CN209961599U - In-situ high-temperature quantitative mechanical experiment table for transmission electron microscope - Google Patents
In-situ high-temperature quantitative mechanical experiment table for transmission electron microscope Download PDFInfo
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- CN209961599U CN209961599U CN201920253494.2U CN201920253494U CN209961599U CN 209961599 U CN209961599 U CN 209961599U CN 201920253494 U CN201920253494 U CN 201920253494U CN 209961599 U CN209961599 U CN 209961599U
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Abstract
The embodiment of the utility model provides a little experimental mechanics technical field is received to material normal position, the transmission electron microscope normal position high temperature quantification mechanics laboratory bench that provides, include: the test device comprises a sample rod body, a tilting platform, a driving module and a micro-electromechanical system integrated test device for acquiring stress-strain information of a sample under a temperature-stress coupling condition; a linear stepping motor and a driving rod are arranged in the sample rod body, and a connecting part of the tilting table is rotatably connected with the sample rod body; the linear stepping motor is connected with the driving rod and used for enabling the driving rod to do reciprocating linear motion along the length direction of the sample rod body, so that the installation part of the tilting table can rotate; the driving module is installed on the installation part of the tilting table and used for mechanically loading a sample on the micro-electromechanical system integrated testing device. The transmission electron microscope in-situ high-temperature quantitative mechanical experiment table can realize quantitative high-temperature mechanical test on micro-nano scale samples, and an optimal observation angle is obtained in real time through double-shaft tilting.
Description
Technical Field
The embodiment of the utility model provides a material normal position is received experimental mechanics technical field a little, especially relates to a transmission electron microscope normal position high temperature quantification mechanics laboratory bench.
Background
In recent years, the in-situ high-temperature experimental mechanical device integrated in the transmission electron microscope has made an important progress, and representative products include PI 95 in-situ sample rod of Hysitron company and TEM-AFM commercial product of Nanofactory company, the device adopts a long shaft structure with a three-dimensional displacement control module and a mechanical sensing module as a mechanical main body module, the sample to be tested is applied with stress through the probe fixed at the front end of the mechanical main body module, and the force thermal coupling application to the sample can be realized through the heating chip carried at the front end of the sample rod, however, the design of the mechanical module of this type causes the sample rod to lose the Y-axis tilting function, so that the sample is difficult to tilt to a specific crystallographic orientation only by the X-axis tilting of the transmission electron microscope goniometer, and atomic scale structure information of the material is obtained, so that researchers are difficult to accurately disclose the micro mechanism of part of scientific problems.
The MEMS device has the characteristics of high integration level, small size, high processing repeatability and the like, is expected to be integrated on a carrying platform at the front end of a sample rod of the transmission electron microscope, and realizes double-shaft tilting of an X shaft and a Y shaft. Therefore, the microchip prepared based on the MEMS processing technology provides a new way for the development of a high-temperature mechanical experiment table under the condition of double-shaft tilting in the transmission electron microscope.
The existing in-situ transmission electron microscope stretching platform for researching mechanical properties of a material at a specific temperature researches the deformation behavior and mechanism of the material at the specific temperature in a mode of simultaneously heating a thermal bimetallic driver and a sample; the deformation displacement of the thermal bimetal driver is gradually increased by gradually increasing the temperature, so that a sample is deformed; in the process, the temperature of the sample is inevitably increased, and the sample is difficult to deform at a fixed temperature; meanwhile, the stretching table is not provided with an integrated sample strain quantitative measurement device, so that the real-time output of a material stress-strain curve is difficult to realize in the microstructure evolution observation process; the heating mode of the stretching table is crucible heating, and the stretching table has the defects of large heating volume, large thermal drift of a sample and an image and the like. The existing electron microscope in-situ experiment platform integrating heating, driving and temperature control into a whole has the advantages of small heating area, high stability, accurate temperature measurement and the like by using a Pt thin film resistor as a heating element and using Au as a lead structure, but does not integrate material mechanics information quantification test parts due to the problems of MEMS device size limitation and process compatibility. Researchers in American Illinois champagne school have developed a SiC-based MEMS integrated test device which can be integrated in a scanning electron microscope and a transmission electron microscope, and can be used for in-situ observation of material microstructure evolution in the experiment uniaxial tensile experiment process and electrifying a structural beam and a sample to generate Joule heat so as to realize high-temperature mechanical test; the disadvantages of this method are: (1) the resistivity of the sample is required to be in a certain range, so that joule heat can be generated in the electrifying process, and the application range of the sample is limited; (2) the current directly passes through the sample, so that the internal microstructure and the deformation behavior of the sample are subjected to unpredictable change, and the analysis of the material deformation mechanism is influenced; (3) the temperature at which the sample is heated at a particular voltage or current is not fixed, depending on the resistivity and size of the material. Researchers at north carolina state university in the united states develop an in-situ high-temperature mechanical MEMS testing device adopting electrostatic comb tooth driving and interdigital capacitive mechanical sensing, and the design adopts a direct energization heating mode for a silicon structure beam, so that the thermal influence on a system is large in a heating process, the heating temperature is low, and meanwhile, in order to ensure the driving force of electrostatic comb teeth and the accuracy of interdigital capacitive mechanical sensing, the number of pairs of interdigital needs to be increased as much as possible, so that the MEMS device is large in size and difficult to integrate on a biaxial tilting sample rod.
SUMMERY OF THE UTILITY MODEL
The embodiment of the utility model provides a can realize the quantitative high temperature mechanics test to receiving the nanometer yardstick sample to vert through the biax and obtain optimum observation angle in real time, in order to obtain the transmission electron microscope normal position high temperature quantitative mechanics laboratory bench of material microstructure evolution and chemical composition change information under the special observation condition, be used for solving the unable normal position observation that realizes the biax simultaneously of current normal position high temperature quantitative mechanics laboratory bench and to the defect of the quantitative test of material mechanics information.
The embodiment of the utility model provides a transmission electron microscope normal position high temperature quantification mechanics laboratory bench, include: the testing device comprises a sample rod body, a tilting platform, a driving module and a micro-electromechanical system integrated testing device for acquiring stress-strain information of a sample under a temperature-stress coupling condition;
a linear stepping motor and a driving rod are arranged in the sample rod body, and a connecting part of the tilting table is rotatably connected with the sample rod body; the linear stepping motor is connected with the driving rod and used for driving the driving rod to do reciprocating linear motion along the length direction of the sample rod body, so that the installation part of the tilting table rotates;
the driving module is installed in the installation part of the tilting table and used for mechanically loading a sample on the micro-electromechanical system integrated testing device.
The integrated test device of the micro electro mechanical system comprises a first suspension body, a second suspension body and a base body provided with a groove;
the first suspension body and the second suspension body are arranged in the groove along the length direction of the groove, and a heating area for placing a sample and heating the sample is arranged between the first suspension body and the second suspension body; and obtaining the deformation information of the sample through the displacement difference between the first suspension body and the second suspension body, wherein the second suspension body is also used for obtaining the stress information borne by the sample.
The drive module comprises a driver carrying platform and a driver; the driver carrying platform is arranged on the mounting part of the tilting platform; the driver is arranged on the driver carrying platform, and the action end of the driver is detachably connected with the first suspension body; the base is connected with the driver stage.
The driver is one of electric heating driving, electrostatic comb tooth driving and piezoelectric ceramic driving.
The heating device comprises a heating area, a first heating area and a second heating area, wherein the heating area comprises a first heating area body and a first doping resistor integrated on the surface of the first heating area body; the second heating zone comprises a second heating zone body and a second doping resistor integrated on the surface of the second heating zone body;
the first heating area body with the first suspended body links to each other, the second heating area body with the second suspended body links to each other, be provided with the region that is used for placing the sample between the first heating area body with the second heating area body.
The first doping resistor forms ohmic contact through a first lead part, and the first lead part provides a first bonding area so as to realize electrical connection between the first doping resistor and a first external electrical control system;
the second doped resistor forms an ohmic contact through a second lead portion, and the second lead portion provides a second bonding area to enable electrical connection between the second doped resistor and a second external electrical control system.
The first heating area body is connected with the base body through a first heat dissipation beam, and the second heating area body is connected with the base body through a second heat dissipation beam.
The first suspension body is connected with the base body through a displacement sensing beam, and the second suspension body is connected with the base body through a stress sensing beam.
A first piezoresistive sensor is integrated on the displacement sensing beam and close to the tail part of one side of the substrate; a second piezoresistive sensor is integrated on the stress sensing beam and close to the tail part of one side of the substrate;
the first piezoresistive sensor comprises a plurality of first piezoresistors, the first piezoresistors are distributed along the axial direction of the displacement sensing beam, and the first piezoresistors form a first Wheatstone bridge;
the second piezoresistive sensor comprises a plurality of second piezoresistors, the second piezoresistors are distributed along the axial direction of the stress sensing beam, and the second piezoresistors form a second Wheatstone bridge.
The first piezoresistors are sequentially connected end to end and then form ohmic contact through a third lead part, and the third lead part provides a third press welding area so as to realize the electrical connection between the first piezoresistors and a third external electrical control system;
and the second piezoresistors are sequentially connected end to end and then form ohmic contact through a fourth lead part, and the fourth lead part is provided with a fourth press welding area so as to realize the electrical connection between the second piezoresistors and a fourth external electrical control system.
The embodiment of the utility model provides a transmission electron microscope normal position high temperature quantification mechanics laboratory bench, before carrying out high temperature mechanics quantification test operation to the sample, in the operation process and after, all can drive the biax that verts the platform and carry out X axle and Y axle through the actuating lever and vert, thereby electron beam incident direction in can real-time adjustment operation, obtain best observation condition, sample to on the micro electro mechanical system integration testing device heaies up to specific temperature, later drive module carries out mechanics loading to the sample, tensile sample, when through observing microstructure evolution in the transmission electron microscope in real time, acquire the stress-strain information of sample under temperature-stress coupling condition through the micro electro mechanical system integration testing device. The in-situ high-temperature quantitative mechanical experiment table for the transmission electron microscope can obtain stress-strain information of a sample at high temperature in real time, and does not need to switch a view field to observe the sample, so that continuous mechanical property-microstructure evolution related information can be obtained, the research on the deformation mechanism of a material under the temperature-stress coupling condition with high spatial resolution can be realized, the technical problem that a metal heating resistor and a piezoresistive sensor process cannot be compatible in an MEMS (micro electro mechanical system) process is solved, the quantitative measurement of the stress-strain signal of the material under the high temperature condition is realized, and the microstructure evolution analysis with atomic scale and high spatial resolution can be realized.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings needed to be used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to these drawings without creative efforts.
FIG. 1 is a schematic structural view of a sample rod body of a transmission electron microscope in-situ high-temperature quantitative mechanical experiment table of the present invention;
FIG. 2 is a schematic view of the whole assembly structure of the in-situ high-temperature quantitative mechanical experiment table of the transmission electron microscope of the present invention;
FIG. 3 is a schematic structural diagram of a MEMS integrated testing device of the in-situ high-temperature quantitative mechanical experiment table of the transmission electron microscope of the present invention;
FIG. 4 is an enlarged structural view of a heating zone of the in-situ high-temperature quantitative mechanical experiment table of the transmission electron microscope of the present invention;
fig. 5 is a schematic structural diagram of the second piezoresistive sensor of the transmission electron microscope in-situ high-temperature quantitative mechanical experiment table.
Description of reference numerals:
1-a sample rod body; 2-a tilt table; 3-a drive rod; 4-a driver; 5-micro electro mechanical system integrated testing device; 6-a first suspension; 7-displacement sensing beam; 8-a first heat-dissipating beam; 9-a stress sensing beam; 10-thin film lead; 11-a substrate; 12-a first heating zone; 13-a pressure welding area; 14-a second piezoresistive sensor; 15-first doping resistance; a 16-ohm contact hole; 17-a sample; 18-second piezo-resistor.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention, and it is obvious that the described embodiments are some, but not all, embodiments of the present invention. Based on the embodiments in the present invention, all other embodiments obtained by a person skilled in the art without creative efforts belong to the protection scope of the present invention.
Since the first Transmission Electron Microscope (TEM) appeared in 1931, decades of development have allowed transmission electron microscopes to gradually increase in resolution from the micron level to the sub-angstrom scale and atomic level, with a progressive increase in functional sophistication. In Situ (in-Situ) electron microscopy was proposed in the 1960 s in an effort to solve major and key scientific problems in material science. Through continuous research and development for many years, a series of in-situ experiment platforms based on a transmission electron microscope are developed, and the in-situ experiment platforms comprise a TEM heating table for heating a sample to a high temperature, a mechanical platform for realizing stretching, compression and bending of the sample, an electrical platform for realizing electrical test, a liquid and gas environment experiment platform for realizing application of environmental atmosphere, an experiment platform for realizing multi-field environment coupling and the like. The experimental platform for researching the mechanical behavior and the microstructure relationship of the material in the high-temperature environment has high application value, but the research and development of the related experimental platform are in an exploration stage. Once the platforms are successfully developed, the creep mechanism, the formation of the internal phase of the blade and the transformation process of the single crystal superalloy of the aircraft engine blade material under the high-temperature stress condition can be explored, and scientific basis can be provided for the design of the high-performance blade material from the source of microstructure design. In order to achieve the purpose, the experiment platform is matched with the transmission electron microscope, and has the functions of high-temperature loading, mechanical loading and quantitative measurement of temperature and mechanical parameters on the premise of not influencing the atomic level spatial resolution of the transmission electron microscope.
The transmission electron microscope has the working principle that the electron microscope emits high-voltage electron beams into a sample to be detected through an electron gun, the incident electron beams interact with the sample to generate elastic and inelastic scattering, and the elastic and inelastic scattering is converted into image information related to the structure, the composition, the morphology and the like of the sample through the processing of a magnetic lens and a signal receiving device. Because the wavelength of the electrons is extremely short and the electrons and the substances act according to a Bragg equation, the diffraction phenomenon is generated, and the structural analysis of the material with high spatial resolution can be realized. However, to study the microstructure evolution of the material at the atomic scale or to determine the structural, orientational information of the grains/internal defects at the nanoscale requires that high voltage electrons are incident along a specific crystal direction of the sample. The realization of the function needs the transmission electron microscope angle measuring platform and the tilting platform mechanism inside the transmission electron microscope sample rod to respectively realize the double-shaft tilting of the sample in X and Y axes.
As shown in fig. 1 and fig. 2, the embodiment of the present invention provides a transmission electron microscope in-situ high temperature quantitative mechanics experiment table, including: the device comprises a sample rod body 1, a tilting table 2, a driving module and a micro-electromechanical system integrated testing device 5 for acquiring stress-strain information of a sample under a temperature-stress coupling condition;
the sample rod body 1 comprises a sample rod rear end, a sample rod body and a rod body front end which are sequentially connected, a linear stepping motor is fixed on the sample rod rear end through a sealing screw, a through hole matched with the size of a driving rod 3 is formed in the center of the sample rod body, the driving rod rear end is in threaded connection with the linear stepping motor, the rod body front end is rotatably connected with a connecting part of a tilting table 2, the rod body front end is fixed with the tilting table 2 through a tilting shaft, and the linear stepping motor is used for driving the driving rod 3 to reciprocate linearly along the length direction of the sample rod body 1, so that the installation part of the tilting table 2 rotates around the tilting shaft;
the driving module is installed on the installation part of the tilting table 2 and used for mechanically loading a sample on the micro-electromechanical system integrated testing device 5.
It should be noted that the mems integrated test device 5 is used for carrying a sample, providing mechanical loading for the sample, providing a quantitative temperature to keep the sample in a certain temperature environment, and obtaining stress-strain information of the sample under a temperature-stress coupling condition.
The embodiment of the utility model provides an in, before carrying out high temperature mechanics quantification test operation to the sample, in the operation process and after, all can drive through actuating lever 3 and vert the platform 2 and carry out the biax of X axle and Y axle and vert, thereby electron beam incident direction in the adjustment operation that can be real-time, obtain best observation condition, sample to on micro electro mechanical system integration testing device 5 heaies up to specific temperature, later drive module carries out mechanics loading to the sample, tensile sample, when through observing the microscopic structure in real time in the transmission electron microscope and evolving, acquire the stress-strain information of sample under the temperature-stress coupling condition through micro electro mechanical system integration testing device. The transmission electron microscope in-situ high-temperature quantitative mechanical experiment table is combined with a transmission electron microscope, can realize quantitative high-temperature mechanical test on micro-nano scale samples, and obtains material microstructure evolution, chemical compositions and spectral change information under an optimal observation angle in real time through double-shaft tilting.
In one embodiment, as shown in fig. 3, the mems integrated test device 5 includes a first suspension 6, a second suspension (not shown), and a substrate 11 provided with a groove;
the substrate 11 can be a rectangular substrate, the groove is formed by extending towards the inside of the rectangular substrate along the edge of the rectangular substrate, the extending direction of the groove is consistent with the length direction of the rectangular substrate, the first suspension body 6 and the second suspension body are arranged in the groove along the length direction of the groove, and a heating zone for placing a sample and heating the sample is arranged between the first suspension body and the second suspension body; and the deformation information of the sample is obtained through the displacement difference between the first suspension body and the second suspension body, and the second suspension body is also used for obtaining the stress information borne by the sample.
It can be understood that the first suspension body 6 and the second suspension body are both hollow structures, rectangular through holes are formed in the first suspension body 6 and the second suspension body, and the abutting portion is further arranged at one end of the first suspension body 6 and can be a rectangular block. The drive module transfers force to the sample located in the heating zone through the abutment to mechanically load the sample.
In a specific embodiment, the driving module comprises a driver stage and a driver 4; the driver stage is mounted on the mounting part of the tilting table 2; the driver 4 is arranged on the driver carrying platform, and the action end of the driver 4 is detachably connected with the first suspension body 6; the base 11 is connected to the driver stage.
It should be noted that the driver 4 is a micro driver, the micro driver can realize precise driving of atom scale step length, a via hole is reserved at the front end of a driver carrier, a screw hole is arranged at the front end of the tilting table, the via hole and the screw hole are correspondingly arranged, the central lines of the via hole and the screw hole are overlapped, the driver carrier is fixed with the tilting table 2 through a fixing screw, and the driver carrier is installed on an installation part of the tilting table; the driver 4 is arranged on the driver carrying platform; the actuating end of the actuator 4 is connected to the abutment of the first suspension 6.
The micro actuator is one of an electrothermal drive, an electrostatic comb drive, and a piezoelectric ceramic drive.
In one embodiment, as shown in fig. 4, the heating zone includes a first heating zone 12 and a second heating zone (not shown), the first heating zone includes a first heating zone body and a first doping resistor 15 integrated on the surface of the first heating zone body; the second heating zone comprises a second heating zone body and a second doping resistor (not shown in the figure) integrated on the surface of the second heating zone body;
the first heating area body is connected with the first suspension body 6, the second heating area body is connected with the second suspension body, and an area for placing a sample 17 is arranged between the first heating area body and the second heating area body.
The first doped resistor forms ohmic contact through a first lead part, and the first lead part provides the first press welding area so as to realize electrical connection between the first doped resistor and a first external electrical control system; the second doped resistor forms an ohmic contact through the second lead portion, and the second lead portion provides a second bonding area for electrical connection between the second doped resistor and a second external electrical control system.
In this embodiment, the first doped resistor 15 is integrated on the upper surface of the first heating area body through the MEMS technology, the second doped resistor is integrated on the upper surface of the second heating area body through the MEMS technology, and the first doped resistor 15, the second doped resistor, the first heating area body and the second heating area body are all horseshoe-shaped structures, and are configured as the horseshoe-shaped structures to reduce the heating power and the thermal influence.
In addition, the temperature of the sample is raised by joule heat generated by electrifying the first doping resistor 15 and the second doping resistor, and the resistance value changes of the first doping resistor 15 and the second doping resistor can be measured by a four-electrode method, so that the temperature of the heating area can be monitored in real time.
In one embodiment, as shown in fig. 3, the first heating zone body is connected to the base 11 via a first heat spreader beam 8, and the second heating zone body is connected to the base 11 via a second heat spreader beam.
It should be noted that the first heat dissipation beams 8 and the second heat dissipation beams function to support, dissipate heat, and arrange the film leads 10.
In one embodiment, as shown in FIG. 3, the first suspended body 6 is connected to the base 11 via the displacement sensing beam 7, and the second suspended body is connected to the base 11 via the stress sensing beam 9.
In this embodiment, the end of the first suspension 6 remote from the first heating zone body is connected to the base 11 via the displacement sensor beam 7, and the end of the second suspension remote from the second heating zone body is connected to the base 11 via the stress sensor beam 9. And, the one end that is provided with the first heating zone body on the first suspended body 6 passes through the third heat dissipation roof beam and links to each other with base member 11, and the one end that is provided with the second heating zone body on the second suspended body passes through the fourth heat dissipation roof beam and links to each other with base member 11.
It should be noted that the total stiffness of the displacement sensing beam 7, the stress sensing beam 9, the first heat dissipation beam 8, the second heat dissipation beam, the third heat dissipation beam, and the fourth heat dissipation beam is much smaller than the stiffness of the microactuator.
It should be noted that the rigidity of the stress sensing beam, the film lead and the heat dissipation beams needs to be designed in a reasonable range according to the strength and the size of the sample to be measured, so as to obtain better mechanical resolution.
It should be noted that the first doped resistor 15, the second doped resistor, the first piezoresistive sensor and the second piezoresistive sensor in the mems integrated test device 5 are integrated on the upper surface of the device, and are all connected to the thin film lead 10 through the ohmic contact hole 16, the thin film lead 10 is respectively contacted to the upper surfaces of the first suspension body 6 and the second suspension body, and the tail end of the thin film lead 10 is provided with a bonding area 13 pattern with the surface insulating layer removed.
In one embodiment, as shown in fig. 3 and 5, a first piezoresistive sensor (not shown) is integrated on the displacement sensing beam 7 near the end of one side of the base body, and a second piezoresistive sensor 14 is integrated on the stress sensing beam 9 near the end of one side of the base body;
the first piezoresistive sensor comprises four first piezoresistors which are distributed along the axial direction of the displacement sensing beam 7, and the four first piezoresistors form a first Wheatstone bridge;
the second piezoresistive sensor 14 comprises four second piezoresistors 18, the four second piezoresistors 18 are distributed along the axial direction of the stress sensing beam 9, and the four second piezoresistors 18 form a second wheatstone bridge.
The first piezoresistors are sequentially connected end to end and then form ohmic contact through the third lead part, and the third lead part provides a third press welding area so as to realize the electrical connection between the first piezoresistors and a third external electrical control system;
the second piezoresistors are sequentially connected end to end and then form ohmic contact through the fourth lead part, and the fourth lead part provides a fourth press welding area so as to realize the electrical connection between the second piezoresistors and a fourth external electrical control system.
The first external electrical control system, the second external electrical control system, the third external electrical control system and the fourth external electrical control system can be the same external electrical control system or different external electrical control systems, and are selected and designed according to actual test requirements.
It should be noted that the first doped resistor 15, the second doped resistor, the first varistor and the second varistor 18 may be implemented by the same doping process, and all use metal as ohmic contact and lead material, and the first doped resistor 15, the second doped resistor, the first heating area body and the second heating area body are all horseshoe-shaped structures to reduce heating power and thermal influence.
The pressure welding area 13 is connected with an external control system and a data acquisition system, and realizes the acquisition of sample stress-strain data in the processes of temperature rise, temperature measurement and mechanical loading of the transmission electron microscope sample.
In one embodiment, the sample rod body 1 is provided with two symmetrically arranged motion guide slots, and a driving rod fixing shaft for connecting a driving rod is arranged in the motion guide slots and used for restraining the driving rod 3 from performing reciprocating linear motion back and forth under the driving of the linear stepping motor.
In this embodiment, the movement guide groove may be an elliptical long hole, the driving rod 3 is provided with a through hole, the driving rod fixing shaft sequentially passes through the first elliptical long hole, the through hole and the second elliptical long hole, and the displacement of the relative movement between the driving rod 3 and the sample rod body 1 can be controlled by controlling the length of the ellipse.
In one embodiment, as shown in fig. 2, the tilt table 2 includes a U-shaped connecting portion and a boss-shaped mounting portion;
the connecting portion of U type rotates with sample rod body 1 to be connected, and the installation department includes the horizontal part, and horizontal part one end is opened there is the boss draw-in groove, and opens the through-hole that is convenient for the electron beam to see through in the middle of the boss draw-in groove, and the horizontal part inlays to be established between the connecting portion of U type.
In this embodiment, the tilting table 2 is integrally of a bilateral symmetry structure, and the mounting portion of the boss shape is also of a bilateral symmetry structure, and two sides of the connecting portion of the U-shape are respectively provided with a tilting shaft hole, and the tilting shaft passes through the tilting shaft hole of the connecting portion of the U-shape and the tilting shaft hole of the front end of the bar body, so as to realize the rotational connection of the connecting portion of the U-shape and the front end of the bar body. Wherein, the sample positioned in the heating area is positioned right above the through hole.
In one embodiment, the mounting portion further includes an inclined portion having an angle θ with the horizontal portion, the inclined portion being pivotally connected to one end of the link, and the other end of the link being pivotally connected to the driving lever 3.
In the embodiment, the theta angle is 30-45 degrees, and the theta angle is designed according to actual design requirements. A rotation shaft hole is formed at the end of the inclined portion, the inclined portion is coupled to a link rod through the rotation shaft hole, the rotation shaft is inserted into the rotation shaft hole, and the link rod is coupled to the driving rod 3 through a rigid driving rod fixing shaft.
The embodiment of the utility model provides a transmission electron microscope normal position high temperature quantification mechanics laboratory bench's theory of operation specifically does: after the temperature of the sample 17 is raised by electrifying the first doping resistor 15 and the second doping resistor to generate heat, the driver is controlled to drive the first suspension body 6 connected with the driver to generate displacement, the sample 17 is subjected to mechanical loading, the sample 17 drives the second suspension body on the other side to generate displacement, the first piezoresistor on the displacement sensing beam and the second piezoresistor on the stress sensing beam are subjected to bending deformation in the process, and the stress information of the sample is obtained through the change of the output electric signal of a second Wheatstone bridge consisting of the second piezoresistors on the stress sensing beam 9; and the deformation of the sample is obtained through the displacement difference of the displacement sensing beam 7 and the stress sensing beam 9.
Before, during and after the high-temperature mechanical quantitative test operation on the sample 17 to be measured, the driving rod 3 can drive the sample rod tilting table 2 to tilt the Y axis, so that the incident direction of the electron beam in the operation can be adjusted in real time to obtain the optimal observation condition.
In the following, the in-situ high-temperature quantitative mechanical tensile test of a bulk sample in a transmission electron microscope is taken as an example, and the specific implementation manner is as follows:
calibrating the first piezoresistive sensor and calibrating the second piezoresistive sensor 14;
applying accurate displacement and stress load to the abutting end of the first suspension body 6 on the micro-electromechanical system integrated testing device 5 when a sample is not carried, and obtaining the change curve of the output electric signals of the first piezoresistive sensor and the second piezoresistive sensor 14 along with the displacement and the stress when the micro-electromechanical system integrated testing device is in no-load;
sampling the focused ion beam; extracting a sample 17 from a bulk sample by FIB technology, carrying the sample on the upper surfaces of the first heating area 12 and the second heating area, and fixing two ends of the sample 17 by Pt deposition;
processing and thinning the sample 17 by a focused ion beam to obtain a micro-nano scale sample for observation in a transmission electron microscope;
fixing a base body 11 of the micro-electromechanical system integrated testing device 5 on the upper surface of a driver carrying platform, and connecting the abutting end of the first suspension body 6 with the action end of the micro-driver;
connecting the lead with the lead of the sample rod body from the bonding area 13 by ultrasonic bonding or gold wire ball bonding;
inserting the sample rod body into a transmission electron microscope, and tilting the sample rod body along an X/Y axis to obtain an optimal observation condition;
electrifying the first doping resistor 15 and the second doping resistor, measuring the resistance value of the doping resistor by using a four-electrode method, and heating to a specific temperature;
applying an electric signal to the micro-driver to drive the first suspension body 6 to displace, and stretching the sample 17;
the method comprises the following steps of collecting output electric signals of a first piezoresistive sensor and a second piezoresistive sensor 14 while observing the microstructure evolution in a transmission electron microscope in real time;
and (4) carrying out conversion calculation on the output electric signal according to a calibration curve to obtain stress-strain information of the sample in the stretching process.
The mechanical experiment table for in-situ high-temperature quantification of the transmission electron microscope can realize mechanical loading and quantification while heating up a sample micro-area in the transmission electron microscope, does not affect biaxial tilting of a sample rod of the transmission electron microscope, and obtains material microstructure evolution and chemical composition change information under special observation conditions.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it should be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; such modifications and substitutions do not depart from the spirit and scope of the present invention in its corresponding aspects.
Claims (10)
1. The utility model provides a transmission electron microscope normal position high temperature quantification mechanics laboratory bench which characterized in that includes: the testing device comprises a sample rod body, a tilting platform, a driving module and a micro-electromechanical system integrated testing device for acquiring stress-strain information of a sample under a temperature-stress coupling condition;
a linear stepping motor and a driving rod are arranged in the sample rod body, and a connecting part of the tilting table is rotatably connected with the sample rod body; the linear stepping motor is connected with the driving rod and used for driving the driving rod to do reciprocating linear motion along the length direction of the sample rod body, so that the installation part of the tilting table rotates;
the driving module is installed in the installation part of the tilting table and used for mechanically loading a sample on the micro-electromechanical system integrated testing device.
2. The in-situ high-temperature quantitative mechanical experiment table of the transmission electron microscope according to claim 1, wherein the mems integrated test device comprises a first suspended body, a second suspended body and a base body provided with a groove;
the first suspension body and the second suspension body are arranged in the groove along the length direction of the groove, and a heating area for placing a sample and heating the sample is arranged between the first suspension body and the second suspension body; and obtaining the deformation information of the sample through the displacement difference between the first suspension body and the second suspension body, wherein the second suspension body is also used for obtaining the stress information borne by the sample.
3. The in-situ high-temperature quantitative mechanical experiment table of the transmission electron microscope according to claim 2, wherein the driving module comprises a driver stage and a driver; the driver carrying platform is arranged on the mounting part of the tilting platform; the driver is arranged on the driver carrying platform, and the action end of the driver is detachably connected with the first suspension body; the base is connected with the driver stage.
4. The in-situ high-temperature quantitative mechanical experiment table of the transmission electron microscope according to claim 3, wherein the driver is one of an electrothermal drive, an electrostatic comb drive and a piezoelectric ceramic drive.
5. The in-situ high-temperature quantitative mechanical experiment table of the transmission electron microscope according to claim 2, wherein the heating zone comprises a first heating zone body and a second heating zone, and the first heating zone comprises a first doping resistor integrated on the surface of the first heating zone body; the second heating zone comprises a second heating zone body and a second doping resistor integrated on the surface of the second heating zone body;
the first heating area body with the first suspended body links to each other, the second heating area body with the second suspended body links to each other, be provided with the region that is used for placing the sample between the first heating area body with the second heating area body.
6. The TEM in-situ high-temperature quantitative mechanical experiment table according to claim 5, wherein the first doped resistor is in ohmic contact with a first lead portion, and the first lead portion provides a first bonding area for electrical connection between the first doped resistor and a first external electrical control system;
the second doped resistor forms an ohmic contact through a second lead portion, and the second lead portion provides a second bonding area to enable electrical connection between the second doped resistor and a second external electrical control system.
7. The TEM in-situ high-temperature quantitative mechanical experiment table according to claim 5, wherein the first heating zone body is connected with the substrate through a first heat-dissipating beam, and the second heating zone body is connected with the substrate through a second heat-dissipating beam.
8. The in-situ high-temperature quantitative mechanical experiment table of the transmission electron microscope according to claim 2, wherein the first suspended body is connected with the base body through a displacement sensing beam, and the second suspended body is connected with the base body through a stress sensing beam.
9. The in-situ high-temperature quantitative mechanical experiment table of the transmission electron microscope according to claim 8, wherein a first piezoresistive sensor is integrated on the displacement sensing beam at a tail part close to one side of the substrate; a second piezoresistive sensor is integrated on the stress sensing beam and close to the tail part of one side of the substrate;
the first piezoresistive sensor comprises a plurality of first piezoresistors, the first piezoresistors are distributed along the axial direction of the displacement sensing beam, and the first piezoresistors form a first Wheatstone bridge;
the second piezoresistive sensor comprises a plurality of second piezoresistors, the second piezoresistors are distributed along the axial direction of the stress sensing beam, and the second piezoresistors form a second Wheatstone bridge.
10. The in-situ high-temperature quantitative mechanical experiment table of the transmission electron microscope of claim 9, wherein the first piezoresistors are sequentially connected end to form ohmic contact through a third lead portion, and the third lead portion provides a third bonding area for electrical connection between the first piezoresistors and a third external electrical control system;
and the second piezoresistors are sequentially connected end to end and then form ohmic contact through a fourth lead part, and the fourth lead part is provided with a fourth press welding area so as to realize the electrical connection between the second piezoresistors and a fourth external electrical control system.
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