Multifunctional sample table for in-situ test of transmission electron microscope and atomic probe

Abstract

The embodiment of the invention relates to the technical field of micro-area microscopic analysis of materials, and particularly provides a transmission electron microscope (TEM) and atomic probe in-situ (APT) test multifunctional sample stage, which comprises: a support stage, which comprises a substrate having a first step layer and a second step layer; the first side of the metal pressing sheet can be fixed to the first-stage step layer, and the second side of the metal pressing sheet can abut against a silicon wafer which is arranged on the second-stage step layer and carries a sample; the sample carrying table assembly can be arranged on the second-stage step layer, and a metal carrying net for carrying a sample can be fixed to the sample carrying table assembly. Through the structure, the sample table disclosed by the invention not only can meet the conventional APT analysis requirement, but also can meet the TEM-APT in-situ analysis requirement. In addition, the device also has the advantages that the device is easy to disassemble and can be quickly transferred between a TEM instrument and an APT instrument without damaging a sample.

Description

Technical Field

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

[0002] Atom probe tomography (abbreviated as atom probe, APT) is an advanced instrument with near-atomic scale spatial resolution (~0.2nm) and ppm-level detection sensitivity. It can confirm the element types and isotope information in the material and reconstruct the three-dimensional (3D) spatial distribution of different elements. At present, the application of APT has expanded from the field of high-conductivity materials (metals, alloys, etc.) to semiconductors, inorganic materials, biomaterials, bones, geological minerals and other fields. It is used to effectively reveal the spatial distribution of light and heavy atoms, solute clusters, nano-precipitated phases and dislocation cores in materials. Although APT is widely used, it can only obtain the composition information of the material, but not the microstructure and crystallographic information of the material. Therefore, it is difficult to establish the relationship between the composition and crystallographic structure and material properties (such as mechanics, optics, electricity, magnetism, etc.) based on APT alone, which affects the design and development of materials.

[0003] Therefore, in recent years, researchers have developed a technology of transmission electron microscopy (TEM) and atom probe in situ testing. Since the transmission electron microscope can analyze the crystallographic structure and microstructure of the material, by performing transmission electron microscopy and atom probe in situ (TEM-APT) testing on the same sample, the material's comprehensive morphology - major components - crystal structure - element valence - atomic occupancy - three-dimensional spatial distribution of elements and other information can be obtained. Based on this, it is expected that this technology can reveal the relationship between the composition, crystallographic structure and material properties of the material.

[0004] The atomic probe test requires the sample to be a needle-like structure (about 100nm in diameter). In response 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-type sample stage based on APT and a silicon wafer for carrying needle-shaped samples. For example, the corresponding test method is roughly as follows: using focused ion beam technology (FIB) to bond the prepared needle-shaped samples to silicon pillars, and 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 the sample is subjected to APT testing, the silicon wafer is mounted on the T-type 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), metal materials are electrolyzed by electrolytic polishing to prepare needle-shaped structures and use them for conventional APT testing.

[0006] Scheme 2: It is mainly used for TEM-APT in-situ testing of samples. There are few research reports on this scheme. The devices used mainly include a clutch T-type 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 to perform a TEM experiment; secondly, after the TEM experiment is completed, fix the crescent-shaped metal grid carrying the needle-shaped structure sample to the clutch T-type stage, and install the clutch T-type stage into the APT instrument to perform an APT three-dimensional reconstruction experiment. Based on the above two step-by-step test processes, the in-situ characterization of the same sample in different instruments is achieved.

[0007] It can be seen that the sample stages of the above two schemes can be used for independent testing needs. However, with the diversified development of testing needs and the need to reduce costs and increase efficiency, in order to meet new technical needs, the research and development of sample stage devices that can simultaneously realize 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, it is extremely costly to develop the above two sample stage devices at the same time to meet conventional APT testing and TEM-APT testing. More importantly, when the aforementioned clutch T-type sample stage is in a closed state, its contact surface is linear, which will make the ultra-thin and fragile metal grid (thickness is only 30μm) difficult to install and unload smoothly, and thus cause the APT needle-shaped sample to be bent and damaged. Finally, the sample holder of the sample stage mentioned in the Chinese invention patent invention (CN110987995A) cannot accommodate the silicon wafer used to support needle-shaped samples in conventional APT testing, and the heights of the APT sample supported by the crescent-shaped metal grid and the APT sample clamped by the copper tube (produced by electrochemical polishing) are inconsistent, making it impossible to conduct APT experiments safely. Summary of the invention

[0008] The present invention provides a multifunctional sample stage that can realize both conventional APT testing and TEM-APT in-situ testing, so as to realize multiple regional composition reconstruction analysis and in-situ microscopic analysis of materials based on the sample stage, thereby revealing the relationship between the composition, crystallographic structure and material properties of the material.

[0009] In view of this, the present invention provides a multifunctional sample stage for in-situ testing of a transmission electron microscope and an atomic probe, the sample stage comprising: a support platform, which includes a substrate, the substrate having a first-level stepped layer and a second-level stepped layer; a metal pressing plate, a first aspect of which can be fixed to the first-level stepped layer, and a second aspect of the metal pressing plate can abut against a silicon wafer carrying a sample arranged on the second-level stepped layer; a sample carrying stage assembly, which can be arranged on the second-level stepped layer, and a metal carrier grid carrying a sample can be fixed to the sample carrying stage assembly.

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

[0011] For the above-mentioned multifunctional sample stage for in-situ testing of transmission electron microscope and atomic probe, in a possible embodiment, the sample carrying stage assembly includes: a concave sample stage, on which at least one groove mounting position is formed, the concave sample stage has a vertical surface at a position corresponding to the groove mounting position, and the metal carrier mesh carrying the sample can be placed at the position of the groove mounting position corresponding to the vertical surface; a convex fixing stage, on which a protruding end that can be adapted to the groove mounting position is formed, so as to: extend the protruding end into the corresponding groove mounting position and thereby clamp the metal carrier mesh carrying the sample between the protruding end and the vertical surface.

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

[0013] Regarding the above-mentioned multifunctional sample stage for transmission electron microscopy and atom probe in-situ testing, 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 multifunctional sample stage for transmission electron microscopy and atom probe in-situ testing, in a possible implementation manner, the concave sample stage and / or the convex fixing stage are fixedly connected to the second step layer 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 is understandable that those skilled in the art can determine the structural form, number, and distribution of the second / third fasteners on the sample mounting platform assembly according to actual needs.

[0018] For the above-mentioned multifunctional sample stage for transmission electron microscopy and atom probe in-situ testing, in a possible implementation, the cross-section of the groove mounting position along the vertical direction is an inverted semicircle 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 mounted on the metal grid to the sample mounting stage assembly.

[0020] For the above-mentioned multifunctional sample stage for in-situ testing of transmission electron microscope and atom probe, in a possible implementation, the metal pressing plate includes a first pressing plate part and a second pressing plate part, wherein the first pressing plate part is arranged on the first step layer, and the second pressing plate part is lower at its end close to the silicon wafer than its end close to the first pressing plate part.

[0021] Through such a structure, the silicon wafer carrying the sample can be reliably pressed by the second pressing part. For example, those skilled in the art can determine the structural form of the first / second pressing part and the way the two constitute the metal pressing part according to actual needs, such as the structures of the two can be the same or different, the two can be fixedly connected or integrally formed, etc.

[0022] For the above-mentioned multifunctional sample stage for transmission electron microscopy and atom probe in-situ testing, in a possible implementation manner, the second pressing portion includes an inclined surface portion and / or a curved surface portion.

[0023] Such a configuration provides a possible structural form for the second tablet pressing part.

[0024] For the above-mentioned multifunctional sample stage for transmission electron microscopy and atom probe in-situ testing, in a possible embodiment, the first pressing part is fixed to the first step layer by means of a first fastener; and / or the support platform is provided with a limiting structure at a position corresponding to the first step layer.

[0025] Through such a configuration, the reliability of the position of the first pressing piece on the first step layer can be ensured by 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 of the first fastener on the first pressing piece according to actual needs.

[0026] For the above-mentioned multifunctional sample stage for transmission electron microscopy and atom probe in-situ testing, in a possible implementation, the sample stage includes a bottom column, which is arranged at the bottom of the support table, and the bottom column is used to match the sample holder of the APT instrument.

[0027] Through such a structure, a possible structural form of the base of the sample stage is provided, such as a support table and forming a roughly T-shaped structure, which can be called a T-shaped support table.

[0028] For the above-mentioned multifunctional sample stage for in-situ testing of transmission electron microscope and atomic probe, in a possible embodiment, the bottom column includes a first bottom column segment and a second bottom column segment arranged from top to bottom, wherein the radial dimension of the first bottom column segment is larger than the radial dimension of the second bottom column segment; and / or the cross-section of the second bottom column segment is circular or D-shaped.

[0029] Through such a construction, a possible structural form of the base column is given. BRIEF DESCRIPTION OF THE DRAWINGS

[0030] The preferred embodiments of the present invention are described below in conjunction with the accompanying drawings, in which:

[0031] Figure 1A schematic diagram showing the structure of a support platform in a multifunctional sample platform for in-situ testing of a transmission electron microscope and an atom probe according to an embodiment of the present invention;

[0032] Figure 2 A schematic diagram showing the structure of a metal pressing piece in a multifunctional sample stage for in-situ testing of a transmission electron microscope and an atom probe according to an embodiment of the present invention;

[0033] Figure 3 A schematic diagram showing the assembly of a support table, a metal pressing sheet and a loaded silicon wafer in a multifunctional sample table for in-situ testing of a transmission electron microscope and an atom probe according to an embodiment of the present invention;

[0034] Figure 4 A schematic diagram showing the structure of a concave sample stage in a mounting stage assembly of a multifunctional sample stage for in-situ testing of a transmission electron microscope and an atom probe according to an embodiment of the present invention;

[0035] Figure 5 A schematic structural diagram showing a convex sample stage in a mounting stage assembly of a multifunctional sample stage for in-situ testing of a transmission electron microscope and an atom probe according to an embodiment of the present invention;

[0036] Figure 6 A schematic diagram showing the assembly of a transmission electron microscope and an atom probe in-situ test multifunctional sample stage when a metal grid is installed according to an embodiment of the present invention;

[0037] Figure 7 An electron microscope image of a silicon wafer in a multifunctional sample stage for in-situ testing using a transmission electron microscope and an atom probe according to an embodiment of the present invention is shown;

[0038] Figure 8 for Figure 7 A magnified schematic diagram of the local A in the middle;

[0039] Fig. 9 is an electron microscope image showing a metal grid in a multifunctional sample stage for in-situ testing using a transmission electron microscope and an atom probe according to an embodiment of the present invention; and

[0040] Fig.10 for Fig. 9 Enlarged schematic diagram of part B in the middle.

[0041] List of reference numerals:

[0042] 100. Multifunctional sample stage for transmission electron microscope and atom probe in-situ testing;

[0043] 1. Support table;

[0044] 11. First step layer; 12. Second step layer; 13. Limiting structure;

[0045] 2. Metal pressing sheet;

[0046] 21. a first tablet pressing part; 22. a second tablet pressing part;

[0047] 3. Sample carrying platform assembly;

[0048] 31. Concave sample stage;

[0049] 311, groove installation position; 312, vertical surface;

[0050] 32. Convex fixed table;

[0051] 321, protruding end;

[0052] 41. a first fastener; 42. a 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 DESCRIPTION

[0060] The preferred embodiments of the present invention are described below with reference to the accompanying drawings. It should be understood by those skilled in the art that these embodiments are only used to explain the technical principles 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 "center", "upper", "lower", "left", "right", "vertical", "horizontal", "inner", "outer" and the like indicating directions or positional relationships are based on the directions or positional relationships shown in the drawings, which are only for the convenience of description, and do not indicate or imply that the device or element must have a specific orientation, be constructed and operated in a specific orientation, and therefore cannot be understood as limiting the present invention. In addition, the terms "first" and "second" are used for descriptive purposes only, 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 limited, 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 a direct connection, an indirect connection through an intermediate medium, or the internal connection 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, in order to better illustrate the present invention, many specific details are given in the specific embodiments below. It should be understood by those skilled in the art that the present invention can also be implemented without certain specific details. In some examples, the principles of conventional APT testing and TEM-APT in-situ testing, which are well known to those skilled in the art, are not described in detail in order to highlight the main purpose of the present invention.

[0064] Main reference Figures 1 to 6 In a possible embodiment, a multifunctional sample stage 100 for transmission electron microscopy and atomic probe in-situ testing mainly includes a support platform 1, a metal pressing sheet 2 and a sample mounting platform assembly 3, wherein the support platform 1 includes a substrate, the substrate has a first-level step layer 11 and a second-level step layer 12, the height of the first-level step layer 11 is greater than the second-level step layer 12, and a silicon wafer 200 carrying a first sample 401 for conventional APT testing can be reliably fixed to the support platform 1 through the cooperation of the metal pressing sheet 2 and the first / second-level step layers, the sample mounting platform assembly 3 can be fixed to the position of the support platform 1 corresponding to the second-level step layer 12, and a metal grid 300 carrying a second sample 402 for TEM-APT in-situ testing can be in a stable testing state through the mounting platform assembly 3.

[0065] Main reference Figures 1 to 3 In a possible implementation, the metal pressing sheet 2 includes a first pressing sheet portion 21 (such as a head portion) and a second pressing sheet portion 22 (such as a tail portion), wherein the first pressing sheet portion 21 is disposed at a position of the support platform 1 corresponding to the first step layer 11, and the second pressing sheet portion 22 is close to the end of the silicon wafer ( Figure 1 The right end of the first pressing part is lower than the end thereof close to the first pressing part ( Figure 1 The second pressing portion is formed by pressing the silicon wafer 200 carrying the first sample. For example, the second pressing portion may be an inclined surface, a curved surface, or a combination of the two. In this example, the second pressing portion is substantially an inclined surface.

[0066] In a possible implementation, the support platform 1 is provided with a limiting structure 13 at a position corresponding to the first step layer 11. When the first pressing sheet part 21 is provided at the first step layer, the reliability of its position can be ensured by the limiting structure. As in this example, the limiting structure includes two limiting plates (disposed on both sides of the width direction of the silicon wafer) provided on the first step layer 11; the first pressing sheet part 21 is clamped between the two limiting plates in the assembled state. For example, on the basis of limiting by the limiting structure, the metal pressing sheet can be fixed to the support platform 1 by a first fastener 41 such as a screw. For example, a first connecting hole 51 (such as including a pair, such as a through hole) is provided on the metal pressing sheet 2, and a second connecting hole 52 (such as including a pair, such as a blind hole or other limiting hole) is provided on the support platform at a position corresponding to the first step layer 11. Through the cooperation of the screw and 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 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 but not limited to replacing the limiting plate with a structure having a groove / protrusion, adding a limiting structure such as a baffle / block between the two limiting structures (the position where the head of the silicon wafer abuts). In addition, the screw is only an exemplary description of the first fastener, and the metal pressing sheet and the support table can also be fixedly connected by an interference fit between a conical pin and the first / second connecting hole.

[0068] Main reference Figures 4 to 6 In a possible embodiment, the mounting platform assembly 3 includes a concave sample platform 31 and a convex fixed platform 32 that match each other, wherein at least one groove mounting position 311 (such as a side-opening groove) is formed on the concave sample platform 31, and the concave sample platform 31 has a vertical surface 312 at a position corresponding to the groove mounting position 311, and the metal carrier mesh 300 carrying the second sample 402 can be placed at a position of the groove mounting position 311 corresponding to the vertical surface 312. A protruding end 321 that can be matched with the groove mounting position 311 is formed on the convex fixed platform 32, and the protruding end is extended into the corresponding groove mounting position and can abut against the metal carrier mesh, thereby reliably clamping the metal carrier mesh between the protruding end and the vertical surface and thus making it 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 mounting stage assembly 3 are connected to each other by a second fastener 42 such as a screw to form 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 a position of the support platform 1 corresponding to the second step 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 fifth connection hole 55 (a pair) and a sixth connection hole 56 are respectively provided on the support platform 1 and the concave sample platform 31, and the screws are inserted 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 fasteners, the way in which they cooperate with the corresponding connecting holes, the structural form / number / distribution of the connecting holes, etc. are all exemplary descriptions, and those skilled in the art can flexibly select according to actual needs. For example, the fasteners can also be pins, bolts, stud bolts, etc. When the assembly is connected to the support table 1, the connecting holes can be respectively arranged on the concave sample table and the convex fixing table, or only on the convex fixing table, etc.

[0072] In a possible implementation, the multifunctional sample stage 100 for transmission electron microscope and atomic probe in-situ testing is provided with a bottom column 6 at the bottom of the support platform 1. For example, 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, wherein the first bottom column section 61 has a larger radial dimension, and is mainly used to enhance the stability of the support platform 1 when it is fixed to the sample holder, thereby realizing the safe testing of the APT sample. The second bottom column section 62 has a smaller radial dimension, and is mainly used to connect with the sample holder of the APT instrument.

[0073] In a possible implementation, a positioning surface 621 may be machined on the second bottom column segment 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 segment and the sample holder of the APT instrument can be achieved by means of the cooperation between the positioning pin and the positioning surface of the second bottom column segment.

[0074] Obviously, the above structure is only an exemplary description of the bottom column, and those skilled in the art can flexibly select the structural form of the base according to actual needs, such as the base only includes the second bottom column section, and the two are fixed by other means. Exemplarily, holes are respectively provided on the sample holder and the second bottom column section, and the two are fixed by the cooperation of the fasteners with the two holes.

[0075] 1. Conventional APT testing

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

[0077] When the transmission electron microscope and atom probe in-situ testing multifunctional sample stage 100 are used for conventional APT testing, the testing method mainly includes the following steps:

[0078] First, a silicon wafer 200 carrying a first sample 401 (APT needle-shaped sample) is placed on the second step layer 12 of the support platform 1;

[0079] Then, the metal pressing sheet 2 is placed on the first step layer 11 of the support platform 1, and at this time, the head of the metal pressing sheet is clamped between the two limiting structures;

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

[0081] At the beginning of the APT test, the second bottom column section 62 is inserted into the sample holder of the APT, and the support platform 1 is fixed to the sample holder through the cooperation between the positioning pins arranged on the sample holder and the positioning surface 621 on the second-level bottom column.

[0082] 2. TEM-APT in-situ testing

[0083] Main reference Fig. 9 and Fig.10 A plurality of comb-shaped teeth 301 are provided on the metal grid 300 , and a second sample (needle-shaped sample) 402 prepared by FIB is bonded to the ends of the comb-shaped teeth 301 .

[0084] When the TEM-APT in-situ test is performed using the above-mentioned transmission electron microscope and atom probe in-situ test multifunctional sample stage 100, the microstructure analysis of the needle-shaped sample prepared by FIB can be performed using TEM first, and then the sample can be taken out and transferred to the APT instrument for three-dimensional reconstruction and characterization of the elements, and finally the transmission electron microscope results and the atom probe data are matched to obtain the 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, the concave sample stage 31 is placed on the second step layer 12 of the support platform 1, and the concave sample stage 31 is fixed to the support platform 1 using a third fastener such as a screw (not shown);

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

[0087] Finally, the convex fixing platform 32 is placed on the second step layer 12 of the support platform 1, and matched with the concave sample platform 31, and then the two are fixedly connected by means of a second fastener such as a screw. When fixed, 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 grid 300 located at the vertical surface 312.

[0088] When used for APT testing, a support table equipped with a concave sample table, a convex fixing table and a metal grid is inserted into the base of the APT to conduct the experiment.

[0089] In this example, there are two groove mounting positions 311 on the concave sample stage 31, and the cross section of the groove mounting position along the vertical direction is a part of a semicircle (such as a cross section equivalent to a truncated cone), such as a semicircle with a diameter of 3mm, and the corresponding protruding ends 321 on the convex fixed stage 32 include two, and the diameter is slightly smaller than the groove mounting position (such as also 2.98mm) to ensure that the concave sample stage 31 and the convex fixed stage 32 can be smoothly matched. Obviously, this is only an exemplary description of the mounting stage assembly, and those skilled in the art can determine the number, relative position, cross-sectional shape, etc. of the groove mounting positions / protruding ends according to actual needs, such as the cross section of the groove mounting position / protruding end can be an isosceles trapezoid, a semicircle, etc.

[0090] It can be seen that in a preferred embodiment of the present invention, the multifunctional sample stage for transmission electron microscope and atom probe in-situ testing can, on the one hand, place silicon wafers carrying needle-shaped samples, thereby realizing conventional APT testing of samples on this basis. Based on conventional APT testing, more needle-shaped samples are carried by using silicon wafers to obtain spatial component reconstruction information of materials in multiple regions. On the other hand, a metal grid carrying needle-shaped samples can be placed, thereby realizing TEM-APT in-situ analysis of samples on this basis. Based on TEM-APT in-situ analysis, comprehensive morphological images, crystal structures, atomic occupancy, element valence states, major element components and three-dimensional spatial distribution information of elements of the material can be obtained. In this way, the test requirements corresponding to the two functions can be completed by introducing a sample stage device, which effectively reduces the cost. In addition, the multifunctional sample stage of the present invention also has the advantages of easy fixing / disassembly of the metal grid, so that the sample can be stably transferred between the TEM and APT instruments. That is, it can effectively avoid the damage of the more fragile needle-shaped samples and has the advantages of simple operation and easy disassembly.

[0091] So far, the technical solutions of the present invention have been described in conjunction with the preferred embodiments shown in the accompanying drawings. However, it is easy for those skilled in the art to 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 multifunctional sample stage for transmission electron microscope and atom probe in-situ testing, characterized in that: The sample stage comprises: A support platform, comprising a base having a first step layer and a second step layer; A metal pressing sheet, a first aspect of which can be fixed to the first step layer, and a second aspect of which can abut against a silicon wafer provided on the second step layer and carrying a sample; The sample carrying platform assembly can be arranged on the second stepped layer, and the metal grid carrying the sample can be fixed to the sample carrying platform assembly.

2. The multifunctional sample stage for transmission electron microscope and atom probe in-situ testing according to claim 1, characterized in that: The sample carrying platform assembly comprises: A concave sample stage, on which at least one groove installation position is formed, the concave sample stage has a vertical surface at a position corresponding to the groove installation position, and a metal grid carrying a sample can be placed at the groove installation position and at a position corresponding to the vertical surface; A convex fixing platform is formed with a protruding end that can be matched with the groove mounting position, so as to: The protruding end is extended into the groove installation position, and thus the metal grid carrying the sample is sandwiched between the protruding end and the vertical surface.

3. The multifunctional sample stage for transmission electron microscope and atom probe in-situ testing according to claim 2, characterized in that: The concave sample stage and the convex fixing stage are fixedly connected by means of a second fastener.

4. The multifunctional sample stage for transmission electron microscope and atom probe in-situ testing according to claim 2 or 3, characterized in that: The concave sample stage and / or the convex fixing stage are fixedly connected to the second stepped layer by means of a third fastener.

5. The multifunctional sample stage for transmission electron microscope and atom probe in-situ testing according to claim 2, characterized in that: The cross section of the groove installation position along the vertical direction is an inverted semicircle or an isosceles trapezoid. Wherein, the waist of the isosceles trapezoid is an arc line.

6. The multifunctional sample stage for transmission electron microscope and atom probe in-situ testing according to claim 1, characterized in that: The metal pressing sheet comprises a first pressing sheet portion and a second pressing sheet portion, The first pressing part is arranged on the first step layer, and the end of the second pressing part close to the silicon wafer is lower than the end of the second pressing part close to the first pressing part.

7. The multifunctional sample stage for transmission electron microscope and atom probe in-situ testing according to claim 6, characterized in that: The second pressing portion includes an inclined surface portion and / or a curved surface portion.

8. The multifunctional sample stage for transmission electron microscope and atom probe in-situ testing according to claim 7, characterized in that: The first pressing piece portion is fixed to the first step layer by means of a first fastener; and / or The support platform is provided with a limiting structure at a position corresponding to the first step layer.

9. The multifunctional sample stage for transmission electron microscope and atom probe in-situ testing according to claim 1, characterized in that: The sample stage comprises a bottom column, which is arranged at the bottom of the support table and is used to match the sample holder of the APT instrument.

10. The multifunctional sample stage for transmission electron microscope and atom probe in-situ testing according to claim 9, characterized in that: The bottom column comprises 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 segment is greater than the radial dimension of the second bottom column segment; and / or The cross section of the second bottom column section is circular or D-shaped.

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