In-situ electrical property real-time analysis system based on environmental scanning electron microscope

Through the in-situ electrical properties real-time analysis system based on environmental scanning electron microscopy, the problem of unclear activity mechanism and structural stability of materials in complex environments has been solved, and in-situ real-time online analysis of material morphology and electrical properties has been realized, thereby improving the application performance of materials in complex environments.

CN120778780APending Publication Date: 2025-10-14TECHNICAL INST OF PHYSICS & CHEMISTRY - CHINESE ACAD OF SCI
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Patent Information

Application Number
CN202510959254.4
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-07-11
Publication Date
2025-10-14

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Abstract

The invention relates to the technical field of in-situ electrics, and provides an in-situ electrical property real-time analysis system based on an environmental scanning electron microscope, comprising: an environmental atmosphere simulation module; an electron gun pole shoe is arranged on the top side of the electron microscope chamber, a low-temperature sample table is arranged in the electron microscope chamber, and the electron microscope chamber is communicated with the environment atmosphere simulation module; the low-temperature Dewar is connected with the low-temperature sample table; the electrical probe is arranged on the inner wall of the electron microscope chamber, and the source meter is used for monitoring electrical signals. An environment atmosphere is simulated through an environment atmosphere simulation module, an electron gun pole shoe is arranged on the top side of an electron microscope chamber and used for imaging, a low-temperature sample table is arranged in the electron microscope chamber and used for bearing a to-be-tested sample, a low-temperature Dewar provides a low-temperature environment for the low-temperature sample table, and an electrical probe in a resistance analysis module conducts electrical monitoring on the sample. And electrical signals are monitored through a source meter, so that in-situ real-time online analysis of electrical properties of a scanning electron microscope observation machine on the surface of the material under different environment atmospheres is realized.
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Description

Technical Field

[0001] The present invention relates to the field of in-situ electrical technology, and in particular to an in-situ electrical performance real-time analysis system based on an environmental scanning electron microscope. Background Art

[0002] In situ electron microscopy characterization technology is a technology that applies external environmental stimulation to the sample during electron microscopy observation, and observes the dynamic changes of the sample's microstructure, composition and physicochemical properties in real time in situ. It plays a vital role in materials research. By introducing single or multiple conditions such as atmosphere, heating, freezing, and liquid, electron microscopy observation can provide multi-dimensional information, present more intuitive results, and simulate an environment closer to the real thing. Therefore, in situ electron microscopy technology has become a key tool for exploring the microscopic mechanisms of semiconductor materials. As a unique branch of scanning electron microscopy, environmental scanning electron microscopy (ESEM) can achieve atmospheric control in the electron microscope, especially maintaining a water vapor atmosphere at the mbar level, which is particularly important for catalytic reactions involving water. For this reason, ESEM has become the preferred method for in situ microscopic characterization of many water-related atmospheres.

[0003] In the existing technology, researchers have gradually shifted their focus from quasi-in situ / in situ research to dynamic research that truly reflects the process. Due to its direct application value, resistive semiconductor gas sensors have become one of the sensors with a long research history and a relatively complete theoretical system. The working principle of resistive semiconductor gas sensors is to achieve gas detection based on the change in resistance value after gas adsorption on the surface of the material. However, in actual applications, the material will be affected by external factors such as temperature, oxygen, and moisture, resulting in structural degradation and performance degradation, thereby limiting its potential for further development and commercial application. In particular, for new perovskite structured photocatalysts, their activity mechanism and structural stability change mechanism in complex application environments are still unclear, and the stability of the catalyst is crucial to its application performance and activity. In a high humidity environment, the material may undergo physical changes (such as dissolution, water absorption) or chemical changes (such as hydrolysis), but research on these change processes and their mechanisms is still relatively scarce.

[0004] Therefore, how to provide an in-situ electrical performance real-time analysis system based on an environmental scanning electron microscope is a technical problem that needs to be solved urgently by those skilled in the art. Summary of the Invention

[0005] The present invention provides an in-situ electrical properties real-time analysis system based on an environmental scanning electron microscope, which is used to solve the defect of the existing technology that the activity mechanism and structural stability change mechanism of materials in complex application environments are unclear. It realizes the in-situ observation of the morphology and performance changes of materials by combining the control of different humidity and atmosphere, thereby gaining a deeper understanding of the structure and performance of materials in complex environments.

[0006] The present invention provides an in-situ electrical performance real-time analysis system based on an environmental scanning electron microscope, comprising: Environmental atmosphere simulation module, used to simulate environmental atmosphere; An electron microscope chamber, with an electron gun pole shoe provided on the top side, a low-temperature sample stage built into the electron microscope chamber, and the electron microscope chamber is connected to the ambient atmosphere simulation module; the low-temperature sample stage is used to carry the sample to be tested; A low-temperature Dewar is located outside the electron microscope chamber and is connected to the low-temperature sample stage; The resistance analysis module includes an electrical probe and a source meter connected to each other. The electrical probe is arranged on the inner wall of the electron microscope chamber and is located on the top side of the sample to be tested. The source meter is used to monitor the electrical signal.

[0007] According to an in-situ electrical performance real-time analysis system based on an environmental scanning electron microscope provided by the present invention, the resistance analysis module also includes a transmission mechanism, which is connected to the electrical probe, the transmission mechanism runs through the electron microscope chamber, and the transmission mechanism is used to manipulate the movement of the electrical probe.

[0008] According to an in-situ electrical performance real-time analysis system based on an environmental scanning electron microscope provided by the present invention, the environmental atmosphere simulation module includes: Gas supply structure with built-in simulated gas; a pipe, one end of which is connected to the gas cylinder and the other end of which extends into the electron microscope chamber; A first valve is provided on the pipeline, and the first valve is used to control the flow of the simulated gas into the electron microscope chamber.

[0009] According to an in-situ electrical property real-time analysis system based on an environmental scanning electron microscope provided by the present invention, the simulated gas is a mixed gas, the gas supply structure includes a water vapor bottle and a reaction gas bottle, the environmental atmosphere simulation module also includes a mixing chamber, the water vapor bottle and the reaction gas bottle are respectively connected to the mixing chamber, and a second valve is provided between the water vapor bottle and the mixing chamber, and a third valve is provided between the reaction gas bottle and the mixing chamber.

[0010] According to an in-situ electrical performance real-time analysis system based on an environmental scanning electron microscope provided by the present invention, the outlet of the water vapor bottle is connected to a first branch pipe, the outlet of the reaction gas bottle is connected to a second branch pipe, the first branch pipe and the second branch pipe merge into a main pipe, the main pipe is connected to the gas mixing chamber, and a check valve is provided on the main pipe.

[0011] According to the present invention, an in-situ electrical performance real-time analysis system based on an environmental scanning electron microscope is provided. The low-temperature sample stage carries a circular sample with a diameter of less than or equal to 10 mm, and the temperature control range of the low-temperature sample stage is 90K-300K; a cooling structure is provided between the low-temperature sample stage and the low-temperature Dewar, and a groove for carrying the sample to be tested is provided on the low-temperature sample stage, and a buffer heating plate is provided on the surrounding side of the groove.

[0012] According to the in-situ electrical performance real-time analysis system based on an environmental scanning electron microscope provided by the present invention, the capacity of the low-temperature Dewar is greater than or equal to 10L, and the lowest temperature of the bottom of the low-temperature Dewar is 60K.

[0013] According to the in-situ electrical performance real-time analysis system based on an environmental scanning electron microscope provided by the present invention, the electrical probe has a telescopic range of 0-50 mm and a horizontal movement range of 0-5 mm.

[0014] According to the present invention, an in-situ electrical performance real-time analysis system based on an environmental scanning electron microscope is provided. The top tank port of the low-temperature dewar is provided with an infusion port, the infusion port is used to input liquid nitrogen, and the infusion port is connected to a polyfluoroethylene tube. The bottom end of the polyfluoroethylene tube is connected to the bottom of the tank body. The top of the low-temperature dewar is also connected to a vacuum pump.

[0015] According to an in-situ electrical performance real-time analysis system based on an environmental scanning electron microscope provided by the present invention, the capacity of the low-temperature Dewar is greater than or equal to 10L, the height between the bottom end of the polyfluoroethylene tube and the bottom of the low-temperature Dewar tank is less than or equal to 100mm; and the vacuum pump speed is not less than 20L / s.

[0016] The present invention provides an in-situ electrical performance real-time analysis system based on an environmental scanning electron microscope. The environmental atmosphere simulation module simulates the environmental atmosphere. An electron gun pole shoe is provided on the top side of the electron microscope chamber for imaging. A low-temperature sample stage is built into the electron microscope chamber for carrying a sample to be tested. The environmental atmosphere simulation module is used to provide a simulated atmosphere environment for the electron microscope chamber. The low-temperature Dewar provides a low-temperature environment for the low-temperature sample stage. The electrical probe in the resistance analysis module performs electrical monitoring on the sample, and the source meter monitors the electrical signal, thereby realizing in-situ real-time online analysis of the electrical performance of the scanning electron microscope observation machine on the material surface under different environmental atmospheres, providing strong technical support for related research. BRIEF DESCRIPTION OF THE DRAWINGS

[0017] In order to more clearly illustrate the technical solutions in the present invention or the prior art, a brief introduction is given below to the drawings required for use in the embodiments or the description of the prior art. Obviously, the drawings described below are some embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying any creative work.

[0018] Figure 1 It is a structural schematic diagram of the in-situ electrical performance real-time analysis system based on environmental scanning electron microscope provided by the present invention.

[0019] Reference numerals: 1. Ambient atmosphere simulation module; 2. Electron microscope chamber; 3. Low-temperature sample stage; 4. Low-temperature Dewar; 5. Resistance analysis module; 6. Vacuum pump; 7. Cooling structure; 8. Buffer heating plate; 9. Liquid nitrogen; 51. Electrical probe; 52. Source meter; 53. Transmission mechanism; 11. First valve; 12. Water vapor bottle; 13. Mixing chamber; 14. Second valve; 15. Third valve; 16. Check valve; 17. Reaction gas bottle; 21. Electron gun pole piece; 71. Bellows; 72. Heat transfer copper wire harness; 73. Through flange; 74. Heat transfer cold finger. DETAILED DESCRIPTION

[0020] To make the objectives, technical solutions, and advantages of the present invention more clear, the technical solutions of the present invention will be clearly and completely described below in conjunction with the accompanying drawings. Obviously, the embodiments described are only some embodiments of the present invention, not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making creative efforts shall fall within the scope of protection of the present invention.

[0021] The following combination Figure 1 The present invention describes an in-situ electrical performance real-time analysis system based on an environmental scanning electron microscope, which is used to realize the morphology observation and in-situ characterization of the electrical properties of materials under different pressure and atmosphere conditions.

[0022] The in-situ electrical real-time performance analysis system based on an environmental scanning electron microscope provided by the present invention includes an environmental atmosphere simulation module 1, an electron microscope chamber 2, a low-temperature sample stage 3, a low-temperature dewar 4 and a resistance analysis module 5.

[0023] The ambient atmosphere simulation module 1 is used to simulate the ambient atmosphere. The electron microscope chamber 2 is connected to the ambient atmosphere simulation module 1 and is used to introduce specific gases into the electron microscope chamber 2 to simulate the actual working environment of the sample. An electron gun pole piece 21 is installed on the top side of the electron microscope chamber 2. This pole piece 21 can achieve high-resolution topographic imaging of the sample, providing a visual basis for electrical performance.

[0024] Electron microscope chamber 2 is built-in with low-temperature sample stage 3, and low-temperature sample stage 3 is used for carrying sample to be measured.Cryogenic dewar 4 is located outside electron microscope chamber 2.Cryogenic dewar 4 is connected with low-temperature sample stage 3, and low-temperature dewar 4 is that low-temperature sample stage 3 transmits cold capacity, can obtain continuous low-temperature cold source, and maintains and regulates temperature by buffer heating plate 8, so that sample temperature is accurately controlled in low-temperature range.Resistance analysis module 5 comprises interconnected electrical probe 51 and source meter 52, and electrical probe 51 is arranged on the inwall of electron microscope chamber 2, and source meter 52 is used for monitoring electrical signal.Electrical probe 51 is located at the top side of sample to be measured, and electrical probe 51 can directly contact sample surface, and accurate current / voltage signal is provided by source meter outside electron microscope chamber, and synchronously measures the electrical parameters such as resistance, current-voltage characteristic of sample.

[0025] The in-situ electrical performance real-time analysis system based on an environmental scanning electron microscope provided by an embodiment of the present invention adds the gas required for the test inside the electron microscope chamber, which can continuously and stably supply the gas. The low-temperature Dewar is used to transfer heat and cool the low-temperature sample stage. There is no vibration problem caused by liquid flow, and the consumption of low-temperature medium is small. Through the electrical probe, SEM observation of the surface morphology of semiconductor materials and in-situ real-time online analysis of electrical properties can be achieved under different environmental atmospheres.

[0026] Among them, the low-temperature sample stage 3 can also be connected to the five-axis motor of the electron microscope sample stage to achieve free movement of the low-temperature sample stage 3. A cooling structure 7 is provided between the low-temperature sample stage 3 and the low-temperature Dewar. A groove for carrying the sample to be tested is provided on the low-temperature sample stage 3, and a buffer heating plate 8 is provided on the side of the groove facing the sample to be tested. The cooling structure 7 can include a bellows 71, a heat transfer copper wire bundle 72, a through flange 73 and a heat conduction cold finger 74. The interior of the low-temperature sample stage 3 is a vacuum chamber, which is connected to the low-temperature Dewar 4 outside the electron microscope chamber 2 through the bellows 71, the heat conduction cold finger 74 and the through flange 73. The bellows 71 is equipped with a heat transfer copper wire bundle 72. One end of the heat transfer copper wire bundle 72 extends into the low-temperature sample stage 3 and is finally fixed on the upper part of the interior of the low-temperature sample stage 3. The other end of the heat transfer copper wire bundle 72 is fixed on the lower part of the interior of the low-temperature Dewar 4. The low-temperature Dewar 4 and the low-temperature sample stage 3 are connected through the heat transfer copper wire bundle 72 for heat transfer and cooling. There is no vibration problem caused by liquid flow, and the consumption of low-temperature medium is small. The heat transfer copper wire bundle 72 is flexible and can be arranged in a mesh shape and wrapped around the bottom side of the tank body to have a larger contact area and improve the heat transfer efficiency.

[0027] The buffer heater 8 can include a thermocouple to maintain and adjust the desired temperature. If the sample stage temperature is too low when changing samples, the buffer heater 8 can be used to increase the temperature appropriately to prevent water mist from forming on the sample surface. The thermocouple is typically integrated with a temperature sensor and intelligent temperature control module to precisely control the sample stage temperature.

[0028] In a feasible embodiment of the present invention, the resistance analysis module 5 also includes a transmission mechanism 53, which is connected to the electrical probe 51. The transmission mechanism 53 runs through the electron microscope chamber 2, and the transmission mechanism 53 is used to manipulate the movement of the electrical probe 51. The electron microscope chamber 2 is usually small and closed, and the precise positioning of the internal probe needs to be achieved through external operation. The transmission mechanism 53 needs to maintain the sealing of the chamber while running through the chamber wall. Among them, the transmission mechanism 53 can be a transmission method of an external screw. In addition, the rotational motion of the external motor can be transmitted to the internal screw or gear mechanism through a high-precision rotary seal, and converted into the realization movement of the electrical probe 51. The operator can adjust the position of the electrical probe 51 in real time without destroying the environment of the electron microscope chamber 2, and is suitable for samples of different sizes and shapes, or quickly switch multiple test points of the same sample.

[0029] In one embodiment of the present invention, the environmental atmosphere simulation module 1 includes a gas supply structure and a first valve 11. The gas supply structure contains simulated gas and can be filled with different gases according to research needs to simulate environments such as humidity, oxidation, and catalytic reactions. A pipe is connected to the gas cylinder, one end of which is connected to the gas cylinder and the other end extends into the electron microscope chamber 2. The first valve 11 is placed on the pipe and is used to control the flow of simulated gas into the electron microscope chamber 2.

[0030] It should be noted that the pipe can be made of corrosion-resistant, low-absorption materials based on the properties of the gas to prevent gas residue or reaction with the pipe. Furthermore, the connection between the pipe and the electron microscope chamber 2 is sealed with a metal seal or welded seal to ensure a leak-free vacuum environment. The first valve 11 is the core of flow control and is typically a high-precision needle valve or proportional solenoid valve.

[0031] In a feasible embodiment of the present invention, further, the simulated gas is a mixed gas, the gas supply structure includes a water vapor bottle 12 and a reaction gas bottle 17, and the environmental atmosphere simulation module 1 also includes a gas mixing chamber 13. The water vapor bottle 12 and the reaction gas bottle 17 are both connected to the gas mixing chamber 13. A second valve 14 is provided between the water vapor bottle 12 and the gas mixing chamber 13, and a third valve 15 is provided between the reaction gas bottle 17 and the gas mixing chamber 13. The second valve 14 is used to control the gas flow rate from the water vapor bottle 12 to the gas mixing chamber 13, and the third valve 15 is used to control the gas flow rate from the reaction gas bottle 17 to the gas mixing chamber 13, so as to obtain the simulated gas with the desired ratio.

[0032] In other feasible embodiments, the simulated gas may be one or more of water, nitrogen, oxygen, hydrogen, carbon dioxide, etc.

[0033] In one feasible embodiment of the present invention, the outlet of the water vapor cylinder 12 is connected to a first branch pipe, and the outlet of the reaction gas cylinder 17 is connected to a second branch pipe. The first branch pipe and the second branch pipe merge into a main pipe, which is connected to the mixing chamber 13 and is provided with a check valve 16. When multiple gas cylinders are connected to the mixing chamber 13 simultaneously, if the pressure of one of the gas cylinders suddenly drops, the mixed gas in the mixing chamber 13 may flow back into the cylinder through the pipe. Therefore, if a gas line leaks or a pipeline failure occurs, the check valve 16 can quickly cut off the connection between that line and the mixing chamber 13, preventing gas from other pipelines from leaking through the fault point and reducing safety risks.

[0034] Specifically, the check valve 16 can be a spring-loaded check valve, which relies on the spring force to close the valve disc and is open when the reverse pressure exceeds the spring force. It is suitable for medium and low pressure systems, has a fast response speed, and is very suitable for most gas simulation scenarios.

[0035] In one feasible embodiment of the present invention, the sample supported by the cryogenic sample stage 3 is circular and has a diameter of 10 mm or less. The temperature control range of the cryogenic sample stage 3 is 90 K to 300 K. The internal space of the scanning electron microscope (SEM) sample chamber is generally limited. A sample size of 10 mm can meet the testing requirements of most micro-nano materials (such as chips, thin films, and nanowire arrays) while ensuring sufficient operating space for the sample stage within the SEM chamber.

[0036] In one feasible embodiment of the present invention, the capacity of the cryogenic dewar 4 is greater than or equal to 10L, and the lowest temperature of the cryogenic dewar 4's bottom is 60K. The combination of a 10L capacity and 60K cryogenic capability enables the cryogenic dewar 4 to support long-term, ultra-low-temperature in-situ electrical experiments, making it particularly suitable for exploring the exotic physical phenomena of quantum materials near absolute zero. The integration of this ultra-low-temperature capability with ambient atmosphere simulation and high-precision resistance measurement will provide a powerful research tool for cutting-edge fields such as condensed matter physics and quantum computing materials.

[0037] In one feasible embodiment of the present invention, the electrical probe 51 has a telescopic range of 0-50mm and a horizontal range of 0-5mm. This combination of a 0-50mm telescopic range and 0-5mm horizontal movement enables high-precision positioning of the electrical probe 51 on complex micro- and nanostructures. Combined with the system's cryogenic and atmospheric control capabilities, this enables pinpoint electrical analysis of materials or devices in extreme environments. This multi-dimensional, high-precision in-situ measurement capability will provide key technical support for research in fields such as semiconductors, nanotechnology, and biomedicine.

[0038] In a feasible embodiment of the present application, the top of the low-temperature Dewar 4 is provided with a liquid inlet for connecting a liquid nitrogen storage tank and inputting liquid nitrogen, and the liquid inlet is connected with a Teflon tube, the bottom end of the Teflon tube is connected to the bottom of the tank body of the low-temperature Dewar, and the top of the low-temperature Dewar is connected with a vacuum pump 6, the vacuum pump 6 is used to rapidly pump the liquid nitrogen to vacuum, so as to accelerate the evaporation of the liquid nitrogen, the heat absorption of the accelerated evaporation can further make the liquid nitrogen at the bottom form solid nitrogen, and the solid nitrogen is used to cool the low-temperature sample table, on the one hand, the liquid nitrogen cannot enter the low-temperature sample table 3, and the low-temperature sample table 3 will not be affected by vibration, and on the other hand, the low-temperature sample table can also obtain a lower temperature.

[0039] In the liquid inlet, two temperature sensors can be inserted at the same time, which are located at the upper part and the bottom part of the Dewar container respectively, and are used to measure the temperature of the top end and the bottom end respectively. In addition, the end of the vacuum pump 6 pipeline can also be provided with a vacuum gauge, and the vacuum gauge is used to confirm the air pressure in the tank body of the low-temperature Dewar.

[0040] In a feasible embodiment of the present application, the distance between the bottom end of the Teflon tube and the bottom of the low-temperature Dewar is less than or equal to 100 mm; the pumping speed of the vacuum pump is not less than 20 L / s, and the pumping speed greater than 20 L / s means that the Dewar sandwich layer is pumped from atmospheric pressure to the target vacuum degree only in 30 minutes, which greatly shortens the test preparation time. The high pumping speed can offset the slight leakage, maintain the stable vacuum degree for a long time, and ensure that the adiabatic performance does not decay.

[0041] Taking water and nitrogen as examples of simulated gas, the experimental process of the in-situ electrical new energy real-time analysis system based on the environmental scanning electron microscope provided by the present application is as follows: 1) A silicon wafer with a GaN device prepared by cutting into 5*5mm 2 is placed on the low-temperature sample table 3, and then the sample cabin door is closed; 2) A large liquid nitrogen tank is used to fill the low-temperature Dewar 4 with liquid nitrogen, then the liquid inlet is closed, the vacuum pump 6 switch and the pipeline valve are opened, and the upper part of the Dewar is pumped to a vacuum lower than 300 Pa; 3) Nitrogen and water are selected as the environmental atmosphere, the valve of the gas cylinder is opened, the nitrogen flow is set to 20 sccm, and the water vapor flow is set to 30 sccm; 4) The temperature of the low-temperature sample table is set to-100℃, and the actual temperature is waited to reach the set temperature; 5) The vacuum value is set to 200 Pa, and the vacuum pump 6 is opened in sequence to start pumping; 6) After the vacuum reaches the preset value, the electron beam is turned on to image and find the sample position; 7) The sample to be measured is placed in the field of view of the electron microscope, and the electrical probe 51 is moved to the position of the electrode; 8) The electron beam imaging is paused, the source table output is turned on, and the electrical signal of the sample is obtained; 9) Close the source table, the electron gun pole shoe 21, reset the electrical probe and the sample stage, close the Dewar vacuum pump 6, close the cylinder flow valve, set the sample stage temperature to room temperature, and finally, release the pressure in the electron microscope chamber 2, remove the sample, and complete the entire experimental procedure.

[0042] In the description of the embodiments of the present application, it should be noted that unless specifically defined and limited, the terms "connected", "connection" should be interpreted broadly, for example, can be fixed connection, can also be detachable connection, or integral connection; can be mechanical connection, can also be electrical connection; can be directly connected, can also be indirectly connected through an intermediate medium. For those skilled in the art, the specific meaning of the above terms in the embodiments of the present application can be understood according to the specific circumstances.

[0043] In the description of the present application, the description of the terms "one embodiment", "some embodiments", "way", "specific way", or "some ways" means that the specific features, structures, materials or characteristics described in conjunction with the embodiment or way are included in at least one embodiment or way of the present application. In the present application, the illustrative description of the above terms is not necessarily for the same embodiment or way. Moreover, the specific features, structures, materials or characteristics described can be combined in any appropriate way in any one or more embodiments or ways. In addition, those skilled in the art can combine and combine the different embodiments or features of the different embodiments or ways described in the present application without contradiction.

[0044] Finally, it should be noted that: the above embodiments are only used to illustrate the technical solutions of the present application, and not to limit them; although the present application has been described in detail with reference to the foregoing embodiments, those skilled in the art should understand that: it can still modify the technical solutions recorded in the foregoing embodiments, or make equivalent replacement for part of the technical features; and these modifications or replacements do not make the essence of the corresponding technical solutions deviate from the spirit and scope of the technical solutions of the embodiments of the present application.

Claims

1. An in-situ electrical performance real-time analysis system based on environmental scanning electron microscope, characterized in that: include: An environmental atmosphere simulation module (1), used for simulating environmental atmosphere; An electron microscope chamber (2) is provided with an electron gun pole shoe (21) on the top side, the electron microscope chamber (2) is provided with a low-temperature sample stage (3) therein, and the electron microscope chamber (2) is connected to the environmental atmosphere simulation module (1); the low-temperature sample stage (3) is used to carry a sample to be tested; A low-temperature Dewar (4) is located outside the electron microscope chamber (2), and the low-temperature Dewar (4) is connected to the low-temperature sample stage (3); The resistance analysis module (5) comprises an electrical probe (51) and a source meter (52) connected to each other, wherein the electrical probe (51) is arranged on the inner wall of the electron microscope chamber (2), and the electrical probe (51) is located on the top side of the sample to be measured; and the source meter (52) is used to monitor the electrical signal.

2. The in-situ electrical performance real-time analysis system based on environmental scanning electron microscope according to claim 1, characterized in that: The resistance analysis module (5) further comprises a transmission mechanism, the transmission mechanism being connected to the electrical probe (51), the transmission mechanism penetrating the electron microscope chamber (2), and the transmission mechanism being used to manipulate the movement of the electrical probe (51).

3. The in-situ electrical performance real-time analysis system based on environmental scanning electron microscope according to claim 1, characterized in that: The environmental atmosphere simulation module (1) comprises: Gas supply structure with built-in simulated gas; a pipe, one end of which is connected to the gas cylinder and the other end of which extends into the electron microscope chamber (2); A first valve (11) is provided on the pipeline, and the first valve (11) is used to control the flow rate of the simulated gas entering the electron microscope chamber (2).

4. The in-situ electrical performance real-time analysis system based on environmental scanning electron microscope according to claim 3, characterized in that: The simulated gas is a mixed gas, the gas supply structure includes a water vapor bottle (12) and a reaction gas bottle (17), and the environmental atmosphere simulation module (1) also includes a gas mixing chamber (13). The water vapor bottle (12) and the reaction gas bottle (17) are respectively connected to the gas mixing chamber (13), and a second valve (14) is provided between the water vapor bottle (12) and the gas mixing chamber (13), and a third valve (15) is provided between the reaction gas bottle (17) and the gas mixing chamber (13).

5. The in-situ electrical performance real-time analysis system based on environmental scanning electron microscope according to claim 4, characterized in that: The outlet of the water vapor bottle (12) is connected to a first branch pipe, and the outlet of the reaction gas bottle (17) is connected to a second branch pipe. The first branch pipe and the second branch pipe merge into a main pipe, and the main pipe is connected to the gas mixing chamber (13). A check valve (16) is provided on the main pipe.

6. The in-situ electrical performance real-time analysis system based on environmental scanning electron microscope according to any one of claims 1 to 5, characterized in that: The sample carried by the low-temperature sample stage (3) is a circle with a diameter less than or equal to 10 mm, and the temperature control range of the low-temperature sample stage (3) is 90K-300K; A cooling structure (7) is provided between the low-temperature sample stage (3) and the low-temperature Dewar (4); a groove for carrying a sample to be tested is provided on the low-temperature sample stage (3); and a buffer heating plate (8) is provided around the groove.

7. The in-situ electrical performance real-time analysis system based on environmental scanning electron microscope according to any one of claims 1 to 5, characterized in that: The capacity of the low-temperature Dewar (4) is greater than or equal to 10L, and the lowest temperature of the bottom of the low-temperature Dewar (4) is 60K.

8. The in-situ electrical performance real-time analysis system based on environmental scanning electron microscope according to any one of claims 1 to 5, characterized in that: The electrical probe (51) has a telescopic range of 0-50 mm and a horizontal movement range of 0-5 mm.

9. The in-situ electrical performance real-time analysis system based on environmental scanning electron microscope according to any one of claims 1 to 5, characterized in that: The top of the low-temperature Dewar (4) is provided with an infusion port for inputting liquid nitrogen, and the infusion port is connected to a PTFE tube, the bottom end of which is connected to the bottom of the tank body; the top of the low-temperature Dewar is also connected to a vacuum pump (6).

10. The in-situ electrical performance real-time analysis system based on environmental scanning electron microscope according to claim 9, characterized in that: The height between the bottom end of the tetrafluoroethylene tube and the bottom of the low-temperature Dewar tank is less than or equal to 100 mm; and the pumping speed of the vacuum pump (6) is not less than 20 L / s.

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