A frozen sample holder for transmission electron microscope

Abstract

The present invention relates to a transmission electron microscope frozen sample rod, comprising a refrigeration pot, a cooling rod assembly fixedly connected to the refrigeration pot, and a sample stage fixedly arranged on the cooling rod assembly, and also comprising a shielding cover, wherein the shielding cover can be movably connected to the cooling rod assembly, and the sample stage can be shielded or opened by the movement of the shielding cover relative to the sample stage. When the transmission electron microscope frozen sample rod of the present invention does not need to observe the sample, the shielding cover can be slid to shield the sample stage to prevent the sample on the sample stage from contacting the outside world, thereby protecting the sample; and the shielding cover can isolate the external light source to prevent the sample from reacting to light.

Description

Technical Field

[0001] The invention relates to a freezing sample rod for a transmission electron microscope. Background Art

[0002] Transmission Electron Microscope (TEM) is a modern large-scale instrument for studying the microstructure of matter. It is widely used in physics, chemistry, material science, life science and other fields. The sample rod is one of the most important components of the transmission electron microscope. The sample rod is provided with a sample carrier for carrying the sample. In the prior art, the sample carrier is usually open, and the sample on the sample carrier cannot be covered. When the sample is not observed, the sample on the sample carrier will continue to contact with the outside world, which is not conducive to the protection of the sample. Especially for some samples that are easy to react to light, the open sample carrier has the hidden danger of causing the sample to react to light. Summary of the invention

[0003] Therefore, in order to solve the above problems, the present invention proposes a transmission electron microscope freezing sample rod with optimized structure.

[0004] The present invention is implemented by the following technical solutions:

[0005] The present invention proposes a transmission electron microscope freezing sample rod, comprising a refrigeration pot, a cooling rod assembly fixedly connected to the refrigeration pot, and a sample carrier fixedly arranged on the cooling rod assembly, and also comprising a shielding cover, which can be movably connected to the cooling rod assembly, and the sample carrier can be shielded or opened by the movement of the shielding cover relative to the sample carrier.

[0006] In order to save space and make the structure of the sampling end of the transmission electron microscope freezing sample rod more compact and reasonable, it is preferred that the shielding cover is slidably connected to the cooling rod assembly.

[0007] In order to achieve better protection and shading effects and to make the sliding connection between the shielding cover and the cooling rod assembly more stable, the shielding cover is preferably a frame-shaped structure, and the shielding cover can be slidably mounted on the cooling rod assembly.

[0008] Among them, in order to avoid frostbite and improve safety, the transmission electron microscope freezing sample rod preferably also includes a driving component for driving the shielding cover to move relative to the sample loading platform, and the driving component includes an operating part for manual force application, and the operating part is arranged away from the sample loading platform.

[0009] Among them, in order to make the driving component occupy less space, have a compact structure, high transmission efficiency, and be convenient for users to operate, the driving component preferably includes a transmission rod, one end of which is linked to the shielding cover, and the other end passes through the cooling rod assembly and extends to the side of the refrigeration kettle away from the cooling rod assembly, and the operating part is linked to the other end of the transmission rod.

[0010] Among them, preferably, the driving assembly also includes a slide rail, the operating part is a slider slidably fitted in the slide rail, the slide rail is fixedly connected to the side of the refrigeration kettle away from the cooling rod assembly, and the other end of the transmission rod is fixedly connected to the slider.

[0011] Preferably, the slide rail is in the shape of an elongated strip to form a gripping portion.

[0012] In order to save copper material and utilize the extended structure of the cooling inner rod to guide the transmission rod, the cooling rod assembly includes a cooling inner rod and an outer sleeve outermostly disposed on the cooling inner rod, the outer sleeve is fixedly connected to the refrigeration pot, one end of the cooling inner rod is disposed in the refrigeration pot, and the other end extends out of the outer sleeve, and the sample carrier is fixedly disposed at the end of the cooling inner rod extending out of the outer sleeve; the cooling inner rod is a hollow structure, and the transmission rod is disposed in the hollow inner cavity of the cooling inner rod. In order to isolate cold conduction and increase the cold preservation time, it is preferred that a vacuum interlayer is formed between the outer sleeve and the cooling inner rod.

[0013] In order to prevent the temperature of the cooling rod assembly from being too low and affecting the coordination between the transmission electron microscope freezing sample rod and other electron microscopes or instruments, a heating patch is fixed on the inner wall of the outer sleeve to control the temperature of the cooling rod assembly.

[0014] In order to isolate cold conduction and increase the cold preservation time, the refrigeration kettle is preferably a double-layer structure, including an inner layer of liquid ammonia kettle and an outer shell, and a vacuum interlayer is formed between the liquid ammonia kettle and the outer shell. In order to increase the cold conduction path, reduce heat conduction, and increase the cold preservation time, the liquid ammonia kettle preferably includes a kettle body arranged in the outer shell, a kettle mouth exposed outside the outer shell, and a connecting pipe connecting the kettle mouth and the kettle body, and the connecting pipe is provided with at least one circle of corrugated folds around it.

[0015] The present invention has the following beneficial effects: when the sample does not need to be observed, the transmission electron microscope frozen sample rod of the present invention can slide the shielding cover to shield the sample stage to prevent the sample on the sample stage from contacting the outside world, thereby protecting the sample; and the shielding cover can isolate the external light source to prevent the sample from reacting to light. BRIEF DESCRIPTION OF THE DRAWINGS

[0016] Figure 1 is a three-dimensional schematic diagram of a frozen sample rod for a transmission electron microscope in an embodiment;

[0017] Figure 2 is a right side view of a frozen sample rod of a transmission electron microscope in an embodiment;

[0018] Figure 3 yes Figure 2 Sectional view at AA in the middle;

[0019] Figure 4 It is a schematic diagram of a feasible alternative solution of the shielding cover in the embodiment. DETAILED DESCRIPTION

[0020] To further illustrate the various embodiments, the present invention provides drawings. These drawings are part of the disclosure of the present invention, which are mainly used to illustrate the embodiments and can be used in conjunction with the relevant descriptions in the specification to explain the operating principles of the embodiments. With reference to these contents, a person of ordinary skill in the art should be able to understand other possible implementations and advantages of the present invention. The components in the figures are not drawn to scale, and similar component symbols are generally used to represent similar components.

[0021] The present invention will now be further described with reference to the accompanying drawings and specific implementation methods.

[0022] See also Figure 1-3 As shown, as a preferred embodiment of the present invention, a transmission electron microscope frozen sample rod is provided, including a refrigeration pot 1, a cooling rod assembly 2, and a sample stage 3 fixedly arranged on the cooling rod assembly 2, wherein the refrigeration pot 1 serves as a cold source, the cooling rod assembly 2 is fixedly connected to the refrigeration pot 1, and the low temperature generated by the refrigeration pot 1 is conducted to the sample stage 3, so that the sample on the sample stage 3 is in a low temperature state. A shielding cover 4 can also be slidably connected to the cooling rod assembly 2, and the shielding cover 4 can shield or open the sample stage 3 by sliding relative to the sample stage 3. Then, when the transmission electron microscope frozen sample rod of this embodiment does not need to observe the sample, the shielding cover 4 can be slid to shield the sample stage 3 to prevent the sample on the sample stage 3 from contacting the outside world, thereby protecting the sample; and more importantly, the shielding cover 4 can isolate the external light source to prevent the sample from reacting to light. When the sample needs to be observed again, the shielding cover 4 is slid to open the sample stage 3, and the observation work can be continued.

[0023] In this embodiment, the shielding cover 4 is a square frame structure, and the shielding cover 4 is slidably mounted on the cooling rod assembly 2. In other embodiments, the shielding cover 4 may also be other structures, such as a sheet-shaped cover. In this embodiment, a frame-shaped shielding cover 4 is slidably mounted on the cooling rod assembly 2. On the one hand, the frame-shaped shielding cover 4 can surround the sample stage 3 from all sides, providing better protection and shading effects for the samples on the sample stage 3. On the other hand, the sliding connection between the shielding cover 4 and the cooling rod assembly 2 is more stable, reducing the position accuracy requirements for the shielding cover 4 when it is installed.

[0024] In this embodiment, the shielding cover 4 is slidably connected to the cooling rod assembly 2. In other embodiments, the shielding cover 4 can also be rotatably connected to the cooling rod assembly 2, that is, whether it is a slidable connection or a rotatable connection or other movable connection methods are feasible. For example, Figure 4 An alternative to the shielding cover 4 of the present embodiment is shown, the shielding cover 4A is a sheet-like structure, the shielding cover 4A can be rotatably connected to the cooling rod assembly 2A, and the sample stage 3A can be shielded or opened by the rotation of the shielding cover 4A. Compared with this alternative, the scheme in which the shielding cover 4 is slidably connected to the cooling rod assembly 2 in the present embodiment can save space, making the structure of the sampling end of the transmission electron microscope frozen sample rod more compact and reasonable.

[0025] When the refrigerating kettle 1 is working, the temperature near the sample loading platform 3 is very low, and it is inconvenient for the user to directly slide the shielding cover 4 by hand, otherwise it may cause health problems such as frostbite. In order to improve safety and facilitate the operation of sliding the shielding cover 4, a driving assembly for driving the shielding cover 4 to slide is also provided in this embodiment. The driving assembly specifically includes a transmission rod 5, a slide rail 6 and a slider 7. The slide rail 6 is fixedly connected to the side of the refrigerating kettle 1 away from the cooling rod assembly 2. The slider 7 can be slidably fitted in the slide rail 6. One end of the transmission rod 5 is linked to the shielding cover 4 (specifically, it is hinged in this embodiment, and it can also be fixedly connected by clamping, screwing, etc. in other embodiments). The other end of the transmission rod 5 passes through the cooling rod assembly 2 and the transmission rod 5 and extends to the side of the refrigerating kettle 1 away from the cooling rod assembly 2. The slider 7 and the other end of the transmission rod 5 are fixedly connected (can also be hinged), so that when the slider 7 is manually moved to slide in the slide rail 6, the shielding cover 4 is driven to slide through the transmission rod 5. Since the slider 7 serving as the manual force operation part is arranged on the side of the refrigeration pot 1 away from the cooling rod assembly 2 and far away from the sample loading platform 3, there will be no frostbite problem when operating the slider 7.

[0026] In other embodiments, the slider 7 as the manual force operation part can be set at other positions away from the sample loading platform 3. For example, the slider 7 and the slide rail 6 can be set at the radially outer position of the refrigerating pot 1, and then the slider 7 and the shielding cover 4 are linked by setting a connecting rod mechanism on the periphery of the refrigerating pot 1. However, in this embodiment, the transmission rod 5 is set to pass through the cooling rod assembly 2 and then fixedly connected to the slider 7, so that the transmission rod 5 can be slidably assembled in the cooling rod assembly 2 and extend to the side of the refrigerating pot 1 away from the cooling rod assembly 2 with the help of the extension direction of the cooling rod assembly 2, so that the space occupied by the drive assembly is small, the structure is compact, and the transmission efficiency is high. The slide rail 6 and the slider 7 are set on the side away from the cooling rod assembly 2, which is also convenient for users to operate.

[0027] In other embodiments, the slider 7 can also be replaced by an operating part for manual force application of other structures. For example, the operating part is implemented by a knob, and the transmission rod is hinged on the end surface of the knob (forming a crank slider mechanism), and the transmission rod is driven to slide by rotating the knob. Under reasonable mechanical mechanism design, the mutual conversion of sliding and rotation can be used to realize the drive of the drive component. Therefore, the operating part for manual force application of its drive component can be either rotating or sliding, which can be determined according to the structural layout and cost considerations of the actual product. This embodiment preferably adopts the sliding drive solution of the slide rail 6 and the slider 7. This sliding drive method has a simple structure, high transmission efficiency, intuitive action, and convenient operation.

[0028] In this embodiment, the slide rail 6 is in a long strip structure to form a gripping portion. When the user holds the TEM frozen sample rod, he can hold the refrigeration pot 1 with one hand and hold the slide rail 6 with the other hand, so as to stably hold the TEM frozen sample rod.

[0029] See also Figure 1 , 3 The cooling rod assembly 2 includes a cooling inner rod 21 and an outer sleeve 22 which is arranged on the cooling inner rod 21. The outer sleeve 22 is fixedly connected to the refrigeration pot 1. One end of the cooling inner rod 21 is arranged in the refrigeration pot 1 to conduct low temperature. The other end of the cooling inner rod 21 extends out of the outer sleeve 22. The sample carrier 3 is fixedly arranged on the end of the cooling inner rod 21 extending out of the outer sleeve 22. In this embodiment, the cooling inner rod 21 specifically adopts a copper rod, and the copper rod conducts cooling more stably and is not easy to fluctuate. The cooling inner rod 21 is a hollow structure, and the transmission rod 5 is a hollow inner cavity penetrated by the cooling inner rod 21. In this embodiment, setting the cooling inner rod 21 as a hollow structure can not only save copper materials, but also utilize the extension structure of the cooling inner rod 21 to guide the transmission rod 5. Furthermore, the present embodiment also has a heating patch (not shown in the figure) fixed on the inner wall of the outer sleeve 22. The heating patch can detect the temperature of the cooling rod assembly 2 and heat the cooling rod assembly 2 through electrical automatic control technology to prevent the cooling rod assembly 2 from being too low and affecting the coordination between the transmission electron microscope freezing sample rod and other electron microscopes or instruments.

[0030] See also Figure 3 The refrigeration pot 1 is a double-layer structure, including an inner layer of a liquid ammonia pot 11 and an outer shell 12, and a sandwich is formed between the liquid ammonia pot 11 and the outer shell 12. Similarly, a sandwich is also formed between the outer sleeve 22 and the cooling inner rod 21, and the inner cavity of the outer sleeve 22 is communicated with the inner cavity of the outer shell 12. The refrigeration pot 1 is also provided with an exhaust valve 8, and the sandwich between the liquid ammonia pot 11 and the outer shell 12, and the sandwich between the outer sleeve 22 and the cooling inner rod 21 are evacuated by the exhaust valve 8. The vacuum sandwich can effectively isolate cold conduction and increase the cold preservation time.

[0031] In addition, in order to further increase the cold preservation time, a thin-wall structure can be provided in the interlayer between the liquid ammonia pot 11 and the outer shell 12, and in the interlayer between the outer sleeve 22 and the cold-conducting inner rod 21, to isolate cold conduction. The connection between the outer sleeve 22 and the outer shell 12 can be connected at multiple connection points rather than surface to surface, so as to reduce the contact area and reduce heat conduction.

[0032] Continue reading Figure 3 The liquid ammonia pot 11 specifically includes a pot body 111 disposed in an outer shell 12, a pot mouth 113 exposed outside the outer shell 12, and a connecting pipe 112 connecting the pot mouth 113 and the pot body 111. The pot body 111 stores liquid ammonia for cooling, and the pot mouth 113 is used to add liquid ammonia. In actual use, a cover is also provided on the pot mouth 113 for sealing (not shown in the figure). The connecting pipe 112 is provided with several circles (at least one circle) of corrugated folds around the body, and the corrugated folds increase the path for the pot body 111 to conduct cooling to the pot mouth 113, reduce heat conduction, and further increase the cold preservation time.

[0033] Although the present invention has been specifically shown and described in conjunction with the preferred embodiments, it should be understood by those skilled in the art that various changes in form and details made to the present invention without departing from the spirit and scope of the present invention as defined in the appended claims will fall within the scope of protection of the present invention.

Claims

1. A transmission electron microscope frozen sample holder, comprising a cooling pot, a cooling rod assembly fixedly connected to the cooling pot, and a sample loading platform fixedly arranged on the cooling rod assembly, characterized in that: It also includes a shielding cover, which can be movably connected to the cooling rod assembly, and the sample platform can be shielded or opened by the movement of the shielding cover relative to the sample platform; it also includes a driving assembly for driving the shielding cover to move relative to the sample platform, the driving assembly includes an operating part for manual force application, and the operating part is arranged away from the sample platform; the driving assembly includes a transmission rod, one end of the transmission rod is linked to the shielding cover, and the other end passes through the cooling rod assembly and extends to the side of the refrigeration kettle away from the cooling rod assembly, and the operating part is linked to the other end of the transmission rod; the operating part is rotating or sliding.

2. The transmission electron microscope frozen sample holder according to claim 1, characterized in that: The shielding cover can be slidably connected to the cooling rod assembly.

3. The transmission electron microscope frozen sample holder according to claim 2, characterized in that: The shielding cover is a frame-shaped structure, and the shielding cover can be slidably sleeved on the cooling rod assembly.

4. The transmission electron microscope frozen sample holder according to claim 1, characterized in that: The driving assembly also includes a slide rail, the operating part is a slider slidably fitted in the slide rail, the slide rail is fixedly connected to the side of the refrigeration kettle away from the cooling rod assembly, and the other end of the transmission rod is fixedly connected to the slider.

5. The transmission electron microscope frozen sample holder according to claim 4, characterized in that: The slide rail is in the shape of an elongated strip to form a gripping portion.

6. The transmission electron microscope frozen sample holder according to claim 1, characterized in that: The cooling rod assembly includes a cooling inner rod and an outer sleeve which is externally mounted on the cooling inner rod, wherein a vacuum interlayer is formed between the outer sleeve and the cooling inner rod; the outer sleeve is fixedly connected to the refrigeration pot, one end of the cooling inner rod is arranged in the refrigeration pot, and the other end extends out of the outer sleeve, and the sample loading platform is fixedly arranged on the end of the cooling inner rod which extends out of the outer sleeve; the cooling inner rod is a hollow structure, and the transmission rod is passed through the hollow inner cavity of the cooling inner rod.

7. The transmission electron microscope frozen sample holder according to claim 6, characterized in that: A heating patch is also fixedly provided on the inner wall of the outer sleeve to control the temperature of the cooling rod assembly.

8. The transmission electron microscope frozen sample holder according to claim 1, characterized in that: The refrigeration kettle has a double-layer structure, including an inner liquid ammonia kettle and an outer shell, and a vacuum interlayer is formed between the liquid ammonia kettle and the outer shell; the liquid ammonia kettle includes a kettle body arranged in the outer shell, a kettle mouth exposed outside the outer shell, and a connecting pipe connecting the kettle mouth and the kettle body, and the connecting pipe is provided with at least one circle of corrugated folds around it.

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