Transmission electron microscope and atomic probe in-situ analysis sample table

Abstract

The embodiment of the utility model relates to the technical field of micro-area microscopic analysis of materials, and particularly provides a transmission electron microscope and atomic probe in-situ analysis sample stage, which comprises a first part, a second part, a third part and a fourth part, at least one part of the second part is arranged at the mounting position; wherein the first part is provided with a plurality of grooves, and the TEM metal carrying net carrying the needle-shaped sample can be arranged in any one of the plurality of grooves. By means of the structure, the assembling reliability between the first part and the second part can be guaranteed through the arrangement of the installation position. On the basis, through the arrangement of a plurality of grooves, a plurality of needle-shaped samples carried on the TEM metal carrying net can be tested at the same time, and the experiment efficiency is improved. The sample table can stably support the TEM metal carrying net to be vertically upward, and the metal carrying net is uniformly stressed, so that the damage possibly caused when a sample is transferred between a transmission electron microscope and an atom probe is avoided, and the accuracy of an in-situ analysis result is ensured.

Description

Technical Field

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

[0002] Microscopic research in materials science and earth science has advanced to the nanoscale and atomic scales. Instruments relevant to microscopic research include transmission electron microscopy (TEM) and atom probe tomography (APT). TEM possesses strong comprehensive analytical capabilities, revealing information such as the crystallographic structure, major composition, atomic occupancy, and elemental valence at the nanoscale and atomic scales. However, because TEM compositional analysis relies on energy dispersive spectroscopy (EDS) and electron energy loss spectroscopy (EELS), it is unable to determine and quantify trace elements, and it is difficult to determine the three-dimensional distribution of individual elements. APTs, on the other hand, offer advantages such as sub-nanometer spatial resolution and uniform sensitivity to all elements. For example, they can accurately reconstruct the positions of atoms, the distribution of major and trace elements, and isotopic information in complex materials in three dimensions. Consequently, they are widely used in fields such as metals and their alloys, geological materials, biomaterials, battery materials, and semiconductors. However, since the atom probe can only characterize the composition information of the material and cannot provide the microstructure and crystallographic information of the material, it is difficult to establish the relationship between the composition and crystal structure / performance of the material based on a single analytical technique, which in turn affects the development and application of the material.

[0003] Based on this, in recent years, an in-situ analysis technique based on the combination of transmission electron microscopy and atom probe (TEM-APT in-situ analysis) has been developed. This technique first performs TEM analysis on the sample, and then performs APT analysis on the same sample, ultimately obtaining comprehensive information such as the material's contrast image, crystal structure, atomic occupancy, element valence, isotopes, and three-dimensional spatial distribution of elements. In this way, it is expected that the relationship between composition, crystallographic structure, and material properties can be revealed based on this technique. In addition, the contrast image and major components of the transmission electron microscope can be used to calibrate the reconstructed data of the atom probe under different test conditions to ensure the authenticity of the atom probe experimental results (atom probe experiments are lossy analyses, so repeated testing and verification of the data are not possible).

[0004] To achieve in-situ analysis of samples using a transmission electron microscope and atom probe (TEM-APT), it is crucial to adapt the two instruments for testing the same sample. Currently, the following solutions for achieving in-situ TEM-APT analysis are disclosed:

[0005] For example, the tip of a transmission electron microscope (TEM) holder from JEOL (Japan) can be modified to hold a copper tube and, therefore, a needle-shaped sample prepared by electropolishing, or to form a simple sample stage capable of holding a TEM metal grid. However, this solution is designed for JEOL's unique transmission electron microscope holder and is not suitable for other transmission electron microscopes, such as those from Thermo Fisher Scientific (USA) and HITACHI (Japan). Therefore, it has limited applicability and cannot be widely used for TEM-APT in-situ analysis.

[0006] Another example is a T-stage designed to hold a semicircular TEM metal grid. The T-stage's fixtures are either grooved or linear. The TEM grid is then clamped using the T-stage's fixtures and subsequently transferred to the TEM and APT instruments for experiments. However, in this solution, whether the T-stage has a grooved or linear fixture, the loading position cannot precisely match the shape of the TEM metal grid. This makes it difficult for fragile needle-shaped samples bonded to the comb-shaped teeth of the metal grid to maintain a perpendicular relationship with the APT instrument's detector. This often leads to problems during APT testing, such as sample damage and deviations in elemental reconstruction results. Utility Model Content

[0007] The present invention aims to at least partially solve the above technical problems and / or solve at least part of the above technical problems. Specifically, it provides a new sample stage so that based on the sample stage, TEM-APT in situ analysis of the sample can be completed as smoothly as possible.

[0008] In view of this, the present invention provides a transmission electron microscope and atomic probe in-situ analysis sample stage, the sample stage comprising: a first part, which includes a first substrate, the first substrate forming a mounting position; and a second part, at least a portion of which can be set in the mounting position; wherein, the first part is provided with a plurality of grooves, and the TEM metal grid carrying a needle-shaped sample can be set in any one of the plurality of grooves.

[0009] This structure ensures reliable assembly between the first and second parts through the placement of mounting points. Furthermore, the provision of multiple grooves allows for simultaneous testing of multiple needle-shaped samples mounted on TEM metal grids, improving efficiency.

[0010] For the above-mentioned transmission electron microscope and atom probe in-situ analysis sample stage, in one possible embodiment, the second part includes a second substrate and a protruding end extending from the second substrate in a direction close to the first part, and the protruding end can extend into the groove and thereby clamp the TEM metal grid carrying the needle-shaped sample between the groove and the protruding end.

[0011] With this configuration, it is possible to reliably fix the needle-shaped sample to the sample stage.

[0012] For the above-mentioned transmission electron microscope and atom probe in-situ analysis sample stage, in a possible implementation manner, the bottom of the groove includes a planar portion, and the protruding end can slide into / out of the groove along the planar portion.

[0013] With this configuration, it is possible to ensure stability in the process of the protruding end sliding into / out of the groove.

[0014] For the above-mentioned transmission electron microscope and atom probe in-situ analysis sample stage, in one possible embodiment, in the cross section of the groove, the length of the groove upper surface is greater than the length of the groove lower surface; and / or the line connecting the groove upper surface and the groove lower surface is a straight line or a curve.

[0015] Through such a configuration, a possible structural form of the groove is given. It should be noted that the cross section of the groove should be understood as the cross section of the groove along the vertical direction.

[0016] For the above-mentioned transmission electron microscope and atom probe in-situ analysis sample stage, in a possible implementation manner, the cross section of the groove is an inverted isosceles trapezoid, wherein the waist of the isosceles trapezoid is an arc line.

[0017] With this configuration, it is possible to reliably fix the needle-shaped sample placed on the TEM metal grid to the sample stage.

[0018] For the above-mentioned transmission electron microscope and atom probe in-situ analysis sample stage, in a possible implementation manner, the first substrate includes a transverse portion and a vertical portion, and the transverse portion and the vertical portion form an L-shaped mounting position.

[0019] Through such a configuration, a possible structural form of the first base / installation position is given. It should be noted that the L-shaped structure here should be understood as a substantially L-shaped structure.

[0020] For the above-mentioned transmission electron microscope and atom probe in-situ analysis sample stage, in one possible embodiment, a first limiting hole is provided on the vertical part, and correspondingly, a second limiting hole is provided on the second part, and the first part and the second part are connected to each other by means of fasteners and the first limiting hole and the second limiting hole.

[0021] With this configuration, it is possible to ensure the connection reliability of the sample stage through fasteners, such as pins, bolts, screws, etc.

[0022] For the above-mentioned transmission electron microscope and atom probe in-situ analysis sample stage, in a possible embodiment, the multiple grooves include a first groove and a second groove, wherein the first groove and the second groove are symmetrically distributed along the first substrate; and / or the first limiting hole is located between the first groove and the second groove and below the first groove and the second groove.

[0023] Through such a construction, a possible structural form of the first substrate is given. For example, "the first groove and the second groove are symmetrically distributed along the first substrate" here should be understood as: the first groove and the second groove are roughly symmetrically distributed along the length direction (along the horizontal direction) of the first substrate (the main part). For example, "the first limiting hole is located below the first groove and the second groove" here should be understood as: the lowest point of the first / second groove (the plane of the groove bottom) is higher than the highest point of the first limiting hole. Exemplarily, the axial symmetry line of the first groove and the second groove just passes through the center of the first limiting hole.

[0024] For the above-mentioned transmission electron microscope and atom probe in-situ analysis sample stage, in a possible implementation manner, the first part includes a bottom column, and the bottom column is arranged at the bottom of the lateral part.

[0025] Through such a composition, a possible structural form of the first part is given.

[0026] For the above-mentioned transmission electron microscope and atom probe in-situ analysis sample stage, in one 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.

[0027] Through such a configuration, a possible structural form of the base column is given. BRIEF DESCRIPTION OF THE DRAWINGS

[0028] The preferred embodiments of the present invention are described below with reference to the accompanying drawings, in which:

[0029] Figure 1 A schematic diagram showing the assembly of a transmission electron microscope and an atom probe in-situ analysis sample stage according to an embodiment of the present invention is shown;

[0030] Figure 2 A schematic structural diagram of an L-shaped support platform (first part) in a transmission electron microscope and an atom probe in-situ analysis sample platform according to an embodiment of the present invention is shown;

[0031] Figure 3 A schematic structural diagram showing a convex fixing platform (second part) in a transmission electron microscope and an atom probe in-situ analysis sample stage according to an embodiment of the present invention;

[0032] Figure 4 A schematic diagram showing the assembly of a transmission electron microscope and an atom probe in-situ analysis sample stage with a TEM metal grid installed in one embodiment of the present invention is shown;

[0033] Figure 5 A schematic diagram showing an explosion of a transmission electron microscope and an atom probe in-situ analysis sample stage according to an embodiment of the present invention when a TEM metal grid is installed;

[0034] Figure 6 A secondary electron image showing a needle-shaped sample on the comb teeth of a TEM metal grid;

[0035] Figure 7 Show Figure 6 A magnified schematic diagram of part A in the figure.

[0036] List of reference numerals:

[0037] 100. Transmission electron microscope and atom probe in-situ analysis sample stage;

[0038] 1. L-shaped support platform (first part);

[0039] 11. a first substrate;

[0040] 12. Installation position;

[0041] 13. groove; 131. flat portion;

[0042] 14. First limiting hole;

[0043] 15. Bottom column; 151. First bottom column section; 152. Second bottom column section; 1521. Positioning surface;

[0044] 2. Convex fixed table (the second part);

[0045] 21. Second base; 22. Protruding end; 23. Second limiting hole;

[0046] 3. Fasteners;

[0047] 200, TEM metal grid;

[0048] 201, comb teeth;

[0049] 300. Needle-shaped samples. DETAILED DESCRIPTION

[0050] The preferred embodiments of the present invention are described below with reference to the accompanying drawings. Those skilled in the art should understand that these embodiments are only used to explain the technical principles of the present invention and are not intended to limit the scope of protection of the present invention.

[0051] It should be noted that in the description of this utility model, terms such as "center," "upper," "lower," "left," "right," "vertical," "horizontal," "inner," and "outer" indicating directions or positional relationships are based on the directions or positional relationships shown in the accompanying drawings. This is merely for ease of description and does not indicate or imply that the device or element described must have a specific orientation, be constructed, or operate in a specific orientation. Therefore, it should not be understood as limiting the utility model. In addition, the terms "first" and "second" are used for descriptive purposes only and should not be understood to indicate or imply relative importance.

[0052] Furthermore, it should be noted that, in the description of this utility model, unless otherwise expressly specified or limited, the terms "installed," "set," and "connected" should be understood in a broad sense. For example, they may refer to fixed connections, detachable connections, or integral connections; they may refer to direct connections, indirect connections through an intermediate medium, or internal communication between two components. Those skilled in the art will understand the specific meanings of the above terms in this utility model based on the specific circumstances.

[0053] In addition, to better illustrate the present invention, numerous specific details are provided in the following detailed description. Those skilled in the art will appreciate that the present invention can be practiced without certain details. In some instances, the principles of TEM and APT experiments, 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.

[0054] Main reference Figures 1 to 5 In one possible embodiment, a transmission electron microscope and atom probe in-situ analysis sample stage 100 primarily comprises a first portion and a second portion. The first portion comprises a first base 11, which is formed with a mounting position 12. At least a portion of the second portion can be accommodated in the mounting position. In this example, the first portion forms a generally L-shaped mounting position on the side facing the second portion. Therefore, in this example, the first portion can be referred to as an L-shaped support platform 1. The second portion comprises a second base 21 and a protruding portion extending in a direction approaching the first portion. The second base is accommodated in the mounting position. The protruding portion includes a plurality of protruding ends 22. Therefore, in this example, the second portion can be referred to as a convex fixing platform 2. The L-shaped support platform 1 comprises a transverse portion and a vertical portion at a position corresponding to the mounting position. The upper surface of the transverse portion has a support surface that can tightly mate with the bottom of the convex fixing platform. The vertical portion is provided with a groove 13 that mates with the protruding ends of the convex fixing platform. In this example, the protruding ends are completely accommodated in the groove when assembled. The TEM metal grid 200 with the needle-shaped sample bonded thereto can be sandwiched between any pair of the grooves 13 and the protruding ends 22 .

[0055] On this basis, the first part and the second part can be connected to each other with the help of fasteners 3 such as screws. In one possible embodiment, a first limiting hole 14 is provided on the L-shaped support table 1, and a second limiting hole 23 is provided on the second base of the convex fixing table 2 at a position corresponding to the first limiting hole, wherein the (first and second) limiting holes can be threaded holes or light holes. As in this example, the (first and second) limiting holes are threaded holes, and the (first and second) sample stages are fixedly connected by means of the cooperation of the fasteners 3 and the (first and second) limiting holes. For example, the cooperation method is: the fasteners pass through the second limiting hole 23 corresponding to the convex fixing table 2 and the first limiting hole 14 corresponding to the L-shaped support table 1 in sequence along the axial direction, so that the convex fixing table 2 and the L-shaped support table 1 are tightly matched, thereby achieving effective fixation of the TEM metal grid 200 with the needle-shaped sample bonded thereto.

[0056] In one possible embodiment, the L-shaped support platform 1 includes a first base 11 and a bottom column 15, wherein the first base is formed with a roughly L-shaped space (mounting position) for cooperating with the second base 21 of the convex fixing platform 2, and the bottom column 15 is arranged at the bottom of the first base 11. As in this example, the bottom column 15 includes a first bottom column section 151 and a second bottom column section 152 from top to bottom, wherein the radial dimension of the first bottom column section 151 is larger and is mainly used to stabilize the TEM metal grid 200 and the needle-shaped sample 300 mounted thereon on the L-shaped support platform 1 (see Figure 6 and Figure 7 ), wherein the radial dimension of the second bottom column segment 152 is relatively small, and it is mainly used to cooperate with the sample holder of the APT instrument, such as realizing the connection between the second bottom column segment and the sample holder of the APT instrument through the cooperation between the positioning pin and the second bottom column segment.

[0057] In a possible embodiment, a positioning surface 1521 can be machined on the second bottom column section 152, as shown in FIG. Figure 2 , which is equivalent to transforming the cylindrical structure into a columnar structure with a D-shaped cross-section. In this way, the L-shaped support platform 1 and the sample holder of the APT instrument can be conveniently oriented and fixed.

[0058] In this example, the grooves 13 provided on the first base of the L-shaped support platform 1 include two grooves distributed along the long side (horizontal direction) of its vertical portion, and the structures of the two grooves are roughly the same and are roughly symmetrically distributed on the vertical portion. As mentioned above, the first limiting hole 14 is located between the two grooves 13 and below the two grooves. Correspondingly, the second base 21 of the convex fixing platform 2 is provided with two protruding ends 22 for forming a concave-convex fit with the grooves 13 of the L-shaped support platform 1. In this example, the groove 13 is formed by the top of the vertical portion being recessed downward, and is along the thickness direction of the vertical portion ( Figure 2In this example, the protruding end is completely accommodated in the corresponding groove in the assembled state, so that the flatness of the upper surface of the sample stage can be guaranteed.

[0059] In this example, the cross-section of the groove (the cross-section in the vertical direction) is roughly a structure that is wide at the top and narrow at the bottom (the width of the groove top is greater than the width of the groove bottom and the groove bottom includes a flat part). As in this example, it is equivalent to replacing the waist of the inverted isosceles trapezoid from a straight line to an arc.

[0060] In a specific example, the depth (thickness dimension) of groove 13 is 1.3 mm, the arc is a circular segment with a radius of 1.5 mm, and the groove bottom width is 2 mm. Accordingly, the length of the protrusion that matches the groove is 1.3 mm, the radius of the arc on both sides of the protrusion 22 is 1.49 mm, and the width of the upper bottom surface is 2.21 mm. This ensures that the protrusion can slide freely along the corresponding groove.

[0061] Obviously, this is only an exemplary description of the groove structure, and those skilled in the art can determine the structural form of the groove according to actual needs, such as an isosceles trapezoid, a right-angled trapezoid, etc. In addition, those skilled in the art can determine the number of grooves and their distribution on the vertical portion according to actual needs, such as including more grooves (≥3), the structures of two grooves can be the same or different, and the two grooves can be asymmetrically distributed.

[0062] Based on the above structure of the present invention, the process of performing TEM-APT in-situ testing on a sample mainly includes the following steps:

[0063] The first step is to conduct TEM experiments.

[0064] In one possible embodiment, the main steps of a TEM experiment include:

[0065] First, a needle-shaped sample is prepared using a focused ion beam (FIB) microscope and bonded to the comb-shaped teeth 201 of a TEM metal grid 200.

[0066] Then, place the TEM metal grid 200 on the transmission electron microscope sample holder;

[0067] Finally, TEM is used to perform fine contrast imaging, crystal structure analysis, major component analysis, atomic imaging, and valence state analysis on the needle-shaped sample 300 on the metal grid 200 .

[0068] The second step is to conduct APT experiments.

[0069] In one possible embodiment, the main steps of the APT experiment include:

[0070] First, place the convex fixing platform 2 on the mounting position 12 of the L-shaped support platform 1, and make the protruding end 22 of the convex fixing platform 2 and the groove 13 of the L-shaped support platform 1 slide axially and fit easily;

[0071] Next, place the TEM metal grid 200 with the needle-shaped sample 300 bonded thereto on the flat portion 131 of the bottom of the groove 13. The specifications (shape, size, etc.) of the two sides (groove walls) of the groove 13 should be compatible with the dimensions of the TEM metal grid 200 (e.g., the metal grid should be semicircular with a flat bottom and 30 μm thick) to ensure that the TEM metal grid can be stably supported and that the needle-shaped sample 300 is in a vertically upward position on the comb teeth 201 of the TEM metal grid 200.

[0072] Then, by means of the cooperation of the fasteners 3 such as screws and the limiting holes (14, 23), the convex fixing platform 2 and the L-shaped support platform 1 are tightly matched, thereby achieving the stable fixation of the TEM metal grid 200 on the sample stage (refer to Figure 4 and Figure 5 );

[0073] Finally, the second bottom column section 152 of the bottom column 15 of the L-shaped support platform 1 equipped with the TEM metal grid 200 is inserted into the sample holder of the APT instrument, and then the positioning surface 1521 of the second bottom column section 152 is tightened by the positioning pin of the sample holder to fix the L-shaped support platform 1. Then, APT analysis is carried out on the needle-shaped sample 300 to perform three-dimensional reconstruction and characterization of the elements.

[0074] Main reference Figure 6 and Figure 7 In one possible embodiment, a needle-shaped sample 300, prepared by FIB and meeting both TEM and APT testing requirements, is bonded to the comb-shaped teeth 201 of a TEM metal grid 200. Using the transmission electron microscope and atom probe in-situ analysis sample stage 100 of the present invention, TEM-APT in-situ analysis of the sample is performed, ultimately providing comprehensive information on the sample's morphology, crystal structure, chemical composition, and three-dimensional atomic distribution.

[0075] It can be seen that in a preferred embodiment of the present invention, by providing multiple (such as two) grooves, the sample stage can fix multiple TEM metal grids at one time, thereby being able to simultaneously achieve TEM and APT in-situ analysis of multiple needle-shaped samples, thereby improving experimental efficiency. By setting the bottom of the groove to a structure including a flat portion, the flat portion of the groove bottom cooperates with the waists on both sides, so that the TEM metal grid can be supported more stably, and the needle-shaped samples on the comb teeth can be in a posture perpendicular to the detector of the APT instrument, effectively avoiding the bending and damage of the needle-shaped samples, and also ensuring the accuracy of the test results. By using a fastener (one) to connect the L-shaped support table and the convex fixing table to each other along their axial direction, it can be ensured that the force is uniform when multiple TEM metal grids (such as two) are installed and unloaded at the same time, thereby effectively avoiding phenomena such as damage to the needle-shaped samples when transferring and installing the needle-shaped samples (mounted on the TEM metal grid) between different instruments.

[0076] Thus 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 readily understood by those skilled in the art that the scope of protection of the present invention is obviously not limited to these specific embodiments. Without departing from the principles of the present invention, those skilled in the art may make equivalent changes or substitutions to the relevant technical features, and the technical solutions after such changes or substitutions will fall within the scope of protection of the present invention.

Claims

1. A transmission electron microscope and atom probe in-situ analysis sample stage, characterized in that: The sample stage comprises: A first part includes a first base body having a mounting location formed therein; and a second portion, at least a portion of which is disposed at the mounting location; The first portion is provided with a plurality of grooves, and the TEM metal grid carrying the needle-shaped sample can be placed in any one of the plurality of grooves; The second portion includes a second base and a protruding end extending from the second base in a direction close to the first portion. The protruding end can extend into the groove and thus sandwich the TEM metal grid carrying the needle-shaped sample between the groove and the protruding end; The bottom of the groove includes a plane portion, and the protruding end can slide into / out of the groove along the plane portion.

2. The transmission electron microscope and atom probe in-situ analysis sample stage according to claim 1, characterized in that: In the cross section of the groove, The length of the upper surface of the groove is greater than the length of the lower surface of the groove; and / or The line connecting the upper surface of the groove and the lower surface of the groove is a straight line or a curve.

3. The transmission electron microscope and atom probe in-situ analysis sample stage according to claim 2, characterized in that: The cross section of the groove is an inverted isosceles trapezoid. Wherein, the waist of the isosceles trapezoid is an arc line.

4. The transmission electron microscope and atom probe in-situ analysis sample stage according to claim 1, characterized in that: The first base includes a transverse portion and a vertical portion, and the transverse portion and the vertical portion form an L-shaped installation position.

5. The transmission electron microscope and atom probe in-situ analysis sample stage according to claim 4, characterized in that: The vertical portion is provided with a first limiting hole, Correspondingly, a second limiting hole is provided on the second part. The first part and the second part are connected to each other by means of a fastener that cooperates with the first limiting hole and the second limiting hole.

6. The transmission electron microscope and atom probe in-situ analysis sample stage according to claim 5, characterized in that: The plurality of grooves include a first groove and a second groove, Wherein, the first groove and the second groove are symmetrically distributed on the first substrate; and / or The first limiting hole is located between the first groove and the second groove and below the first groove and the second groove.

7. The transmission electron microscope and atom probe in-situ analysis sample stage according to claim 4, characterized in that: The first portion includes a bottom post disposed at the bottom of the transverse portion.

8. The transmission electron microscope and atom probe in-situ analysis sample stage according to claim 7, 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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