Sample rod for detecting sample preparation quality in in-situ atmosphere and liquid atmosphere experiment

Abstract

The utility model provides a sample rod for detecting the quality of a prepared sample in an in-situ atmosphere and liquid atmosphere experiment, which comprises a sample rod head which is provided with a first chip groove, a second chip groove, a first tabletting assembly and a second tabletting assembly, the second chip groove is located in the first chip groove, the first tablet pressing assembly is used for pressing and fixing the first chip, the second tablet pressing assembly is used for pressing and fixing the second chip, and a tested sample is dripped on the first chip or the second chip; the annular first elastic gasket is arranged in the first chip groove and annularly arranged outside the second chip groove; the second elastic cushion block is arranged in the second chip groove, and the first chip is placed on the annular first elastic gasket and then electrically connected with the second chip; the power supply electrode assembly is arranged on the sample rod head and located at the rear end of the first chip groove, the first chip is electrically connected with the power supply electrode assembly, and the power supply electrode assembly is connected to an external controller of the transmission electron microscope.

Description

Technical Field

[0001] The utility model belongs to the technical field of transmission electron microscope and nano material measurement, in particular to a sample rod for detecting the quality of sample preparation in in-situ atmosphere and liquid atmosphere experiments. Background Art

[0002] Transmission Electron Microscopy (TEM) is a high-resolution microscopy technique, a type of electron microscope (EM). It uses electron beams instead of light to image and analyze materials, and to study the microstructure and chemical composition of materials. It is an important tool in the current field of materials science research. With it, information such as the microscopic morphology, structure, and orientation of materials with a scale less than 0.2um can be obtained. The in-situ technology in transmission electron microscopy is a rapidly developing research field. Its advantage is that it can observe various structural changes and physical properties of materials and devices in real time under microscopic conditions, which is conducive to studying the macroscopic performance and use effects of materials and devices.

[0003] With the deepening of scientific research, more and more scientific researchers hope to use transmission electron microscopes to carry out in-situ or quasi-in-situ experiments in multiple fields (such as force, electricity, magnetism, heat, light, gas and liquid, etc.). Among them, the gas atmosphere has an important influence on the structure and properties of the material. For example, after hydrogen atoms enter the material, they can diffuse in the crystal lattice or be captured by defects, inducing cracks or generating hydrogen bubbles, affecting the mechanical properties of the material. In addition to surface oxidation, the effect of oxygen on material properties can also cause the material to harden and become brittle due to the intense oxygen absorption under high temperature conditions. In addition, the atmosphere and liquid atmosphere are also important factors affecting the catalytic process. Therefore, introducing gas into the transmission electron microscope and observing the interaction process between gas and solid in the in-situ environment is of great significance for understanding the gas-solid mechanism and exploring solutions to the problem.

[0004] In-situ liquid transmission electron microscopy is a scientific and technological project further developed on the basis of ordinary electron transmission microscopy. In the early days of electron microscope development, researchers tried to observe liquid samples, but because electron microscopes require a high vacuum environment, it was extremely difficult. In recent years, with the development of micro-machining technology and electron microscope technology itself, in-situ electron microscope technology using silicon nitride and graphene as liquid sample pools or window materials has made great progress. The liquid sample pool can separate the ultra-thin liquid layer from the high vacuum environment of the electron microscope, thereby ensuring that the liquid can exist stably in the electron microscope.

[0005] However, when preparing samples for in-situ gas and liquid experiments, it is generally necessary to drop a solution containing the sample on the chip. It is difficult to ensure that the prepared sample is an ideal sample, or even no sample exists, and the sample preparation process may affect the resistance of the chip. Therefore, not every prepared sample can be successfully used for in-situ experiments. At this time, it is generally necessary to change the sample, but the sample change process is cumbersome and has a long cycle, which wastes the machine time of the transmission electron microscope. Therefore, in order to further improve the efficiency of in-situ gas and liquid experiments, multiple samples can be screened to ensure that the sample in the in-situ sample rod is an ideal sample each time, thereby saving the machine time of the transmission electron microscope. Utility Model Content

[0006] In view of the shortcomings of the prior art, the purpose of the utility model is to provide a sample rod for detecting the quality of sample preparation in in-situ atmosphere and liquid atmosphere experiments, so as to obtain qualified samples before conducting in-situ atmosphere and liquid atmosphere experiments, reduce the use time of high-precision electron microscopes, improve work efficiency and reduce use costs.

[0007] To achieve this purpose, the utility model adopts the following technical solutions:

[0008] A sample rod for detecting the quality of sample preparation in an in-situ atmosphere or liquid atmosphere experiment, comprising a sample rod head, wherein the sample rod head is provided with a first chip slot, a second chip slot, a first pressing sheet assembly and a second pressing sheet assembly, wherein the second chip slot is located inside the first chip slot, the first chip slot is used to place a first chip, and the second chip slot is used to place a second chip:

[0009] The first pressing assembly is used to press and fix the first chip, and the second pressing assembly is used to press and fix the second chip, and the sample to be tested is dropped on the first chip or the second chip;

[0010] an annular first elastic gasket, which is arranged in the first chip slot and is arranged outside the second chip slot, and the annular first elastic gasket is used to support the first chip;

[0011] A second elastic pad, which is disposed in the second chip slot, the second elastic pad is used to support the second chip, and the first chip is placed on the first annular elastic gasket and electrically connected to the second chip;

[0012] The power supply electrode assembly is arranged on the sample rod head and is located at the rear end of the first chip slot. The first chip is electrically connected to the power supply electrode assembly, and the power supply electrode assembly is connected to an external controller of the transmission electron microscope.

[0013] Preferably, the first annular elastic gasket is an annular silicone gasket;

[0014] The second elastic pad is a strip-shaped silicone pad.

[0015] Preferably, an observation area is arranged on the sample rod head, and the observation area is a circular area with a center of the second chip slot as the center and a radius of a first preset radius.

[0016] Preferably, the first pressing assembly includes a sample pressing piece and a fixing part, the sample pressing piece is rotatably connected to the fixing part, the fixing part is connected to the sample rod head, and the sample pressing piece can rotate around the fixing part to be quickly pressed onto or released from the first chip.

[0017] Preferably, the sample rod head is further provided with an electrode groove, and the electrode groove is located at the rear end of the first chip groove;

[0018] The power supply electrode assembly includes a power supply electrode and a cable. The power supply electrode is arranged in the electrode slot. One end of the cable is connected to the power supply electrode, and the other end of the cable is connected to the external controller.

[0019] Preferably, the second pressing sheet assembly includes a slide rail platform, a slide rail pressing sheet and a sliding member, one end of the slide rail pressing sheet is connected to the sliding member, a slide rail groove and a guide groove arranged parallel to the slide rail groove are provided on the slide rail platform, the sliding member drives the slide rail pressing sheet to slide in the slide rail groove, a guide member is provided on the slide rail pressing sheet, and the guide member is slidably arranged in the guide groove.

[0020] Preferably, the sample rod also includes a sample rod body connected to the sample rod head, the sample rod body includes a coaxially arranged front end thin rod and a rear end thick rod, the rear end thick rod and the front end thin rod are connected by a conical transition section, and a sealing ring is arranged on the conical transition section.

[0021] Preferably, the sample rod further comprises a hand gripping handle arranged on the rear end thick rod, and a lead-out port is provided at the end of the hand gripping handle, and the lead-out port can be connected to an external controller of the transmission electron microscope.

[0022] Compared with the prior art, the utility model has the following beneficial effects:

[0023] The second elastic pad is provided to prevent the second chip from contacting with the second chip slot, causing the second chip to be squeezed, and the second elastic pad cushions the second chip. Similarly, the annular first elastic gasket is arranged around the outer circumference of the first chip slot, and the first chip is placed on the annular first elastic gasket to support the second chip without contacting the first chip, thereby preventing the first chip from squeezing the second chip during the experimental detection process.

[0024] A first chip is placed in the first chip slot of the sample rod head, a second chip is placed in the second chip slot, and a sample to be tested is dropped on the first chip or the second chip.

[0025] When testing the first chip or the second chip, the first chip or the second chip needs to be installed at the same time, and the sample is only dropped on one of the chips. During the test, the first chip is placed in the first chip slot, and the first pressing assembly is used to press and fix the first chip. The second chip is placed in the second chip slot, and the second pressing assembly is used to press and fix the second chip.

[0026] After the installation is completed, the first chip and the second chip are in electrical contact, the first chip is electrically connected to the power supply electrode assembly, and the first chip, the power supply electrode assembly and the external controller form an electrical circuit to achieve electrical communication with the outside. The sample rod is inserted into the electron microscope to observe the degree of agglomeration and particle size of the sample of the first chip. After the above two parameters are qualified, the electrical transport properties, i.e. resistance, of the first chip or the second chip with the sample are further tested.

[0027] By placing the sample holder in a common electron microscope, it is possible to detect whether the samples in the first chip and the second chip are ideal samples, and confirm that the chip with the oil drop sample is an ideal sample. The chip with the qualified sample is moved into the in-situ sample holder, and the in-situ sample holder is placed in a transmission electron microscope or a spherical aberration electron microscope to perform in-situ atmosphere and liquid atmosphere experiments on the sample.

[0028] The sample rod in the utility model is used to determine in advance that the sample placed in the in-situ sample rod is an ideal sample, which reduces the time for detecting whether the sample is qualified, the time for replacing the sample with the sample rod, and the time for the sample rod to be inserted into the transmission electron microscope or the spherical aberration electron microscope and wait for vacuuming when using the transmission electron microscope or the spherical aberration electron microscope for experiments. Therefore, compared with the in-situ atmosphere and liquid atmosphere detection experiments on samples in the prior art, the technical solution in this embodiment saves the machine time of the transmission electron microscope or the spherical aberration electron microscope, greatly reduces the production cost, and further improves the efficiency of the in-situ atmosphere and liquid atmosphere experiments. BRIEF DESCRIPTION OF THE DRAWINGS

[0029] Figure 1 It is a schematic structural diagram of a first angle of a sample rod for detecting sample preparation quality in an in-situ atmosphere or liquid atmosphere experiment in the utility model;

[0030] Figure 2 It is a schematic structural diagram of the second angle of the sample rod for detecting the sample preparation quality in the in-situ atmosphere and liquid atmosphere experiments in the utility model;

[0031] Figure 3 It is a schematic diagram of the structure of the sample rod head in the utility model;

[0032] Figure 4 A top view of the sample rod head in the utility model;

[0033] Figure 5 It is a structural schematic diagram of the second tablet pressing assembly in the utility model.

[0034] Among them, 1. Hand grip; 2. Sample rod body; 3. Sample rod head; 4. First guide pin; 5. Thick rod at the rear end; 6. Conical transition section; 7. Thin rod at the front end; 8. Second guide pin; 9. Lead-out port; 10. Branch connector; 11. Built-in cable; 12. Guide groove; 13. Sealing ring; 14. Strip silicone gasket groove; 15. Second chip groove; 16. Ring silicone gasket groove; 17. First chip groove; 18. Power supply electrode; 19. Sample pressing tablet; 20. Slide table; 21. First slide groove; 22. Second slide groove; 23. Slide pressing tablet. DETAILED DESCRIPTION

[0035] In order to make the purpose, technical scheme and advantages of the embodiments of the utility model clearer, the technical scheme in the embodiments of the utility model will be clearly and completely described below in conjunction with the drawings in the embodiments of the utility model. Obviously, the described embodiments are part of the embodiments of the utility model, not all of the embodiments. Generally, the components of the embodiments of the utility model described and shown in the drawings here can be arranged and designed in various different configurations.

[0036] Therefore, the following detailed description of the embodiments of the present invention provided in the accompanying drawings is not intended to limit the scope of the present invention to be protected, but merely represents selected embodiments of the present invention. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0037] It should be noted that similar reference numerals and letters denote similar items in the following drawings, and therefore, once an item is defined in one drawing, further definition and explanation thereof is not required in subsequent drawings.

[0038] In the description of the present utility model, it should be noted that the terms "upper", "lower", "left", "right", "vertical", "horizontal", "inside", "outside", etc. indicate the orientation or position relationship based on the orientation or position relationship shown in the accompanying drawings, or the orientation or position relationship in which the utility model product is usually placed when in use. They are only for the convenience of describing the present utility model and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and therefore cannot be understood as a limitation on the present utility model. In addition, the terms "first", "second", "third", etc. are only used to distinguish the description, and cannot be understood as indicating or implying relative importance. In the description of the present utility model, unless otherwise specified, "multiple" means two or more.

[0039] In the description of the present invention, it is also necessary to explain that, unless otherwise clearly specified and limited, the terms "set" and "connection" should be understood in a broad sense, for example, it can be a fixed connection, a detachable connection, or an integral connection; it can be a mechanical connection or an electrical connection. For ordinary technicians in this field, the specific meanings of the above terms in the present invention can be understood according to specific circumstances.

[0040] In the present utility model, unless otherwise clearly specified and limited, a first feature being "above" or "below" a second feature may include that the first and second features are in direct contact, or may include that the first and second features are not in direct contact but are in contact through another feature between them. Moreover, a first feature being "above", "above" and "above" a second feature includes that the first feature is directly above and obliquely above the second feature, or simply indicates that the first feature is higher in level than the second feature. A first feature being "below", "below" and "below" a second feature includes that the first feature is directly below and obliquely below the second feature, or simply indicates that the first feature is lower in level than the second feature.

[0041] The embodiments of the present invention are described in detail below, and examples of the embodiments are shown in the accompanying drawings, wherein the same or similar reference numerals throughout represent the same or similar elements or elements having the same or similar functions. The embodiments described below with reference to the accompanying drawings are exemplary and are only used to explain the present invention, and cannot be understood as limiting the present invention.

[0042] like Figure 1-Figure 5 As shown, in this embodiment, a sample rod for detecting the quality of sample preparation in an in-situ atmosphere or liquid atmosphere experiment is provided, which includes a sample rod head 3, a sample rod body 2 and a hand grip 1, wherein the sample rod head 3 and the hand grip 1 are respectively arranged at both ends of the sample rod body 2. The sample rod head 3 is provided with a first chip slot 17, a second chip slot 15, a first pressing sheet assembly and a second pressing sheet assembly, the second chip slot 15 is located inside the first chip slot 17, the first chip slot 17 is used to place a first chip, and the second chip slot 15 is used to place a second chip.

[0043] The first pressing assembly and the second pressing assembly are both arranged on the sample rod head 3. The first pressing assembly is used to press and fix the first chip, and the second pressing assembly is used to press and fix the second chip. The sample to be tested is placed in the first chip or the second chip.

[0044] An annular first elastic gasket is arranged in the first chip slot 17 and is arranged outside the second chip slot 15. The annular first elastic gasket is used to support the first chip;

[0045] The second elastic pad is disposed in the second chip slot 15 and is used to support the second chip. The first chip is placed on the annular first elastic gasket and is electrically connected to the second chip.

[0046] The second elastic pad is provided to prevent the second chip from contacting the second chip slot 15, causing the second chip to be squeezed, and the second elastic pad cushions the second chip. Similarly, the annular first elastic gasket is arranged around the outer periphery of the first chip slot 17, and the first chip is placed on the annular first elastic gasket to support the second chip without contacting the first chip, thereby preventing the first chip from squeezing the second chip during the experimental detection process.

[0047] The power supply electrode assembly is arranged on the sample rod head 3 and is located at the rear end of the first chip slot 17. The first chip is electrically connected to the power supply electrode assembly, and the power supply electrode assembly is connected to an external controller of the transmission electron microscope.

[0048] In this embodiment, a first chip is placed in the first chip slot 17 of the sample rod head 3, and a second chip is placed in the second chip slot 15, wherein a sample to be tested is dropped on the first chip or the second chip.

[0049] When testing the sample on the first chip or the second chip, the first chip and the second chip need to be installed at the same time, and the sample is only dropped on one of the chips. During the test, the first chip is placed in the first chip slot 17, and the first pressing assembly is used to press and fix the first chip. The second chip is placed in the second chip slot 15, and the second pressing assembly is used to press and fix the second chip.

[0050] After the installation is completed, the sample is dropped on the first chip or the second chip, the first chip and the second chip are in electrical contact, and the first chip is electrically connected to the power supply electrode assembly, so that the first chip, the power supply electrode assembly and the external controller form an electrical circuit to achieve electrical connection with the outside. The sample rod is inserted into the electron microscope to observe the degree of agglomeration and particle size of the sample in the first chip or the second chip. After the above two parameters are qualified, the electrical transport properties of the first chip or the second chip with the sample dropped, that is, the resistance, are further detected.

[0051] By placing the sample holder in a common electron microscope, it is possible to detect whether the samples in the first chip and the second chip are ideal samples, and confirm that the chip with the oil drop sample is an ideal sample. The chip with the qualified sample is moved into the in-situ sample holder, and the in-situ sample holder is placed in a transmission electron microscope or a spherical aberration electron microscope to perform in-situ atmosphere and liquid atmosphere experiments on the sample.

[0052] The sample rod in this embodiment is used to determine in advance that the sample placed in the in-situ sample rod is an ideal sample, which reduces the time for detecting whether the sample is qualified when using a transmission electron microscope or a spherical aberration electron microscope experiment, the time for the sample rod to replace the sample, and the time for the sample rod to be inserted into the transmission electron microscope or the spherical aberration electron microscope waiting for vacuum extraction. Therefore, compared with the in-situ atmosphere and liquid atmosphere detection experiments on samples in the prior art, the technical solution in this embodiment saves the use time of the transmission electron microscope or the spherical aberration electron microscope, greatly reduces production costs, and further improves the efficiency of the in-situ atmosphere and liquid atmosphere experiments.

[0053] Preferably, the first annular elastic gasket is an annular silicone gasket. The second elastic pad is a strip-shaped silicone gasket.

[0054] Preferably, an annular silicone gasket groove 16 is provided in the first chip groove 17, and the annular silicone gasket groove 16 is used to place an annular first elastic gasket, that is, an annular silicone gasket. The annular silicone gasket groove 16 is arranged around the outer periphery of the first chip groove 17, and its structure occupies a small size and is compact, so that the overall size of the sample rod head 3 is small.

[0055] Preferably, two groups of strip-shaped silicone gasket grooves 14 are provided in the second chip groove 15 for placing strip-shaped silicone gaskets. Since the first chip groove 17 is small in size, it occupies less space and has a compact structure.

[0056] Preferably, an observation area is provided on the sample rod head 3, and the observation area is a circular area with a radius of a first preset radius and a center of the second chip slot 15. When the sample rod is inserted into the electron microscope for detection, the light spot is located in the observation area.

[0057] The two groups of strip-shaped silicone gasket grooves 14 and the annular silicone gasket groove 16 are both arranged symmetrically about the observation area axis.

[0058] Preferably, the power supply electrode assembly is arranged below the first pressing sheet assembly, and the first pressing sheet assembly is symmetrically arranged on both sides of the power supply electrode assembly to further reduce the size of the sample rod.

[0059] Preferably, the first pressing plate assembly includes a sample pressing plate 19 and a fixing member, the sample pressing plate 19 is rotatably connected to the fixing member, the fixing member is connected to the sample rod head 3, and the sample pressing plate 19 can rotate around the fixing member to quickly press on the first chip to fix the first chip. Or when the first chip needs to be replaced, the sample pressing plate 19 is lifted and rotated to quickly disengage the first chip. In this embodiment, the sample pressing plate 19 is rotated to achieve the compression or loosening of the first chip, and the compression or loosening of the second chip is achieved by the extension and contraction of the sliding pressing plate, which simplifies the fixing process of the first chip and the second chip. Compared with the existing structure of fixing the first chip on the in-situ sample rod with a cover plate and screws, the sample rod in this embodiment adopts a fixing method of screws and a rotatable sample pressing plate 19, and there is no need to consider the sealing of the first chip, and the structure is simple and the cost is low.

[0060] With regard to the position of the power supply electrode assembly on the sample rod head 3, preferably, an electrode groove is also provided on the sample rod head 3, and the electrode groove is located at the rear end of the first chip groove 17. The power supply electrode assembly includes a power supply electrode 18 and a cable, and the power supply electrode 18 is provided in the electrode groove. One end of the cable is connected to the power supply electrode 18, and the other end is connected to an external controller. The upper surface of the power supply electrode 18 contacts the lower surface of the first chip to ensure that the two are in contact to form a connected circuit.

[0061] A plurality of tungsten electrodes are integrated on the power supply electrode 18, and the tungsten electrodes are connected to the external controller of the transmission electron microscope through cables. The tungsten electrodes are in contact with and connected to the first chip. A precision power supply / measurement unit is used to perform real-time electrical signal testing on the experimental sample, and the signal is controlled and read through the test software attached to the instrument. Among them, a GPIB connection is used between the precision power supply and the computer to realize real-time transmission of signal instructions, thereby realizing accurate measurement of the electrical transport properties of the chip.

[0062] Preferably, the second pressing piece assembly is disposed at the front end of the sample rod head 3 so that there is enough space for installing the second pressing piece assembly.

[0063] Preferably, the second pressing component includes a slide rail platform 20, a slide rail pressing sheet 23 and a sliding member, one end of the slide rail pressing sheet 23 is connected to the sliding member, a slide rail groove and a guide groove arranged parallel to the slide rail groove are provided on the slide rail platform 20, the sliding member drives the slide rail pressing sheet 23 to slide in the slide rail groove, a guide member is provided on the slide rail pressing sheet 23, and the guide member is slidably arranged in the guide groove. The slide rail platform 20 is installed on the sample rod head 3, and the second chip is pressed by the slide rail pressing sheet 23. The structure is simple, low-cost, and easy to implement.

[0064] Preferably, the sliding member is a bolt, which is directly connected to the slide rail pressing sheet 23 by the bolt, which has a simple structure and low cost.

[0065] Preferably, the guide groove is arranged below the slide rail groove and is arranged in parallel with the slide rail groove.

[0066] Preferably, the sample rod body 2 comprises a coaxially arranged front end thin rod 7 and a rear end thick rod 5, and the rear end thick rod 5 and the front end thin rod 7 are connected by a tapered transition section 6. A sealing ring 13 is provided on the tapered transition section 6, and the sealing ring 13 is used to seal the lens barrel of the transmission electron microscope and the sample rod.

[0067] Preferably, coaxial and interconnected guide grooves 12 are provided inside the rear end thick rod 5 and the front end thin rod 7 , and the cable is arranged in the guide groove 12 .

[0068] Preferably, the sample rod further comprises a hand grip 1 arranged on the rear end thick rod 5, and a lead-out port 9 is provided at the end of the hand grip 1, and the lead-out port 9 can be connected to an external controller of the transmission electron microscope.

[0069] Preferably, a branching connector 10 is provided at the connection between the rear end thick rod 5 and the hand grip 1, and the cables laid in the guide groove 12 are separated by the branching structure to avoid mutual influence of electrical signals between the cables.

[0070] Preferably, a first guide pin 4 is provided on the side of the hand grip 1 for positioning the sample rod during the experiment.

[0071] Preferably, a second guide pin 8 is provided on the front end thin rod 7 for controlling the switch of the transmission electron microscope valve.

[0072] In this embodiment, the electron microscope machine time is wasted due to sample preparation problems. Specifically, because the sample to be tested placed in the first chip or the second chip in the in-situ atmosphere or liquid atmosphere experiment is not necessarily an ideal sample, at this time, the sample needs to be replaced, but the transmission electron microscope has high precision. Generally, a spherical aberration electron microscope needs to wait for 10 minutes before each rod insertion, and the in-situ sample rod replacement process is cumbersome. If the sample installed in the in-situ sample rod is unqualified, it is easy to cause a long waste of machine time, resulting in a significant increase in experimental costs.

[0073] The sample loading process of the sample rod is simple. If the sample is unqualified, the sample can be quickly replaced multiple times, and whether the sample is qualified can be known by testing under an ordinary electron microscope, which reduces the sample loading time during in-situ atmosphere and liquid atmosphere experiments, and greatly saves the use time of high-precision transmission electron microscopes such as spherical aberration electron microscopes used in the above-mentioned in-situ atmosphere and liquid atmosphere tests.

[0074] In addition, when an ordinary electron microscope is testing whether a sample is qualified, the vacuuming time is 3 minutes after the sample rod is inserted, which reduces the vacuuming time, improves the experimental efficiency, and further reduces the operating time of the above-mentioned high-precision transmission electron microscopes such as spherical aberration electron microscopes.

[0075] This embodiment also provides a working method of an in-situ sample holder of a transmission electron microscope, comprising the following steps:

[0076] S1. Place the first chip in the first chip slot 17 and fix the first chip with the first pressing assembly. Place the second chip in the second chip slot 15 and press and fix the second chip with the second pressing assembly. The first chip and the second chip are in electrical contact.

[0077] S2. Insert the sample rod into the transmission electron microscope, position the sample rod, and control the valve of the transmission electron microscope to open.

[0078] S3, testing the sample in the first chip or the second chip with the sample dropped thereon, that is, gradually magnifying and focusing the first chip or the second chip, and observing whether there is an ideal sample required for the in-situ experiment under a suitable field of view;

[0079] Detecting the agglomeration of the sample. Generally, when preparing the samples of the first chip and the second chip, it is necessary to prepare a solution containing the sample, perform ultrasonic treatment, and then drop the solution onto the first chip and the second chip;

[0080] If after the experiment, it is determined that the degree of agglomeration of the sample meets the predetermined requirements of the next step of the experiment, such as the in-situ atmosphere and liquid atmosphere experiments, then the sample is qualified;

[0081] If after the experiment, it is determined that the degree of agglomeration of the sample in the first chip or the second chip does not meet the predetermined requirement for the next step of the experiment, it means that the sample is unqualified, and the sample rod is pulled out, and the above steps S1-S3 are repeated until it is qualified.

[0082] If the degree of agglomeration of the sample is determined to be too high, it will cause sample stacking, which is not conducive to the observation and characterization of the test sample. At the same time, if the degree of agglomeration of the sample is determined to be too high or too low than the predetermined requirement, it will affect the in-situ experiment.

[0083] S4, detecting the particle size of the sample in the first chip or the second chip, if the particle size value of the sample is detected to be within a predetermined particle size range, it means that the sample is qualified;

[0084] If the particle size value of the sample is not within the predetermined particle size range, the sample rod is pulled out and the above steps S1-S4 are repeated until a suitable sample is obtained;

[0085] If the particle size of the sample exceeds the predetermined particle size range, it is not conducive to observing the characterization of the sample, and it is also not conducive to conducting in-situ atmosphere and liquid atmosphere experiments on the sample;

[0086] After the aggregation degree and particle size of the samples in the first chip or the second chip are qualified, proceed to step S5;

[0087] S5. Insert the sample rod into the transmission electron microscope, and detect the electrical transport properties of the first chip or the second chip in the experiment. Specifically, when preparing the chip sample, it is necessary to first prepare a solution containing the sample and perform ultrasonic treatment, then drop the solution containing the sample onto the first chip or the second chip, and after the first chip or the second chip is dried, place it in the transmission electron microscope to observe the characteristics of the sample;

[0088] However, in this process, it is difficult to confirm whether the solution prepared during sample dropping is sputtered into the flexible circuit of the chip, causing changes in the electrical transport properties of the chip circuit. Therefore, the sample rod is connected to the external controller of the transmission electron microscope, and a closed electrical circuit is formed through the external controller, the cable, the first chip and the second chip. The resistance value detected by the external controller is compared with the standard resistance value of the chip to confirm whether the electrical transport properties of the chip are changed.

[0089] If the detected resistance value is within the predetermined error range, the sample is qualified.

[0090] If the detected resistance value is not within the standard error range, steps S1-S5 are repeated and the experimental test is performed again until it is qualified.

[0091] After the sample in the first chip or the second chip is tested to be qualified, the chip with the sample is moved to the in-situ sample rod to carry out the next experiment, such as in-situ atmosphere or liquid atmosphere experiment.

[0092] Obviously, the above embodiments of the present invention are merely examples for clearly illustrating the present invention, and are not intended to limit the implementation methods of the present invention. For those skilled in the art, other different forms of changes or modifications can be made based on the above description. It is not necessary and impossible to list all implementation methods here. Any modifications, equivalent substitutions, and improvements made within the spirit and principles of the present invention shall be included in the scope of protection of the claims of the present invention.

Claims

1. A sample rod for detecting the quality of sample preparation in in-situ atmosphere and liquid atmosphere experiments, characterized in that: The invention comprises a sample rod head (3), wherein the sample rod head (3) is provided with a first chip slot (17), a second chip slot (15), a first pressing assembly and a second pressing assembly, wherein the second chip slot (15) is located inside the first chip slot (17), the first chip slot (17) is used to place a first chip, and the second chip slot (15) is used to place a second chip: The first pressing assembly is used to press and fix the first chip, and the second pressing assembly is used to press and fix the second chip, and the sample to be tested is dropped on the first chip or the second chip; an annular first elastic gasket, which is arranged in the first chip slot (17) and is arranged outside the second chip slot (15), and the annular first elastic gasket is used to support the first chip; a second elastic pad, which is arranged in the second chip slot (15), the second elastic pad being used to support the second chip, the first chip being placed on the first annular elastic gasket and electrically connected to the second chip; A power supply electrode assembly is arranged on the sample rod head (3) and is located at the rear end of the first chip slot (17); the first chip is electrically connected to the power supply electrode assembly, and the power supply electrode assembly is connected to an external controller of the transmission electron microscope.

2. The sample rod for detecting the sample preparation quality in the in-situ atmosphere and liquid atmosphere experiments according to claim 1, characterized in that: The annular first elastic gasket is an annular silicone gasket; The second elastic pad is a strip-shaped silicone pad.

3. The sample rod for detecting the sample preparation quality in the in-situ atmosphere and liquid atmosphere experiments according to claim 1 or 2, characterized in that: An observation area is provided on the sample rod head (3), and the observation area is a circular area with the center of the second chip slot (15) as the center and a radius of a first preset radius.

4. The sample rod for detecting the sample preparation quality in the in-situ atmosphere and liquid atmosphere experiments according to claim 1 or 2, characterized in that: The first pressing piece assembly comprises a sample pressing piece (19) and a fixing piece, wherein the sample pressing piece (19) is rotatably connected to the fixing piece, and the fixing piece is connected to the sample rod head (3), and the sample pressing piece (19) can rotate around the fixing piece to be quickly pressed onto or released from the first chip.

5. The sample rod for detecting the sample preparation quality in the in-situ atmosphere and liquid atmosphere experiments according to claim 1 or 2, characterized in that: The sample rod head (3) is also provided with an electrode groove, and the electrode groove is located at the rear end of the first chip groove (17); The power supply electrode assembly comprises a power supply electrode (18) and a cable. The power supply electrode (18) is arranged in the electrode slot. One end of the cable is connected to the power supply electrode (18), and the other end is connected to the external controller.

6. The sample rod for detecting the sample preparation quality in the in-situ atmosphere and liquid atmosphere experiments according to claim 1 or 2, characterized in that: The second pressing plate assembly comprises a slide rail platform (20), a slide rail pressing plate (23) and a sliding member, one end of the slide rail pressing plate (23) is connected to the sliding member, a slide rail groove and a guide groove arranged parallel to the slide rail groove are provided on the slide rail platform (20), the sliding member drives the slide rail pressing plate (23) to slide in the slide rail groove, and a guide member is provided on the slide rail pressing plate (23), and the guide member is slidably arranged in the guide groove.

7. The sample rod for detecting the sample preparation quality in the in-situ atmosphere and liquid atmosphere experiments according to claim 1 or 2, characterized in that: The sample rod also includes a sample rod body (2) connected to the sample rod head (3), the sample rod body (2) including a front end thin rod (7) and a rear end thick rod (5) coaxially arranged, the rear end thick rod (5) and the front end thin rod (7) are connected via a conical transition section (6), and a sealing ring (13) is arranged on the conical transition section (6).

8. The sample rod for detecting the sample preparation quality in the in-situ atmosphere and liquid atmosphere experiments according to claim 7, characterized in that: The sample rod further comprises a hand grip (1) arranged on the rear end thick rod (5), and a lead-out port (9) is provided at the end of the hand grip (1), and the lead-out port (9) can be connected to an external controller of the transmission electron microscope.

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