WO2024060658A1 - Multi-functional sample chamber system applicable to electron microscope, and simulation method - Google Patents

Abstract

A multi-functional sample chamber system applicable to an electron microscope, and a simulation method. A simulation structure of the multi-functional sample chamber system is arranged in a chamber of a scanning electron microscope, and an internal chamber of the simulation structure is isolated from a vacuum chamber of the scanning electron microscope. By means of adjusting a simulation environment of the internal chamber of the simulation structure, and loading a sample made of a material of a relatively large size, real-time dynamic in-situ observation and data collection are performed on the sample without contact with the sample made of the material of a relatively large size, thus achieving whole-process detection of changes in properties of the sample made of the material of a relatively large size. The system has a simple structure, is convenient to use, is used for simulating an application environment of a material more realistically, and can implement whole-process microscopic detection on any tissue and in any condition. In addition, the structure is provided with an observation window of a relatively large size that allows an electron beam signal to pass therethrough, thereby achieving the aim of whole-process detection of changes in properties of the material of a relatively large size.

Description

A multifunctional sample chamber system and simulation method suitable for electron microscope Technical field

The present invention relates to the technical field of optical detection equipment, and in particular, to a multifunctional sample chamber system and a simulation method suitable for electron microscopes.

Background technique

At present, scanning electron microscopy is one of the main tools for testing the microstructure of materials. It can measure the microstructure of materials from macro to micro, and even nanometer size. It is an important means for studying the mechanism of materials. Energy spectrometer (EDS) and electron backscatter diffractometer (EBSD) can connect the microstructure and micro-region composition information of materials as well as crystallographic orientation and other data to facilitate integrated research.

At the same time, some loading devices placed in the scanning electron microscope chamber have also been gradually developed, which can conduct in-situ research on the microstructural evolution of materials under stress and strain loads such as tension/compression; and some air-sensitive samples , use vacuum transfer to effectively isolate the air and prevent oxidative deterioration of the materials to be studied for research; others build visualization windows in scanning electron microscopes and introduce external fields such as thermal fields, light fields, and electrochemical fields. Perform real-time dynamic in-situ observation of samples. However, these operations require the transfer of the sample to complete, and it is easy to cause contamination of the sample when the sample is transferred.

Existing electron microscopy detection technology requires samples to be kept dry, and some biological tissues need to be frozen and pre-processed, and then scanned and detected in a vacuum environment. This causes the sample to lose some specific properties. Including taking into account the actual application environment in the later stage.

Contents of the invention

The invention discloses a multifunctional sample chamber system and a simulation method suitable for electron microscopes to solve any of the above and other potential problems of the prior art.

In order to achieve the above purpose, the technical solution of the present invention is: a multifunctional sample chamber system suitable for electron microscopes, the simulation structure of the multifunctional sample chamber structure is arranged in the scanning electron microscope chamber, and the simulation structure The internal chamber is isolated from the scanning electron microscope vacuum chamber. By adjusting the simulation environment of the internal chamber of the simulation simulation structure and loading the larger material sample, the sample can be dynamically in situ in real time without contacting the larger material sample. Observation and data collection enable the entire process of detecting property changes of larger material samples.

The larger size material sample is 10cm×15cm that is not suitable for cutting, such as a wafer.

Further, the simulation structure includes a main body, a sample stage assembly, an electron transmission observation window, a data acquisition unit and a heating unit;

The electrons pass through the observation window to allow the electron beam to enter the interior of the body, and at the same time realize the entire process of observing the property changes of the sample in the body;

The sample stage assembly is used to place the sample and move the sample;

The heating unit is used to adjust the internal temperature of the main body;

The data acquisition unit is used to collect test data during the entire simulation process;

The main body is used to provide a sealed test space;

Wherein, one end of the main body is provided with a warehouse door, and the side wall of the other end is provided with an air inlet, an air outlet, a water inlet and a water outlet;

The electron transmission observation window is arranged at a central position on the top of the main body, the sample stage assembly is arranged at a central position inside the main body, and the water inlet and outlet are connected to the sample stage assembly through pipelines;

The heating unit is disposed inside the main body and connected with the sample stage assembly.

Further, the multifunctional sample chamber structure also includes: feedthrough and auxiliary units;

The feedthrough is used to transmit electrical energy to the inside of the main body in a specific environment;

The auxiliary unit is used to send various gases into the interior of the main body, or to evacuate the interior of the main body;

The feedthrough is provided on a side wall on one side of the main body;

The auxiliary unit is connected to the air inlet and the air outlet respectively.

Further, the differential pressure grating assembly includes a first grating, a second grating and an air extraction tube;

The second grating is arranged on the electron transmission observation window, and both ends of the second grating are fixedly connected to the main body, the first grating is arranged on the upper end of the second grating, so that a cavity structure is formed between the first grating and the second grating, and the exhaust pipe is connected to the inside of the cavity structure;

The first grating and the second grating are each provided with a through hole at the center for the electron beam to pass through and to converge the electron beam.

Furthermore, the electron transmission window is made of silicon nitride, chromium-coated silicon nitride or graphene.

Furthermore, the diameter of the through hole on the second grating is smaller than the diameter of the through hole on the first grating.

Further, the data acquisition unit includes BSE electronic detector, EDS electronic detector, CL fluorescence, EDS and EBSD;

The heating unit is a bias voltage module;

A sealing strip is provided between the main body and the door.

Further, the sample stage assembly includes a tensile unit, a support structure, and a cooling and heating stage sample stage made using the Peltier principle;

Wherein, the stretching unit is arranged on the upper end surface of the cooling and heating stage sample stage made by the Peltier principle, and the cooling and heating stage sample stage made by the Peltier principle is arranged on the support seat structure.

The widest temperature of the cooling and heating stage sample stage in high vacuum mode is -50℃-70℃, the temperature control accuracy is ±1.2℃, the temperature stability is ±0.2℃, and the cooling medium is distilled water or deionized water.

Further, the support base structure includes a base, a guide rail, a lifting mechanism and a driving motor;

Wherein, the base is arranged on the bottom plate inside the main body through guide rails, the lifting mechanism is arranged on the base, and the driving motor is arranged inside the base.

Further, the support base structure is a motor stage assembly, the motor stage assembly is located on the bottom plate inside the main body, the cooling and heating stage sample stage is fixedly located on the top of the motor stage assembly, and is mounted on the The motor table assembly moves along the X-direction and/or Y-direction.

Another object of the present invention is to provide a method for conducting simulation environment testing using the above-mentioned multifunctional sample warehouse structure. The method specifically includes the following steps:

S1) Place the sample to be tested on the sample stage assembly inside the main body;

S2) Adjust the position of the sample stage assembly so that the loading axis coincides with the axis of the sample to be tested, and at the same time start the heating unit and auxiliary unit to adjust the temperature and humidity inside the body to simulate the real use environment of the sample to be tested;

S3) Slowly apply load to the sample to be tested through the sample stage assembly, and deform until it breaks under the steady increase of load. The tested data is collected in real time, that is, the simulation test of the sample to be tested is completed, and finally the sample to be tested is obtained in the real environment. Strength indicators, plasticity indicators, and microscopic data during the fracture process.

The beneficial effects of the present invention are as follows: due to the adoption of the above technical solution, the device of the present invention has a simple structure and is easy to use, and is used to simulate the application environment of the material more realistically, and can implement full-process microscopic detection in any organization and under any circumstances. At the same time, the structure is provided with a larger-sized observation window, which allows the electron beam signal to pass through, thereby achieving the purpose of full-process detection of changes in the properties of larger-sized materials. For example, chips require a clean environment during the detection process, and this device can be used for vacuum transfer; for example, paper, plastic, rubber, metal, etc., we can simulate different usage scenarios by introducing atmosphere, heating, stretching, and increasing humidity, and study the influence of corrosion conditions on the mechanical properties of materials and the influence of different atmospheres on the mechanical properties of materials through full-process detection.

Description of drawings

Figure 1 is a schematic structural diagram of a multifunctional sample chamber system suitable for electron microscopes according to the present invention.

Figure 2 is a schematic structural diagram of the first embodiment of the system of the present invention.

Figure 3 is a schematic structural diagram of the second embodiment of the system of the present invention.

Figure 4 is a schematic diagram of the internal structure of the system of the present invention.

In the picture:

1. Electron beam, 2. Main body, 2-1. Door, 2-2. Air inlet, 2-3. Air outlet, 2-4. Water inlet, 2-5. Water outlet, 3. Sample stage assembly , 3-1. Tensile unit, 3-2. Support structure, 3-21. Base, 3-22. Guide rail, 3-23. Lifting mechanism, 3-24. Drive motor, 3-3. Cooling and heating Sample stage, 3-4. Motor stage assembly, 4. Electron transmission observation window, 5. Data acquisition unit, 6. Heating unit, 7. Feedthrough, 8. Differential pressure grating assembly, 8-1. First grating , 8-2. Second grating, 8-3. Air extraction pipe, 8-4. Through hole.

Detailed ways

The technical solution of the present invention will be further described below in conjunction with the accompanying drawings and examples.

The present invention is a multifunctional sample chamber system suitable for electron microscopes. The simulation structure of the multifunctional sample chamber structure is arranged in a scanning electron microscope chamber, and the internal chamber of the simulation structure is isolated from the scanning electron microscope vacuum chamber. , by adjusting the simulation environment of the internal chamber of the simulation structure and applying loads to larger-size material samples, real-time dynamic in-situ observation and data collection of samples without contacting larger-size material samples can be achieved to achieve larger-size materials. The property changes of the sample are detected throughout the process.

As shown in Figure 1, the simulation structure includes a main body 2, a sample stage assembly 3, an electron transmission observation window 4, a data acquisition unit 5 and a heating unit 6;

The electrons pass through the observation window 4, which is used to allow the electron beam to enter the interior of the main body 2, and at the same time realize the entire process of observing the property changes of the sample in the main body 2;

The sample stage assembly 3 is used to place samples and move the samples;

The heating unit 6 is used to adjust the internal temperature of the main body;

The data acquisition unit 5 is used to collect test data during the entire simulation process;

The main body 2 is used to provide a sealed test space;

Among them, one end of the main body 2 is provided with a warehouse door 2-1, and the side wall of the other end is provided with an air inlet 2-2, an air outlet 2-3, a water inlet 2-4 and a water outlet 2-5;

The electron transmission observation window 4 is arranged at the central position on the top of the main body 1, the sample stage assembly 3 is arranged at the central position inside the main body 1, and the water inlet 2-4 and the water outlet 2-5 pass through The pipeline is connected to the sample stage assembly 3;

The heating unit 6 is disposed inside the main body 1 and connected to the sample stage assembly 3 .

The multifunctional sample bin structure also includes: feedthrough 7 and auxiliary unit;

The feedthrough 7 is used to transmit electrical energy to the interior of the main body 1 in a specific environment;

The auxiliary unit is used to send various gases into the interior of the main body 1, or to evacuate the interior of the main body 1;

The feedthrough 7 is provided on the side wall on one side of the main body 1;

The auxiliary unit is connected to the air inlet 2-1 and the air outlet 2-2 respectively.

As shown in FIG2 , the multifunctional sample chamber structure further includes: a pressure difference grating component 8 for adjusting the electron beam 1 entering the main body;

The differential pressure grating assembly 8 includes a first grating 8-1, a second grating 8-2 and an air extraction pipe 8-3;

Wherein, the second grating 8-2 is disposed on the electron transmission observation window 4, and both ends of the second grating 8-2 are fixedly connected to the main body 1, and the first grating 8-1 It is arranged at the upper end of the second grating 8-2 so that a cavity structure is formed between the first grating-1 and the second grating 8-2, and the air extraction pipe 8-3 is internally connected with the cavity structure;

The first grating 8-1 and the second grating-2 are each provided with a through hole 8-4 at the center for the electron beam to pass through and to converge the electron beam.

The electron transmission observation window 4 is made of silicon nitride, chromium-coated silicon nitride or graphene.

The diameter of the through hole 8-4 on the second grating 8-2 is smaller than the diameter of the through hole 8-4 on the first grating 8-1.

The data acquisition unit 5 includes BSE electronic detector, EDS electronic detector, CL fluorescence, EDS and EBSD;

Receiver spectrometer EDS, backscattered electron imaging BSE, or other cathodoluminescence spectra, CL spectra, X-Ray, electron backscatter diffraction EBSD, etc. that can be customized according to customer needs

The heating unit 6 is a bias voltage module;

A sealing strip is provided between the main body 2 and the door 2-1.

The sample stage assembly 3 includes a stretching unit 3-1, a support structure 3-2, and a cooling and heating stage sample stage 3-3 made using the Peltier principle;

Among them, the stretching unit 3-1 is arranged on the upper end surface of the cooling and heating stage sample stage 3-3 made of the Peltier principle, and the cooling and heating stage sample 3-3 is arranged on the On the support base structure 3-2;

The cooling and heating stage sample stage 3-3 has a widest temperature range of -50°C to 70°C in high vacuum mode, a temperature control accuracy of ±1.2°C, a temperature stability of ±0.2°C, and the cooling medium is distilled water or deionized water. Ionized water.

The support structure 3-2 includes a base 3-21, a guide rail 3-22, a lifting mechanism 3-23 and a driving motor 3-24;

Among them, the base 3-21 is set on the bottom surface inside the main body 2 through the guide rail 3-22, the lifting mechanism 3-23 is set on the base 3-21, and the driving motor 3-23 is set inside the base 3-21 and connected to the connector, which is used to drive the base to move along the guide rail and the lifting structure to rise and fall, and provide power for the pulling unit.

As shown in Figures 3 and 4, the support base structure is a motor stage assembly 3-4. The motor stage assembly 3-4 is located on the bottom plate inside the main body 2. The cooling and heating stage sample stage 3 -3 is fixedly installed on the top of the motor table assembly 3, and moves along the X direction and/or Y direction under the action of the motor table assembly 3-4.

The motor table assembly 3-4 includes a Y-direction motor 3-41, an X-direction motor 3-42, a Y-direction slide table and an X-direction slide table. The X direction is perpendicular to the door, and the Y direction is parallel to the door. The bottom of the Y-direction slide table is provided with a Y-direction slide block, and the bottom plate of the cavity is provided with a Y-direction slide rail. The Y-direction slide table is slidingly connected to the Y-direction slide rail through the Y-direction slide block at the bottom; the end of the Y-direction slide table is connected to the Y-direction slide rail. The Y-direction motor is connected, and the Y-direction motor is fixed on the bottom plate of the cavity. The Y-direction sliding table realizes sliding along the Y-direction slide rail under the action of the Y-direction motor. An X-direction slide rail is provided on the upper surface of the Y-direction slide table, and an X-direction slide block is provided on the bottom of the X-direction slide table and is slidingly connected to the X-direction slide rail through the X-direction slide block. The end of the X-direction sliding table is slidingly connected to the X-direction motor, and the X-direction motor is fixedly connected to the inner wall of the warehouse door. The specific method for the sliding connection between the end of the X-direction slide table and the X-direction motor is that the motor shaft of the X-direction motor is fixedly connected to a Y-direction connecting slide rail, and the connecting slide rail is slidably connected to the end of the The X-direction slide table moves along the Y-direction when the Y-direction motor operates. The X-direction sliding table slides along the X-direction slide rail under the action of the X-direction motor. The sample stage is fixed on the X-direction slide table and moves with the movement of the X-direction slide table. As another implementation, the end of the X-direction slide table is not slidingly connected to the X-direction motor, but is fixedly connected. At this time, in order to ensure the position stability of the X-direction motor, the X-direction motor is fixedly connected to the Y-direction slide table. This makes the X-direction motor move along with the Y-direction slide table. After the Y-direction position adjustment is completed, the X-direction slide table moves along the X direction during operation.

A method for conducting simulation environment testing using the above-mentioned multifunctional sample warehouse structure. The method specifically includes the following steps:

S1) Place the sample to be tested on the sample stage assembly 3 inside the main body 2;

S2) Adjust the position of the sample stage assembly 3 so that the loading axis coincides with the axis of the sample to be tested, and at the same time start the heating unit 6 and the auxiliary unit to adjust the temperature, humidity and atmosphere inside the main body to simulate the real use environment of the sample to be tested;

S3) Slowly apply load to the sample to be tested through the sample stage assembly 3, and deform until it breaks when the load increases steadily. The tested data is collected in real time, that is, the simulation test of the sample to be tested is completed, and finally the sample to be tested is obtained in the real environment. Strength indicators, plasticity indicators, and microscopic data during the fracture process.

Example 1

A multifunctional sample chamber system suitable for an electron microscope, the structure comprising a simulation structure, the simulation structure comprising a main body 2, a sample stage assembly 3, an electron transmission observation window 4, a data acquisition unit 5, a heating unit 6 and a feedthrough 7;

Among them, one end of the main body 2 is provided with a warehouse door 2-1, and the side wall of the other end is provided with an air inlet 2-2, an air outlet 2-3, a water inlet 2-4 and a water outlet 2-5;

The electron transmission observation window 4 is arranged at the central position on the top of the main body 1, the sample stage assembly 3 is arranged at the central position inside the main body 1, and the water inlet 2-4 and the water outlet 2-5 pass through The pipeline is connected to the sample stage assembly 3;

The heating unit 6 is disposed inside the main body 1 and connected to the sample stage assembly 3 .

The feedthrough 7 is provided on the side wall on one side of the main body 1;

All the atmosphere is introduced through the auxiliary unit, and the property changes of the sample are carried out inside the simulation structure. After the chamber door 2-1 is closed, it is completely isolated from the outside of the device. It can be opened and closed controlled manually or electronically.

Example 2

As shown in Figure 2, the system also includes a pressure differential grating assembly 8, which consists of a first grating 8-1, a second grating 8-2 and an air extraction pipe 8-3;

The second grating 8-2 is disposed at the upper end of the electron transmission observation window 4, and both ends of the second grating 8-2 are fixedly connected to the main body 1. The first grating 8-1 is disposed at The upper end of the second grating 8-2 forms a cavity structure between the first grating-1 and the second grating 8-2, and the air extraction pipe 8-3 is internally connected with the cavity structure;

The first grating 8-1 and the second grating 8-2 are each provided with a through hole at the center position for electron beams to pass through. The diameter of the through hole of the second grating 8-2 is smaller than that of the first grating 8-1. The diameter of the through hole plays the role of converging the electron beam; at the same time, the gas can also pass through the through hole unobstructed, but because the opening is small, the diffusion speed is relatively slow. When used with the continuous working evacuation equipment, it can cause the side of the opening to The vacuum is very good, but the vacuum on the other side is not so good. It can ensure the vacuum of the electron microscope sample chamber while also allowing the structure to maintain low pressure or even normal pressure.

A ring of sealing strips is provided on the edge of the link of the warehouse door 2-1. The warehouse door 2-1 closely fits the sealing strip. When the sealing cover is closed and the air pressure in the sealing chamber is lower than the outside world, This structure can maintain a stable sealing state under the action of pressure difference.

The sample stage assembly 3 is used to observe the entire real-time change process of the sample to be tested, the expansion path and direction of slippage, plastic deformation, and cracking under real-time dynamic stretching conditions, and the entire real-time change process until fracture; also It can study the sensitivity of the sample to the crack size and the crack expansion speed in the presence of invisible cracks, that is, the study of fracture properties; observe the changes in the base material around the inclusions, which is a good way to study the type, shape, size, and The dynamic changes in distribution and fracture instant provide intuitive video images of real-time changes; corroded samples can also be loaded and then subjected to tensile tests to study the impact of corrosion conditions on the mechanical properties of materials; different atmospheres can also be filled into the device. , conduct microscopic characterization of samples and study the effects of different atmospheres on the mechanical properties of materials;

The air inlet 2-2 and the air outlet 2-3 of the main body 2 are used to connect the gas path or auxiliary unit in the electron microscope to realize the changes in the properties of the main body 1 under different atmospheres and water vapor; electromagnetic can be used for implementation. Valve, manual needle valve and other methods to control opening and closing;

The water inlet 2-2 and the water outlet 2-3 are used to provide cooling medium for the cooling and heating stage sample stage 3-3 of the sample stage assembly 3, and the cooling medium is distilled water or deionized water;

The BSE electronic detector 13 and EDS electronic detector 14 of the data acquisition unit 5 are built-in detectors, and can also be optionally used according to customer needs to use cathode fluorescence spectrum (CL spectrum), X-Ray, electron backscatter diffraction (EBSD) ), LVSE, etc.

The atmosphere includes argon, helium, water, etc.;

The sealing strip is a vacuum sealing ring, an O-shaped sealing ring made of Teflon, which is used to maintain the difference in internal and external air pressure after the warehouse door 2-1 is tightly closed;

The wall thickness of the main body 2 is not less than 4mm to ensure the shape stability of the sealed cavity under the action of large internal and external pressure difference stress;

The size of the electron transmission observation window 4 is between 2 mm and 10 mm, and the thickness of the observation plate is between 10 and 100 μm. The specific size can be customized as needed.​

A device and method suitable for electron microscope sample chambers. The method includes the following specific steps:

(1) The metal sheet sample is placed on the sample stage assembly 3 in the simulation structure and fixed on both sides;

(2) Move the sample stage assembly 3 so that the loading axis coincides with the axis of the metal sheet sample, and apply the load slowly;

(3) The metal sheet sample deforms until it breaks under a steady increase in load. During this process, the scanning electron microscope sets the continuous scanning parameters and continues scanning;

(4) Finally, a series of strength indicators (tensile strength and yield strength), plasticity indicators (elongation after fracture and shrinkage of area) and microscopic data during the fracture process can be obtained;

(5) Depending on the situation, the sample stage assembly 3 can be heated, and creep data can also be obtained from the tensile test of the metal sheet sample at high temperature. And obtain corresponding microscopic data to facilitate further analysis of material properties.

By adopting a device and method suitable for electron microscope sample chambers provided by the present invention, different usage scenarios can be well simulated, and the microscopic properties of materials under different environmental conditions can be studied through whole-process detection.

If testing rubber materials:

Take a sample from the finished product, place it on the sample stage assembly 3, heat it up, and observe the aging phenomenon. Gradually heating up: CR, NR, and SBR will be brittle at 150 degrees, and NBR EPDM is still elastic; ordinary NBR will be brittle at 180 degrees; HNBR will also be brittle at 230 degrees, and fluorine rubber and silicone still have a lot of elasticity. Good elasticity.

Example 3

A multifunctional sample compartment system suitable for electron microscopes. The structure includes a simulation structure. The simulation structure includes a main body 2, a sample stage assembly 3, an electron transmission observation window 4, a data acquisition unit 5, a heating unit 6 and a feedthrough. 7;

Among them, one end of the main body 2 is provided with a warehouse door 2-1, the warehouse door 2-1 and the main body 2 are sealed with a Teflon sealing ring, and the side wall of the other end is provided with an air inlet 2-2 and an air outlet 2 -3. Water inlet 2-4 and water outlet 2-5;

The electron transmission observation window 4 is arranged at the central position on the top of the main body 1, the sample stage assembly 3 is arranged at the central position inside the main body 1, and the water inlet 2-4 and the water outlet 2-5 pass through The pipeline is connected to the sample stage assembly 3;

The support structure is a motor stage assembly 3-4. The motor stage assembly 3-4 is provided on the bottom plate inside the main body 2. The cooling and heating stage sample stage 3-3 is fixedly provided on the motor stage. The top of the assembly 3, and moves along the X direction and/or Y direction under the action of the motor table assembly 3-4. The heating unit 6 is disposed inside the main body 1 and connected to the sample stage assembly 3 .

The feedthrough 7 is provided on the side wall on one side of the main body 1; the feedthrough 7 uses a vacuum electrically controlled connector;

All the atmosphere is introduced through the auxiliary unit, and the property changes of the sample are carried out inside the simulation structure. After the chamber door 2-1 is closed, it is completely isolated from the outside of the device. It can be opened and closed manually or electronically.

Embodiment 1

Load the sample, clamp and fix the chip to be tested on the sample stage assembly 3, and then close the door 2-1. After closing the door 2-1, check the air inlet/exhaust interface, which should be in a completely closed state;

Keep the door 2-1 closed and move the entire simulation structure into the electron microscope; then connect the air inlet 2-2 and the air outlet 2-3 to the reserved gas interface inside the electron microscope and open the gas valve to move the inside of the electron microscope. The data communication line of the host computer is connected to the connector of the simulation structure; then the electron microscope door can be closed and conventional vacuuming operations can be performed.

After the simulated structure enters the electron microscope, the electrons searching for the structure in the electron microscope pass through the observation window 4, adjust the position of the sample stage assembly 3 in the body 2, and adjust the electron microscope observation parameters until the sample can be imaged, that is, on the sample stage assembly 3 The sample is placed directly below the electron transmission observation window 4, and then the height of the sample stage assembly 3 is adjusted to make it as close as possible to the electron transmission observation window 4. This can reduce the loss of the electron beam incident into the filled atmosphere.

After finding a suitable observation position in the field of view of the electron microscope, the reaction gas can be input into the device through the air inlet 2-1 on the structure by controlling the gas source in the electron microscope; the gas flow rate can be controlled through the air inlet flow valve. Finally, the entire process of material property changes is detected through electron transmission through the observation window 4.

Embodiment 2

Load the sample, fix the plastic clamp of the sample to be tested on the sample stage assembly 3, and then close the door 2-1. After closing the door, check the air inlet/exhaust interface, which should be in a completely closed state;

Keep the door 2-1 closed and move the entire simulation structure into the electron microscope; then connect the air inlet 2-2 and the air outlet 2-3 to the reserved gas interface inside the electron microscope and open the gas valve to move the inside of the electron microscope. The data communication line of the host computer is connected to the connector of the simulation structure; then the electron microscope door can be closed and conventional vacuuming operations can be performed.

After the simulated structure enters the electron microscope, the electrons searching for the device in the electron microscope pass through the observation window 4, adjust the position of the sample stage assembly 3 in the main body 2, and adjust the electron microscope observation parameters until the sample can be imaged, that is, the sample stage assembly 3 The sample on the sample is directly below the electron transmission observation window 4, and then adjust the Z-axis direction of the sample stage assembly 3 to make it as close as possible to the electron observation window 4.

After finding a suitable observation position in the field of view of the electron microscope, you can control the air source in the electron microscope, input water vapor into the body 2 through the air inlet 2-2 on the device, and finally use the electrons to pass through the observation window 4 to determine the material properties. Detection of changes throughout the process.

Embodiment 3

Load the sample, clamp and fix the sample to be tested on the sample stage assembly 4, and then close the chamber door. After closing the chamber door, check the air inlet/exhaust interface, which should be in a completely closed state;

Keep the warehouse door closed and move the entire structure into the electron microscope; then connect the air inlet and outlet to the reserved gas interface inside the electron microscope and open the gas valve. Connect the data communication line of the host computer inside the electron microscope to the simulation structure. The connectors are connected; the microscope door can then be closed and normal vacuuming can be performed.

After the reaction device enters the electron microscope, search for the electrons of the device in the electron microscope through the observation window 4, adjust the position of the sample stage assembly 3 in the device, and adjust the electron microscope observation parameters until the sample can be imaged, that is, the sample on the sample stage assembly 3 It is directly below the electron transmission observation window 4, and then adjust the Z-axis direction of the sample stage assembly so that it is as close as possible to the electron transmission observation window 4. This can reduce the loss of the electron beam entering the filled atmosphere.

After finding a suitable observation position in the field of view of the electron microscope, the sample stage assembly 3 can be controlled to stretch the sample, and the slip and plasticity under stretching conditions can be detected dynamically in real time through the electrons through the observation window 4 during the entire process. The expansion path and direction of deformation and cracking, and even the entire real-time change process until fracture; it can also be used to study the sensitivity of the sample to the crack size and the crack expansion speed in the presence of invisible cracks, that is, the study of fracture performance; to observe inclusions Changes in the base material around the object provide real-time intuitive video images for studying the type, shape, size, distribution and dynamic changes of the inclusion moment; the corroded sample can also be loaded and subjected to tensile testing. Study the impact of corrosion conditions on the mechanical properties of materials; you can also fill the device with different atmospheres, perform microscopic characterization of the samples, and study the effects of different atmospheres on the mechanical properties of materials.

Embodiment 4

(1) Sample loading: Keep the warehouse door open, fix the chip sample to be tested on the sample stage by pasting, and then close and lock the warehouse door to ensure that the sealing ring is pressed tightly to prevent it from being transferred to the electron microscope. Gas exchange occurs in the air; check the air inlet/exhaust interface after closing the door and it should be in a completely closed state.

(2) Transfer to the electron microscope chamber: Keep the door closed and move the entire reaction device into the electron microscope; then connect the air inlet and outlet ports to the reserved gas ports inside the electron microscope and open the gas valve, move the upper part of the electron microscope inside. Connect the machine data communication line to the connector of the device; then close the electron microscope door and perform regular vacuuming operations.

(3) Searching for the observation position: After the reaction device enters the electron microscope, find the observation window of the device in the electron microscope, adjust the position of the XY motor stage in the reaction device, and adjust the observation parameters of the electron microscope until the sample can be imaged; the appropriate observation position is shown in Figures 3 and 4, that is, the sample on the sample stage is directly below the observation window, and the electron beam in the electron microscope passes through the observation window and hits the sample surface, thereby achieving imaging.

(4) Start and control the gas-solid reaction and observe in situ in real time: After finding a suitable observation position in the field of view of the electron microscope, you can control the gas source in the electron microscope and input the reaction into the device through the air outlet and air inlet on the device. Gas; the gas flow rate can be controlled through the air inlet flow rate valve, thereby controlling the gas-solid reaction rate in the reaction device. During the reaction, the reaction can be observed in situ in real time through the observation window.

The above is a detailed introduction to a multifunctional sample chamber system and method for an electron microscope provided in the embodiment of the present application. The description of the above embodiment is only used to help understand the method and its core idea of the present application; at the same time, for a person skilled in the art, according to the idea of the present application, there will be changes in the specific implementation method and application scope. In summary, the content of this specification should not be understood as limiting the present application.

For example, certain words are used in the description and claims to refer to specific components. Those skilled in the art will understand that hardware manufacturers may use different names to refer to the same component. This specification and the claims do not use differences in names as a means to distinguish components; rather, differences in functions of the components serve as a criterion for distinction. For example, the words "include" and "include" mentioned in the entire description and claims are open-ended terms, so they should be interpreted as "includes/includes but is not limited to." "Approximately" means that within an acceptable error range, those skilled in the art can solve the technical problem within a certain error range and basically achieve the technical effect. The following descriptions of the specification are preferred implementation modes for implementing the present application. However, the descriptions are for the purpose of illustrating the general principles of the present application and are not intended to limit the scope of the present application. The scope of protection of this application shall be determined by the appended claims.

It should also be noted that the terms "includes", "includes" or any other variation thereof are intended to cover a non-exclusive inclusion, such that a good or system including a list of elements includes not only those elements but also those not expressly listed other elements, or elements inherent to the product or system. Without further limitation, an element defined by the statement "comprises a..." does not exclude the presence of other identical elements in the goods or systems that include the stated element.

It should be understood that the term "and/or" used in this article is only an association relationship describing related objects, indicating that there can be three relationships, for example, A and/or B, which can mean: A alone exists, and A and A exist simultaneously. B, there are three situations of B alone. In addition, the character "/" in this article generally indicates that the related objects are an "or" relationship.

The above description shows and describes several preferred embodiments of the present application, but as mentioned above, it should be understood that the present application is not limited to the form disclosed herein, and should not be regarded as excluding other embodiments, but can be used in various Other combinations, modifications and environments, and can be modified through the above teachings or technology or knowledge in related fields within the scope of the application concept described herein. Any modifications and changes made by those skilled in the art that do not deviate from the spirit and scope of this application shall be within the protection scope of the appended claims of this application.

Claims (10)

1. A multifunctional sample compartment system suitable for electron microscopes, characterized in that the multifunctional sample compartment system includes a simulation structure, the simulation structure is arranged in a scanning electron microscope chamber, and the simulation structure has an internal cavity The chamber is isolated from the vacuum chamber of the scanning electron microscope. By adjusting the simulation environment of the internal chamber of the simulation simulation structure and loading the larger material sample, the sample can be moved in real-time and dynamically in situ without contacting the larger material sample. Observation and data collection enable the entire process of detecting property changes of larger material samples.
2. The multifunctional sample warehouse system according to claim 1, characterized in that the simulation structure includes a main body, a sample stage assembly, an electron transmission observation window, a data acquisition unit and a heating unit;

   The electrons pass through the observation window to allow the electron beam to enter the interior of the body, and at the same time realize the entire process of observing the property changes of the sample in the body;

   The sample stage assembly is used to place the sample and move the sample;

   The heating unit is used to heat the sample to be measured and also regulates the internal temperature of the body;

   The data acquisition unit is used to collect test data during the entire simulation process;

   The main body is used to provide a sealed test space;

   Wherein, one end of the main body is provided with a warehouse door, and the side wall of the other end is provided with an air inlet, an air outlet, a water inlet and a water outlet;

   The electron transmission observation window is arranged at a central position on the top of the main body, the sample stage assembly is arranged at a central position inside the main body, and the water inlet and outlet are connected to the sample stage assembly through pipelines;

   The heating unit is disposed inside the main body and connected to the sample stage assembly.
3. The multifunctional sample bin system according to claim 2, wherein the multifunctional sample bin structure further includes: feedthrough and auxiliary units;

   The feedthrough is used to transmit electrical energy to the inside of the main body in a specific environment;

   The auxiliary unit is used to send various gases into the interior of the main body, or to evacuate the interior of the main body;

   The feedthrough is provided on a side wall on one side of the main body;

   The auxiliary unit is connected to the air inlet and the air outlet respectively.
4. The multifunctional sample chamber system according to claim 2, wherein the multifunctional sample chamber structure further includes: a differential pressure grating assembly for adjusting the electron beam entering the main body;

   The differential pressure grating assembly includes a first grating, a second grating and an air extraction tube;

   Wherein, the second grating is disposed on the electron transmission observation window, and both ends of the second grating are fixedly connected to the main body, and the first grating is disposed on the upper end of the second grating, so that A cavity structure is formed between the first grating and the second grating, and the air extraction pipe is internally connected to the cavity structure;

   The first grating and the second grating are both provided with through holes at their center for electron beams to pass through and for converging the electron beams.
5. The multifunctional sample compartment structure according to claim 4, wherein the diameter of the through hole on the second grating is smaller than the diameter of the through hole on the first grating.
6. The multifunctional sample warehouse system according to claim 2, characterized in that the data collection unit includes BSE electronic detector, EDS electronic detector, CL fluorescence, EDS and EBSD;

   The heating unit is a bias voltage module;

   A sealing strip is provided between the main body and the door.
7. The multifunctional sample bin system according to claim 2, wherein the sample stage assembly includes a stretching unit, a support structure and a cooling and heating stage sample stage made of the Peltier principle;

   Wherein, the stretching unit is arranged on the upper end surface of the cooling and heating stage sample stage made of Peltier principle, and the cooling and heating stage sample stage made of Peltier principle is arranged on the On the support base structure;

   The cooling and heating stage sample stage made of the Peltier principle has a widest temperature range of -50°C to 70°C in high vacuum mode, a temperature control accuracy of ±1.2°C, a temperature stability of ±0.2°C, and a cooling The medium is distilled or deionized water.
8. The multifunctional sample chamber system according to claim 7, wherein the support base structure includes a base, a guide rail, a lifting mechanism and a driving motor;

   Wherein, the base is arranged on the bottom plate inside the main body through guide rails, the lifting mechanism is arranged on the base, and the driving motor is arranged inside the base.
9. The multifunctional sample compartment system according to claim 7, characterized in that the support base structure is a motor stage assembly, the motor stage assembly is located on the bottom plate inside the main body, and the cooling and heating stage sample stage It is fixed on the top of the motor table assembly and moves along the X direction and/or Y direction under the action of the motor table assembly.
10. 10. A method for conducting simulation environment testing using the multifunctional sample warehouse system as claimed in any one of claims 2 to 9, characterized in that the method specifically includes the following steps:

    S1) placing the sample to be tested on the sample stage assembly inside the main body;

    S2) Adjust the position of the sample stage assembly so that the loading axis coincides with the axis of the sample to be tested, and at the same time start the heating unit and auxiliary unit to adjust the temperature and humidity inside the body to simulate the real use environment of the sample to be tested;

    S3) Slowly apply load to the sample to be tested through the sample stage assembly, and deform until it breaks under the steady increase of load. The tested data is collected in real time, that is, the simulation test of the sample to be tested is completed, and finally the sample to be tested is obtained in the real environment. Strength indicators, plasticity indicators, and microscopic data during the fracture process.