A device and method for preparing a liquid nitrogen slush frozen sample

Abstract

The application relates to the technical field of frozen sample preparation, and particularly relates to a liquid nitrogen mud frozen sample preparation device and method, which comprises a machine body, a partition plate, an electric push rod, a movable plate, a vacuum pump, a liquid nitrogen pump, a liquid nitrogen tank and a cylinder; the push rod is fixedly installed on the cylinder; a sample feeding assembly is arranged; a transfer box is arranged on the sample feeding assembly; two openings are symmetrically arranged on the top and bottom outer walls of the transfer box; four rotating shafts are fixedly installed in the two openings respectively, and the two rotating shafts in one opening are symmetrically arranged; four rotating plates are rotatably sleeved on the rotating shafts; a linkage assembly is arranged; and a sealing assembly is arranged. Compared with the prior art, the transfer box can maintain a low-temperature vacuum environment inside when being closed, which is very important for samples needing low-temperature preservation, can effectively protect the state of the samples, ensures that the samples are not affected by the external environment during the transfer and cooling process, and ensures the accuracy of the observation results.

Description

Technical Field

[0001] This invention relates to the field of frozen sample preparation technology, and in particular to an apparatus and method for preparing liquid nitrogen mud frozen samples. Background Technology

[0002] Liquid nitrogen sludge freezing is a freezing method that utilizes liquid nitrogen to transform into liquid nitrogen sludge under vacuum, rapidly lowering the sample temperature to prevent ice crystal formation and preserve the sample's microstructure. This method ensures that the sample is not damaged during freezing and is suitable for analyzing the microstructure and composition of samples in fields such as scanning electron microscopy.

[0003] A search revealed that Chinese Patent CN107991330A discloses an apparatus for preparing frozen liquid nitrogen mud samples, including a sample injection device, a liquid nitrogen mud cooling device, and a vacuum pump connected to both the sample injection device and the liquid nitrogen mud cooling device. The sample injection device is used to fix the sample and deliver it into the liquid nitrogen mud cooling device. The vacuum pump is used to place the sample injection device and the liquid nitrogen mud cooling device in a vacuum state, where the liquid nitrogen in the liquid nitrogen mud cooling device is converted into liquid nitrogen mud, and the sample is inserted into the liquid nitrogen mud to obtain a frozen liquid nitrogen mud sample. The frozen sample prepared by this apparatus can prevent the formation of ice crystals and does not damage the microstructure.

[0004] After the frozen sample is prepared by liquid nitrogen cooling, it needs to be kept under vacuum and low temperature at all times. This is because the sample needs to be in a low-temperature and dry state during scanning electron microscopy observation to avoid changes in the sample structure and the deposition of small particles during the drying process. If the sample is exposed to a non-vacuum environment after cooling, it may cause the ice crystals to melt, the sample to sublimate or become contaminated, thus affecting the observation results. However, after the above-mentioned device is prepared, the sample injection device needs to be opened manually to take out the sample. This requires the operator to quickly perform a series of operations to place the sample into the transfer device. This not only provides insufficient protection for the sample, but may also lead to safety hazards due to the haste of the operation. In addition, the sample injection device is in a low-temperature state when the sample is prepared and when the sample is stored. At this time, the operator needs to put his hands into the sample injection device to take out the sample. The confined space is not convenient for operation and increases the risk of frostbite to the operator due to the low temperature.

[0005] Therefore, this application provides an apparatus and method for preparing liquid nitrogen mud frozen samples to meet the requirements of maintaining a low-temperature vacuum environment for the samples after preparation while facilitating operation. Summary of the Invention

[0006] In view of this, the purpose of this invention is to provide an apparatus and method for preparing liquid nitrogen mud frozen samples, so as to solve the problem of inconvenience in sampling, transferring and storing samples after preparation.

[0007] To achieve the above objectives, the present invention provides an apparatus and method for preparing liquid nitrogen mud frozen samples, comprising:

[0008] The machine body has a sample delivery port.

[0009] A partition plate is fixedly installed inside the machine body to separate the sample chamber and the liquid nitrogen chamber, and the partition plate is provided with a connection port;

[0010] An electric actuator is mounted on the machine body;

[0011] A movable plate is slidably mounted on the partition plate and adapted to the connection port; the movable plate is fixedly connected to the movable end of the electric push rod.

[0012] A vacuum pump is mounted on the machine body and connected to the upper and lower chambers of the machine body, respectively.

[0013] A liquid nitrogen pump is mounted on the machine body;

[0014] A liquid nitrogen tank is fixedly installed on the bottom wall of the machine body and connected to the liquid nitrogen pump;

[0015] The cylinder is fixedly installed on the top wall of the machine body.

[0016] The push rod is fixedly installed on the movable end of the cylinder that passes through the machine body;

[0017] The sample delivery component is disposed within the machine body;

[0018] A transfer box is disposed on the sample delivery component;

[0019] Two openings are symmetrically provided on the top and bottom outer walls of the transfer box;

[0020] Four rotating shafts are fixedly installed in two of the openings, and the two rotating shafts in one of the openings are symmetrically arranged.

[0021] Four rotating plates are rotatably mounted on the rotating shaft;

[0022] A shelf is installed inside the transfer box;

[0023] Several sample slots are provided on the rack;

[0024] Several elastic sheets are fixedly installed at positions corresponding to the sample groove;

[0025] The linkage component is located inside the transfer box;

[0026] A closed assembly is located within the body.

[0027] Preferably, the linkage component includes:

[0028] Two linkage rods are respectively hinged between the two rotating plates on both sides, and the distance between the end of the linkage rod that is hinged to the rotating plate at the bottom and the corresponding rotating shaft is less than the distance between the other end of the linkage rod and the corresponding rotating shaft.

[0029] The connecting block is located inside the transfer box;

[0030] The baffle is fixedly fitted onto the connecting block, and when the transfer box is in the closed state, the upper surface of the baffle is in contact with the lower surface of the two rotating plates located at the top;

[0031] Two magnetic blocks are symmetrically fixedly installed inside the transfer box and located at positions corresponding to the shelf.

[0032] A locking assembly is disposed within the transfer box;

[0033] The top wall of the carrier is fixedly connected to the bottom wall of the connecting block. Both the connecting block and the carrier are made of magnetic metal. A strong magnet is fixedly installed at the end of the push rod away from the cylinder. The two rotating plates at the top of the transfer box are provided with slots that are compatible with the connecting block. When the transfer box is in the closed state, the top surface of the connecting block is coplanar with the upper surface of the rotating plate.

[0034] Preferably, the locking component includes:

[0035] Two locking slots are symmetrically formed on the two rotating plates located at the top;

[0036] Two lock holes are symmetrically provided on the transfer box and are adapted to the lock groove;

[0037] Two latches are slidably mounted in the two said lock slots and are made of magnetic metal;

[0038] Two elastic bands are fixedly installed in the two lock holes respectively, and the other end is fixedly connected to the corresponding lock tongue.

[0039] Preferably, the enclosure component includes:

[0040] Two guide plates are fixedly installed on the inner side wall of the machine body;

[0041] Two sliding plates are respectively slidably installed inside the two guide plates;

[0042] A door panel is located inside the machine body at a position corresponding to the sample delivery port, and the top of the door panel is provided with an inclined surface that slopes from the outside to the inside.

[0043] Several return springs are fixedly installed between the sliding plate and the door panel;

[0044] A locking block is fixedly installed on the top inclined surface of the door panel;

[0045] A sliding frame is slidably mounted between the two guide plates;

[0046] A fixed arm is fixedly installed at one end of the sliding frame away from the cylinder, and the other end of the fixed arm is provided with an inclined surface adapted to the door panel;

[0047] A slot is formed on the inclined surface at the end of the fixed arm and is adapted to the locking block;

[0048] A drive assembly is mounted on the fixed arm.

[0049] Preferably, the driving component includes:

[0050] A groove is formed at one end of the fixed arm near the push rod;

[0051] A drive rod is slidably installed in the slide groove, and the end of the drive rod away from the slide groove is fixedly connected to the push rod;

[0052] A clearance groove is formed on the fixed arm;

[0053] A limiting rod is rotatably installed at the center of the relief groove, and a torsion spring is fixedly installed between the limiting rod and the fixed arm.

[0054] Preferably, the sample delivery component includes:

[0055] A fixing plate is fixedly installed on the inner top wall of the machine body;

[0056] A bevel gear is rotatably mounted on the fixed plate;

[0057] The second bevel gear is rotatably mounted on the inner top wall of the machine body and meshes with the first bevel gear;

[0058] The worm gear is fixedly installed at the end of the bevel gear two that is away from the machine body;

[0059] The rack is slidably mounted on the inner side wall of the machine body and meshes with the worm gear;

[0060] The connecting rod is hinged to the bottom of the rack;

[0061] A groove is formed on the first bevel gear;

[0062] A fixing rod is fixedly installed on the push rod and is adapted to the groove;

[0063] The placement components are mounted on the body.

[0064] Preferably, the placement component includes:

[0065] The sample feeding plate is fixedly installed on the machine body at a position corresponding to the sample feeding port;

[0066] The slide rail is fixedly installed on the sample feeding plate, and a notch is provided at the position corresponding to the sample feeding port;

[0067] A limiting frame is fixedly installed on the sample delivery plate and is adapted to the transfer box;

[0068] The storage tray is slidably mounted on the slide rail and hinged to the end of the connecting rod away from the rack. The storage tray and the sample feeding plate are provided with openings that are adapted to the opening.

[0069] The limiting edge is fixedly installed on the storage tray and is adapted to the transfer box.

[0070] Preferably, a sealing plate is fixedly installed at the end of the door panel away from the push rod.

[0071] Preferably, a step is provided at the position corresponding to the rotating plate in the transfer box, and a sealing part is fixedly installed at the end of the rotating plate near the step.

[0072] The method for preparing samples for liquid nitrogen mud freezing includes the following steps:

[0073] Step 1: Open the locking assembly and press the connecting block down from the center of the top of the transport box. The connecting block will cause the carrier to slide down along the magnetic block. At the same time, the baffle will move down with the connecting block. Take out the carrier and place the sample in the corresponding sample slot on the carrier. The elastic sheet will ensure that the sample is installed firmly. Install the transport box from the bottom up. The carrier will be attracted to the magnetic block, thus keeping the transport box closed. Place the transport box on the sample handling tray at the sample delivery port.

[0074] Step 2: Start the equipment. The push rod begins to move downwards a certain distance, first driving the fixed rod to move and engage in the groove. Then, through the sample feeding assembly, the placement tray moves along the sample feeding plate from the sample feeding port to directly below the push rod. The fixed rod slides out of the groove. The push rod continues to move downwards, driving the drive rod to move the fixed arm downwards. The door panel moves downwards with the fixed arm and is squeezed outwards after contacting the sample feeding port. The door panel moves horizontally and blocks the sample feeding port. When the fixed arm also reaches the bottom, the system closure is complete.

[0075] Step 3: The push rod can move downwards along the slide groove independently via the limit rod. At the same time, the end of the push rod can attract the connecting block and attract the locking tongue, causing it to slide into the locking groove. This releases the rotating plate and opens the transfer box, moving the carrier out of the transfer box. The liquid nitrogen pump is started to inject liquid nitrogen, and the vacuum pump is started. After the liquid nitrogen enters the liquid nitrogen mud state, the movable plate is opened by the electric push rod. The push rod continues to move downwards to insert the carrier into the liquid nitrogen mud, allowing the sample to cool and complete the freezing process.

[0076] Step 4: After cooling, lift the push rod upward to raise the rack. Driven by the push rod, install the connecting block into the transfer box. The transfer box is fixed by the limit frame. As the push rod continues to move upward, it separates from the connecting block. The elastic band pulls the locking tongue to slide along the lock groove and into the lock hole, locking the top rotating plate. At the same time, the movable plate is closed by the electric push rod.

[0077] Step 5: When it is necessary to remove the sample, move the push rod upward, the drive rod moves along the slide groove and contacts the limit rod, driving the fixed arm to move upward. When the fixed arm moves to the top of the door panel, the locking block and the locking groove are re-engaged under the action of the return spring, driving the door panel to move upward synchronously, opening the sample delivery port. When the push rod continues to move upward, the fixed rod moves to the point where it separates from the groove, slides back into the groove, drives the bevel gear to reverse, and then pushes the placement tray to move outward along the slide rail to the sample delivery port.

[0078] The beneficial effects of this invention are:

[0079] 1. The apparatus and method for preparing liquid nitrogen mud frozen samples, by setting up a transfer box, can maintain an internal low-temperature vacuum environment when closed. This environment is crucial for samples that need to be preserved at low temperatures, effectively protecting the state of the sample and ensuring that the sample is not affected by the external environment during transfer and cooling, thus ensuring the accuracy of the observation results.

[0080] 2. The apparatus and method for preparing liquid nitrogen mud frozen samples achieve automatic closing and opening of the sample delivery port by setting a push rod to drive a series of components such as a drive rod, a limit rod, and a fixing arm. Before the push rod contacts the transfer box, the door plate has been automatically pushed to the sample delivery port and sealed, thereby ensuring the airtightness of the machine body during vacuuming and freezing processes. This improves work efficiency and effectively avoids safety problems caused by human error.

[0081] 3. The apparatus and method for preparing liquid nitrogen mud frozen samples, by setting bevel gears, worm gears, racks, connecting rods, etc., realizes the automatic delivery, positioning and retrieval of sample transfer boxes, making the entire freezing sample preparation process more intelligent and automated. It avoids the need for operators to manually reach into the machine to take or place samples, thereby reducing the direct contact between operators and the low temperature environment and reducing the risk of frostbite caused by the low temperature environment. Attached Figure Description

[0082] To more clearly illustrate the technical solutions in this invention or the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are only for this invention. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0083] Figure 1 This is a three-dimensional structural diagram of the present invention;

[0084] Figure 2 This is a schematic diagram of the cross-sectional structure of the present invention;

[0085] Figure 3 This is a schematic diagram of the open state of the transfer box of the present invention;

[0086] Figure 4 This is a schematic diagram of the structure of the enclosed component of the present invention;

[0087] Figure 5 This is a schematic diagram of the door panel structure of the present invention;

[0088] Figure 6 For the present invention Figure 2 Enlarged structural diagram at point A;

[0089] Figure 7 This is a schematic diagram of the sample delivery component structure of the present invention;

[0090] Figure 8 This is a schematic diagram of the component placement structure of the present invention;

[0091] Figure 9 This is a schematic diagram of the closed state of the transfer box of the present invention;

[0092] Figure 10 For the present invention Figure 3 A magnified structural diagram at point B in the middle.

[0093] The diagram is marked as follows:

[0094] 1. Body; 2. Divider plate; 21. Electric push rod; 22. Movable plate; 3. Vacuum pump; 4. Liquid nitrogen pump; 5. Liquid nitrogen tank; 6. Cylinder; 61. Push rod; 62. Transfer box; 63. Opening; 64. Rotating shaft; 65. Rotating plate; 66. Linkage rod; 67. Connecting block; 68. Baffle; 69. Loading rack; 610. Magnetic block; 611. Sample tank; 612. Elastic sheet; 7. Guide plate; 71. Sliding plate; 72. Door panel; 73. Return spring; 74. Locking block; 75. Sliding frame; 76. 77. Fixed arm; 78. Slot; 89. Sealing plate; 80. Slide groove; 81. Drive rod; 82. Clearance groove; 83. Limiting rod; 90. Fixed plate; 91. Bevel gear one; 92. Bevel gear two; 93. Worm gear; 94. Rack; 95. Connecting rod; 96. Storage tray; 97. Groove; 98. Fixed rod; 99. Limiting edge; 10. Sample feeding plate; 101. Slide rail; 102. Limiting frame; 11. Lock groove; 111. Lock hole; 112. Lock tongue; 113. Elastic band; 12. Step; 121. Sealing part. Detailed Implementation

[0095] To make the objectives, technical solutions, and advantages of this invention clearer, the invention will be further described in detail below with reference to specific embodiments.

[0096] It should be noted that, unless otherwise defined, the technical or scientific terms used in this invention should have the ordinary meaning understood by one of ordinary skill in the art to which this invention pertains. The terms "first," "second," and similar terms used in this invention do not indicate any order, quantity, or importance, but are merely used to distinguish different components. Terms such as "comprising" or "including" mean that the element or object preceding the word encompasses the elements or objects listed following the word and their equivalents, without excluding other elements or objects. Terms such as "connected" or "linked" are not limited to physical or mechanical connections, but can include electrical connections, whether direct or indirect. Terms such as "upper," "lower," "left," and "right" are used only to indicate relative positional relationships; when the absolute position of the described object changes, the relative positional relationship may also change accordingly.

[0097] like Figures 1 to 10As shown, the apparatus and method for preparing liquid nitrogen mud frozen samples include a body 1 with a sample inlet; a partition plate 2, fixedly installed inside the body 1, used to separate the sample chamber and the liquid nitrogen chamber, and a connection port on the partition plate 2; an electric push rod 21, mounted on the body 1; a movable plate 22, slidably mounted on the partition plate 2 and adapted to the connection port, and fixedly connected to the movable end of the electric push rod 21; a vacuum pump 3, mounted on the body 1 and connected to the upper and lower chambers of the body 1 respectively; a liquid nitrogen pump 4, mounted on the body 1; a liquid nitrogen tank 5, fixedly mounted on the bottom wall of the body 1 and connected to the liquid nitrogen pump 4; and a cylinder 6, fixedly mounted on... The following components are installed on the top wall of the machine body 1: a push rod 61, fixedly installed on the movable end of the cylinder 6 passing through the machine body 1; a sample delivery assembly, located inside the machine body 1; a transfer box 62, located on the sample delivery assembly; two openings 63, symmetrically opened on the top and bottom outer walls of the transfer box 62; four rotating shafts 64, respectively fixedly installed in the two openings 63, with the two rotating shafts 64 in one opening 63 symmetrically arranged; four rotating plates 65, rotatably mounted on the rotating shafts 64; a carrier 69, located inside the transfer box 62; several sample slots 611, opened on the carrier 69; and several elastic plates 612, fixedly installed at positions corresponding to the sample slots 611. The following components are included: a linkage assembly, located within the transfer box 62; and a sealing assembly, located within the body 1. The linkage assembly includes: two linkage rods 66, respectively hinged between two rotating plates 65 on both sides, with the distance between one end hinged to the bottom rotating plate 65 and the corresponding rotating shaft 64 being less than the distance between the other end and the corresponding rotating shaft 64; a connecting block 67, located within the transfer box 62; a baffle 68, fixedly fitted onto the connecting block 67, with the upper surface of the baffle 68 contacting the lower surfaces of the two rotating plates 65 at the top when the transfer box 62 is closed; and two magnetic blocks 610, symmetrically fixedly installed within the transfer box 62 and located within the body 1. A locking assembly is located in the transfer box 62, corresponding to the position of the shelf 69. The top wall of the shelf 69 is fixedly connected to the bottom wall of the connecting block 67. Both the connecting block 67 and the shelf 69 are made of magnetic metal. A strong magnet is fixedly installed at the end of the push rod 61 away from the cylinder 6. The two rotating plates 65 at the top of the transfer box 62 are provided with slots that are compatible with the connecting block 67. When the transfer box 62 is closed, the top surface of the connecting block 67 is coplanar with the upper surface of the rotating plate 65. A step 12 is provided at the position of the transfer box 62 corresponding to the rotating plate 65. A sealing part 121 is fixedly installed at the end of the rotating plate 65 near the step 12.

[0098] In use, open the locking assembly and press the connecting block 67 downwards from the center of the top of the transfer box 62. The connecting block 67 causes the carrier 69 to slide downwards along the magnetic block 610. The carrier 69 gradually detaches from the attraction of the magnetic block 610. At the same time, the baffle 68 moves downwards with the connecting block 67, and the rotating plate 65 disengages from the baffle 68, allowing it to rotate downwards under gravity. Since the distance between the hinged end of the linkage rod 66 at the bottom of the rotating plate 65 and the corresponding rotating shaft 64 is smaller than the distance between the other end and the corresponding rotating shaft 64, the bottom rotating plate 65 can rotate at a greater angle than the top rotating plate 65. When the bottom rotating plate 65 rotates to a vertical position, the connecting block 67 and the carrier 69 can be easily removed from the transfer box 62. At this point, the sample is placed on the carrier. After the sample is securely installed in the corresponding sample slot 611 on the rack 69 by the elastic sheet 612, the connecting block 67 is installed upwards from the bottom of the transfer box 62. At this time, the baffle 68 will first contact the open top rotating plate 65. Under the pushing action of the baffle 68, the top rotating plate 65 gradually returns to its original position and closes. At the same time, under the action of the linkage rod 66, the bottom rotating plate 65 also closes. Simultaneously, the rack 69 is attracted to the magnetic block 610, fixing the rack 69 and keeping the transfer box 62 in a closed state. The locking component can also be closed. Then, the sample feeding component sends the transfer box 62 from the sample feeding port into the machine body 1 at the position corresponding to the push rod 61. After being sent to the designated position, the push rod 61 moves down to attract the connecting block 67. It can continue to move down and press down. The moving connecting block 67 opens the transfer box 62, simultaneously driving the sealing component to close the sample delivery port. At this time, liquid nitrogen can be injected into the liquid nitrogen tank 5 by the liquid nitrogen pump 4, and then the vacuum pump 3 is turned on to evacuate the two chambers. When the transfer box 62 is closed, it has a heat preservation and sealing effect. The push rod 61 closes the sample delivery port and opens the transfer box 62 at the same time, adsorbing the connecting block 67, which in turn drives the carrier 69 to move. Then, after the liquid nitrogen enters the liquid nitrogen mud state, the electric push rod 21 opens the movable plate, and the push rod 61 continues to move down to insert the carrier 69 into the liquid nitrogen mud, so that the sample cools down. After cooling is complete, the push rod 61 can be lifted up. When the push rod 61 is lifted, it drives the connecting block 67 and the carrier 69 to rise. At this time, because the movable plate 22 is open during the cooling process, the entire body 1 is uniformly heated. In a low-temperature environment, the process of installing the connecting block 67 into the transfer box 62 can be repeated under the action of the push rod 61. After the rotating plate 65 closes, the transfer box 62 is fixed, and the push rod 61 can continue to move upward to separate from the connecting block 67. At this time, the transfer box 62 can be sent to the sample delivery port through the sample delivery component. The staff can directly transfer the transfer box 62 to the next preparation step. Since the body 1 is in a low-temperature vacuum environment when closed, the interior of the transfer box 62 is also in a low-temperature vacuum environment after it is closed. In addition, the body of the transfer box 62 has a certain heat preservation effect, which can maintain the sample in a low-temperature vacuum environment throughout the entire process from preparation to sample transfer, which is beneficial to protecting the sample properties. Moreover, the automatic sealing of the transfer box 62 reduces the manual sampling and transfer steps.This design makes the device convenient to use while reducing the safety risks associated with human contact with low-temperature environments.

[0099] like Figure 3 , Figure 9 , Figure 10 As shown, the locking assembly includes: two locking slots 11 symmetrically opened on two rotating plates 65 located at the top; two locking holes 111 symmetrically opened on the transfer box 62 and adapted to the locking slots 11; two locking tongues 112 slidably installed in the two locking slots 11 and made of magnetic metal; and two elastic bands 113 respectively fixedly installed in the two locking holes 111, with their other ends respectively fixedly connected to the corresponding locking tongues 112.

[0100] When the transfer box 62 is closed, the elastic band 113 can pull the locking tongue 112 to slide along the locking groove 11 and into the lock hole 111, thereby preventing the top rotating plate 65 from rotating along the rotating shaft 64, thus locking the top rotating plate 65. At the same time, since the top and bottom rotating plates 65 are connected by the linkage rod 66, locking the top rotating plate 65 can lock the bottom rotating plate 65 at the same time. When it is necessary to open the transfer box 62, by placing a magnet at the top center connecting block 67, the locking tongues 112 on both sides are attracted and pull the elastic band 113 to slide into the locking groove 11. At this time, the rotating plate 65 can rotate, thereby opening the transfer box 62. Locking the rotating plate 65 by locking the latch 112 enhances the pressure resistance of the transfer box 62 after sample preparation, ensuring the maintenance of vacuum conditions inside the box, protecting the sample while facilitating opening. By setting the latch 112 which can be attracted by magnets, the transfer box 62 can still be automatically opened inside the machine body 1 under the action of the strong magnet on the push rod 61. After sample preparation, when the push rod 61 leaves the connecting block 67, the latch 112 can automatically lock the transfer box 62 under the action of the elastic band 113, avoiding the need for manual operation. The transfer box 62 can be easily opened by magnets, making it convenient for staff to open the transfer box 62 and easy to adapt to other equipment.

[0101] like Figures 4 to 7As shown, the sealing assembly includes: two guide plates 7, fixedly installed on the inner wall of the body 1; two sliding plates 71, respectively slidably installed within the two guide plates 7; a door plate 72, located inside the body 1 at a position corresponding to the sample inlet, and the top of the door plate 72 is provided with an inclined surface sloping from the outside to the inside; several return springs 73, all fixedly installed between the sliding plates 71 and the door plate 72; a locking block 74, fixedly installed on the inclined surface at the top of the door plate 72; a sliding frame 75, slidably installed between the two guide plates 7; and a fixing arm 76, fixedly installed at the end of the sliding frame 75 away from the cylinder 6, and the other end of the fixing arm 76 is provided with a connection to the door. The door panel 72 has a beveled surface that is compatible with the plate; a slot 77 is formed on the beveled surface at the end of the fixed arm 76 and is compatible with the locking block 74; a drive assembly is set on the fixed arm 76; the drive assembly includes: a slide groove 8, formed on the end of the fixed arm 76 near the push rod 61; a drive rod 81, slidably installed in the slide groove 8, and the end of the drive rod 81 away from the slide groove 8 is fixedly connected to the push rod 61; a clearance groove 82, formed on the fixed arm 76; a limiting rod 83, rotatably installed at the center of the clearance groove 82, and a torsion spring is fixedly installed between the limiting rod 83 and the fixed arm 76; a sealing plate 78 is fixedly installed on the end of the door panel 72 away from the push rod 61;

[0102] After the sample delivery assembly delivers the transfer box 62 into the machine body 1, the push rod 61 descends. Before contacting the transfer box 62, it can drive the drive rod 81 to move within the slide groove 8. Initially, the limit rod 83 is in a horizontal position, and the drive rod 81 is located between the limit rod 83 and the top of the fixed arm 76. At this time, the push rod 61 drives the drive rod 81 to move downward, pressing the limit rod 83. The limit rod 83 will not rotate directly under the action of the torsion spring, thus causing the drive rod 81 to press the limit rod 83, thereby driving the fixed arm 76 to move downward along the guide plate 7. In the initial position, the return spring 73 pulls the door panel 72 towards the sliding plate 71, and the locking block 74 is engaged in the slot 77. The door panel 72 is located at the bottom of the fixed arm 76, and... As the fixed arm 76 moves downwards, the door panel 72 initially contacts the sample inlet. Initially, the door panel 72 cannot move downwards. However, under the action of the appropriate inclined plane, the door panel 72 is pushed outwards as the fixed arm 76 continues to move downwards. At this point, the locking block 74 separates from the locking groove 77, and the door panel 72 moves horizontally to block the sample inlet. When the fixed arm 76 also reaches the bottom and cannot move downwards, the push rod 61 drives the drive rod 81 to apply a large force to the limiting rod 83. The limiting rod 83 drives the torsion spring to rotate and enter the relief groove 82. At this point, the drive rod 81 can move downwards independently along the slide groove 8 via the limiting rod 83. After moving downwards, the push rod 61 can contact the transfer box 62 and thus move the sample. The limiting rod 83, through its action, allows the sample to be transferred downwards. This ensures that the push rod 61 closes the sample delivery port before contacting the transfer box 62, guaranteeing that the body 1 remains sealed during vacuuming and freezing, thus ensuring experimental safety and preventing safety issues caused by human error such as forgetting to close the sample delivery port or incomplete closure. The clearance groove 82 and slide 8 allow the push rod 61 to continue moving downwards unimpeded after closing, temporarily disengaging it from the sealing assembly and ensuring smooth subsequent freezing. The inclined surface pushes the door plate 72 outwards, ensuring a seal between the door plate 72 and the sample delivery port, guaranteeing complete sealing of the body 1 during freezing. When the sample preparation is complete and the push rod 61 moves upwards, the drive rod 81 first moves along the slide 8, and then... After the transport box 62 is separated, the drive rod 81 contacts the limit rod 83, causing the limit rod 83 and the fixed arm 76 to move upward. When the fixed arm 76 moves to the top of the door panel 72, under the action of the return spring 73, the door panel 72 moves inward through the relative inclined plane. At the same time, the locking block 74 and the locking groove 77 re-engage, so that the fixed arm 76 can drive the door panel 72 to move upward, opening the sample delivery port, so that the sample delivery assembly can send out the transport box 62. When the sliding frame 75 reaches the top of the machine body 1, the drive rod 81 squeezes the limit rod 83 again into the relief groove 82, and the drive rod 81 returns to the initial position between the limit rod 83 and the top of the fixed arm 76, so as to ensure that the sample delivery port can be automatically closed during the next sample delivery.

[0103] like Figure 2 , Figure 7 and Figure 8As shown, the sample delivery assembly includes: a fixed plate 9, fixedly installed on the inner top wall of the machine body 1; a first bevel gear 91, rotatably installed on the fixed plate 9; a second bevel gear 92, rotatably installed on the inner top wall of the machine body 1, and meshing with the first bevel gear 91; a worm gear 93, fixedly installed at the end of the second bevel gear 92 away from the machine body 1; a rack 94, slidably installed on the inner wall of the machine body 1, and meshing with the worm gear 93; a connecting rod 95, hinged to the bottom of the rack 94; a groove 97, formed on the first bevel gear 91; a fixed rod 98, fixedly installed on the push rod 61 and adapted to the groove 97; and a placement assembly. On the body 1, the placement components include: a sample feeding plate 10, fixedly installed on the body 1 at a position corresponding to the sample feeding port; a slide rail 101, fixedly installed on the sample feeding plate 10, and having a notch at a position corresponding to the sample feeding port; a limiting frame 102, fixedly installed on the sample feeding plate 10 and adapted to the transfer box 62; a storage tray 96, slidably installed on the slide rail 101, and hinged to the end of the connecting rod 95 away from the rack 94, with openings on the storage tray 96 and the sample feeding plate 10 adapted to the opening 63; and a limiting edge 99, fixedly installed on the storage tray 96 and adapted to the transfer box 62.

[0104] When the equipment is started and push rod 61 begins to move downwards, the sealing assembly is not yet activated. Push rod 61 first drives fixed rod 98 to move and engages in groove 97. As fixed rod 98 moves downwards, it drives bevel gear 1 91 to rotate, which in turn drives bevel gear 2 92 to rotate. When bevel gear 2 92 rotates, it drives worm gear 93 to rotate. When worm gear 93 rotates, it drives rack 94 to slide upwards along the side wall of machine body 1. Then, through connecting rod 95 hinged at the bottom, it pulls the sample tray 96 along the sample feeding plate 10 from the sample feeding port to the push rod 96. Directly below rod 61, the fixing rod 98 slides out of the groove 97. As the push rod 61 continues to move downward, it drives the sealing component to close the sample delivery port. At this time, the opening on the sample delivery plate 10 corresponds to the opening 63 on the transfer box 62. When the sample preparation is completed, the push rod 61 moves upward, first in conjunction with the sealing component to open the sample delivery port. Then, the fixing rod 98 moves to the point where it separates from the groove 97. The fixing rod 98 slides back into the groove 97, causing the bevel gear 91 to reverse, which in turn causes the rack 94 to move downward, pushing the placement tray 96 outward along the slide rail 101. The transfer box 62 moves to the sample delivery port, and the fixed rod 98 drives the bevel gear 91 to rotate. After the equipment is started, the transfer box 62 can be automatically moved to the working area when the sample delivery port is closed, and the transfer box 62 is automatically sent to the sample delivery port after the sample preparation is completed. The operator only needs to place the transfer box 62 on the storage tray 96 or remove the transfer box 62 from the storage tray 96 to complete the freezing sample preparation process, which greatly simplifies the manual operation steps, improves the linkage and automation of the system function, and can avoid the operator being frostbitten by the low temperature environment when reaching into the machine body 1 to take samples. The two ends of the transfer box 62 are fixed by the limiting edge 99, and can move with the storage tray 96 without shifting. After moving to the center position, the transfer box 62 can be locked by the limiting frame 102, so that the limiting frame 102 can ensure that the push rod 61 and the transfer box 62 can be smoothly separated, improving the stability of the system operation. This allows the system to automatically realize sample delivery, sampling, freezing, sealing and other tasks, which not only saves labor, but also better protects the frozen samples and protects the safety of the operators.

[0105] The method for preparing samples for liquid nitrogen mud freezing includes the following steps:

[0106] Step 1: Open the locking assembly and press the connecting block 67 downward from the center of the top of the transfer box 62. The connecting block 67 drives the carrier 69 to slide downward along the magnetic block 610. At the same time, the baffle 68 moves down with the connecting block 67. Take out the carrier 69 and place the sample in the corresponding sample slot 611 on the carrier 69. The elastic sheet 612 ensures that the sample is installed firmly. Install the transfer box 62 from the bottom upward. The carrier 69 is attracted to the magnetic block 610, thus keeping the transfer box 62 in a closed state. Place the transfer box 62 on the sample delivery port tray 96.

[0107] Step 2: Start the equipment. Push rod 61 begins to move downwards a certain distance, first driving fixed rod 98 to move and engage in groove 97. Then, through the sample feeding assembly, it drives the placement tray 96 to move along the sample feeding plate 10 from the sample feeding port to directly below push rod 61. Fixed rod 98 slides out of groove 97. Push rod 61 continues to move downwards, driving drive rod 81 to move fixed arm 76 downwards. Door panel 72 moves downwards with fixed arm 76 and is squeezed outwards after contacting sample feeding port. Door panel 72 moves horizontally and blocks sample feeding port. When fixed arm 76 also reaches the bottom, the system is closed.

[0108] Step 3: Push rod 61 can move downward along slide groove 8 independently via limit rod 83. At the same time, the end of push rod 61 can attract connecting block 67 and attract locking tongue 112, causing it to slide into locking groove 11, releasing rotating plate 65 and opening transfer box 62, driving the carrier 69 out of transfer box 62, starting liquid nitrogen pump 4 to inject liquid nitrogen, and starting vacuum pump 3. After liquid nitrogen enters liquid nitrogen mud state, the movable plate 22 is opened by electric push rod 21, and push rod 61 continues to move downward to insert carrier 69 into liquid nitrogen mud, so that the sample cools and completes freezing.

[0109] Step 4: After cooling is complete, lift the push rod 61 upwards to raise the carrier 69. Driven by the push rod 61, install the connecting block 67 into the transfer box 62. The transfer box 62 is fixed by the limit frame 102. The push rod 61 continues to move upwards and separates from the connecting block 67. The elastic band 113 pulls the locking tongue 112 to slide along the locking groove 11 and slide into the lock hole 111 to lock the top rotating plate 65. At the same time, the movable plate 22 is closed by the electric push rod 21.

[0110] Step 5: When it is necessary to remove the sample, move the push rod 61 upward, drive the rod 81 to move along the slide groove 8 and contact the limit rod 83, driving the fixed arm 76 to move upward. When the fixed arm 76 moves to the top of the door panel 72, the locking block 74 and the locking groove 77 are re-engaged under the action of the return spring 73, driving the door panel 72 to move upward synchronously, opening the sample delivery port. When the push rod 61 continues to move upward, the fixed rod 98 moves to the position where it separates from the groove 97, slides back into the groove 97, drives the bevel gear 91 to reverse, and then pushes the storage tray 96 to move outward along the slide rail 101 to the sample delivery port.

[0111] Those skilled in the art should understand that the discussion of any of the above embodiments is merely exemplary and is not intended to imply that the scope of the invention (including the claims) is limited to these examples; within the framework of the invention, the technical features of the above embodiments or different embodiments can also be combined, the steps can be implemented in any order, and there are many other variations of the different aspects of the invention as described above, which are not provided in the details for the sake of brevity.

[0112] This invention is intended to cover all such substitutions, modifications, and variations that fall within the broad scope of the appended claims. Therefore, any omissions, modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of this invention should be included within the scope of protection of this invention.

Claims

1. An apparatus for preparing liquid nitrogen mud frozen samples, characterized in that, include: The machine body (1) is provided with a sample delivery port; A partition plate (2) is fixedly installed inside the body (1) to separate the sample chamber and the liquid nitrogen chamber, and a connection port is provided on the partition plate (2); An electric push rod (21) is mounted on the body (1); The movable plate (22) is slidably installed on the partition plate (2) and adapted to the connection port. The movable plate (22) is fixedly connected to the movable end of the electric push rod (21). A vacuum pump (3) is installed on the body (1) and connected to the sample compartment and the liquid nitrogen compartment respectively; A liquid nitrogen pump (4) is mounted on the body (1); The liquid nitrogen tank (5) is fixedly installed on the bottom wall of the machine body (1) and connected to the liquid nitrogen pump (4); Cylinder (6) is fixedly installed on the top wall of the machine body (1); The push rod (61) is fixedly installed on the movable end of the cylinder (6) that passes through the body (1); A sample delivery assembly is disposed within the body (1); A transfer box (62) is disposed on the sample delivery assembly; Two openings (63) are symmetrically provided on the top and bottom outer walls of the transfer box (62); Four rotating shafts (64) are fixedly installed in the two openings (63) respectively, and the two rotating shafts (64) in one opening (63) are symmetrically arranged; Four rotating plates (65) are rotatably mounted on the rotating shaft (64); A shelf (69) is disposed inside the transfer box (62); Several sample slots (611) are provided on the shelf (69); Several elastic sheets (612) are fixedly installed at positions corresponding to the sample groove (611); The linkage component is located inside the transfer box (62); A closed assembly is disposed within the body (1); The linkage component includes: Two linkage rods (66) are respectively hinged between the two rotating plates (65) on both sides, and the distance between the end of the rod hinged to the rotating plate (65) at the bottom and the corresponding rotating shaft (64) is smaller than the distance between the other end and the corresponding rotating shaft (64); A connecting block (67) is disposed inside the transfer box (62); The baffle (68) is fixedly fitted on the connecting block (67), and when the transfer box (62) is in the closed state, the upper surface of the baffle (68) is in contact with the lower surface of the two rotating plates (65) located at the top; Two magnetic blocks (610) are symmetrically fixedly installed inside the transfer box (62) and located at positions corresponding to the shelf (69); A locking assembly is provided inside the transfer box (62); The top wall of the rack (69) is fixedly connected to the bottom wall of the connecting block (67). Both the connecting block (67) and the rack (69) are made of magnetic metal. A strong magnet is fixedly installed at the end of the push rod (61) away from the cylinder (6). The two rotating plates (65) at the top of the transfer box (62) are provided with slots that are compatible with the connecting block (67). When the transfer box (62) is in the closed state, the top surface of the connecting block (67) is coplanar with the upper surface of the rotating plate (65). The locking component includes: Two locking slots (11) are symmetrically opened on the two rotating plates (65) located at the top; Two lock holes (111) are symmetrically opened on the transfer box (62) and are adapted to the lock groove (11); Two latches (112) are slidably mounted in the two said latches (11) and are made of magnetic metal; Two elastic bands (113) are fixedly installed in the two lock holes (111) respectively, and the other end is fixedly connected to the corresponding lock tongue (112); The enclosed component includes: Two guide plates (7) are fixedly installed on the inner side wall of the body (1); Two sliding plates (71) are respectively slidably installed in the two guide plates (7); The door panel (72) is located inside the body (1) at a position corresponding to the sample delivery port, and the top of the door panel (72) is provided with an inclined surface that slopes from the outside to the inside; Several return springs (73) are fixedly installed between the sliding plate (71) and the door panel (72); The locking block (74) is fixedly installed on the top slope of the door panel (72); A sliding frame (75) is slidably mounted between the two guide plates (7); A fixed arm (76) is fixedly installed on one end of the sliding frame (75) away from the cylinder (6), and the other end of the fixed arm (76) is provided with an inclined surface that is compatible with the door panel (72); A slot (77) is formed on the inclined surface at the end of the fixed arm (76) and is adapted to the card block (74); A drive assembly is disposed on the fixed arm (76); The driving component includes: A groove (8) is formed at one end of the fixed arm (76) near the push rod (61); The drive rod (81) is slidably installed in the slide groove (8), and the end of the drive rod (81) away from the slide groove (8) is fixedly connected to the push rod (61); A clearance groove (82) is provided on the fixed arm (76); A limiting rod (83) is rotatably installed at the center of the relief groove (82), and a torsion spring is fixedly installed between the limiting rod (83) and the fixed arm (76); The sample delivery component includes: A fixing plate (9) is fixedly installed on the inner top wall of the body (1); A bevel gear (91) is rotatably mounted on the fixed plate (9); The second bevel gear (92) is rotatably mounted on the inner top wall of the body (1) and meshes with the first bevel gear (91); The worm gear (93) is fixedly installed at the end of the bevel gear (92) away from the body (1); The rack (94) is slidably mounted on the inner side wall of the machine body (1) and meshes with the worm (93); The connecting rod (95) is hinged to the bottom of the rack (94); A groove (97) is formed on the first bevel gear (91); A fixing rod (98) is fixedly installed on the push rod (61) and is adapted to the groove (97); The placement components are mounted on the body (1); The placement component includes: Sample plate (10) is fixedly installed on the machine body (1) at a position corresponding to the sample inlet; The slide rail (101) is fixedly installed on the sample feeding plate (10), and a notch is provided at the position corresponding to the sample feeding port; The limiting frame (102) is fixedly installed on the sample delivery plate (10) and is adapted to the transfer box (62); The storage tray (96) is slidably mounted on the slide rail (101) and hinged to the end of the connecting rod (95) away from the rack (94). The storage tray (96) and the sample plate (10) are provided with openings that are compatible with the opening (63). The limiting edge (99) is fixedly installed on the storage tray (96) and adapted to the transfer box (62).

2. The apparatus for preparing a liquid nitrogen mud frozen sample according to claim 1, characterized in that, A sealing plate (78) is fixedly installed at the end of the door panel (72) away from the push rod (61).

3. The apparatus for preparing a liquid nitrogen mud frozen sample according to claim 1, characterized in that, A step (12) is provided at the position corresponding to the rotating plate (65) of the transfer box (62), and a sealing part (121) is fixedly installed at one end of the rotating plate (65) near the step (12).

4. A method for preparing frozen samples of liquid nitrogen mud, based on the apparatus for preparing frozen samples of liquid nitrogen mud according to any one of claims 1-3, characterized in that, Includes the following steps: Step 1: Open the locking assembly and press the connecting block (67) down from the center of the top of the transfer box (62). The connecting block (67) will drive the carrier (69) to slide down along the magnetic block (610). At the same time, the baffle (68) will move down with the connecting block (67). Take out the carrier (69) and place the sample in the corresponding sample slot (611) on the carrier (69). Ensure that the sample is installed firmly by the elastic sheet (612). Install from the bottom of the transfer box (62) upward. The carrier (69) will be attracted to the magnetic block (610), thereby keeping the transfer box (62) closed. Place the transfer box (62) on the sample delivery port tray (96). Step 2: Start the equipment. The push rod (61) starts to move downward a distance. First, it drives the fixed rod (98) to move and engage in the groove (97). Then, through the sample feeding assembly, it drives the placement tray (96) to move along the sample feeding plate (10) from the sample feeding port to directly below the push rod (61). The fixed rod (98) slides out of the groove (97). The push rod (61) continues to move downward, driving the drive rod (81) to move the fixed arm (76) downward. The door panel (72) moves downward with the fixed arm (76) and is squeezed outward after contacting the sample feeding port. The door panel (72) moves horizontally and blocks the sample feeding port. When the fixed arm (76) also reaches the bottom, the system is closed. Step 3: The push rod (61) can move downward along the slide groove (8) by the limiting rod (83). At the same time, the end of the push rod 61 can attract the connecting block (67) and attract the locking tongue (112) to slide into the locking groove (11). Release the rotating plate (65) and open the transfer box (62). Move the carrier (69) out of the transfer box (62). Start the liquid nitrogen pump (4) to inject liquid nitrogen and start the vacuum pump (3). After the liquid nitrogen enters the liquid nitrogen mud state, open the movable plate (22) by the electric push rod (21). Continue to move the push rod (61) down to insert the carrier (69) into the liquid nitrogen mud so that the sample is cooled and frozen. Step 4: After cooling is complete, lift the push rod (61) upwards to raise the rack (69). Driven by the push rod (61), install the connecting block (67) into the transfer box (62). The transfer box (62) is fixed by the limit frame (102). The push rod (61) continues to move upwards and separates from the connecting block (67). The elastic band (113) pulls the locking tongue (112) to slide along the lock groove (11) and slide into the lock hole (111) to lock the top rotating plate (65). At the same time, the movable plate (22) is closed by the electric push rod (21). Step 5: When it is necessary to remove the sample, move the push rod (61) upward, drive the rod (81) to move along the slide groove (8) and contact the limit rod (83), drive the fixed arm (76) to move upward, when the fixed arm (76) moves to the top of the door panel (72), under the action of the return spring (73), the locking block (74) and the locking groove (77) are re-engaged, driving the door panel (72) to move upward synchronously, opening the sample delivery port, when the push rod (61) continues to move upward, the fixed rod (98) moves to the point where it separates from the groove (97), slides back into the groove (97) and drives the bevel gear (91) to reverse, thereby pushing the storage tray (96) to move outward along the slide rail (101) to the sample delivery port.

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