High vacuum low temperature storage device
By designing a high-vacuum low-temperature storage device, the problem of sample contamination during transfer was solved, enabling contamination-free transport and efficient storage of samples, ensuring sample quality and the smooth progress of subsequent experiments.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- INSTITUTE OF BIOPHYSICS CHINESE ACADEMY OF SCIENCES
- Filing Date
- 2025-04-30
- Publication Date
- 2026-05-29
AI Technical Summary
During sample transfer, samples are easily contaminated in existing technologies, especially during liquid nitrogen storage and multiple transfers, where ice crystals are adsorbed, leading to sample damage and affecting subsequent data collection and structural analysis.
Design a high-vacuum cryogenic storage device, including a main body, a cooling body and a sample delivery channel. The sample is stored in a low-temperature and high-vacuum environment through the vacuum chamber and the cooling body, and the sample delivery channel is used to achieve contamination-free delivery and avoid contact between the sample and the outside environment.
This effectively avoids sample contamination, improves sample quality, increases the number and area of effective samples, and ensures the smooth progress of subsequent data collection and high-resolution structure analysis.
Smart Images
Figure CN224298328U_ABST
Abstract
Description
Technical Field
[0001] This utility model relates to the field of microscopic imaging technology, specifically to a high-vacuum cryogenic storage device. Background Technology
[0002] Cryo-electron microscopy is widely used in the field of microscopic imaging. It preserves high-resolution structures by freezing biological samples to near-physiological conditions using rapid freezing or autoclaving. For cellular tissue samples a few micrometers or even thicker, direct observation with transmission electron microscopy is not possible, necessitating sample thinning. Currently, a commonly used sample thinning technique is cryo-focused ion beam (CFFER), which uses a high-energy ion beam focused to a few nanometers to process the sample, yielding cryo-biological thin sections up to 200 nm. With the development of automated cutting and fluorescence-assisted localization techniques, CFFER has become an important technique for studying the in-situ three-dimensional structure of cells and tissues.
[0003] Samples can be thinned using an ion beam in a dual-beam scanning electron microscope (SEM) and then transferred to a transmission electron microscope (TEM) for electron tomography (ETM) data collection. These samples require stringent storage conditions, needing to be preserved at temperatures below -150°C, with minimal adsorption of ice crystals and other contaminants on the sample surface. Samples with excessive adsorption of contaminants are damaged and unusable. Currently, these samples are stored in liquid nitrogen tanks before being transferred to cryo-TEM for imaging. During this storage process, the samples undergo multiple transfers, coming into contact with the humid atmosphere and liquid nitrogen containing small ice crystals, resulting in some degree of contamination. Furthermore, during storage in the liquid nitrogen tank, the liquid nitrogen inevitably contains ice crystals, causing further adsorption of small ice crystals onto the sample surface, further contaminating the sample. This significantly reduces the number of usable samples and the effective area per slice, impacting subsequent data collection and high-resolution structural analysis. Utility Model Content
[0004] To address the problems existing in the prior art, according to one aspect of this utility model, a high-vacuum cryogenic storage device is provided. This high-vacuum cryogenic storage device includes a main body, a cooling body, and a sample delivery channel connected to the main body. A vacuum chamber is formed within the main body. The cooling body includes a Dewar flask disposed within the vacuum chamber, and the Dewar flask is filled with coolant. A sample storage position is formed within the vacuum chamber and is adjacent to the cooling body. The sample delivery channel has an outer delivery port and an inner delivery port. The outer delivery port is used to connect with an external electron microscope sample delivery device, and the inner delivery port communicates with the vacuum chamber and is aligned with the sample storage position.
[0005] The high-vacuum cryogenic storage device provided in this application achieves sample transport through a sample transport channel. The entire transport process takes place within the sample transport channel and vacuum chamber, thus avoiding sample contamination during transport. The sample is stored in the sample storage position, and a cooling element ensures that the sample is in a high-vacuum cryogenic environment (e.g., temperature below -150°C, vacuum degree better than 5×10⁻⁶). -3 Pa) to avoid sample contamination during storage. This prevents sample contamination, ensures sample quality, increases the number of effective samples and the effective area of individual samples during experiments, and ensures the smooth progress of subsequent data collection and high-resolution structural analysis.
[0006] For example, the sample transport channel includes a first transport channel extending in a horizontal direction, the inner transport port includes a first inner transport port located on the side wall of the main body, the outer transport port includes a first outer transport port located on the outside of the main body, and the sample transport component includes a sample transport rod, with the first outer transport port used to cooperate with the sample transport rod.
[0007] For example, a mounting plate is provided at the end of the first conveying channel away from the first inner conveying port, and a first outer conveying port is opened on the mounting plate. The mounting plate is provided with a positioning post adapted to the positioning hole of the sample conveying rod. A fixing claw is also connected to the mounting plate. At least a part of the structure of the sample conveying rod is sandwiched between the fixing claw and the mounting plate. A sample pre-vacuuming channel is provided on the mounting plate, and a pre-vacuuming pump is connected to the sample pre-vacuuming channel.
[0008] For example, the bottom of the Dewar flask is provided with a turntable assembly that is rotatable relative to the Dewar flask. The turntable assembly includes a rotary motor, a rotating platform, and a transmission platform. The output end of the rotary motor is connected to the transmission platform and drives the rotating platform to rotate through the transmission platform. Multiple sample storage positions are formed on the rotating platform along the rotation direction. The sample storage positions are used to place the first sample holder.
[0009] For example, the bottom of the Dewar flask is provided with a baffle cover, which includes a top cover that contacts the bottom of the Dewar flask and a side cover that extends downward along the outer edge of the top cover. Multiple sample storage positions are located inside the side cover, and the side cover has a communication port corresponding to the first inner conveying port. A first hollow structure is provided at the center of the rotating table, and a second hollow structure is provided at the center of the top cover. The bottom of the Dewar flask is provided with a protrusion that extends into the first and second hollow structures.
[0010] For example, the sample transport channel includes a second transport channel extending vertically, the inner transport port includes a second inner transport port located on the bottom wall of the main body, the outer transport port includes a second outer transport port located on the outside of the main body, the sample transport component includes a liquid nitrogen cup, the second outer transport port is used to connect with the liquid nitrogen cup, the high vacuum cryogenic storage device includes a frame, the main body is disposed on the frame, an elastic component is disposed on the frame, and the liquid nitrogen cup is installed above the elastic component.
[0011] For example, a movable arm is provided in the vacuum chamber that is movable in the vertical direction relative to the main body. A gripper is provided at the bottom of the movable arm for gripping the second sample holder. The gripper extends into or out of the liquid nitrogen cup under the drive of the movable arm. The gripper includes a claw for locking into the groove of the second sample holder and a blocking and limiting member for blocking the slot of the second sample holder.
[0012] For example, a pusher is also provided inside the vacuum chamber. When the second sample holder moves to the sample storage position under the action of the gripper, the pusher moves and clamps the second sample holder between the pusher and the cooling body.
[0013] For example, the cooling body also includes an extension block disposed on the side of the Dewar flask, and a sample storage position is formed on the side of the extension block away from the Dewar flask. When the second sample holder moves to the sample storage position under the action of the gripper, the pusher moves and clamps the second sample holder between the pusher and the extension block.
[0014] For example, an isolation valve is provided on the side of the sample delivery channel near the main body. The opening and closing of the isolation valve realizes the connection and disconnection between the sample delivery channel and the vacuum chamber. The main body is also connected to a vacuum pump group, which includes a mechanical pump and a molecular pump. The mechanical pump is connected to the molecular pump, and the molecular pump is connected to the vacuum chamber.
[0015] This utility model description introduces a series of simplified concepts, which will be further explained in detail in the detailed description section. This utility model description is not intended to limit the key features and essential technical features of the claimed technical solution, nor is it intended to limit the scope of protection of the claimed technical solution.
[0016] The advantages and features of this utility model will be described in detail below with reference to the accompanying drawings. Attached Figure Description
[0017] The following drawings, which are incorporated herein by reference as part of this invention, are provided for understanding the invention. The drawings illustrate embodiments of the invention and their descriptions, serving to explain the principles of the invention. In the drawings,
[0018] Figure 1 This is a perspective view of a high-vacuum cryogenic storage device according to an exemplary embodiment of the present invention;
[0019] Figure 2 This is a cross-sectional view of a high-vacuum cryogenic storage device and a first sample holder according to an exemplary embodiment of the present invention;
[0020] Figure 3 A perspective view of a turntable assembly, a enclosure cover, and a first sample holder according to an exemplary embodiment of the present invention;
[0021] Figure 4 A perspective view of a high-vacuum cryogenic storage device and a liquid nitrogen cup according to an exemplary embodiment of the present invention;
[0022] Figure 5 This is a cross-sectional view of a high-vacuum cryogenic storage device, a liquid nitrogen cup, and a second sample holder according to an exemplary embodiment of the present invention;
[0023] Figure 6 A perspective view of a portion of the structure of a high-vacuum cryogenic storage device, a liquid nitrogen cup, and a second sample holder according to an exemplary embodiment of the present invention;
[0024] Figure 7 This is a perspective view of a high-vacuum cryogenic storage device according to an exemplary embodiment of the present invention;
[0025] Figure 8 This is a perspective view of a high-vacuum cryogenic storage device according to an exemplary embodiment of the present invention.
[0026] The above figures include the following reference numerals:
[0027] 10. High vacuum cryogenic storage device; 110. Main body; 1101. Vacuum chamber; 1102. Sample storage position; 1110. Turntable assembly; 1111. Rotating stage; 1112. Rotary motor; 1113. Transmission stage; 1120. Enclosure cover; 1121. Top cover; 1122. Side cover; 1123. Connecting port; 120. Cooling body; 1210. Protrusion; 1220. Extension block; 130. Sample conveying channel; 1310. First conveying channel; 1311. First external conveying port; 1312. First internal conveying port; 1313. Mounting plate; 131 4. Positioning column; 1315. Fixing claw; 1316. Sample pre-extraction channel; 1320. Second transport channel; 1321. Second external transport port; 1322. Second internal transport port; 1323. Sealed installation structure; 1330. Sample pre-extraction channel; 140. Frame; 1410. Elastic component; 1510. Moving arm; 1520. Gripping component; 1521. Clamp; 1522. Blocking and limiting component; 1530. Lead screw; 160. Pushing component; 170. Isolation valve; 180. Molecular pump; 20. Liquid nitrogen cup; 30. Second sample holder; 40. First sample holder. Detailed Implementation
[0028] In the following description, numerous details are provided to enable a thorough understanding of the present invention. However, those skilled in the art will appreciate that the following description merely illustrates preferred embodiments of the present invention, which may be practiced without one or more of these details. Furthermore, to avoid confusion with the present invention, some technical features well-known in the art have not been described in detail.
[0029] To fully understand the embodiments of this utility model, a detailed structure will be presented in the following description. Obviously, the implementation of the embodiments of this utility model is not limited to the specific details familiar to those skilled in the art. Preferred embodiments of this utility model are described in detail below; however, in addition to these detailed descriptions, this utility model may have other embodiments.
[0030] This invention provides a high-vacuum cryogenic storage device. This device can be used to store frozen samples, such as frozen slide samples. (Refer to reference...) Figure 1 , Figure 2 , Figure 4 , Figure 7 and Figure 8 The high-vacuum cryogenic storage device 10 includes a main body 110, a cooling body 120, and a sample delivery channel 130 connected to the main body 110. A vacuum chamber 1101 is formed within the main body 110, isolated from the external space. The cooling body 120 includes a Dewar flask disposed within the vacuum chamber 1101, which may be filled with coolant. The cooling body 120 is used to maintain the low temperature of frozen samples. The Dewar flask contains any type of coolant. Specifically, the coolant may be liquid nitrogen. The Dewar flask may be a metal component, such as copper. A sample storage position 1102 is formed within the vacuum chamber 1101 and is adjacent to the cooling body 120. The sample delivery channel 130 has an external delivery port and an internal delivery port. The external delivery port can be used to connect with an external electron microscope sample delivery device, and the internal delivery port can communicate with the vacuum chamber 1101 and be aligned with the sample storage position 1102. The sample storage position 1102 and the inner delivery port can be arranged adjacent to each other or at a certain distance. The cooling body 120 can maintain the temperature of the sample storage position 1102 below -150°C. The sample storage position 1102 can be used to store samples. It should be noted that frozen samples are usually located in the sample holder. Hereafter, when referring to the sample holder, it refers to both the sample holder and the sample located within it. The sample storage position 1102 can be configured according to usage requirements. For example, if it is necessary to support the sample holder, the sample storage position 1102 is formed on a support platform (e.g., ...). Figure 2Alternatively, sample storage location 1102 may not be contained in a physical entity; it can be understood simply as a space (e.g., ...). Figure 4 The sample storage position 1102 is arranged adjacent to the cooling body 120, ensuring a tight fit between the sample holder and the sample storage position to better guarantee that the sample holder is in a low-temperature environment. When it is necessary to transport a sample to the high-vacuum cryogenic storage device 10, the electron microscope sample transport component is connected to the external transport port, and the sample enters the vacuum chamber 1101 through the sample transport channel 130 (the sample transport process depends on the type of electron microscope sample transport component; the sample can be moved by the moving arm 1510 or the push rod of the electron microscope sample transport component, the specific movement method is described in detail below). Since the inner transport port is aligned with the inner transport port, that is, after being removed from the sample transport channel 130, the sample can directly reach the sample storage position 1102 for storage. Similarly, when it is necessary to remove the sample from the high-vacuum cryogenic storage device 10, similar to the transport process, the sample is moved from the sample storage position 1102 to the external transport port by the push rod or the moving arm 1510, until the sample enters the corresponding electron microscope sample transport component.
[0031] The high-vacuum cryogenic storage device 10 provided in this application achieves sample transport through a sample transport channel 130. The entire transport process takes place within the sample transport channel 130 and the vacuum chamber 1101, thus avoiding sample contamination during transport. The sample is stored in the sample storage position 1102, and a cooling body 120 ensures the sample is in a high-vacuum cryogenic environment (temperature below -150°C, vacuum degree better than 5×10⁻⁶). -3 Pa (with a shielding device) is used to prevent sample contamination during storage. This avoids sample contamination, ensures sample quality, increases the number of effective samples and the effective area of individual samples during experiments, and ensures the smooth progress of subsequent data collection and high-resolution structural analysis.
[0032] For example, in conjunction with reference Figure 1 , Figure 2 and Figure 3The sample transport channel 130 may include a first transport channel 1310 extending horizontally, an inner transport port may include a first inner transport port 1312 located on the side wall of the main body 110, and an outer transport port may include a first outer transport port 1311 located on the outer side of the main body 110. The sample transport component may include a sample transport rod, and the first outer transport port 1311 can be used to connect with the sample transport rod. The sample transport rod is a cryogenic sample transport rod commonly used in scanning electron microscopes on the market. The sample transport rod is usually provided with a push rod, and the sample holder includes a first sample holder 40, which is disposed in the storage cavity of the sample transport rod. The push rod pushes the first sample holder 40 to move. The horizontally extending first transport channel 1310 can better cooperate with the sample transport rod. In the embodiment equipped with a pre-vacuum pump, isolation valve 170, fixing claw 1315, and mounting plate 1313, the movement process of the first sample holder 40 can be as follows: the sample transfer rod is connected to the mounting plate, the sample transfer rod is locked by the claw 1315, the pre-vacuum valve is opened, the first transport channel 1310 is pre-vacuumed by the pre-vacuum pump, then the pre-vacuum valve is closed, the isolation valve 170 is opened, the valve on the transfer rod is opened, and the first sample holder 40 is pushed through the first inner transport port 1312, and can then be directly pushed to the sample storage position 1102. The setting of the first transport channel makes sample transport between the high vacuum cryogenic storage device 10 and the scanning electron microscope more convenient. The scanning electron microscope can be of any type, for example, a cryogenic dual-beam scanning electron microscope.
[0033] For example, in conjunction with reference Figure 1 , Figure 2 , Figure 7 and Figure 8A mounting plate 1313 may be provided at the end of the first conveying channel 1310 away from the first inner conveying port 1312. The first outer conveying port 1311 is opened on the mounting plate 1313. A positioning post 1314 adapted to the positioning hole of the sample conveying rod may be provided on the mounting plate 1313. Typically, one end of the sample conveying rod is a plate-shaped structure, and the positioning hole is provided on the plate-shaped structure. During installation, the plate-shaped structure of the sample conveying rod abuts against the mounting plate 1313, and the positioning post 1314 is inserted into the positioning hole, forming a rapid positioning of the sample conveying rod and the first sample holder 40 inside it, which can improve the efficiency of the sample conveying process. Exemplarily, a fixing claw 1315 may also be connected to the mounting plate 1313, and at least a part of the structure of the sample conveying rod may be clamped between the fixing claw 1315 and the mounting plate 1313. A sample pre-vacuum channel 1316 may be provided on the mounting plate 1313, and a pre-vacuum pump may be connected to the sample pre-vacuum channel 1316. The pre-vacuum pump can pre-evacuate the first delivery channel 1310. Specifically, when the sample delivery rod is installed on the mounting plate 1313, the fixing claw 1315 can abut against the plate-like structure of the sample delivery rod, so that the plate-like structure is clamped between the mounting plate 1313 and the fixing claw 1315, further ensuring the stability of the connection between the sample delivery rod and the first delivery channel 1310.
[0034] For example, in conjunction with reference Figure 2 and Figure 3 The bottom of the Dewar flask can be provided with a turntable assembly 1110 that is rotatable relative to the Dewar flask. Multiple sample storage positions 1102 can be formed on the turntable assembly 1110 along the rotation direction. These sample storage positions 1102 can be used to place the first sample holder 40. The multiple sample storage positions 1102 are spaced apart from each other. By rotating the turntable assembly 1110, the first inner delivery port 1312 can be aligned with different sample storage positions 1102, thus enabling multiple samples to be placed into different sample storage positions 1102 respectively. This allows for the storage of multiple samples, improving the storage capacity of the high-vacuum cryogenic storage device 10. In some embodiments, such as... Figure 7 The sample storage position 1102 can be set adjacent to the side wall of the Dewar flask.
[0035] For example, in conjunction with reference Figure 2 and Figure 3The bottom of the Dewar flask may be provided with a protective cover 1120. The protective cover 1120 may include a top cover 1121 that contacts the bottom of the Dewar flask and a side cover 1122 that extends downward along the outer edge of the top cover 1121. Multiple sample storage positions 1102 may all be located inside the side cover 1122, and the side cover 1122 may have a connecting port 1123 corresponding to the first inner conveying port 1312. The protective cover 1120 covers the turntable assembly 1110 and surrounds the multiple sample storage positions 1102, that is, surrounds the first sample holder 40 within the sample storage positions 1102. The top cover 1121 contacts the bottom of the Dewar flask and conducts low temperature to the side cover 1122, forming a low temperature cavity within the protective cover 1120. The sample storage positions 1102 and the first sample holder 40 therein are located within the low temperature cavity. This arrangement can better ensure that the first sample holder 40 is in a low temperature environment. The enclosure cover 1120 can adsorb impurity gases in the vacuum chamber 1101, effectively reducing contamination of the sample by impurity gases. Specifically, the turntable assembly 1110 may include a rotary motor 1112, a turntable 1111, and a transmission stage 1113. The output end of the rotary motor 1112 is connected to the transmission stage 1113, which drives the turntable 1111 to rotate. There are multiple sample storage positions 1102, which are formed on the turntable 1111 along the rotation direction. The rotary motor 1112 can drive the transmission stage 1113 to rotate, which in turn drives the turntable 1111 to rotate, exposing different sample storage positions 1102 to the communication port 1123 for sample transfer.
[0036] For example, in conjunction with reference Figure 2 and Figure 3 The rotating platform 1111 may have a first hollow structure at its center, and the top cover 1121 may have a second hollow structure at its center. The bottom of the Dewar flask has a protrusion 1210 that extends into the first and second hollow structures. A rotary motor 1112 may be connected to the bottom of the protrusion 1210. For example, a heat-insulating gasket may be provided between the protrusion 1210 and the rotary motor 1112. In this way, the protrusion 1210 extends into the low-temperature chamber, further ensuring the effect of low-temperature storage, and the heat-insulating material is used to connect and fix the rotary motor 1112.
[0037] For example, in conjunction with reference Figure 1 , Figure 2 , Figure 4 and Figure 7The main body 110 can be connected to a vacuum pump assembly to ensure a vacuum environment in the vacuum chamber 1101. Exemplarily, the vacuum pump assembly may include a molecular pump 180 and a mechanical pump. The mechanical pump is connected to the molecular pump 180, and the molecular pump 180 is connected to the vacuum chamber 1101. Exemplarily, the first delivery channel 1310 can be connected to a pre-vacuum pump via a pre-evacuation valve. The pre-evacuation pump can pre-evacuate the first delivery channel 1310 to ensure a vacuum environment in the first delivery channel 1310 during sample transfer.
[0038] For example, the process of transporting the sample into the vacuum chamber 1101 through the first transport channel 1310 can be as follows: the sample transport rod with the sample fixed thereon is connected to the first external transport port 1311, the positioning post 1314 is inserted into the positioning hole, the sample transport rod abuts against the mounting plate 1313, and the sample transport rod is locked by the fixing claw 1315; the pre-vacuum pump and pre-vacuum valve are turned on to pre-vacuum the first transport channel 1310, and after the vacuum degree in the first transport channel 1310 is better than a set value (e.g., 20 Pa), the pre-vacuum valve is closed, the isolation valve 170 is opened, and the first sample holder 40 is moved to the sample storage position 1102 by the push rod. The first transport channel 1310 can be connected to the sample injection pre-vacuum channel 1330. The pre-vacuum pump is connected to the sample injection pre-vacuum channel 1330 through the pre-vacuum valve. When it is necessary to pre-vacuum the first transport channel 1310, the pre-vacuum pump works and evacuates the first transport channel 1310 through the pre-vacuum valve and the sample injection pre-vacuum channel 1330. In this application, the vacuuming of the first delivery channel 1310 can be achieved by a pre-vacuum pump, a pre-vacuum valve, and the sample injection pre-vacuum channel 1330.
[0039] Similarly, the process of transporting the sample outward from the vacuum chamber 1101 through the first transport channel 1310 can be as follows: the sample transport rod is connected to the first external transport port 1311, the positioning post 1314 is inserted into the positioning hole, the sample transport rod abuts against the mounting plate 1313, and the sample transport rod is locked by the fixing claw 1315; the pre-vacuum pump and pre-vacuum valve are turned on to pre-vacuum the first transport channel 1310. After the vacuum degree in the first transport channel 1310 is better than the set value (e.g., 20 Pa), the pre-vacuum valve is closed, the isolation valve 170 is opened, and the first sample holder 40 is moved outward from the sample storage position 1102 by the push rod of the sample transport rod. After the first sample holder 40 is moved out, the isolation valve 170 is closed.
[0040] For example, in conjunction with reference Figure 4 , Figure 5 and Figure 6The sample transport channel 130 may include a second transport channel 1320 extending vertically. The inner transport port may include a second inner transport port 1322 located on the bottom wall of the main body 110, and the outer transport port includes a second outer transport port 1321 located on the outside of the main body 110. The sample transport component may include a liquid nitrogen cup, and the second outer transport port 1321 is used to connect with the external liquid nitrogen cup 20. The liquid nitrogen cup 20 is a sample transport component commonly used in transmission electron microscopes (TEM). The sample holder includes a second sample holder 30, in which the sample is mounted. The second sample holder 30 is placed inside the liquid nitrogen cup 20. The second transport port can dock with the liquid nitrogen cup 20, and a sealing installation structure 1323 may be provided at the second transport port to ensure the sealing between the high-vacuum cryogenic storage device 10 and the liquid nitrogen cup 20 after docking. This arrangement facilitates the transfer of the second sample holder 30 between the high-vacuum cryogenic storage device 10 and the TEM. After the transfer is completed, the second sample holder 30 is located at the sample storage position 1102 to ensure the effectiveness of cryogenic storage. The second transport channel 1320 facilitates sample transport between the high-vacuum cryogenic storage device 10 and the transmission electron microscope. In this embodiment, the sample storage position 1102 can be located on the side of the cooling body 120. Exemplarily, the storage device 10 may include a frame 140, with the main body 110 disposed on the frame 140. An elastic component 1410 may be disposed on the frame 140, and the liquid nitrogen cup 20 may be mounted above the elastic component 1410. In this way, the elastic component 1410 pushes against the liquid nitrogen cup 20, making the connection between the liquid nitrogen cup 20 and the second transport channel 1320 more stable.
[0041] It should be noted here that the high vacuum cryogenic storage device 10 in this application may only have the first transport channel 1310 (e.g., Figure 1 and Figure 2 It may only have a second conveying channel 1320 (e.g.) Figure 4 and Figure 5 It can also simultaneously have a first conveying channel 1310 and a second conveying channel 1320 (e.g. Figure 7 and Figure 8 ).
[0042] For example, in conjunction with reference Figure 5 and Figure 6A movable arm 1510, vertically movable relative to the main body 110, is provided within the vacuum chamber 1101. A gripping element 1520 for grasping the second sample holder 30 is provided at the bottom of the movable arm 1510. The gripping element 1520 extends into or retracts from the liquid nitrogen cup 20 under the action of the movable arm 1510. The second sample holder 30 is placed inside the liquid nitrogen cup 20, and the gripping element 1520 can extend into the liquid nitrogen cup 20 to grasp or release the second sample holder 30. In this way, by using the movable arm 1510 to drive the gripping element 1520, the transfer process of the second sample holder 30 between the high vacuum cryogenic storage device 10 and the transmission electron microscope is more efficient. Furthermore, during the transfer process, the second sample holder 30 is isolated from the outside world within the liquid nitrogen cup 20, the second transfer channel, and the main body 110, preventing sample contamination. For example, a lead screw 1530 may be provided within the main body 110 to drive the movable arm 1510.
[0043] For example, in conjunction with reference Figure 4 and Figure 6 The gripper 1520 may include a claw 1521 for engaging with a groove in the second sample holder 30 and a blocking and limiting member 1522 for blocking the slot in the second sample holder 30. The blocking and limiting member 1522 may include a blocking strip and limiting strips located on opposite sides of the blocking strip, the limiting strips abutting against the side wall of the second sample holder 30 for limiting. This ensures the gripper 1520's stability during the gripping process of the second sample holder 30. During the movement of the second sample holder 30 in the second transfer channel, the liquid nitrogen cup 20, and the vacuum chamber 1101, the blocking and limiting member 1522 can reduce the contact between the sample and the outside, further preventing sample contamination.
[0044] For example, in conjunction with reference Figure 4 and Figure 6 A pusher 160 can also be provided inside the vacuum chamber 1101. When the second sample holder 30 moves to the sample storage position 1102 under the action of the gripper 1520, the pusher 160 moves and clamps the second sample holder 30 between the pusher 160 and the cooling body 120. The pusher 160 can move horizontally. In this way, the pusher 160 makes the second sample holder 30 adhere to the cooling body 120, further ensuring that the second sample holder 30 is in a high vacuum low temperature environment (temperature below -150°C, vacuum degree better than 5×10⁻⁶). -3 (Pa). For example, the cooling body 120 may include an extension block 1220 disposed on the side of the Dewar flask, and the sample storage position 1102 may be formed on the side of the extension block 1220 away from the Dewar flask. When the second sample holder 30 moves to the sample storage position 1102 under the action of the gripper 1520, the pusher moves and clamps the second sample holder 30 between the pusher 160 and the extension block 1220. The extension block 1220 may be a copper metal block.
[0045] For example, in conjunction with reference Figure 2 , Figure 5 and Figure 8 An isolation valve 170 is provided on the side of the sample transport channel 130 near the main body 110. The opening and closing of the isolation valve 170 controls the connection between the sample transport channel 130 and the vacuum chamber 1101. Understandably, during storage, the isolation valve 170 is closed to ensure the isolation of the vacuum chamber 1101 from the external environment. When sample transport is required, the isolation valve 170 opens to allow for smooth sample transport. When the sample is transported via the second transport channel 1320, which is connected to a liquid nitrogen cup 20, dry nitrogen gas can be introduced into the vacuum chamber 1101 before the isolation valve 170 is opened for sample transport.
[0046] For example, the process of transporting the sample into the vacuum chamber 1101 through the second transport channel 1320 can be as follows: the liquid nitrogen cup containing the second sample holder 30 is connected to the second external transport port 1321. Through the cooperation of the sealing installation structure 1323 and the elastic component 1410, the liquid nitrogen cup 20 is securely connected to the second external transport port 1321. Dry nitrogen gas is introduced into the vacuum chamber 1101. The isolation valve 170 is opened. The moving arm 1510 drives the gripper 1520 to extend into the liquid nitrogen cup 20. The gripper 1520 grips the second sample holder 30. The moving arm 1510 drives the gripper 1520 to move the second sample holder 30 upward to the sample storage position 1102. The pusher 160 pushes the second sample holder 30 to make the second sample holder 30 stick to the Dewar flask.
[0047] For example, the process of transporting the sample from the vacuum chamber 1101 to the outside through the second transport channel 1320 can be as follows: the liquid nitrogen cup 20 is stably connected to the second external transport port 1321 by the cooperation of the sealing installation structure 1323 and the elastic component 1410, the moving arm 1510 drives the gripper 1520 to the sample storage position 1102, and dry nitrogen gas is introduced into the vacuum chamber 1101. When the pressure in the vacuum chamber reaches atmospheric pressure, the isolation valve 170 is opened, and the second sample holder 30 is moved down by the moving arm 1510 driving the gripper 1520 until the second sample holder 30 is placed in the liquid nitrogen cup 20. The moving arm 1510 moves up, the isolation valve 170 is closed, and the vacuum pump group evacuates the vacuum chamber 1101.
[0048] For example, in conjunction with reference Figure 7 and Figure 8 In this embodiment, the main body 110 is connected to a first transport channel 1310 and a second transport channel 1320. Thus, the high-vacuum cryogenic storage device 10 can be adapted to the sample transport components of both scanning electron microscopes (SEMs) and transmission electron microscopes (TEMs).
[0049] In the description of this utility model, it should be understood that the directional terms such as "front", "rear", "up", "down", "left", "right", "horizontal", "vertical", "horizontal", "top", and "bottom" indicate the orientation or positional relationship, which are usually based on the orientation or positional relationship shown in the accompanying drawings. They are only for the convenience of describing this utility model and simplifying the description. Unless otherwise stated, these directional terms do not indicate or imply that the device or element referred to must have a specific orientation or be constructed and operated in a specific orientation, and therefore should not be construed as a limitation on the scope of protection of this utility model. The directional terms "inner" and "outer" refer to the inner and outer contours of each component itself.
[0050] For ease of description, relative terms such as "above," "over," "on the upper surface of," and "above" are used here to describe the regional positional relationship of one or more components or features shown in the figures to other components or features. It should be understood that relative terms include not only the orientation of the component as depicted in the figure but also different orientations during use or operation. For example, if the components in the figures are inverted as a whole, "above" or "above other components or features" will include cases where the component is "below" or "under" other components or features. Thus, the exemplary term "above" can include both "above" and "below." Furthermore, these components or features may also be positioned at other different angles (e.g., rotated 90 degrees or other angles), and this document intends to include all such cases.
[0051] It should be noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to limit the exemplary embodiments according to this application. As used herein, the singular form is intended to include the plural form as well, unless the context clearly indicates otherwise. Furthermore, it should be understood that when the terms "comprising" and / or "including" are used in this specification, they indicate the presence of features, steps, operations, parts, components, and / or combinations thereof.
[0052] It should be noted that the terms "first," "second," etc., used in the specification, claims, and accompanying drawings of this application are used to distinguish similar objects and are not necessarily used to describe a specific order or sequence. It should be understood that such data can be interchanged where appropriate so that the embodiments of this application described herein can be implemented in sequences other than those illustrated or described herein.
[0053] This utility model has been described through the above embodiments. However, it should be understood that the above embodiments are for illustrative purposes only and are not intended to limit the utility model to the described embodiments. Furthermore, those skilled in the art will understand that this utility model is not limited to the above embodiments, and many more variations and modifications can be made based on the teachings of this utility model, all of which fall within the scope of protection claimed by this utility model. The scope of protection of this utility model is defined by the appended claims and their equivalents.
Claims
1. A high-vacuum cryogenic storage device, characterized in that, The device includes a main body, a cooling body, and a sample delivery channel connected to the main body. A vacuum chamber is formed within the main body. The cooling body includes a Dewar flask disposed within the vacuum chamber and filled with coolant. A sample storage position is formed within the vacuum chamber and is disposed adjacent to the cooling body. The sample delivery channel has an outer delivery port and an inner delivery port. The outer delivery port is used to connect with an external electron microscope sample delivery device, and the inner delivery port communicates with the vacuum chamber and is aligned with the sample storage position.
2. The high-vacuum cryogenic storage device according to claim 1, characterized in that, The sample transport channel includes a first transport channel extending horizontally, the inner transport port includes a first inner transport port located on the side wall of the main body, the outer transport port includes a first outer transport port located on the outside of the main body, the sample transport component includes a sample transport rod, and the first outer transport port is used to cooperate with the sample transport rod.
3. The high-vacuum cryogenic storage device according to claim 2, characterized in that, An installation plate is provided at the end of the first conveying channel away from the first inner conveying port. The first outer conveying port is opened on the installation plate. The installation plate is provided with a positioning post adapted to the positioning hole of the sample conveying rod. A fixing claw is also connected to the installation plate. At least a part of the structure of the sample conveying rod is sandwiched between the fixing claw and the installation plate. A sample pre-vacuuming channel is provided on the installation plate. The sample pre-vacuuming channel is connected to a pre-vacuuming pump.
4. The high-vacuum cryogenic storage device according to claim 2, characterized in that, The bottom of the Dewar flask is provided with a turntable assembly that can rotate relative to the Dewar flask. The turntable assembly includes a rotary motor, a rotating platform, and a transmission platform. The output end of the rotary motor is connected to the transmission platform and drives the rotating platform to rotate through the transmission platform. Multiple sample storage positions are formed on the rotating platform along the rotation direction. The sample storage positions are used to place the first sample holder.
5. The high-vacuum cryogenic storage device according to claim 4, characterized in that, The bottom of the Dewar flask is provided with a baffle cover, which includes a top cover that contacts the bottom of the Dewar flask and a side cover that extends downward along the outer edge of the top cover. Multiple sample storage positions are located inside the side cover, and the side cover has a communication opening corresponding to the first inner conveying port. The center of the rotating platform is provided with a first hollow structure, and the center of the top cover is provided with a second hollow structure. The bottom of the Dewar flask is provided with a protrusion that extends into the first hollow structure and the second hollow structure.
6. The high-vacuum cryogenic storage device according to claim 1, characterized in that, The sample transport channel includes a second transport channel extending vertically, the inner transport port includes a second inner transport port located on the bottom wall of the main body, the outer transport port includes a second outer transport port located on the outside of the main body, the sample transport component includes a liquid nitrogen cup, the second outer transport port is used to cooperate and connect with the liquid nitrogen cup, the high vacuum cryogenic storage device includes a frame, the main body is disposed on the frame, the frame is provided with an elastic component, and the liquid nitrogen cup is installed above the elastic component.
7. The high-vacuum cryogenic storage device according to claim 6, characterized in that, The vacuum chamber is provided with a movable arm that is vertically movable relative to the main body. The bottom of the movable arm is provided with a gripper for gripping the second sample holder. The gripper extends into or out of the liquid nitrogen cup under the drive of the movable arm. The gripper includes a claw for locking into the groove of the second sample holder and a blocking and limiting member for blocking the slot of the second sample holder.
8. The high-vacuum cryogenic storage device according to claim 7, characterized in that, The vacuum chamber is also provided with a pusher. When the second sample holder moves to the sample storage position under the action of the gripper, the pusher moves and clamps the second sample holder between the pusher and the cooling body.
9. The high-vacuum cryogenic storage device according to claim 8, characterized in that, The cooling body also includes an extension block disposed on the side of the Dewar flask. The sample storage position is formed on the side of the extension block away from the Dewar flask. When the second sample holder moves to the sample storage position under the action of the gripper, the pusher moves and clamps the second sample holder between the pusher and the extension block.
10. The high-vacuum cryogenic storage device according to claim 1, characterized in that, An isolation valve is provided on the side of the sample delivery channel near the main body. The opening and closing of the isolation valve realizes the connection and disconnection between the sample delivery channel and the vacuum chamber. The main body is also connected to a vacuum pump group, which includes a mechanical pump and a molecular pump. The mechanical pump is connected to the molecular pump, and the molecular pump is connected to the vacuum chamber.