A sample fixture for realizing the combination of FIB-TKD and a scanning electron microscope detection system

Abstract

The present invention discloses a sample fixture for realizing the combination of FIB-TKD and a scanning electron microscope detection system. The sample fixture includes a sample holder and a semi-copper mesh clamping piece rotatably mounted on the sample holder. The sample holder is detachably connected to the sample stage of the scanning electron microscope. At least one semi-circular groove is provided on the semi-copper mesh clamping piece for placing the semi-copper mesh, and each semi-circular groove is equipped with a pressing spring piece for clamping and fixing the semi-copper mesh on the semi-circular groove. A positioning unit is provided between the sample holder and the semi-copper mesh clamping piece to fix the position of the semi-copper mesh clamping piece after rotating a certain angle by using the positioning unit. Based on this sample fixture, the present application also proposes a scanning electron microscope detection system for simultaneously realizing FIB sample preparation and TKD experiments, including a TKD experiment unit, a sample preparation system, etc. By adjusting the position of the sample using the sample fixture, a planar transmission electron microscope sample that meets the test requirements can be prepared quickly and efficiently, and a transmission EBSD (TKD) experiment can also be completed.

Description

Technical Field

[0001] The present invention relates to the technical field of material test sample preparation, and in particular to a device capable of realizing the preparation of planar transmission electron microscope samples by FIB and the combination with TKD. Background Art

[0002] Focused ion beam technology FIB is an important means for spot processing and preparing transmission electron microscope samples. Transmission electron backscattering technology (TKD) is a crystallographic experiment using a common EBSD probe. Compared with the conventional EBSD spatial resolution of about 50 nm, the lateral TKD spatial resolution can reach below 30 nm, and the TKD sample is universal with the transmission electron microscope sample, and two microscopic characterization experiments can be completed at one time.

[0003] The existing FIB processing and TKD testing methods have the following obvious deficiencies:

[0004] (1) Each experiment requires the use of an independent sample holder, and the sample prepared by FIB needs to be transferred to the TKD sample holder for use. Therefore, the existing sample holders cannot directly combine FIB and TKD;

[0005] (2) The size of the transmission electron microscope sample prepared by FIB is generally more than ten micrometers in length and less than 100 nm in thickness, and there are risks such as dropping and solder joint detachment during the sample transfer process;

[0006] (3) The function of the sample holder used in FIB sample preparation is simple, strictly restricting the height of the original sample (a planar sample with a height not greater than 2 mm), and the versatility is poor;

[0007] (4) When preparing planar transmission electron microscope samples by FIB, a special pre-tilting stage needs to be used, the operation difficulty is large, and the sample preparation efficiency is not high. Summary of the Invention

[0008] In order to solve the deficiencies existing in the prior art, the present invention proposes a sample fixture and a scanning electron microscope detection system for realizing FIB-TKD combination, which uses the same sample fixture to realize the FIB-TKD combination of planar transmission electron microscope samples, has a simple sample preparation process, high sample preparation efficiency and success rate, and can meet the increasing high-end microscopic characterization requirements.

[0009] In order to solve the above technical problems, the present invention adopts the following technical solutions:

[0010] A sample fixture for realizing FIB-TKD combination, comprising:

[0011] A sample seat, which is detachably connected between the sample seat and the scanning electron microscope sample stage;

[0012] Half - copper mesh clamping piece, the half - copper mesh clamping piece is rotatably installed on the sample holder; at least one semi - circular groove is provided on the half - copper mesh clamping piece, and each semi - circular groove is equipped with a pressing spring piece; one end of the pressing spring piece is a fixed end, and the other end is a free end and faces the semi - circular groove;

[0013] Half - copper mesh, the half - copper mesh is used to support the thin - film sample cut by FIB and for thinning the thickness of the thin - film;

[0014] Positioning unit, the positioning unit includes a limiting convex rod and an angular through - hole; the limiting convex rod is arranged on the half - copper mesh clamping piece, and a plurality of angular through - holes are arranged on the sample holder opposite to the rotation trajectory of the limiting convex rod.

[0015] Further, a groove is opened on the half - copper mesh clamping piece between the fixed end and the free end of the pressing spring piece, a sliding piece is slidably placed in the groove, and a convex part is provided on the sliding piece, and the convex part is higher than the height of the pressing spring piece without external force.

[0016] Further, a rotating shaft is respectively arranged on both side walls of the half - copper mesh clamping piece, and a corresponding rotating shaft hole is opened on the sample holder; the rotating shafts of the half - copper mesh clamping piece are respectively inserted into the rotating shaft holes.

[0017] Further, at least one side of the rotating shaft is detachably connected to the half - copper mesh clamping piece.

[0018] Further, the limiting convex rod is arranged on the side wall of the half - copper mesh clamping piece where a certain rotating shaft is located, and the limiting convex rod is arranged parallel to the rotating shaft.

[0019] Further, a spring is sleeved on the rotating shaft on the side where the limiting convex rod is not installed.

[0020] Further, the bottom of the sample holder is connected to the scanning electron microscope sample stage through a threaded rod, and a limiting block with a height - adjusting function is provided on the threaded rod.

[0021] A scanning electron microscope detection system for simultaneously realizing FIB sample preparation and TKD experiment, including:

[0022] Scanning electron microscope sample stage,

[0023] Sample fixture, the sample fixture is installed on the scanning electron microscope sample stage; the sample fixture is used to clamp the half - copper mesh and change the angle of the half - copper mesh and the sample to be measured on the half - copper mesh;

[0024] TKD experiment unit, performing TKD experiment on the sample on the half - copper mesh;

[0025] The sample preparation system includes a FIB sample preparation unit, a sample extraction unit, a sample welding unit, and a sample thinning unit; the FIB sample preparation unit extracts a thin slice sample from an original sample; the sample extraction unit transfers the thin slice sample to a half-copper mesh on a sample fixture; the sample welding unit welds and fixes the thin slice sample and the half-copper mesh; and the sample thinning unit thins the thickness of the thin slice sample.

[0026] Furthermore, the sample extraction unit adopts a robotic arm.

[0027] Furthermore, the sample welding unit uses a small beam of Pt to weld and fix both sides of the thin film sample to the half copper mesh.

[0028] Beneficial effects

[0029] 1. The sample holder designed in this invention can simultaneously perform FIB planar TEM sample preparation and TKD experiments, realizing FIB-TKD functional integration. FIB sample preparation and TKD experiments are completed simultaneously on the same device. This allows for the rapid and efficient preparation of planar TEM samples suitable for testing, as well as transmission EBSD experiments with a spatial resolution below 30 nm. This overcomes the shortcomings of conventional FIB sample holders, which are limited to sample preparation and TKD sample holders, which can only hold prepared samples for experiments. It also solves a series of problems such as the difficulty in transferring small TEM / TKD samples and their easy detachment. This method has no special requirements for sample shape, is widely applicable, is simple to operate, and the combined technology is efficient and has a high success rate.

[0030] 2. The present invention does not require the placement and transfer of the prepared half-copper mesh with thin slice samples. The angle change is achieved only through the designed sample fixture, which avoids the secondary loading of the half-copper mesh with tiny samples, and avoids the problems of the half-copper mesh falling off and the solder feet falling off during the transfer process, which can easily lead to experimental failure.

[0031] 3. The present invention breaks through the height restriction requirement of FIB sample preparation on the original sample. The height adjustment screw assembly ensures that the height difference between the highest point of the semi-copper mesh and the original sample is less than 1mm, which greatly expands the range of FIB sample preparation capabilities and has good versatility.

[0032] 4. The present invention does not require the use of a special pre-tilt table to prepare FIB planar transmission electron microscopy samples, which reduces the difficulty of operation and improves the sample preparation efficiency. It can also be used for the preparation of FIB cross-sectional transmission electron microscopy samples and has a wide range of applications.

[0033] 5. The system designed in the present invention can realize the fixing method of four-leg welding between the thin sheet and the semi-copper mesh on both sides, so that the prepared transmission electron microscope sample or TKD sample is highly firm, which not only ensures the success rate of the experiment, but also allows the thin sheet samples to be processed and used multiple times or repeatedly. BRIEF DESCRIPTION OF THE DRAWINGS

[0034] Figure 1 Schematic diagram of the device for preparing a planar transmission electron microscope sample;

[0035] Figure 2 Schematic diagram of the half copper mesh clamping piece;

[0036] Figure 3 Schematic diagram of the sample holder;

[0037] Figure 4 Schematic diagram of height adjustment;

[0038] Figure 5 Experimental effect diagram of alloy bulk FIB-TKD;

[0039] Figure 6 Experimental effect diagram of metal powder FIB-TKD;

[0040] Figure 7 Schematic diagram of the thin sample being welded and fixed on the half copper mesh;

[0041] In the figure, 1. Height adjustment screw assembly; 2. Sample holder; 2-1. Rotating screw through hole; 2-2. Angle through hole; 2-3. Support rod through hole; 3. Rotating screw; 4. Half copper mesh clamping piece; 4-1. Half circular groove; 4-2. Compression spring piece; 4-3. Groove; 4-4. Sliding piece; 4-5. Limit convex rod; 5. Spring; 6. Support rod; 7. Scanning electron microscope sample stage; 8. Small nail stage. Specific implementation mode

[0042] In order to make the objectives, technical solutions and advantages of the present invention clearer, the present invention will be further described in detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are only used to explain the present invention and are not used to limit the present invention.

[0043] Embodiment 1

[0044] Combined with the attached Figures 1-4 , this application proposes a sample fixture for realizing the combination of FIB-TKD, including a sample holder 2, a half copper mesh clamping piece 4 and a positioning unit. Among them, the bottom of the sample holder 2 is connected to the scanning electron microscope sample stage 7 through a height adjustment screw assembly 1.

[0045] The half copper mesh clamping piece 4 is rotatably connected to the sample holder 2. Two opposite support parts can be arranged on the upper surface of the sample holder 2. A rotating shaft is arranged on each of the two side walls of the half copper mesh clamping piece 4, and corresponding rotating shaft holes are opened at the support parts. The rotating shafts on both sides of the half copper mesh clamping piece 4 are respectively inserted into the rotating shaft holes to realize the rotatable connection of the half copper mesh clamping piece 4 on the sample holder 2.

[0046] On the upper surface of the semi - copper mesh clamping piece 4, at least one semi - circular ring groove 4 - 1 is provided for clamping the semi - copper mesh; in this embodiment, 3 semi - circular ring grooves 4 - 1 are provided, and the 3 semi - circular ring grooves 4 - 1 are arranged along the rotation axis of the semi - copper mesh clamping piece 4. Each semi - circular ring groove 4 - 1 is equipped with a pressing spring piece 4 - 2. One end of the pressing spring piece 4 - 2 is fixedly connected to the wall surface of the semi - copper mesh clamping piece 4, and the other end of the pressing spring piece 4 - 2 contacts the wall surface at the semi - circular ring groove 4 - 1, for fixing the semi - copper mesh placed in the semi - circular ring groove 4 - 1.

[0047] The semi - copper mesh is a semi - circular copper mesh with a diameter of about 3 mm. The arc part of the semi - copper mesh can cooperate with the semi - circular ring groove 4 - 1 during installation; 4 tooth - shaped parts can be provided on the straight edge side of the semi - copper mesh, and the tooth - shaped parts are used to place samples, and the samples are fixed on the semi - copper mesh by welding, such as Figure 7 . The semi - copper mesh is a commonly used component in the art and will not be elaborated here. The size of the semi - circular ring groove 4 - 1 in this application can be designed according to the specifications of the existing semi - copper mesh, so that this fixture can be applicable to the existing general semi - copper mesh.

[0048] To facilitate the loading and unloading of the semi - copper mesh, a groove 4 - 3 is provided on the upper surface of the semi - copper mesh clamping piece 4 along the rotation axis direction. A sliding piece 4 - 4 that can move along the groove 4 - 3 is placed in the groove 4 - 3, and a convex part is provided on the sliding piece 4 - 4, and the convex part is higher than the height of the pressing spring piece 4 - 2 without external force. When the convex part of the sliding piece 4 - 4 contacts the lower surface of the pressing spring piece 4 - 2, the pressing spring piece 4 - 2 will be lifted upward, and then the pressing spring piece 4 - 2 will be far away from the semi - circular ring groove 4 - 1, facilitating the removal of the semi - copper mesh in the semi - circular ring groove 4 - 1; conversely, when the convex part of the sliding piece 4 - 4 no longer contacts the lower surface of the pressing spring piece 4 - 2, the pressing spring piece 4 - 2 will be reset downward, and then the pressing spring piece 4 - 2 will be close to the semi - circular ring groove 4 - 1 to press the semi - copper mesh in the semi - circular ring groove 4 - 1.

[0049] The positioning unit includes a limit convex rod 4 - 5 and an angular through - hole 2 - 2. The limit convex rod 4 - 5 is arranged on one side wall of the semi - copper mesh clamping piece 4 parallel to the rotation axis; the angular through - hole 2 - 2 is arranged on the wall surface of the sample holder 2 opposite to the limit convex rod 4 - 5, and a plurality of angular through - holes 2 - 2 are arranged on an arc with the rotation axis hole as the center and the center distance between the rotation axis and the limit convex rod 4 - 5 as the radius. Therefore, after rotating to the target angle, the limit convex rod 4 - 5 can be inserted into the angular through - hole 2 - 2 corresponding to the target angle to realize the positioning of the semi - copper mesh clamping piece 4 at this time. For example, the horizontal position is set as 0°, and an angular through - hole 2 - 2 is set every 10°, and they are 0°, 10°, 20°, …, 90° in the counter - clockwise direction in turn.

[0050] More specifically, the semi-circular groove 4-1 has an outer diameter of 3 mm, an inner diameter of 2 - 2.5 mm, and a depth of 0.2 - 0.5 mm; the pressing spring piece 4-2 has a width of 1 - 2 mm and a fixing screw at the bottom; the groove 4-3 has a length that runs through the entire clamping piece and a width of 0.8 - 1.8 mm and a depth of 0.2 - 0.5 mm; the sliding piece 4-4 has two protrusions with a diameter of 0.5 - 1.5 mm and a height of 0.4 - 0.8 mm at the position where the length is trisected; the limiting convex rod 4-5 has a length of 0.5 - 1 mm and a diameter of 0.2 - 0.5 mm.

[0051] More specifically, the rotating shafts on the two side walls of the semi-copper mesh clamping piece 4 can be integrally designed with the semi-copper mesh clamping piece 4.

[0052] More specifically, in order to facilitate the disassembly and assembly of the semi-copper mesh clamping piece 4 on the sample holder 2, the rotating shaft on one side of the semi-copper mesh clamping piece 4 is detachably connected. For example, by opening an internal threaded hole on the side wall of the semi-copper mesh clamping piece 4, the rotating screw 3 is used for the rotating shaft, and the rotating screw 3 passes through the rotating shaft hole and is fitted and installed with the internal threaded hole of the semi-copper mesh clamping piece 4.

[0053] More specifically, the rotating shafts on both sides of the semi-copper mesh clamping piece 4 are both detachably connected. For example, by respectively opening internal threaded holes on the two side walls of the semi-copper mesh clamping piece 4, the rotating screw 3 and the support rod 6 are used for the rotating shafts, and the rotating screw 3 and the support rod 6 respectively pass through the rotating shaft holes and are fitted and installed with the internal threaded holes of the semi-copper mesh clamping piece 4.

[0054] More specifically, a spring 5 is sleeved on the support rod 6; when adjusting the angle of the semi-copper mesh clamping piece 4, it is necessary to first push it towards the support rod 6 side, so that the limiting convex rod 4-5 is separated from the angle through hole 2-2, and at the same time the spring 5 is compressed; then rotate the rotating screw 3 to drive the semi-copper mesh clamping piece 4 to rotate to the target angle, and then no longer apply a thrust to the support rod 6. Under the action of the spring 5, the semi-copper mesh clamping piece 4 is pushed towards the rotating screw 3 side until the limiting convex rod 4-5 is combined with the angle through hole 2-2 corresponding to the target angle, realizing the automatic positioning of the semi-copper mesh clamping piece 4 after the angle adjustment.

[0055] More specifically, if a spring 5 is sleeved on the support rod 6, the limiting convex rod 4-5 needs to be arranged on the side wall of the semi-copper mesh clamping piece 4 where the rotating screw 3 is located.

[0056] More specifically, the height adjustment screw assembly 1 includes a threaded rod and a limiting block. The limiting block is provided with an internal threaded hole that cooperates with the threaded rod, and the threaded rod is also threadedly connected to the scanning electron microscope sample stage. The height of the sample holder 2 in the vertical direction can be adjusted through the height adjustment screw assembly 1.

[0057] Embodiment 2

[0058] Based on the sample fixture designed in Embodiment 1, the present application also proposes a scanning electron microscope detection system that simultaneously realizes FIB sample preparation and TKD experiments. The system includes: a scanning electron microscope sample stage 7, a sample preparation system (sample extraction unit, sample welding unit, sample thinning unit), a TKD experiment unit, and the above-mentioned sample fixture.

[0059] The scanning electron microscope sample stage 7 is used to place the sample fixture and the small nail stage 8; the small nail stage 8 is used to fix the original sample;

[0060] The FIB sample preparation unit extracts a thin sample from the sample fixed on the small nail stage 8, mainly including:

[0061] The sample extraction unit is used to extract a thin sample from the original sample on the small nail stage 8 and transfer it to the half copper mesh on the sample fixture; the sample extraction unit can use a robotic arm.

[0062] The sample welding unit is used to weld and fix between the thin sample and the half copper mesh. In this embodiment, welding and fixing can be achieved with a small beam of Pt.

[0063] The sample thinning unit is used to thin the thickness of the thin sample fixed on the half copper mesh. In this embodiment, thinning can be achieved using a Ga ion beam.

[0064] The TKD experiment unit is used to perform TKD experiments on the thinned thin sample on the half copper mesh.

[0065] The sample fixture is used to realize the loading of the half copper mesh and the angle conversion of the welding, thinning unit and TKD experiment unit during the FIB sample preparation process.

[0066] The following combines two different types of samples to illustrate the process of the sample fixture and system designed by the present invention for the combined use of FIB sample preparation and TKD experiments, specifically as follows:

[0067] 1. Using a superalloy block with a length of 15 mm, a width of 10 mm, and a height of 8 mm as the original sample

[0068] 1. Use the rotating screw 3 to push the half copper mesh clamping piece 4 inward, so that the limit convex rod 4-5 leaves the initial angle through hole 2-2 and is adjusted to the 40° position for fixation; at this time, the semi-circular ring groove 4-1 is tilted downward at a certain angle.

[0069] 2. Move the sliding piece 4-4, move the protruding part of the sliding piece 4-4 under the pressing spring piece 4-2, lift the pressing spring piece 4-2, and clamp the half copper mesh into the semi-circular ring groove 4-1 under the pressing spring piece 4-2.

[0070] 3. Move the sliding piece 4-4 again, so that the protruding part of the sliding piece 4-4 leaves under the pressing spring piece 4-2, and the pressing spring piece 4-2 is pressed down to lock the half copper mesh.

[0071] 4. Push the semi - copper mesh clamping piece 4 inward with the rotating screw 3 so that the limit convex rod 4 - 5 leaves the angle through - hole 2 - 2 and adjust it to the 0° position for fixation; at this time, the semi - circular groove 4 - 1 is in the horizontal position.

[0072] 5. Fix the polished superalloy block on the test surface to the small nail table 8 with conductive silver glue.

[0073] 6. Adjust the height - adjusting screw assembly 1 so that the highest point of the semi - copper mesh and the alloy block on the small nail table 8 are visually at the same height, and the height difference is less than 1 mm. As shown in Figure 4 the figure, cooperate with the scanning electron microscope sample stage 7 and fix it in the electron microscope sample chamber.

[0074] 7. Use the FIB planar sample preparation technology to extract a thin slice with a length of 12 μm, a width of 10 μm, and a thickness of 1 μm from the alloy block. Move the robotic arm, adjust the X / Z position, and finally use the micro - motion control in the Y direction to slowly move the thin slice horizontally to the semi - copper mesh and stop moving after the thin slice slightly touches the semi - copper mesh.

[0075] 8. Due to the limitation of the equipment operation angle, use a small ion beam current of Pt to preliminarily bond one end of the thin slice far from the robotic arm.

[0076] 9. Cut the connection between the robotic arm and the thin slice with a Ga ion beam.

[0077] 10. Push the semi - copper mesh clamping piece 4 inward with the rotating screw 3 so that the limit convex rod 4 - 5 leaves the angle through - hole 2 - 2 and adjust it to the 90° position for fixation; at this time, both the semi - copper mesh and the thin slice are in the vertical position.

[0078] 11. Weld the left and right two contact feet of the thin slice and the semi - copper mesh with a small ion beam current of Pt under the ion beam.

[0079] 12. Then rotate the sample stage 180°, and use a small ion beam current of Pt to weld the back of the thin slice and the left and right two contact feet of the semi - copper mesh again to complete the firm welding of the four feet on both sides of the thin slice.

[0080] 13. Tilt the sample stage angle to 52° so that the top surface of the thin slice faces the ion beam, and perform Ga ion beam thinning until the thickness of the thin area reaches 50 nm.

[0081] 14. Push the semi - copper mesh clamping piece 4 inward with the rotating screw 3 so that the limit convex rod 4 - 5 leaves the angle through - hole 2 - 2 and adjust it to the 20° position for fixation.

[0082] 15. Adjust the height of the sample stage. Under the electron beam, set the WD to 4 mm, the voltage to 30 kV, and the beam current to 6.4 nA. Turn on the -20° calibration function for the electron beam image. Slowly insert the EBSD probe to 176.5 mm, set the TKD parameters, with the total tilt angle at -20° and the scanning step size at 15 nm, and conduct the TKD experiment. The experimental results are as Figure 5 shown.

[0083] II. Use metal powder with a particle size of 5 - 20 μm as the original sample

[0084] 1. Push the semi - copper mesh clamping piece 4 inward with the rotating screw 3, so that the limit convex rod 4 - 5 leaves the initial angular through - hole 2 - 2, and adjust it to the 40° position for fixation; make the semi - circular ring groove 4 - 1 tilt downward at a certain angle at this time.

[0085] 2. Move the sliding piece 4 - 4, move the protrusion of the sliding piece 4 - 4 under the pressing spring piece 4 - 2, lift the pressing spring piece 4 - 2, and clamp the semi - copper mesh into the semi - circular ring groove 4 - 1 under the pressing spring piece 4 - 2.

[0086] 3. Move the sliding piece 4 - 4 again, so that the protrusion of the sliding piece 4 - 4 leaves the lower part of the pressing spring piece 4 - 2, and the pressing spring piece 4 - 2 presses down to lock the semi - copper mesh.

[0087] 4. Push the semi - copper mesh clamping piece 4 inward with the rotating screw 3, so that the limit convex rod 4 - 5 leaves the angular through - hole 2 - 2, and adjust it to the 0° position for fixation; make the semi - circular ring groove 4 - 1 in a horizontal position at this time.

[0088] 5. First, fix a 5×5 mm single - crystal silicon wafer on the small nail table 8 with double - sided carbon conductive tape, then sprinkle the original powder sample on the single - crystal silicon wafer, and blow it with an ear - pipette.

[0089] 6. Adjust the height - adjusting screw assembly ① so that the highest point of the semi - copper mesh and the top of the powder particles are visually at the same height, with a height difference of less than 1 mm. Use it in combination with the scanning electron microscope sample stage 7 and fix it in the electron microscope sample chamber.

[0090] 7. Deposit Pt with a small electron beam current to adhesively bond the bottom of the powder to the silicon wafer at multiple angles.

[0091] 8. Use the FIB planar sample preparation technique to extract a thin slice with a length of 10 μm, a width of 10 μm, and a thickness of 1.5 μm. Use the silicon wafer as a carrier to support the powder. Move the robotic arm, adjust the X / Z position, and finally use the Y - direction fine - motion control to slowly move the thin slice horizontally to the semi - copper mesh and stop moving after slight contact.

[0092] 9. Due to the limitation of the equipment operation angle, use a small ion beam current of Pt to preliminarily adhesively bond one end of the thin slice far from the robotic arm.

[0093] 10. Cut the connection between the robotic arm and the wafer with a Ga ion beam.

[0094] 11. Push the semi - copper mesh clamping piece 4 inward with the rotating screw 3, so that the limit convex rod 4 - 5 leaves the angle through - hole 2 - 2, and adjust it to the 90° position and fix it.

[0095] 12. Under the ion beam, weld the left and right two pins of the wafer and the semi - copper mesh with a small beam current of Pt.

[0096] 13. Then rotate the sample stage 180°, and again weld the back of the wafer and the left and right two pins of the semi - copper mesh with a small beam current of Pt to complete the firm welding of the four pins on both sides of the wafer.

[0097] 14. Tilt the sample stage angle to 52°, make the top surface of the wafer face the ion beam, perform Ga ion beam thinning, and finally the thickness of the thin area reaches 150 nm.

[0098] 15. Push the semi - copper mesh clamping piece 4 inward with the rotating screw 3, so that the limit convex rod 4 - 5 leaves the angle through - hole 2 - 2, and adjust it to the 20° position and fix it.

[0099] 16. Adjust the height of the sample stage. Under the electron beam, set WD to 3.8 mm, voltage to 30 kV, beam current to 6.4 nA. Turn on the electron beam image - 20° calibration function, slowly insert the EBSD probe to 176.5 mm, set the TKD parameters, the total tilt angle is - 20°, the scanning step size is 10 nm, and perform the TKD experiment. The experimental results are as Figure 6 shown.

[0100] Combined with the attached Figures 5-6 And for the above - mentioned two different types of samples, the combined FIB - TKD experiment can be completed for various types of samples. The experimental results have achieved the expected effect, which is convenient and efficient.

[0101] The above embodiments are only used to illustrate the design concept and characteristics of the present invention, and their purpose is to enable those skilled in the art to understand the content of the present invention and implement it accordingly. The protection scope of the present invention is not limited to the above embodiments. Therefore, all equivalent changes or modifications made according to the principles and design ideas disclosed by the present invention are within the protection scope of the present invention.

Claims

1. A sample fixture for realizing the combination of FIB-TKD, characterized in that, Comprising: A sample holder (2), which is detachably connected between the sample holder (2) and the scanning electron microscope sample stage (7); A semi-copper mesh clamping piece (4), which is rotatably mounted on the sample holder (2); at least one semi-circular groove (4-1) is provided on the semi-copper mesh clamping piece (4), and each semi-circular groove (4-1) is equipped with a pressing spring piece (4-2); one end of the pressing spring piece (4-2) is a fixed end, and the other end is a free end and faces the semi-circular groove (4-1); A semi-copper mesh, which is used to support the thin slice sample cut by FIB and is used for thinning the thickness of the thin slice; A positioning unit, which includes a limiting convex rod (4-5) and an angular through hole (2-2); the limiting convex rod (4-5) is arranged on the semi-copper mesh clamping piece (4), and a plurality of angular through holes (2-2) are provided on the sample holder (2) opposite to the rotation track of the limiting convex rod (4-5); A groove (4-3) is opened on the semi-copper mesh clamping piece (4) between the fixed end and the free end of the pressing spring piece (4-2), and a sliding piece (4-4) is slidably placed in the groove (4-3), and a convex portion is provided on the sliding piece (4-4), and the convex portion is higher than the height of the pressing spring piece (4-2) when there is no external force; A rotating shaft is respectively arranged on both side walls of the semi-copper mesh clamping piece (4), and a rotating shaft hole corresponding to the rotating shaft is opened on the sample holder (2); the rotating shafts of the semi-copper mesh clamping piece (4) are respectively inserted into the rotating shaft holes.

2. The sample fixture for realizing the combination of FIB-TKD according to claim 1, wherein At least one side of the rotating shaft is detachably connected to the semi-copper mesh clamping piece (4).

3. A sample fixture for realizing the combined use of FIB-TKD according to claim 1 or 2, characterized in that, The limiting convex rod (4-5) is arranged on the side wall of the semi-copper mesh clamping piece (4) where a certain rotating shaft is located, and the limiting convex rod (4-5) is arranged parallel to the rotating shaft.

4. A sample fixture for realizing the combination of FIB-TKD according to claim 3, characterized in that A spring (5) is sleeved on the rotating shaft on the side where the limiting convex rod (4-5) is not installed.

5. A sample fixture for realizing the combination of FIB-TKD according to claim 1, characterized in that, The bottom of the sample holder (2) is connected to the scanning electron microscope sample stage (7) through a threaded rod, and the threaded rod is provided with a limiting block with a height adjustment function.

6. A scanning electron microscope detection system that simultaneously realizes FIB sample preparation and TKD experiments, characterized in that, Comprising: A scanning electron microscope sample stage (7), A sample fixture for realizing the combination of FIB-TKD as described in claim 1, and the sample fixture is installed on the scanning electron microscope sample stage (7); the sample fixture is used for clamping the semi-copper mesh and changing the angle of the semi-copper mesh and the sample to be measured on the semi-copper mesh; A TKD experimental unit, which performs a TKD experiment on the sample on the semi-copper mesh; A sample preparation system, which includes an FIB sample preparation unit, a sample extraction unit, a sample welding unit, and a sample thinning unit; the FIB sample preparation unit extracts a thin slice sample from the original sample; the sample extraction unit transfers the thin slice sample to the semi-copper mesh on the sample fixture; the sample welding unit welds and fixes between the thin slice sample and the semi-copper mesh; the sample thinning unit thins the thickness of the thin slice sample.

7. A scanning electron microscope detection system that simultaneously realizes FIB sample preparation and TKD experiments according to claim 6, characterized in that, The sample extraction unit uses a robotic arm to extract and transfer the sample.

8. A scanning electron microscope detection system that simultaneously realizes FIB sample preparation and TKD experiments according to claim 6, characterized in that, The sample welding unit uses a small beam current of Pt to weld and fix both sides of the thin slice sample to the semi-copper mesh respectively.

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