A sealed transfer type transmission electron microscope sample holder

Abstract

The present invention discloses a transmission electron microscope sample rod for sealed transfer, which belongs to the research field of transmission electron microscope accessories and nanomaterial microscopic analysis. The transmission electron microscope sample rod of the present invention mainly includes a sample transfer device, an atmosphere pipeline system, a telescopic device and a vacuum seal ring. The sample rod can simultaneously realize the sealed transfer and microscopic analysis of transmission electron microscope samples, especially the transfer and microscopic analysis of air-sensitive samples in a controllable atmosphere (including vacuum). The electron microscope sample rod for sealed transfer provided by the present invention realizes "seamless connection" between the electron microscope and other characterization and performance evaluation devices, comprehensively protects the surface state of the sample to be tested, and ensures the reliability of the structure-activity relationship between the studied structure and performance.

Description

Technical Field

[0001] The present invention belongs to the research field of transmission electron microscope accessories and nano material microscopic analysis, and specifically relates to a transmission electron microscope sample rod with sealed transfer, which is used for the sealed transfer and in-situ microscopic analysis of transmission electron microscope samples, and realizes the transfer and in-situ microscopic analysis of electron microscope samples of air-sensitive materials in a controllable atmosphere (including vacuum). Background Art

[0002] Transmission electron microscopy has atomic resolution and chemical valence state detection capabilities. It is a key technology involving multiple disciplines such as materials, physics, and chemistry. It is widely used in many fields such as new energy materials, chemical catalysts, equipment manufacturing materials, and semiconductor information materials. Especially in the field of energy and catalysis research, with the development of spherical aberration correction technology and in-situ environmental loading technology in recent years, with the help of advanced electron microscopy technology, it has been possible to observe the atomic-scale microstructure evolution process of materials and evaluate their performance under working conditions (for example, specific temperature, gas, liquid and other environmental loads). Advanced in-situ electron microscopy technology enables people to understand the essence of energy and catalytic processes at the atomic scale, and then establish a reliable structure-activity relationship between structure and performance, thereby providing key guidance for continuously improving material performance and material utilization.

[0003] At present, the improvement and function development of the sample holder of the transmission electron microscope in the world mostly focuses on the in-situ environmental loading after the sample is sent into the electron microscope, and often ignores the protection of the sample during the transfer process to the electron microscope. In order to meet the increasingly in-depth microscopic characterization needs of energy and catalysis research, in terms of the characteristics of electron microscopy technology, in addition to a high-resolution electron microscope, a sample stage suitable for various sample types and characterization needs is also required, so that the sample to be tested can be sent into the electron microscope and maintain a high degree of stability.

[0004] As far as energy and catalytic materials are concerned, the surface state of the nanoparticles that constitute the main body of the material is crucial to the material's energy storage and catalytic activity. After the material is prepared, modified, and the reaction performance is evaluated, it is characterized by electron microscopy. The surface state of the particles in the electron microscope should be completely consistent with these test links, so as to ensure the correspondence and correlation between the microstructure and the material performance, that is, to establish a reliable "structure-activity relationship". However, during the preparation of electron microscope samples and their transfer to the electron microscope, they are inevitably exposed to the air atmosphere, resulting in oxidation, contamination and other problems. Especially for high-end electron microscope equipment, they are often installed in places far away from other preparation and evaluation equipment due to environmental requirements. The long-distance transfer of samples is more challenging. It is urgent to develop an electron microscope sample rod with vacuum and controllable protective atmosphere to achieve "seamless connection" between the electron microscope and other preparation and performance evaluation equipment, to protect the surface state of the sample to be tested in all directions, and to ensure the reliability of the established structure-activity relationship. Summary of the invention

[0005] In view of this, the present invention aims to provide a transmission electron microscope sample rod for sealed transfer, so as to achieve "seamless connection" between the electron microscope and other characterization and performance evaluation devices, comprehensively protect the structural state of the sample to be tested, and ensure the reliability of the structure-activity relationship between the structure and performance of the sample under study.

[0006] To achieve the above-mentioned purpose, the present invention provides a sealed transfer type transmission electron microscope sample holder, which can realize the sealed transfer and microscopic analysis of transmission electron microscope samples, realize the controllable atmosphere (including vacuum) transfer of electron microscope samples sensitive to air, and realize the effective conversion between the sealed transfer mode and the microscopic observation mode, and mainly includes a sample loading device, an atmosphere pipeline system and a telescopic device;

[0007] The sample loading device comprises an inner core (1) and a sample holder (14); the inner core (1) vertically penetrates the large sleeve (18) and the small sleeve (2); the sample holder (14) is located at the front end of the inner core (1); a first set of sealing rings is arranged at the front end of the sample holder (14) for sealing the front end of the sample holder (14); a second set of sealing rings is arranged at the rear end of the inner core (1) and is in contact and sealed with the small sleeve (2);

[0008] The atmosphere pipeline system (15) is arranged inside the inner core (1) and is a through hollow structure, extending from the outlet of the sealing ball valve (5) through the cavity of the inner core (1) to the through hole of the sample holder (14);

[0009] The telescopic device comprises a base (4), a large sleeve (18), and a small sleeve (2); the large sleeve (18) is connected to the inner core (1) by threaded engagement, and the sealing of the sample to be transferred is achieved by the telescoping of the inner core (1); a vacuum sealing ring (8) is provided on the outer shell of the small sleeve (2), and cooperates with the electron microscope equipment to achieve vacuum sealing of the electron microscope sample chamber in the working state.

[0010] Further, the first group of sealing rings includes 1-10 adjacent sealing rings, and the second group of sealing rings includes 1-10 adjacent sealing rings.

[0011] Furthermore, the small sleeve (2) comprises a small-diameter sleeve at the front end and a large-diameter sleeve at the rear end, and the vacuum sealing ring (8) is located at the connection between the small-diameter sleeve and the large-diameter sleeve.

[0012] Furthermore, the inner core (1) is contacted and connected with the groove on the inner surface of the large diameter of the small sleeve (2) via a guide column (19), and the guide column (19) is fixedly connected to the outer surface of the inner core (1).

[0013] Furthermore, at the threaded engagement connection, the inner surface of the large sleeve (18) is provided with an internal thread (16), and the outer surface of the inner core (1) is provided with an external thread.

[0014] Furthermore, the sealing ball valve (5) is provided with an interface connected to a gas supply pipeline, which is used to be connected to an external vacuum pump or a protective gas supply end.

[0015] Furthermore, the base (4) and the sealing ball valve (5) are fixedly connected.

[0016] Furthermore, a third group of sealing rings is provided at the contact point between the inner core (1) and the large sleeve (18) and adjacent to the end of the small sleeve (2), and the third group of sealing rings includes 1 to 10 adjacent sealing rings.

[0017] Furthermore, a positioning pin (3) perpendicular to the axis of the inner core (1) is provided on the small diameter portion of the small sleeve (2).

[0018] Furthermore, a safety valve (17) is provided.

[0019] Furthermore, the sealing ring is an O-ring, and the material is selected from any one of polyethylene, polypropylene, polyvinyl chloride, nitrile rubber, styrene rubber, silicone rubber, fluororubber, acrylic rubber, butyl rubber, and chloroprene rubber.

[0020] Furthermore, the sealing ring is made of fluororubber.

[0021] The beneficial effects of the present invention compared with the prior art are as follows:

[0022] 1. The sealed transfer type transmission electron microscope sample holder of the present invention has the ability to effectively switch between the sealed transfer and microscopic observation modes, thereby achieving a "seamless connection" between the electron microscope and other characterization and performance evaluation equipment, comprehensively protecting the surface state of the sample to be tested, and ensuring the reliability of the established structure-activity relationship.

[0023] 2. The sealed transfer type transmission electron microscope sample holder of the present invention not only provides vacuum transfer for electron microscope samples, but also realizes controllable atmosphere transfer and is compatible with functions such as in-situ environmental characterization heating. BRIEF DESCRIPTION OF THE DRAWINGS

[0024] In order to more clearly illustrate the embodiments of the present invention, the drawings related to the embodiments are briefly introduced below.

[0025] Figure 1 It is a schematic diagram of the overall structure of the transmission electron microscope sample rod of the present invention, wherein 1: inner core, 2: small sleeve, 3: positioning pin, 4: base, 5: sealing ball valve, 6: vacuum sealing ring, 7: vacuum sealing ring, 8: vacuum sealing ring, 17: safety valve, 18: large sleeve.

[0026] Figure 2 It is a schematic structural diagram of a sample carrying device of a transmission electron microscope sample rod of the present invention, wherein 6: vacuum sealing ring, 7: vacuum sealing ring, 14: sample holder.

[0027] Figure 3 1 is a schematic diagram of the atmosphere piping system of the transmission electron microscope sample holder of the present invention, wherein 15: atmosphere piping system.

[0028] Figure 4 It is a schematic diagram of the telescopic device of the transmission electron microscope sample rod of the present invention, wherein 1: inner core, 5: sealing ball valve, 16: internal thread.

[0029] Figure 5 It is a schematic diagram of the position of the vacuum sealing ring of the transmission electron microscope sample rod of the present invention, wherein 6: vacuum sealing ring, 7: vacuum sealing ring, 8: vacuum sealing ring, 9: vacuum sealing ring, 10: vacuum sealing ring, 11: vacuum sealing ring, 12: vacuum sealing ring, 19: guide column.

[0030] Figure 6 It is a schematic structural diagram of a transmission electron microscope sample rod of the present invention in a microscopic observation mode.

[0031] Figure 7 It is a schematic structural diagram of a transmission electron microscope sample rod of the present invention in a sealed transfer mode. DETAILED DESCRIPTION

[0032] The present invention is described in detail below with reference to the embodiments, but the embodiments of the present invention are not limited thereto. Obviously, the embodiments described below are only partial embodiments of the present invention. For those skilled in the art, other similar embodiments obtained without creative labor all fall within the protection scope of the present invention.

[0033] In the description of this embodiment, it should be understood that the terms "upper", "lower", "front", "back", "left", "right", "top", "bottom", "inside", "outside", "front", "back", etc. indicate orientations or positional relationships based on the orientations or positional relationships shown in the accompanying drawings. They are only for the convenience of describing the present invention and simplifying the description, and do not indicate or imply that the referred device or element must have a specific orientation, be constructed and operated in a specific orientation. Therefore, they should not be understood as limitations on the present invention.

[0034] Example 1

[0035] A sealed transfer type transmission electron microscope sample rod has an inner and outer double-layer structure, mainly comprising a sample loading device, an atmosphere pipeline system and a telescopic device; the sample loading device comprises an inner core (1) and a sample holder (14); the inner core (1) vertically penetrates a large sleeve (18) and a small sleeve (2); the sample holder (14) is located at the front end of the inner core (1); adjacent vacuum sealing rings (6) and (7) are arranged in sequence at the front end of the sample holder (14); adjacent vacuum sealing rings (9) and (10) are arranged in sequence at the rear end of the inner core (1) and are connected to the small sleeve (2). (2) contact seal; the atmosphere pipeline system (15) is arranged inside the inner core (1), presenting a through hollow structure, extending from the outlet of the sealing ball valve (5) through the cavity of the inner core (1) to the through hole of the sample holder (14); the sealing ball valve (5) is provided with an interface for connecting to a gas supply pipeline, which is used to connect to an external vacuum pump or a protective gas supply end; the telescopic device comprises a base (4), a large sleeve (18), and a small sleeve (2); the base (4) and the sealing ball valve (5) are fixedly connected, and the inner surface of the large sleeve (18) is provided with an internal thread The inner core (1) has a groove (16), the outer surface of the inner core (1) is provided with an external thread, the large sleeve (18) is connected to the inner core (1) by threaded engagement, and the sealing of the sample to be transferred is achieved by the expansion and contraction of the inner core (1). Adjacent vacuum sealing rings (11) and (12) are arranged at the contact point between the large sleeve (18) and the inner core (1) and near the end of the small sleeve (2). The small sleeve (2) includes a small diameter sleeve at the front end and a large diameter sleeve at the rear end. A vacuum sealing ring (8) is arranged at the connection between the small diameter sleeve and the large diameter sleeve, and cooperates with the electron microscope angle measuring stage to achieve a working state. The invention relates to a vacuum seal for an electron microscope sample chamber under a state; a positioning pin (3) perpendicular to the axis of an inner core (1) is provided on the small diameter portion of a small sleeve (2); the inner core (1) and the groove on the inner surface of a large diameter sleeve of the small sleeve (2) are contacted and connected via a guide column (19); the guide column (19) is fixedly connected to the outer surface of the inner core (1), thereby preventing the inner core (1) from rotating radially when the inner core (1) is axially extended or contracted; vacuum sealing rings (6), (7), (8), (9), (10), (11), and (12) are all O-type sealing rings made of fluororubber material.

[0036] The large sleeve (18) is rotated counterclockwise, the inner core (1) is retracted into the small sleeve (2), and the vacuum sealing rings (6) and (7) at the front end of the inner core (1) are pressed against the front end of the small sleeve (2) to achieve front end sealing; at the same time, the vacuum sealing rings (9) and (10) on the inner core (1) are pressed against the inner wall surface of the small sleeve (2) to form a closed space, and the closed space is connected to a vacuum pump or a protective gas cylinder through a sealing ball valve connected to the atmosphere pipeline system (15) to achieve a vacuum or atmosphere environment in the closed space, and to transfer the vacuum or atmosphere environment of the sample. At this time, the electron microscope sample rod is in a sealed transfer mode. When in the sealed transfer mode, the sealing ball valve (5) controls the inflow or outflow of gas, and the external vacuum pump maintains the vacuum state of the sealed chamber where the sample is located, or the protective gas keeps the sample in the atmosphere of the protective gas.

[0037] After the electron microscope sample rod is inserted into the electron microscope, the large sleeve (18) is rotated clockwise, and the sample holder (14) at the front section of the inner core (1) is extended outward to the working position. The vacuum sealing ring (8) arranged outside the small sleeve (2) cooperates with the electron microscope to realize the vacuum sealing of the electron microscope sample chamber in the working state. At this time, the sample rod is in the microscopic observation mode.

[0038] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention, rather than to limit it. Although the present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that they can still modify the technical solutions described in the aforementioned embodiments, or replace some or all of the technical features therein with equivalents. However, these modifications or replacements do not cause the essence of the corresponding technical solutions to deviate from the scope of the technical solutions of the embodiments of the present invention.

Claims

1. A sealed transfer type transmission electron microscope sample holder, characterized in that: It mainly includes sample loading device, atmosphere piping system and telescopic device; The sample loading device comprises an inner core (1) and a sample holder (14); the inner core (1) vertically penetrates the large sleeve (18) and the small sleeve (2); the sample holder (14) is located at the front end of the inner core (1); a first set of sealing rings is arranged at the front end of the sample holder (14) for sealing the front end of the sample holder (14); a second set of sealing rings is arranged at the rear end of the inner core (1) and is in contact and sealed with the small sleeve (2); The atmosphere pipeline system (15) is arranged inside the inner core (1) and is a through hollow structure, extending from the outlet of the sealing ball valve (5) through the cavity of the inner core (1) to the through hole on the sample holder (14); The telescopic device comprises a base (4), a large sleeve (18), and a small sleeve (2); the large sleeve (18) is connected to the inner core (1) by threaded engagement, and the sealing of the sample to be transferred is achieved by the telescoping of the inner core (1); a vacuum sealing ring (8) is arranged on the outer shell of the small sleeve (2), and cooperates with the electron microscope equipment to achieve vacuum sealing of the electron microscope sample chamber in the working state; The sealing ball valve (5) is provided with an interface connected to a gas supply pipeline, and is used to be connected to an external vacuum pump or a protective gas supply end.

2. The sealed transfer type transmission electron microscope sample holder according to claim 1, characterized in that: The small sleeve (2) comprises a small-diameter sleeve at the front end and a large-diameter sleeve at the rear end, and the vacuum sealing ring (8) is located at the connection between the small-diameter sleeve and the large-diameter sleeve.

3. The sealed transfer type transmission electron microscope sample holder according to claim 1, characterized in that: The inner core (1) is contacted and connected with the groove on the inner surface of the large diameter sleeve of the small sleeve (2) via a guide column (19), and the guide column (19) is fixedly connected with the outer surface of the inner core (1).

4. The sealed transfer type transmission electron microscope sample holder according to any one of claims 1 to 3, characterized in that: The first group of sealing rings includes 1-10 sealing rings, and the second group of sealing rings includes 1-10 sealing rings.

5. The sealed transfer type transmission electron microscope sample holder according to claim 4, characterized in that: The inner surface of the large sleeve (18) in threaded engagement connection is provided with an internal thread, and the outer surface of the inner core (1) is provided with an external thread.

6. The sealed transfer type transmission electron microscope sample holder according to claim 5, characterized in that: The base (4) and the sealing ball valve (5) are fixedly connected.

7. The sealed transfer type transmission electron microscope sample holder according to claim 6, characterized in that: A third group of sealing rings is arranged at the contact point between the inner core (1) and the large sleeve (18) and near the end of the small sleeve (2), and the third group of sealing rings includes 1 to 10 sealing rings.

8. The sealed transfer type transmission electron microscope sample holder according to claim 7, characterized in that: A positioning pin (3) which is perpendicular to the axis of the inner core (1) is provided on the small diameter sleeve of the small sleeve (2).

9. The sealed transfer type transmission electron microscope sample holder according to claim 7, characterized in that: The sealing ring is an O-type sealing ring, and the material is selected from any one of polyethylene, polypropylene, polyvinyl chloride, nitrile rubber, styrene rubber, silicone rubber, fluororubber, acrylic rubber, butyl rubber, and chloroprene rubber.

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