An in-situ cryo-laser irradiation system with pluggable optical fibers for use in a transmission electron microscope

Abstract

This invention relates to an in-situ cryogenic laser irradiation system for transmission electron microscopes (TEM) with pluggable optical fibers. The system includes a sample rod housing a nanoscale fiber optic controller; a sample stage located at the front of the sample rod for holding a specially designed electron microscope grid, secured with paraffin wax; a liquid nitrogen chamber located at the end of the sample rod, through which liquid nitrogen is injected; and an optical fiber slot placed within the hollow liquid nitrogen chamber and sample rod; a vacuum pump, which can be connected to the system for pre-experiment preparation; a control system connected to the sample rod via a communication cable for controlling fiber movement; a laser emitting laser light, which is transmitted via optical fiber to the sample in the slot; a vacuum pump connected to the liquid nitrogen chamber; and an electron microscope providing the experimental platform for the sample rod. This invention utilizes a unique design to integrate an in-situ sample rod that simultaneously provides a cryogenic environment and laser irradiation, enabling in-situ experiments related to cryogenic laser irradiation after placement within a TEM.

Description

Technical Field

[0001] This invention relates to the field of in-situ experiments in electron microscopy, and in particular to an in-situ cryo-laser irradiation technique for use in transmission electron microscopes with pluggable optical fibers. Background Technology

[0002] In transmission electron microscopy, pluggable optical fibers require in-situ cryo-laser irradiation, and currently no system can achieve this function. Summary of the Invention

[0003] The purpose of this invention is to provide an in-situ cryo-laser irradiation system for transmission electron microscopes with pluggable optical fibers.

[0004] This invention achieves the above objective through the following technical solution: an in-situ cryo-laser irradiation system for use in a transmission electron microscope with pluggable and pluggable optical fibers, comprising:

[0005] The sample stage is located at the front end of the sample rod, and the sample groove is located at the front end of the sample stage for placing the transmission electron microscope grid. The rubber hose converges at the sample stage, and the optical fiber groove passes through the sample stage and terminates at the sample groove.

[0006] The sample rod body contains a spherical controller.

[0007] A liquid nitrogen chamber is located at the end of the sample rod, a detachable sealing head is located at the front end of the liquid nitrogen chamber, and a motor controller is located in the hollow cavity of the liquid nitrogen chamber. An optical fiber enters the sample rod through the optical fiber groove and leads to the sample groove. A liquid nitrogen layer is located inside the liquid nitrogen chamber to store liquid nitrogen. A thermal insulation layer is widely provided on the inner surface of the liquid nitrogen chamber and the sample rod body. A liquid nitrogen chamber head is located on the surface of the liquid nitrogen chamber to deliver liquid nitrogen into the liquid nitrogen chamber and to relieve internal pressure.

[0008] A control system, connected to the sample rod via a communication cable, controls the movement of the optical fiber;

[0009] A laser that emits laser light, which is transmitted via optical fiber to the sample in the sample slot;

[0010] A vacuum pump, which is connected to the liquid nitrogen chamber;

[0011] An electron microscope that provides a sample rod experimental platform.

[0012] Furthermore, the rubber hoses in the sample stage converge at the end and conduct heat to the sample slot through a copper plate, while the optical fiber slot passes through a relatively far distance above it and terminates at the sample slot. The rubber hoses and the optical fiber slots are far apart and separated, so they have little mutual influence.

[0013] Furthermore, the sample rod is equipped with a free spherical controller to control the movement of the optical fiber at the micrometer level. Combined with piezoelectric control, it can move the optical fiber with nanometer-level precision.

[0014] Furthermore, the liquid nitrogen chamber has a detachable sealing head, and the hollow chamber contains fiber optic channels and a motor controller, allowing for comprehensive inspection during preparation.

[0015] An in-situ cryo-laser irradiation method for pluggable optical fibers in a transmission electron microscope includes the following steps:

[0016] S1. Pretreatment: The empty liquid nitrogen chamber is evacuated to 100°C using a vacuum pump. -5 For vacuum chambers below 10 Pa, dry and clean the chamber; when using, disconnect the vacuum pump and wait for the vacuum to rise to 10 Pa. 3 Pa, separates the vacuum pump;

[0017] S2. Connect the sample rod and the liquid nitrogen chamber, and insert the optical fiber into the sample rod along the fiber groove.

[0018] S3. Couple the optical fiber to the laser;

[0019] S4. Place the carrier mesh into the sample cell and fix it with paraffin wax;

[0020] S5. Insert the sample rod into the electron microscope;

[0021] S6. After the vacuum level of the electron microscope reaches the standard, liquid nitrogen is introduced through the opening of the liquid nitrogen chamber using a funnel. After the liquid nitrogen is filled, a rubber hose is connected for decompression.

[0022] S7. After the vacuum level of the electron microscope reaches the standard, the experiment will be carried out.

[0023] S8. After the experiment, when pulling out the sample rod, first tilt it and pull it out after the liquid nitrogen has drained.

[0024] S9. Separate the liquid nitrogen chamber from the sample rod, and connect the liquid nitrogen layer to a vacuum pump for vacuum preservation.

[0025] Compared with the prior art, the advantages of the in-situ cryo-laser irradiation system with pluggable optical fibers in a transmission electron microscope of the present invention are:

[0026] 1. Place both the rubber tubing containing liquid nitrogen and the fiber optic slot containing optical fibers inside the sample rod.

[0027] 2. The sample rod and liquid nitrogen chamber can be separated, which facilitates vacuum preparation;

[0028] 3. By simultaneously using a motor controller and a ball controller, combined with piezoelectric technology, nanometer-level control of optical fibers can be achieved. Attached Figure Description

[0029] Figure 1 This is a schematic diagram of the structure of the present invention.

[0030] Figure 2 yes Figure 1 One of the detailed images of a part.

[0031] Figure 3 yes Figure 1 Part 2 of the detailed images.

[0032] Figure 4 yes Figure 1 The third detailed view. Detailed Implementation

[0033] like Figure 1 The in-situ cryo-laser irradiation system with pluggable fiber optic cable shown in the transmission electron microscope includes: a sample stage 1, a sample rod body 2, a liquid nitrogen chamber 3, a control system 4, a laser 5, a vacuum pump 6, and an electron microscope 7. The sample stage 1 and the sample rod body 2 constitute the sample rod.

[0034] A sample stage 1 is located at the front end of the sample rod, and a sample groove 101 is provided at the front end of the sample stage for placing the transmission electron microscope (TEM) grid. A rubber hose 102 converges at the sample stage. An optical fiber groove 103 passes through the sample stage and terminates in the sample groove; a spherical controller 201 is located inside the sample rod body 2; a liquid nitrogen chamber 3 is located at the end of the sample rod. A detachable sealing head 301 is provided at the front end of the liquid nitrogen chamber 3, and a motor controller 302 is located within the cavity of the liquid nitrogen chamber 3. An optical fiber 303 enters the sample rod through the optical fiber groove 103 and leads to the sample groove 101. A liquid nitrogen layer 304 is located inside the liquid nitrogen chamber for storing liquid nitrogen. An insulation layer 305 is widely distributed on the inner surfaces of the liquid nitrogen chamber and the sample rod body. The liquid nitrogen head 306 is located on the surface of the liquid nitrogen tank and is used to transport liquid nitrogen into the liquid nitrogen tank and relieve internal pressure; the control system 4 is connected to the sample rod via a communication cable and controls the movement of the optical fiber, etc.; the laser 5 emits a laser, which is transmitted through the optical fiber to the sample on the sample tank 101; the vacuum pump 6 is connected to the liquid nitrogen tank 3; and the electron microscope 7 provides an experimental platform for the sample rod.

[0035] An in-situ cryo-laser irradiation method for pluggable optical fibers in transmission electron microscopy includes the following steps: pretreatment, in which the empty liquid nitrogen chamber 3 is evacuated to 10°C using a vacuum pump 6 (model: Edwards-E2M18). -5 Dry and clean the chamber when the pressure is below 10 Pa. Before use, disconnect vacuum pump 6 and wait for the vacuum to rise to 10 Pa. 3Disconnect vacuum pump 6. Connect sample rod and liquid nitrogen tank 3, and insert optical fiber 303 into sample rod along optical fiber groove 103. Couple optical fiber to laser 5. Place the grid into sample tank 101 and fix it with paraffin wax; insert sample rod into electron microscope 7. After the vacuum degree of electron microscope reaches the standard, introduce liquid nitrogen through liquid nitrogen tank head 306 using a funnel. After liquid nitrogen is filled, connect rubber hose 102 for decompression. After the vacuum degree of electron microscope 7 reaches the standard, conduct the experiment. After the experiment, when removing the sample rod, first tilt it, and after the liquid nitrogen has drained, pull out the sample rod. Separate liquid nitrogen tank 3 from sample rod, and connect liquid nitrogen tank 3 to vacuum pump 6 for vacuum preservation.

[0036] This invention utilizes a special design to integrate an in-situ sample holder that simultaneously provides a low-temperature environment and laser irradiation. After being placed in a transmission electron microscope, it enables in-situ experiments related to laser irradiation under freezing conditions.

[0037] The foregoing has shown and described the basic principles, main features, and advantages of the present invention. It will be apparent to those skilled in the art that the present invention is not limited to the details of the exemplary embodiments described above, and that the invention can be implemented in other specific forms without departing from its spirit or essential characteristics. Therefore, the embodiments should be considered illustrative and non-limiting in all respects, and the scope of the invention is defined by the appended claims rather than the foregoing description. Thus, all variations falling within the meaning and scope of equivalents of the claims are intended to be included within the present invention. No reference numerals in the claims should be construed as limiting the scope of the claims.

[0038] Furthermore, it should be understood that although this specification describes embodiments, not every embodiment contains only one independent technical solution. This narrative style is merely for clarity. Those skilled in the art should consider the specification as a whole, and the technical solutions in each embodiment can also be appropriately combined to form other embodiments that can be understood by those skilled in the art.

Claims

1. An in-situ cryo-laser irradiation system for use in a transmission electron microscope with pluggable optical fibers, characterized in that, include: The sample stage (1) is located at the front end of the sample rod. The sample stage (1) includes a sample groove (101), a rubber hose (102), and an optical fiber groove (103). The sample groove (101) is located at the front end of the sample stage and is used to place the transmission electron microscope grid. The rubber hose (102) converges at the sample stage. The optical fiber groove (103) passes through the sample stage and terminates at the sample groove. The sample rod body (2) and the spherical controller (201) are located inside the sample rod body; Liquid nitrogen chamber (3), the liquid nitrogen chamber (3) is located at the end of the sample rod, the detachable sealing head (301) is located at the front end of the liquid nitrogen chamber, and the motor controller (302) is located in the hollow cavity of the liquid nitrogen chamber. The optical fiber (303) enters the sample rod through the optical fiber groove (103) and leads to the sample groove (101); the liquid nitrogen layer (304) is located in the liquid nitrogen chamber for storing liquid nitrogen, the heat insulation layer (305) is widely located on the inner surface of the liquid nitrogen chamber and the sample rod body (2), and the liquid nitrogen chamber head (306) is located on the surface of the liquid nitrogen chamber for transporting liquid nitrogen into the liquid nitrogen chamber and relieving internal pressure; The control system (4) is connected to the sample rod via a communication cable and controls the movement of the optical fiber; Laser (5), which emits laser light, and the laser light is transmitted through an optical fiber to the sample in the sample slot (101); A vacuum pump (6) is connected to the liquid nitrogen tank (3); Electron microscope (7), which provides a sample rod experimental platform.

2. The in-situ cryo-laser irradiation system for a transmission electron microscope with pluggable optical fibers according to claim 1, characterized in that: The rubber hose (102) in the sample stage (1) converges at the end and conducts heat to the sample groove (101) through the copper sheet, while the fiber optic groove (103) passes through a relatively far distance above it and terminates at the sample groove (101). The rubber hose (102) and the fiber optic groove (103) are far apart and separated, so they have little mutual influence.

3. The in-situ cryo-laser irradiation system for pluggable optical fibers in a transmission electron microscope according to claim 1, characterized in that: The sample rod body (2) is equipped with a free spherical controller (201) to perform micron-level movement control of the optical fiber. Combined with piezoelectric control, it can perform nanometer-level precise movement of the optical fiber.

4. The in-situ cryo-laser irradiation system for pluggable optical fibers in a transmission electron microscope according to claim 1, characterized in that: The liquid nitrogen chamber (3) has a detachable sealing head (301) and a hollow chamber with an optical fiber channel (103) and a motor controller (302) for comprehensive inspection during preparation.

5. A laser irradiation method for an in-situ cryo-laser irradiation system with pluggable optical fibers in a transmission electron microscope as described in any one of claims 1-4, characterized in that, Includes the following steps: S1. Pretreatment: The empty liquid nitrogen chamber is evacuated to 100°C using a vacuum pump. -5 For vacuum chambers below 10 Pa, dry and clean the chamber; when using, disconnect the vacuum pump and wait for the vacuum to rise to 10 Pa. 3 Pa, separates the vacuum pump; S2. Connect the sample rod and the liquid nitrogen chamber, and insert the optical fiber into the sample rod along the fiber groove. S3. Couple the optical fiber to the laser; S4. Place the carrier mesh into the sample cell and fix it with paraffin wax; S5. Insert the sample rod into the electron microscope; S6. After the vacuum level of the electron microscope reaches the standard, liquid nitrogen is introduced through the opening of the liquid nitrogen chamber using a funnel. After the liquid nitrogen is filled, a rubber hose is connected for decompression. S7. After the vacuum level of the electron microscope reaches the standard, the experiment will be carried out. S8. After the experiment, when pulling out the sample rod, first tilt it and pull it out after the liquid nitrogen has drained. S9. Separate the liquid nitrogen chamber from the sample rod, and connect the liquid nitrogen layer to a vacuum pump for vacuum preservation.

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