Rapid cooling sample table for freezing scanning electron microscope, cooling system and use method of cooling system

Abstract

In the rapid cooling sample table, in order to avoid the influence caused by the Leyton-Fowster effect, on the structural thermal armor in the rapid cooling sample table for the freezing scanning electron microscope, a steam channel is jointly formed by a low-temperature-resistant heat insulation film and a plurality of heat conduction columns which are arranged in a criss-cross manner, and during working, a sample is fixedly placed on a sample placement surface, so that the steam channel is formed by the low-temperature-resistant heat insulation film and a plurality of heat conduction columns which are arranged in a criss-cross manner; the sample stage body is put into liquid nitrogen snow mud, liquid nitrogen enters the steam channel through the low-temperature-resistant heat-insulating film, the heat conduction column absorbs and evaporates the liquid nitrogen, nitrogen generated by evaporation of the liquid nitrogen is led out through the steam channel, meanwhile, the heat conduction column makes contact with the liquid nitrogen, the liquid nitrogen is absorbed and / or dispersed through the low-temperature-resistant heat-insulating film, and the liquid nitrogen is led out in cooperation with the steam channel. According to the sample stage for the freezing scanning electron microscope, an insulating barrier formed by a steam layer is broken through, the problem that the cooling rate is insufficient due to the formation of the steam layer of a traditional sample stage is solved fundamentally, and the problem that in the prior art, a sample stage for the freezing scanning electron microscope has the Leyton-Fowster effect is solved.

Description

Technical Field

[0001] This invention relates to the field of rapid cooling technology, and specifically to a rapid cooling sample stage, cooling system, and method of using the cooling system for cryo-scanning electron microscopes. Background Technology

[0002] Cryo-scanning electron microscopy (Cryo-SEM) is an advanced microscopic morphology observation technique developed based on traditional scanning electron microscopy. It is especially useful for directly observing biological samples with high water content. It has the ability to observe electron beam sensitive samples, liquids, semi-liquids and multiphase systems (such as dairy products, cosmetics and biological tissues), and is now widely used in biology, medicine, materials science, food industry and pharmaceutical fields.

[0003] The sample chamber of a scanning electron microscope (SEM) typically requires a high-vacuum environment. Placing untreated, highly hydrated biological samples directly into this chamber can lead to severe dehydration, shrinkage, and deformation, resulting in the loss of their original morphological information. While conventional sample preparation methods such as chemical fixation, dehydration, and critical point drying can be used for some sample pretreatment, these methods are cumbersome, time-consuming (often exceeding 24 hours), and require a high level of operator skill. Furthermore, the repeatability and consistency of experimental results are difficult to guarantee.

[0004] In contrast, cryo-scanning electron microscopy does not require complex pretreatment of samples with high water content.

[0005] The main steps of existing cryo-scanning electron microscopy (cryo-SEM) involve rapidly fixing the target sample onto a dedicated stage and immersing it in liquid nitrogen slush (-210°C) for rapid freezing. This causes the water in the sample to transform directly from a liquid state to an amorphous glassy ice state, rather than forming crystalline ice crystals. This process preserves the original structural and morphological information of the sample to the greatest extent possible. However, during the immersion of the sample stage in liquid nitrogen slush, the Leidenfrost effect occurs. This effect occurs when a liquid comes into contact with a hot surface much above its boiling point (typically 200°C), causing rapid evaporation at the bottom to form an insulating vapor layer, which suspends the droplets and delays evaporation. The Leidenfrost effect significantly inhibits the cooling rate of the sample stage, resulting in only a few tens of micrometers of the sample surface forming glassy ice. Other areas produce artifacts, thus affecting the true morphological information of the sample.

[0006] Improving the sample cooling rate is a key technique for obtaining high-quality imaging. To reduce ice crystal formation, the sample cooling rate must be increased. Several methods are currently available for improving the cooling rate:

[0007] First, liquid ethane / propane mixed medium

[0008] Compared to pure liquid nitrogen, liquid ethane and propane have higher thermal conductivity, with cooling rates reaching 10 kilometres per second. 4 -10 6 The K value is 300-400 times higher than that of liquid nitrogen. Ethane has a freezing point of 90K and a boiling point of 184K, possessing a high heat capacity that enables ultra-high-speed cooling. This method is generally used for sample preparation in cryo-transmission electron microscopy. Due to cost and safety considerations, there are no commercially available devices suitable for this coolant for cryo-scanning electron microscopy.

[0009] Second, high-pressure refrigeration technology

[0010] For thicker samples (≤200μm), high-pressure freezing technology is used, operating at 2100 bar, with a surface freezing rate of up to 80,000 K / s, which can completely eliminate artifacts and illusory structures caused by ice crystals. However, this requires the purchase of expensive high-pressure freezing equipment, and the integration between the high-pressure freezing equipment and the sample preparation process of cryoscanning electron microscopy is not very good.

[0011] In view of this, this patent invention provides a rapid cooling sample stage for cryo-scanning electron microscopy to improve the sample cooling rate.

[0012] More specifically, commercially available sample stages for cryo-scanning electron microscopy are primarily made of copper with a thin gold plating on the outer surface to increase the cooling rate. However, in practice, it has been found that the Leidenfrost effect still occurs when samples are prepared in liquid nitrogen, leading to the formation of a vapor layer on the sample stage surface and slowing down the cooling rate. This slower cooling rate causes crystalline ice crystals to form inside the sample, obscuring its true internal morphology. Summary of the Invention

[0013] The purpose of this invention is to provide a rapid cooling sample stage, cooling system, and method of using the cooling system for cryo-scanning electron microscopy, in order to solve the problem of insufficient sample cooling rate during cryo-scanning electron microscopy sample preparation, which leads to artifacts in the internal microstructure of the sample.

[0014] To address the problems existing in the prior art, the present invention adopts the following technical solution:

[0015] A rapid cooling sample stage for cryo-scanning electron microscopy includes a sample stage body with a nitrogen channel penetrating the body. The sample stage body includes a structural heat armor. A low-temperature resistant insulating film and multiple heat-conducting pillars are disposed on the same surface of the structural heat armor. The multiple heat-conducting pillars are arranged in the same direction on the top of the structural heat armor and pass through the low-temperature resistant insulating film. The multiple heat-conducting pillars are arranged in a crisscross pattern, and a vapor channel is formed between every two horizontal rows and / or every two vertical rows of heat-conducting pillars and under the low-temperature resistant insulating film. A sample placement surface for placing a sample is provided on the top of the low-temperature resistant insulating film.

[0016] During operation, the sample is fixedly placed on the sample placement surface, and the main body of the sample stage is immersed in liquid nitrogen slush. The liquid nitrogen enters the vapor channel through the low-temperature resistant insulation membrane. The liquid nitrogen evaporates in the heat-conducting column, and the nitrogen gas generated by the evaporation of the liquid nitrogen is discharged through the vapor channel. At the same time, the heat-conducting column comes into contact with the liquid nitrogen and absorbs and / or disperses the liquid nitrogen through the low-temperature resistant insulation membrane, which works in conjunction with the vapor channel to discharge the liquid nitrogen.

[0017] As an improvement to the technical solution of the rapid cooling sample stage for cryo-scanning electron microscope of the present invention, the main body of the sample stage is made of pure copper.

[0018] As an improvement to the technical solution of the rapid cooling sample stage for cryo-scanning electron microscope of the present invention, each of the vapor channels is a U-shaped channel.

[0019] As an improvement to the technical solution of the rapid cooling sample stage for cryo-scanning electron microscope of the present invention, the low-temperature resistant heat insulation film is a low-temperature resistant heat insulation porous film, so as to absorb liquid nitrogen into the heat-conducting column more quickly and will not evaporate when in contact with the heat insulation film.

[0020] As an improvement to the technical solution of the rapid cooling sample stage for cryo-scanning electron microscope of the present invention, the horizontal position of the low-temperature resistant heat insulation film is at a distance from the top of the structural heat armor.

[0021] A rapid cooling system for cryo-scanning electron microscopes includes a rapid cooling sample stage for cryo-scanning electron microscopes as described above, and further includes a slush preparation stage for making liquid nitrogen slush, a heat exchanger, a transfer rod for loading and transporting the rapid freezing sample stage for cryo-scanning electron microscopes, a preparation chamber, and an electron microscope chamber, arranged sequentially in the order described above.

[0022] A method of using a rapid cooling system for a cryo-scanning electron microscope, comprising the following steps:

[0023] The sample is fixedly placed on the rapid cooling sample stage for cryo-scanning electron microscope, and the rapid cooling stage for cryo-scanning electron microscope is mounted on one end of the transfer rod.

[0024] One end of the transfer rod, which is equipped with a rapid cooling stage for cryo-scanning electron microscopy, is quickly inserted into liquid nitrogen slush. At the same time, a vacuum is drawn to observe the liquid nitrogen. Before the liquid nitrogen turns into slush, the sample is lifted into the vacuum chamber and then transferred to the preparation chamber, where fracture, sublimation and / or coating can be performed.

[0025] As an improvement to the technical solution of the rapid cooling system for cryo-scanning electron microscope of the present invention, the sample is adsorbed onto the sample placement surface by conductive adhesive.

[0026] The beneficial effects of this invention are:

[0027] In this invention, a structural heat armor is used for the cryo-scanning electron microscope (CSE) stage, achieving rapid cooling. To avoid the Leidenfrost effect, a low-temperature resistant insulating membrane and multiple crisscrossing high-temperature heat-conducting columns form a vapor channel on the structural heat armor of the stage body. During operation, nitrogen gas generated from liquid nitrogen evaporation is discharged through the vapor channel. Simultaneously, the high-temperature heat-conducting columns contact the liquid nitrogen, absorbing and / or dispersing it through the low-temperature resistant insulating membrane, which, in conjunction with the vapor channel, discharges the liquid nitrogen. This addresses the Leidenfrost effect problem in existing cryo-scanning electron microscope (CSE) stages, maximizing the preservation of the sample's original structural and morphological information by suppressing the Leidenfrost effect. Attached Figure Description

[0028] Figure 1 This is a schematic diagram of the rapid cooling sample stage for cooling a scanning electron microscope according to the present invention;

[0029] Figure 2 This is a schematic diagram of the connection of the rapid cooling system for cryo-scanning electron microscopes according to the present invention.

[0030] Explanation of reference numerals in the attached figures: 1 - Structural heat armor; 2 - High-temperature heat-conducting column; 3 - Low-temperature heat-insulating membrane; 4 - Vapor channel; 5 - Sample placement surface; 6 - Sample stage body; 7 - Transfer rod; 8 - Vacuum chamber; 9 - Preparation chamber. Detailed Implementation

[0031] To make the objectives, technical solutions, and beneficial effects of this invention clearer, the technical solutions in the embodiments of this invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of this invention, and not all embodiments.

[0032] like Figure 1As shown, the present invention provides a rapid cooling sample stage for cryo-scanning electron microscopes, comprising a sample stage body 6, a nitrogen channel penetrating the sample stage body 6, a structural heat armor 1, a low-temperature resistant insulating film 3 and multiple heat-conducting pillars 2 disposed on the same surface of the structural heat armor 1, the multiple heat-conducting pillars 2 being disposed in the same direction on the top of the structural heat armor 1, the multiple heat-conducting pillars 2 passing through the low-temperature resistant insulating film 3, the multiple heat-conducting pillars 2 being arranged in a crisscross pattern, and a vapor channel 4 being formed between every two horizontal rows and / or every two vertical rows of heat-conducting pillars 2 and under the low-temperature resistant insulating film 3; and a sample placement surface 5 for placing samples is provided on the top of the low-temperature resistant insulating film 3.

[0033] During operation, the sample is fixedly placed on the sample placement surface 5, and the sample stage body 6 is immersed in liquid nitrogen slush. The liquid nitrogen enters the vapor channel 4 through the low-temperature resistant insulating membrane 3. The liquid nitrogen evaporates in the heat-conducting column 2, and the nitrogen gas produced by the evaporation is discharged through the vapor channel 4. At the same time, the heat-conducting column 2 is in contact with the liquid nitrogen, and the low-temperature resistant insulating membrane 3 absorbs and / or disperses the liquid nitrogen, which is then discharged through the vapor channel 4. The heat-conducting column 2 is a high-temperature heat-conducting column 2.

[0034] Firstly, in this invention, to avoid the effects of the Leidenfrost effect, a vapor channel 4 is formed on the structural heat armor 1 of the rapid cooling sample stage used in cryo-scanning electron microscopy by means of a low-temperature resistant insulating film 3 and multiple crisscrossing heat-conducting columns 2. During operation, the sample is fixed on the sample placement surface 5, and the sample stage body 6 is immersed in liquid nitrogen slush. The liquid nitrogen enters the vapor channel 4 through the low-temperature resistant insulating film 3. The liquid nitrogen evaporates on the heat-conducting columns 2, and the nitrogen gas generated by the evaporation is discharged through the vapor channel 4. At the same time, the heat-conducting columns 2 are in contact with the liquid nitrogen, and the low-temperature resistant insulating film 3 absorbs and / or disperses the liquid nitrogen. Combined with the discharge of liquid nitrogen through the vapor channel 4, the insulating barrier formed by the vapor layer is broken, which fundamentally solves the problem of insufficient cooling rate caused by the formation of vapor layer in traditional sample stages and solves the problem of Leidenfrost effect in sample stages used in cryo-scanning electron microscopy in the prior art.

[0035] Secondly, by eliminating the interference of the vapor layer, the heat exchange efficiency between this invention and liquid nitrogen is significantly improved, allowing water in the sample to rapidly transform into amorphous glassy ice. This avoids artifacts in the sample's internal microstructure, expands the glassy ice formation area, and overcomes the traditional 30μm limitation. Simultaneously, the rapid cooling rate ensures that high-water-content samples such as biological tissues, dairy products, and cosmetics do not experience water loss, shrinkage, or structural damage during freezing, maximizing the restoration of the sample's natural microstructure and providing a true and reliable observational basis for scanning electron microscopy imaging.

[0036] Furthermore, this invention does not rely on a mixture of liquid ethane and liquid propane, thus avoiding cost and safety risks. It also eliminates the need for additional high-pressure freezing equipment, reducing equipment investment costs, and can be directly adapted to existing cryo-scanning electron microscope sample preparation processes.

[0037] In detail, the Leidenfrost effect refers to the phenomenon that when a liquid comes into contact with a hot surface much above its boiling point, it will rapidly vaporize at the bottom to form a heat-insulating vapor layer, causing the droplets to suspend and slowly evaporate.

[0038] In existing technologies, sample stages are often made of copper with a thin gold plating. When cooled in liquid nitrogen slush, the Leidenfrost effect easily occurs, forming an insulating vapor layer. This results in insufficient cooling of the sample, leading to the formation of crystalline ice crystals within the sample, damaging its original microstructure and producing artifacts, thus affecting image quality. Although copper has excellent thermal conductivity, the thermal contribution of the thin gold plating is negligible. However, if the thin gold plating has pores or is oxidized, it can actually act as a thermal resistance layer, exacerbating localized overheating, causing uneven heat distribution, and easily forming localized high-temperature points.

[0039] In other words, existing sample stages are mostly made of copper with a thin layer of gold plated on the outer surface to increase the cooling rate. However, in practice, it has been found that a significant Leidenfrost effect still occurs when preparing samples in liquid nitrogen, resulting in a large vapor layer on the sample stage surface, which slows down the cooling rate of the sample stage. The slowed cooling rate of the sample will cause crystalline ice crystals to form inside the sample, destroying the true morphological information of the sample's interior.

[0040] Moreover, generally speaking, if the purpose is simply to remove nitrogen, a combination of a thermally conductive film and a thermally conductive column is usually used to improve the heat conduction effect and thus better remove the nitrogen.

[0041] In this invention, a low-temperature resistant insulating film 3 is fused between multiple heat-conducting pillars 2 and attracted to the position of the heat-conducting pillars 2. Liquid nitrogen is absorbed by the heat-conducting pillars 2, and the liquid nitrogen evaporates on the sample stage body 6 of this invention. The nitrogen gas escapes through the vapor channel 4 formed by the low-temperature resistant insulating film 3 and the multiple heat-conducting pillars 2.

[0042] In this invention, the heat is rapidly conducted between the sample stage body 6 and the heat-conducting column 2 and the low-temperature resistant insulation film 3 through their combined action. However, the heat transfer is slow at the low-temperature resistant insulation film 3. Since liquid nitrogen evaporation occurs at the contact point between the heat-conducting column 2 and the low-temperature resistant insulation film 3, it does not interfere with the absorption of liquid nitrogen by the low-temperature resistant insulation film 3, thus ensuring cooling efficiency.

[0043] If, using existing technology, a thermally conductive film is used to replace the low-temperature resistant insulation film 3, the cooling efficiency will decrease significantly after multiple tests.

[0044] More specifically, in this invention, the Leidenfrost effect is suppressed by combining the structural heat armor 1 and the heat-conducting pillars 2 into a combined heat-conducting structure. This breaks through the simple heat-conducting structure of the traditional sample stage made of a single copper material with a thin gold plating. Multiple heat-conducting pillars 2 are arranged horizontally and vertically on the top of the structural heat armor 1. The heat-conducting pillars 2 directly penetrate the low-temperature resistant insulation film 3 and come into contact with liquid nitrogen. The high temperature and high thermal conductivity of the heat-conducting pillars 2 are used to quickly transfer heat. At the same time, the low-temperature resistant insulation film 3 absorbs and disperses the liquid nitrogen, breaking the limitation that the traditional sample stage surface is prone to forming a vapor insulation layer. The Leidenfrost effect is suppressed structurally, and the heat conduction efficiency and cooling efficiency are greatly improved.

[0045] Moreover, since the vapor channel 4 is formed by the space between every two horizontal and / or two vertical heat-conducting columns 2 and below the low-temperature resistant insulation film 3, it forms a grid-like flow-guiding structure on the top of the structural heat armor 1, which realizes the effect of directional nitrogen flow to optimize the cooling environment. It can timely and directionally export the nitrogen generated by liquid nitrogen evaporation, avoid nitrogen accumulation on the surface of the sample stage body 6 to form a vapor layer, further weaken the influence of the Leidenfrost effect, provide a continuous and efficient heat exchange environment for sample cooling, and ensure the stability of the cooling rate.

[0046] Furthermore, the sample stage body 6 is made of pure copper, where liquid nitrogen evaporates and escapes through the vapor channel 4.

[0047] In some embodiments of the present invention, the horizontal position of the low-temperature resistant heat insulation film 3 is at a distance from the top of the structural heat armor 1.

[0048] In detail, because there is a distance between the horizontal position of the low-temperature heat-resistant insulation film 3 and the top of the structural heat armor 1, the low-temperature heat-resistant insulation film 3 is prevented from being attached to the top of the structural heat armor 1, so that the low-temperature heat-resistant insulation film 3, the top of the structural heat armor 1, and the multiple high-temperature heat-conducting columns 2 can jointly form a vapor channel 4.

[0049] In some embodiments of the present invention, each steam channel 4 is a U-shaped channel, which can buffer the steam flow rate, balance the pressure fluctuations in the system, and reduce the water hammer phenomenon caused by steam and condensate impacting the pipe.

[0050] In some embodiments of the present invention, the low-temperature resistant heat insulation film 3 is a low-temperature resistant heat insulation porous film, so as to absorb liquid nitrogen into the high-temperature heat-conducting column 2 more quickly, and will not evaporate when in contact with the heat insulation film.

[0051] In this invention, by heating the structural heat armor 1 and the high-temperature heat-conducting column 2, the high-temperature heat-conducting column 2 comes into direct contact with liquid nitrogen. The liquid nitrogen is absorbed and rapidly dispersed by the low-temperature resistant insulation film 3, and the nitrogen is guided by the steam channel 4, thereby suppressing the Leidenfrost effect and improving the heat conduction efficiency.

[0052] like Figure 2 As shown, another aspect of the present invention provides a rapid cooling system for cryo-scanning electron microscopes, including the aforementioned rapid cooling sample stage for cryo-scanning electron microscopes, and further including a slush preparation stage for making liquid nitrogen slush, a heat exchanger, a transfer rod 7 for loading and transporting the rapid freezing sample stage for cryo-scanning electron microscopes, a preparation chamber 9, and an electron microscope chamber, arranged sequentially in the order described above.

[0053] Based on the rapid cooling system for cryo-scanning electron microscopes, the present invention also provides a method of using the rapid cooling system for cryo-scanning electron microscopes, comprising the following steps:

[0054] The sample is fixedly placed on the sample stage body 6 in the rapid cooling sample stage for cryo-scanning electron microscope, and the sample stage body 6 is mounted on the transfer rod 7.

[0055] The head of the transfer rod 7, which is loaded with the sample stage body 6, is quickly inserted into the liquid nitrogen slush device. At the same time, a vacuum is drawn to observe the liquid nitrogen. Before the liquid nitrogen turns into slush, the sample is lifted into the vacuum chamber 8 inside the transfer rod 7 and then transferred to the preparation chamber 9. In the preparation chamber 9, it can be fractured, sublimated and / or coated. Then it is transferred to the scanning electron microscope to observe the sample.

[0056] The sample is adsorbed onto the sample placement surface 5 using conductive adhesive.

[0057] In detail, the method of using the rapid cooling system for cryo-scanning electron microscopes according to the present invention includes the following steps:

[0058] The sample is fixed to the sample placement surface 5 of the rapid cooling sample stage for cryo-scanning electron microscope using carbon conductive cryo-adhesive, and then the rapid cooling sample stage for cryo-scanning electron microscope is loaded onto the transfer rod 7.

[0059] Liquid nitrogen snow was prepared using a snowmaking stage. Then, the head of the transfer rod 7, which is equipped with a rapid cooling sample stage for cryo-scanning electron microscopy, was quickly inserted into the liquid nitrogen snow. At the same time, a vacuum operation was started and the liquid state was observed.

[0060] Before the liquid nitrogen is converted into slush, the sample is lifted into the vacuum chamber 8 of the transfer rod 7 and then quickly transferred to the preparation chamber 9. The sample can then be subjected to fracture, sublimation and / or coating treatment in the preparation chamber 9 according to the test requirements.

[0061] After completing the above steps, transfer the sample to the electron microscope chamber of the scanning electron microscope, and start the microscope to observe the sample.

[0062] The method of using the rapid cooling system for cryo-scanning electron microscopes of the present invention is based on the rapid cooling sample stage for cryo-scanning electron microscopes. Therefore, the technical effects of the method of using the rapid cooling system for cryo-scanning electron microscopes of the present invention include, but are not limited to, the technical effects of the rapid cooling sample stage for cryo-scanning electron microscopes, which will not be elaborated here.

[0063] Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

Claims

1. A rapid cooling sample stage for a cryo-scanning electron microscope comprising a sample stage body having a nitrogen gas channel therethrough, characterised in that, The sample stage body comprises a structure thermal armor, a low-temperature-resistant thermal insulation film and a plurality of heat-conducting columns are arranged on the same surface of the structure thermal armor, the plurality of heat-conducting columns are arranged in the same direction on the upper surface of the structure thermal armor, the plurality of heat-conducting columns pass through the low-temperature-resistant thermal insulation film, the plurality of heat-conducting columns are arranged in a crisscross manner, the heat-conducting columns between every two horizontal rows and / or every two vertical columns and the lower surface of the low-temperature-resistant thermal insulation film jointly form a steam channel, and the upper surface of the low-temperature-resistant thermal insulation film is provided with a sample placement surface for placing a sample; In operation, the sample is fixed and placed on the sample placement surface, the sample stage body is put into liquid nitrogen slush, liquid nitrogen enters the steam channel through the low-temperature-resistant thermal insulation film, the liquid nitrogen evaporates on the heat-conducting columns, nitrogen gas generated by the evaporation of the liquid nitrogen is guided out of the steam channel, meanwhile, the heat-conducting columns are in contact with the liquid nitrogen, the liquid nitrogen is absorbed and / or dispersed by the low-temperature-resistant thermal insulation film, and the liquid nitrogen is guided out of the steam channel in cooperation with the steam channel.

2. The rapid cooling sample stage for a cryogenic scanning electron microscope of claim 1, wherein, The sample stage body is made of pure copper material.

3. The rapid cooling sample stage for a cryogenic scanning electron microscope of claim 1, wherein, Each steam channel is a U-shaped channel.

4. The rapid cooling sample stage for a cryogenic scanning electron microscope of claim 1, wherein, The low-temperature-resistant thermal insulation film is a low-temperature-resistant thermal insulation porous film, so that the liquid nitrogen can be absorbed into the heat-conducting columns more quickly and the liquid nitrogen cannot evaporate when contacting the thermal insulation film.

5. The rapid cooling sample stage for a cryogenic scanning electron microscope of claim 1, wherein, The horizontal position of the low-temperature-resistant thermal insulation film is away from the upper surface of the structure thermal armor.

6. A rapid cooling system for a cryo-scanning electron microscope, characterized by, The quick cooling sample stage for a cryo scanning electron microscope comprises the quick cooling sample stage for a cryo scanning electron microscope according to any one of claims 1-5, a slush manufacturing table for manufacturing liquid nitrogen slush, a heat exchanger, a transmission rod for loading and transmitting the quick cooling sample stage for a cryo scanning electron microscope, a preparation chamber and an electron microscope chamber which are sequentially arranged in sequence.

7. A method of use for a rapid cooling system for a cryogenic scanning electron microscope, characterized by, The quick cooling system for a cryo scanning electron microscope according to claim 6 comprises the following steps: A sample is fixed and placed on the quick cooling sample stage for a cryo scanning electron microscope, and the quick cooling sample stage for a cryo scanning electron microscope is loaded on one end of a transmission rod; One end of the transmission rod loaded with the quick cooling sample stage for a cryo scanning electron microscope is quickly inserted into liquid nitrogen slush, and vacuum is drawn to observe the liquid nitrogen, the sample is lifted into a vacuum chamber before the liquid nitrogen becomes slush, and then is transferred to a preparation chamber, and can be fractured, sublimed and / or coated in the preparation chamber.

8. The method of using a rapid cooling system for a cryogenic scanning electron microscope of claim 7, wherein, The sample is adsorbed on the sample placement surface by conductive glue.

Images