阅读说明：本技术 一种双束扫描电镜真空冷冻传输装置 (Vacuum freezing transmission device for double-beam scanning electron microscope ) 是由 季刚 张建国 李硕果 孙飞 于 2021-08-11 设计创作，主要内容包括：本发明涉及一种双束扫描电镜真空冷冻传输装置,包括真空样品腔门、样品传输管、冷冻样品传输杆和角度调节装置。真空样品腔门密封连接于真空样品腔室的开口处,并设有样品传输窗口,样品传输管密封连接于样品传输窗口位置,与真空样品腔室连通。冷冻样品传输杆穿设于样品传输管内,外周与样品传输管动密封连接,用于将冷冻样品输送至真空样品腔室内,冷冻样品传输杆的端部能够与样品传输管卡接和/或解除卡接。角度调节装置设于真空样品腔门上,与样品传输管连接,当冷冻样品传输杆与样品传输管卡接时,角度调节装置适于带动样品传输管和冷冻样品传输杆同步转动,调节冷冻样品的倾转角度,满足冷冻样品的离子束加工和扫描电镜成像的需求。(The invention relates to a double-beam scanning electron microscope vacuum freezing transmission device which comprises a vacuum sample cavity door, a sample transmission pipe, a frozen sample transmission rod and an angle adjusting device. The vacuum sample cavity door is connected to the opening of the vacuum sample cavity in a sealing mode and provided with a sample transmission window, and the sample transmission pipe is connected to the position of the sample transmission window in a sealing mode and communicated with the vacuum sample cavity. The freezing sample transmission rod is arranged in the sample transmission pipe in a penetrating mode, the periphery of the freezing sample transmission rod is connected with the sample transmission pipe in a dynamic sealing mode and used for conveying a freezing sample to the vacuum sample cavity, and the end portion of the freezing sample transmission rod can be clamped with the sample transmission pipe and/or can be unlocked. The angle adjusting device is arranged on the vacuum sample cavity door and connected with the sample transmission pipe, and when the frozen sample transmission rod is clamped with the sample transmission pipe, the angle adjusting device is suitable for driving the sample transmission pipe and the frozen sample transmission rod to synchronously rotate, adjusts the tilting angle of the frozen sample, and meets the requirements of ion beam processing and scanning electron microscope imaging of the frozen sample.)

1. The utility model provides a two scanning electron microscope vacuum refrigeration transmission device which characterized in that includes:

the vacuum sample chamber door (1) is connected to the opening of the vacuum sample chamber (2) in a sealing mode, and a sample transmission window (120) is arranged on the vacuum sample chamber door (1);

the sample transmission pipe (4) is hermetically connected to the position of the sample transmission window (120) and is communicated with the vacuum sample chamber (2);

the frozen sample transmission rod (3) is arranged in the sample transmission pipe (4) in a penetrating way, the periphery of the frozen sample transmission rod is connected with the inner wall of the sample transmission pipe (4) in a dynamic sealing way, and the frozen sample transmission rod is used for transmitting a frozen sample (17) into the vacuum sample chamber (2);

one end of the frozen sample transmission rod (3) far away from the frozen sample (17) can be clamped with the sample transmission pipe (4) and/or unlocked;

the angle adjusting device (6) is arranged on the vacuum sample cavity door (1) and is connected with the sample transmission pipe (4);

when freezing sample transmission pole (3) with when sample transmission pipe (4) joint, angle adjusting device (6) are suitable for to drive sample transmission pipe (4) with freezing sample transmission pole (3) synchronous revolution, in order to adjust the angle of verting of freezing sample (17).

2. The dual-beam scanning electron microscope vacuum freeze transmission device according to claim 1, characterized by further comprising a three-dimensional translation stage (5);

the sample transmission pipe (4) is connected to the position of the sample transmission window (120) through a corrugated pipe (12);

the three-dimensional translation stage (5) is connected with the sample transmission pipe (4) and arranged on a translation stage bracket (16), and the translation stage bracket (16) is connected with the angle adjusting device (6);

when the frozen sample transmission rod (3) is clamped with the sample transmission pipe (4), the three-dimensional translation table (5) works to drive the sample transmission pipe (4) and the frozen sample transmission rod (3) to synchronously move so as to adjust the position of the frozen sample (17).

3. The dual-beam scanning electron microscope vacuum freeze transmission device according to claim 2, characterized in that the angle adjustment device (6) comprises:

a shaft sleeve vacuum plate valve shell assembly (610), one end of which is hermetically connected to the position of the freezing transmission window (120), and the other end of which is hermetically connected with the corrugated pipe (12);

the worm wheel (630) is arranged on the shaft disc (620), and the shaft disc (620) is rotatably sleeved on the periphery of the shaft sleeve vacuum plate valve shell assembly (610) and is fixedly connected with the translation table bracket (16);

the worm (650) is rotationally connected to the worm support (640), and the worm support (640) is connected to the vacuum sample cavity door (1);

one end of the worm (650) is connected with a motor (660) and meshed with the worm wheel (630), the motor (660) can drive the worm wheel (630) meshed with the worm (650) to rotate when working, and further drive the shaft disc (620), the translation table bracket (16), the three-dimensional translation table (5), the sample transmission pipe (4) and the frozen sample transmission rod (3) to synchronously rotate.

4. The dual-beam scanning electron microscope vacuum freeze transmission device according to claim 3, characterized in that the angle adjustment device (6) further comprises a synchronization sleeve (670);

the synchronous sleeve (670) is sleeved on the periphery of the corrugated pipe, one end of the synchronous sleeve is fixedly connected with the end part of the corrugated pipe, and the other end of the synchronous sleeve is connected with the translation table bracket (16);

the synchronous sleeve (670) is arranged in the shaft sleeve vacuum plate valve shell assembly (610), and the periphery of the synchronous sleeve is connected with the inner wall of the shaft sleeve vacuum plate valve shell assembly (610) in a dynamic sealing manner.

5. The dual-beam scanning electron microscope vacuum freezing transmission device according to claim 3, further comprising a vacuum plate valve (8);

the vacuum plate valve (8) is connected to the side opening end of the vacuum plate valve shell of the shaft sleeve vacuum plate valve shell assembly (610) in a sealing mode, a sealing channel can be formed among the frozen sample transmission rod (3), the sample transmission pipe (4), the corrugated pipe (12), the shaft sleeve vacuum plate valve shell assembly (610) and the vacuum plate valve (8), and the vacuum plate valve (8) is used for controlling the communication and/or closing of the sealing channel and the vacuum sample chamber (2);

when the sealed channel is communicated with the vacuum sample chamber (2), the frozen sample transmission rod (3) sends one end containing the frozen sample (17) into the vacuum sample chamber (2) under the action of manual control and negative pressure.

6. The dual-beam scanning electron microscope vacuum freeze transmission device according to claim 5, characterized by further comprising a pre-evacuation valve (7);

the pre-vacuumizing valve (7) is connected to the sample transmission pipe (4) in a sealing mode, is communicated with the sealing channel and is used for pre-vacuumizing the sealing channel.

7. The dual-beam scanning electron microscope vacuum freeze transmission device according to claim 1, characterized by further comprising a positioning sleeve (15);

the positioning sleeve (15) is arranged in the sample transmission pipe (4), is connected with the sample transmission pipe (4) in an axial and circumferential positioning manner, and is positioned on one side of the sample transmission pipe (4) close to the vacuum sample cavity door (1);

a Z-shaped sliding groove (151) is formed in the positioning sleeve (15), and a limiting pin (310) is arranged on the frozen sample transmission rod (3);

the frozen sample transmission rod (3) is arranged in the positioning sleeve (15) in a penetrating way, and the limiting pin (310) can slide into and/or out of the Z-shaped sliding groove (151);

when the limit pin (310) slides into the Z-shaped sliding groove (151) and is positioned at the turning part of the Z-shaped sliding groove (151), the pre-insertion position of the frozen sample transmission rod (3) is limited.

8. The dual-beam scanning electron microscope vacuum freezing transmission device according to claim 1, wherein a clamping needle (410) is arranged on one side of the sample transmission tube (4) far away from the vacuum sample cavity door (1), and a clamping groove (320) is arranged on one end of the frozen sample transmission rod (3) far away from the frozen sample (17);

the card needle (410) can be inserted into and/or pulled out of the card slot (320);

when the clamping needle (410) is inserted into the clamping groove (320), the frozen sample transmission rod (3) is clamped with the sample transmission pipe (4);

when the clamping needle (410) is pulled out of the clamping groove (320), the frozen sample transmission rod (3) and the sample transmission pipe (4) are released from clamping.

9. The dual-beam scanning electron microscope vacuum freezing transmission device according to claim 1, wherein a dewar (340) is disposed at one end of the frozen sample transmission rod (3) far away from the frozen sample (17), and the dewar (340) is used for providing a cold source for the frozen sample (17) disposed on the frozen sample transmission rod (3).

10. The dual-beam scanning electron microscope vacuum freeze transmission device according to any one of claims 1 to 9, characterized by further comprising a controller (11);

the controller (11) is in communication connection with the angle adjusting device (6), the three-dimensional translation table (5), the vacuum plate valve (8) and the pre-vacuumizing valve (7) respectively and is used for controlling starting and stopping of the equipment.

Technical Field

The invention relates to the technical field of microscopic imaging, in particular to a vacuum freezing transmission device for a double-beam scanning electron microscope.

Background

The cryoelectron microscopy freezes the biological sample in a near-physiological state by a rapid freezing or high-pressure freezing technique to preserve the high-resolution structure of the sample. By another important technical means of the cryoelectron microscope technology, namely the electron tomography technology, the frozen sample is subjected to serial tilting imaging, so that a high-resolution three-dimensional structure is reconstructed. Since tissue samples are typically several microns to tens of microns or even larger, they are much larger than the thickness of the sample that can be penetrated by a transmission electron microscope (hundreds of nanometers). The use of a frozen focused ion beam is a very effective technique for cutting and thinning a sample. The sample can be thinned to about 200 nm by the technology, and the sample has no problems of deformation, wrinkle and the like.

One of the problems currently affecting the application of this technique is the technique of frozen transfer of the sample. During the transmission process of the frozen sample, the problems of ice crystal pollution, sample slice damage and even loss, sample position rotation and the like are easily caused. These problems cause partial loss of the frozen thin slice samples elaborately prepared in the frozen dual-beam scanning electron microscope, greatly affect the success rate of the experiment, and become one of the bottlenecks of the current technology.

Disclosure of Invention

Technical problem to be solved

In view of the above disadvantages and shortcomings of the prior art, the present invention provides a dual-beam scanning electron microscope vacuum freezing transmission device, which is used for performing frozen sample transmission of a frozen sample cutting and thinning experiment by using a dual-beam scanning electron microscope and frozen sample transmission between the dual-beam scanning electron microscope and a freezing transmission electron microscope or a freezing fluorescence microscope, and solves the problem of low success rate in the frozen sample transmission technology in the prior art, thereby greatly reducing the pollution of ice crystals and the damage of sample slices, improving the success rate of sample transfer, and having simple operation.

(II) technical scheme

In order to achieve the purpose, the invention provides a vacuum freezing transmission device, which has the following specific technical scheme:

a vacuum freeze transfer device comprising:

the vacuum sample cavity door is hermetically connected to the opening of the vacuum sample cavity, and a sample transmission window is arranged on the vacuum sample cavity door;

the sample transmission pipe is hermetically connected to the position of the sample transmission window and is communicated with the vacuum sample chamber;

the frozen sample transmission rod is arranged in the sample transmission pipe in a penetrating way, the periphery of the frozen sample transmission rod is in dynamic sealing connection with the inner wall of the sample transmission pipe, and the frozen sample transmission rod is used for transmitting a frozen sample into the vacuum sample chamber;

one end of the frozen sample transmission rod, which is far away from the frozen sample, can be clamped with and/or unlocked from the sample transmission pipe;

the angle adjusting device is arranged on the vacuum sample cavity door and is connected with the sample transmission pipe;

when freezing sample transmission pole and sample transmission pipe joint, angle adjusting device is suitable for and drives sample transmission pipe and the synchronous rotation of freezing sample transmission pole to adjust the angle of verting of freezing sample.

Further, the device also comprises a three-dimensional translation table;

the sample transmission pipe is connected to the position of the sample transmission window through a corrugated pipe;

the three-dimensional translation stage is connected with the sample transmission pipe and arranged on a translation stage bracket, and the translation stage bracket is connected with the angle adjusting device;

when the frozen sample transmission rod is clamped with the sample transmission pipe, the three-dimensional translation table can drive the sample transmission pipe and the frozen sample transmission rod to synchronously move so as to adjust the position of the frozen sample.

Further, the angle adjusting device includes:

one end of the shaft sleeve vacuum plate valve shell assembly is hermetically connected to the position of the freezing transmission window, and the other end of the shaft sleeve vacuum plate valve shell assembly is hermetically connected with the corrugated pipe;

the worm wheel is arranged on the shaft disc, and the shaft disc is rotatably sleeved on the periphery of the shell assembly of the shaft sleeve vacuum plate valve and is fixedly connected with the translation table bracket;

the worm is rotationally connected to the worm support, and the worm support is connected to the vacuum sample cavity door;

one end of the worm is connected with the motor and meshed with the worm wheel, and the motor can drive the worm wheel meshed with the worm to rotate so as to drive the shaft disc, the translation table bracket, the three-dimensional translation table, the sample transmission pipe and the frozen sample transmission rod to synchronously rotate.

Further, the angle adjusting device also comprises a synchronous sleeve;

the synchronous sleeve is sleeved on the periphery of the corrugated pipe, one end of the synchronous sleeve is fixedly connected with the end part of the corrugated pipe, and the other end of the synchronous sleeve is connected with the translation table bracket;

the synchronous sleeve is positioned in the shaft sleeve vacuum plate valve shell combination body, and the periphery of the synchronous sleeve is connected with the inner wall of the shaft sleeve vacuum plate valve shell combination body in a dynamic sealing manner.

Further, the vacuum plate valve is also included;

the vacuum plate valve is connected with the open end of the side face of the vacuum plate valve shell of the shaft sleeve vacuum plate valve shell assembly in a sealing manner, a sealing channel can be formed among the frozen sample transmission rod, the sample transmission pipe, the corrugated pipe, the shaft sleeve vacuum plate valve shell assembly and the vacuum plate valve, and the vacuum plate valve is used for controlling the communication and/or closing of the sealing channel and the vacuum sample cavity;

when the sealed channel is communicated with the vacuum sample chamber, the frozen sample transmission rod sends the end containing the frozen sample into the vacuum sample chamber under the action of manual control and negative pressure.

Further, the device also comprises a pre-vacuum-pumping valve;

the pre-vacuumizing valve is connected to the sample transmission pipe in a sealing mode, communicated with the sealing channel and used for pre-vacuumizing the sealing channel.

Further, the device also comprises a positioning sleeve;

the positioning sleeve is arranged in the sample transmission pipe, is connected with the sample transmission pipe in an axial and radial positioning way, and is positioned at one side of the sample transmission pipe close to the vacuum sample cavity door;

a Z-shaped chute is arranged on the positioning sleeve, and a limit pin is arranged on the frozen sample transmission rod;

the frozen sample transmission rod is arranged in the positioning sleeve in a penetrating way, and the limiting pin can slide into and/or slide out of the Z-shaped sliding groove;

when the limiting pin slides into the Z-shaped chute and is positioned at the turning part of the Z-shaped chute, the pre-insertion position of the frozen sample transmission rod is limited.

Furthermore, a clamping needle is arranged on one side of the sample transmission pipe, which is far away from the vacuum sample cavity door, and a clamping groove is arranged at one end of the frozen sample transmission rod, which is far away from the frozen sample;

the clamping needle can be inserted into and/or pulled out of the clamping groove;

when the clamping needle is inserted into the clamping groove, the frozen sample transmission rod is clamped with the sample transmission pipe;

when the clamping needle is pulled out of the clamping groove, the frozen sample transmission rod and the sample transmission pipe are released from clamping.

Furthermore, the end of the frozen sample transmission rod, which is far away from the frozen sample, is provided with a dewar flask, and the dewar flask is used for providing a cold source for the frozen sample arranged on the frozen sample transmission rod.

Further, the device also comprises a controller;

the controller is respectively in communication connection with the angle adjusting device, the three-dimensional translation table, the vacuum plate valve and the pre-vacuumizing valve and is used for controlling starting and stopping of the equipment.

(III) advantageous effects

The double-beam scanning electron microscope vacuum freezing transmission device provided by the invention has the following beneficial effects.

In the invention, the angle adjusting device is arranged and connected with the sample transmission pipe. The frozen sample transmission rod penetrates through the sample transmission pipe, can slide along the sample transmission pipe and is used for transmitting a frozen sample into the vacuum sample cavity. Wherein, the frozen sample transmission rod is far away from one end of the frozen sample and can be clamped with or unlocked from the sample transmission pipe. During the joint, control angle adjusting device starts, and angle adjusting device work can drive the freezing sample transmission pole rotation with sample transmission pipe joint to adjust the angle of verting of freezing sample, and then satisfied the cutting of freezing focus ion beam of freezing sample and the demand of formation of image.

According to the invention, the frozen sample is conveyed into the vacuum sample chamber through the frozen sample conveying rod, the frozen sample conveying rod is used as a conveying device and a storage table, the frozen sample is not required to be transferred in the double-beam scanning electron microscope vacuum sample chamber and is conveyed to a frozen transmission electron microscope or other equipment from the double-beam scanning electron microscope, the frozen sample can be effectively prevented from being deformed, polluted by ice, damaged and moved and rotated in the position of the frozen sample in the clamping process, and the experiment success rate is greatly improved.

Drawings

The accompanying drawings, which are included to provide a further understanding of the application and are incorporated in and constitute a part of this application, illustrate embodiment(s) of the application and together with the description serve to explain the application and not to limit the application, and in which:

FIG. 1 is a schematic structural diagram of a dual-beam scanning electron microscope and a dual-beam scanning electron microscope vacuum freeze transmission device according to an embodiment;

FIG. 2 is a schematic view of a partial structure of a dual-beam scanning electron microscope vacuum freezing transmission device according to an embodiment;

FIG. 3 is an exploded view of a sample transfer tube and a frozen sample transfer rod according to one embodiment;

FIG. 4 is a schematic structural view of an angle adjusting apparatus according to an embodiment;

FIG. 5 is a sectional view taken along line A-A of FIG. 4;

FIG. 6 is a cross-sectional view taken along line B-B of FIG. 3;

FIG. 7 is a schematic diagram of a vacuum sample chamber door according to an embodiment;

FIG. 8 is a schematic view of a positioning sleeve according to an embodiment;

FIG. 9 is a schematic diagram of a sample transfer tube according to an embodiment.

[ description of reference ]

1. A vacuum sample chamber door; 110. a vacuum sample chamber door flange; 120. a sample transmission window;

2. a vacuum sample chamber;

3. a frozen sample transfer rod; 310. a limit pin; 320. a card slot; 330. an indicator line; 340. a dewar flask;

4. a sample transfer tube; 410. clamping a needle; 420. stopping the opening; 430. a protrusion;

5. a three-dimensional translation stage;

6. an angle adjusting device; 610. a shaft sleeve vacuum plate valve shell assembly; 620. a reel; 630. a worm gear; 640. a worm support; 650. a worm; 660. a motor; 670. a synchronous sleeve; 680. a bearing;

7. a pre-vacuum valve; 8. a vacuum plate valve; 9. an ion beam system; 10. an electron beam system; 11. a controller; 12. a bellows; 14. a threaded sleeve;

15. positioning the sleeve; 151. a Z-shaped chute; 152. a through hole; 153. positioning the flange;

16. a translation stage support; 17. the samples were frozen.

Detailed Description

In order to make the objects, technical solutions and advantages of the present invention clearer, the technical solutions in the embodiments of the present invention will be described in more detail below with reference to the accompanying drawings in the preferred embodiments of the present invention. In the drawings, the same or similar reference numerals denote the same or similar elements or elements having the same or similar functions throughout. The described embodiments are only some, but not all embodiments of the invention. The embodiments described below with reference to the drawings are illustrative and intended to be illustrative of the invention and are not to be construed as limiting the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention. Embodiments of the present invention will be described in detail below with reference to the accompanying drawings.

In the description of the present embodiment, it is to be understood that the terms "center", "longitudinal", "lateral", "front", "back", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", etc. indicate orientations or positional relationships based on those shown in the drawings, and are only for convenience of description and simplicity of description, and do not indicate or imply that the device or element being referred to must have a particular orientation, be constructed in a particular orientation, and be operated, and therefore, should not be construed as limiting the scope of the present embodiment.

Referring to fig. 1 to 9, the present embodiment provides a frozen dual-beam sem vacuum freezing transmission device for delivering a frozen sample 17 to a vacuum sample chamber 2, which includes a vacuum sample chamber door 1, a frozen sample transmission rod 3, a sample transmission tube 4 and an angle adjustment device 6.

Specifically, the vacuum sample chamber door 1 is hermetically connected to an opening of the vacuum sample chamber 2, and the vacuum sample chamber door 1 is provided with a sample transmission window 120. The vacuum sample cavity door 1 is of an inwards concave structure, a vacuum sample cavity door flange 110 is arranged on the edge of the inwards concave structure, the inwards concave structure is arranged in the vacuum sample cavity 2, the vacuum sample cavity door flange 110 is connected to the opening of the vacuum sample cavity 2 through a bolt, and a sealing rubber strip is arranged at the contact position of the vacuum sample cavity door flange 110 and the vacuum sample cavity 2 so as to meet the requirement of the vacuum degree of the vacuum sample cavity 2. The angle adjusting device 6 is arranged on the vacuum sample cavity door 1 and connected with the sample transmission pipe 4, and the angle adjusting device 6 is suitable for driving the sample transmission pipe 4 to rotate. The sample transfer tube 4 is hermetically connected to the position of the sample transfer window 120 and is communicated with the vacuum sample chamber 2. One end of the frozen sample transmission rod 3 is used for fixing the frozen sample 17, the other end of the frozen sample transmission rod is provided with a Dewar flask 340, and the Dewar flask 340 is used for providing a cold source for the frozen sample 17 arranged on the frozen sample transmission rod 3. Further, the fixed end of the frozen sample 17 of the frozen sample transmission rod 3 is inserted into the sample transmission tube 4, and can slide along the sample transmission tube 4 and pass through the sample transmission window 120 under the pushing of an external force to transmit the frozen sample 17 into the vacuum sample chamber 2. Further, a clamping groove 320 is further formed in the freezing sample transmission rod 3 on the side where the Dewar flask 340 is located, a clamping needle 410 is correspondingly arranged on the sample transmission tube 4, when the freezing sample transmission rod 3 slides towards the vacuum sample chamber 2 side and reaches a specified position, the clamping needle 410 is clamped in the clamping groove 320, and the freezing sample transmission rod 3 stops sliding to limit the position of the freezing sample 17 in the vacuum sample chamber 2. When the frozen sample transmission rod 3 needs to be pulled out, the frozen sample transmission rod 3 is pulled out in the direction away from the vacuum cavity 2, the clamping needle 410 is pulled out from the clamping groove 320, and the frozen sample transmission rod 3 and the sample transmission pipe 4 are released from clamping.

During the specific use, on being fixed in freezing sample transmission pole 3 with freezing sample 17 in advance, wear to locate sample transmission pipe 4 with freezing sample 17 stiff end, external force promotes freezing sample transmission pole 3 and will freeze sample 17 and transmit to vacuum sample cavity 2 in, freezing sample transmission pole 3 and sample transmission pipe 4 joint. According to the demand of using focused ion beam to freezing sample 17 cutting angle, control angle adjusting device 6 starts, drives sample transmission pipe 4 and freezing sample transmission pole 3 synchronous revolution, adjusts freezing sample 17's the angle of verting, and then has satisfied the angle requirement when freezing sample 17 carries out focused ion beam cutting. In this embodiment, frozen sample transmission rod 3 is used for carrying frozen sample 17 on the one hand, and on the other hand can bear frozen sample 17 as the cold platform and use, and when frozen sample 17 passed into two beam scanning electron microscope and transmitted the sample to freezing transmission electron microscope from two beam scanning electron microscope, need not to shift the sample between the microscope carrier of difference, can effectively avoid pressing from both sides to get frozen sample 17 in the transfer process and take place deformation, ice pollution and frozen sample 17 position removal, has improved the experiment success rate greatly.

Further, referring to fig. 1 and 2, the vacuum freezing transmission device in this embodiment further includes a three-dimensional translation stage 5, the three-dimensional translation stage 5 is disposed on a translation stage support 16 and connected to the sample transmission tube 4, and the translation stage support 16 is fixedly connected to the angle adjustment device 6 through a bolt. Correspondingly, the sample transmission pipe 4 is flexibly connected to the vacuum sample chamber door 1 through a corrugated pipe 12, and the corrugated pipe 12 has the functions of length direction, horizontal direction and vertical direction expansion and contraction. The three-dimensional translation stage 16 is suitable for position adjustment in X, Y, Z three directions, the three-dimensional translation stage 16 can drive one end of the corrugated pipe 12 connected with the sample transmission pipe 4 to move correspondingly when working, the sample transmission pipe 4 moves relative to the position of the vacuum sample chamber 2, the penetration length of the frozen sample transmission rod 3 is correspondingly changed, and the position of the frozen sample 17 relative to the ion beam system 9 or the electron beam system 10 in the vacuum sample chamber 2 can be accurately adjusted, so that the requirements of adjusting the focused ion beam cutting position and the scanning electron microscope imaging position of the frozen sample 17 in the vacuum sample chamber 2 are met.

Specifically, referring to fig. 4, the angle adjusting device 6 in the present embodiment includes a bushing vacuum plate valve housing assembly 610, a shaft disc 620, a worm gear 630, a worm 650 and a motor 660. One end of the shaft sleeve vacuum plate valve housing assembly 610 is connected to the vacuum sample chamber door 1 in a sealing manner, the other end of the shaft sleeve vacuum plate valve housing assembly is connected to the bellows 12 in a dynamic sealing manner, the worm wheel 630 is fixed to the shaft disc 620 through a bolt, and the shaft disc 620 is rotatably sleeved on the periphery of the shaft sleeve vacuum plate valve housing assembly 610 through a turntable bearing 680 and is fixedly connected to the translation stage support 16 through a bolt. The two ends of the worm 650 are rotatably connected to the worm bracket 640 through bearings, and the worm bracket 640 is arranged on the vacuum sample chamber door 1 through bolts. The worm 650 is meshed with the worm wheel 630, the end part of the worm is connected with the motor 660, and the motor 660 can drive the worm 650 and the worm wheel 630 to be meshed for transmission. Further, the angle adjusting device 6 further comprises a synchronous sleeve 670, the periphery of the corrugated pipe 12 is sleeved with the synchronous sleeve 670, one end of the synchronous sleeve 670 is fixedly connected with the end of the corrugated pipe 12 in a welding mode, the other end of the synchronous sleeve 670 is detachably connected with the translation table support 16 through a bolt, the synchronous sleeve 670 is arranged in the shaft sleeve vacuum plate valve housing assembly 610, and the periphery of the synchronous sleeve 670 is connected with the shaft sleeve vacuum plate valve housing assembly 610 in a dynamic sealing mode. When the angle is required to be adjusted, the frozen sample transmission rod 3 is confirmed to be clamped with the sample transmission pipe 4, the motor 660 is controlled to be started, the motor 660 drives the worm 650 and the worm wheel 630 to be meshed for transmission, and then the shaft disc 620, the translation table support 16, the sample transmission pipe 4, the corrugated pipe 12, the synchronous sleeve 670, the frozen sample transmission rod 3 and the frozen sample 17 are driven to synchronously rotate, so that the requirements of tilting imaging or ion beam processing of the frozen sample 17 are met. In this embodiment, by providing the synchronizing sleeve 670, the synchronizing sleeve 670 and the hub 620 are both connected to the translation stage bracket 16, and the hub 620 rotates to drive the synchronizing sleeve 670 and the bellows 12 to rotate synchronously via the translation stage bracket 16.

Further, referring to fig. 2, the vacuum freezing transmission device of the present embodiment further includes a vacuum conveying system for driving the frozen sample transmission rod 3 to slide along the sample transmission tube 4 by using the negative pressure working principle. Specifically, the vacuum conveying system comprises a vacuum plate valve 8 and a pre-vacuumizing valve 7, the vacuum plate valve 8 is connected to the shaft sleeve vacuum plate valve housing assembly 610 in a sealing mode, so that a sealing channel is formed among the frozen sample transmission rod 3, the sample transmission pipe 4, the corrugated pipe 12, the shaft sleeve vacuum plate valve housing assembly 610 and the vacuum plate valve 8, and the vacuum plate valve 8 is used for controlling the communication and the closing of the sealing channel and the vacuum sample chamber 2. The pre-vacuum valve 7 is hermetically connected to the sample transfer tube 4 and is communicated with the sealed channel for vacuumizing the sealed channel. During the specific use, control vacuum plate valve 8 and close, insert freezing sample transmission pole 3 in sample transmission pipe 4, then control vacuum valve 7 of taking out in advance and open, begin to take out the low vacuum to the sealed passageway with the vacuum pump, when reaching the setting value, control vacuum valve 7 of taking out in advance and close, control vacuum plate valve 8 and open, because the vacuum degree of vacuum sample cavity 2 is far less than external atmospheric pressure, freezing sample transmission pole 3 slides along sample transmission pipe 4 under the effect of manual control and negative pressure to carry freezing sample 17 to in the vacuum sample cavity 2. In this embodiment, the operation of the transmission process of the frozen sample 17 is simple, convenient and fast.

Further, referring to fig. 3, 6, 8 and 9, the vacuum freeze transfer device further comprises a positioning sleeve 15 for defining a pre-insertion position of the frozen sample transfer pins 3. Specifically, the positioning sleeve 15 is provided inside the sample-transporting tube 4 on the side close to the bellows 12. A spigot 420 is arranged in the sample transmission pipe 4, a projection 430 is arranged on the spigot 420, and the projection extends towards one side of the corrugated pipe 12. The positioning sleeve 15 is correspondingly provided with a positioning flange 153, the positioning sleeve 15 is arranged in the sample transmission pipe 4, the positioning flange 153 abuts against the position of the spigot 420, the threaded sleeve 14 is screwed in the sample transmission pipe 4, the end part of the threaded sleeve abuts against the positioning flange 153, and the axial direction of the positioning sleeve 15 is limited so as to prevent the positioning sleeve 15 from axially sliding. Furthermore, the positioning sleeve 15 is provided with a through hole 152, and the pre-vacuum valve 7 is communicated with the sealing channel through the through hole 152. The positioning sleeve 15 is further provided with a Z-shaped sliding groove 151, the protrusion 430 is arranged in the Z-shaped sliding groove 151 and located on one side close to the positioning flange 153, and the protrusion 430 is flush with the inner surface of the positioning sleeve 15 and limits the circumferential direction of the positioning sleeve 15 to prevent the positioning sleeve 15 from rotating. The frozen sample transmission rod 3 is provided with a limit pin 310, the frozen sample transmission rod 3 is arranged in the positioning sleeve 15 in a penetrating way, the limit pin 310 can slide into or slide out of the Z-shaped sliding groove 151, when the limit pin 310 is positioned at the turning part of the Z-shaped sliding groove 151, the position is the pre-insertion position of the frozen sample transmission rod 3, and the consistency of the pre-insertion position of the frozen sample transmission rod 3 in each sample loading process is ensured.

When the freezing sample transmission rod is used, the freezing sample transmission rod 3 is inserted into the sample transmission tube 4, the limiting pin 310 is connected in the Z-shaped sliding groove 151 in a sliding mode and is located at the turning part of the Z-shaped sliding groove 151, and the freezing sample transmission rod 3 is limited at the pre-insertion position. The vacuum pre-pumping system is controlled to be started, the sealed channel is pumped to be vacuum, when the pre-pumping reaches a set value, the pre-pumping vacuum valve 7 is controlled to be closed, the vacuum plate valve 8 is controlled to be opened, the frozen sample transmission rod 3 is manually controlled to rotate, the frozen sample transmission rod 3 slides along the sample transmission pipe 4 under the action of negative pressure, the limiting pin 310 slides along the Z-shaped sliding groove 151 and slides out of the Z-shaped sliding groove 151, the frozen sample transmission rod 3 continues to slide along the sample transmission pipe 4 until the clamping pin 410 is clamped in the clamping groove 320, and the transmission of the frozen sample 17 is completed.

Referring to fig. 8, in the present embodiment, the side of the Z-shaped chute 151 away from the vacuum sample chamber 2 is at an angle of 30 ° to 40 ° with respect to the vertical direction, and the frozen sample transfer rod 3 is rotated at a certain angle when inserted. In order to ensure that the limiting pin 310 is quickly and accurately aligned with the Z-shaped sliding groove 151 and slides in when the frozen sample transmission rod 3 is inserted, an indicating line 330 is arranged at the side of the clamping groove 320 of the frozen sample transmission rod 3, an included angle between the indicating line 330 and the central line of the clamping groove 320 is 30-40 degrees, and when the frozen sample transmission rod 3 is inserted, the indicating line 330 is rotated to correspond to the position of the clamping pin 410, and then the frozen sample transmission rod is inserted. When the frozen sample is pulled out, the frozen sample transmission rod 3 is kept to be vertically pulled out, and the limiting pin 310 can accurately slide into the Z-shaped sliding groove 151, so that the frozen sample transmission rod is convenient and quick.

Further, a controller 11 is included. The controller 11 is in communication connection with the three-dimensional translation stage 5 and is used for controlling starting and stopping of the three-dimensional translation stage 5 and adjusting the moving distance. The controller 11 is in communication connection with the angle adjusting device 6 and is used for controlling the angle adjusting device to be started, closed and adjusted in angle. The controller 11 is also in communication connection with the pre-vacuum valve 7 and the vacuum plate valve 8, and is used for controlling the opening and closing of the pre-vacuum valve 7 and the vacuum plate valve 8 so as to control the communication and closing of the sealing channel and the vacuum sample chamber 2, and realize the vacuum transmission of the frozen sample 17. According to the embodiment, the controller 11 is added to control the equipment, so that the automatic control of the double-beam scanning electron microscope vacuum freezing transmission device is improved, and the convenience and the rapidness are realized.

Based on the double-beam scanning electron microscope vacuum freezing transmission device, the transmission of the frozen sample 17 and the imaging and processing process of the frozen sample 17 comprise the following steps:

1) and, evacuating the vacuum sample chamber 2:

controlling the vacuum plate valve 8 and the pre-vacuumizing valve 7 to be closed, and starting to control the double-beam scanning electron microscope vacuum system to vacuumize the vacuum sample cavity 2 to a high vacuum state until the vacuum set value is better than the vacuum set value;

2) filling liquid nitrogen into the Dewar flask 340 of the frozen sample transmission rod 3, and precooling the frozen sample 17 to the temperature of the liquid nitrogen;

3) fixing the frozen sample 17 to the end of the frozen sample transfer rod 3;

4) and vacuumizing the sealing channel:

inserting the frozen sample transmission rod 3 filled with the frozen sample 17 into the sample transmission pipe 4, controlling the pre-vacuum valve 7 to be opened, starting the vacuum pump to vacuumize the sealed channel, controlling the pre-vacuum valve 7 to be closed when the vacuum degree reaches a set value (for example, 10Pa), opening the vacuum plate valve 8, manually controlling the frozen sample transmission rod 3 and slowly inserting the frozen sample transmission rod into the vacuum sample chamber 2 under the action of negative pressure;

5) controlling the three-dimensional translation stage 5 to accurately adjust the horizontal position and the height of the frozen sample transmission rod 3 so that the frozen sample 17 is positioned at the intersection point of the ion beam system 9 and the electron beam system 10;

6) and (4) adjusting the tilting angle of the frozen sample 17:

the angle adjusting device 6 is controlled to be started to drive the frozen sample 17 to rotate so as to meet the requirement of the ion beam system 9 on focused ion beam processing or imaging.

7) And controlling the three-dimensional translation stage 5 to accurately adjust the position of the frozen sample transmission rod 3, and selecting a proper sample position for focused ion beam processing or imaging.

8) After the focused ion beam processing or imaging is completed, the frozen sample transfer rod 3 is pulled out of the vacuum sample chamber 2 by an operation opposite to the insertion of the frozen sample transfer rod 3 into the vacuum sample chamber 2.

9) And the frozen sample transmission rod 3 is sent into a frozen transmission electron microscope for frozen transmission electron microscopic imaging, and then the electron tomography imaging is carried out, a series of tilting images are collected, and then the three-dimensional high-resolution structure of the sample is reconstructed.

The specific structure and the using method of the vacuum freezing transmission device provided by the embodiment can be widely applied to the application fields of freezing double-beam scanning electron microscope and scanning electron microscope imaging technologies, so that the high-resolution imaging of the frozen sample 17 of the double-beam scanning electron microscope after cutting or scanning electron microscope imaging and then transferring to a transmission electron microscope is realized, and the sample transfer among different devices is facilitated. The shape and the size of the vacuum sample cavity door 1 can be changed, and the freezing sample transmission rod 3 with different models can be matched with the sample transmission among the double-beam scanning electron microscope, the scanning electron microscope and the transmission electron microscope of different manufacturers and models. Meanwhile, the device can be matched with other types of sample transmission rods for use, multiple abundant operation modes such as normal temperature, freezing, temperature changing, liquid sample observation and the like are realized, and the device is suitable for ion beam micromachining or scanning electron microscopy imaging, component analysis and the like under different conditions. The vacuum freezing transmission device transmits the frozen sample 17 to the vacuum sample chamber 2 for imaging or processing in a vacuum transmission mode, in-situ processing and imaging are realized, then the frozen sample transmission rod 3 is directly transferred to a transmission electron microscope for high-resolution imaging, the operations of directly clamping and transferring the frozen sample 17 and the like are not needed, and the problems of sample damage and pollution caused in the transferring process of the frozen sample 17 are further avoided.

In summary, the vacuum freezing transmission device for freezing dual-beam scanning electron microscope system provided by the present invention is only a preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art can be considered to be within the scope of the present invention, and equivalent substitutions or changes according to the technical solution and the inventive concept thereof are also within the scope of the present invention.