Transmission electron microscope sample rod vacuum storage and different partial pressure atmosphere pretreatment device

By designing the vacuum storage of the transmission electron microscope sample rods in vacuum systems and pipelines and the pretreatment devices for different partial pressure atmospheres, the problem of sample rod pollution and single function is solved, and a variety of atmosphere pretreatment is realized, ensuring good conditions for electron microscope tests and Easy to operate.

CN119198791APending Publication Date: 2024-12-27DALIAN INSTITUTE OF CHEMICAL PHYSICS CHINESE ACADEMY OF SCIENCES
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Patent Information

Application Number
CN202310752313.1
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2023-06-25
Publication Date
2024-12-27

AI Technical Summary

Technical Problem

The existing transmission electron microscope sample rods are contaminated when exposed to the atmosphere, and the vacuum storage device has a single function, which cannot effectively support multiple atmosphere pretreatment, affecting the electron microscope test effect.

Method used

A transmission electron microscope sample rod vacuum storage and different pressure-dividing atmosphere pretreatment device are designed, equipped with angle valves, transparent glass tubes, air intake valves, pressure display devices and other components, and are closed and externally connected by angle valves. The gas circuit realizes partial pressure pretreatment of different atmospheres, avoids pollution and supports multiple atmosphere treatments.

Benefits of technology

It effectively avoids the adhesion of water vapor and pollutants on the surface of the sample rod, realizes pretreatment of different atmospheres, maintains good electron microscope testing conditions, is not affected by the vacuum environment, is simple to operate and convenient to maintain.

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Abstract

The invention discloses a transmission electron microscope sample rod vacuum storage and different partial pressure atmosphere pretreatment device. An external assembly capable of being externally connected with a gas pipe fitting is additionally arranged on an original pipeline capable of storing a sample rod, the external assembly comprises an air inlet valve and an air inlet, a pressure display device is matched, the device only has a vacuum storage function before being transformed, and the device can serve as pretreatment equipment for different partial pressures under the atmosphere condition after being transformed; meanwhile, the pretreatment effect can be kept when the device is matched with a frozen sample rod for use, so that the device is not influenced by the vacuum condition of an electron microscope to meet the requirements of different types of test conditions.
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Description

Technical Field

[0001] The present application relates to a transmission electron microscope sample rod vacuum storage and different partial pressure atmosphere pretreatment device, belonging to the field of electron microscope equipment. Background Art

[0002] At present, the sample rods of existing transmission electron microscopes are directly exposed to the outside. Due to long-term exposure to the atmosphere, water vapor and pollutants in the air will adhere to the surface of the sample rod. When the sample rod is sent into the transmission electron microscope, the contaminants attached to the surface are slowly released under the action of vacuum, which will prolong the vacuum pumping time of the electron microscope. What is more serious is that the contaminants enter the vacuum chamber of the electron microscope and contaminate the vacuum chamber, pole shoes and other components. Therefore, it is necessary to store the transmission electron microscope sample rod in a vacuum device.

[0003] For frozen sample rods, low temperature is achieved by transferring the low temperature (liquid nitrogen temperature) of the tail end of the Dewar tank to the sample end. It is necessary to ensure that the vacuum layer of the Dewar tank is maintained at a high vacuum condition to prevent temperature loss. There are molecular sieves that absorb water vapor in the vacuum layer of the Dewar tank. For better use effect, the frozen sample rod needs to be baked before and after use to maintain a good vacuum degree of the vacuum layer. At the same time, the low temperature part of the front end of the sample rod will condense water vapor when exposed to the atmosphere, and it also needs to be heated and vacuumed to recover quickly. The frozen sample rod is equipped with a heating and temperature control device. It is necessary to equip it with vacuum equipment for heating treatment and storage.

[0004] In addition, there are usually some pretreatment conditions before testing TEM samples, such as pretreatment for a certain period of time under a certain atmosphere and a certain partial pressure. The current vacuum storage station has a single function, and the vacuum conditions of the electron microscope itself will affect the effect of pretreatment. Therefore, it is worth paying attention to develop new functions on this basis to solve the problem of TEM sample rods being exposed to air and contaminated, as well as how to support multiple atmosphere pretreatments and maintain good pretreatment effects without being affected by the vacuum environment of the electron microscope. Summary of the invention

[0005] In order to better solve the problem of transmission electron microscope sample holders being contaminated when exposed to the air and how to support multiple atmosphere pretreatments and maintain good pretreatment effects without being affected by the vacuum environment of the electron microscope, according to one aspect of the present application, a transmission electron microscope sample holder vacuum storage and different partial pressure atmosphere pretreatment device is provided, including a vacuum system and a pipeline fixedly connected to the system through a connector, and a plurality of angle valves are correspondingly arranged on the pipeline;

[0006] Several levels of sample rod sockets are fixedly connected to the pipeline through adapter flanges;

[0007] The pipeline is also connected to several levels of transparent glass tubes;

[0008] The sample rod socket and / or the transparent glass tube are provided with an external component, and the external component includes an air inlet valve and an air inlet, and can be externally connected to a gas pipe;

[0009] At least one of the sample rod sockets provided with an external component and / or the transparent glass tube is also provided with a pressure display device;

[0010] The pipeline is also provided with a vacuum gauge.

[0011] Optionally, a plurality of levels of sample rod sockets are arranged in one-to-one correspondence with a plurality of levels of transparent glass tubes.

[0012] Optionally, a first external component is provided at one end of at least one of the transparent glass tubes away from the pipeline, wherein the first external component includes a first air inlet valve and a first air inlet port;

[0013] In this form, the angle valve connected to the vacuum system and the pipeline is closed. After the sample rod carrying the sample is inserted into the sample rod socket, the angle valves connected to the pipeline are closed uniformly, the external gas line is connected to the first air inlet valve, and then the first air inlet valve is opened. The gas required for pretreatment, such as carbon dioxide, nitrogen, ethylene, ethane, methane, oxygen, etc., is introduced from the external gas line. The pressure display device is observed. After reaching the required partial pressure, the first air inlet valve is closed. At this time, the sample pretreatment can be carried out under this condition, and then the subsequent electron microscope test can be carried out;

[0014] If a vacuum transfer freezing sample rod is used, the front end of the sample can be sealed and then frozen with liquid nitrogen for storage before subsequent electron microscopy testing.

[0015] Optionally, an external component is provided on at least one set of the transparent glass tube and the sample rod socket, specifically comprising:

[0016] A first external component is arranged at one end of the transparent glass tube away from the pipeline, wherein the first external component comprises a first air inlet valve and a first air inlet port;

[0017] A second external component is arranged on the sample rod socket, wherein the second external component includes a second air inlet valve and a second air inlet;

[0018] In this form, the angle valve connecting the vacuum system and the pipeline is closed, and after the sample rod carrying the sample is inserted into the sample rod socket, the set of pipelines with the sample rod is connected to the pipeline with the external component after the modification, and the external gas circuit is connected to the first air inlet valve and the second air inlet valve, and then the first air inlet valve and the second air inlet valve are opened, and the gas required for pretreatment, such as carbon dioxide, nitrogen, ethylene, ethane, methane, oxygen, etc., is introduced from the external air circuit, and gas replacement is first performed, and then the second air inlet valve is closed, and the pressure display device is observed. After reaching the required partial pressure, the first air inlet valve and the second air inlet valve are closed. At this time, the sample pretreatment can be carried out under this condition, and then the subsequent electron microscope test can be carried out;

[0019] If a vacuum transfer freezing sample rod is used, the front end of the sample can be sealed and then frozen with liquid nitrogen for storage before subsequent electron microscopy testing.

[0020] Optionally, the transparent glass tube and the sample rod socket are respectively arranged on both sides of the pipeline.

[0021] Optionally, a plugging piece is inserted into the sample rod socket where the sample rod is not inserted to seal it.

[0022] Optionally, the pressure display device is one of a pressure gauge, a pressure sensor, and a vacuum gauge.

[0023] Optionally, the pipeline is also provided with an external interface.

[0024] Optionally, the external interface is externally connected to a hose, and the hose is connected to a vacuum layer of the frozen sample rod, and is used to dry the water-absorbing material in the vacuum layer before / after the frozen sample rod is used.

[0025] Optionally, the vacuum system includes vacuum equipment such as a mechanical pump and a molecular pump and connecting pipelines.

[0026] The beneficial effects of this application include:

[0027] 1) A transmission electron microscope sample holder vacuum storage and different partial pressure atmosphere pretreatment device provided in the present application, which is provided with an air inlet valve and an air inlet, respectively, and can be externally connected to a gas pipe, so as to realize the function of pretreatment in different atmospheres and different partial pressures, and at the same time, when used with a frozen sample holder, the pretreatment effect can be maintained, so that it is not affected by the vacuum conditions of the electron microscope;

[0028] 2) The TEM sample holder vacuum storage and different partial pressure atmosphere pretreatment device provided in the present application avoids the problem that the TEM sample holder is exposed to the atmosphere for a long time and water vapor and pollutants in the air adhere to the surface of the sample holder;

[0029] 3) The transmission electron microscope sample holder vacuum storage and different partial pressure atmosphere pretreatment device provided in the present application is simple to operate, easy to install, and convenient to maintain and disassemble. BRIEF DESCRIPTION OF THE DRAWINGS

[0030] Figure 1 This is a schematic diagram of the vertical structure of the transmission electron microscope sample holder vacuum storage and different partial pressure atmosphere pretreatment device provided in Example 1 of the present application.

[0031] List of parts and reference numerals:

[0032] 1. Vacuum system; 2. Angle valve; 3. Connectors; 4. Transparent glass tube; 5. Sample rod socket; 6. Adapter flange; 7. Plug; 8. Vacuum gauge; 9. External interface; 10. Pressure display device; 11. First air inlet valve; 12. First air inlet port; 13. Second air inlet valve; 14. Second air inlet port; 15. Pipeline. DETAILED DESCRIPTION

[0033] The present application is described in detail below with reference to embodiments, but the present application is not limited to these embodiments.

[0034] Example 1

[0035] A transmission electron microscope sample holder vacuum storage and different partial pressure atmosphere pretreatment device, comprising a vacuum system 1 and a pipeline 15 fixedly connected to the vacuum system 1 through a connector 3, and a four-stage angle valve 2 is correspondingly arranged on the pipeline 15;

[0036] The third-level sample rod socket 5 is fixedly connected to the pipeline 15 through the adapter flange 6;

[0037] The pipeline 15 is also connected to a three-stage transparent glass tube 4;

[0038] The sample rod socket 5 is arranged one-to-one with the transparent glass tube 4, and an angle valve 2 is arranged accordingly;

[0039] The transparent glass tube 4 and the sample rod socket 5 are respectively arranged on both sides of the pipeline 15;

[0040] The sample rod socket 5 provided with an external component is also provided with a pressure display device 10;

[0041] The pressure display device 10 is a vacuum gauge;

[0042] The pipeline 15 is also provided with a vacuum gauge 8 and an external interface 9, the external interface 9 is externally connected to a hose, the hose is connected to the vacuum layer of the frozen sample rod, and is used to dry the water-absorbing material in the vacuum layer before / after the frozen sample rod is used;

[0043] Insert a plugging member 7 into the sample rod insertion port 5 where the sample rod is not inserted to seal it;

[0044] The vacuum system 1 includes vacuum equipment such as a mechanical pump and a molecular pump and a connecting pipeline 15. It should be understood that this solution does not limit the form of the vacuum system 1. Figure 1 The figure shows a vertical vacuum storage station, but it can also be applied to horizontal or other types of vacuum storage stations.

[0045] An external component is provided on a set of the transparent glass tube 4 and the sample rod socket 5, specifically comprising:

[0046] A first external component is disposed at one end of the transparent glass tube 4 away from the pipeline 15, wherein the first external component includes a first air inlet valve 11 and a first air inlet 12;

[0047] A second external component is arranged on one of the sample rod sockets 5, wherein the second external component includes a second air inlet valve 13 and a second air inlet 14;

[0048] In this form, the angle valve 2 connecting the vacuum system 1 and the pipeline 15 is closed, and after the sample rod carrying the sample is inserted into the sample rod socket 5, the group of pipelines with the sample rod is connected to the pipeline with the external component after the modification, and the external gas circuit is connected to the first air inlet valve 11 and the second air inlet valve 13, and then the first air inlet valve 11 and the second air inlet valve 13 are opened, and the gas required for pretreatment, such as carbon dioxide, nitrogen, ethylene, ethane, methane, oxygen, etc., is introduced through the external gas circuit, and the pressure display device 10 is observed. First, gas replacement is performed, and then the second air inlet valve is closed. After reaching the required partial pressure, the first air inlet valve 11 and the second air inlet valve 13 are closed. At this time, the sample pretreatment can be carried out under this condition, and then the subsequent electron microscope test can be carried out;

[0049] If a vacuum transfer freezing sample rod is used, the front end of the sample can be sealed and then frozen with liquid nitrogen for storage before subsequent electron microscopy testing.

[0050] Example 2

[0051] A transmission electron microscope sample holder vacuum storage and different partial pressure atmosphere pretreatment device, comprising a vacuum system 1 and a pipeline 15 fixedly connected to the vacuum system 1 through a connector 3, and a six-stage angle valve 2 is correspondingly arranged on the pipeline 15;

[0052] The pipeline 15 is also connected to a five-level transparent glass tube 4;

[0053] The five-level sample rod socket 5 is fixedly connected to the pipeline 15 through the adapter flange 6. The sample rod socket 5 is arranged one-to-one with the transparent glass tube 4, and an angle valve 2 is correspondingly arranged;

[0054] The transparent glass tube 4 and the sample rod socket 5 are respectively arranged on both sides of the pipeline 15;

[0055] A first external component is disposed at one end of the transparent glass tube 4 away from the pipeline 15, wherein the first external component includes a first air inlet valve 11 and a first air inlet 12;

[0056] The sample rod socket 5 provided with an external component and the transparent glass tube 4 are also provided with a pressure display device 10;

[0057] The pressure display device 10 is a vacuum gauge;

[0058] The pipeline 15 is also provided with a vacuum gauge 8 and an external interface 9, the external interface 9 is externally connected to a hose, the hose is connected to the vacuum layer of the frozen sample rod, and is used to dry the water-absorbing material in the vacuum layer before and after the frozen sample rod is used;

[0059] Insert a plugging member 7 into the sample rod insertion port 5 where the sample rod is not inserted to seal it;

[0060] The vacuum system 1 includes vacuum equipment such as a mechanical pump and a molecular pump and a connecting pipeline 15. It should be understood that this solution does not limit the form of the vacuum system 1.

[0061] In this form, the angle valve 2 connected to the vacuum system 1 and the pipeline 15 is closed. After the sample rod carrying the sample is inserted into the sample rod socket 5, the angle valves 2 connected to the pipeline 15 are closed uniformly, the external gas line is connected to the first air inlet valve 11, and then the first air inlet valve 11 is opened, and the gas required for pretreatment, such as carbon dioxide, nitrogen, ethylene, ethane, methane, oxygen, etc., is introduced from the external gas line. The pressure display device 10 is observed. After reaching the required partial pressure, the first air inlet valve 11 is closed. At this time, the sample pretreatment can be carried out under this condition, and then the subsequent electron microscope test can be carried out;

[0062] If a vacuum transfer freezing sample rod is used, the front end of the sample can be sealed and then frozen with liquid nitrogen for storage before subsequent electron microscopy testing.

[0063] The above two embodiments respectively modify only the transparent glass tube 4 or modify the transparent glass tube 4 and the sample rod socket 5 at the same level. However, it is also feasible to modify only the sample rod socket 5 or modify the transparent glass tubes 4 and the sample rod sockets 5 at different levels.

[0064] The above description is only a partial embodiment of the present application and does not constitute any form of limitation to the present application. Although the present application is disclosed as above with preferred embodiments, it is not intended to limit the present application. Any technician familiar with the profession, without departing from the scope of the technical solution of the present application, using the above disclosed technical content to make slight changes or modifications are equivalent to equivalent implementation cases and fall within the scope of the technical solution.

Claims

1. A transmission electron microscope sample holder vacuum storage and different partial pressure atmosphere pretreatment device, characterized in that: It includes a vacuum system and a pipeline fixedly connected to the vacuum system through a connector, and a plurality of angle valves are correspondingly arranged on the pipeline; Several levels of sample rod sockets are fixedly connected to the pipeline through adapter flanges; The pipeline is also connected to several levels of transparent glass tubes; The sample rod socket and / or the transparent glass tube are provided with an external component, and the external component includes an air inlet valve and an air inlet; At least one of the sample rod sockets provided with an external component and / or the transparent glass tube is also provided with a pressure display device; The pipeline is also provided with a vacuum gauge.

2. A transmission electron microscope sample holder vacuum storage and different partial pressure atmosphere pretreatment device according to claim 1, characterized in that: A plurality of levels of sample rod sockets are arranged in one-to-one correspondence with a plurality of levels of transparent glass tubes.

3. A transmission electron microscope sample holder vacuum storage and different partial pressure atmosphere pretreatment device according to claim 2, characterized in that: A first external component is arranged at one end of at least one of the transparent glass tubes away from the pipeline, and the first external component includes a first air inlet valve and a first air inlet port.

4. The transmission electron microscope sample holder vacuum storage and different partial pressure atmosphere pretreatment device according to claim 2, characterized in that: An external component is arranged on at least one set of the transparent glass tube and the sample rod socket, specifically comprising: A first external component is arranged at one end of the transparent glass tube away from the pipeline, wherein the first external component comprises a first air inlet valve and a first air inlet port; A second external component is arranged on the sample rod socket, and the second external component comprises a second air inlet valve and a second air inlet.

5. The transmission electron microscope sample holder vacuum storage and different partial pressure atmosphere pretreatment device according to claim 1, characterized in that: The transparent glass tube and the sample rod socket are respectively arranged on both sides of the pipeline.

6. The transmission electron microscope sample holder vacuum storage and different partial pressure atmosphere pretreatment device according to claim 1, characterized in that: A plugging piece is inserted into the sample rod insertion port where no sample rod is inserted to seal the sample rod.

7. The device for vacuum storage and pretreatment of sample holders of transmission electron microscope according to claim 1, characterized in that: The pressure display device is one of a pressure gauge, a pressure sensor and a vacuum gauge.

8. The transmission electron microscope sample holder vacuum storage and different partial pressure atmosphere pretreatment device according to claim 1, characterized in that: The pipeline is also provided with an external interface.

9. A transmission electron microscope sample holder vacuum storage and different partial pressure atmosphere pretreatment device according to claim 8, characterized in that: The external interface is externally connected to a hose, and the hose is connected to the vacuum layer of the frozen sample rod.

10. The transmission electron microscope sample holder vacuum storage and different partial pressure atmosphere pretreatment device according to claim 1, characterized in that: The vacuum system includes vacuum equipment such as a mechanical pump and a molecular pump and connecting pipelines.