 is connected to the power supply 6 through the control switch 7.

[0045] The TEM compression device of the present invention is provided with a battery positive electrode, an electrolyte, a negative electrode, a sample material 9 to be compressed, a metal electrode, a power supply 6, an ammeter 4, a switch, etc. Its principle is based on realizing the function of compression control of the coated sample particles by controlling the volume expansion induced by ion intercalation into the coating material.

[0046] This device can perform in-situ compression experiments on the sample material 9 under uniaxial tilt or biaxial tilt conditions, and can couple environmental variables such as temperature and electric field to realize in-situ or ex-situ research on pressure-induced microstructures, behaviors, phenomena, and properties at the nano, atomic, and sub-angstrom scales. Through techniques such as diffraction and high-resolution imaging of the transmission electron microscope, in-situ dynamic comprehensive characterization of the crystal structure, chemical composition, element valence state, etc. of the sample material 9 is carried out. Specifically, first, a core-shell structure is obtained by synthesizing and preparing the battery negative electrode material 10 to coat the sample material 9 to be compressed, and then the ion intercalation into the coating negative electrode material 11 is controlled through an electrochemical reaction, causing the volume expansion of the coating layer, and further realizing the inward compression of the coated sample material 9.

[0047] The advantages of the present invention are as follows:

[0048] 1. The principle and process are simple, and the compression function can be realized by using the simple secondary battery principle.

[0049] 2. It can perform in-situ compression experiments on the sample material 9 under uniaxial tilt or biaxial tilt conditions, and conduct in-situ or ex-situ research on the deformation process and microstructure of the material under high-pressure environments (millions of atmospheres).

[0050] 3. This device can better achieve precise control of pressure, and at the same time can greatly reduce the damage problem of the sample material 9 caused by long-term electron beam irradiation, and effectively solve the problem of high-temperature experimental condition limitations in traditional high-voltage electron microscope methods.

[0051] 4. It can not only be widely applied to the microscopic research of various types of high-pressure materials, expanding high-pressure scientific experimental research from the micron scale to the nano, atomic, and sub-angstrom scales (from the average effect of hundreds or thousands of unit cells to single-atom resolution), but also enable the direct experimental observation and research of high-pressure induction and the coupling of high pressure with other mature in-situ environmental electron microscopy techniques (such as temperature, atmosphere, and electric field), making it possible to conduct experimental research on high-pressure thermodynamics, kinetics, mechanics, electricity, and environmental science based on the control of two or more environmental variables, and to study the microscopic nature of the interface effect, defect behavior, nano-size effect, structural order-disorder, stress field, phase transformation, etc. of materials. At the same time, it is expected to lead to the formation of multiple new research fields and directions in high-pressure science and the innovative development of related theories.

[0052] In one embodiment, according to Figures 1-5 As shown, the transmission electron microscope sample rod 1 includes a MEMS micro electrical chip structure and a scanning probe control structure; the MEMS micro electrical chip structure is the transmission electron microscope sample rod 1 with a micro electrical measurement chip made by MEMS technology; the scanning probe control structure is the transmission electron microscope sample rod 1 with a scanning probe control unit. The in-situ compression device for transmission electron microscope provided by the present invention can be placed in a micro electrical measurement chip made by MEMS technology, installed in the transmission electron microscope sample rod 1, and comprehensively characterize the crystal structure, chemical composition, element valence state, etc. of the sample material 9 in-situ dynamically and with high resolution.

[0053] The in-situ compression device for transmission electron microscope provided by the present invention can also be placed in the transmission electron microscope sample rod 1 and equipped with a scanning probe control unit, and a single nanostructure can be manipulated by the probe to comprehensively characterize the crystal structure, chemical composition, element valence state, etc. of the sample material 9 in-situ dynamically and with high resolution. The driving mode of the compression experiment can adopt various methods such as piezoelectric ceramics, electromagnetism, and shape memory alloy.

[0054] Taking the compression device placed in the chip as an example: a metal electrode, a battery positive electrode material 13, a battery electrolyte material 12, and a battery negative electrode material 10 (coating the sample material 9 to be compressed) form a secondary battery unit. An ultra-thin micro battery device unit suitable for transmission electron microscope observation is prepared by focused ion beam or other techniques and fixed on the micro electrical measurement chip stage of the transmission electron microscope sample rod 1. The transmission electron microscope sample rod 1 is externally connected to a power supply 6 for control and an electrochemical cycling test device, etc., to form a complete battery charging circuit. On this basis, the pressure can be adjusted by adjusting the ion intercalation amount.

[0055] Taking the probe-type compression device as an example: The sample material 9 to be compressed coated with the negative electrode material 10 of the battery is placed on the conductive sample stage 15. The positive electrode material 13 of the battery and the electrolyte material are respectively placed at the tips of metal electrode materials such as tungsten needle tips. The metal electrode materials are connected to a driving device 17 such as a piezoelectric ceramic. By using the driving device 17 such as a piezoelectric ceramic to control the movement of the metal electrode materials until they contact the negative electrode material, the transmission electron microscope sample rod 1 is externally connected to a power supply 6 for control and an electrochemical cycling test device, etc., to form a complete battery charging circuit. On this basis, by adjusting the ion intercalation amount, the pressure adjustment is further realized.

[0056] In one embodiment, according to Figures 2-3 As shown, the MEMS micro electrical chip structure is arranged on the sample stage 2 of the sample rod through the transmission electron microscope sample rod 1 and is connected to the power supply 6 through the control system 8; the MEMS micro electrical chip structure includes: a battery negative electrode material 10, a coated negative electrode material 11, a battery electrolyte material 12, a battery positive electrode material 13, and a first metal electrode material 14. The coated negative electrode material 11, the battery electrolyte material 12, and the battery positive electrode material 13 are connected together in sequence. On one side of the coated negative electrode material 11 away from the battery electrolyte material 12 and on one side of the battery positive electrode material 13 away from the battery electrolyte material 12, first metal electrode materials 14 are respectively provided. The first metal electrode materials 14 are respectively connected to the positive and negative poles of the power supply 6; the battery negative electrode material 10 is coated inside the coated negative electrode material 11, and the sample material 9 is embedded in the battery negative electrode material 10.

[0057] In the MEMS micro electrical chip structure, the ways of fixing the first metal electrode, the battery positive electrode material 13, the battery electrolyte material 12, and the battery negative electrode material 10 to the chip stage include: fixing them one by one in sequence or fixing them as a whole. The solution can be that the first metal electrode, the battery positive electrode material 13, the battery electrolyte material 12, and the battery negative electrode material 10 (coating the sample material 9 to be compressed) form a secondary battery unit. An ultra-thin micro battery device unit suitable for transmission electron microscope observation is prepared by focused ion beam or other technologies and fixed on the sample stage 2 of the sample rod. Together with the CPU 3, the power supply 6, and the electrochemical test and control unit 5, etc., a complete battery charging circuit is formed. On this basis, by adjusting the ion intercalation amount, the volume of the battery negative electrode material 10 expands, and then the sample material 9 to be compressed coated is compressed. The crystal structure, chemical composition, element valence state, etc. of the sample material 9 are in-situ dynamically comprehensively characterized by technologies such as diffraction and high-resolution imaging of the transmission electron microscope.

[0058] The ways of fixing the first metal electrode material 14, the battery positive electrode material 13, the battery electrolyte material 12, the battery negative electrode material 10, and the sample material 9 to be compressed coated to the chip stage are not limited to the overall secondary battery unit. They can be fixed one by one or fixed as a whole.

[0059] In one embodiment, according to Figures 4-5 as shown, the scanning probe control structure includes: a battery electrolyte material 12, a battery positive electrode material 13, a conductive sample stage 15, a second metal electrode material 16, and a driving device 17. One end of the driving device 17 is connected to a power source 6 and a control system 8, and the other end of the driving device 17 is sequentially connected to the second metal electrode material 16, the battery positive electrode material 13, and the battery electrolyte material 12 to form an integral body. A conductive sample stage 15 is spaced on a side of the battery electrolyte material 12 away from the battery positive electrode material 13. A side of the conductive sample stage 15 away from the battery electrolyte material 12 forms a loop with the control system 8, the power source 6, and the driving device 17 through a power source 6 wire; a battery negative electrode material 10 is provided on a side of the conductive sample stage 15 close to the battery electrolyte material 12, and a sample material 9 is used to be coated inside the battery negative electrode material 10.

[0060] In the probe type compression control structure, the sample material 9 to be compressed coated with the battery negative electrode material 10 is placed on the conductive sample stage 15. The battery positive electrode material 13 and the battery electrolyte material 12 are respectively adhered to the tip of a metal electrode material such as a tungsten tip. The metal electrode material is connected to the driving device 17 of a piezoelectric ceramic. By using the driving device 17 of the piezoelectric ceramic to control the movement of the second metal electrode material 16 until it contacts the battery negative electrode material 10, a complete battery charging loop is formed together with a CPU 3, an electrochemical test and control unit 5, a power source 6, etc. On this basis, by adjusting the ion insertion amount of the inserted ions, the volume of the battery negative electrode material 10 expands, and further the sample material 9 to be compressed coated is compressed. The crystal structure, chemical composition, element valence state, etc. of the sample material 9 are in-situ dynamically comprehensively characterized by techniques such as diffraction and high-resolution imaging of a transmission electron microscope.

[0061] In one embodiment, according to Figures 4-5 as shown, in the probe type compression device, there are various ways to combine the battery positive electrode material 13 and the battery electrolyte material 12 to the second metal electrode material 16.

[0062] According to Figure 4 as shown, one of them is: the second metal electrode material 16 is a tungsten tip, and the battery positive electrode material 13 and the battery electrolyte material 12 are adhered to the tip of the tungsten tip. The battery positive electrode material 13 and the battery electrolyte material 12 are combined to the second metal electrode material 16 by respectively adhering the positive electrode material and the electrolyte material to the tip of a metal electrode material such as a tungsten tip through a focused ion beam bulk sampling technique.

[0063] According to Figure 5As shown, in another case, the second metal electrode material 16 is a tungsten tip, and the battery positive electrode material 13 and the battery electrolyte material 12 are deposited on the tip of the tungsten tip by coating. By using coating technology to deposit the positive electrode material and the electrolyte material on the tip of a metal electrode material such as a tungsten tip, the battery positive electrode material 13 and the battery electrolyte material 12 are combined onto the second metal electrode material 16.

[0064] In the third case, the battery electrolyte material 12 is a gel electrolyte, and the battery positive electrode material 13 and the second metal electrode material 16 are combined into one body and are in contact with the gel electrolyte. After combining the positive electrode material with the metal electrode, the tip is dipped into the gel electrolyte to realize the combination of the battery positive electrode material 13 and the battery electrolyte material 12 onto the second metal electrode material 16.

[0065] Obviously, those skilled in the art can make various changes and modifications to the present invention without departing from the spirit and scope of the present invention. Thus, if these modifications and variations of the present invention fall within the scope of the claims of the present invention and their equivalent technologies, the present invention also intends to include these modifications and variations.

Claims

1. A transmission electron microscope in-situ compression device, characterized in that, Including: A transmission electron microscope sample rod, a sample rod sample stage, and a control system. The input end of the sample rod sample stage is connected to the control system through a power line. The output end of the sample rod sample stage is connected to the transmission electron microscope sample rod. The transmission electron microscope sample rod is used to place the sample stage. The transmission electron microscope sample rod sample stage is used to place the sample material to be compressed and perform an electrochemical reaction on the sample material. By controlling the ion intercalation into the coated layer negative electrode material through the electrochemical reaction, the volume expansion of the coated layer is caused to achieve inward compression of the coated sample material.

2. The in-situ compression device for a transmission electron microscope according to claim 1, wherein The control system includes: a CPU, an ammeter, an electrochemical test and control unit 5, a control switch, and a power supply. The output end of the CPU is connected to the transmission electron microscope sample rod. The input end of the CPU is sequentially connected to the ammeter and the electrochemical test and control unit 5. One end of the electrochemical test and control unit 5 away from the ammeter is connected to the power supply through the control switch.

3. The in-situ compression device for a transmission electron microscope according to claim 1, characterized in that, The transmission electron microscope sample rod includes a MEMS microelectrical chip structure and a scanning probe control structure; The MEMS microelectrical chip structure is a transmission electron microscope sample rod with a microelectrical measurement chip made by MEMS technology; The scanning probe control structure is a transmission electron microscope sample rod with a scanning probe control unit.

4. The in-situ compression device for a transmission electron microscope according to claim 3, characterized in that, The MEMS microelectrical chip structure is arranged on the sample rod sample stage through the transmission electron microscope sample rod and is connected to the power supply through the control system; The MEMS microelectrical chip structure includes: a sample material to be compressed, a first coated layer battery negative electrode material, a second coated layer battery negative electrode material, a battery electrolyte material, a battery positive electrode material, and a first metal electrode material, The coated layer negative electrode material, the battery electrolyte material, and the battery positive electrode material are connected in sequence as a whole. On one side of the coated layer negative electrode material away from the battery electrolyte material and on one side of the battery positive electrode material away from the battery electrolyte material, first metal electrode materials are respectively provided. The first metal electrode materials are respectively connected to the positive and negative electrodes of the power supply; The coated layer negative electrode material wraps the sample.

5. The in-situ compression device for a transmission electron microscope according to claim 3, characterized in that, The scanning probe control structure includes: a battery electrolyte material, a battery positive electrode material, a conductive sample stage, a second metal electrode material, and a driving device; One end of the driving device is connected to the power supply and the control system. The other end of the driving device is sequentially connected to the second metal electrode material, the battery positive electrode material, and the battery electrolyte material as a whole. On one side of the battery electrolyte material away from the battery positive electrode material, a conductive sample stage is provided at intervals. On one side of the conductive sample stage away from the battery electrolyte material, a loop is formed with the control system, the power supply, and the driving device through a power line; On one side of the conductive sample stage close to the battery electrolyte material, a battery negative electrode material is provided. The battery negative electrode material is used to wrap the sample inside.

6. The in-situ compression device for a transmission electron microscope according to claim 5, characterized in that The second metal electrode material is a pure metal or alloy material such as a tungsten tip, and the battery positive electrode material and the battery electrolyte material adhere to the tip of the second metal electrode material.

7. The in-situ compression device for a transmission electron microscope according to claim 5, characterized in that The second metal electrode material is a pure metal or alloy material such as a tungsten tip, and the battery positive electrode material and the battery electrolyte material are deposited on the tip of the second metal electrode material through coating.

8. The in-situ compression device for a transmission electron microscope according to claim 5, wherein, The battery electrolyte material is a gel electrolyte, and the battery positive electrode material and the second metal electrode material are combined into one body and are in contact with the gel electrolyte.

9. The in-situ compression device for a transmission electron microscope according to claim 4, wherein The coated layer negative electrode material encapsulates a battery negative electrode material, and a sample is embedded in the battery negative electrode material.

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