Multifunctional Sample Stage for In-situ Transmission Electron Microscopy and Atom Probe

Abstract

Embodiments of the present invention relate to the technical field of micro-area microscopic analysis of materials, and specifically provide a multifunctional sample stage for transmission electron microscopy (TEM) and in-situ atom probe tomography (APT) testing. The sample stage includes: a support stage, which includes a substrate having a first-stage stepped layer and a second-stage stepped layer; a metal pressing sheet, which can be fixed to the first-stage stepped layer on one hand, and can abut against a silicon wafer carrying a sample provided on the second-stage stepped layer on the other hand; a sample mounting stage assembly, which can be disposed on the second-stage stepped layer, and a metal mesh carrying a sample can be fixed to the sample mounting stage assembly. With such a configuration, the sample stage of the present invention can not only meet the requirements of conventional APT analysis, but also meet the requirements of TEM-APT in-situ analysis. In addition, the present invention also has the advantages of being easy to disassemble and being able to be quickly transferred between TEM and APT instruments without damaging the sample.

Description

Technical Field

[0001] The present invention relates to the technical field of micro-area microscopic analysis of materials, and specifically provides a multifunctional sample stage for in-situ testing of a transmission electron microscope and an atom probe. Background Art

[0002] Atom probe tomography microscope (abbreviated as atom probe, APT) is an advanced instrument with a spatial resolution of nearly atomic scale (~0.2 nm) and a detection sensitivity of ppm level. Through it, the types of elements and isotope information in materials can be confirmed, and the three-dimensional (3D) spatial distribution of different elements can be reconstructed. Currently, the application of APT has been extended from the field of highly conductive materials (such as metals, alloys, etc.) to the fields of semiconductors, inorganic materials, biological materials, bones, and geological minerals, etc., for effectively revealing the spatial distribution of light and heavy atoms, solute clusters, nano-precipitates, and dislocation cores in materials. Although the application of APT is relatively extensive, only the composition information of materials can be obtained through it, and the microstructural and crystallographic information of materials cannot be obtained. Therefore, it is difficult to establish the relationship between composition and crystallographic structure and material properties (such as mechanical, optical, electrical, magnetic, etc.) only based on APT, thus affecting the design and development of materials.

[0003] Therefore, in recent years, researchers have developed a technology for in-situ testing of a transmission electron microscope (abbreviated as transmission electron microscope, TEM) and an atom probe. Since the transmission electron microscope can analyze the crystallographic structure and microstructure of materials, in this way, by performing TEM and in-situ atom probe (TEM-APT) tests on the same sample, information such as the full-range morphology - major composition - crystal structure - element valence state - atomic occupancy - three-dimensional spatial distribution of elements of the material can be obtained. Based on this, it is expected to reveal the relationship between the composition, crystallographic structure, and material properties of the material based on this technology.

[0004] The atom probe test requires the sample to be in a needle-like structure (with a diameter of about 100 nm). To adapt to this requirement, researchers at home and abroad have mainly developed two APT test schemes.

[0005] Solution 1: It is mainly used for most conventional APT tests. The device of this solution mainly includes a T-shaped sample stage dedicated to APT and a silicon wafer for carrying needle-shaped samples. The corresponding test method is roughly as follows: Use the focused ion beam technology (FIB) to bond the prepared needle-shaped sample to the silicon pillar. The silicon pillars are arranged in an array on the surface of the silicon wafer (exemplarily, the length of the silicon wafer is 7 mm and the width is 3 mm). When performing APT tests on the sample, install the silicon wafer on the T-shaped sample stage. In this way, APT analysis of multiple needle-shaped samples can be achieved at one time. In addition, as mentioned in the Chinese invention patent application (CN110987995A), the needle-shaped structure is prepared by electro-polishing a metal material and used for the conventional test of APT.

[0006] Solution 2: It is mainly used for the in-situ TEM-APT test of samples. There are few research reports on this solution. The device used mainly includes a separable T-shaped sample stage and a crescent-shaped metal grid (such as Zschiesche H.et al., Ultramicroscopy, 2019, 206: 112807; Povstugar Ivan et al., Microscopy and Microanalysis, 2019, 1–10; Chinese invention patent CN110987995A). The corresponding test method is roughly as follows: First, use FIB to bond the prepared needle-shaped sample to the crescent-shaped metal grid, and then directly place the crescent-shaped metal grid on the TEM sample rod for TEM experiments. Second, after the TEM experiment is completed, fix the crescent-shaped metal grid carrying the needle-shaped structure sample to the separable T-shaped stage, and install the separable T-shaped stage into the APT instrument for APT three-dimensional reconstruction experiments. Based on the above two-step test process, in-situ characterization of the same sample on different instruments can be achieved.

[0007] It can be seen that the sample stages of the above two schemes can be used for independent test requirements. However, with the diversified development of test requirements and the need to reduce costs and increase efficiency, in order to meet new technical requirements, the development of a sample stage device that can simultaneously achieve conventional APT testing and TEM-APT in-situ testing has become extremely urgent. This is because: Since the APT sample stage is a precision device, assuming that the above two sample stage devices are developed simultaneously to meet conventional APT testing and TEM-APT testing, the cost is extremely high. More importantly, when the aforementioned clutch-type T-shaped sample stage is in the closed state, its contact surface is linear, which will make it difficult to stably install and unload the ultra-thin and fragile metal support grid (with a thickness of only 30 μm), and as a result, the APT needle-shaped sample will be bent and damaged. Finally, the sample holder of the sample stage mentioned in the Chinese invention patent (CN110987995A) cannot install the silicon wafer used to support the needle-shaped sample in conventional APT testing, and the heights of the APT sample supported by the crescent-shaped metal support grid and the APT sample clamped by the copper tube (prepared by electro-chemical polishing method) are inconsistent, resulting in the inability to safely conduct APT experiments. Summary of the Invention

[0008] The present invention provides a multi-functional sample stage that can not only achieve conventional APT testing but also achieve TEM-APT in-situ testing, in order to realize the compositional reconstruction analysis and in-situ microscopic analysis of multiple regions of the material based on this sample stage, so as to reveal the relationship between the composition, crystallographic structure and material properties of the material.

[0009] In view of this, the present invention provides a multi-functional sample stage for transmission electron microscopy and atom probe in-situ testing. The sample stage includes: a support stage, which includes a base body having a first-stage stepped layer and a second-stage stepped layer; a metal pressing piece, which can be fixed to the first-stage stepped layer on the one hand, and can abut against the silicon wafer carrying the sample provided on the second-stage stepped layer on the other hand; a sample carrying stage assembly, which can be arranged on the second-stage stepped layer, and the metal support grid carrying the sample can be fixed to the sample carrying stage assembly.

[0010] With such a configuration, it is possible to achieve conventional APT analysis and TEM-APT in-situ analysis based on the sample stage of the present invention.

[0011] For the above-mentioned transmission electron microscope and in-situ atomic probe testing multi-functional sample stage, in a possible implementation manner, the sample mounting stage assembly includes: a concave sample stage on which at least one groove mounting position is formed, and the concave sample stage has a vertical surface at a position corresponding to the groove mounting position, and a metal mesh carrying a sample can be placed at a position corresponding to the vertical surface of the groove mounting position; a convex fixing stage on which a protruding end that can be adapted to the groove mounting position is formed, so that: by inserting the protruding end into the corresponding groove mounting position, the metal mesh carrying the sample is clamped between the protruding end and the vertical surface.

[0012] With such a configuration, it is possible to ensure that the needle-shaped sample carried on the metal mesh can be reliably in a state to be tested.

[0013] For the above-mentioned transmission electron microscope and in-situ atomic probe testing multi-functional sample stage, in a possible implementation manner, the concave sample stage and the convex fixing stage are fixedly connected by means of a second fastener.

[0014] With such a configuration, it is possible to ensure the reliability of the sample mounting stage assembly.

[0015] For the above-mentioned transmission electron microscope and in-situ atomic probe testing multi-functional sample stage, in a possible implementation manner, the concave sample stage and / or the convex fixing stage and the second-level stepped layer are fixedly connected by means of a third fastener.

[0016] With such a configuration, it is possible to ensure the reliability of the sample mounting stage assembly constituting the sample stage.

[0017] It can be understood that those skilled in the art can determine the structural form, number, and distribution manner of the second / third fasteners on the sample mounting stage assembly according to actual needs.

[0018] For the above-mentioned transmission electron microscope and in-situ atomic probe testing multi-functional sample stage, in a possible implementation manner, the cross-section of the groove mounting position in the vertical direction is an inverted semi-circle or an isosceles trapezoid, wherein the waist of the isosceles trapezoid is an arc line.

[0019] With such a configuration, it is possible to reliably fix the sample carried on the metal mesh to the sample mounting stage assembly.

[0020] For the above-mentioned transmission electron microscope and in-situ atomic probe testing multi-functional sample stage, in a possible implementation manner, the metal pressing piece includes a first pressing part and a second pressing part, wherein the first pressing part is arranged on the first-level stepped layer, and the end of the second pressing part close to the silicon wafer is lower than the end close to the first pressing part.

[0021] With such a configuration, it is possible to reliably press the silicon wafer carrying the sample by the second pressing part. Those skilled in the art can determine the structural forms of the first / second pressing parts and the way they form a metal pressing part according to actual needs. For example, their structures can be the same or different, and they can be fixedly connected or integrally formed with each other, etc.

[0022] For the above-mentioned transmission electron microscope and in-situ atomic probe test multi-functional sample stage, in a possible implementation manner, the second pressing part includes an inclined surface part and / or a curved surface part.

[0023] With such a configuration, a possible structural form of the second pressing part is given.

[0024] For the above-mentioned transmission electron microscope and in-situ atomic probe test multi-functional sample stage, in a possible implementation manner, the first pressing part is fixed to the first-level stepped layer by means of a first fastener; and / or the support stage is provided with a limiting structure at a position corresponding to the first-level stepped layer.

[0025] With such a configuration, it is possible to ensure the reliability of the position of the first pressing part on the first-level stepped layer through the limiting structure. In addition, similar to the aforementioned second / third fasteners, those skilled in the art can determine the structural form, number, and distribution manner of the first fastener on the first pressing part according to actual needs.

[0026] For the above-mentioned transmission electron microscope and in-situ atomic probe test multi-functional sample stage, in a possible implementation manner, the sample stage includes a bottom column, the bottom column is arranged at the bottom of the support stage, and the bottom column is used to match the sample holder of the APT instrument.

[0027] With such a configuration, a possible structural form of the base of the sample stage is given. For example, the support stage and the bottom column form a generally T-shaped structure, which can be called a T-shaped support stage.

[0028] For the above-mentioned transmission electron microscope and in-situ atomic probe test multi-functional sample stage, in a possible implementation manner, the bottom column includes a first bottom column section and a second bottom column section arranged from top to bottom. Among them, the radial dimension of the first bottom column section is larger than that of the second bottom column section; and / or the cross-section of the second bottom column section is circular or D-shaped.

[0029] With such a configuration, a possible structural form of the bottom column is given. BRIEF DESCRIPTION OF THE DRAWINGS

[0030] The following describes the preferred embodiments of the present invention in conjunction with the drawings. In the drawings:

[0031] Figure 1Schematic structural diagram of the support stage in the transmission electron microscope and atomic probe in-situ testing multi-functional sample stage according to an embodiment of the present invention;

[0032] Figure 2 Schematic structural diagram of the metal pressing sheet in the transmission electron microscope and atomic probe in-situ testing multi-functional sample stage according to an embodiment of the present invention;

[0033] Figure 3 Schematic assembly diagram of the support stage, metal pressing sheet and loaded silicon wafer in the transmission electron microscope and atomic probe in-situ testing multi-functional sample stage according to an embodiment of the present invention;

[0034] Figure 4 Schematic structural diagram of the concave sample stage in the carrier stage assembly of the transmission electron microscope and atomic probe in-situ testing multi-functional sample stage according to an embodiment of the present invention;

[0035] Figure 5 Schematic structural diagram of the convex sample stage in the carrier stage assembly of the transmission electron microscope and atomic probe in-situ testing multi-functional sample stage according to an embodiment of the present invention;

[0036] Figure 6 Schematic assembly diagram of the transmission electron microscope and atomic probe in-situ testing multi-functional sample stage when installing a metal carrier mesh;

[0037] Figure 7 Electron microscope image of the silicon wafer in the transmission electron microscope and atomic probe in-situ testing multi-functional sample stage according to an embodiment of the present invention;

[0038] Figure 8 is Figure 7 Enlarged schematic diagram of local area A in;

[0039] Figure 9 Is an electron microscope image of the metal carrier mesh in the transmission electron microscope and atomic probe in-situ testing multi-functional sample stage according to an embodiment of the present invention; and

[0040] Figure 10 is Figure 9 Enlarged schematic diagram of local area B in.

[0041] List of reference numerals:

[0042] 100, Transmission electron microscope and atomic probe in-situ testing multi-functional sample stage;

[0043] 1, Support stage;

[0044] 11, First-level stepped layer; 12, Second-level stepped layer; 13, Limiting structure;

[0045] 2, Metal pressing sheet;

[0046] 21, First pressing part; 22, Second pressing part;

[0047] 3. Sample mounting table assembly;

[0048] 31. Concave sample table;

[0049] 311. Groove mounting position; 312. Vertical surface;

[0050] 32. Convex fixing table;

[0051] 321. Protruding end;

[0052] 41. First fastener; 42. Second fastener;

[0053] 51. First connection hole; 52. Second connection hole; 53. Third connection hole; 54. Fourth connection hole; 55. Fifth connection hole; 56. Sixth connection hole;

[0054] 6. Bottom column;

[0055] 61. First bottom column section;

[0056] 62. Second bottom column section; 621. Positioning surface;

[0057] 200. Silicon wafer; 201. Silicon column;

[0058] 300. Metal carrier mesh; 301. Comb-shaped teeth;

[0059] 401. First sample; 402. Second sample. Detailed implementation manners

[0060] The preferred implementation manners of the present invention will be described below with reference to the accompanying drawings. Those skilled in the art should understand that these implementation manners are only used to explain the technical principle of the present invention and are not intended to limit the protection scope of the present invention.

[0061] It should be noted that in the description of the present invention, the terms indicating the direction or positional relationship such as "center", "upper", "lower", "left", "right", "vertical", "horizontal", "inner", "outer", etc. are based on the direction or positional relationship shown in the drawings. This is only for the convenience of description and does not indicate or imply that the device or element must have a specific orientation, be constructed and operated in a specific orientation. Therefore, it cannot be understood as a limitation to the present invention. In addition, the terms "first" and "second" are only used for descriptive purposes and cannot be understood as indicating or implying relative importance.

[0062] In addition, it should be noted that in the description of the present invention, unless otherwise clearly specified and defined, the terms "installation", "setting", and "connection" should be understood in a broad sense. For example, it can be a fixed connection, a detachable connection, or an integral connection; it can be directly connected, indirectly connected through an intermediate medium, or the internal communication of two components. For those skilled in the art, the specific meanings of the above terms in the present invention can be understood according to specific circumstances.

[0063] In addition, to better illustrate the present invention, numerous specific details are given in the following specific embodiments. Those skilled in the art should understand that the present invention can still be implemented without some specific details. In some instances, the principles of conventional APT tests and TEM-APT in-situ tests well-known to those skilled in the art are not described in detail to highlight the main idea of the present invention.

[0064] Mainly referring to Figures 1 to 6 , in a possible embodiment, the transmission electron microscope and atom probe in-situ test multi-functional sample stage 100 mainly includes a support stage 1, a metal pressing sheet 2, and a sample mounting stage assembly 3. Among them, the support stage 1 includes a base body, and the base body has a first-stage stepped layer 11 and a second-stage stepped layer 12. The height of the first-stage stepped layer 11 is greater than that of the second-stage stepped layer 12. A silicon wafer 200 carrying a first sample 401 for performing a conventional APT test can be reliably fixed to the support stage 1 through the cooperation of the metal pressing sheet 2 with the first / second-stage stepped layers. The sample mounting stage assembly 3 can be fixed to the position of the support stage 1 corresponding to the second-stage stepped layer 12, and a metal mesh 300 carrying a second sample 402 for performing TEM-APT in-situ test can be in a stable test state through the mounting stage assembly 3.

[0065] Mainly referring to Figures 1 to 3 , in a possible embodiment, the metal pressing sheet 2 includes a first pressing part 21 (such as a head) and a second pressing part 22 (such as a tail). Among them, the first pressing part 21 is arranged at the position of the support stage 1 corresponding to the first-stage stepped layer 11, and the end of the second pressing part 22 close to the silicon wafer ( Figure 1 the right end in Figure 1 ) is lower than the end close to the first pressing part (

[0066] the left end in

[0066] ), so as to reliably press the silicon wafer 200 carrying the first sample through the second pressing part. For example, the second pressing part can be an inclined surface, a curved surface, and a combination of the two, etc. In this example, the second pressing part is approximately an inclined surface.In a possible implementation, the support platform 1 is provided with a limiting structure 13 at a position corresponding to the first-level stepped layer 11. When the first pressing part 21 is disposed on the first-level stepped layer, the reliability of its position can be ensured through the limiting structure. As in this example, the limiting structure includes two limiting plates disposed on the first-level stepped layer 11 (disposed on both sides in the width direction of the silicon wafer); the first pressing part 21 is clamped between the two limiting plates in the assembled state. On the basis of being limited by the limiting structure, the metal pressing sheet can be fixed to the support platform 1 through a first fastener 41 such as a screw. As the metal pressing sheet 2 is provided with a first connection hole 51 (such as including a pair, such as through holes), and the support platform is provided with a second connection hole 52 (such as including a pair, such as blind holes or other limiting holes) at a position corresponding to the first-level stepped layer 11. Through the cooperation of the screw with the through hole / limiting hole, the metal pressing sheet can tightly press the silicon wafer 200, thereby reliably fixing the silicon wafer to the support platform 1.

[0067] Obviously, the combination of the two limiting plates is only an exemplary description of the limiting structure. Those skilled in the art can determine the specific form of the limiting structure according to actual needs, such as including but not limited to replacing the limiting plates with structures having grooves / protrusions, adding a limiting structure such as a baffle / stop block between the two limiting structures (the position where the head of the silicon wafer abuts). Also, the screw is only an exemplary description of the first fastener. For example, the fixed connection between the metal pressing sheet and the support platform can also be achieved by the interference fit of a tapered pin with the first / second connection holes.

[0068] Mainly referring to Figures 4 to 6 , in a possible implementation, the loading platform assembly 3 includes a concave sample stage 31 and a convex fixing stage 32 that cooperate with each other. Among them, at least one groove mounting position 311 (such as a side-opening groove) is formed on the concave sample stage 31. The concave sample stage 31 has a vertical surface 312 at a position corresponding to the groove mounting position 311. The metal carrier mesh 300 carrying the second sample 402 can be placed at a position corresponding to the vertical surface 312 of the groove mounting position 311. A protruding end 321 that can be adapted to the groove mounting position 311 is formed on the convex fixing stage 32. By inserting the protruding end into the corresponding groove mounting position and abutting against the metal carrier mesh, the metal carrier mesh can be reliably clamped between the protruding end and the vertical surface and thus be reliably in a state to be tested.

[0069] In a possible implementation, the concave sample stage 31 and the convex fixing stage 32 in the loading platform assembly 3 are connected to each other through a second fastener 42 such as a screw, thereby forming a combined body. As in this example, a third connection hole 53 (one) and a fourth connection hole 54 corresponding to the screw are respectively provided on the concave sample stage 31 and the convex fixing stage 32.

[0070] In a possible implementation, when the assembly is placed at the position of the support platform 1 corresponding to the second-level stepped layer 12, the assembly can be fixedly connected to the support platform 1 by means of a third fastener (not shown) such as a screw. For example, a pair of fifth connection holes 55 and sixth connection holes 56 are respectively provided on the support platform 1 and the concave sample stage 31, and the screw penetrates upward from the bottom of the support platform 1 into the fifth connection hole 55 and the sixth connection hole 56.

[0071] Obviously, the structural form of the aforementioned fastener, its matching method with the corresponding connection hole, the structural form / number / distribution method of the connection hole, etc. are all exemplary descriptions. Those skilled in the art can flexibly select according to actual needs. For example, the fastener can also be a pin, a bolt, a stud bolt, etc. When the assembly is connected to the support platform 1, the connection holes can be respectively provided on the concave sample stage and the convex fixing platform, or only provided on the convex fixing platform, etc.

[0072] In a possible implementation, the transmission electron microscope and the in-situ atomic probe tomography multifunctional sample stage 100 are provided with bottom columns 6 at the bottom of the support platform 1. In this example, the bottom column 6 includes a first bottom column section 61 and a second bottom column section 62 from top to bottom. Among them, the radial dimension of the first bottom column section 61 is larger, which is mainly used to enhance the stability of the support platform 1 when it is fixed to the sample holder, so as to realize the safe testing of the APT sample. The radial dimension of the second bottom column section 62 is smaller, which is mainly used to connect with the sample holder of the APT instrument.

[0073] In a possible implementation, a positioning surface 621 can be machined on the second bottom column section 62, which is equivalent to transforming the cylindrical structure into a columnar structure with a roughly D-shaped cross-section. In this way, if the sample holder of the APT instrument is equipped with a positioning pin, the directional fixation between the second bottom column section and the sample holder of the APT instrument can be realized by means of the cooperation between the positioning pin and the positioning surface of the second bottom column section.

[0074] Obviously, the above structure is only an exemplary description of the bottom column. Those skilled in the art can flexibly select the structural form of the base according to actual needs. For example, the base only includes the second bottom column section, and the fixation between the two is achieved by other means. Exemplarily, holes are respectively provided on the sample holder and the second bottom column section, and the fixation between the two is realized by the cooperation of the fastener and the two holes.

[0075] I. Conventional APT testing

[0076] Mainly referring to Figure 7 and Figure 8 , a plurality of silicon pillars 201 are arranged on the surface of the silicon wafer 200 in an array manner, and the first sample (needle-shaped APT sample) 401 prepared by FIB is arranged at the tip of the silicon pillar 201.

[0077] When using the above-mentioned transmission electron microscope and in-situ testing multi-functional sample stage 100 for conventional APT testing, the testing method mainly includes the following steps:

[0078] First, place the silicon wafer 200 carrying the first sample 401 (APT needle-shaped sample) on the second-level stepped layer 12 of the support stage 1;

[0079] Then, place the metal pressing sheet 2 on the first-level stepped layer 11 of the support stage 1. At this time, the head of the metal pressing sheet is clamped between two limiting structures;

[0080] Finally, use a first fastener such as a screw to fix the metal pressing sheet to the support stage, so that the metal pressing sheet 2 can tightly press the silicon wafer 200, thereby reliably fixing the silicon wafer 200 to the support stage 1.

[0081] At the beginning of the APT test, insert the second bottom column section 62 into the sample holder of the APT, and fix the support stage 1 to the sample holder through the cooperation between the positioning pin configured on the sample holder and the positioning surface 621 on the second-level bottom column.

[0082] II. TEM-APT in-situ testing

[0083] Mainly refer to Figure 9 and Figure 10 , a plurality of comb-shaped teeth 301 are provided on the metal support grid 300, and the second sample (needle-shaped sample) 402 prepared by FIB is bonded to the end of the comb-shaped tooth 301.

[0084] When using the above-mentioned transmission electron microscope and in-situ testing multi-functional sample stage 100 for TEM-APT in-situ testing, first, the microscopic structure of the needle-shaped sample prepared by FIB can be analyzed by TEM, then the sample is taken out and transferred to the APT instrument for three-dimensional reconstruction and characterization of elements, and finally, the transmission electron microscope results and atomic probe data are matched to obtain comprehensive morphology, crystal structure, chemical composition, and atomic occurrence state information of the same position of the sample. Specifically, the steps of using the sample stage for TEM-APT in-situ testing mainly include:

[0085] First, place the concave sample stage 31 on the second-level stepped layer 12 of the support stage 1, and use a third fastener (not shown) such as a screw to fix the concave sample stage 31 to the support stage 1;

[0086] Then, place the metal support grid 300 bonded with the second sample 402 vertically in the groove installation position 311 of the concave sample stage 31;

[0087] Finally, place the convex fixing platform 32 on the second-step layer 12 of the support platform 1, cooperate it with the concave sample platform 31, and then fix and connect the two with a second fastener such as a screw. In the fixed state, the protruding end 321 on the convex fixing platform 32 extends into the groove installation position 311 of the concave sample platform 31 and thus abuts against the metal carrier grid 300 located at the vertical surface 312.

[0088] Among them, when used for APT testing, insert the support platform equipped with the concave sample platform, convex fixing platform and metal carrier grid into the base of the APT for experiments.

[0089] In this example, the groove installation positions 311 on the concave sample platform 31 include two, and the cross-section of the groove installation position along the vertical direction is a part of a semi-circle (such as corresponding to the cross-section of a frustum of a cone). For example, the diameter of the semi-circle is 3 mm. Correspondingly, the protruding ends 321 on the convex fixing platform 32 include two, and the diameter is slightly smaller than the groove installation position (such as also 2.98 mm) to ensure that the concave sample platform 31 and the convex fixing platform 32 can be smoothly matched. Obviously, this is only an exemplary description of the carrier platform assembly. Those skilled in the art can determine the number, relative position, cross-sectional shape, etc. of the groove installation position / protruding end according to actual needs. For example, the cross-section of the groove installation position / protruding end can be an isosceles trapezoid, a semi-circle, etc.

[0090] It can be seen that in the preferred embodiment of the present invention, on the one hand, the transmission electron microscope and the atomic probe in-situ test multi-functional sample platform can place the silicon wafer carrying the needle-shaped sample, and on this basis, realize the conventional APT test of the sample. Based on the conventional APT test, by using the silicon wafer to carry more needle-shaped samples, the spatial composition reconstruction information of the material in multiple regions can be obtained. On the other hand, it can place the metal carrier grid carrying the needle-shaped sample, and on this basis, realize the TEM-APT in-situ analysis of the sample. Based on the TEM-APT in-situ analysis, the comprehensive morphology image, crystal structure, atomic occupancy, element valence state, main element composition and three-dimensional spatial distribution information of the material can be obtained. In this way, by introducing a sample platform device, the test requirements corresponding to two functions can be completed, effectively reducing the cost. In addition, the multi-functional sample platform of the present invention also has the advantages of being easy to fix / detach the metal carrier grid and enabling the sample to be stably transferred between the TEM and APT instruments. That is, it can effectively avoid the damage of relatively fragile needle-shaped samples and has the advantages of simple operation and easy disassembly.

[0091] So far, the technical solution of the present invention has been described in connection with the preferred embodiments shown in the accompanying drawings. However, those skilled in the art can easily understand that the protection scope of the present invention is obviously not limited to these specific embodiments. Without departing from the principle of the present invention, those skilled in the art can make equivalent changes or substitutions to the relevant technical features, and the technical solutions after these changes or substitutions will fall within the protection scope of the present invention.

Claims

1. A transmission electron microscope and an in-situ testing multi-functional sample stage for atom probe, characterized in that, The sample stage includes: A support stage, which includes a base body having a first - level stepped layer and a second - level stepped layer; A metal pressing sheet, one side of which can be fixed to the first - level stepped layer, and the other side of the metal pressing sheet can abut against a silicon wafer carrying a sample and arranged on the second - level stepped layer; and A sample - carrying stage assembly, which can be arranged on the second - level stepped layer, and a metal grid carrying a sample can be fixed to the sample - carrying stage assembly; Wherein, the sample - carrying stage assembly includes: A concave - type sample stage, on which at least one groove mounting position is formed, and the concave - type sample stage has a vertical surface at a position corresponding to the groove mounting position, and a metal grid carrying a sample can be placed at the groove mounting position and at a position corresponding to the vertical surface; and A convex - type fixing stage, on which a protruding end that can be adapted to the groove mounting position is formed, so that: By inserting the protruding end into the groove mounting position, and thus clamping the metal grid carrying a sample between the protruding end and the vertical surface.

2. The transmission electron microscope and in-situ atomic probe test multi-functional sample stage according to claim 1, characterized in that, The concave - type sample stage and the convex - type fixing stage are fixedly connected by means of a second fastener.

3. The transmission electron microscope and in-situ atomic probe test multi-functional sample stage according to claim 1 or 2, characterized in that, The concave - type sample stage and / or the convex - type fixing stage and the second - level stepped layer are fixedly connected by means of a third fastener.

4. The transmission electron microscope and in-situ atomic probe test multi-functional sample stage according to claim 1, wherein The cross - section of the groove mounting position in the vertical direction is an inverted semi - circle or an isosceles trapezoid, Wherein, the waist of the isosceles trapezoid is an arc line.

5. The transmission electron microscope and in-situ atomic probe test multi-functional sample stage according to claim 1, characterized in that, The metal pressing sheet includes a first pressing - sheet part and a second pressing - sheet part, Wherein, the first pressing - sheet part is arranged on the first - level stepped layer, and the end of the second pressing - sheet part close to the silicon wafer is lower than its end close to the first pressing - sheet part.

6. The transmission electron microscope and in-situ atomic probe testing multi-functional sample stage according to claim 5, characterized in that, The second pressing - sheet part includes an inclined - surface part and / or a curved - surface part.

7. The transmission electron microscope and in-situ atomic probe test multi-functional sample stage according to claim 6, characterized in that, The first pressing - sheet part is fixed to the first - level stepped layer by means of a first fastener; and / or The support stage is provided with a limiting structure at a position corresponding to the first - level stepped layer.

8. The transmission electron microscope and in-situ atomic probe test multi-functional sample stage according to claim 1, characterized in that The sample stage includes a bottom column, the bottom column is arranged at the bottom of the support stage, and the bottom column is used to match the sample holder of the APT instrument.

9. The transmission electron microscope and in-situ atomic probe testing multi-functional sample stage according to claim 8, characterized in that, The bottom column includes a first bottom - column section and a second bottom - column section arranged from top to bottom, Wherein, the radial dimension of the first bottom - column section is larger than that of the second bottom - column section; and / or The cross - section of the second bottom - column section is circular or D - shaped.

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