In-situ liquid nitrogen cooling and heating stage
By designing an in-situ liquid nitrogen heating and cooling stage, combined with a temperature-controlled heating and cooling mechanism, the problem of observing samples with high water content in low temperature, high temperature and high temperature switching environments in existing technologies has been solved, realizing the accurate detection of biological materials and in-situ observation of structural changes.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- TAIYUAN UNIVERSITY OF TECHNOLOGY
- Filing Date
- 2022-12-13
- Publication Date
- 2026-04-10
AI Technical Summary
Existing hot and cold stages cannot meet the in-situ observation requirements of samples with high water content, such as biological materials, under low temperature, high temperature and high temperature switching environments, and existing scanning electron microscopes have adverse effects when testing samples with high water content.
An in-situ liquid nitrogen heating and cooling stage was designed, comprising a temperature-controlled heating mechanism, a cooling mechanism, and a vibration damping mechanism. Temperature regulation is achieved through heating components and piping components, cooling is achieved using liquid nitrogen, and vibration damping materials are used to improve the stability and accuracy of the device. In-situ observation is performed in conjunction with a tensile device.
It enables precise detection of biological materials and materials with high water content under different temperature conditions, improving the accuracy and stability of sample detection, and allowing observation of structural changes in biological tissues under stress and low-to-high temperature coupling conditions.
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Figure CN116067119B_ABST
Abstract
Description
TECHNICAL FIELD
[0001] The present application relates to the technical field of small cold and hot stage, in particular to an in-situ liquid nitrogen cold and hot stage. BACKGROUND
[0002] For the existing conventional scanning electron microscope, the sample observed in the test process should generally be anhydrous and free of other volatile solvents. If a sample with a high water content such as biological material is tested, it will have many adverse effects on the scanning electron microscope. The current solution is usually to dehydrate and dry the sample after fixation, and then test it with the conventional scanning electron microscope according to the method for testing ordinary samples, or to load a low-temperature freezing preparation transmission system and an integrated liquid nitrogen tank freezing sample stage on the conventional scanning electron microscope to upgrade the conventional scanning electron microscope to a frozen scanning electron microscope.
[0003] However, in actual testing, the sample to be tested has various types, and the test conditions include low-temperature environment, high-temperature environment, and high-low temperature switching environment, etc. to realize in-situ observation of the mechanical properties. The cold and hot stage in the prior art cannot well meet our actual needs.
[0004] Therefore, an in-situ liquid nitrogen cold and hot stage is provided. SUMMARY
[0005] The purpose of the present application is to provide an in-situ liquid nitrogen cold and hot stage, which aims to solve or improve at least one of the above technical problems.
[0006] To achieve the above purpose, the present application provides the following scheme: the present application provides an in-situ liquid nitrogen cold and hot stage, comprising:
[0007] A temperature control heating mechanism, the temperature control heating mechanism comprises a heating assembly and a sealing upper plate; the heating assembly is installed on the sealing upper plate, and a conduction plate is installed on the heating assembly;
[0008] A cooling mechanism, the cooling mechanism comprises a pipeline assembly and a cold and heat exchange tank; the cold and heat exchange tank is fixedly connected to the bottom of the sealing upper plate, and the sealing upper plate and the sealing upper plate are combined to form a sealed cavity; the pipeline assembly is used for introducing liquid nitrogen into the sealed cavity;
[0009] A damping mechanism, the damping mechanism comprises a base assembly and a spring assembly; the base assembly is detachably connected to the bottom of the cold and heat exchange tank, the spring assembly is arranged between the base assembly and the cold and heat exchange tank, and the base assembly is embedded with a damping material.
[0010] Preferably, the base assembly comprises:
[0011] A hanging support plate is detachably connected to the bottom of the cold-heat exchange tank, and a gap is provided between the bottom end face of the cold-heat exchange tank and the hanging support plate.
[0012] An isolation seat is detachably connected to the bottom of the hanging support plate, and the inner cavity of the isolation seat is embedded with the damping material.
[0013] A base is fixed to the bottom of the isolation seat.
[0014] The spring assembly is installed in the gap, and the two ends of the spring assembly abut against the top face of the hanging support plate and the bottom face of the cold-heat exchange tank, respectively.
[0015] Preferably, the top face of the hanging support plate is provided with a plurality of installation grooves arranged in sequence at intervals.
[0016] The spring assembly includes a plurality of support springs located in the gap, and a plurality of the support springs are arranged one-to-one with a plurality of the installation grooves; the bottom of the support spring abuts against the bottom wall of the installation groove, and the top of the support spring abuts against the bottom face of the cold-heat exchange tank.
[0017] Preferably, the top face of the base is provided with insulating mounting plates on both sides, and the two ends of the insulating mounting plates are detachably connected to the base by fourth screws.
[0018] Preferably, the heating assembly includes:
[0019] A connecting seat is detachably mounted on one side of the top face of the sealing upper plate by first screws.
[0020] An insulating pad is mounted on the top face of the connecting seat.
[0021] A heating rod is mounted on the top face of the sealing upper plate.
[0022] The conducting plate is detachably mounted at the center of the top face of the sealing upper plate by second screws, and the conducting plate and the sealing upper plate form an installation cavity, and the heating rod is located in the installation cavity; the wire of the heating rod extends out of the installation cavity and is electrically connected with a positive terminal post and a negative terminal post; the positive terminal post and the negative terminal post are detachably connected to the insulating pad by fixing screws.
[0023] Preferably, a cooling channel is provided on the top face of the cold-heat exchange tank, the cooling channel is located in the sealing cavity; the two ends of the cooling channel are communicated with the pipeline assembly; a plurality of heat exchange fins arranged in sequence at intervals are fixed to the inner wall of the cooling channel.
[0024] Preferably, the pipeline assembly comprises:
[0025] The connecting head is provided with two; two The inner cavities of the two connecting heads are communicated with the two ends of the cooling channel respectively;
[0026] The connecting pipe is provided with two; two The connecting pipe is detachably connected with two connecting heads respectively;
[0027] The liquid pipe is provided with two; two The liquid pipe is detachably connected at the end of the connecting pipe away from the connecting head respectively;
[0028] Among them, the liquid pipe, the connecting pipe and the connecting head inner cavity are communicated with each other.
[0029] Preferably, the outer side wall of the cold and hot exchange groove is fixed with a plurality of connecting wing plates at the bottom; the connecting wing plates are threadedly connected with third screws; the bottom of the third screw is threadedly connected with the top surface of the suspended support plate.
[0030] Preferably, the cooling channel is arranged in Z shape.
[0031] Preferably, the damping material is any one or several of porous alumina ball, aluminum silicate fiber brick and damping rubber block.
[0032] The present application discloses the following technical effects:
[0033] The present application sets up a heating assembly to heat the surface of the conducting plate, sets up a pipeline assembly to pass liquid nitrogen into the sealed cavity, and then realizes the cooling treatment of the surface of the sealed upper plate and the conducting plate, so as to facilitate the regulation and control of the surface temperature of the conducting plate according to the actual working condition, and realize the test of biological materials and materials with high water content such as liquid under different temperature conditions;
[0034] The present application sets up a base assembly, and embeds damping material in the base assembly, improves the damping performance of the cold and hot table as a whole, improves the running stability of the device, and improves the accuracy of sample detection on the surface of the conducting plate;
[0035] The present application sets up a spring assembly between the base assembly and the cold and hot exchange groove, so that an air insulation layer is formed between the base assembly and the cold and hot exchange groove, direct conduction of temperature is avoided, insulation and temperature isolation of cold and hot liquid are realized, loss of heat and cold is reduced, and running efficiency of the device is improved;
[0036] The present application can be equipped with a stretching device on the surface of the conducting plate, so as to observe the structural changes of biological tissues under the coupling of stress and low / high temperature, and synchronously study the biological tissue structure under the action of multiple fields. BRIEF DESCRIPTION OF DRAWINGS
[0037] In order to more clearly illustrate the technical solutions in the embodiments of the present application or the prior art, the drawings needed to be used in the embodiments will be briefly introduced as follows. Obviously, the drawings in the following description are only some embodiments of the present application, and other drawings can be obtained by those skilled in the art without any creative effort on the basis of these drawings.
[0038] Figure 1 It is an exploded view of the in-situ liquid nitrogen cooling and heating table of the present application;
[0039] Figure 2 It is a perspective view of the present application;
[0040] Figure 3 It is a structural schematic view of the temperature control heating mechanism in the present application;
[0041] Figure 4 It is a structural schematic view of the cooling mechanism in the present application;
[0042] Figure 5 It is a structural schematic view of the cooling and heating exchange tank in the present application;
[0043] Figure 6 It is a structural schematic view of the damping mechanism in the present application;
[0044] Figure 7 It is a front view of the present application;
[0045] Figure 8 It is a practical refrigeration test data graph of the present application;
[0046] Figure 9 It is a practical heating temperature data graph of the present application;
[0047] Wherein, 101, positive pole terminal; 102, negative pole terminal; 103, heating rod; 104, insulating pad; 105, connecting seat; 106, sealing upper plate; 107, first screw; 108, second screw; 109, conducting plate; 201, cold and heat exchange groove; 202, third screw; 203, connecting head; 204, connecting pipe; 205, liquid pipe; 301, suspended support plate; 302, support spring; 304, isolation seat; 305, fourth screw; 306, damping material; 307, base; 308, insulating mounting plate. DETAILED DESCRIPTION
[0048] The technical solutions in the embodiments of the present application will be clearly and completely described below with reference to the drawings in the embodiments of the present application. Obviously, the described embodiments are only part of the embodiments of the present application, rather than all the embodiments. Based on the embodiments in the present application, all other embodiments obtained by those skilled in the art without creative work fall within the scope of protection of the present application.
[0049] In order to make the above-mentioned purposes, features and advantages of the present application more obvious and easy to understand, the present application will be further described in detail below with reference to the drawings and specific embodiments.
[0050] Reference Figures 1-9 The present application provides an in-situ liquid nitrogen cold and heat platform, comprising:
[0051] The temperature control heating mechanism comprises a heating assembly and a sealing upper plate 106; the heating assembly is installed on the sealing upper plate 106, and a conducting plate 109 is installed on the heating assembly; the upper surface of the conducting plate 109 is used for placing a detection sample;
[0052] The cooling mechanism comprises a pipeline assembly and a cold and heat exchange groove 201; the cold and heat exchange groove 201 is fixedly connected at the bottom of the sealing upper plate 106 and is combined with the sealing upper plate 106 to form a sealed cavity; in this embodiment, the cold and heat exchange groove 201 is welded with the sealing upper plate 106 to form a complete sealed cavity; the pipeline assembly is used for introducing liquid nitrogen into the sealed cavity; in this way, the surface of the conducting plate 109 is heated by the heating assembly, the pipeline assembly is arranged to introduce liquid nitrogen into the sealed cavity, and then the temperature of the surface of the conducting plate 109 is reduced, so that the temperature of the surface of the conducting plate 109 can be adjusted and controlled according to actual working conditions, and the testing of biological materials and materials with high water content such as liquid can be realized under different temperature conditions;
[0053] The damping mechanism comprises a base assembly and a spring assembly; the base assembly is detachably connected at the bottom of the cold and heat exchange groove 201, the spring assembly is arranged between the base assembly and the cold and heat exchange groove 201, and the damping material 306 is embedded in the base assembly;
[0054] In this way, the vibration damping material 306 improves the overall vibration damping performance of the cold and hot table, improves the stability of the device, and improves the accuracy of sample detection on the surface of the conduction plate 109; the spring assembly forms an air isolation layer between the base assembly and the cold and heat exchange tank 201, avoids direct conduction of temperature, realizes insulation and temperature isolation of the cold and hot liquid, reduces the loss of heat and cold, and improves the operation efficiency of the device;
[0055] When the heating treatment is performed, the liquid nitrogen is stopped from being introduced into the sealed cavity, and the heating assembly is started to heat the surface of the conduction plate 109; when the low-temperature refrigeration treatment is performed, the liquid nitrogen is introduced into the sealed cavity through the pipeline assembly, and the heating assembly is started; by adjusting the heating power of the heating assembly, the refrigeration temperature is accurately controlled, and the sample detection accuracy is improved;
[0056] The present application can be equipped with a stretching device (not shown in the figure) on the surface of the conduction plate 109, and the stretching device is used for stretching the sample on the surface of the conduction plate 109. The working principle and internal structure of the stretching device are both prior art, and will not be repeated here; by cooperating with the stretching device, the structural changes of biological tissues under the stress and low-high temperature coupling state can be observed, and the biological tissue structure under the action of multiple fields can be studied synchronously. Through the combination of the stretching device, in-situ observation experiments can be carried out, so that researchers can directly observe the real-time changes of the organization and structure of biological materials and liquid materials and other materials that are not easy to observe under the combined state of stress and low-high temperature, solving the problem that conventional scanning electron microscopes cannot test samples with high water content or liquid samples.
[0057] Further optimization scheme, the base assembly comprises:
[0058] The overhanging support plate 301 is detachably connected to the bottom of the cold and heat exchange tank 201, and a gap is provided between the bottom end face of the cold and heat exchange tank 201;
[0059] The isolation seat 304 is detachably connected to the bottom of the overhanging support plate 301, and the inner cavity of the isolation seat 304 is embedded with the vibration damping material 306;
[0060] The base 307 is fixedly connected to the bottom of the isolation seat 304;
[0061] The spring assembly is installed in the gap, and the two ends of the spring assembly are respectively in abutment with the top surface of the overhanging support plate 301 and the bottom surface of the cold and heat exchange tank 201;
[0062] In this way, the air gap layer is formed between the suspension support plate 301 and the cold and heat exchange tank 201 through the spring assembly, which can avoid the direct contact between the suspension support plate 301 and the cold and heat exchange tank 201, thereby reducing the loss of heat or cold and improving the refrigeration or heating efficiency of the device; the damping and heat insulation performance of the device as a whole is improved through the damping material 306 in the isolation seat 304, and the detection accuracy is improved.
[0063] Further optimization scheme, the top surface of the suspension support plate 301 is provided with a plurality of installation grooves arranged in sequence (not shown in the figure);
[0064] The spring assembly includes a plurality of support springs 302 located in the gap, and the plurality of support springs 302 are arranged one by one corresponding to the plurality of installation grooves (not shown in the figure); the bottom of the support spring 302 abuts against the bottom wall of the installation groove, and the top of the support spring 302 abuts against the bottom surface of the cold and heat exchange tank 201;
[0065] In this way, the support spring 302 is pressed and assembled between the installation groove and the cold and heat exchange tank 201, which avoids the displacement of the support spring 302 during the extension and contraction process, absorbs part of the vibration force through the extension and contraction of the plurality of support springs 302, improves the stability of the detection process, and at the same time, the plurality of support springs 302 separates the suspension support plate 301 from the cold and heat exchange tank 201 to form an air heat insulation layer and reduce heat loss.
[0066] Further optimization scheme, the top surface of the base 307 is provided with insulating mounting plates 308 on both sides, and the two ends of the insulating mounting plates 308 are detachably connected to the base 307 through fourth screws 305; the insulating mounting plates 308 are made of insulating materials, and the material of the insulating mounting plates 308 in this embodiment is insulating ceramic, which is used for electrical insulation.
[0067] Further optimization scheme, the heating assembly includes:
[0068] The connecting seat 105 is detachably mounted on one side of the top surface of the sealing upper plate 106 through the first screw 107;
[0069] The insulating pad 104 is mounted on the top surface of the connecting seat 105; the insulating pad 104 is made of insulating material and plays an electrical insulation role;
[0070] The heating rod 103 is mounted on the top surface of the sealing upper plate 106;
[0071] The conduction plate 109 is detachably installed at the center of the top surface of the sealing upper plate 106 through the second screw 108, and the conduction plate 109 is combined with the sealing upper plate 106 to form an installation cavity, and the heating rod 103 is located in the installation cavity; the wire of the heating rod 103 extends out of the installation cavity and is electrically connected with the positive terminal post 101 and the negative terminal post 102; the positive terminal post 101 and the negative terminal post 102 are detachably connected on the insulating pad 104 through the fixing screw;
[0072] In this way, by connecting to a power supply device (not shown in the figure), the heating rod 103 is powered to heat, thereby regulating the surface temperature of the conduction plate 109, facilitating the adaptation to different detection conditions.
[0073] Further optimization scheme, the top surface of the cold and heat exchange groove 201 is provided with a cooling channel, the cooling channel is located in the sealing cavity; the two ends of the cooling channel are communicated with the pipeline assembly; a plurality of heat exchange fins are fixedly connected on the inner wall of the cooling channel; in this way, the contact area of liquid nitrogen and the cooling channel is increased through the plurality of heat exchange fins, thereby improving the cold and heat exchange efficiency.
[0074] Further optimization scheme, the pipeline assembly comprises:
[0075] The connecting head 203 is provided with two; the two connecting heads 203 are fixedly connected on the outer wall of the cold and heat exchange groove 201 side by side, and the inner cavities of the two connecting heads 203 are respectively communicated with the two ends of the cooling channel;
[0076] The connecting pipe 204 is provided with two; the two connecting pipes 204 are respectively detachably connected with the two connecting heads 203;
[0077] The liquid pipe 205 is provided with two side by side; the two liquid pipes 205 are respectively detachably connected at one end of the connecting pipe 204 away from the connecting head 203;
[0078] Among them, the inner cavities of the liquid pipe 205, the connecting pipe 204 and the connecting head 203 are communicated with each other;
[0079] In this way, during refrigeration, liquid nitrogen is introduced into one of the liquid pipes 205, the liquid nitrogen enters the cooling channel through the connecting pipe 204 and the connecting head 203, and the heat exchange is carried out through the heat exchange fins in the cooling channel, and the heat exchanged liquid nitrogen is discharged through the other connecting head 203, the connecting pipe 204 and the liquid pipe 205, realizing the continuous introduction of liquid nitrogen, and further realizing the refrigeration treatment of the surface of the sealing upper plate 106 and the conduction plate 109.
[0080] Further optimization scheme, a plurality of connecting wing plates are fixedly connected on the bottom of the outer side wall of the cold and heat exchange groove 201; the third screw 202 is threadedly connected on the connecting wing plate; the bottom of the third screw 202 is threadedly connected with the top surface of the suspended support plate 301.
[0081] Further optimization scheme, cooling channel is arranged in Z shape, and the cooling channel is arranged in a plurality of ring channels in the cold and heat exchange tank 201, further increasing the contact area of liquid nitrogen and the body of the cold and heat exchange tank 201, and improving the cold and heat exchange efficiency.
[0082] Further optimization scheme, the damping material 306 is any one or several of porous aluminum oxide balls, aluminum silicate fiber bricks and damping rubber blocks; in this way, the damping material 306 plays a good temperature insulation, waterproof and damping performance, thereby improving the sample detection accuracy.
[0083] In the description of the present application, it should be understood that the terms "longitudinal", "transverse", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer" and the like indicate the orientation or positional relationship based on the orientation or positional relationship shown in the drawings, and are only for the convenience of describing the present application, and do not indicate or imply that the device or element referred to must have a particular orientation, be constructed and operated in a particular orientation, therefore cannot be understood as a limitation on the present application.
[0084] The above-described embodiments are only preferred modes of the present application, and do not limit the scope of the present application, and various modifications and improvements to the technical solutions of the present application made by those skilled in the art without departing from the design spirit of the present application shall fall within the protection scope determined by the claims of the present application.
Claims
1. An in situ liquid nitrogen cold stage, characterized by, The utility model relates to a temperature control heating mechanism, cooling mechanism and damping mechanism for a vacuum chamber. The temperature control heating mechanism comprises a heating assembly and a sealing upper plate (106), the heating assembly is installed on the sealing upper plate (106), and a conduction plate (109) is installed on the heating assembly. The cooling mechanism comprises a pipeline assembly and a cold heat exchange groove (201), the cold heat exchange groove (201) is fixed to the bottom of the sealing upper plate (106) and is combined with the sealing upper plate (106) to form a sealed cavity, and the pipeline assembly is used for introducing liquid nitrogen into the sealed cavity. The damping mechanism comprises a base assembly and a spring assembly, the base assembly is detachably connected to the bottom of the cold heat exchange groove (201), the spring assembly is arranged between the base assembly and the cold heat exchange groove (201), and a damping material (306) is embedded in the base assembly. The base assembly comprises a suspended support plate (301), a spacer (304) and a base (307). The suspended support plate (301) is detachably connected to the bottom of the cold heat exchange groove (201) and has a gap between the bottom end surface of the cold heat exchange groove (201). The spacer (304) is detachably connected to the bottom of the suspended support plate (301), and the inner cavity of the spacer (304) is embedded with the damping material (306). The base (307) is fixed to the bottom of the spacer (304). The spring assembly is installed in the gap, and the two ends of the spring assembly are respectively in abutment with the top surface of the suspended support plate (301) and the bottom surface of the cold heat exchange groove (201). The top surface of the suspended support plate (301) is provided with a plurality of installation grooves arranged in sequence at intervals. The spring assembly comprises a plurality of support springs (302) arranged in the gap, and the plurality of support springs (302) are arranged one-to-one with the plurality of installation grooves.
2. The in situ liquid nitrogen cryotherapy stage of claim 1, wherein: The bottom of the support spring (302) is in abutment with the bottom wall of the installation groove, and the top of the support spring (302) is in abutment with the bottom surface of the cold heat exchange groove (201).
3. The in situ liquid nitrogen cryotherapy stage of claim 1, wherein: The top surface of the base (307) is provided with insulating mounting plates (308) on both sides, and the two ends of the insulating mounting plates (308) are detachably connected to the base (307) through fourth screws (305). The heating assembly comprises a connecting seat (105), an insulating pad (104) and a heating rod (103). The two ends of the connecting seat (105) are detachably installed on one side of the top surface of the sealing upper plate (106) through first screws (107). The insulating pad (104) is installed on the top surface of the connecting seat (105). The heating rod (103) is installed on the top surface of the sealing upper plate (106). The conductive plate (109) is detachably installed at the center of the top surface of the sealing upper plate (106) through the second screw (108), the conductive plate (109) is combined with the sealing upper plate (106) to form an installation cavity, and the heating rod (103) is located in the installation cavity; the wire of the heating rod (103) extends out of the installation cavity and is electrically connected with the positive terminal post (101) and the negative terminal post (102); the positive terminal post (101) and the negative terminal post (102) are detachably connected on the insulating pad (104) through fixing screws.
4. The in situ liquid nitrogen cryotherapy stage of claim 1, wherein: A cooling channel is formed on the top surface of the cold-heat exchange tank (201), and the cooling channel is located in the sealing cavity; the two ends of the cooling channel are communicated with the pipeline assembly; a plurality of heat exchange fins are fixedly connected to the inner wall of the cooling channel.
5. The in situ liquid nitrogen cryotherapy stage of claim 4, wherein: The pipeline assembly comprises: The connecting head (203) is provided with two; the two connecting heads (203) are fixedly connected to the outer wall of the cold-heat exchange tank (201) side by side, and the inner cavities of the two connecting heads (203) are respectively communicated with the two ends of the cooling channel; The connecting pipe (204) is provided with two; the two connecting pipes (204) are respectively detachably connected with the two connecting heads (203); The liquid pipe (205) is provided with two; the two liquid pipes (205) are respectively detachably connected to one end of the connecting pipe (204) away from the connecting head (203); The liquid pipe (205), the connecting pipe (204) and the inner cavity of the connecting head (203) are communicated with each other.
6. The in situ liquid nitrogen cryotherapy stage of claim 1, wherein: A plurality of connecting wing plates are fixedly connected to the bottom of the outer side wall of the cold-heat exchange tank (201); the third screw (202) is threadedly connected to the connecting wing plate; and the bottom of the third screw (202) is threadedly connected to the top surface of the suspended support plate (301).
7. The in situ liquid nitrogen cryotherapy stage of claim 4, wherein: The cooling channel is arranged in a Z shape.
8. The in situ liquid nitrogen cryotherapy stage of claim 1, wherein: The damping material (306) is any one or several of porous alumina balls, aluminum silicate fiber bricks and damping rubber blocks.
Citation Information
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