Inert atmosphere transfer transmission electron microscope sample rod based on magnetic sealing

Abstract

The invention relates to an inert atmosphere transfer transmission electron microscope sample rod based on magnetic sealing. The inert atmosphere transfer transmission electron microscope sample rod comprises a handle with a first cavity; the outer rod is connected with the handheld handle and is provided with a second cavity in the axial direction, and the second cavity is communicated with the first cavity; the inner core is arranged in the second cavity in a sliding manner; the sample carrying table and the inner magnetic piece are respectively arranged at the front end and the rear end of the inner core, the inner magnetic piece is arranged in the first cavity, and the sample carrying table is used for placing a tested sample; the outer magnetic piece can move along the outside of the handle and generates magnetic attraction force with the inner magnetic piece; and when the sample carrying table slides along with the inner core and extends into the second cavity, the front end of the sample carrying table can be in sealed contact with the front end of the outer rod, so that the first cavity and the second cavity form a sealed environment. Compared with the prior art, the device integrates sample loading, precise magnetic expansion and contraction and comprehensive sealing, realizes stable transfer and instant microscopic analysis of a sample from a sample preparation state to a completely sealed state, and is particularly suitable for controllable atmosphere operation of a high-activity sample.

Description

Technical Field

[0001] The invention belongs to the technical field of transmission electron microscope accessories and relates to an inert atmosphere transfer transmission electron microscope sample rod based on magnetic sealing. Background Art

[0002] With its excellent characterization ability, the transmission electron microscope has shown a wide range of application prospects in many disciplines such as materials science, biology, physics, chemistry and semiconductors. At the same time, it plays an irreplaceable key role in the research process of these fields, providing strong technical support for in-depth exploration and discovery. The transmission electron microscope sample holder is an important part of the transmission electron microscope and also the medium for delivering samples to the inside of the electron microscope. Many scientific researchers are committed to the innovative research and development of the sample holder, and have successfully integrated a variety of in-situ functional units on it, such as advanced technologies such as electricity, thermoelectric coupling and electro-hydraulic coupling. The realization of these functions is cleverly designed in the internal environment of the electron microscope. These in-situ functions are all carried out in the internal environment of the electron microscope, and the protection of the sample before entering the electron microscope is not considered. However, the current design focus is mostly on the operating environment inside the electron microscope, and the protection measures required for the sample before passing through the electron microscope are still insufficient. Especially for samples with high reactivity, if timely and effective protection measures are not taken before entering the electron microscope, the accuracy and reliability of the characterization results will be significantly affected.

[0003] In the field of energy materials, for key active substances such as lithium, when exploring their battery performance under diversified electrolyte and positive electrode material systems, in-depth analysis of the surface chemical evolution and electrochemical mechanism differences of these materials during the electrochemical reaction process is the key to promoting technological progress. This process requires us to take highly rigorous protective measures in the material characterization process to ensure that a solid and reliable "structure-activity relationship" is established between the material structure and performance. This is particularly urgent for the development of a high-efficiency sealed sample stage. This sample stage must have excellent sealing performance and be able to achieve seamless connection between sample transfer, fine preparation and high-precision electron microscopy characterization, thereby minimizing the interference of the external environment on the sample, ensuring the original state and authenticity of the sample during the test process, and then providing a solid data foundation for the accurate interpretation of material performance. However, the current transmission electron microscope sample rods are difficult to meet the above requirements, and the present invention is formally proposed based on this. Summary of the invention

[0004] The purpose of the present invention is to provide an inert atmosphere transfer transmission electron microscope sample rod based on magnetic sealing, which can achieve seamless connection between sample transfer, preparation and electron microscope characterization, fully guarantee the originality and authenticity of the sample to be tested during the test characterization process, and ensure the true "structure-activity relationship" between the characterization data and the material structure.

[0005] The purpose of the present invention can be achieved by the following technical solutions:

[0006] An inert atmosphere transfer transmission electron microscope sample holder based on magnetic sealing, comprising:

[0007] a hand grip having a first cavity;

[0008] An outer rod connected to the hand grip and having a second cavity along the axial direction, wherein the second cavity is connected to the first cavity;

[0009] an inner core slidably disposed in the second cavity;

[0010] A sample carrier and an inner magnetic component respectively mounted on the front and rear ends of the inner core, the inner magnetic component is placed in the first cavity, and the sample carrier is used to place the sample to be tested;

[0011] and an outer magnetic member capable of moving along the outside of the hand grip and generating magnetic attraction with the inner magnetic member;

[0012] When the sample carrier slides along with the inner core and extends into the second cavity, the front end of the sample carrier can be in sealing contact with the front end of the outer rod, so that the first cavity and the second cavity form a sealed environment.

[0013] Furthermore, the first cavity is opened at one end away from the outer rod, and a detachable tail gland is provided at the opening for sealing.

[0014] Furthermore, the outer rod includes a thick end and a thin end that are connected together, the thick end of the outer rod is connected to the hand handle, and the sample carrier is installed on the thin end of the outer rod. A first sealing member is also provided at the junction of the thick end of the outer rod and the thin end of the outer rod. The first sealing member is configured as follows: when the thin end of the outer rod is extended into the transmission electron microscope, the opening for the thin end of the outer rod to be extended is sealed by the first sealing member.

[0015] Furthermore, a positioning pin for cooperating with a transmission electron microscope is vertically provided at the thin end of the outer rod.

[0016] Furthermore, the sample carrier is also provided with a sample pressing sheet for fixing the sample to be tested.

[0017] Furthermore, a second sealing member is provided at the front end of the sample carrier for sealing with the front end of the outer rod.

[0018] Furthermore, the surface of the inner core is provided with a plurality of grooves along the axial direction.

[0019] Furthermore, the external magnetic member includes an external magnetic ring and a plurality of external magnets mounted on the external magnetic ring, the outer edges of all the external magnets together form a circle, and the external magnetic ring is slidably sleeved on the hand grip;

[0020] The inner magnetic component comprises an inner magnetic ring and a plurality of inner magnets mounted on the inner magnetic ring, the outer edges of all the inner magnets together form a circle, and the inner magnetic ring is fixedly connected to the inner core.

[0021] Furthermore, the material of the outer magnet and the inner magnet is any one of rare earth permanent magnet, samarium cobalt permanent magnet, aluminum nickel cobalt permanent magnet, and ferrite permanent magnet material, and the magnetization direction is along the radial direction of the circle.

[0022] Furthermore, the external magnetic member is slidably matched with the outer wall surface of the hand grip via a slide rail structure;

[0023] The inner magnetic component is slidably matched with the inner wall surface of the first cavity in the hand grip via a slide rail structure.

[0024] Compared with the prior art, the present invention has the following advantages:

[0025] (1) The sample holder can be directly used with a focused ion beam electron microscope for sample preparation. The sample does not need to be converted in the middle and can be seamlessly connected to a transmission electron microscope for microscopic characterization.

[0026] (2) The magnetic telescopic system of the present invention operates in a vacuum and does not have any risk of airtightness leakage, and the sealing effect of the sample rod is better. BRIEF DESCRIPTION OF THE DRAWINGS

[0027] Figure 1 The overall structure diagram of the magnetically sealed inert atmosphere transfer transmission electron microscope sample holder;

[0028] Figure 2 It is an enlarged schematic diagram of the front end of the sample rod;

[0029] Figure 3 is a cross-sectional schematic diagram of the tail end of the sample rod;

[0030] Figure 4 It is a schematic diagram of the structure of the inner magnetic part;

[0031] Figure 5 is a cross-sectional schematic diagram of an inner magnetic component;

[0032] Figure 6 It is a schematic diagram of the structure of the external magnetic component;

[0033] Figure 7 is a cross-sectional schematic diagram of an external magnetic component;

[0034] Figure 8 is a schematic diagram of a sample rod of the present invention in a sealing mode;

[0035] Description of the markings in the figure:

[0036] 1-sample carrier, 2-thin end of outer rod, 3-thick end of outer rod, 4-hand grip, 5-tail pressure cover, 6-outer magnetic ring, 7-trigger pin, 8-first seal, 9-positioning pin, 10-second seal, 11-outer magnet, 12-inner core, 13-inner magnetic ring, 14-third seal, 15-inner magnet, 16-sample press. DETAILED DESCRIPTION

[0037] The present invention is described in detail below in conjunction with the accompanying drawings and specific embodiments. This embodiment is implemented based on the technical solution of the present invention, and provides a detailed implementation method and specific operation process, but the protection scope of the present invention is not limited to the following embodiments.

[0038] In the following implementation manners or examples, unless otherwise specified, functional components or structures are conventional components or conventional structures used in the art to achieve corresponding functions.

[0039] In order to achieve seamless connection between sample transfer, preparation and electron microscope characterization, fully guarantee the originality and authenticity of the sample to be tested during the test characterization process, and ensure the true "structure-activity relationship" between the characterization data and the material structure, the present invention provides an inert atmosphere transfer transmission electron microscope sample rod based on magnetic sealing, the structure of which can be seen in Figure 1 As shown in the following, including:

[0040] A hand grip 4 having a first cavity;

[0041] An outer rod connected to the hand grip 4 and having a second cavity along the axial direction, wherein the second cavity is connected to the first cavity;

[0042] An inner core 12 slidably disposed in the second cavity;

[0043] A sample carrier 1 and an internal magnetic component respectively mounted on the front and rear ends of the inner core 12, wherein the internal magnetic component is placed in the first cavity, and the sample carrier 1 is used to place the sample to be tested;

[0044] and an outer magnetic part capable of moving along the outside of the hand grip 4 and generating magnetic attraction with the inner magnetic part;

[0045] When the sample carrier 1 slides along with the inner core 12 and extends into the second cavity, the front end of the sample carrier 1 can be in sealing contact with the front end of the outer rod, so that the first cavity and the second cavity form a sealed environment.

[0046] In some specific embodiments, the first cavity is opened at one end away from the outer rod, and a detachable tail gland 5 is provided at the opening for sealing. Exemplarily, the tail gland 5 can improve the sealing effect of the opening of the first cavity by means of a third sealing member 14. In addition, in some embodiments, an openable and closable air injection hole can be further provided on the tail gland 5, through which the inert atmosphere in the first cavity and the second cavity can be flexibly adjusted.

[0047] In some specific embodiments, the outer rod includes an outer rod thick end 3 and an outer rod thin end 2 which are connected as one body, the outer rod thick end 3 is connected to the hand grip 4, the sample carrier 1 is mounted on the outer rod thin end 2, and a first seal is also provided at the junction of the outer rod thick end 3 and the outer rod thin end 2, and the first seal is configured as follows: when the outer rod thin end 2 extends into the transmission electron microscope, the first seal seals the opening for the outer rod thin end 2 to extend into. It should be pointed out here that "thick" and "thin" are only used to distinguish the two sections of the outer rod by the rod diameter, and do not actually limit the specific size of the two sections of the outer rod. By setting the first seal, the closed environment inside the electron microscope can be ensured during the subsequent electron microscope characterization process.

[0048] In a more specific embodiment, the thin end 2 of the outer rod is also vertically provided with a positioning pin 9 for cooperating with a transmission electron microscope. The positioning pin 9 here is for cooperating with other electron microscope components to perform specific electron microscope scanning characterization, etc.

[0049] In some specific embodiments, the front edge of the hand grip 4 is further provided with a trigger pin 7. During the transfer process, when the sample to be tested is transferred to the inside of the electron microscope for electron microscope characterization, the trigger pin 7 will synchronously trigger the start button on the electron microscope device as the sample rod moves to adjust the characterization environment inside the electron microscope.

[0050] In some specific embodiments, the sample carrier 1 is further provided with a sample pressing sheet 16 for fixing the sample to be tested.

[0051] In some specific embodiments, the front end of the sample carrier 1 is provided with a second sealing member 10 for sealing with the front end of the outer rod.

[0052] In some specific embodiments, the surface of the inner core 12 is further provided with a plurality of grooves along the axial direction, which can cooperate with rapid air extraction to prevent the inert gas from being retained in the interlayer space between the inner and outer rods.

[0053] In some specific embodiments, the external magnetic member includes an external magnetic ring 6 and a plurality of external magnets 11 mounted on the external magnetic ring 6, the outer edges of all the external magnets 11 together form a circle, and the external magnetic ring 6 is slidably mounted on the hand grip 4;

[0054] The inner magnetic component includes an inner magnetic ring 13 and a plurality of inner magnets 15 mounted on the inner magnetic ring 13 . The outer edges of all the inner magnets 15 together form a circle. The inner magnetic ring 13 is fixedly connected to the inner core 12 .

[0055] In a more specific embodiment, the material of the outer magnet 11 and the inner magnet 15 is any one of rare earth permanent magnet, samarium cobalt permanent magnet, aluminum nickel cobalt permanent magnet, and ferrite permanent magnet material, and the magnetization direction is along the radial direction of the circle. When installed, the magnetization directions of adjacent magnets (i.e., two adjacent inner magnets and two adjacent outer magnets) are opposite to ensure the best magnetic force distribution. The magnetic force distribution setting here does not belong to the innovation of the present invention and will not be repeated here.

[0056] In some specific embodiments, the external magnetic member and the outer wall of the hand grip 4 are slidably matched via a slide rail structure;

[0057] The inner magnetic component and the inner wall surface of the first cavity in the handle 4 are slidably matched via a slide rail structure.

[0058] The above embodiments may be implemented individually or in any combination of two or more.

[0059] The above implementation is described in more detail below in conjunction with specific examples.

[0060] Embodiment 1:

[0061] In order to achieve seamless connection between sample transfer, preparation and electron microscope characterization, fully guarantee the originality and authenticity of the sample to be tested during the test characterization process, and ensure the true "structure-activity relationship" between the characterization data and the material structure, this embodiment provides an inert atmosphere transfer transmission electron microscope sample rod based on magnetic sealing, the structure of which can be seen in Figure 1 As shown in the following, including:

[0062] A hand grip 4 having a first cavity;

[0063] An outer rod connected to the hand grip 4 and having a second cavity along the axial direction, wherein the second cavity is connected to the first cavity;

[0064] An inner core 12 slidably disposed in the second cavity;

[0065] A sample carrier 1 and an internal magnetic component respectively mounted on the front and rear ends of the inner core 12, wherein the internal magnetic component is placed in the first cavity, and the sample carrier 1 is used to place the sample to be tested;

[0066] and an outer magnetic part capable of moving along the outside of the hand grip 4 and generating magnetic attraction with the inner magnetic part;

[0067] When the sample carrier 1 slides along with the inner core 12 and extends into the second cavity, the front end of the sample carrier 1 can be in sealing contact with the front end of the outer rod, so that the first cavity and the second cavity form a sealed environment.

[0068] The first cavity is open at one end away from the outer rod, and a detachable tail gland 5 is provided at the opening for sealing. Exemplarily, the tail gland 5 can improve the sealing effect of the opening of the first cavity by means of a third sealing member 14. In addition, in some embodiments, an openable and closable air injection hole can be further provided on the tail gland 5, through which the inert atmosphere in the first cavity and the second cavity can be flexibly adjusted.

[0069] The outer rod comprises an outer rod thick end 3 and an outer rod thin end 2 which are connected as one body, the outer rod thick end 3 is connected to the hand grip 4, the sample carrier 1 is mounted on the outer rod thin end 2, and a first seal is also provided at the junction of the outer rod thick end 3 and the outer rod thin end 2, and the first seal is configured as follows: when the outer rod thin end 2 extends into the transmission electron microscope, the first seal seals the opening for the outer rod thin end 2 to extend into. It should be pointed out here that "thick" and "thin" are only used to distinguish the two sections of the outer rod by the rod diameter, and do not actually limit the specific size of the two sections of the outer rod. By setting the first seal, the closed environment inside the electron microscope can be ensured in the subsequent electron microscope characterization process.

[0070] The thin end 2 of the outer rod is also vertically provided with a positioning pin 9 for cooperating with a transmission electron microscope. The positioning pin 9 here is for cooperating with other electron microscope components to perform specific electron microscope scanning characterization, etc.

[0071] The front edge of the hand grip 4 is also provided with a trigger pin 7. During the transfer process, when the sample is transferred to the inside of the electron microscope for electron microscope characterization, the trigger pin 7 will synchronously trigger the start button on the electron microscope device as the sample rod moves to adjust the characterization environment inside the electron microscope.

[0072] The sample carrier 1 is also provided with a sample pressing sheet 16 for fixing the sample to be tested.

[0073] The front end of the sample carrier 1 is provided with a second sealing member 10 for sealing with the front end of the outer rod.

[0074] The surface of the inner core 12 is also provided with a plurality of grooves along the axial direction, which can cooperate with rapid air extraction to prevent the inert gas from being retained in the interlayer space between the inner and outer rods.

[0075] The external magnetic member includes an external magnetic ring 6 and a plurality of external magnets 11 mounted on the external magnetic ring 6, the outer edges of all the external magnets 11 together form a circle, and the external magnetic ring 6 is slidably mounted on the hand grip 4;

[0076] The inner magnetic component includes an inner magnetic ring 13 and a plurality of inner magnets 15 mounted on the inner magnetic ring 13 . The outer edges of all the inner magnets 15 together form a circle. The inner magnetic ring 13 is fixedly connected to the inner core 12 .

[0077] The material of the outer magnet 11 and the inner magnet 15 is any one of rare earth permanent magnet, samarium cobalt permanent magnet, aluminum nickel cobalt permanent magnet, and ferrite permanent magnet material, and the magnetization direction is along the radial direction of the circle. When installed, the magnetization directions of adjacent magnets are opposite to ensure the best magnetic force distribution. The magnetic force distribution setting here does not belong to the innovation of the present invention and will not be repeated here.

[0078] The outer magnetic component and the outer wall surface of the handle 4 are slidably matched through a slide rail structure; the inner magnetic component and the inner wall surface of the first cavity in the handle 4 are slidably matched through a slide rail structure.

[0079] The working principle of the sample rod of this embodiment is as follows: the outer magnetic part slides back and forth on the hand grip 4, driving the inner magnetic part that attracts it to move in the first cavity, thereby driving the inner core 12 to slide and retract, thereby realizing the conversion of the sample rod sealing and microscopic analysis mode. The sealing of the sample rod is mainly completed by the first seal, the second seal 10, and the third seal 14, including the sealing of the internal space of the rod body and the sealing of the sample rod and the electron microscope, wherein the sealing of the internal space of the sample rod itself is completed by the second seal 10 and the third seal 14, the former forms a seal by contacting with the end of the thin end 2 of the outer rod, and the latter is formed by extrusion between the tail gland 5 and the hand grip 4, and finally, the entire outer rod between the second seal 10 and the third seal 14 and the first cavity and the second cavity of the hand grip 4 form a sealed space. The sealing effect with the electron microscope is formed by the first seal outside the sample rod body and the electron microscope contacting each other. In this embodiment, the first seal, the second seal 10, and the third seal 14 can independently select different sealing rings, or other sealing elements can be selected.

[0080] The magnetic telescopic system constructed by the sample rod, which is composed of an external magnetic part, an internal magnetic part, the above-mentioned sealing structure, etc., realizes remote, non-contact telescoping of the inner core 12 without destroying the sealing, thereby realizing seamless switching between the sealing protection state and the microscopic analysis mode.

[0081] In general, the present invention adopts magnetically driven sealing technology and is designed for TEM accessories and nanomaterial microscopic characterization research. The sample rod integrates a sample loading device, a precise magnetic telescopic system and a comprehensive sealing system, which realizes the stable transfer of samples from sample preparation to a completely sealed state and instant microscopic analysis, and is particularly suitable for controlled atmosphere operation of highly active samples. This invention ensures the authenticity and reliability of the state stability and structure-performance relationship of the sample during the entire research process by constructing a "seamless" connection process from the sample to the electron microscope and subsequent characterization and performance testing.

[0082] The above description of the embodiments is to facilitate the understanding and use of the invention by those skilled in the art. It is obvious that those skilled in the art can easily make various modifications to these embodiments and apply the general principles described herein to other embodiments without creative work. Therefore, the present invention is not limited to the above embodiments, and improvements and modifications made by those skilled in the art based on the disclosure of the present invention without departing from the scope of the present invention should be within the scope of protection of the present invention.

Claims

1. An inert atmosphere transfer transmission electron microscope sample holder based on magnetic sealing, characterized in that: include: a hand grip having a first cavity; An outer rod connected to the hand grip and having a second cavity along the axial direction, wherein the second cavity is connected to the first cavity; An inner core slidably disposed in the second cavity; A sample carrier and an inner magnetic component respectively mounted on the front and rear ends of the inner core, the inner magnetic component is placed in the first cavity, and the sample carrier is used to place the sample to be tested; and an outer magnetic member capable of moving along the outside of the hand grip and generating magnetic attraction with the inner magnetic member; When the sample carrier slides along with the inner core and extends into the second cavity, the front end of the sample carrier can be in sealing contact with the front end of the outer rod, so that the first cavity and the second cavity form a sealed environment.

2. The inert atmosphere transfer transmission electron microscope sample holder based on magnetic sealing according to claim 1, characterized in that: The first cavity is opened at one end away from the outer rod, and a detachable tail gland is provided at the opening for sealing.

3. The inert atmosphere transfer transmission electron microscope sample holder based on magnetic sealing according to claim 1, characterized in that: The outer rod includes an outer rod thick end and an outer rod thin end which are connected as one body, the outer rod thick end is connected to the hand grip, the sample carrier is mounted on the outer rod thin end, and a first sealing member is provided at the junction of the outer rod thick end and the outer rod thin end, and the first sealing member is configured as follows: when the outer rod thin end is extended into the transmission electron microscope, the opening for the outer rod thin end to be extended is sealed by the first sealing member.

4. The inert atmosphere transfer transmission electron microscope sample holder based on magnetic sealing according to claim 3, characterized in that: The thin end of the outer rod is also vertically provided with a positioning pin for matching with a transmission electron microscope.

5. The inert atmosphere transfer transmission electron microscope sample holder based on magnetic sealing according to claim 1, characterized in that: The sample carrier is also provided with a sample pressing sheet for fixing the sample to be tested.

6. The inert atmosphere transfer transmission electron microscope sample holder based on magnetic sealing according to claim 1, characterized in that: The front end of the sample carrier is provided with a second sealing member for sealing with the front end of the outer rod.

7. The inert atmosphere transfer transmission electron microscope sample holder based on magnetic sealing according to claim 1, characterized in that: The surface of the inner core is also provided with a plurality of grooves along the axial direction.

8. The inert atmosphere transfer transmission electron microscope sample holder based on magnetic sealing according to claim 1, characterized in that: The external magnetic member comprises an external magnetic ring and a plurality of external magnets mounted on the external magnetic ring, the outer edges of all the external magnets together form a circle, and the external magnetic ring is slidably sleeved on the hand grip; The inner magnetic component comprises an inner magnetic ring and a plurality of inner magnets mounted on the inner magnetic ring, the outer edges of all the inner magnets together form a circle, and the inner magnetic ring is fixedly connected to the inner core.

9. The inert atmosphere transfer transmission electron microscope sample holder based on magnetic sealing according to claim 8, characterized in that: The material of the outer magnet and the inner magnet is any one of rare earth permanent magnet, samarium cobalt permanent magnet, aluminum nickel cobalt permanent magnet and ferrite permanent magnet, and the magnetization direction is along the radial direction of the circle.

10. The inert atmosphere transfer transmission electron microscope sample holder based on magnetic sealing according to claim 1, characterized in that: A trigger pin is also provided at the front edge of the hand grip.

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