Device and method for preparing liquid nitrogen mud frozen sample

Abstract

The invention relates to the technical field of frozen sample preparation, in particular to a liquid nitrogen mud frozen sample preparation device and method.The device 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 an air cylinder; the push rod is fixedly mounted on the air cylinder; a sample feeding assembly; the transfer box is arranged on the sample feeding assembly; the two openings are symmetrically formed in the outer walls of the top and the bottom of the transfer box; the four rotating shafts are fixedly mounted in the two openings respectively, and the two rotating shafts in one opening are symmetrically arranged; the four rotating plates are rotationally arranged on the rotating shaft in a sleeving manner; a linkage assembly; and a closing assembly. Compared with the prior art, the transfer box is arranged, the internal low-temperature vacuum environment can be maintained when the transfer box is closed, the environment is crucial for samples needing to be stored at low temperature, the state of the samples can be effectively protected, it is ensured that the samples are not affected by the external environment in the transfer and cooling process, and the accuracy of observation results is ensured.

Description

Technical Field

[0001] The present invention relates to the technical field of frozen sample preparation, and in particular to a device and method for preparing a liquid nitrogen mud frozen sample. Background Art

[0002] Liquid nitrogen mud freezing is a freezing method that uses liquid nitrogen to turn into liquid nitrogen mud under vacuum to quickly lower the sample temperature, thereby preventing ice crystals from forming and maintaining the sample's microstructure. This method ensures that the sample is not damaged during the freezing process and is suitable for analyzing the microstructure and composition of samples in fields such as scanning electron microscopy.

[0003] After searching, a Chinese patent with publication number CN107991330A discloses a device for preparing liquid nitrogen mud frozen samples, including a sampling device, a liquid nitrogen mud cooling device, and a vacuum pump connected to the sampling device and the liquid nitrogen mud cooling device respectively; the sampling device is used to fix the sample and send the sample into the liquid nitrogen mud cooling device; the vacuum pump is used to put the sampling device and the liquid nitrogen mud cooling device into a vacuum state, and the liquid nitrogen under vacuum 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 liquid nitrogen mud frozen sample; the frozen sample prepared by the device can prevent the formation of ice crystals without destroying the microstructure.

[0004] After the preparation of the frozen sample cooled by liquid nitrogen is completed, it is necessary to always maintain a vacuum and low temperature state, because during the scanning electron microscope observation process, the sample needs to be in a low temperature and dry state 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 melting of ice crystals, sublimation or contamination of the sample, thereby affecting the observation results. However, after the preparation of the above-mentioned device is completed, it is necessary to manually open the sampling device directly to take out the sample from it. This requires the operator to quickly perform a series of operations to place the sample in the transfer device. Not only is the protection of the sample insufficient, but it may also cause safety hazards due to anxious operation. When the sample preparation is completed and the sample is stored, the sampling device is in a low temperature state. At this time, the operator needs to reach into the sampling device to take the sample. The small space is not convenient for operation, and the risk of frostbite to the operator due to low temperature is increased.

[0005] Therefore, the present application provides a liquid nitrogen mud frozen sample preparation device and method to meet the requirements of maintaining the low temperature vacuum environment of the sample after sample preparation is completed while facilitating operation. Summary of the invention

[0006] In view of this, the purpose of the present invention is to provide a liquid nitrogen mud frozen sample preparation device and method to solve the problem of inconvenience in sampling, transfer and storage after sample preparation.

[0007] Based on the above purpose, the present invention provides a device and method for preparing a liquid nitrogen mud frozen sample, comprising:

[0008] A machine body, wherein a sample delivery port is provided on the machine body;

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

[0010] An electric push rod, arranged on the machine body;

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

[0012] A vacuum pump is disposed on the machine body and connected to the upper and lower chambers of the machine body respectively;

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

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

[0015] A cylinder, fixedly mounted on the top wall of the machine body;

[0016] A push rod, fixedly mounted on the movable end of the cylinder passing through the body;

[0017] A sample delivery component is disposed in the body;

[0018] A transport box, arranged on the sample delivery component;

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

[0020] Four rotating shafts are fixedly installed in the two openings respectively, and the two rotating shafts in one opening are symmetrically arranged;

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

[0022] A carrier, arranged in the transfer box;

[0023] A plurality of sample slots are provided on the carrier;

[0024] A plurality of elastic sheets are fixedly installed at positions corresponding to the sample slots;

[0025] A linkage component is arranged in the transfer box;

[0026] The sealing component is arranged in the body.

[0027] Preferably, the linkage component comprises:

[0028] Two linkage rods are respectively hinged between the two rotating plates on both sides, and the distance between one end hinged to the rotating plate arranged at the bottom and the corresponding rotating shaft is smaller than the distance between the other end and the corresponding rotating shaft;

[0029] A connecting block is arranged in the transfer box;

[0030] A baffle, fixedly sleeved on the connecting block, and the upper surface of the baffle is in contact with the lower surfaces of the two rotating plates located at the top when the transfer box is in a closed state;

[0031] Two magnetic blocks are symmetrically fixedly installed in the transfer box and located at positions corresponding to the carrier;

[0032] A locking assembly is arranged in the transfer box;

[0033] Among them, the top wall of the carrier is fixedly connected to the bottom wall of the connecting block, the connecting block and the carrier are both made of magnetic metal, a strong magnet is fixedly installed on the end of the push rod away from the cylinder, and the two rotating plates located on the top of the transfer box are provided with grooves adapted to the connecting block. When the transfer box is in a closed state, the top surface of the connecting block is coplanar with the upper surface of the rotating plate.

[0034] Preferably, the locking assembly comprises:

[0035] Two locking grooves are symmetrically arranged on the two rotating plates at the top;

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

[0037] Two locking tongues are slidably mounted in the two locking grooves and are made of magnetic metal;

[0038] The two elastic bands are respectively fixedly installed in the two lock holes, and the other ends are respectively fixedly connected to the corresponding lock tongues.

[0039] Preferably, the closure assembly comprises:

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

[0041] Two sliding plates are slidably mounted in the two guide plates respectively;

[0042] A door panel is arranged at a position in the body corresponding to the sample delivery port, and a top of the door panel is provided with an inclined surface inclined from outside to inside;

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

[0044] A clamping block, fixedly mounted on the top inclined surface of the door panel;

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

[0046] A fixed arm is fixedly mounted on 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 card slot is provided on the inclined surface of the end of the fixed arm and is adapted to the card block;

[0048] The driving assembly is arranged on the fixed arm.

[0049] Preferably, the drive assembly comprises:

[0050] A slide groove is provided at one end of the fixed arm close to the push rod;

[0051] A driving rod is slidably mounted in the slide slot, and one end of the driving rod away from the slide slot is fixedly connected to the push rod;

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

[0053] The limiting rod is rotatably mounted at the center of the giving way slot, and a torsion spring is fixedly mounted between the limiting rod and the fixed arm.

[0054] Preferably, the sample delivery component comprises:

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

[0056] Bevel gear 1, rotatably mounted on the fixed plate;

[0057] Bevel gear 2 is rotatably mounted on the inner top wall of the body and meshes with bevel gear 1;

[0058] A worm, fixedly mounted on the end of the second bevel gear away from the machine body;

[0059] A rack, slidably mounted on the inner wall of the body and meshing with the worm;

[0060] A connecting rod, hinged to the bottom of the rack;

[0061] A groove is provided on the bevel gear one;

[0062] A fixing rod, fixedly mounted on the push rod and adapted to the groove;

[0063] A placement component is arranged on the machine body.

[0064] Preferably, the placement component comprises:

[0065] A sample delivery plate, fixedly mounted on the machine body at a position corresponding to the sample delivery port;

[0066] A slide rail is fixedly mounted on the sample delivery plate and is provided with a notch at a position corresponding to the sample delivery port;

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

[0068] A storage support plate is slidably mounted on the slide rail and is hinged to an end of the connecting rod away from the rack. The storage support plate and the sample delivery plate are provided with openings that match the openings.

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

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

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

[0072] The method for preparing a sample frozen with liquid nitrogen mud comprises the following steps:

[0073] Step 1: Open the locking assembly, press the connecting block downward from the center of the top of the transport box, the connecting block drives the carrier to slide downward along the magnetic block, and the baffle moves downward with the connecting block, take out the carrier, place the sample in the corresponding sample slot on the carrier, ensure that the sample is firmly installed through the elastic sheet, install it from the bottom of the transport box upward, the carrier is adsorbed by the magnetic block, and the transport box is kept in a closed state, and the transport box is placed on the sample delivery port disposal tray;

[0074] Step 2: Start the equipment, the push rod starts to move downward for a distance, first driving the fixed rod to move and snap into the groove, and then the sample feeding assembly drives the storage tray to move along the sample feeding plate from the sample feeding port to just below the push rod, the fixed rod slides out of the groove, the push rod continues to move downward, driving the drive rod to move the fixed arm downward, the door panel moves downward with the fixed arm, and is squeezed outward after contacting the sample feeding port, the door panel moves horizontally and blocks the sample feeding port, and when the fixed arm also reaches the bottom, the system is closed;

[0075] Step 3: The push rod can be moved downward along the slide groove alone through the limit rod. At the same time, the end of the push rod can absorb the connection block and attract the lock tongue to slide into the lock groove, release the rotating plate to open the transport box, drive the carrier to move out of the transport box, start the liquid nitrogen pump to inject liquid nitrogen, and start the vacuum pump. After the liquid nitrogen enters the liquid nitrogen mud state, open the movable plate through the electric push rod, continue to move the push rod downward to insert the carrier into the liquid nitrogen mud, so that the sample is cooled and frozen;

[0076] Step 4: After cooling, lift the push rod upward to drive the carrier to rise. Driven by the push rod, install the connecting block into the transfer box. The transfer box is fixed by the limit frame. The push rod continues to move upward to separate from the connecting block. The elastic belt pulls the lock tongue to slide along the lock groove and slide into the lock hole to lock the top rotating plate. At the same time, the movable plate is closed by the electric push rod;

[0077] Step 5: When the sample needs to be taken out, move the push rod upward, the driving 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 card block is re-engaged with the card groove under the action of the reset spring, driving the door panel to move up synchronously, opening the sample delivery port, and when the push rod continues to move upward, the fixed rod moves to the point where it is separated from the groove, slides back into the groove, driving the bevel gear to reverse, and then pushes the storage tray to move outward along the slide rail to the sample delivery port.

[0078] Beneficial effects of the present invention:

[0079] 1. This liquid nitrogen mud frozen sample preparation device and method, by providing a transport box, can maintain an internal low-temperature vacuum environment when closed. This environment is crucial for samples that need to be stored at low temperatures. It can effectively protect the state of the sample, ensure that the sample is not affected by the external environment during transportation and cooling, and ensure the accuracy of the observation results.

[0080] 2. This liquid nitrogen mud frozen sample preparation device and method realizes the automatic closing and opening of the sample delivery port by setting a push rod to drive the movement of a series of components such as a driving rod, a limit rod and a fixed arm. Before the push rod contacts the transfer box, the door panel is automatically pushed to the sample delivery port and sealed, thereby ensuring the airtightness of the body during the vacuuming and freezing process, improving work efficiency, and effectively avoiding safety problems caused by manual operation errors.

[0081] 3. This liquid nitrogen mud frozen sample preparation device and method realizes the automatic transportation, positioning and removal of the sample transport box by setting bevel gears, worm gears, racks, connecting rods, etc., making the entire freezing sample preparation process more intelligent and automated, avoiding the need for operators to manually reach into the body to take samples 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. BRIEF DESCRIPTION OF THE DRAWINGS

[0082] In order to more clearly illustrate the technical solutions in the present invention or the prior art, the drawings required for use in the embodiments or the description of the prior art will be briefly introduced below. Obviously, the drawings in the following description are only for the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying creative work.

[0083] Figure 1 It is a schematic diagram of the three-dimensional structure of the present invention;

[0084] Figure 2 It is a schematic diagram of the cutaway structure of the present invention;

[0085] Figure 3 It is a structural schematic diagram of the transport box of the present invention in an open state;

[0086] Figure 4 It is a schematic diagram of the structure of the closure assembly of the present invention;

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

[0088] Figure 6 For the present invention Figure 2 A schematic diagram of the enlarged structure at A in the middle;

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

[0090] Figure 8 It is a schematic diagram of the structure of the components placed in the present invention;

[0091] Fig. 9 It is a structural schematic diagram of the closed state of the transfer box of the present invention;

[0092] Fig.10 For the present invention Figure 3 Schematic diagram of the enlarged structure at point B in the middle.

[0093] The markings in the figure are:

[0094] 1. Machine body; 2. Partition 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 slot; 612. Elastic sheet; 7. Guide plate; 71. Sliding plate; 72. Door plate; 73. Reset spring; 74. Block; 75. Sliding rack; 76. Fixed arm; 77, slot; 78, sealing plate; 8, slide groove; 81, drive rod; 82, give way groove; 83, limit rod; 9, fixed plate; 91, bevel gear one; 92, bevel gear two; 93, worm; 94, rack; 95, connecting rod; 96, storage tray; 97, groove; 98, fixed rod; 99, limit edge; 10, sample delivery plate; 101, slide rail; 102, limit frame; 11, lock groove; 111, lock hole; 112, lock tongue; 113, elastic band; 12, step; 121, sealing part. DETAILED DESCRIPTION

[0095] In order to make the objectives, technical solutions and advantages of the present invention more clearly understood, the present invention is further described in detail below in conjunction with specific embodiments.

[0096] It should be noted that, unless otherwise defined, the technical terms or scientific terms used in the present invention should be understood by people with ordinary skills in the field to which the present invention belongs. The "first", "second" and similar words used in the present invention do not indicate any order, quantity or importance, but are only used to distinguish different components. "Include" or "comprise" and similar words mean that the elements or objects appearing before the word include the elements or objects listed after the word and their equivalents, without excluding other elements or objects. "Connect" or "connected" and similar words are not limited to physical or mechanical connections, but may include electrical connections, whether direct or indirect. "Up", "down", "left", "right" and the like are only used 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 preparation device and method of liquid nitrogen mud frozen sample include a body 1, which is provided with a sample delivery port; a partition plate 2, which is fixedly installed in the body 1 and is used to separate the sample chamber and the liquid nitrogen chamber, and the partition plate 2 is provided with a connection port; an electric push rod 21, which is arranged on the body 1; a movable plate 22, which is slidably installed on the partition plate 2 and adapted to the connection port, and the movable plate 22 is fixedly connected to the movable end of the electric push rod 21; a vacuum pump 3, which is arranged on the body 1 and is respectively connected to the upper and lower chambers of the body 1; a liquid nitrogen pump 4, which is arranged on the body 1; a liquid nitrogen tank 5, which is fixedly installed on the inner bottom wall of the body 1 and is connected to the liquid nitrogen pump 4; a cylinder 6, which is fixedly installed Installed on the top wall of the body 1; the push rod 61 is fixedly installed on the movable end of the cylinder 6 passing through the body 1; the sample delivery component is arranged in the body 1; the transfer box 62 is arranged on the sample delivery component; two openings 63 are symmetrically opened on the top and bottom outer walls of the transfer box 62; four rotating shafts 64 are respectively fixedly installed in the two openings 63, and the two rotating shafts 64 in one opening 63 are symmetrically arranged; four rotating plates 65 are rotatably mounted on the rotating shafts 64; the carrier 69 is arranged in the transfer box 62; a plurality of sample slots 611 are opened on the carrier 69; a plurality of elastic sheets 612 are fixedly installed at positions corresponding to the sample slots 611 The linkage assembly is arranged in the transfer box 62; the closing assembly is arranged in the body 1; the linkage assembly includes: two linkage rods 66, which are respectively hinged between the two rotating plates 65 on both sides, and the distance between one end hinged to the rotating plate 65 arranged at the bottom and the corresponding rotating shaft 64 is smaller than the distance between the other end and the corresponding rotating shaft 64; the connecting block 67 is arranged in the transfer box 62; the baffle 68 is fixedly mounted 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 at the top; two magnetic blocks 610 are symmetrically fixedly installed in the transfer box 62 and located The position corresponding to the carrier 69; the locking assembly is arranged in the transport box 62; wherein the top wall of the carrier 69 is fixedly connected to the bottom wall of the connecting block 67, the connecting block 67 and the carrier 69 are both made of magnetic metal, a strong magnet is fixedly installed on the end of the push rod 61 away from the cylinder 6, and notches adapted to the connecting block 67 are provided on the two rotating plates 65 located at the top of the transport box 62, and the top surface of the connecting block 67 is coplanar with the upper surface of the rotating plate 65 when the transport box 62 is in the closed state; a step 12 is provided at the position corresponding to the rotating plate 65 of the transport box 62, and a sealing portion 121 is fixedly installed on the end of the rotating plate 65 close to the step 12;

[0098] When in use, open the locking assembly, press the connecting block 67 downward from the top center of the transport box 62, and the connecting block 67 drives the sample rack 69 to slide downward along the magnetic block 610, and the sample rack 69 gradually breaks away from the attraction of the magnetic block 610, and at the same time, the baffle 68 moves downward with the connecting block 67, and the rotating plate 65 breaks away from the abutment with the baffle 68 and can rotate downward under the action of gravity. At the same time, since the distance between the hinged end of the rotating plate 65 at the bottom of the linkage rod 66 and the corresponding rotating shaft 64 is smaller than the distance between the other end and the corresponding rotating shaft 64, the rotation angle of the bottom rotating plate 65 can be greater than that of the top rotating plate 65. When the bottom rotating plate 65 is rotated to a vertical state, the connecting block 67 and the sample rack 69 can easily take out the transport box 62, and at this time, the sample is placed on the carrier. After ensuring that the sample is firmly installed in the sample slot 611 on the rack 69 through the elastic sheet 612, the connecting block 67 is installed upward from the bottom of the transport box 62. At this time, the baffle 68 will first contact the opened top rotating plate 65. Under the push 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 is also closed. At the same time, the carrier 69 is adsorbed by the magnetic block 610, so that the carrier 69 is fixed, so that the transport box 62 can be kept in a closed state. At the same time, the locking assembly can be closed, and then the transport box 62 is sent from the sample delivery port into the body 1 to the position corresponding to the push rod 61 through the sample delivery assembly. After it is sent to the specified position, the push rod 61 moves downward to adsorb the connecting block 67, and can continue to move downward to press down. The connecting block 67 is moved to open the transfer box 62, and at the same time, the sealing component is driven to close the sample delivery port. At this time, liquid nitrogen can be injected into the liquid nitrogen tank 5 through 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 the effect of heat preservation and sealing. The transfer box 62 is opened while the sample delivery port is closed by the push rod 61, and the connecting block 67 is adsorbed to drive the carrier 69 to move. After the liquid nitrogen enters the liquid nitrogen mud state, the movable plate is opened by the electric push rod 21, and the push rod 61 is continuously moved downward to insert the carrier 69 into the liquid nitrogen mud to cool the sample. After cooling, the push rod 61 can be lifted upward. When the push rod 61 is lifted, the connecting block 67 and the carrier 69 are driven to rise. At this time, since the movable plate 22 is opened during the cooling process, the whole body 1 is The transfer box 62 is in a low-temperature environment. At this time, the process of installing the connecting block 67 into the transfer box 62 can be repeated under the drive of the push rod 61. After the rotating plate 65 is closed, since the transfer box 62 is fixed, the push rod 61 continues 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 preparation of the next process. 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, and the box body of the transfer box 62 has a certain heat preservation effect, which can maintain the sample in a low-temperature vacuum environment during the entire process from preparation to transfer of the sample, which is beneficial to protecting the properties of the sample, and the transfer box 62 is automatically closed, which reduces the manual sampling and transfer processes.It is convenient to use and reduces the potential safety hazard of human body contact with low temperature environment.

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

[0100] When the transfer box 62 is closed, the elastic band 113 can pull the locking tongue 112 to slide along the lock groove 11 and slide into the lock hole 111, so that the top rotating plate 65 cannot rotate along the rotating shaft 64, so that the top rotating plate 65 is locked. At the same time, since the top and bottom rotating plates 65 are connected by the linkage rod 66, the bottom rotating plate 65 can be locked while locking the top rotating plate 65. When the transfer box 62 needs to be opened, the magnet is placed at the top center connecting block 67, and the locking tongues 112 on both sides are attracted to pull the elastic band 113 to slide into the lock groove 11. At this time, the rotating plate 65 can be rotated, and the transfer box 62 can be opened. The rotating plate 65 is locked by the locking tongue 112, thereby enhancing the ability of the transfer box 62 to withstand air pressure after sample preparation is completed, which can ensure that the vacuum condition in the box is maintained, protecting the sample while facilitating opening. By setting a locking tongue 112 that can be attracted by magnets, the transfer box 62 can still be automatically opened in the machine body 1 under the action of the strong magnet on the push rod 61, and when the push rod 61 leaves the connecting block 67 after sample preparation is completed, the locking tongue 112 can automatically lock the transfer box 62 under the action of the elastic band 113, avoiding the need for manual operation, and the transfer box 62 can be easily opened by a magnet, which is convenient for staff to open the transfer box 62 and can be conveniently adapted to other equipment.

[0101] like Figures 4 to 7As shown, the closing assembly includes: two guide plates 7, fixedly mounted on the inner side wall of the body 1; two sliding plates 71, slidably mounted in the two guide plates 7 respectively; a door plate 72, arranged at a position corresponding to the sample delivery port in the body 1, and a slope inclined from the outside to the inside is arranged on the top of the door plate 72; a plurality of return springs 73, all fixedly mounted between the sliding plate 71 and the door plate 72; a block 74, fixedly mounted on the top slope of the door plate 72; a sliding frame 75, slidably mounted between the two guide plates 7; a fixed arm 76, fixedly mounted 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 a The inclined surface of the plate 72 is matched; the card slot 77 is provided on the inclined surface of the end of the fixed arm 76 and is matched with the card block 74; the driving assembly is arranged on the fixed arm 76; the driving assembly includes: a slide slot 8, which is provided at one end of the fixed arm 76 close to the push rod 61; a driving rod 81 is slidably installed in the slide slot 8, and the end of the driving rod 81 away from the slide slot 8 is fixedly connected to the push rod 61; a clearance slot 82 is provided on the fixed arm 76; a limiting rod 83 is rotatably installed at the center of the clearance slot 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 at one end of the door panel 72 away from the push rod 61;

[0102] When the sample delivery assembly delivers the transport box 62 to the body 1, the push rod 61 descends, and when it does not contact the transport box 62, it can drive the driving rod 81 to move in the slide groove 8. Initially, the limit rod 83 is in a horizontal position, and the driving 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 driving 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, so that the driving rod 81 squeezes the limit rod 83 and then drives the fixed arm 76 to move downward along the guide plate 7. At the starting position, the return spring 73 pulls the door plate 72 in the direction of the sliding plate 71, and the block 74 is engaged in the slot 77. The door plate 72 is located at the bottom of the fixed arm 76, and When the locking cam 74 is in the state of being moved downward, the locking cam 74 is in the state of being moved downward, and the locking cam 74 is in the state of being moved downward, so that the locking cam 74 is in the state of being moved downward, and the locking cam 74 is in the state of being moved downward, so that the locking cam 74 is in the state of being moved downward, and the locking cam 74 is in the state of being moved downward, and the locking cam 74 is in the state of being moved downward, and the locking cam 74 is in the state of being moved downward, and the locking cam 74 is in the state of being moved downward, and the locking cam 74 is in the state of being moved downward, and the locking cam 74 is in the state of being moved downward, and the locking cam 74 is in the state of being moved downward, and the locking cam 74 is in the state of being moved downward, and the locking cam 74 is in the state of being moved downward, and the locking cam The push rod 61 closes the sample delivery port before contacting the transfer box 62, thereby ensuring that the body 1 is in a sealed state during vacuuming and freezing, ensuring the safety of the experiment, and avoiding safety problems caused by forgetting to close the sample delivery port or incomplete closing due to manual operation errors. Through the yield groove 82 and the slide groove 8, the push rod 61 can still move downward without hindrance after the closing is completed, so that the push rod 61 is temporarily separated from the sealing component to ensure the smooth progress of the subsequent freezing process. The door panel 72 is pushed outward by the inclined surface to ensure the sealing effect between the door panel 72 and the sample delivery port, ensuring that the body 1 is completely closed during freezing. When the push rod 61 moves upward after the sample preparation is completed, the driving rod 81 first moves along the slide groove 8, and then moves with the transfer box 62 to close the sample delivery port. After the transport box 62 is separated, the driving rod 81 contacts the limit rod 83 to drive 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 reset spring 73, the door panel 72 moves inward through the relative inclined surfaces, and at the same time, the clamping block 74 is re-engaged with the clamping slot 77, so that the fixed arm 76 can drive the door panel 72 to move upward, open the sample delivery port, and allow the sample delivery assembly to deliver the transport box 62. When the sliding frame 75 arrives at the top of the body 1, the driving rod 81 squeezes the limit rod 83 again to enter the yield slot 82, and the driving rod 81 returns to the initial position between the limit rod 83 and the top of the fixed arm 76, thereby ensuring that the sample delivery port can be automatically closed when the sample is delivered next time.

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

[0104] When the device is started and the push rod 61 starts to move downward, the closing assembly has not yet taken effect. The push rod 61 first drives the fixing rod 98 to move. The fixing rod 98 is engaged in the groove 97. When the fixing rod 98 moves downward, it drives the bevel gear 1 91 to rotate, and then drives the bevel gear 2 92 to rotate. When the bevel gear 2 92 rotates, it can drive the worm 93 to rotate. When the worm 93 rotates, it can drive the rack 94 to slide upward along the side wall of the body 1, and then pull the storage tray 96 along the sample delivery plate 10 from the sample delivery port to the push rod 96 through the bottom hinged connecting rod 95. The push rod 61 is directly below the rod 61, and then the fixed rod 98 slides out of the groove 97. When the push rod 61 continues to move downward, it drives the sealing component to close the sample delivery port. At this time, the through hole 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 up, firstly linked with the sealing component to open the sample delivery port, and then the fixed rod 98 moves to the separation from the groove 97. The fixed rod 98 slides into the groove 97 again to drive the bevel gear 91 to reverse, and then drives the rack 94 to move downward, pushing the storage tray 96 to move outward along the slide rail 101. The transfer box 62 is moved to the sample delivery port, and the bevel gear 91 is driven to rotate by the fixing rod 98. 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 can be 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 process of frozen sample preparation, which greatly simplifies the steps of manual operation, improves the linkage and automation of the system function work, and can avoid the situation where the operator is frostbitten by the low temperature environment when reaching into the body 1 to take samples. The two ends of the transfer box 62 are fixed by the limiting edges 99 and can move with the storage tray 96 without deviation. After moving to the center position, the transfer box 62 can be clamped by the limiting frame 102, so that the limiting frame 102 can ensure that the push rod 61 and the transfer box 62 are separated smoothly, improve the stability of the system operation, and enable the system to automatically realize sample delivery, sampling, freezing, sealing and other tasks, which not only saves labor, but also can better protect the frozen samples, and also can protect the safety of the operators.

[0105] The method for preparing a sample frozen with liquid nitrogen mud comprises the following steps:

[0106] Step 1: Open the locking assembly, press the connecting block 67 downward from the top center of the transport box 62, the connecting block 67 drives the sample rack 69 to slide downward along the magnetic block 610, and the baffle 68 moves downward with the connecting block 67, take out the sample rack 69, place the sample in the corresponding sample slot 611 on the sample rack 69, ensure that the sample is firmly installed by the elastic sheet 612, install it upward from the bottom of the transport box 62, the sample rack 69 is adsorbed by the magnetic block 610, and the transport box 62 is kept in a closed state, and the transport box 62 is placed on the sample delivery port disposal tray 96;

[0107] Step 2: Start the device, the push rod 61 starts to move downward for a distance, first driving the fixed rod 98 to move and snap into the groove 97, and then driving the storage tray 96 along the sample feeding plate 10 from the sample feeding port to just below the push rod 61 through the sample feeding assembly, 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 plate 72 moves downward with the fixed arm 76, and is squeezed outward after contacting the sample feeding port, the door plate 72 moves horizontally and blocks the sample feeding port, and when the fixed arm 76 also reaches the bottom, the system is closed;

[0108] Step 3: The push rod 61 can be moved downward along the slide groove 8 alone through the limit rod 83. At the same time, the end of the push rod 61 can absorb the connecting block 67 and attract the lock tongue 112 to slide into the lock groove 11, release the rotating plate 65 and then open the transport box 62, drive the carrier 69 to move out of the transport 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, the movable plate 22 is opened by the electric push rod 21, and the push rod 61 is continued to move downward to insert the carrier 69 into the liquid nitrogen mud, so that the sample is cooled and the freezing is completed;

[0109] Step 4: After cooling, lift the push rod 61 upward to drive the carrier 69 to rise. Driven by the push rod 61, the connecting block 67 is installed in the transfer box 62. The transfer box 62 is fixed by the limit frame 102. The push rod 61 continues to move upward to separate from the connecting block 67. The elastic band 113 pulls the lock 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.

[0110] Step 5: When the sample needs to be taken out, the push rod 61 is moved upward, and the driving rod 81 moves along the slide groove 8 and contacts 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 block 74 is re-engaged with the slot 77 under the action of the reset spring 73, driving the door panel 72 to move upward synchronously, opening the sample delivery port, and when the push rod 61 continues to move upward, the fixed rod 98 moves to the separation point from the groove 97, slides back into the groove 97, driving 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 illustrative and is not intended to imply that the scope of the present invention (including the claims) is limited to these examples. Under the concept of the present invention, the technical features in the above embodiments or different embodiments may be combined, the steps may be implemented in any order, and there are many other variations of the different aspects of the present invention as described above, which are not provided in detail for the sake of simplicity.

[0112] The present 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 the present invention should be included in the scope of protection of the present invention.

Claims

1. A liquid nitrogen sludge frozen sample preparation device, characterized in that: include: A machine body (1), wherein the machine body (1) is provided with a sample delivery port; A partition plate (2) is fixedly installed in the body (1) and is used 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 arranged on the machine body (1); A movable plate (22) is slidably mounted on the partition plate (2) and adapted to the connection port, and the movable plate (22) is fixedly connected to the movable end of the electric push rod (21); A vacuum pump (3) is arranged on the machine body (1) and is respectively connected to the upper and lower chambers of the machine body (1); A liquid nitrogen pump (4) is arranged on the machine body (1); A liquid nitrogen tank (5) is fixedly mounted on the inner bottom wall of the machine body (1) and is connected to the liquid nitrogen pump (4); A cylinder (6) is fixedly mounted on the top wall of the machine body (1); A push rod (61) fixedly mounted on the movable end of the cylinder (6) passing through the machine body (1); A sample delivery component, arranged in the machine body (1); A transport box (62), arranged on the sample delivery component; Two openings (63) are symmetrically arranged on the top and bottom outer walls of the transfer box (62); Four rotating shafts (64) are respectively fixedly installed in the two openings (63), and the two rotating shafts (64) in one opening (63) are symmetrically arranged; Four rotating plates (65) rotatably mounted on the rotating shaft (64); A carrier (69) disposed in the transfer box (62); A plurality of sample slots (611) are provided on the sample carrier (69); A plurality of elastic sheets (612) are fixedly mounted at positions corresponding to the sample slots (611); A linkage assembly is arranged in the transfer box (62); A sealing component is arranged in the machine body (1).

2. The device for preparing a liquid nitrogen sludge frozen sample according to claim 1, characterized in that: The linkage components include: Two linkage rods (66) are respectively hinged between the two rotating plates (65) on both sides, and the distance between one end hinged to the rotating plate (65) arranged 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 arranged in the transfer box (62); a baffle (68) fixedly mounted on the connecting block (67), and an upper surface of the baffle (68) is in contact with lower surfaces of the two rotating plates (65) located at the top when the transfer box (62) is in a closed state; Two magnetic blocks (610) are symmetrically fixedly installed in the transfer box (62) and located at positions corresponding to the object carrier (69); A locking assembly, arranged in the transfer box (62); The top wall of the carrier (69) is fixedly connected to the bottom wall of the connecting block (67); the connecting block (67) and the carrier (69) are both made of magnetic metal; a strong magnet is fixedly mounted on the end of the push rod (61) away from the cylinder (6); the two rotating plates (65) located on the top of the transfer box (62) are both provided with grooves matching the connecting block (67); when the transfer box (62) is in a closed state, the top surface of the connecting block (67) is coplanar with the upper surface of the rotating plate (65).

3. The device for preparing a liquid nitrogen sludge frozen sample according to claim 2, characterized in that: The locking assembly comprises: Two locking grooves (11) are symmetrically arranged on the two rotating plates (65) located at the top; Two lock holes (111) are symmetrically arranged on the transfer box (62) and are adapted to the lock slot (11); Two locking tongues (112) are slidably mounted in the two locking grooves (11) and are made of magnetic metal; The two elastic bands (113) are respectively fixedly installed in the two lock holes (111), and the other ends are respectively fixedly connected to the corresponding lock tongues (112).

4. The device for preparing a liquid nitrogen sludge frozen sample according to claim 1, characterized in that: The closure assembly comprises: Two guide plates (7) fixedly mounted on the inner wall of the machine body (1); Two sliding plates (71) are respectively slidably mounted in the two guide plates (7); A door panel (72) is arranged at a position in the machine body (1) corresponding to the sample delivery port, and a top of the door panel (72) is provided with an inclined surface inclined from the outside to the inside; A plurality of return springs (73) are fixedly mounted between the sliding plate (71) and the door plate (72); A clamping block (74) is fixedly mounted on the top inclined surface of the door panel (72); A sliding frame (75) is slidably mounted between the two guide plates (7); A fixed arm (76) is fixedly mounted 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 adapted to the door panel (72); A card slot (77) is provided on the inclined surface of the end of the fixed arm (76) and is adapted to fit the card block (74); A driving assembly is arranged on the fixed arm (76).

5. The device for preparing a liquid nitrogen sludge frozen sample according to claim 4, characterized in that: The drive assembly comprises: A slide groove (8) is provided at one end of the fixed arm (76) close to the push rod (61); A driving rod (81) is slidably mounted in the slide groove (8), and one end of the driving 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 mounted at the center of the clearance groove (82), and a torsion spring is fixedly mounted between the limiting rod (83) and the fixed arm (76).

6. The device for preparing a liquid nitrogen sludge frozen sample according to claim 1, characterized in that: The sample delivery component comprises: A fixing plate (9) fixedly mounted on the inner top wall of the machine body (1); A bevel gear (91) rotatably mounted on the fixed plate (9); Bevel gear 2 (92) is rotatably mounted on the top wall inside the machine body (1) and meshes with bevel gear 1 (91); A worm (93) is fixedly mounted on an end of the second bevel gear (92) away from the machine body (1); A rack (94) is slidably mounted on the inner wall of the body (1) and meshes with the worm (93); A connecting rod (95) is hinged to the bottom of the rack (94); A groove (97) is provided on the bevel gear (91); A fixing rod (98) fixedly mounted on the push rod (61) and adapted to the groove (97); A placement component is arranged on the machine body (1).

7. The device for preparing a liquid nitrogen sludge frozen sample according to claim 6, characterized in that: The placement component comprises: A sample delivery plate (10) is fixedly mounted on the machine body (1) at a position corresponding to the sample delivery port; A slide rail (101) is fixedly mounted on the sample delivery plate (10), and is provided with a notch at a position corresponding to the sample delivery port; A limiting frame (102) is fixedly mounted on the sample delivery plate (10) and is adapted to fit the transfer box (62); A storage support plate (96) is slidably mounted on the slide rail (101) and is hinged to an end of the connecting rod (95) away from the rack (94); the storage support plate (96) and the sample delivery plate (10) are provided with openings that are compatible with the opening (63); The limiting edge (99) is fixedly mounted on the storage support plate (96) and is adapted to the transfer box (62).

8. The device for preparing a liquid nitrogen sludge frozen sample according to claim 4, characterized in that: A sealing plate (78) is fixedly mounted on one end of the door plate (72) away from the push rod (61).

9. The device for preparing a liquid nitrogen sludge frozen sample according to claim 1, characterized in that: A step (12) is provided at a position of the transfer box (62) corresponding to the rotating plate (65), and a sealing portion (121) is fixedly installed at one end of the rotating plate (65) close to the step (12).

10. A method for preparing a liquid nitrogen mud frozen sample, based on the device for preparing a liquid nitrogen mud frozen sample according to any one of claims 1 to 9, characterized in that: The following steps are involved: Step 1: Open the locking assembly, press the connecting block (67) downward from the center of the top of the transfer box (62), the connecting block (67) drives the sample rack (69) to slide downward along the magnetic block (610), and the baffle (68) moves downward with the connecting block (67), take out the sample rack (69), place the sample in the corresponding sample slot (611) on the sample rack (69), ensure that the sample is firmly installed by the elastic sheet (612), install it from the bottom of the transfer box (62) upward, the sample rack (69) and the magnetic block (610) are adsorbed, so that the transfer box (62) remains in a closed state, and the transfer box (62) is placed on the sample delivery port disposal tray (96); Step 2: Start the device, the push rod (61) starts to move downward for a distance, first driving the fixed rod (98) to move and engage in the groove (97), and then driving the storage tray (96) along the sample delivery plate (10) from the sample delivery port to directly below the push rod (61) through the sample delivery component, 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 plate (72) moves downward with the fixed arm (76), contacts the sample delivery port and is squeezed outward, the door plate (72) moves horizontally and blocks the sample delivery port, and when the fixed arm (76) also reaches the bottom, the system is closed; Step 3: The push rod (61) can be moved downward along the slide groove (8) alone through the limit rod (83), and at the same time, the end of the push rod 61 can absorb the connecting block (67) and attract the lock tongue (112) to slide into the lock groove (11), release the rotating plate (65) and then open the transport box (62), drive the carrier (69) to move out of the transport 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, the movable plate (22) is opened by the electric push rod (21), and the push rod (61) is continued to move downward to insert the carrier (69) into the liquid nitrogen mud, so that the sample is cooled and the freezing is completed; Step 4: After cooling, the push rod (61) is lifted upward to drive the carrier (69) to rise. Under the drive of the push rod (61), the connecting block (67) is installed in the transfer box (62). The transfer box (62) is fixed by the limit frame (102). The push rod (61) continues to move upward to separate from the connecting block (67). The elastic band (113) pulls the lock tongue (112) to slide along the lock groove (11) and slide into the lock hole (111), locking 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 take out the sample, the push rod (61) is moved upward, the driving rod (81) moves along the slide groove (8) and contacts 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 clamping block (74) and the clamping 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, and when the push rod (61) continues to move upward, the fixed rod (98) moves to the point where it is separated from the groove (97), slides back into the groove (97), driving 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.

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