An atom-resolved in-situ non-magnetic environment transmission electron microscope experimental system

Abstract

The present application relates to the field of transmission electron microscopy, and more particularly to an atomic resolution in-situ non-magnetic environment transmission electron microscopy experimental system, comprising a sample rod body, a rod head, a double-inclination device, a magnetic shielding device and a sample mounting device, one end of the rod head being connected with the sample rod body; the double-inclination device being arranged at the other end of the rod head. By clamping the sample mounting device between two adjacent high-permeability screens, i.e. clamping the sample mounting probe between two adjacent high-permeability screens, a "sandwich" structure is formed, and in combination with a three-stage centering mechanism, a stable and uniform non-magnetic environment can be constructed in the magnetic flux absorption cavity, meeting the intrinsic characterization requirements of sensitive samples such as magnetic materials and superconducting materials; at the same time, the sample can be precisely tilted in two axes, and the magnetic shielding structure does not block the electron beam, ensuring that the transmission electron microscope can obtain clear atomic resolution images, realizing the integration of the "non-magnetic environment-two-axis tilting-atomic resolution" sample rod, and effectively breaking through the technical bottleneck of the prior art.

Description

Technical Field

[0001] This invention relates to the field of transmission electron microscopy, and more particularly to an atomic-resolution in-situ non-magnetic environment transmission electron microscopy experimental system. Background Technology

[0002] The statements herein are provided only as background information in connection with this application and do not necessarily constitute prior art.

[0003] Transmission electron microscopy (TEM), as a core characterization tool in materials science, nanotechnology, condensed matter physics, and other fields, can intuitively reveal the microstructure, crystal defects, and elemental distribution of materials with its atomic-level spatial resolution, providing irreplaceable technical support for the study of the correlation between intrinsic properties and microstructure of materials. With the deepening research on magnetic field-sensitive materials such as magnetic materials, superconducting materials, semiconductor devices, and magnetic element metallic materials (steel, high-entropy magnetic alloys, etc.), in-situ characterization techniques have become crucial for overcoming the limitations of traditional characterization methods and realizing the observation of dynamic microscopic behavior of materials.

[0004] As the core connecting component between the transmission electron microscope (TEM) and the sample, the performance of the sample holder directly determines the accuracy, stability, and applicability of in-situ characterization. An ideal in-situ sample holder must simultaneously meet two core requirements: first, it must provide a non-magnetic environment for magnetically sensitive samples, preventing the magnetic field inside the TEM (such as the objective lens magnetic field) from interfering with the intrinsic microstructure and physical properties of the sample, thus ensuring the authenticity of the characterization results; second, it must have a dual-axis tilting function, allowing flexible adjustment of the sample's orientation so that the electron beam is incident along the low-index crystal plane of the sample, thereby obtaining clear electron diffraction patterns and high-quality atomic resolution images, meeting the needs of multi-directional and multi-angle in-situ observation.

[0005] Currently, research in fields such as magnetic materials and superconducting materials places higher demands on the non-magnetic properties and tilting accuracy of sample rods. This requires both atomic-level resolution observation and strict control of the magnetic field strength in the sample region to avoid problems such as magnetic field damage to the intrinsic magnetic structure of the sample, induced magnetic moment disorder, and destruction of the superconducting state. Furthermore, in-situ studies often require consideration of external conditions such as temperature and stress, further demanding that the sample rod, in addition to achieving non-magnetic and biaxial tilting capabilities, possess a compact structure, strong compatibility, and high stability, adapting to existing mainstream transmission electron microscopes without requiring large-scale modifications to the microscope itself.

[0006] In the field of transmission electron microscopy (TEM) sample characterization, the biaxial tilting sample rod is a core component for achieving multi-pose observation of samples and acquiring clear atomic-scale images. The design of its dual-tilt mechanism directly determines the tilting accuracy, stability, and imaging quality. Currently, biaxial tilting sample rods are incompatible with magnetic shielding, and non-magnetic characterization techniques require modifications to the electron microscope structure, making it difficult to maintain atomic resolution. Summary of the Invention

[0007] This invention aims to solve at least one of the technical problems existing in related technologies. To this end, this invention proposes an atomic-resolution in-situ non-magnetic environment transmission electron microscopy experimental system, which can construct a stable and uniform non-magnetic environment within a magnetic flux absorption cavity, while simultaneously achieving precise biaxial tilting of the sample, ensuring that the transmission electron microscope can obtain clear atomic resolution images in a magnetic field-free environment.

[0008] An atomic-resolution in-situ transmission electron microscopy experimental system for a non-magnetic environment according to an embodiment of the present invention includes: Sample rod body; A rod head, one end of which is connected to the sample rod body; A double tilting device is provided at the other end of the rod head. The double tilting device includes a double tilting platform and a micro displacement actuator. The double tilting platform is located on the side of the micro displacement actuator away from the sample rod body. The double tilting platform is rotatably connected to the rod head and movably connected to the micro displacement actuator. A magnetic shielding device is provided on the double tilting platform. The magnetic shielding device includes multiple high-permeability magnetic screens, which are stacked sequentially. The central holes of the multiple high-permeability magnetic screens are connected to form a magnetic flux absorption cavity. The sample mounting device is clamped between two adjacent high-permeability magnetic screens. The sample mounting device is equipped with a sample support stage, which is located inside the magnetic flux absorption cavity.

[0009] According to one embodiment of the present invention, the sample mounting device includes: The sample-mounted probe is clamped between two high-permeability magnetic screens. One end of the sample-mounted probe extends to the outside of the two high-permeability magnetic screens, and the other end extends into the magnetic flux absorption cavity. The sample support stage is disposed at the other end of the sample-mounted probe.

[0010] According to one embodiment of the present invention, at least one of two adjacent high-permeability magnetic screens is provided with a sample probe assembly slot on one side facing each other, and the sample-mounted probe is embedded in the sample probe assembly slot.

[0011] According to one embodiment of the present invention, the two high-permeability magnetic screens are each provided with a sample probe mounting slot on one side facing each other, and the two sample probe mounting slots are symmetrically arranged about the central axis of the sample-mounted probe.

[0012] According to one embodiment of the present invention, the double tilting platform is provided with a magnetic shield mounting groove, one side of the double tilting platform is provided with an opening communicating with the magnetic shield mounting groove, the other side of the double tilting platform is provided with a through hole communicating with the magnetic shield mounting groove, and the magnetic shielding device is embedded inside the magnetic shield mounting groove.

[0013] According to one embodiment of the present invention, the magnetic shielding device further includes: A magnetic shield cover plate, which closes to the opening and is detachably connected to the double tilting platform.

[0014] According to one embodiment of the present invention, the edge of the magnetic screen mounting groove is detachably connected to the magnetic screen cover plate.

[0015] According to one embodiment of the present invention, a probe limiting groove is provided on the edge of the magnetic screen mounting groove, and the tail limiting structure of the other end of the sample-mounted probe is embedded in the probe limiting groove. A protrusion is provided on the magnetic screen cover near the micro displacement actuator. The protrusion is embedded in the probe limiting groove and abuts against the tail limiting structure of the sample-mounted probe.

[0016] According to one embodiment of the present invention, a double tilting platform mounting groove is provided at the other end of the rod head. The double tilting platform mounting groove has two opposing side walls that extend along the length direction of the rod head. Both side walls are provided with double tilting platform limiting holes. The double tilting platform is disposed in the double tilting platform mounting groove. Rotating shafts are provided on both sides of the double tilting platform, and the rotating shafts are rotatably engaged with the double tilting platform limiting holes.

[0017] According to one embodiment of the present invention, the sample rod body, the rod head, and the double tilting device are all made of antimagnetic alloy.

[0018] The above-described one or more technical solutions in the embodiments of the present invention have at least one of the following technical effects: By mounting the sample carrier device within a high-permeability magnetic screen—specifically, assembling the sample carrier stage at the front end of the sample carrier probe clip at the center of the flux absorption cavity constructed by the high-permeability magnetic screen—and employing a three-stage alignment mechanism, a stable and uniform non-magnetic environment can be constructed within the flux absorption cavity, meeting the intrinsic characterization requirements of sensitive samples such as magnetic and superconducting materials. Simultaneously, precise biaxial tilting of the sample is achieved, and the magnetic shielding structure does not obstruct the electron beam, ensuring that the transmission electron microscope can obtain clear atomic resolution images. This integrated sample holder, encompassing a non-magnetic environment, biaxial tilting, and atomic resolution, effectively overcomes existing technological bottlenecks.

[0019] Additional aspects and advantages of the invention will be set forth in part in the description which follows, and in part will be obvious from the description, or may be learned by practice of the invention. Attached Figure Description

[0020] To more clearly illustrate the technical solutions in the embodiments of the present invention or related technologies, the drawings used in the description of the embodiments or related technologies will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present invention and are not considered as limitations on this application. Moreover, those skilled in the art can obtain other drawings based on these drawings without creative effort.

[0021] Figure 1 This is a top view schematic diagram of the atomic resolution in-situ non-magnetic environment transmission electron microscope experimental system provided by the present invention.

[0022] Figure 2 This is a side view cross-sectional structural diagram of the atomic resolution in-situ non-magnetic environment transmission electron microscope experimental system provided by the present invention.

[0023] Figure 3 This is a top view of the double tilting device provided by the present invention.

[0024] Figure 4 This is an exploded structural diagram of the double-tilting device provided by the present invention.

[0025] Figure 5 This is a three-dimensional structural diagram of the double-tilting device provided by the present invention.

[0026] Figure label: 1. Pole head; 101. Double tilting platform mounting slot; 102. Double tilting platform limiting hole; 103. Driver mounting slot; 2. Sample rod body; 201. Electrical interface; 3. Magnetic shielding device; 301. High-permeability magnetic shield; 303. Magnetic shield cover plate; 304. Second screw; 4. Sample mounting device; 401. Sample mounting probe; 402. Sample probe assembly slot; 5. Double tilting device; 501. Double tilting stage; 502. Magnetic screen mounting groove; 503. Probe limiting groove; 504. Elliptical connecting hole; 505. Miniature displacement actuator; 506. Double tilting connecting shaft; 507. Double tilting stage fixing cover plate; 508. First screw. Detailed Implementation

[0027] Embodiments of the present invention are described in detail below. Examples of these embodiments are shown in the accompanying drawings, wherein the same or similar reference numerals denote the same or similar elements or elements having the same or similar functions throughout. The embodiments described below with reference to the accompanying drawings are exemplary and are only used to explain the present invention, and should not be construed as limiting the present invention.

[0028] The specific terms used in this specification are for illustrative purposes only and are not intended to limit the illustrated embodiments. For example, expressions such as "same" and "identical" not only indicate a strictly identical state, but also indicate a state with tolerances or differences in the degree of functionality. For example, expressions indicating relative or absolute arrangement such as "in a certain direction," "along a certain direction," "side by side," "perpendicular," "centered on," "concentric," or "coaxial" not only strictly indicate such an arrangement, but also indicate a state of relative displacement by tolerances or angles or distances with the same degree of functionality.

[0029] The terms “center,” “longitudinal,” “lateral,” “length,” “width,” “thickness,” “upper,” “lower,” “front,” “rear,” “left,” “right,” “vertical,” “horizontal,” “top,” “bottom,” “inner,” “outer,” “clockwise,” “counterclockwise,” “axial,” “radial,” and “circumferential” indicate the orientation or positional relationship based on the orientation or positional relationship shown in the accompanying drawings. They are used only for the convenience of describing the present invention and simplifying the description, and are not intended to indicate or imply that the device or element referred to must have a specific orientation, or be constructed and operated in a specific orientation. Therefore, they should not be construed as limiting the present invention.

[0030] Furthermore, features specified as "first" or "second" may explicitly or implicitly include one or more of those features. In the description of this invention, unless otherwise stated, "a plurality of" means two or more.

[0031] In the description of this invention, it should be noted that, unless otherwise explicitly specified and limited, the terms "installation," "connection," and "linking" should be interpreted broadly. For example, they can refer to a fixed connection, a detachable connection, or an integral connection; they can refer to a mechanical connection or an electrical connection; they can refer to a direct connection or an indirect connection through an intermediate medium; and they can refer to the internal connection of two components. Those skilled in the art can understand the specific meaning of the above terms in this invention based on the specific circumstances.

[0032] Before introducing the atomic-resolution in-situ non-magnetic environment transmission electron microscopy experimental system of the present invention, let's first introduce the relevant technical terms: Piezoelectric ceramic actuator: abbreviated as PZT, commonly known in the industry as piezoelectric ceramic actuator, is a component that uses the piezoelectric effect to convert electrical energy into mechanical energy. It can generate minute extension and contraction displacement by receiving electrical signals, and is used to precisely drive the tilting of a double tilting table.

[0033] TEM: Transmission Electron Microscope, commonly known in the industry as a transmission electron microscope, is the adapter device for the sample holder of this invention, used to achieve atomic-scale imaging of samples.

[0034] High permeability magnetic shield: refers to a shielding component made of magnetic material with high permeability and high saturation magnetization. It is commonly known in the industry as a high permeability magnetic shield and is used to guide magnetic fields and create a non-magnetic environment in the sample area.

[0035] The following is combined Figures 1 to 5 The specific structure and working principle of the atomic-resolution in-situ non-magnetic environment transmission electron microscopy experimental system of the present invention are described.

[0036] like Figures 1 to 5 As shown, the atomic resolution in-situ non-magnetic environment transmission electron microscopy experimental system includes a sample rod body 2, a rod head 1, a double tilting device 5, a magnetic shielding device 3, and a sample mounting device 4. One end of the rod head 1 is connected to the sample rod body 2, and the double tilting device 5 is located at the other end of the rod head 1. The double tilting device 5 includes a double tilting stage 501 and a micro displacement actuator 505. The double tilting stage 501 is located on the side of the micro displacement actuator 505 away from the sample rod body 2. The double tilting stage 501 is rotatably connected to the rod head 1 and movably connected to the micro displacement actuator 505. The magnetic shielding device 3 is located on the double tilting stage 501 and includes two high-permeability magnetic screens 301. The two high-permeability magnetic screens 301 are stacked sequentially, and their central holes are connected to form a magnetic flux absorption cavity. The sample mounting device 4 is clamped between the two high-permeability magnetic screens 301 and has a sample support stage located at the center of the magnetic flux absorption cavity.

[0037] The atomic resolution in-situ non-magnetic environment transmission electron microscopy experimental system provided by this invention forms a "sandwich" structure by clamping the sample mounting device 4 between two high-permeability magnetic screens 301, i.e., the sample mounting probe 401 is clamped between two high-permeability magnetic screens 301. Combined with a three-stage centering mechanism, a stable and uniform non-magnetic environment can be constructed within the magnetic flux absorption cavity, meeting the intrinsic characterization requirements of sensitive samples such as magnetic materials and superconducting materials. At the same time, it achieves precise biaxial tilting of the sample, and the magnetic shielding structure does not block the electron beam, ensuring that the transmission electron microscope can obtain clear atomic resolution images. It realizes the integrated sample rod integration of "non-magnetic environment - biaxial tilting - atomic resolution", effectively breaking through the bottleneck of existing technology. The atomic resolution in-situ non-magnetic environment transmission electron microscopy experimental system provided by this invention can be adapted to FIB sample preparation, ∅3 samples, etc.

[0038] In one embodiment of the present invention, such as Figures 1 to 5 As shown, each of the two adjacent high-permeability magnetic screens 301 has a central hole. The two high-permeability magnetic screens 301 are the same size and are coaxially arranged so that the two central holes are on the same straight line.

[0039] The high-permeability magnetic shield 301 is made of a high-permeability, high-saturation-magnetization magnetic material, precision-machined into a ring structure. The material of the high-permeability magnetic shield 301 is a high-permeability shielding material, possessing excellent magnetic field guiding and focusing capabilities. The dimensions of the high-permeability magnetic shield 301 are specifically determined based on the dimensions of the sample-mounted probe 401 and the magnetic shield mounting slot 502 to ensure smooth assembly and the formation of a sufficient magnetic flux absorption cavity. Due to its ring structure, the high-permeability magnetic shield 301 has a large specific surface area (surface area / volume), which effectively reduces magnetic flux density, improves the magnetic field line carrying capacity, and avoids a decrease in shielding effect caused by magnetic saturation. The inner wall of the central hole of the high-permeability magnetic shield 301 is a smooth, rounded surface, without sharp edges or bends, reducing end-face magnetic leakage and local magnetic distortion, and ensuring the uniformity of the internal magnetic field.

[0040] In one embodiment of the present invention, such as Figures 1 to 5 As shown, the sample mounting device 4 includes a sample mounting probe 401, which is a slender rod-shaped structure. This slender rod-shaped structure reduces obstruction of the electron beam, ensuring smooth penetration of the sample and facilitating precise placement of the sample into the center of the flux absorption cavity. The sample mounting probe 401 is made of antimagnetic hard alloy to prevent magnetization and the introduction of magnetic interference. The sample mounting probe 401 possesses good mechanical strength and electrical conductivity.

[0041] The sample-mounted probe 401 carries the sample and precisely fixes it at the center of the flux-absorbing cavity (i.e., on the electron beam incident path), ensuring atomic-resolution observation of the sample in a non-magnetic environment. The sample-mounted probe 401 is clamped between two high-permeability magnetic screens 301. The tail-end limiting structure of the sample-mounted probe 401 extends to the outside of the two high-permeability magnetic screens 301 and is embedded in the probe limiting groove 503. The other end of the sample-mounted probe 401 extends into the flux-absorbing cavity; that is, the length of the sample-mounted probe 401 is greater than the diameter of the high-permeability magnetic screens 301. A sample support stage is located at the other end of the sample-mounted probe 401 and is used to hold the sample. The sample support stage has undergone precision polishing to ensure stable sample placement, prevent displacement during tilting, and guarantee image clarity.

[0042] In one embodiment of the present invention, such as Figures 1 to 5As shown, at least one of the two high-permeability magnetic screens 301 has a sample probe mounting groove 402 on one of its opposing sides. This groove is located on the inner surface of the high-permeability magnetic screen 301, allowing the outer wall of the sample-mounted probe 401 to contact the inner wall of the groove after insertion, thus reducing the possibility of rotation or axial displacement of the probe within the magnetic screen. The sample probe mounting groove 402 extends radially along the high-permeability magnetic screen 301, perpendicular to its central axis, providing a radially guiding channel for the sample-mounted probe 401. The sample-mounted probe 401 is embedded within the sample probe mounting groove 402. When the probe is inserted into the groove, its side surface contacts the two side walls of the groove, restricting its oscillation in the direction perpendicular to the radial direction.

[0043] The sample probe mounting slot 402 is a conical slot, and the axis of the sample probe mounting slot 402 coincides with the axis of the sample probe. The size of the sample probe mounting slot 402 is adapted to the size of the sample mounting probe 401 to ensure that the sample is fixed in the center of the magnetic flux absorption cavity. At the same time, it minimizes the magnetic field distortion and shielding effect loss caused by the irregular structure. The conical structure can avoid sharp edges and reduce the local accumulation of magnetic field, ensuring that the magnetic field around the sample is uniform.

[0044] In one embodiment of the present invention, such as Figures 1 to 5 As shown, each of the two high-permeability magnetic screens 301 has a sample probe mounting slot 402 on one side facing each other. This arrangement provides each high-permeability magnetic screen 301 with an independent limiting structure, and the two limiting slots together exert a double-sided constraint on the sample-mounted probe 401. The two sample probe mounting slots 402 are symmetrically arranged about the central axis of the sample-mounted probe 401. This symmetrical arrangement makes the positions of the two limiting slots mirror those of the probe's central axis, so that after the probe is inserted, the inner walls of the two limiting slots contact the corresponding parts on both sides of the probe. Due to the symmetrical arrangement of the two limiting slots, the lateral constraint forces on both sides are equal in magnitude and opposite in direction, balancing the forces on both sides of the sample-mounted probe 401. This reduces the deflection or tilting of the sample-mounted probe 401 caused by uneven forces on one side, ensuring that the central axis of the probe remains aligned with the preset position during movement.

[0045] In one embodiment of the present invention, such as Figures 1 to 5 As shown, the double tilting platform 501 is provided with a magnetic shield mounting groove 502. One side of the double tilting platform 501 is provided with an opening that communicates with the magnetic shield mounting groove 502, and the other side of the double tilting platform 501 is provided with a through hole that communicates with the magnetic shield mounting groove 502. The magnetic shielding device 3 is embedded inside the magnetic shield mounting groove 502.

[0046] The magnetic shield mounting slot 502 has a recessed structure, and its dimensions are adapted to the dimensions of the high-permeability magnetic shield 301 to ensure that the high-permeability magnetic shield 301 is flush with the end face of the double tilting stage 501 after being embedded, avoiding displacement or tilting, which could block the electron beam or cause distortion of the magnetic field distribution. The design of the magnetic shield mounting slot 502, the opening, and the through holes gives the double tilting stage 501 a stepped structure, which reduces weight, lowers tilting inertia, and provides installation space for various components. The double tilting stage 501 is made of antimagnetic alloy.

[0047] In one embodiment of the present invention, such as Figures 1 to 5 As shown, the magnetic shielding device 3 also includes a magnetic shield cover plate 303. The magnetic shield cover plate 303 has a through hole in its center, allowing more of the magnetic shield to be exposed, facilitating better guidance of the magnetic flux and achieving a magnetic field-free environment within the flux absorption cavity. It also reduces the obstruction and scattering of the electron beam by the cover plate and contributes to weight reduction. The magnetic shield cover plate 303 is made of an antimagnetic alloy to prevent itself from being magnetized. The dimensions of the magnetic shield cover plate 303 are adapted to the dimensions of the double tilting stage 501, ensuring a tight fit between the magnetic shield cover plate 303 and the double tilting stage 501.

[0048] The magnetic screen cover 303 closes onto the opening. The magnetic screen cover 303 is detachably connected to the double tilting stage 501. This detachable connection allows the magnetic screen cover 303 to be separated from the double tilting stage 501. Thus, when it is necessary to install or remove the high-permeability magnetic screen 301, the magnetic screen cover 303 can be removed first to expose the opening, which facilitates the operation of the high-permeability magnetic screen 301. After the high-permeability magnetic screen 301 is placed in place, the magnetic screen cover 303 can be installed back onto the double tilting stage 501.

[0049] The magnetic shield cover 303 abuts against the high-permeability magnetic shield 301 located near the magnetic shield cover 303. This abutment occurs between the inner surface of the magnetic shield cover 303 and the outer surface of the high-permeability magnetic shield 301. As the magnetic shield cover 303 connects to and gradually locks into the double tilting platform 501, the magnetic shield cover 303 continuously moves towards the opening relative to the double tilting platform 501 until the inner surface of the magnetic shield cover 303 contacts the outer surface of the high-permeability magnetic shield 301. At this point, the magnetic shield cover 303 stops moving, while the locking force continues to increase, causing the magnetic shield cover 303 to apply pressure to the high-permeability magnetic shield 301. The direction of this pressure is perpendicular to the surface of the high-permeability magnetic shield 301 and towards the other high-permeability magnetic shield 301. Under this pressure, the high-permeability magnetic shield 301 contacts and remains in a close fit with the other high-permeability magnetic shield 301, thereby reducing the magnetic circuit gap between the two magnetic shields.

[0050] In one embodiment of the present invention, the edge of the magnetic shield mounting groove 502 is detachably connected to the magnetic shield cover plate 303. Specifically, as shown in the figure... Figures 1 to 5As shown, the magnetic shield mounting groove 502 has a second threaded hole along its edge. In this embodiment, there are four second threaded holes, which are arranged circumferentially around the outer periphery of the magnetic shield mounting groove 502. Of course, the number of second threaded holes is not limited to this; three, five, six, or more can also be provided. The magnetic shield cover plate 303 has a second through hole, the number of which is the same as the number of second threaded holes. The positions of the second through holes correspond one-to-one with the positions of the second threaded holes. The second screw 304 inside the second through hole is threadedly engaged with the second threaded hole.

[0051] Furthermore, the second screw 304 is made of an antimagnetic alloy, and its head is countersunk to prevent it from protruding and obstructing the electron beam. The second screw 304 is used to securely connect the magnetic shielding cover 303 to the double tilting stage 501, ensuring the overall stability of the magnetic shielding device 3.

[0052] The magnetic shielding device 3 is fully embedded in the magnetic screen mounting groove 502, with a clearance fit between the magnetic screen mounting groove 502 and the magnetic shielding device 3 to ensure assembly accuracy. After assembly, it is axially pressed by the magnetic screen cover plate 303, and then axially fixed by the second screw 304, so that the magnetic shielding device 3 and the double tilting device 5 are aligned, ensuring that the center of the magnetic shielding device 3 coincides with the center of the sample support stage and the electron beam incident direction, avoiding magnetic field distortion and electron beam obstruction caused by the offset of the magnetic shielding structure.

[0053] In one embodiment of the present invention, such as Figures 1 to 5 As shown, a probe limiting groove 503 is provided along the edge of the magnetic screen mounting groove 502. The probe limiting groove 503 is a trapezoidal groove structure, and its size is adapted to the size of the other end of the sample-mounted probe 401. The probe limiting groove 503 is used to fix the tail limiting structure of the other end of the sample-mounted probe 401. The tail limiting structure is embedded in the probe limiting groove 503. The high-permeability magnetic screen 301 near the opening of the magnetic screen mounting groove 502 is provided with a protrusion, which is embedded in the probe limiting groove 503 and abuts against the other end of the sample-mounted probe 401. This ensures the precise positioning of the sample-mounted probe 401 and also provides a clamping effect on the sample-mounted probe 401 and the high-permeability magnetic screen 301, preventing loosening of the assembly.

[0054] Installation method of magnetic shielding device 3: First, embed a high-permeability magnetic screen 301 into the magnetic screen mounting groove 502 of the double tilting stage 501, ensuring that the high-permeability magnetic screen 301 fits tightly against the bottom of the magnetic screen mounting groove 502; then, embed one end of the sample-carrying probe 401 into the sample probe assembly groove 402 of the high-permeability magnetic screen 301, and the other end into the probe limiting groove 503 of the double tilting stage 501; then, cover the sample-carrying probe 401 with another high-permeability magnetic screen 301 and embed it into the magnetic screen mounting groove 502, so that the sample probe assembly grooves 402 of the two high-permeability magnetic screens 301 clamp the sample-carrying probe 401; finally, cover the opening of the magnetic screen mounting groove 502 with the magnetic screen cover plate 303, so that the protrusion is embedded in the probe limiting groove 503, and pass the second screw 304 through the second through hole of the magnetic screen cover plate 303 and fasten it to the second threaded hole of the double tilting stage 501 to complete the overall assembly of the magnetic shielding device 3.

[0055] The magnetic shielding device 3 serves to shield the strong magnetic field in the objective region of the transmission electron microscope (TEM), creating a stable and uniform non-magnetic environment in the sample mounting area (magnetic flux absorption cavity). This meets the requirements for characterizing the intrinsic microstructure of magnetically sensitive samples. Specifically, the high-permeability magnetic shield 301 is made of a high-permeability material with high saturation magnetization and high permeability. When the sample mounting probe 401 is inserted into the TEM pole shoe region, the strong magnetic field lines generated by the objective pole shoe are actively guided and converged by the high-permeability material. The magnetic field lines preferentially travel along the wall of the high-permeability magnetic shield 301 (rather than penetrating the wall to enter the interior); the two high-permeability magnetic shields 301 form a... The hollow region serves as the magnetic flux absorption cavity. This region acts as a low-magnetic-field-energy annular magnetic potential trap, which can "trap" the guided magnetic field and prevent magnetic field lines from entering the cavity and contacting the sample. At the same time, the large specific surface area of ​​the high-permeability magnetic shield 301 reduces the magnetic flux density and improves the magnetic field line carrying capacity, avoiding the decrease in shielding effect caused by magnetic saturation. The smooth inner wall of the central hole reduces end-face leakage and local magnetic distortion, ensuring a stable and uniform non-magnetic environment inside the magnetic flux absorption cavity. The antimagnetic material magnetic shield cover 303 and fastening screws prevent themselves from being magnetized, preventing the introduction of additional magnetic interference and further ensuring the stability of the non-magnetic environment.

[0056] Furthermore, the coaxiality of the magnetic shielding device 3 directly affects the magnetic shielding effect and electron beam transmission. This invention ensures coaxiality through three levels of positioning: First, the magnetic shielding device 3 achieves initial alignment through the clearance fit between the magnetic shielding mounting groove 502 and the double tilting device 5; Second, the precise fit between the double tilting stage limiting hole 102 and the rotating shaft further ensures that the relative positions of the double tilting device 5, the rod head 1, and the sample rod body 2 are fixed, thereby driving the magnetic shielding device 3 to maintain alignment with the sample rod axis; Third, after the magnetic shielding device 3 enters the pole shoe space, it can be finely adjusted through the transmission electron microscope goniometer stage displacement system to eliminate assembly errors and positional offsets, ensuring that the center of the magnetic shielding device 3 is strictly axially aligned with the center of the pole shoe and the electron beam incident direction, avoiding damage to the original magnetic field distribution of the objective lens due to positional offsets.

[0057] The atomic resolution in-situ non-magnetic environment transmission electron microscope experimental system provided by this invention can be directly adapted to existing conventional transmission electron microscopes through optimized overall structural design, without any modification to the microscope, and has a wide range of compatibility; at the same time, the modular design facilitates assembly, disassembly and maintenance, greatly reducing the user's operating threshold.

[0058] The atomic resolution in-situ non-magnetic environment transmission electron microscopy experimental system provided by this invention features precise assembly and secure connection of all core components, resulting in high structural stability and meeting the durability requirements of conventional use scenarios. Furthermore, the sample-mounted probe is conductive, and the magnetic shielding device 3 and the micro displacement actuator 505 can be replaced with equivalent components as needed, adapting to different observation scenarios. Compared to existing technologies, its scalability is significantly improved.

[0059] In one embodiment of the present invention, such as Figures 1 to 5 As shown, the other end of the pole head 1 is provided with a double tilting platform mounting groove 101. The double tilting platform mounting groove 101 is a hollowed-out frame structure. The interior of the double tilting platform mounting groove 101 has sufficient space to ensure that the double tilting platform 501 has no motion interference within the maximum tilting angle range. This provides sufficient movement space for the tilting of the double tilting platform 501, reduces the weight of the pole head 1, reduces the inertia during the tilting process, and improves the tilting accuracy and stability.

[0060] The double tilting platform mounting groove 101 has two opposing sidewalls extending along the length of the rod head 1. Both sidewalls are provided with double tilting platform limiting holes 102. The double tilting platform 501 is disposed within the double tilting platform mounting groove 101. Rotating shafts are provided on both sides of the double tilting platform 501, and these shafts are rotatably engaged with the double tilting platform limiting holes 102. The rotating shafts provide support and limit for the tilting of the double tilting platform 501, ensuring that the rotating shafts do not radially deviate during tilting.

[0061] Furthermore, the rotating shaft is fitted with the limiting hole 102 of the double tilting platform with a clearance fit, leaving an appropriate margin to ensure that the platform rotates smoothly during the double tilting process.

[0062] Furthermore, the mating surfaces of the rotating shaft and the double tilting stage limiting holes 102 are precision polished to reduce vibration and offset during tilting and ensure precise control of the tilting angle.

[0063] The function of the dual-tilt device 5 is to achieve precise biaxial tilting of the sample, adjust the sample orientation, and allow the electron beam to be incident along the low-index crystal plane of the sample, obtaining clear electron diffraction patterns and high-quality atomic resolution images. Specifically, the working principle is as follows: the control circuit converts the externally input driving signal into a driving current, which is transmitted to the micro-displacement actuator 505. The micro-displacement actuator 505 generates a corresponding minute displacement (stretching or contraction) according to the magnitude and direction of the driving current. This displacement is transmitted to the dual-tilt stage 501 through the dual-tilt connecting shaft 506, causing the dual-tilt stage 501 to rotate around the central axis of the rotating shaft inside the dual-tilt stage limiting hole 102, thus achieving precise tilting of the sample and meeting the precise control requirements of atomic resolution imaging for sample attitude. The elliptical design of the elliptical connecting hole 504 and the precision polishing of each mating surface jointly ensure the stability and accuracy of the tilting process: the elliptical connecting hole 504 buffers the deformation stress of the micro-displacement actuator 505, avoiding vibration; the precision polished mating surfaces reduce friction, minimizing jamming and positioning deviations during tilting.

[0064] like Figures 1 to 5 As shown, the dual-tilting device 5 includes a dual-tilting stage 501, a micro-displacement actuator 505, and a dual-tilting connecting shaft 506. The dual-tilting stage 501 is located on the side of the micro-displacement actuator 505 away from the sample rod body 2, and is rotatably connected to the rod head 1. The dual-tilting stage 501 is provided with a connecting part, and an elliptical connecting hole 504 is provided at the end of the connecting part near the micro-displacement actuator 505. The dual-tilting connecting shaft 506 is movably inserted into the elliptical connecting hole 504 and connected to the displacement shaft of the micro-displacement actuator 505. A magnetic shielding device 3 is disposed on the dual-tilting stage 501, and a sample mounting device 4 is disposed inside the magnetic shielding device 3.

[0065] By placing the double tilting device 5 at the other end of the rod head 1, the conventional long rod transmission structure design is abandoned, which can shorten the transmission path, reduce the accumulation of transmission gap, and thus improve the repeatability of tilting positioning. The double tilting connecting shaft 506 is movably inserted into the interior of the elliptical connecting hole 504 and connected to the displacement shaft of the micro displacement actuator 505. The double tilting connecting shaft 506 can slide and rotate relative to the long axis within the elliptical connecting hole 504. When the output shaft of the micro displacement actuator 505 extends or retracts, the double tilting connecting shaft 506 is driven, which in turn pushes the double tilting platform 501 to tilt around its rotational connection point with the rod head 1 through the inner wall of the elliptical connecting hole 504, thereby realizing the connection between the double tilting platform 501 and the micro displacement actuator 505. This connection method allows the double tilting connecting shaft 506 to have a certain displacement compensation space within the elliptical connecting hole 504, thereby reducing interference during transmission. Because the elliptical connecting hole 504 is used in conjunction with the double tilting connecting shaft 506, it can directly compensate for the minute deformations generated during the drive process. These minute deformations can be absorbed by the relative motion between the elliptical connecting hole 504 and the double tilting connecting shaft 506, thus avoiding the transmission of these minute deformations as stress to the double tilting platform 501. This fundamentally solves the problems of stress concentration and vibration, allowing the displacement generated by the piezoelectric drive to be transmitted to the double tilting platform 501 more smoothly, reducing mechanical vibration during tilting and improving tilting stability.

[0066] The atomic-resolution in-situ non-magnetic environment transmission electron microscopy experimental system provided by this invention overcomes the defects of conventional long rod driven double tilting mechanisms such as vibration, deformation, and difficulty in vacuum sealing. It also solves the problems of insufficient stability, inability to integrate functional modules, and complex assembly of existing piezoelectric ceramic driven double tilting mechanisms. The tilting accuracy and stability are significantly improved, which can meet the stringent requirements of atomic-scale characterization.

[0067] In one embodiment of the present invention, such as Figures 1 to 5As shown, the connecting part has a sheet-like structure and extends along the length of the rod head 1. This allows the connecting part to transmit the driving force generated by the output shaft of the micro displacement actuator 505 to the double tilting platform 501 along the length of the rod head 1, shortening the force transmission path and reducing elastic deformation during transmission. There are two connecting parts, symmetrically arranged on both sides of the output shaft. The elliptical connecting holes 504 of the two connecting parts are symmetrically arranged about the output shaft. The elliptical connecting holes 504 of the two connecting parts are connected to the same double tilting connecting shaft 506. The double tilting connecting shaft 506 passes through both elliptical connecting holes 504 simultaneously and can slide along the major axis and rotate relative to each other within the two elliptical connecting holes 504. When the output shaft of the micro displacement actuator 505 extends or retracts, the double tilting connecting shaft 506 is driven, and simultaneously pushes the double tilting platform 501 to tilt through the inner walls of the two elliptical connecting holes 504. This symmetrical arrangement can distribute the driving force evenly on both sides of the double tilting platform 501, which can reduce the additional bending moment caused by eccentric loading, thereby reducing the torsional deformation of the double tilting platform 501 during the tilting process and improving the coaxiality of the tilting motion.

[0068] In one embodiment of the present invention, such as Figures 1 to 5 As shown, the wall of the elliptical connecting hole 504 is precision polished to reduce transmission friction. The elliptical connecting hole 504 addresses the issue of minute axial deformation that occurs when the micro displacement actuator 505 drives the dual tilting stage 501 to tilt. The elliptical connecting hole 504 provides buffer space for deformation, preventing tilting jamming and vibration caused by stress concentration, significantly improving tilting positioning accuracy, and achieving long-term high-precision stable tilting. This meets the requirements of atomic-scale in-situ characterization for tilting accuracy and stability, showing a significant improvement in tilting stability and positioning accuracy compared to existing technologies. Simultaneously, it ensures flexible rotation between the dual tilting connecting shaft 506 and the elliptical connecting hole 504.

[0069] In one embodiment of the present invention, such as Figures 1 to 5 As shown, the double-tilt connecting shaft 506 has a cylindrical structure and is made of hard antimagnetic alloy. The surface of the double-tilt connecting shaft 506 is precision polished. The middle part of the double-tilt connecting shaft 506 is located in the through hole at the front end of the output shaft of the micro displacement actuator 505. Both ends of the double-tilt connecting shaft 506 are located in corresponding elliptical connecting holes 504, using a clearance fit to achieve a movable connection. This ensures that the displacement of the micro displacement actuator 505 can be accurately transmitted to the double-tilt stage 501, while allowing the double-tilt stage 501 to tilt flexibly.

[0070] In one embodiment of the present invention, such as Figures 1 to 5As shown, one end of the rod head 1 is threadedly connected to the sample rod body 2. This threaded connection ensures the rigidity and coaxiality of the connection, reducing relative displacement caused by vibration or external forces during use. Coaxiality provides a consistent baseline for the assembly of subsequent functional components, facilitating disassembly and maintenance. This detachable feature allows for separation when rod head 1 or sample rod body 2 needs replacement or repair, reducing maintenance difficulty. The coaxiality of rod head 1 and sample rod body 2 provides a reference for the assembly of subsequent functional components. This reference reduces assembly stress caused by axial deviation, ensuring that components such as the double-tilting device 5 and magnetic shielding device 3 maintain their predetermined positional relationship after assembly. It also prevents a decrease in tilting accuracy and obstruction of electron beam transmission due to coaxiality deviation. In other words, by controlling the coaxiality within the tolerance range, additional oscillations during tilting can be reduced, while also minimizing obstruction or deviation of the electron beam when passing through the sample area.

[0071] Of course, the connection method between rod head 1 and sample rod body 2 is not limited to this. Welding can also be used. Welding is suitable for scenarios with extremely high requirements for connection rigidity. The integral structure formed by welding can eliminate microscopic gaps at the connection interface, thereby improving torsional stiffness. During welding, it is necessary to avoid welding deformation affecting coaxiality. Alternatively, rod head 1 and sample rod body 2 can also use an interference fit, which is suitable for scenarios where disassembly is not required, avoiding the use of additional fasteners and saving internal space.

[0072] In one embodiment of the present invention, such as Figures 1 to 5 As shown, the miniature displacement actuator 505 is a piezoelectric ceramic actuator (PZT). By selecting a suitable piezoelectric ceramic structure, precise displacement output can be achieved. A through-hole is provided at the front end of the output shaft of the miniature displacement actuator 505, which is used to connect to the dual-axis tilting connection shaft 506. The miniature displacement actuator 505 is connected to the control circuit and receives the drive current output by the control circuit to achieve precise displacement output. The piezoelectric ceramic structure has the advantages of large output force, high displacement accuracy, and fast response speed, which can meet the high-precision control requirements of dual-axis tilting.

[0073] In one embodiment of the present invention, such as Figures 1 to 5As shown, the other end of the rod head 1 is provided with a driver mounting groove 103. The driver mounting groove 103 provides a mounting position for the micro displacement driver 505, thereby reducing the positional displacement of the micro displacement driver 505 during assembly. The shape of the driver mounting groove 103 is adapted to the shape of the micro displacement driver 505, so that the micro displacement driver 505 can fit against the inner wall of the mounting groove after being installed in place. Thus, when the micro displacement driver 505 moves in extension and retraction, the inner wall of the mounting groove limits the micro displacement driver 505, suppressing the shaking of the micro displacement driver 505 in directions other than extension and retraction. The driver mounting groove 103 has an opening, which allows the micro displacement driver 505 to be inserted into the mounting groove from the outside of the rod head 1 through the opening, and to be removed from the opening when maintenance or replacement is required, reducing the difficulty of assembly and disassembly. The micro displacement driver 505 is embedded in the inside of the driver mounting groove 103. The driver mounting groove 103 has a notch on the side near the double tilting device 5, which allows the output shaft of the micro displacement driver 505 to extend out from one side of the mounting groove.

[0074] In one embodiment of the present invention, such as Figures 1 to 5 As shown, the miniature displacement actuator 505 is clearance-fitted with the actuator mounting slot 103. This clearance allows the miniature displacement actuator 505 to have a preset small radial movement space within the actuator mounting slot 103. The actuator mounting slot 103 can axially limit the miniature displacement actuator 505. The radial clearance provided by the clearance allows the miniature displacement actuator 505 to undergo a slight radial wobble during extension and retraction without rigidly pressing against the inner wall of the actuator mounting slot 103. This ensures the precise assembly of the miniature displacement actuator 505. That is, during assembly, there is no need to perform precision grinding on the mating surfaces between the miniature displacement actuator 505 and the actuator mounting slot 103. The clearance and axial limiting are sufficient to keep the miniature displacement actuator 505 in the predetermined working position within the actuator mounting slot 103.

[0075] In one embodiment of the present invention, such as Figures 1 to 5 As shown, the double tilting device 5 also includes a double tilting platform fixing cover 507. The double tilting platform fixing cover 507 has a sheet-like structure and is made of an antimagnetic alloy. The size and shape of the double tilting platform fixing cover 507 are adapted to the size and shape of the opening. The double tilting platform fixing cover 507 covers the opening of the driver mounting slot 103 and is connected to the rod head 1. The double tilting platform fixing cover 507 abuts against the micro displacement driver 505 to limit the micro displacement driver 505.

[0076] In one embodiment of the present invention, such as Figures 1 to 5As shown, the double tilting platform fixing cover 507 is detachably connected to the rod head 1. When maintenance or replacement of the micro displacement actuator 505 is required, the connection between the cover and the rod head 1 is disconnected, and the cover is removed from the rod head 1, exposing one end of the micro displacement actuator 505 through the opening. This allows the micro displacement actuator 505 to be removed from the mounting slot, thereby reducing the difficulty of installing and maintaining the micro displacement actuator 505.

[0077] In one embodiment of the present invention, such as Figures 1 to 5 As shown, the edge of the driver mounting slot 103 is provided with a first threaded hole. In this embodiment, there are four first threaded holes, which are respectively distributed at the four corners of the driver mounting slot 103. Of course, the number of first threaded holes is not limited to this, and can also be three, five, six or more. The double tilting platform fixing cover plate 507 is provided with a first through hole, the number of first through holes is the same as the number of first threaded holes, the position of the first through hole corresponds one-to-one with the position of the first threaded hole, and the first screw 508 in the first through hole is threadedly engaged with the first threaded hole.

[0078] In one embodiment of the present invention, such as Figures 1 to 5 As shown, the specifications of the first screw 508 are the same as those of the second screw 304. The first screw 508 is made of antimagnetic alloy and has a countersunk head design. The first screw 508 is used to fasten the double tilting platform fixing cover plate 507 to the rod head 1 to ensure the axial fixation of the micro displacement actuator 505 and prevent loosening during the driving process.

[0079] In one embodiment of the present invention, such as Figures 1 to 5 As shown, the sample rod body 2, rod head 1, and double tilting device 5 are all made of antimagnetic alloy. The high-permeability magnetic shield 301 is made of high-permeability magnetic material. With its smooth inner wall and central positioning design, it can effectively avoid the generation of additional magnetic interference, protect the intrinsic microstructure of sensitive samples, avoid distortion of characterization results, and ensure the stability of the magnetic shielding effect.

[0080] In one embodiment of the present invention, such as Figures 1 to 5 As shown, the probe head 1 is made of an antimagnetic material to prevent the probe head 1 from being magnetized, thus preventing the introduction of additional magnetic interference and ensuring a non-magnetic environment in the sample area. Along the direction away from the sample probe body 2, the outer diameter of the probe head 1 gradually decreases, that is, the outer diameter of the probe head 1 gradually decreases from the rear end to the front end. This structural design facilitates coaxial fixation with the sample probe body 2, adapts to the pole shoe space, prevents collisions between the sample probe and the pole shoes, and reduces the obstruction of the electron beam by the probe head 1, ensuring that the electron beam can penetrate the sample smoothly.

[0081] In one embodiment of the present invention, such as Figures 1 to 5As shown, the sample rod body 2 adopts a hollow cylindrical structure, which provides installation space for the driving components, control circuit and wires of the double tilting device 5, while reducing the overall weight of the sample rod body 2 and avoiding positioning deviation caused by excessive weight when inserting it into the electron microscope.

[0082] The sample rod body 2 is made of antimagnetic alloy to prevent the sample rod body 2 itself from being magnetized by the strong magnetic field inside the transmission electron microscope, to prevent the sample rod body 2 from becoming a new source of magnetic interference, and to ensure that the non-magnetic environment of the sample area is not affected. The appropriate antimagnetic alloy can be selected according to actual needs.

[0083] The rod head 1 and the sample rod body 2 have internal wire channels. The sample rod body 2 is equipped with an electrical interface 201 and a control circuit. The control circuit is electrically connected to the micro displacement actuator 505 through the wires inside the wire channels. Two piezoelectric ceramic electrical interfaces are used to connect an external driving power supply to power and transmit driving signals to the micro displacement actuator 505 in the double tilting device 5. The control circuit converts the externally input driving signal into a precise driving current. By precisely controlling the magnitude and direction of the driving current, the micro displacement actuator 505 in the double tilting device 5 is driven to produce a small displacement, thereby driving the double tilting stage 501 to achieve precise dual-axis tilting, providing power support for precise control of the sample attitude.

[0084] like Figures 1 to 5 As shown, the atomic-resolution in-situ non-magnetic environment transmission electron microscopy experimental system provided by this invention includes the following installation, debugging, and usage methods: Following the above connection, assemble the rod head 1, sample rod body 2, magnetic shielding device 3, sample mounting device 4, and double tilting device 5, ensuring precise alignment of each component and tightening the screws at each location to enhance stability. Place the sample on the sample support stage of the sample mounting probe 401 and adjust the sample position to ensure it is centered in the magnetic flux absorption cavity. Insert the sample rod into the sample rod interface of a conventional transmission electron microscope and fine-tune the sample rod position using the electron microscope's goniometer stage displacement system to ensure that the magnetic shielding device 3 is aligned with the center of the pole shoe and the direction of electron beam incidence.

[0085] After the sample rod is inserted into the electron microscope, the double-layer high-permeability magnetic screen 301 of the magnetic shielding device 3 actively guides and converges the strong magnetic field lines generated by the objective lens pole shoes. The magnetic field lines are transmitted along the wall of the high-permeability magnetic screen 301, forming a stable and uniform non-magnetic environment in the magnetic flux absorption cavity. The antimagnetic materials of each component avoid introducing additional magnetic interference, ensuring that the intrinsic microstructure of the magnetic field-sensitive sample is not damaged.

[0086] The drive signal is input to the electrical interface 201 by an external drive power supply. The control circuit converts the drive signal into a drive current and transmits the drive current to the micro displacement actuator 505. The micro displacement actuator 505 generates a small displacement, which is transmitted to the double tilt stage 501 through the double tilt connecting shaft 506. This causes the double tilt stage 501 to rotate around the central axis of the rotating shaft, realizing the precise and controllable tilting of the sample. By adjusting the magnitude and direction of the drive current, the tilt angle is precisely controlled, and the sample is adjusted to the optimal observation posture so that the electron beam is incident along the low index crystal plane of the sample.

[0087] With the support of a non-magnetic environment and precise tilting posture, the electron beam successfully penetrates the sample, avoiding magnetic field interference and electron beam obstruction. The transmission electron microscope obtains clear electron diffraction patterns and atomic resolution images, enabling the intrinsic microstructure characterization and in-situ study of magnetic materials, superconducting materials, and other magnetic field-sensitive samples.

[0088] The atomic resolution in-situ non-magnetic environment transmission electron microscope experimental system provided by this invention can be directly adapted to existing conventional electron microscopes without the need to purchase additional special equipment, which can significantly reduce the user's equipment investment costs, and is especially suitable for research institutions, corporate laboratories and other scenarios with limited budgets.

[0089] The atomic resolution in-situ non-magnetic environment transmission electron microscope experimental system provided by this invention adopts a modular design that facilitates disassembly and maintenance, and makes component replacement convenient, which can effectively reduce maintenance costs. At the same time, it does not require modification of the electron microscope, avoiding the high cost of electron microscope modification. Moreover, the structure is reliable and durable, which can further reduce the long-term use costs for users.

[0090] The atomic-resolution in-situ non-magnetic environment transmission electron microscopy experimental system provided by this invention enables one-stop in-situ characterization of sensitive samples without the need for frequent sample rod replacements or equipment parameter adjustments, effectively shortening sample characterization time. Simultaneously, it achieves precise characterization at atomic resolution, helping research institutions accelerate R&D progress in related fields, assisting enterprises in improving product quality testing efficiency, and indirectly creating significant economic benefits.

[0091] Finally, it should be noted that the above embodiments are only for illustrating the present invention and not for limiting the present invention. Although the present invention has been described in detail with reference to the embodiments, those skilled in the art should understand that various combinations, modifications, or equivalent substitutions of the technical solutions of the present invention do not depart from the spirit and scope of the technical solutions of the present invention and should be covered within the scope of the claims of the present invention.

Claims

1. An atomic-resolution in-situ transmission electron microscopy experimental system in a non-magnetic environment, characterized in that, include: Sample rod body (2); Rod head (1), one end of which is connected to the sample rod body (2); A double tilting device (5) is provided at the other end of the rod head (1). The double tilting device (5) includes a double tilting stage (501) and a micro displacement actuator (505). The double tilting stage (501) is located on the side of the micro displacement actuator (505) away from the sample rod body (2). The double tilting stage (501) is rotatably connected to the rod head (1) and movably connected to the micro displacement actuator (505). A magnetic shielding device (3) is provided on the double tilting platform (501). The magnetic shielding device (3) includes multiple high permeability magnetic screens (301). The multiple high permeability magnetic screens (301) are stacked in sequence, and the central holes of the multiple high permeability magnetic screens (301) are connected to form a magnetic flux absorption cavity. The sample mounting device (4) is clamped between two adjacent high-permeability magnetic screens (301). The sample mounting device (4) is provided with a sample carrier stage, which is located inside the magnetic flux absorption cavity. The sample mounting device (4) includes: A sample-mounted probe (401) is clamped between two high-permeability magnetic screens (301). One end of the sample-mounted probe (401) extends to the outside of the two high-permeability magnetic screens (301), and the other end of the sample-mounted probe (401) extends into the magnetic flux absorption cavity. The sample support stage is disposed at the other end of the sample-mounted probe (401). The sample-carrying probe (401) is a slender rod-shaped structure. The sample-carrying probe (401) is used to carry the sample and fix the sample in the center of the magnetic flux absorption cavity.

2. The atomic-resolution in-situ non-magnetic environment transmission electron microscopy experimental system according to claim 1, characterized in that, At least one of the two adjacent high-permeability magnetic screens (301) is provided with a sample probe assembly slot (402) on one side facing each other, and the sample-mounted probe (401) is embedded in the sample probe assembly slot (402).

3. The atomic-resolution in-situ non-magnetic environment transmission electron microscopy experimental system according to claim 2, characterized in that, The two high-permeability magnetic screens (301) are each provided with a sample probe mounting slot (402) on one side facing each other, and the two sample probe mounting slots (402) are symmetrically arranged about the central axis of the sample-mounted probe (401).

4. The atomic-resolution in-situ non-magnetic environment transmission electron microscopy experimental system according to any one of claims 1 to 3, characterized in that, The double tilting platform (501) is provided with a magnetic shield mounting groove (502). One side of the double tilting platform (501) is provided with an opening that communicates with the magnetic shield mounting groove (502), and the other side of the double tilting platform (501) is provided with a through hole that communicates with the magnetic shield mounting groove (502). The magnetic shielding device (3) is embedded inside the magnetic shield mounting groove (502).

5. The atomic-resolution in-situ non-magnetic environment transmission electron microscopy experimental system according to claim 4, characterized in that, The magnetic shielding device (3) further includes: A magnetic shield cover (303) is provided, which covers the opening and is detachably connected to the double tilting platform (501).

6. The atomic-resolution in-situ non-magnetic environment transmission electron microscopy experimental system according to claim 5, characterized in that, The edge of the magnetic screen mounting groove (502) is detachably connected to the magnetic screen cover plate (303).

7. The atomic-resolution in-situ non-magnetic environment transmission electron microscopy experimental system according to claim 5, characterized in that, The magnetic screen mounting slot (502) is provided with a probe limiting slot (503) along its edge. The tail limiting structure of the other end of the sample-mounted probe (401) is embedded in the probe limiting slot (503). The magnetic screen cover (303) is provided with a protrusion at one end near the micro displacement actuator. The protrusion is embedded in the probe limiting slot (503) and abuts against the tail limiting structure of the sample-mounted probe (401).

8. The atomic-resolution in-situ non-magnetic environment transmission electron microscopy experimental system according to any one of claims 1 to 3, characterized in that, The other end of the rod head (1) is provided with a double tilting platform mounting groove (101). The double tilting platform mounting groove (101) has two opposing side walls. The side walls extend along the length direction of the rod head (1). Both side walls are provided with double tilting platform limiting holes (102). The double tilting platform (501) is provided in the double tilting platform mounting groove (101). Both sides of the double tilting platform (501) are provided with rotating shafts. The rotating shafts are rotatably engaged with the double tilting platform limiting holes (102).

9. The atomic-resolution in-situ non-magnetic environment transmission electron microscopy experimental system according to any one of claims 1 to 3, characterized in that, The sample rod body (2), the rod head (1), and the double tilting device (5) are all made of antimagnetic alloy.

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