CN210108849U - Transmission electron microscope in-situ liquid environment mechanical test platform - Google Patents

Abstract

The utility model relates to the field of material in-situ micro-nano experimental platforms, and provides a transmission electron microscope in-situ liquid environmental mechanics test platform, which comprises a sample rod and a loading table, and the loading table includes a lower chip, an upper chip and a loading device. The upper surface of the lower chip is provided with a first groove, the bottom surface of the first groove is provided with a groove, and the bottom surface of the groove is provided with a lower film window and two first through holes; the lower surface of the upper chip is provided with a second groove and an upper film The window, the second groove and the first groove form an accommodating space for installing the loading device, the upper surface of the upper chip is provided with a thermal resistance; the lower surface of the upper chip is connected with the upper surface of the lower chip, and the lower surface of the loading device is connected to the first recessed The bottom surface of the groove is connected, the loading device is provided with a driving beam, and the driving beam is provided with a sample carrying area; the lower film window, the sample carrying area and the upper film window are centered. The utility model can realize the mechanical test of the sample in the liquid corrosive environment, and solves the problem that the current transmission electron microscope cannot effectively perform the mechanical test in the in-situ liquid environment.

Description

Transmission electron microscope in situ liquid environmental mechanics test platform

technical field

The utility model relates to the field of material in-situ micro-nano experimental platforms, in particular to a transmission electron microscope in-situ liquid environmental mechanics experiment platform.

Background technique

Transmission Electron Microscope (TEM), referred to as Transmission Electron Microscope, is a modern large-scale instrument for studying the microstructure of substances. It has a wide range of applications in the fields of physics, chemistry, material science and life science. The traditional TEM characterization technology realizes the characterization and analysis of the microstructure, chemical composition and defects of materials by means of bright field image, dark field image, electron diffraction, X-ray energy spectrum and electron energy loss spectrum.

The macroscopic mechanical properties of materials (such as strength, hardness, plasticity and toughness, etc.) are closely related to their microstructures, that is, the macroscopic mechanical properties of materials are only the external comprehensive performance of the deformation of countless grains in the material. It cannot represent the continuity of its microscopic deformation. Usually, the degree of deformation at each point in the material is not the same or even has obvious differences. The strain of a material is an important manifestation of its mechanical properties, especially the strain of the microscopic grains of the material. Therefore, it is necessary to characterize the material from the micro-nano scale to reveal the basic properties and mechanical phenomena of the material. Since the plastic deformation of materials usually starts from the interior of the grain or at the grain boundary, the study of the grain strain in the microstructure of the material is helpful to understand the slip and twin formation process of the material during the plastic deformation process. Using transmission electron microscopy to study the deformation mechanism of the material microstructure, usually only non-real-time post-position observation can be performed, and the deformation mechanism can be speculated by the sample information before or after external loading. However, many years of experimental studies have found that this posterior observation often misses many key information in the time-related changes.

The development of structural materials with high strength, high hardness, high toughness and high specific strength is the eternal pursuit of scientists in the field of materials, but at the same time it cannot be ignored that the actual service conditions of some structural materials are often in liquid environments, such as in nuclear reactors, Structural materials used in the shipbuilding industry, bridges, and petroleum industries, the actual service performance of the above-mentioned industrial materials is obviously different from the ordinary environment. Under the combined action of corrosion and stress in the liquid environment, failure behavior often occurs. Using transmission electron microscopy to study the mechanism of stress corrosion cracking of materials in liquid medium, usually the sample is loaded on a micro loading table that can provide static stress, and then the entire loading table is immersed in a liquid corrosion environment. Then transfer the loading stage and the sample to the electron microscope for observation. This research method can achieve "quasi-in situ" research through multiple cycles of liquid corrosion and observation, but the work is time-consuming and it is difficult to ensure that the sample does not change during the transfer process.

It is of great significance to use transmission electron microscopy to conduct in-situ observation of mechanical tests of materials in liquid environments, and to realize the mechanical tests of micro-nano-scale samples in liquid corrosion environments and the microscopic research on the deformation and crack propagation mechanisms of samples under stress corrosion conditions. However, there is no in-situ mechanical test platform in liquid environment for transmission electron microscopy.

Utility model content

The embodiment of the utility model provides a transmission electron microscope in-situ liquid environment mechanical test platform, which is used to solve the problem that the existing transmission electron microscope cannot perform the mechanical test in the in-situ liquid environment.

The embodiment of the present utility model provides a transmission electron microscope in-situ liquid environmental mechanics test platform, including a sample rod and a loading table, the loading table is installed on the observation end of the sample rod, and the loading table includes a lower chip and an upper chip and loading the device;

The upper surface of the lower chip is provided with a first groove, the bottom surface of the first groove is provided with a groove, and the bottom surface of the groove is provided with a lower film window and two first through holes;

The lower surface of the upper chip is provided with a second groove and an upper film window, and the second groove and the first groove are used to form an accommodating space for installing the loading device. The surface is provided with thermal resistance;

The lower surface of the upper chip is connected to the upper surface of the lower chip, the lower surface of the loading device is connected to the bottom surface of the first groove, the loading device is provided with a second through hole, and the loading device is provided with a second through hole. A driving beam is arranged in the second through hole, and the driving beam is connected with the hole wall of the second through hole; a sample carrying area is arranged on the driving beam, and the lower film window, the sample carrying area and the The above film window centering settings.

In the transmission electron microscope in-situ liquid environmental mechanics test platform provided by the embodiment of the present invention, the loading platform includes an upper chip, a lower chip and a loading device. The loading device not only provides a sample loading area for placing the sample, but also can load the sample through the driving beam. Deformation stress is applied, the loading stage is installed on the observation end of the sample rod, and the gap structure between the upper chip and the lower chip makes the sample in a liquid environment that can flow, through the upper film window set on the upper chip and the lower film set on the lower chip. The window realizes the in-situ observation of the sample, thereby providing an in-situ platform that can realize mechanical testing and real-time characterization in a liquid environment in a transmission electron microscope. The microscopic study of the deformation, crack propagation and other mechanisms of the sample under stress corrosion state solves the problem that the current transmission electron microscope cannot effectively perform the mechanical test in the in-situ liquid environment.

Description of drawings

In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the following briefly introduces the accompanying drawings used in the description of the embodiments or the prior art. Obviously, the accompanying drawings in the following description These are some embodiments of the present invention. For those of ordinary skill in the art, other drawings can also be obtained from these drawings without creative efforts.

1 is a schematic structural diagram of a transmission electron microscope in-situ liquid environmental mechanics test platform according to an embodiment of the utility model;

Fig. 2 is a schematic diagram of the exploded structure of a transmission electron microscope in-situ liquid environmental mechanics test platform according to an embodiment of the utility model;

3 is a schematic structural diagram of a loading platform according to an embodiment of the present invention;

4 is a schematic cross-sectional view of a loading platform according to an embodiment of the present invention;

5 is a partial cross-sectional schematic diagram of a loading platform according to an embodiment of the present invention;

6 is a schematic structural diagram of a lower chip according to an embodiment of the present invention;

7 is a schematic diagram of the structure of the lower surface of the upper chip according to an embodiment of the present invention;

8 is a schematic diagram of the upper surface structure of the upper chip according to an embodiment of the present invention;

9 is a schematic structural diagram of a loading device according to an embodiment of the present invention;

10 is a schematic diagram of the structure of the lower surface of the pressing plate according to the embodiment of the present invention;

11 is a schematic diagram of a base structure of an embodiment of the present invention;

In the figure: 1. Sample rod; 11. Power supply lead; 12. Infusion channel; 2. Loading table; 3. Lower chip; 31. Lower film window; 32. First groove; 33. Groove; 34. First through hole; 4. loading device; 41, sample loading area; 42, driving beam; 43, second through hole; 44, positioning through hole; 5, upper chip; 51, upper film window; 52, second groove; 53, positioning protrusion; 54, thermal resistance; 55, second conductive sheet; 6, base; 61, third groove; 62, third through hole; 63, infusion hole; 64, first sealing ring groove; 641 65, the fourth groove; 66, the second sealing ring groove; 661, the second sealing ring; 67, the first conductive sheet; 68, the positioning protrusion; 7, the pressure plate; 71, the fourth pass holes; 72, the third conductive sheet; 73, threaded through holes; 74, fastening screws.

Detailed ways

In order to make the purposes, technical solutions and advantages of the embodiments of the present utility model clearer, the technical solutions in the embodiments of the present utility model will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present utility model. The embodiments described above are a part of the embodiments of the present invention, but not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative work fall within the protection scope of the present invention.

As shown in FIGS. 1-9 , the transmission electron microscope in-situ liquid environmental mechanics test platform provided by the embodiment of the present invention includes a sample rod 1 and a loading table 2 . The loading stage 2 is installed on the observation end of the sample rod 1, and the loading stage 2 includes a lower chip 3, an upper chip 5 and a loading device 4; the upper surface of the lower chip 3 is provided with a first groove 32, and the bottom surface of the first groove 32 is provided with The groove 33, the bottom surface of the groove 33 is provided with a lower film window 31 and two first through holes 34; the lower surface of the upper chip 5 is provided with a second groove 52 and an upper film window 51, the second groove 52 and the first A groove 32 is used to form an accommodating space for installing the loading device 4, the upper surface of the upper chip 5 is provided with a thermal resistance 54; the lower surface of the upper chip 5 is connected with the upper surface of the lower chip 3, and the lower surface of the loading device 4 Connected to the bottom surface of the first groove 32, the loading device 4 is provided with a second through hole 43, a driving beam 42 is arranged in the second through hole 43, and the driving beam 42 is connected with the hole wall of the second through hole 43; the driving beam 42 is provided with a sample carrying area 41, and the lower film window 31, the sample carrying area 41 and the upper film window 51 are centered.

In the transmission electron microscope in-situ liquid environmental mechanics test platform provided by the embodiment of the present invention, the upper surface of the lower chip 3 is provided with a first groove 32, and the bottom surface of the first groove 32 is provided with a groove 33 to form a stepped structure. The lower surface of the upper chip 5 is attached to the upper surface of the lower chip 3 and is located at the same height, the upper film window 51 is arranged on the lower surface of the upper chip 5, and the lower film window 31 is arranged on the bottom of the groove 33 in the lower chip 3. The lower film window 31 and the bottom surface of the groove 33 are located at the same height, so there is a height difference between the upper film window 51 and the lower film window 31, and this height difference can be used to place the sample to be observed, and the sample carrying area for placing the sample 41 is located in this altitude range. The lower surface of the loading device 4 is placed on the bottom surface of the first groove 32, so that the groove 33 provided on the bottom surface of the first groove 32 can form a liquid flow channel for providing a liquid environment for the sample; the bottom surface of the groove 33 is provided with two first The through holes 34, for example, two first through holes 34 can be located at two ends of the bottom surface of the groove 33, respectively, and the liquid can flow in from one first through hole 34, so that a preset gap space between the lower chip 3 and the upper chip 5 is formed. It is filled with liquid to provide a liquid environment for sample observation, and the liquid flows out from another first through hole 34 to form a liquid environment that can continuously circulate. The sustainable circulation of the liquid in the chip avoids the problem that trace liquids are easily volatile and lost during the process of sealing the chip with resin glue and other materials developed by the laboratory, and the properties of the liquid may change. The upper film window 51 and the lower film window 31 are electron beam transmission windows, which are based on technologies such as ultra-thin silicon nitride film windows or graphene films. The electron beam penetrates the chip inside the thin film window, enabling in situ imaging of the liquid environment within the transmission electron microscope. The upper film window 51 and the lower film window 31 not only cooperate with each other to provide an observation window of the transmission electron microscope, but also play a role in sealing the liquid environment. The upper surface of the upper chip 5 is provided with a thermal resistor 54 , which can generate heat and conduct it to the driving beam 42 when energized, and the driving beam 42 can apply deformation stress to the sample in the sample mounting area 41 .

In the transmission electron microscope in-situ liquid environmental mechanics test platform provided by the embodiment of the present invention, the loading table 2 includes an upper chip 5, a lower chip 3 and a loading device 4. The loading device 4 not only provides a sample loading area 41 for placing samples, but also Deformation stress can be applied to the sample through the driving beam 42. The loading stage 2 is installed on the observation end of the sample rod 1. The gap structure between the upper chip 5 and the lower chip 3 makes the sample in a liquid environment that can flow. The upper film window 51 and the lower film window 31 arranged on the lower chip 3 realize the in-situ observation of the sample, thereby providing an in-situ platform that can realize mechanical testing and real-time characterization in a liquid environment in a transmission electron microscope, which can realize the in-situ observation of the sample. Mechanical testing of micro- and nano-scale samples in a liquid corrosion environment, and at the same time, the microscopic study of the deformation, crack propagation and other mechanisms of the samples under stress corrosion state is realized, which solves the problem that the current transmission electron microscope cannot effectively perform in-situ mechanical testing in a liquid environment. .

In the transmission electron microscope in-situ liquid environmental mechanics test platform provided by the embodiment of the present invention, the groove depth of the first groove 32 can be 100-980 nanometers, and the groove depth of the groove 33 can be 20-100 nanometers. The lower chip 3 may include a substrate, a silicon nitride film on the upper surface of the substrate, and an interlayer structure on the upper surface of the silicon nitride film. The substrate is provided with a conical through groove corresponding to the lower film window 31 , and the bottom of the conical through groove is the silicon nitride film and forms the lower film window 31 . A first groove 32 and a groove 33 are provided on the spacer structure. The thickness of the silicon nitride film is usually 10-50 nanometers, the thickness of the spacer structure at the upper surface of the lower chip 3 is 200-1000 nanometers, the thickness of the spacer structure at the bottom surface of the first groove 32 is 20-100 nanometers, and the grooves The bottom surface of 33 is a silicon nitride film.

As shown in FIG. 10 and FIG. 11 , in the transmission electron microscope in-situ liquid environmental mechanics test platform provided by the embodiment of the present invention, the loading table 2 may also include a base 6 and a pressure plate 7, so as to facilitate the upper chip 5, the lower chip 3 and the loading device 4. Installation of sample holder 1. The upper surface of the base 6 may be provided with a third groove 61 for placing the lower chip 3 . A third through hole 62 and two infusion holes 63 are provided on the bottom surface of the third groove 61 . The third through hole 62 is provided corresponding to the lower membrane window 31 , and the two infusion holes 63 are one with the two first through holes 34 . One correspondence, so that the liquid is input from one infusion hole 63 into the corresponding first through hole 34, enters the preset gap between the upper chip 5 and the lower chip 3, and flows out from the other first through hole 34 to the corresponding first through hole 34. Correspondingly communicated with another infusion hole 63 . The bottom surface of the third groove 61 may also be provided with a first sealing ring groove 64, the third through hole 62 is located in the inner area of the first sealing ring groove 64, the two infusion holes 63 are located in the outer area of the first sealing ring groove 64, A first sealing ring 641 is accommodated in a sealing ring groove 64. When the lower surface of the lower chip 3 is attached to the bottom surface of the third groove 61, the first sealing ring 641 can form an annular seal on the abutting surface to prevent liquid infusion The connection seam between the hole 63 and the first through hole 34 leaks liquid to the third through hole 62 , which destroys the vacuum state of the transmission electron microscope.

The pressing plate 7 is used to cover and press the upper chip 5 , and the lower surface of the pressing plate 7 is connected with the upper surface of the upper chip 5 , so that the entire loading table 2 including the upper chip 5 , the lower chip 3 and the loading device 4 is tightly attached up and down. The pressing plate 7 is provided with a fourth through hole 71 , and the fourth through hole 71 is arranged corresponding to the upper film window 51 .

Further, in the transmission electron microscope in-situ liquid environmental mechanics test platform provided by the embodiment of the present invention, the upper surface of the base 6 may also be provided with a fourth groove 65 for placing the upper chip 5, and the upper chip 5 is stuck in the fourth groove. In the groove 65 , the lower surface of the upper chip 5 is connected with the bottom surface of the fourth groove 65 . A second sealing ring groove 66 is provided on the bottom surface of the fourth groove 65, the third groove 61 is located in the inner area of the second sealing ring groove 66, and a second sealing ring 661 is accommodated in the second sealing ring groove 66. When the lower surface of the chip 5 is attached to the bottom surface of the fourth groove 65 , the second sealing ring 661 can form an annular seal on the abutting surface, so that the lower surface of the upper chip 5 is in contact with the bottom surface of the fourth groove 65 . The fitting connection is tighter; through the sealing of the first sealing ring 641 and the second sealing ring 661, the liquid that may leak at the joint between the infusion hole 63 and the first through hole 34 can be sealed to prevent leakage of liquid It will adversely affect the observation and reduce the processing accuracy requirements of the surface where the base 6 is connected to the chip.

In the transmission electron microscope in-situ liquid environmental mechanics test platform provided by the embodiment of the present invention, the sample rod 1 is provided with a power supply lead 11, the upper surface of the base 6 is provided with a first conductive sheet 67 connected to the power supply lead 11, and the upper chip 5 is provided with a first conductive sheet 67 connected to the power supply lead 11. The upper surface is provided with a second conductive sheet 55 connected with the thermal resistor 54 , and the lower surface of the pressing plate 7 is provided with a third conductive sheet 72 connected with the first conductive sheet 67 and the second conductive sheet 55 . After the pressing plate 7 is pressed against the upper chip 5, the conductive leads of the sample holder 1, the first conductive sheet 67 of the base 6, the third conductive sheet 72 of the pressing plate 7, the second conductive sheet 55 of the upper chip 5, and the The thermal resistance 54 realizes the circuit connection, so that the transmission electron microscope can supply power to the thermal resistance 54 through the sample rod 1 . The sample carrying area 41 and the sample are immersed in the liquid environment. When the thermal resistor 54 integrated on the upper surface of the upper chip 5 is supplied with electric current to generate Joule heat, the temperature rises, which drives the driving beam 42 on the loading device 4 and causes the sample to be stressed. Deformation, to achieve mechanical testing in a liquid environment, the sample area that needs to be observed by transmission electron microscopy is sealed by the silicon nitride film on the liquid chip, and the high-voltage electron beam penetrates the two layers of silicon nitride film to realize the in-situ observation of the sample .

In the transmission electron microscope in-situ liquid environmental mechanics test platform provided by the embodiment of the present invention, the sample rod 1 can also be provided with two infusion channels 12. The infusion channel 12 has a liquid inlet channel and a liquid outlet channel, which are respectively connected with the base 6 for liquid inlet. The infusion hole 63 communicates with the infusion hole 63 from which the liquid is discharged, so that the transmission electron microscope can provide a flowing liquid environment for observation through the sample rod 1 .

In the transmission electron microscope in-situ liquid environmental mechanics test platform provided by the embodiment of the present invention, the driving beam 42 may include an inclined groove, the side groove wall of the inclined groove is inclined, and the cross-sectional width from the groove to the groove bottom gradually becomes smaller , the bottom surface of the groove bottom slope groove is the sample carrying area 41 . An annular groove is formed on the lower surface of the upper chip 5, and the depth of the annular groove is greater than the thickness of the driving beam 42; the upper film window 51 is provided in the inner ring area of the annular groove. As shown in FIG. 5 , the matching arrangement of the annular groove and the inclined groove makes the upper film window 51 and the lower film window 31 have a small gap and is thin enough to ensure the in-situ observation effect of the transmission electron microscope. The drive beam 42 may be one of a bimetallic beam drive, a memory alloy drive, or a thermal drive such as a V-beam.

In the transmission electron microscope in-situ liquid environmental mechanics test platform provided by the embodiment of the present invention, the lower chip 3 may be circular, and the third groove 61 on the base 6 for placing the lower chip 3 is also a circular groove. The edge of the lower chip 3 is provided with a positioning gap, and the groove edge of the third groove 61 is provided with a positioning protrusion 68 corresponding to the positioning gap. Positioning and installation of the three grooves 61; the upper chip 5 can also be rectangular, the loading device 4 is circular, the circular loading device 4 is provided with a positioning through hole 44, and the bottom surface of the second groove 52 is provided with a positioning through hole The positioning protrusion 53 corresponding to 44, the positioning protrusion 53 cooperates with the positioning through hole 44 to facilitate the positioning of the loading device 4 relative to the upper chip 5; The grooves 65 are arranged in a rectangular shape corresponding to the upper chip 5 , so that the rectangular upper chip 5 can be conveniently positioned and mounted on the base 6 .

In the transmission electron microscope in-situ liquid environmental mechanics test platform provided by the embodiment of the present invention, the upper film window 51 and the lower film window 31 can both be set to be rectangular, and the upper film window 51 and the lower film window 31 are cross-shaped in the length direction. The vertical arrangement enables the transmission electron microscope to have a better effect on the in-situ observation of the sample through the upper film window 51 and the lower film window 31 .

In order to make the upper chip 5 , the loading device 4 and the lower chip 3 fit more closely, as shown in FIG. 2 and FIG. Corresponding threaded through holes 73 , the base 6 and the pressing plate 7 are threadedly connected by fastening screws 74 passing through the threaded through holes 73 , so that the pressing plate 7 has a better pressing effect.

In the transmission electron microscope in-situ liquid environmental mechanics test platform provided by the embodiment of the present invention, the pressure plate 7, the base 6, the fastening screw 74 and the sample rod 1 can be obtained by machining, and the upper chip 5 and the lower chip 3 can be obtained by MEMS Technology semiconductor processing is obtained, and the main processes include: step 1, substrate preparation; step 2, deposition and growth of silicon nitride window film; step 3, growth of interlayer or thermal resistance 54 film; step 4, interlayer or thermal resistance 54 film The patterning and thin film resistance passivation layer growth; Step 5, etching of grooves and raised structures; Step 6, wet etching of the 51-level channel of the upper film window; Corrosion etc. The loading device 4 can be obtained by semiconductor process photolithography, deposition, etching, and focused ion beam fine etching of the sample carrying region 41 .

The transmission electron microscope in-situ liquid environmental mechanics test platform provided by the embodiment of the present invention, its assembly and test process may include:

Step S1: carrying the bulk or thin film, nanowire sample to the sample carrying area 41 of the driving beam 42;

Step S2: assembling the first sealing ring 641 and the second sealing ring 661 to the first sealing ring groove 64 and the second sealing ring groove 66 respectively;

Step S3: put the lower chip 3 into the third groove 61, so that the length direction of the rectangular lower film window 31 is perpendicular to the axial direction of the sample rod 1;

Step S4: placing the loading device 4 carrying the sample on the surface of the lower chip 3 under a light microscope, and the lower surface of the loading device 4 is in contact with the bottom surface of the first groove 32, so that the position of the sample is aligned with the lower film window 31;

Step S5: put the upper chip 5 into the fourth groove 65, so that the positioning protrusions 53 on the bottom surface of the second groove 52 and the positioning through holes 44 on the loading device 4 are mechanically positioned and matched;

Step S6: Check whether the lower film window 31, the sample, and the upper film window 51 are aligned under a light microscope, and perform fine adjustment;

Step S7: cover the pressing plate 7 and fix it with the fastening screws 74;

Step S8: conduct an electrical connection test;

Step S9: pass the liquid through the infusion channel 12 of the sample rod 1, check whether there are bubbles and film ruptures and other phenomena with a light microscope, and perform a vacuum leak detection test;

Step S10: after the vacuum leak detection confirms that the liquid is well sealed, insert the sample rod 1 into the transmission electron microscope;

Step S11: After confirming that the vacuum of the transmission electron microscope is good, turn on the electron beam, find the sample, and adjust the magnification to an appropriate magnification;

Step S12: After the electrical control system is connected, the thermal resistance 54 on the upper chip 5 is energized step by step, thereby heating the lower driving beam 42 to realize the stretching of the sample;

Step S13: Real-time recording of sample deformation and fracture behavior through transmission electron beam imaging.

The assembling and testing process of the transmission electron microscope in-situ liquid environmental mechanics test platform provided by the embodiment of the present utility model may further include: sealing the first through hole 34 on the lower chip 3 with resin glue before starting the test; after the above step S4 A small amount of liquid is dropped onto the loading device 4, and the contact area between the lower chip 3 and the upper chip 5 is sealed with resin glue; the flow of the liquid in the above step S9 is replaced by the pre-drop. This test procedure reduces the complexity of the test system.

In addition, in the above step S12, a constant electrical load can also be maintained after the sample is mechanically loaded until cracks are generated, so as to realize the in-situ stress corrosion test under static stress to observe the crack propagation behavior of the sample.

It can be seen from the above embodiments that the in-situ liquid environmental mechanics test platform for transmission electron microscopy provided by the present utility model, the loading table 2 includes an upper chip 5, a lower chip 3 and a loading device 4, and the loading device 4 not only provides a The sample loading area 41 can apply deformation stress to the sample through the driving beam 42, the loading stage 2 is installed on the observation end of the sample rod 1, and the gap structure between the upper chip 5 and the lower chip 3 makes the sample in a flowing liquid environment, The in-situ observation of the sample is realized through the upper thin film window 51 disposed on the upper chip 5 and the lower thin film window 31 disposed on the lower chip 3, thereby providing an original mechanical test and real-time characterization in a liquid environment in a transmission electron microscope. It can realize the mechanical test of micro-nano-scale samples in liquid corrosion environment, and realize the microscopic research on the deformation and crack propagation of samples under stress corrosion state, which solves the problem that the current transmission electron microscope cannot effectively carry out in-situ liquid testing. The problem of mechanical testing in the environment. The transmission electron microscope in-situ liquid environment mechanics test platform provided by the embodiment of the present invention utilizes the lower chip 3, the upper chip 5 and the corresponding first sealing ring 641 and the second sealing ring 661 to achieve good sealing of the liquid environment in the transmission electron microscope; The design of the first groove 32 and the groove 33 on the lower chip 3, on the one hand, ensures that there is a controllable liquid gap between the sample to be tested and the upper and lower silicon nitride films of the liquid chip, and on the other hand, avoids the need for assembly. The mechanical damage that the upper and lower chip structures may cause to the sample or the silicon nitride film; the loading device 4 integrated with the driving beam 42 is packaged between the upper and lower liquid chips, and the external thermal resistance 54 on the upper chip 5 is used to realize The heating of the liquid chip and the moving beam can realize the mechanical loading of the sample in a tiny sealed environment, and avoid the introduction of redundant leads or structures in the liquid; Additional interference to the sample and system when the electrical leads are connected by ultrasonic aluminum wire bonding or gold wire ball bonding when the overall assembly is completed.

The device embodiments described above are only illustrative, wherein the units described as separate components may or may not be physically separated, and the components shown as units may or may not be physical units, that is, they may be located in One place, or it can be distributed over multiple network elements. Some or all of the modules may be selected according to actual needs to achieve the purpose of the solution in this embodiment. Those of ordinary skill in the art can understand and implement it without creative effort.

Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present utility model, but not to limit them; although the present utility model has been described in detail with reference to the foregoing embodiments, those of ordinary skill in the art should understand that: It is still possible to modify the technical solutions recorded in the foregoing embodiments, or perform equivalent replacements to some of the technical features; and these modifications or replacements do not make the essence of the corresponding technical solutions depart from the spirit of the technical solutions of the embodiments of the present invention and range.

Claims (10)

1. A transmission electron microscope in-situ liquid environmental mechanics test platform, comprising a sample rod and a loading platform, the loading platform is mounted on the observation end of the sample bar, it is characterized in that, the loading platform comprises a lower chip, an upper chip and load device; The upper surface of the lower chip is provided with a first groove, the bottom surface of the first groove is provided with a groove, and the bottom surface of the groove is provided with a lower film window and two first through holes; The lower surface of the upper chip is provided with a second groove and an upper film window, and the second groove and the first groove are used to form an accommodating space for installing the loading device. The surface is provided with thermal resistance; The lower surface of the upper chip is connected to the upper surface of the lower chip, the lower surface of the loading device is connected to the bottom surface of the first groove, the loading device is provided with a second through hole, and the loading device is provided with a second through hole. A driving beam is arranged in the second through hole, and the driving beam is connected with the hole wall of the second through hole; a sample carrying area is arranged on the driving beam, and the lower film window, the sample carrying area and the The above film window centering settings. 2. The transmission electron microscope in-situ liquid environmental mechanics test platform according to claim 1, wherein the loading platform further comprises a base and a pressing plate; The upper surface of the base is provided with a third groove for placing the lower chip, and the bottom surface of the third groove is connected with the lower surface of the lower chip; the bottom surface of the third groove is provided with A third through hole and two infusion holes, the third through hole is arranged corresponding to the lower film window, and the two infusion holes are arranged in a one-to-one correspondence with the two first through holes; The bottom surface of the three grooves is further provided with a first sealing ring groove, the third through hole is located in the inner area of the first sealing ring groove, each of the infusion holes is located in the outer area of the first sealing ring groove, the A first sealing ring is arranged in the first sealing ring groove; The lower surface of the pressing plate is connected with the upper surface of the upper chip, and is used to cover and press the upper chip; the pressing plate is provided with a fourth through hole, and the fourth through hole is connected with the upper film window. corresponding settings. 3. The transmission electron microscope in-situ liquid environmental mechanics test platform according to claim 2, wherein the upper surface of the base is further provided with a fourth groove for placing the upper chip, and the lower surface of the upper chip is further provided with a fourth groove. The surface is connected with the bottom surface of the fourth groove; the bottom surface of the fourth groove is provided with a second sealing ring groove, the third groove is located in the inner area of the second sealing ring groove, the A second sealing ring is accommodated in the groove of the second sealing ring. 4. The transmission electron microscope in-situ liquid environmental mechanics test platform according to claim 2, wherein the sample rod is provided with a power supply lead, and the upper surface of the base is provided with a first power supply lead connected to the power supply lead. A conductive sheet, the upper surface of the upper chip is provided with a second conductive sheet connected to the thermal resistor, and the lower surface of the pressing plate is provided with a third conductive sheet connected to the first conductive sheet and the second conductive sheet Conductive sheet. 5. The transmission electron microscope in-situ liquid environmental mechanics test platform according to claim 2, wherein the sample rod is further provided with two infusion channels, the two infusion channels and the two infusion holes one by one Corresponding connection. 6. The transmission electron microscope in-situ liquid environmental mechanics test platform according to claim 1, wherein the groove depth of the first groove is 100-980 nanometers, and the groove depth of the groove is 20-100 nanometers . 7 . The transmission electron microscope in-situ liquid environmental mechanics test platform according to claim 1 , wherein the driving beam comprises an inclined groove, and the bottom surface of the inclined groove is the sample carrying area; The lower surface of the chip is provided with an annular groove, and the depth of the annular groove is greater than the thickness of the driving beam; the upper film window is arranged in the inner ring area of the annular groove. 8. The transmission electron microscope in-situ liquid environmental mechanics test platform according to claim 2, wherein the lower chip is circular, the edge of the lower chip is provided with a positioning notch, and the groove edge of the third groove is A positioning protrusion corresponding to the positioning notch is provided. 9. The transmission electron microscope in-situ liquid environmental mechanics test platform according to claim 2, wherein the upper chip is rectangular, the loading device is circular, and the loading device is provided with positioning through holes, so The bottom surface of the second groove is provided with a positioning protrusion corresponding to the positioning through hole. 10. The transmission electron microscope in-situ liquid environmental mechanics test platform according to claim 2, wherein the loading platform further comprises fastening screws, and the base and the pressing plate are provided with corresponding threaded through holes, The base and the pressing plate are threadedly connected by the fastening screws passing through the threaded through holes.

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