Sample vacuum transfer system and sample preparation method

Abstract

The present disclosure provides a sample vacuum transfer system and a sample preparation method. The sample vacuum transfer system includes a storage rod, a control handle and a control console; the storage rod includes an inner rod and an outer tube movably sleeved on the outer side of the inner rod, the two ends of the inner rod are respectively formed with a connecting portion and a sample portion for storing the sample, the two ends of the sample portion are respectively provided with sealing rings, and the two sealing rings can be sealed and connected with the inner wall of the outer tube to enclose a first sealed space; the control console includes a driving device, a base for installation in a FIB instrument and a vacuum chamber for storing the sample, the driving device and the vacuum chamber are arranged on the base and connected to each other; when the storage rod is inserted into a TEM detector, the control handle is detachably connected to the outer tube and the connecting portion; when the storage rod is arranged in the FIB instrument, the outer tube is detachably connected to the base, and the driving device is detachably connected to the connecting portion; after the sample preparation is completed, the sample is protected and transferred in the first sealed space for detection to prevent the sample from being oxidized.

Description

Technical Field

[0001] The present disclosure relates to the technical field of electron microscope devices, and in particular to a sample vacuum transfer system and a sample preparation method. Background Art

[0002] Transmission Electron Microscope (TEM) is widely used in scientific research because it can see fine structures smaller than 0.2um that cannot be seen under an optical microscope. Samples need to be prepared before TEM. Since TEM has high requirements for sample size, powder samples need to use dispersion and other technologies to make the size of a single powder particle less than 1μm. Block samples generally need to be thinned to a thickness of less than 100nm before TEM detection. FIB (Focused ion Beam) technology has unique advantages in preparing TEM samples. It processes the surface of the material through a focused ion beam to obtain samples in a specific position and orientation, and further prepare samples of the required shape and size.

[0003] Usually, the sample to be tested is placed in the cavity of the FIB instrument, and the cavity of the FIB instrument is evacuated to a vacuum or inert gas environment for ion beam thinning. After the ion beam thinning of the sample to be tested is completed, the cavity of the FIB instrument is inflated to restore the atmospheric pressure, and the thinned sample to be tested is taken out of the cavity of the FIB instrument and inserted into the TEM detector for TEM detection. However, when the sample to be tested is an air-sensitive material (such as alkali metal materials such as lithium and sodium), the sample to be tested will be exposed to air (including oxygen and water vapor, etc.) when it is taken out of the cavity of the FIB after ion beam thinning and when the detection rod containing the sample to be tested is inserted into the TEM detector. The thickness of the sample to be tested is very small and it is easy to oxidize or hydrolyze, which makes the characterization result of the sample to be tested in the subsequent TEM detection inaccurate, affecting the accuracy of TEM detection of the sample to be tested. Summary of the invention

[0004] In order to solve the above technical problems or at least partially solve the above technical problems, the present disclosure provides a sample vacuum transfer system and a sample preparation method.

[0005] The present disclosure provides a sample vacuum transfer system, comprising a preservation rod, a control handle and a console;

[0006] The storage rod comprises an inner rod and an outer tube movably sleeved on the outer side of the inner rod, the two ends of the inner rod are respectively formed with a connecting portion and a sample portion for storing samples, the two ends of the sample portion are respectively provided with sealing rings, the two sealing rings can be sealed and connected with the inner wall of the outer tube to enclose a first sealed space, and the inner rod can move relative to the outer tube to drive the sample portion to extend out of and retract into the outer tube;

[0007] The console comprises a driving device, a base for installation in the FIB instrument and a vacuum chamber for storing the sample, wherein the driving device and the vacuum chamber are arranged on the base and connected to each other;

[0008] When the preservation rod is inserted into the TEM detector, the control handle is detachably connected to the outer tube and the connecting portion to drive the inner rod to move;

[0009] When the preservation rod is arranged in the FIB instrument, the outer tube is detachably connected to the base, and the driving device is detachably connected to the connecting part to drive the inner rod to move and the vacuum chamber to open and close.

[0010] Optionally, the base is provided with a first mounting portion and a second mounting portion which are spaced apart along the width direction of the base, the vacuum chamber is detachably connected to the first mounting portion, the storage rod is detachably connected to the second mounting portion, and the driving device is arranged between the first mounting portion and the second mounting portion and is respectively connected to the vacuum chamber and the connecting portion.

[0011] Optionally, the driving device includes a sliding member and a driving member;

[0012] The sliding member is slidably connected to the base along the length direction of the base, the driving member is arranged on the base and connected to the sliding member, the storage rod is detachably connected to the base along the length direction of the base, and the sliding member is detachably connected to the vacuum chamber and the connecting portion;

[0013] The driving member drives the sliding member to slide relative to the base to drive the vacuum chamber to open and close, and drives the sample part to extend out of and retract into the outer tube.

[0014] Optionally, the vacuum chamber includes an external tube and a movable rod;

[0015] The external tube is movably sleeved on the outside of the movable rod, a storage part for placing the sample is formed on the movable rod, two vacuum sealing rings are provided on the movable rod, and the two vacuum sealing rings are respectively located at two ends of the storage part along the extension direction of the movable rod, and the movable rod can move relative to the external tube to drive the storage part to move between the inside and the outside of the external tube;

[0016] When the storage part is located in the external tube, the two vacuum sealing rings are both sealed and connected to the inner wall of the external tube to jointly enclose a second sealed space;

[0017] The external tube and the movable rod are arranged along the length direction of the base, and one end of the movable rod is connected to the sliding member.

[0018] Optionally, the control handle includes a handle body and a core rod;

[0019] The handle body is provided with an installation channel, the core rod is inserted into the installation channel, the outer tube is detachably connected to one side of the handle body, and one end of the core rod close to the outer tube is detachably connected to the connecting portion.

[0020] Optionally, a rotating tube is provided on the side of the handle body facing the outer tube, the rotating tube is rotatably connected to the handle body, an avoidance channel is provided in the rotating tube, the avoidance channel is coaxially arranged with the installation channel, the core rod is passed through the avoidance channel and the installation channel to be connected with the connecting portion, a thread is provided at one end of the rotating tube and the outer tube that is close to each other, and the rotating tube is threadedly connected to the outer tube;

[0021] And / or, a hook is provided on one end of the core rod facing the inner rod, the connecting portion comprises a slot, and the hook is connected to the slot by snapping.

[0022] Optionally, the sample vacuum transfer system further comprises a connecting bracket, a mounting table and a moving table, wherein the mounting table and the moving table are arranged on one side of the connecting bracket, and the mounting table and the moving table are arranged relatively to each other along a first direction, the moving table is slidably connected to the bracket along the first direction, the mounting table is movably connected to the connecting bracket, the mounting table can move relative to the connecting bracket along the first direction and the second direction, and the mounting table can be lifted and lowered along a third direction, and the first direction, the second direction and the third direction are perpendicular to each other;

[0023] The handle body is connected to the moving platform, the storage rod is installed on the mounting platform along the first direction, and the connecting portion is exposed on one side of the mounting platform facing the moving platform along the first direction.

[0024] Optionally, comb teeth are provided in the sample portion, and the sample is arranged on the comb teeth.

[0025] Optionally, the console further includes a controller, which is connected to the driving device, and controls the driving device to open and close the vacuum chamber, and the controller controls the driving device to drive the sample part to extend and retract the outer tube.

[0026] The present disclosure also provides a sample preparation method, using the sample vacuum transfer system as described in any one of the above items, comprising:

[0027] The sample, the preservation rod and the console are placed in a glove box in a vacuum environment, the sample is placed in a vacuum chamber, the outer tube is mounted on the base, the connecting portion is detachably connected to the driving device, and the driving device drives the vacuum chamber to close and drives the sample portion to retract into the outer tube;

[0028] The console is taken out of the glove box and placed inside the FIB instrument. The inside of the FIB instrument is evacuated to form a vacuum environment. A driving device drives the vacuum chamber to open and drives the sample part to extend out of the outer tube. The probe of the FIB instrument moves the sample in the vacuum chamber to the sample part, and an ion beam is used to perform a sample preparation operation on the sample in the sample part.

[0029] After the sample preparation operation on the sample part is completed, the driving device drives the sample part to retract into the outer tube, the FIB instrument is opened, the preservation rod is taken out, and the control handle is detachably connected to the outer tube and the inner rod of the preservation rod;

[0030] The preservation rod detachably connected to the control handle is inserted into the TEM detector, the interior of the TEM detector is evacuated, and the control handle drives the inner rod to move relative to the outer tube so that the sample part extends out of the outer tube and is located in the TEM detector, and TEM detection is performed on the sample in the sample part.

[0031] Compared with the prior art, the technical solution provided by the present invention has the following advantages:

[0032] The present disclosure provides a sample vacuum transfer system and a sample preparation method. The sample vacuum transfer system includes a storage rod, a control handle and a control console. The storage rod includes an inner rod and an outer tube movably sleeved on the outer side of the inner rod. The two ends of the inner rod are respectively formed with a connecting portion and a sample portion for storing samples. The two ends of the sample portion are respectively provided with sealing rings. The two sealing rings can be sealed and connected with the inner wall of the outer tube to enclose a first sealed space. The inner rod can move relative to the outer tube to drive the sample portion to extend and retract the outer tube, so that the sample portion is in the first sealed space in the outer tube to avoid the sample in the sample portion from contacting the external gas environment. The control console includes a driving device, a base for installation in a FIB instrument and a vacuum chamber for storing samples. The driving device and the vacuum chamber are arranged on the base and connected to each other. When the storage rod is inserted into the TEM detector, the control handle is detachably connected to the outer tube and the connecting portion, so that the control handle can drive the inner rod to move relative to the outer tube to drive the sample portion to extend and retract the outer tube, so that the sample portion is in the first sealed space in the outer tube to avoid the sample in the sample portion from contacting the external gas environment. The rod moves so that the sample part extends out of the outer tube for TEM detection; when the preservation rod is set in the FIB instrument, the outer tube is detachably connected to the base, and the driving device is detachably connected to the connecting part to drive the inner rod to move and the opening and closing of the vacuum chamber, so that the sample placed in the vacuum chamber can be transferred to the extended sample part in the vacuum environment of the FIB instrument for ion beam thinning, and the sample after ion beam thinning is stored in the first sealed space as the sample part is retracted into the outer tube; through the cooperation of the preservation rod, the control handle and the control console, the sample is in the vacuum environment of the closed space during the whole process from the completion of sample preparation in the FIB instrument to the placement into the TEM detector for detection, thereby avoiding oxidation and contamination of the sample during the process of placing the sample into the TEM detector after sample preparation is completed, and improving the accuracy of TEM detection of the sample. BRIEF DESCRIPTION OF THE DRAWINGS

[0033] The accompanying drawings, which are incorporated in and constitute a part of this specification, illustrate embodiments consistent with the present disclosure and, together with the description, serve to explain the principles of the present disclosure.

[0034] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings required for use in the embodiments or the description of the prior art will be briefly introduced below. Obviously, for ordinary technicians in this field, other drawings can be obtained based on these drawings without paying any creative labor.

[0035] Figure 1 This is a schematic structural diagram of the sample portion retracted into the outer tube after the storage rod and the control handle are assembled according to the embodiment of the present disclosure;

[0036] Figure 2 This is a schematic structural diagram of the sample portion extending out of the outer tube after the storage rod and the control handle are assembled according to the embodiment of the present disclosure;

[0037] Figure 3It is a schematic diagram of the structure when the sample portion of the storage rod according to the embodiment of the present disclosure is retracted into the outer tube;

[0038] Figure 4 It is a schematic diagram of the structure when the sample portion of the storage rod according to the embodiment of the present disclosure extends out of the outer tube;

[0039] Figure 5 for Figure 4 A schematic diagram of the structure enlargement at the center A;

[0040] Figure 6 It is a partial cross-sectional structural schematic diagram of the console and the storage rod according to the embodiment of the present disclosure being arranged in a FIB instrument;

[0041] Figure 7 It is a structural schematic diagram of the console and the preservation rod of the embodiment of the present disclosure after being assembled, the vacuum chamber is in a closed state and the sample part is retracted into the outer tube;

[0042] Figure 8 This is a structural schematic diagram of the console and the storage rod of the embodiment of the present disclosure after being assembled, with the vacuum chamber in an open state and the sample portion extending out of the outer tube;

[0043] Fig. 9 It is a structural schematic diagram of the storage rod and the control handle according to the embodiment of the present disclosure when they are installed on the installation platform and the moving platform respectively;

[0044] Fig.10 for Fig. 9 A schematic diagram of the structure enlarged at B in the middle;

[0045] Fig.11 This is a schematic diagram of the structure of the vacuum chamber in an open state according to an embodiment of the present disclosure;

[0046] Fig.12 This is a schematic diagram of the structure of the vacuum chamber in a closed state according to an embodiment of the present disclosure;

[0047] Fig.13 The present invention is a flow chart of the sample preparation method described in the embodiment of the present invention.

[0048] Among them, 1. preservation rod; 11. outer tube; 12. inner rod; 13. sample part; 14. connection part; 15. sealing ring; 16. comb teeth; 2. control handle; 21. handle body; 22. core rod; 23. rotating tube; 3. control console; 31. base; 32. vacuum chamber; 321. external tube; 322. movable rod; 323. storage part; 324. vacuum sealing ring; 33. driving device; 34. first mounting part; 35. second mounting part; 4. FIB instrument; 41. blind plate; 42. remote control; 51. connecting bracket; 52. mounting table; 53. moving table. DETAILED DESCRIPTION

[0049] In order to more clearly understand the above-mentioned objectives, features and advantages of the present disclosure, the scheme of the present disclosure will be further described below. It should be noted that the embodiments of the present disclosure and the features in the embodiments can be combined with each other without conflict.

[0050] In the following description, many specific details are set forth to facilitate a full understanding of the present disclosure, but the present disclosure may also be implemented in other ways different from those described herein; it is obvious that the embodiments in the specification are only part of the embodiments of the present disclosure, rather than all of the embodiments.

[0051] Reference Figures 1 to 12 As shown, the embodiment of the present disclosure provides a sample vacuum transfer system, including a storage rod 1, a control handle 2 and a control console 3; the storage rod 1 includes an inner rod 12 and an outer tube 11 movably sleeved on the outer side of the inner rod 12, and the two ends of the inner rod 12 are respectively formed with a connecting portion 14 and a sample portion 13 for storing samples, and the two ends of the sample portion 13 are respectively provided with sealing rings 15, and the two sealing rings 15 can be sealed and connected with the inner wall of the outer tube 11 to enclose a first sealed space, and the inner rod 12 can move relative to the outer tube 11 to drive the sample portion 13 to extend and retract the outer tube 11; the control console 3 comprises a driving device 33, a base 31 for being installed in the FIB instrument 4 and a vacuum chamber 32 for storing samples, wherein the driving device 33 and the vacuum chamber 32 are arranged on the base 31 and are connected to each other; when the preservation rod 1 is inserted into the TEM detector, the control handle 2 is detachably connected to the outer tube 11 and the connecting portion 14 to drive the inner rod 12 to move; when the preservation rod 1 is arranged in the FIB instrument 4, the outer tube 11 is detachably connected to the base 31, and the driving device 33 is detachably connected to the connecting portion 14 to drive the inner rod 12 to move and the vacuum chamber 32 to be opened and closed.

[0052] Specifically, the outer tube 11 can be selected as a straight tube, the interior of the outer tube 11 has an active channel that penetrates the outer tube 11, the inner rod 12 is inserted in the active channel, and there is a gap between the surface of the inner rod 12 and the inner wall of the active channel, so that the inner rod 12 can move along the active channel, or the diameter of the sealing rings 15 at both ends of the sample part 13 is larger than the diameter of the inner rod 12, so that after the sample part 13 is located in the active channel inside the outer tube 11, the surface of the sealing ring 15 abuts against the inner wall of the active channel, so that the sealing ring 15 is sealed and connected to the inner wall of the active channel.

[0053] The above-mentioned inner rod 12 is a straight rod, and a slot can be optionally set at one end of the inner rod 12 as the connecting part 14. A movable part is provided on the control handle 2, and the movable part can be moved relative to the control handle, and the movable part is connected to the slot by a snap-on connection; of course, the connecting part 14 can also be selected as a thread, and a nut that can move relative to the control handle is provided on the control handle 2, and the nut is threadedly connected to the connecting part 14.

[0054] The above-mentioned sample part 13 can be selected as a block structure, and the extension direction of the sample part 13 is consistent with the extension direction of the inner rod 12. A groove can be selected to be set on the sample part 13 so that the sample can be placed in the groove. Of course, a tray or a metal carrier can also be set on the block structure of the sample part 13 so that the sample can be set on the tray or the metal carrier; two sealing rings 15 are set at both ends of the sample part 13 along the extension direction of the inner rod 12, so that after the sample part 13 is located inside the outer tube 11, the two sealing rings 15 can abut against the inner wall of the outer tube 11 and be sealed, and the space between the two sealing rings 15 forms a first sealed space.

[0055] The length of the inner rod 12 can be selected to be greater than the length of the outer tube 11, so that the sample portion 13 and the connecting portion 14 of the inner rod 12 can be simultaneously exposed on the outside of the outer tube 11. Of course, the length of the inner rod 12 can also be selected to be equal to or less than the length of the outer tube 11, so that when the sample portion 13 is located on the outside of the outer tube 11, the connecting portion 14 is located inside the outer tube 11, as long as the connecting portion 14 can be connected to the driving device 33 and the control handle 2, the inner rod 12 can move relative to the outer tube 11.

[0056] The above-mentioned console 3 can be installed in the FIB instrument 4 through the base 31. When the base 31 is separated from the FIB instrument 4, the console 3 can be placed in the glove box. The base 31 can be selected as a block or a disk structure. Screw holes or bolts can be set on the base 31 so that the base 31 can be detachably installed in the FIB instrument 4; the vacuum chamber 32 can be detachably connected to the base 31 by bolts. Of course, a clamp can also be set on the base 31, and the vacuum chamber 32 is clamped on the base 31.

[0057] The above-mentioned vacuum chamber 32 can be optionally provided with a chamber door, which is connected to the driving device 33 so that the driving device 33 can drive the vacuum chamber 32 to open or close; of course, the vacuum chamber 32 can also be selected to include an external tube 321 and a movable rod 322, the external tube 321 is movably sleeved on the outside of the movable rod 322, and the movable rod 322 is provided with a storage part 323 for the user to place samples, and vacuum sealing rings 324 are provided at both ends of the storage part 323. After the movable rod 322 moves relative to the external tube 321, so that the storage part 323 is located in the outer tube 11, the two vacuum sealing rings 324 can be sealed and connected to the outer tube 11, so that the space between the two vacuum sealing rings 324 forms a second sealed space, and the driving device 33 drives the movable rod 322 to move relative to the external tube 321, so that when the storage part 323 is exposed on the outside of the external tube 321, the vacuum chamber 32 is in an open state, and the storage part 323 is located on the inner side of the external tube 321, and when it is located in the second sealed space, the vacuum chamber 32 is in a closed state.

[0058] The above-mentioned control handle 2 can be selected to have a movable part that can move relative to the control handle 2. The movable part is detachably connected to the connecting part 14, and the movable part can move relative to the control handle 2 along the extension direction of the inner rod 12. The outer tube 11 is detachably connected to the control handle 2, so that when the movable part moves relative to the control handle 2, it can drive the inner rod 12 to move.

[0059] A buckle can be optionally provided on the above-mentioned control handle 2, and the end of the outer tube 11 close to the control handle 2 can be connected with the buckle. Of course, a rotating tube 23 can also be optionally provided on the control handle 2, and the rotating tube 23 is rotatably connected to the control handle 2. The end of the outer tube 11 close to the control handle 2 is provided with a thread, and the end of the rotating tube 23 away from the control handle 2 is provided with a thread, so that the rotating tube 23 and the outer tube 11 are threadedly connected.

[0060] The above-mentioned FIB instrument can be selected to be an ion beam emission device installed on a scanning electron microscope (SEM) to make the scanning electron microscope have FIB function. The FIB instrument is equipped with a probe, and the user can operate the probe to take the sample. Since the size of the sample required for TEM detection is very small, when preparing the sample before TEM detection, the sample to be prepared needs to be cut and thinned to one millimeter or 0.5 mm, so as to facilitate the subsequent use of ion beam to continue thinning the sample to be prepared. Since the sample to be prepared needs to be in a very air environment when rotating and moving, the sample to be prepared is usually placed in alcohol or a sealed cylinder, and the sample to be prepared and the stage for FIB are placed in a glove box. The sample to be prepared is transferred by hand or tweezers in the glove box. Since the glove box affects the operating accuracy and the thickness of the sample to be prepared is very small, it is easy to cause the sample to be damaged and contaminated when transferring the sample to be prepared.

[0061] Using the sample vacuum transfer system provided by the present application, the sample to be prepared is placed in the vacuum chamber 32, the console 3, the vacuum chamber 32 and the preservation rod 1 are placed in the FIB instrument 4, the inside of the FIB instrument 4 is evacuated, and then the vacuum chamber 32 is opened by the driving device 33 and the sample part 13 is extended out of the outer tube 11. In the vacuum environment in the FIB instrument 4, the sample to be prepared is placed on the sample part 13 extending out of the outer tube 11 using a probe, and the FIB instrument 4 uses an ion beam to thin the sample to be prepared on the sample part 13, and the sample on the sample part 13 is thinned to more than ten nanometers. After the sample preparation is completed, the sample part 13 is driven back into the outer tube 11, and the sample part 13 is protected in the first sealed space. The preservation rod 1 is taken out of the FIB instrument 4 and inserted into the TEM detector. The preservation rod 1 is connected to the control handle 2, and the TEM detector is evacuated. The control handle 2 controls the sample part 13 to extend out of the outer tube 11, so that the sample part 13 is located inside the TEM detector for transmission detection. The sample is protected by the preservation rod 1 during the entire process from the completion of sample preparation to entering the TEM detector, so that the sample is isolated from the external gas environment to prevent the sample from being oxidized and contaminated.

[0062] A buckle or a slot can be optionally provided on the base 31, and the outer tube 11 is snapped into the buckle or the slot, so that the outer tube 11 is detachably connected to the base 31, and the connecting portion 14 is connected to the driving device 33. When the driving device 33 drives the vacuum chamber 32 to open, the driving device 33 synchronously drives the inner rod 12 to move relative to the outer tube 11 so that the sample portion 13 extends out of the outer tube 11.

[0063] The above-mentioned driving device 33 can be selected to include a motor and a pull rod. A protrusion is arranged on the base 31, and a through hole is arranged on the protrusion. The through hole is arranged along the length direction of the base 31. The pull rod is slidably connected with the through hole. The motor is arranged on the base 31. The motor and the pull rod can be selected to cooperate with each other through a gear and a rack so that the motor can drive the pull rod to move along the length direction of the base 31. The preservation rod 1 is arranged on the base 31 along the length direction of the base 31, so that the pull rod is connected to the connecting part 14, and the door of the vacuum chamber 32 or one end of the movable rod 322 is connected to the pull rod, so that when the pull rod is driven by the motor to move, the pull rod drives the vacuum chamber 32 to open and extend the sample part 13.

[0064] Of course, the driving device 33 can also be selected as a motor, the motor has a telescopic end, the telescopic end can be arranged along the length direction of the base 31, the outer tube 11 is arranged along the length direction of the base 31, and the telescopic end is connected to the vacuum chamber 32 and the connecting part 14, so that the motor drives the telescopic end to extend along the length direction of the base 31, thereby driving the vacuum chamber 32 to open and extend the sample part 13.

[0065] When the sample vacuum transfer system provided by the embodiment of the present disclosure is used, the preservation rod 1 is installed on the console 3, the sample to be prepared and the console 3 installed with the preservation rod 1 are placed in a glove box, the glove box is evacuated, and in the glove box with a vacuum environment, the sample is placed in a vacuum chamber 32, the outer tube 11 is installed on the base 31, the connecting part 14 is detachably connected to the driving device 33, and the driving device 33 drives the vacuum chamber 32 to close, and drives the sample part 13 to retract into the outer tube 11.

[0066] The glove box is opened, and the console 3 is taken out and placed inside the FIB instrument 4. The inside of the FIB instrument 4 is evacuated to form a vacuum environment. The driving device 33 drives the vacuum chamber 32 to open and drives the sample part 13 to extend out of the outer tube 11. The probe of the FIB instrument 4 moves the sample in the vacuum chamber 32 to the sample part 13, and uses an ion beam to thin the sample ions in the sample part 13 to perform sample preparation operations.

[0067] After the sample preparation operation is completed for the sample in the sample part 13, the driving device 33 drives the sample part 13 to retract into the outer tube 11, the FIB instrument 4 is opened, the preservation rod 1 is taken out, and the control handle 2 is detachably connected to the outer tube 11 and the inner rod 12 of the preservation rod 1.

[0068] The preservation rod 1 detachably connected with the control handle 2 is inserted into the TEM detector, the interior of the TEM detector is evacuated, and the control handle 2 drives the inner rod 12 to move relative to the outer tube 11, so that the sample part 13 extends out of the outer tube 11 and is located in the TEM detector, and TEM detection is performed on the sample in the sample part 13.

[0069] The sample vacuum transfer system provided by the embodiment of the present disclosure includes a preservation rod 1, a control handle 2 and a control console 3; the preservation rod 1 includes an inner rod 12 and an outer tube 11 movably sleeved on the outer side of the inner rod 12, and the two ends of the inner rod 12 are respectively formed with a connecting portion 14 and a sample portion 13 for storing the sample, and the two ends of the sample portion 13 are respectively provided with a sealing ring 15, and the two sealing rings 15 can be sealed and connected with the inner wall of the outer tube 11 to enclose a first sealed space, and the inner rod 12 can move relative to the outer tube 11 to drive the sample portion 13 to extend and retract the outer tube 11, so that the sample portion 13 is in the first sealed space in the outer tube 11 to avoid the sample in the sample portion 13 from contacting the external gas environment; the control console 3 includes a driving device 33, a base 31 for installation in the FIB instrument 4 and a vacuum chamber 32 for storing the sample, and the driving device 33 and the vacuum chamber 32 are arranged on the base 31 and are connected to each other; when the preservation rod 1 is inserted into the TEM detector, the control handle 2 is connected with the outer tube 11 and the connecting portion 14 is detachably connected so that the control handle 2 can drive the inner rod 12 to move so that the sample part 13 extends out of the outer tube 11 for TEM detection; when the preservation rod 1 is set in the FIB instrument 4, the outer tube 11 is detachably connected to the base 31, and the driving device 33 is detachably connected to the connecting part 14 to drive the inner rod 12 to move and the vacuum chamber 32 to be opened and closed, so that the sample placed in the vacuum chamber 32 can be transferred to the extended sample part 13 in the vacuum environment of the FIB instrument for ion beam thinning, and the sample after ion beam thinning is completed is stored in the first sealed space as the sample part 13 is retracted into the outer tube 11; through the cooperation of the preservation rod 1, the control handle 2 and the control console 3, the sample is in a vacuum environment during the whole process from the completion of sample preparation in the FIB instrument to the placement into the TEM detector for detection, thereby avoiding oxidation and contamination of the sample during the process of placing the sample into the TEM detector after sample preparation is completed, thereby improving the accuracy of TEM detection of the sample.

[0070] Reference Figure 6 , Figure 7 and Figure 8As shown, in some embodiments, the base 31 is provided with a first mounting portion 34 and a second mounting portion 35 which are spaced apart along the width direction of the base 31, the vacuum chamber 32 is detachably connected to the first mounting portion 34, the preservation rod 1 is detachably connected to the second mounting portion 35, and the driving device 33 is arranged between the first mounting portion 34 and the second mounting portion 35 and is respectively connected to the vacuum chamber 32 and the connection portion 14. In this arrangement, the sample to be prepared can be placed in the vacuum chamber 32 first and then the vacuum chamber 32 can be installed on the first mounting portion 34, which is convenient for placing the sample to be prepared in the vacuum chamber 32 in the glove box, and the driving device 33 is arranged between the first mounting portion 34 and the second mounting portion 35, so that the driving device 33 can be connected to the vacuum chamber 32 on the first mounting portion 34 and the preservation rod 1 on the second mounting portion 35 at the same time, so that the driving device 33 can simultaneously drive the opening and closing of the vacuum chamber 32 and the extension and retraction of the sample portion 13.

[0071] Specifically, the first mounting portion 34 and the second mounting portion 35 can be selected to be two clamping claws respectively, and the two clamping claws are arranged at intervals along the width direction of the base 31, and the driving device 33 is arranged between the two clamping claws, so that the driving device 33 is convenient to be connected with the vacuum chamber 32 on the first mounting portion 34 and the connecting portion 14 of the preservation rod 1 on the second mounting portion 35 respectively; of course, it is also possible to select a protrusion on the base 31, and two through grooves are formed on the protrusion as the first mounting portion 34 and the second mounting portion 35 respectively, and the through groove passes through the protrusion along the length direction of the base 31, and the vacuum chamber 32 is clamped in the through groove of the first mounting portion 34, and a limiting plate that can slide along the width direction of the base 31 can be selected in the through groove of the second mounting portion 35, and the outer tube 11 is arranged in the through groove of the second mounting portion 35, and the limiting plate is slid so that the limiting plate and the side wall of the through groove of the second mounting portion 35 clamp the outer tube 11, so that the preservation rod 1 is detachably connected to the second mounting portion 35.

[0072] A through hole can be optionally set between the two raised through grooves of the base 31, and the driving device 33 is provided with a telescopic end, which passes through the raised through hole and is connected to the vacuum chamber 32 and the connecting part 14. Of course, the driving device 33 can also be selected to include a motor and a pull rod, the pull rod is passed through the raised through hole, and the end of the pull rod is connected to the vacuum chamber 32 and the connecting part 14, so that when the motor drives the pull rod to move, the pull rod moves to drive the vacuum chamber 32 to open and close, and drive the sample part 13 to extend and retract the outer tube 11.

[0073] Reference Figure 6 , Figure 7 and Figure 8 As shown, in some embodiments, the driving device 33 includes a sliding member and a driving member;

[0074] The sliding member is slidably connected to the base 31 along the length direction of the base 31, the driving member is arranged on the base 31 and connected to the sliding member, the storage rod 1 is detachably connected to the base 31 along the length direction of the base 31, and the sliding member is detachably connected to the vacuum chamber 32 and the connecting portion 14;

[0075] The driving member drives the sliding member to slide relative to the base 31 to drive the vacuum chamber 32 to open and close, and to drive the sample part 13 to extend and retract into the outer tube 11. In this way, the driving member can drive the sliding member to slide along the length direction of the base 31, so that the sliding member can simultaneously drive the inner rod 12 to move and drive the vacuum chamber 32 to open and close when sliding, so that when the console 3 and the preservation rod 1 are set together in the FIB instrument, the driving member can simultaneously open the vacuum chamber 32 and extend the sample part 13 out of the outer tube 11 through the sliding member, so that the user can move the sample in the vacuum chamber 32 to the sample part 13 through the probe in the FIB instrument, and after the sample on the sample part 13 is thinned by ion beam, the driving member can close the vacuum chamber 32 through the sliding member, and at the same time retract the sample part 13 into the outer tube 11, so that the sample in the sample part 13 is in the first closed space, and when the preservation rod 1 is transferred to the TEM detector, the sample on the sample part 13 is always protected in the first closed space to avoid oxidation and contamination of the sample on the sample part 13.

[0076] Specifically, the sliding member can be selected as a rod-shaped structure, the driving member can be selected to include a motor or a cylinder, and a hollow sleeve can be selected to be provided on the base 31. The sliding member is inserted into the channel, and the sleeve is arranged along the length direction of the base 31, so that when the sliding member slides relative to the sleeve, the sliding member slides along the length direction of the base 31; of course, a convex structure can also be selected to be provided on the base 31, and a through hole along the length direction of the base 31 is provided on the convex structure, and the sliding member is inserted into the through hole, so that when the sliding member slides relative to the convex structure, the sliding member can slide along the length direction of the base 31. After the driving member is started, power is output to the sliding member, and the sliding member slides relative to the base 31 along the length direction of the base 31.

[0077] The storage rod 1 is installed on the base 31 along the length direction of the base 31, and the connecting portion 14 is connected to the sliding member, so that when the sliding member slides along the length direction of the base 31, it can drive the inner rod 12 to move relative to the outer tube 11, so that the sliding of the sliding member drives the sample portion 13 to extend and retract into the outer tube 11. The sliding member is connected to the door of the vacuum chamber 32 or the movable rod 322 of the vacuum chamber 32, so that when the sliding member slides, the door of the vacuum chamber 32 can be opened and closed, or the sliding member can push the movable rod 322 to move so that the storage portion 323 is located outside and inside the external tube 321, so as to realize the operation of opening and closing the vacuum chamber 32.

[0078] Reference Figure 6 , Figure 7 , Figure 8 , Fig.11 and Fig.12 As shown, in some embodiments, the vacuum chamber 32 includes an external tube 321 and a movable rod 322;

[0079] The external tube 321 is movably sleeved on the outside of the movable rod 322. The movable rod 322 is formed with a storage portion 323 for placing samples. The movable rod 322 is provided with two vacuum sealing rings 324. The two vacuum sealing rings 324 are respectively located at the two ends of the storage portion 323 along the extension direction of the movable rod 322. The movable rod 322 can move relative to the external tube 321 to drive the storage portion 323 to move between the inside and the outside of the external tube 321.

[0080] When the storage part 323 is located in the external tube 321, the two vacuum sealing rings 324 are both sealed and connected to the inner wall of the external tube 321 to jointly enclose a second sealed space;

[0081] The external tube 321 and the movable rod 322 are arranged along the length direction of the base 31, and one end of the movable rod 322 is connected to the sliding member.

[0082] Specifically, the external tube 321 is a hollow straight tube, the movable rod 322 is a straight rod, and a groove is provided on the side of the movable rod 322 as a storage part 323. The movable rod 322 moves relative to the external tube 321 along the extension direction of the external tube 321, so that the storage part 323 can move between the position inside and outside the external tube 321. When the storage part 323 is located inside the external tube 321, the two vacuum sealing rings 324 abut against the inner wall of the external tube 321 to be sealed, so that the space between the two vacuum sealing rings 324 forms a second sealed space. In this way, after the movable rod 322 is connected to the sliding member, the sliding of the sliding member can simultaneously drive the movable rod 322 and the inner rod 12 to move, so that the sliding member can slide along the length direction of the base 31 to conveniently realize that the storage part 323 is located outside the external tube 321 and the sample part 13 extends out of the external tube 11, so that the user can use the probe storage part 323 of the FIB instrument to move the sample to the sample part 13.

[0083] The above-mentioned storage portion 323 may optionally include a groove, and the sample to be prepared is placed in the groove; of course, the storage portion 323 may also be selected to include two limiting plates, which are arranged opposite to each other, and the sample to be prepared is placed between the two limiting plates and abutted against the opposite side of the two limiting plates, so that the sample to be prepared is stably placed on the storage portion 323.

[0084] The above-mentioned external tube 321 and movable rod 322 are arranged along the length direction of the base 31, and the storage rod 1 is also arranged along the length direction of the base 31. When the sliding member is connected to the movable rod 322 and the connecting part 14, the sliding member moves along the length direction of the base 31, and the sliding member can drive the movable rod 322 and the inner rod 12 to move along the length direction of the base 31. Since the external tube 321 and the outer tube 11 are arranged on the base 31, the sliding of the sliding member can drive the storage part 323 to move between the inside and the outside of the external tube 321. At the same time, the sliding member can also drive the sample part 13 to extend and retract the outer tube 11, so that the storage part 323 is in the second sealed space when it is inside the external tube 321 to protect the sample to be prepared on the storage part 323.

[0085] When the sample portion 13 extends out of the outer tube 11 and the storage portion 323 is located outside the external tube 321, the probe of the FIB instrument can move the sample to be prepared on the storage portion 323 to the sample portion 13, so that the sample to be prepared is subjected to ion beam thinning on the sample portion 13. After the sample on the sample portion 13 completes the sample preparation operation of ion beam thinning, the sliding part moves to drive the sample portion 13 to retract into the outer tube 11, so that the sample can be located in the first sealed space after ion beam thinning to be protected.

[0086] Reference Figure 1 , Figure 2 , Fig. 9 and Fig.10 As shown, in some embodiments, the control handle 2 includes a handle body 21 and a core rod 22;

[0087] The handle body 21 is provided with an installation channel, the core rod 22 is inserted in the installation channel, the outer tube 11 is detachably connected to one side of the handle body 21, and the end of the core rod 22 close to the outer tube 11 is detachably connected to the connecting portion 14. With such a configuration, the handle body 21 can keep the outer tube 11 in a stable position, and the user can control the movement of the core rod 22 to control the sample part 13 to extend out of the outer tube 11. When the preservation rod 1 is inserted into the TEM detector, the control handle 2 can be on the outside of the TEM detector, so that the user can push the core rod 22 to push the sample part 13 out of the outer tube 11 to perform TEM detection, and realize that after the preservation rod 1 is removed into the TEM detector, the sample part 13 is controlled to extend and retract into the outer tube 11 through the cooperation of the core rod 22 and the handle body 21.

[0088] Specifically, the handle body 21 can be selected as a columnar structure, and of course, it can also be selected as a rectangular structure. The installation channel on the handle body 21 runs through the handle body 21. The core rod 22 is a straight rod. One end of the core rod 22 can be selected to be detachably connected to the connecting part 14, and the other end can be selected to be provided with a handle rod. The handle rod is set perpendicular to the extension direction of the core rod 22. The core rod 22 can move relative to the handle body 21 along the installation channel, and the core rod 22 can rotate in the installation channel.

[0089] A buckle can be optionally provided on the side of the handle body 21 facing the outer tube 11, so that the end of the outer tube 11 close to the handle body 21 is snapped into the buckle. Of course, a rotatable rotating tube 23 can also be provided on the side of the handle body 21 facing the outer tube 11, and a thread is provided on the rotating tube 23. A screw hole is provided on the side of the outer tube 11 close to the handle body 21. The rotating tube 23 is coaxially arranged with the installation channel, and the rotating tube 23 is rotatably connected to the handle body 21, so that the rotating tube 23 and the outer tube 11 are detachably connected through threads.

[0090] After the above-mentioned preservation rod 1 is inserted into the TEM detector, the outer tube 11 is detachably connected to the handle body 21, and the connecting part 14 of the inner rod 12 is connected to the core rod 22. The user pushes the core rod 22 to make the sample part 13 extend out of the outer tube 11, so that the sample part 13 can be TEM detected in the TEM detector after it extends out of the outer tube 11.

[0091] Reference Figure 1 , Figure 2 , Fig. 9 and Fig.10 As shown, in some embodiments, a rotating tube 23 is provided on the side of the handle body 21 facing the outer tube 11, and the rotating tube 23 is rotatably connected with the handle body 21. An avoidance channel is provided in the rotating tube 23, and the avoidance channel is coaxially arranged with the installation channel. The core rod 22 is inserted into the avoidance channel and the installation channel to be connected with the connecting portion 14. The end of the rotating tube 23 close to the outer tube 11 is provided with a thread, and the rotating tube 23 is threadedly connected with the outer tube 11. In this way, the rotating tube 23 can be rotated relative to the handle body 21, so that the connecting portion 14 can be connected with the core rod 22 first, and then the handle body 21 is moved to make the rotating tube 23 fit with the end of the outer tube 11. The rotating tube 23 can be rotated to make the outer tube 11 and the rotating tube 23 threadedly connected, so as to avoid the inner rod 12 rotating toward the outer tube 11 and destroying the contact between the sealing ring 15 and the inner wall of the outer tube 11, thereby improving the convenience of the detachable connection between the outer tube 11 and the control handle 2.

[0092] Specifically, the rotating tube 23 can be selected as a hollow straight tube, and the space inside the rotating tube 23 is the avoidance channel. A bearing can be selected to be set inside the installation channel, and one end of the rotating tube 23 is inserted into the installation channel and connected to the bearing, so that the rotating tube 23 is rotatably connected to the handle body 21, and the avoidance channel inside the rotating tube 23 is coaxial with the installation channel, so that the core rod 22 passing through the installation channel can pass through the avoidance channel and the installation channel; of course, it is also possible to choose to set a bearing on the side surface of the handle body 21 facing the outer tube 11, the outer ring of the bearing is connected to the handle body 21, the inner ring of the bearing is connected to one end of the rotating tube 23, the bearing is coaxial with the installation channel, and the rotating tube 23 is coaxial with the bearing, so that the core rod 22 passing through the installation channel can pass through the avoidance channel and the installation channel.

[0093] The above-mentioned rotating tube 23 can be optionally provided with threads on the inner wall of the end away from the handle body 21, and threads are provided on the outer side of the outer tube 11 facing the handle body 21, so that the rotating tube 23 and the outer tube 11 at one end close to each other are threadedly connected to each other; however, it is also possible to choose to provide threads on the outer side of the rotating tube 23 away from the handle body 21, and provide threads on the inner wall of the end close to the outer tube 11, so that the rotating tube 23 and the outer tube 11 at one end close to each other are threadedly connected to each other.

[0094] Reference Figure 1 , Figure 2 , Fig. 9 and Fig.10 As shown, in some embodiments, a hook is provided at one end of the core rod 22 facing the inner rod 12, and the connecting portion 14 includes a slot, and the hook is connected to the slot by a snap connection. In this way, the snap connection between the hook and the slot can drive the inner rod 12 to move when the core rod 22 moves, thereby improving the convenience of the detachable connection between the core rod 22 and the inner rod 12.

[0095] Specifically, a hook can be set at one end of the core rod 22 facing the inner rod 12, and the connecting part 14 includes a groove formed on the side of the inner rod 12. The core rod 22 can be moved along the radial direction of the inner rod 12 to allow the hook to be inserted into or leave the groove. After the hook is inserted into the groove, the core rod 22 moves along the length direction of the inner rod 12, and the hook abuts against the inner wall of the groove to drive the inner rod 12 to move relative to the outer tube 11 along the length direction of the inner rod 12.

[0096] Reference Figure 1 , Figure 2 , Fig. 9 and Fig.10 As shown, in some embodiments, the sample vacuum transfer system further includes a connecting bracket 51, a mounting platform 52 and a moving platform 53, the mounting platform 52 and the moving platform 53 are arranged on one side of the connecting bracket 51, and the mounting platform 52 and the moving platform 53 are arranged opposite to each other along a first direction, the moving platform 53 is slidably connected with the bracket along the first direction, the mounting platform 52 is movably connected with the connecting bracket 51, the mounting platform 52 can slide relative to the connecting bracket 51 along the first direction and the second direction, and the mounting platform 52 can be lifted and lowered along a third direction, and the first direction, the second direction and the third direction are perpendicular to each other;

[0097] The handle body 21 is connected to the moving platform 53, the storage rod 1 is installed on the mounting platform 52 along the first direction, and the connecting portion 14 is exposed on the side of the mounting platform 52 along the first direction toward the moving platform 53. In this way, after the storage rod 1 is installed on the mounting platform, the mounting platform 52 moves relative to the connecting bracket 51 along the first direction, the second direction and the third direction to challenge the spatial position of the storage rod 1, so that the storage rod 1 is precisely coaxial with the core rod 22 of the control handle 2 on the moving platform 53, and the moving platform 53 moves toward the mounting platform 52, so that the control handle 2 and the storage rod 1 are close to each other and conveniently connected to each other detachably.

[0098] Specifically, Fig. 9 The directions indicated by the middle arrows are respectively the first direction a, the second direction b and the third direction c; the first direction a can be selected as the length direction of the connecting bracket 51, the second direction b can be selected as the width direction of the connecting bracket 51, and the third direction c can be selected as the height direction of the connecting bracket 51.

[0099] The above-mentioned mounting platform 52 may optionally include a sliding base and a moving block. The sliding base is slidably connected to the connecting bracket 51 along a first direction. The moving block is slidably arranged on the connecting bracket 51 along a second direction. A lifting platform is provided on the moving block. The lifting platform is slidably connected to the moving block along a third direction. A driving device may be optionally arranged between the sliding base and the connecting bracket 51, a driving device is arranged between the sliding base and the moving block, and a driving device is arranged between the lifting platform and the moving block, so that the driving device can drive the sliding base to slide relative to the connecting bracket 51 in the first direction, the moving block to slide relative to the sliding base in the second direction, the lifting platform to slide relative to the moving block in the third direction, and the storage rod 1 is connected to the moving block.

[0100] The above-mentioned driving device can select a matching structure of a screw and a nut, the screw is arranged on the connecting bracket 51 along the first direction, the nut is threadedly connected to the screw and connected to the sliding base, so that the screw rotates to drive the nut to drive the sliding base to slide relative to the connecting bracket 51 along the first direction; the screw is arranged on the sliding base along the second direction, the nut is threadedly connected to the screw and connected to the moving block, so that the screw rotates to drive the nut to drive the moving block to slide relative to the sliding base along the second direction; the screw is arranged on the moving block along the second direction, the nut is threadedly connected to the screw and connected to the lifting platform, so that the screw rotates to drive the nut to drive the lifting platform to slide relative to the moving block along the third direction.

[0101] A clamping claw can be optionally provided on the above-mentioned lifting platform so that the storage rod 1 can be clamped and connected with the clamping claw. Of course, a plug-in hole can also be optionally provided on the lifting platform. The plug-in hole is arranged along the first direction. The storage rod 1 can be inserted into the plug-in hole, and the outer tube 11 abuts against the inner wall of the plug-in hole so that the storage rod 1 can be stably inserted in the plug-in hole.

[0102] The connection bracket 51 may be provided with a track along the first direction, and the moving platform 53 is slidably connected to the track, so that the moving platform 53 can move along the first direction to approach or move away from the mounting platform 52 .

[0103] Reference Figure 1 , Figure 2 , Figure 3 , Figure 4 and Figure 5 As shown, in some embodiments, comb teeth 16 are provided in the sample portion 13, and the sample is connected to the comb teeth 16. In this way, the comb teeth 16 can guide the charge generated by the sample due to the impact of the ion beam while fixing the sample, thereby preventing the charge from accumulating on the sample and ensuring that the sample thinned by the ion beam can be stably set on the sample portion 13.

[0104] Specifically, the comb teeth 16 are multiple sheet structures made of metal, and the multiple sheet structures intersect each other so that the sample can be clamped between the intersecting metal sheets. The comb teeth 16 can fix the sample and guide the charge generated by the sample due to the impact of the ion beam to avoid the accumulation of charge on the sample.

[0105] Reference Figure 1 , Figure 2 , Figure 3 , Figure 4 and Figure 5 As shown, in some embodiments, the console 3 further includes a controller, which is connected to the driving device 33. The controller controls the driving device 33 to open and close the vacuum chamber 32, and the controller controls the driving device 33 to drive the sample part 13 to extend and retract the outer tube 11. This configuration enables the controller to control the console 3 in the FIB instrument, so that after the FIB instrument is evacuated, the user controls the driving device 33 to open and close the vacuum chamber 32 and extend and retract the sample part 13 to the outer tube 11, so as to facilitate the movement of the sample in the vacuum chamber 32 to the sample part 13, and the sample on the sample part 13 that has completed ion beam thinning is located in the first sealed space, so as to achieve the protection effect on the sample.

[0106] Specifically, the controller can be selected as a circuit board or a chip, and the controller can be connected to the drive device 33 through a wire. Of course, it is also possible to provide a wireless signal receiver and transmitter on both the controller and the drive device 33 so that the controller and the drive device 33 are wirelessly connected.

[0107] The controller sends a signal to the driving device 33, so that the driving device 33 can drive the vacuum chamber 32 to open, and at the same time drive the sample part 13 to extend the outer tube 11, so as to transfer the sample in the vacuum chamber 32 to the sample part 13. After the sample on the sample part 13 completes ion beam thinning, the controller sends a signal to the driving device 33. After receiving the signal, the driving device 33 drives the vacuum chamber 32 to close and the sample part to retract the outer tube 11, so that the sample after completing ion beam thinning is in the first sealed space.

[0108] Fig. 9 As shown, a blind plate 41 can be optionally provided on the FIB instrument, a connecting hole is provided on the blind plate 41, a remote controller 42 is used as a controller, a connecting wire is provided on the remote controller, and the connecting wire passes through the connecting hole and is electrically connected to the console 3, so that the remote controller 42 controls the driving device 33, and the connecting wire is sealed and connected to the connecting hole, so that the interior of the FIB instrument can be vacuumed.

[0109] Reference Figures 1 to 13 As shown, the embodiment of the present disclosure also provides a sample preparation method, using the sample vacuum transfer system as described in any one of the above items, comprising:

[0110] The sample, the preservation rod 1 and the control console 3 are placed in a glove box in a vacuum environment, the sample is placed in the vacuum chamber 32, the outer tube 11 is installed on the base 31, the connecting part 14 is detachably connected to the driving device 33, the driving device 33 drives the vacuum chamber 32 to close, and drives the sample part 13 to retract into the outer tube 11; wherein the sample is placed in the storage part 323 of the vacuum chamber 32, the outer tube 11 is installed on the second installation part 35 on the base 31, the connecting part 14 is detachably connected to the sliding part of the driving device 33, the driving device 33 drives the movable rod 322 to move, so that the storage part 323 is located inside the external tube 321 and is in the second sealed space, and the driving device 33 simultaneously drives the sample part 13 to retract into the outer tube 11, and at this time the sample is located in the second sealed space in a vacuum state.

[0111] The control console 3 is taken out of the glove box and placed in the interior of the FIB instrument 4. The interior of the FIB instrument 4 is evacuated to form a vacuum environment. The driving device 33 drives the vacuum chamber 32 to open and drives the sample part 13 to extend out of the outer tube 11. The probe of the FIB instrument 4 moves the sample in the vacuum chamber 32 to the sample part 13, and uses the ion beam to perform sample preparation operations on the sample in the sample part 13; wherein a controller is used to control the driving device 33, so that the driving device 33 drives the movable rod 322 to move, so that the storage part 323 is located outside the external tube 321, and drives the sample part 13 to extend out of the outer tube 11; the probe of the FIB instrument 4 is used to transfer the sample to the comb teeth 16 of the sample part 13, and uses the ion beam to perform a thinning operation on the sample on the comb teeth 16.

[0112] After the sample on the sample part 13 completes the sample preparation operation, the driving device 33 drives the sample part 13 to retract into the outer tube 11, the FIB instrument 4 is opened, the preservation rod 1 is taken out, and the control handle 2 is detachably connected to the outer tube 11 and the inner rod 12 of the preservation rod 1; after the sample on the sample part 13 completes the thinning operation, the driving device 33 drives the sample part 13 to retract into the outer tube 11, so that the sample on the sample part 13 is in the first sealed space; the FIB instrument 4 is opened, and the outer tube 11 is separated from the second mounting part 35.

[0113] When the above-mentioned storage rod 1 and control handle 2 are detachably connected, the storage rod 1 is taken out of the FIB instrument 4 and installed on the mounting table 52, and the control handle 2 is installed on the moving table 53. The mounting table 52 moves relative to the connecting bracket 51 in the first direction, the second direction and the third direction, so that the inner rod 12 is coaxial with the core rod 22, and the moving table 53 is driven to move toward the mounting table 52, so that the hook on the core rod 22 is connected to the connecting part 14 on the inner rod 12, and then the rotating tube 23 is threadedly connected to the outer tube 11 to complete the installation of the storage rod 1 and the control handle 2.

[0114] The preservation rod 1 detachably connected with the control handle 2 is inserted into the TEM detector, the interior of the TEM detector is evacuated, and the control handle 2 drives the inner rod 12 to move relative to the outer tube 11, so that the sample part 13 extends out of the outer tube 11 and is located in the TEM detector, and TEM detection is performed on the sample in the sample part 13.

[0115] By using the sample vacuum transfer system as described above in the sample preparation method, the sample is protected in the first sealed space during the entire process from thinning in the FIB instrument to TEM detection in the TEM detector, thereby preventing the sample from being oxidized and contaminated, thereby improving the accuracy of TEM detection of the sample.

[0116] It should be noted that, in this article, relational terms such as "first" and "second" are only used to distinguish one entity or operation from another entity or operation, and do not necessarily require or imply any such actual relationship or order between these entities or operations. Moreover, the terms "include", "comprise" or any other variants thereof are intended to cover non-exclusive inclusion, so that a process, method, article or device including a series of elements includes not only those elements, but also other elements not explicitly listed, or also includes elements inherent to such process, method, article or device. In the absence of further restrictions, the elements defined by the sentence "comprise a ..." do not exclude the existence of other identical elements in the process, method, article or device including the elements.

[0117] The above description is only a specific embodiment of the present disclosure, so that those skilled in the art can understand or implement the present disclosure. Various modifications to these embodiments will be apparent to those skilled in the art, and the general principles defined herein may be implemented in other embodiments without departing from the spirit or scope of the present disclosure. Therefore, the present disclosure will not be limited to the embodiments described herein, but will conform to the widest scope consistent with the principles and novel features disclosed herein.

Claims

1. A sample vacuum transfer system, characterized in that: It comprises a storage rod (1), a control handle (2) and a control console (3); The storage rod (1) comprises an inner rod (12) and an outer tube (11) movably sleeved on the outer side of the inner rod (12); two ends of the inner rod (12) are respectively formed with a connecting portion (14) and a sample portion (13) for storing samples; two ends of the sample portion (13) are respectively provided with sealing rings (15); the two sealing rings (15) can be sealedly connected to the inner wall of the outer tube (11) to enclose a first sealed space; the inner rod (12) can move relative to the outer tube (11) to drive the sample portion (13) to extend out of and retract into the outer tube (11); The console (3) comprises a driving device (33), a base (31) for being installed in a FIB instrument (4), and a vacuum chamber (32) for storing the sample, wherein the driving device (33) and the vacuum chamber (32) are arranged on the base (31) and are connected to each other; When the preservation rod (1) is inserted into the TEM detector, the control handle (2) is detachably connected to the outer tube (11) and the connecting portion (14) to drive the inner rod (12) to move; When the storage rod (1) is arranged in the FIB instrument (4), the outer tube (11) is detachably connected to the base (31), and the driving device (33) is detachably connected to the connecting portion (14) to drive the movement of the inner rod (12) and the opening and closing of the vacuum chamber (32).

2. The sample vacuum transfer system according to claim 1, characterized in that: The base (31) is provided with a first mounting portion (34) and a second mounting portion (35) which are arranged at intervals along the width direction of the base (31); the vacuum chamber (32) is detachably connected to the first mounting portion (34); the storage rod (1) is detachably connected to the second mounting portion (35); the driving device (33) is arranged between the first mounting portion (34) and the second mounting portion (35) and is respectively connected to the vacuum chamber (32) and the connecting portion (14).

3. The sample vacuum transfer system according to claim 1, characterized in that: The driving device (33) comprises a sliding member and a driving member; The sliding member is slidably connected to the base (31) along the length direction of the base (31); the driving member is arranged on the base (31) and connected to the sliding member; the storage rod (1) is detachably connected to the base (31) along the length direction of the base (31); and the sliding member is detachably connected to the vacuum chamber (32) and the connecting portion (14); The driving member drives the sliding member to slide relative to the base (31) to drive the vacuum chamber (32) to open and close, and drives the sample part (13) to extend and retract the outer tube (11).

4. The sample vacuum transfer system according to claim 3, characterized in that: The vacuum chamber (32) comprises an external tube (321) and a movable rod (322); The external tube (321) is movably sleeved on the outer side of the movable rod (322); a storage portion (323) for placing the sample is formed on the movable rod (322); two vacuum sealing rings (324) are provided on the movable rod (322); the two vacuum sealing rings (324) are respectively located at two ends of the storage portion (323) along the extension direction of the movable rod (322); the movable rod (322) can move relative to the external tube (321) to drive the storage portion (323) to move between the inside and the outside of the external tube (321); When the storage portion (323) is located in the external tube (321), the two vacuum sealing rings (324) are both sealedly connected to the inner wall of the external tube (321) to jointly enclose a second sealed space; The external tube (321) and the movable rod (322) are arranged along the length direction of the base (31), and one end of the movable rod (322) is connected to the sliding member.

5. The sample vacuum transfer system according to claim 1, characterized in that: The control handle (2) comprises a handle body (21) and a core rod (22); The handle body (21) is provided with a mounting channel, the core rod (22) is inserted into the mounting channel, the outer tube (11) is detachably connected to one side of the handle body (21), and one end of the core rod (22) close to the outer tube (11) is detachably connected to the connecting portion (14).

6. The sample vacuum transfer system according to claim 5, characterized in that: A rotating tube (23) is provided on the side of the handle body (21) facing the outer tube (11), the rotating tube (23) is rotatably connected to the handle body (21), an escape channel is provided in the rotating tube (23), the escape channel is coaxially arranged with the installation channel, the core rod (22) is inserted into the escape channel and the installation channel to be connected to the connecting portion (14), a thread is provided at one end of the rotating tube (23) and the outer tube (11) close to each other, and the rotating tube (23) is threadedly connected to the outer tube (11); And / or, a hook is provided at one end of the core rod (22) facing the inner rod (12), the connecting portion (14) comprises a slot, and the hook is connected to the slot by a snap connection.

7. The sample vacuum transfer system according to any one of claims 1 to 6, characterized in that: The sample vacuum transfer system further comprises a connecting bracket (51), a mounting platform (52) and a moving platform (53), wherein the mounting platform (52) and the moving platform (53) are arranged on one side of the connecting bracket (51), and the mounting platform (52) and the moving platform (53) are arranged relative to each other along a first direction, the moving platform (53) is slidably connected to the bracket along the first direction, the mounting platform (52) is movably connected to the connecting bracket (51), the mounting platform (52) can move relative to the connecting bracket (51) along the first direction and the second direction, and the mounting platform (52) can be raised and lowered along a third direction, and the first direction, the second direction and the third direction are perpendicular to each other; The handle body (21) is connected to the movable platform (53), the storage rod (1) is installed on the mounting platform (52) along the first direction, and the connecting portion (14) is exposed on one side of the mounting platform (52) facing the movable platform (53) along the first direction.

8. The sample vacuum transfer system according to any one of claims 1 to 6, characterized in that: The sample portion (13) is provided with comb teeth (16), and the sample is arranged on the comb teeth (16).

9. The sample vacuum transfer system according to any one of claims 1 to 6, characterized in that: The console (3) further comprises a controller, wherein the controller is connected to the driving device (33), wherein the controller controls the driving device (33) to open and close the vacuum chamber (32), and wherein the controller controls the driving device (33) to drive the sample portion (13) to extend and retract the outer tube (11).

10. A sample preparation method, characterized in that: Use of the sample vacuum transfer system according to any one of claims 1 to 9, comprising: The sample, the preservation rod (1) and the console (3) are placed in a glove box in a vacuum environment, the sample is placed in a vacuum chamber (32), the outer tube (11) is mounted on the base (31), the connecting portion (14) is detachably connected to the driving device (33), and the driving device (33) drives the vacuum chamber (32) to close and drives the sample portion (13) to retract into the outer tube (11); The control console (3) is taken out of the glove box and placed inside a FIB instrument (4), the inside of the FIB instrument (4) is evacuated to form a vacuum environment, a driving device (33) drives the vacuum chamber (32) to open, and drives the sample part (13) to extend out of the outer tube (11), a probe of the FIB instrument (4) moves the sample in the vacuum chamber (32) to the sample part (13), and an ion beam is used to perform a sample preparation operation on the sample in the sample part (13); After the sample preparation operation on the sample part (13) is completed, the driving device (33) drives the sample part (13) to retract into the outer tube (11), opens the FIB instrument (4), takes out the storage rod (1), and the control handle (2) is detachably connected to the outer tube (11) and the inner rod (12) of the storage rod (1); The storage rod (1) detachably connected to the control handle (2) is inserted into a TEM detector, the interior of the TEM detector is evacuated, and the control handle (2) drives the inner rod (12) to move relative to the outer tube (11), so that the sample part (13) extends out of the outer tube (11) and is located in the TEM detector, and TEM detection is performed on the sample in the sample part (13).

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