CN105758711B - Transmission electron microscope double shaft tilting in-situ mechanical specimen holder based on Piezoelectric Ceramic - Google Patents
Transmission electron microscope double shaft tilting in-situ mechanical specimen holder based on Piezoelectric Ceramic Download PDFInfo
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Abstract
Transmission electron microscope double shaft tilting in-situ mechanical specimen holder based on Piezoelectric Ceramic belongs to material microstructure mechanical property in-situ characterization field, including shaft main body and Piezoelectric Ceramic system two parts.Sample club body main body includes swivel angle plate, specimen holder, linear stepping motor, drive rod, drive link.Piezoelectric Ceramic system includes piezoelectric ceramics microscope carrier, piezoelectric ceramics, connecting seat and the sample stage that can realize stretching or compression function.Drive rod front-rear reciprocation movement is made by stepper motor, realizes sample in X and the double shaft tilting of Y-axis.Piezoelectric ceramics is produced by applying voltage and displacement and sample stage is promoted by connecting seat, so as to realize the stretching or compression to sample.The present invention coordinates with high-resolution TEM, while atomic scale, even sub- angstrom of yardstick microstructure observation is carried out, carries out controllable deforming to nano material, realize the Study on Integration of material microstructure-mechanical property, disclose the Deformation Mechanism of material.
Description
Technical field：
The present invention relates to a kind of TEM double shaft tilting in-situ mechanical specimen holders based on Piezoelectric Ceramic, match with TEM
Close, can be realized under conditions of double shaft tilting under the even sub- angstrom yardstick of atomic scale to material in draw-texture process
Monte Carlo method carry out home position observation.In draw-texture process, drive displacement can be accurately controlled, the invention belongs to saturating
Penetrate electron microscope accessories field.
Background technology：
One of an important factor for development of material science is a national science and technology progress.The quality of structural material performance is main
Depending on its mechanical property includes：Impact resistance, fatigue behaviour and the plasticity of material can working abilities etc..The high property of Development of Novel
Energy material need to deeply understand deformation mechanism of the material in the even sub- angstrom yardstick of nanometer, atom.Transmission electron microscope (TEM) is
One of important means of research material microstructure, the method that part researcher is studied by TEM ex situs, interception is different respectively
The material of deformation stage as sample, observe its microstructure, so as to infer the deformation mechanism of material；By TEM range of observation
(nanometer scale) and viewing area are the limitation of non-the same area, are sometimes difficult to obtain the accurate deformation mechanism of material.In recent years,
Part researcher and apparatus manufacture are directed to developing TEM original positions deformation technology, apply the field of force to sample in TEM, so as to realize
Home position observation is carried out to the Monte Carlo method of the same area on sample, provided for the elastic-plastic deformation mechanism of research material
Handedness section.
At present, the type of drive for applying stress loading to microcosmic and macroscopical sample mainly has：Electrostatic drive, memorial alloy drive
The several ways such as dynamic, Piezoelectric Driving, fluid driving, electromagnetic drive and thermal drivers.Wherein electrostatic drive and fluid driving is due to chi
It is very little larger not to be suitable in TEM.And the driving force of electromagnetic drive is smaller and is magnetic and is not also suitable for TEM.Memorial alloy
Drive the output of its power and displacement is unstable not also to be suitable in TEM.The TEM in-situ mechanical specimen holders having been commercialized at present are main
By way of Piezoelectric Ceramic, typical commercially produced product has：654 types of GATAN companies of the U.S. and 671 type mechanics samples
Bar, the PI95 type mechanics specimen holders etc. of Hysitron companies of the U.S..Three-dimensional is driven precision piezoelectric by these commercialization specimen holders
Ceramics are placed in stretching or compression of the sample club body through hole realization to sample；Its advantage is：Test convenience, influenceed without temperature,
Deformation can accurately control, can be with quantification test sample stressing conditions；But because piezoelectric ceramics is located at shaft rear end, limit
Specimen holder therefore it is difficult to ensure that electron beam is incident along the low index crystal plane of sample, and then can not be obtained in the function of verting of Y direction
The clearly full resolution pricture of electron diffraction pattern and atomic scale or sub- angstrom yardstick.
In order to solve the limitation that commercialization specimen holder is unable to double shaft tilting, many seminars, which develop, can implement double shaft tilting
TEM mechanics specimen holder in situ or type of drive.The TEM bimetallic strip drivers of the research and development such as Beijing University of Technology Han Xiao east are (specially
Profit number：CN 200910086803), the principle driven using thermal expansion, it can be realized while big strained tensile deformable material
The function of double shaft tilting, so as to obtain clearly atomic lattice picture and high quality diffraction picture.The advantages of this method, is：
(1) double shaft tilting (X is being ensured:±30°/±20°,Y:± 30 °/± 20 °) on the premise of, realize the loading of face internal force；(2)
By adjusting temperature controller, it can be very good to control its rate of extension, 10 can be realized-5-10-1s-1The tune of strain rate
Control；(3) temperature can realize the big deformational behavior of bimetal leaf less than 100 DEG C, so as to carry out big strained tensile experiment to sample.
The shortcomings that this method, is：(1) driving of bimetal leaf stretcher must lean on temperature control, the deformation mechanism of research material
Meanwhile introduce the influence of temperature, it is difficult to study the deformation mechanism of some temperature-sensitive materials；(2) output driving power is smaller, difficult
With the sample that driving dimensions are big, modulus of elasticity is high.
The TEM original positions deformation technology (patent No. based on V-type beam thermal drivers has been developed in Beijing University of Technology Han Xiao east etc.：ZL
2015 2 0191419.X).Its advantage is：Output displacement is big, and the stretching of sample super large deflection can be achieved.Uniaxiality is good, sample
Shear stress will not be produced in horizontal direction.But simultaneously there is also it is certain the shortcomings that, such as：Its realization driven also relies on temperature
Degree, it is difficult to study the deformation mechanism of some temperature-sensitive materials and because its actuation temperature is higher, be not suitable for coordinating mechanics sensing
The use of device, influence the quantification output of its sample mechanical property.
The content of the invention：
For it is existing the problem of, the invention provides a kind of TEM double shaft tilting in-situ mechanicals based on Piezoelectric Ceramic
Specimen holder, stretcher strain sample in TEM is may be implemented in, and microcosmic microstructure of the home position observation material in drawing process is drilled
Change.Piezoelectric ceramic actuator can provide larger driving force, and realize that drive displacement is controllable.The specimen holder coordinates with TEM and made
With, can under nanometer, the even sub- angstrom yardstick of atom integrated research material mechanical property-microstructure correlation, and
To the SEAD style and high quality full resolution pricture of any crystal grain clearly low index tape spool.
To achieve the above object, the present invention is to be achieved through the following technical solutions：
Transmission electron microscope double shaft tilting in-situ mechanical specimen holder based on Piezoelectric Ceramic, it is characterised in that bag
Include：Sample club body main body and Piezoelectric Ceramic system；Before sample club body main part includes sample club body, shaft
End, swivel angle plate, sample rod rear end, linear stepping motor, drive rod, drive link；Piezoelectric Ceramic components of system as directed is by piezoelectricity
Ceramic microscope carrier, piezoelectric ceramics, connecting seat and the sample stage composition for realizing stretching or compression function；
Sample rod rear end, sample club body and shaft front end are fixed together；Linear stepping motor is consolidated by sealing screw
It is scheduled on sample rod rear end；The center of sample club body is provided with through hole and places drive rod, drives rod rear end and linear stepping motor
Threaded connection；Shaft front end is fixed with swivel angle plate by tiliting axis, and tiliting axis passes through two axis holes that vert of swivel angle plate both sides, and
Axis hole is fixed with verting；
Swivel angle plate generally bilateral symmetry, it is the combination of U-shape structure and boss, boss is bilateral symmetry, bag
Horizontal component and the sloping portion into θ angle with horizontal component are included, θ angles are 30-45 degree；Rotary shaft axle is provided with sloping portion end
Hole；Boss horizontal component one end is provided with boss neck, and centre is provided with the through hole for being easy to electron beam to pass through；The horizontal component of boss
Between U-shaped structure, connecting rod one end is drive rod fixing axle, and the other end is rotary shaft, by rotary shaft and connecting rod by boss
The neck that the centre of horizontal component is provided with is connected with drive rod neck；Sample club body front end both sides Position Design symmetrical two
The motion guide groove of individual insertion, motion guide groove is interior to carry out fixed drive bar provided with drive rod fixing axle, and Constraints driven bar is in straight line stepping
Under motor driving, oscillating rectilinear motion before and after progress, and then swivel angle plate is rotated around tiliting axis；
Via is left in piezoelectric ceramics microscope carrier front end, while there is a screw swivel angle plate front end, on piezoelectric ceramics microscope carrier and swivel angle plate
Under be fixed together, piezoelectric ceramics is fixed with piezoelectric ceramics microscope carrier；Connecting seat one end is connected to piezoelectric ceramics one end, connecting seat
The other end is connected with sample stage.
For the horizontal component of boss between the swivel angle plate of U-shaped, connecting rod one end is drive rod fixing axle, and the other end is rotation
Axle, it is connected by rotary shaft with connecting rod by the neck that the centre of boss horizontal component is provided with drive rod neck.
The motion guide groove of symmetrical two insertions of sample club body front end both sides Position Design, motion guide groove is interior to be provided with driving
Bar fixing axle carrys out fixed drive bar, and Constraints driven bar oscillating rectilinear motion before and after progress, enters under linear stepping motor driving
And swivel angle plate is set to be rotated around tiliting axis.
Further, sample stage is integrally formed using body silicon etching technology, and wherein substrate thickness is 400 μm, housing chi
Very little is 3 × 3mm2, inside is " work " type inside casing, and substrate connects support beam.The support beam other end is connected with mass, mass
For the hook-shaped rectangular flat in two front ends.Go out triangular sample carrying platform in the hook-shaped region etch of mass.Support beam, quality
The thickness of block and sample carrying platform is 60 μm.
Further, sample stage is fixed by gluing mode and piezoelectric ceramics microscope carrier.Sample stage drives with piezoelectric ceramics
Dynamic face keep level, using the power for ensureing to be applied on sample as uniaxial tension power.Mass end uses gluing with connecting seat
Mode connects.By piezoelectric ceramics microscope carrier, piezoelectric ceramics, connecting seat and sample stage being fixed as one platform, it is easy to pass through spiral shell
Nail is fixed on swivel angle plate and dismantles.
Further, the centre of sample club body is provided with the through hole that matches with drive rod to ensure drive rod and piezoelectric ceramics
Wire is fixed on shaft rear end by, motor, and the end of shaft is provided with the electrical interface that can ensure vacuum.
Advantage of the invention is that the TEM original position stretchings experiment under atomic lattice resolution ratio can be carried out, and test big driving
Power is stretched, while driving force and drive displacement are accurately controlled.While sample in-situ mechanical property is obtained, constituency electricity is obtained
Sub- diffraction pattern and high quality full resolution pricture, so as to obtain the more comprehensive microstructure change process of sample.The present apparatus can
It is wide for universal transmission electron microscope, versatility.
Brief description of the drawings：
Fig. 1 is that the double Piezoelectric Ceramics in situ of inclining of TEM stretch sample bar overall structure diagram；
Fig. 2 is that the double Piezoelectric Ceramics in situ of inclining of TEM stretch sample bar front end mplifying structure schematic diagram；
Fig. 3 is piezoelectric ceramics drawing stand and swivel angle plate assembling schematic diagram；
Fig. 4 is sample stage structure enlargement diagram.
Picture is described as follows in picture：
The drive rod fixing axle of 1 sample rod rear end, 2 sample club body, 3 shaft front end, 4 swivel angle plate, 5 drive rod, 6 connecting rod 7
The screw 16 of 14 piezoelectric ceramics of the neck 11 of 8 rotary shaft, 9 tiliting axis 10 motion guide groove 12 sample stage, 13 connecting seat 15 is pressed
The rotary shaft hole 20 of 17 via of electroceramics microscope carrier, 18 boss 19 verts the support beam 24 of 21 square hole of axis hole, 22 substrate housing 23
The sample carrying platform of mass 25.
Embodiment：
Preset screw and be used to fix piezoelectric ceramics microscope carrier in swivel angle plate one end.Piezoelectric ceramics microscope carrier is located above swivel angle plate, with
Swivel angle plate is fitted close, and screw is left in order to be fixed using screw and swivel angle plate in upper end.
Swivel angle plate leaves tiliting axis axis hole, is connected by tiliting axis with sample club body front end.Swivel angle plate lower surface is set
There is boss.Boss includes horizontal component and the sloping portion into θ angle with horizontal component, and θ angles are 30-45 degree in sloping portion end
Provided with rotary shaft axis hole, boss is bilateral symmetry；The horizontal component of boss is between the swivel angle plate of U-shaped, connecting rod one end
For drive rod fixing axle, the other end is rotary shaft, the neck being provided with by rotary shaft and connecting rod by the centre of boss horizontal component
It is connected with drive rod neck.The motion guide groove of symmetrical two insertions of sample club body front end both sides Position Design, motion are led
Carry out fixed drive bar provided with drive rod fixing axle in groove, Constraints driven bar is reciprocal before and after progress under linear stepping motor driving
Formula moves along a straight line, and then swivel angle plate is rotated around tiliting axis.
Below, refer to the attached drawing, the present invention is further described, the exemplary implementation of the present invention is illustrated in accompanying drawing
Example.
Sample rod rear end 1, sample club body 2 and shaft front end 3 are fixed together.Linear stepping motor passes through sealing screw
It is fixed on sample rod rear end 1.The center of sample club body 2 is provided with the through hole being adapted with the size of drive rod 5, after drive rod 5
End is threadedly coupled with linear stepping motor.Shaft front end 3 is fixed with swivel angle plate 4 by tiliting axis, and tiliting axis 9 passes through swivel angle plate 4
Two of both sides are verted axis hole 20, and are fixed with weldering with the axis hole 20 that verts.
The generally bilateral symmetry of swivel angle plate 4, it is the combination of U-shape structure and boss, the boss is symmetrical knot
Structure, including horizontal component and the sloping portion into θ angle with horizontal component, θ angles are 30-45 degree；Rotation is provided with sloping portion end
Rotating shaft axis hole；Boss horizontal component one end is provided with boss neck, and centre is provided with and is easy to electron beam to pass through through hole 21；The water of boss
Flat to be partially embedded between the swivel angle plate of U-shaped, connecting rod one end be drive rod fixing axle, and the other end is rotary shaft, by rotary shaft with
Connecting rod is connected by the neck that the centre of boss horizontal component is provided with drive rod neck.The side position of sample club body front end two is set
The motion guide groove of symmetrical two insertions is counted, motion guide groove is interior to come fixed drive bar, Constraints driven bar provided with drive rod fixing axle
Under linear stepping motor driving, oscillating rectilinear motion before and after progress, and then swivel angle plate is rotated around tiliting axis.
Via 17 is left in the front end of piezoelectric ceramics microscope carrier 16, while there are screw 15, the He of piezoelectric ceramics microscope carrier 16 in swivel angle plate front end
Swivel angle plate is fixed together up and down, and piezoelectric ceramics is fixed by gluing mode and piezoelectric ceramics microscope carrier.Connecting seat one end connects
In piezoelectric ceramics one end, the other end of connecting seat is connected with sample stage.
Boss 18 is linked together by rotary shaft hole 19 and drive link 6, and rotary shaft 8 is inserted in rotary shaft hole 19, is driven
Dynamic connecting rod 6 is linked together by rigid drive rod fixing axle 7 with drive rod 5, and drive rod fixing axle 7 is fixed on sample club body
It can move in the motion guide groove 11 of the both sides of front end 3 and along the tandem of guide groove 11 is moved.By rotary shaft 8 make drive link 6,
The neck that boss neck is provided with the one end of drive rod 5 is connected.
Drive rod 5 is connected with linear stepping motor is used as driving part, is existed by drive rod fixing axle 7 and motion guide groove 11
Effect of contraction on vertical direction, moves along a straight line, while promotes connected drive link 6, and drives front end to vert
Rotation centered on tiliting axis 9 occurs for platform 4.
M1.2 vias 17 are left in the front end of piezoelectric ceramics microscope carrier 16, while there are M1.2 screws 15 front end of swivel angle plate 4, and both can lead to
Cross screw to fix and dismantle, piezoelectric ceramics 14 is cube (2 × 2 × 2mm3) pass through gluing mode and piezoelectric ceramics microscope carrier 16
It is fixed.Connecting seat 13 is to be process using high-accuracy, and the one end of piezoelectric ceramics 14 is connected to using gluing mode,
The other end of connecting seat 13 is connected with sample stage 12.
Sample stage 12 is integrally formed using body silicon etching technology, and its concrete structure is as shown in figure 4, wherein substrate housing 22
Size is 3 × 3mm2, thickness is 400 μm, and inside is " work " type inside casing, and substrate connects support beam 23.The other end of support beam 23 with
Mass 24 is connected, and mass 24 is the hook-shaped rectangular flat in two front ends.24 hook-shaped region etch of mass goes out triangle
Sample carrying platform 25.Support beam 23, mass 24 and the thickness of sample carrying platform 25 are 60 μm.Sample stage 12 passes through
Gluing mode is fixed with piezoelectric ceramics microscope carrier 16, and ensures that triangular sample carrying platform 25 is located under piezoelectric ceramics microscope carrier
Hold the center of square hole 21.By piezoelectric ceramics microscope carrier, piezoelectric ceramics, connecting seat and sample stage being fixed as one platform, it is easy to lead to
It is fixed with dismantling (as shown in Figure 3) on swivel angle plate to cross screw.
In TEM original position stretching experimentations, taken using block sample or nano wire sample made of focused ion beam (FIB)
It is loaded between two triangular sample carrying platforms 25.0-120V voltages are applied to piezoelectric ceramics 14 simultaneously, now piezoelectric ceramics
14 promote connecting seat 13 and sample stage 12, make mass 24 drive left side sample carrying platform 25 to make to be mounted in left movement
TEM sample among sample carrying platform realizes stretcher strain.
Claims (2)
1. the transmission electron microscope double shaft tilting in-situ mechanical specimen holder based on Piezoelectric Ceramic, it is characterised in that including sample
Product club body main body and Piezoelectric Ceramic system；Sample club body main part includes sample club body, shaft front end, verted
Platform, sample rod rear end, linear stepping motor, drive rod, drive link；Piezoelectric Ceramic components of system as directed is carried by piezoelectric ceramics
Platform, piezoelectric ceramics, connecting seat and the sample stage composition for realizing stretching or compression function；
Sample rod rear end, sample club body and shaft front end are fixed together；Linear stepping motor is fixed on by sealing screw
On sample rod rear end；The center of sample club body is provided with through hole and places drive rod, driving rod rear end and linear stepping motor screw thread
Connection；Shaft front end is fixed with swivel angle plate by tiliting axis, and tiliting axis passes through two axis holes that vert of swivel angle plate both sides, and with inclining
Shaft hole is fixed；
Swivel angle plate generally bilateral symmetry, is the combination of U-shape structure and boss, and boss is bilateral symmetry, including water
Flat part and the sloping portion into θ angle with horizontal component, θ angles are 30-45 degree；Rotary shaft axis hole is provided with sloping portion end；
Boss horizontal component one end is provided with boss neck, and centre is provided with the through hole for being easy to electron beam to pass through；The horizontal component of boss is embedding
Between U-shaped structure, connecting rod one end is drive rod fixing axle, and the other end is rotary shaft, by rotary shaft and connecting rod by boss water
The neck that the centre of flat part is provided with is connected with drive rod neck；Symmetrical two of sample club body front end both sides Position Design
The motion guide groove of insertion, motion guide groove is interior to carry out fixed drive bar provided with drive rod fixing axle, and Constraints driven bar is in straight line stepping electricity
Under machine driving, oscillating rectilinear motion before and after progress, and then swivel angle plate is rotated around tiliting axis；
Via is left in piezoelectric ceramics microscope carrier front end, while there is screw swivel angle plate front end, and piezoelectric ceramics microscope carrier and swivel angle plate are solid up and down
It is scheduled on together, piezoelectric ceramics is fixed with piezoelectric ceramics microscope carrier；Connecting seat one end is connected to piezoelectric ceramics one end, connecting seat it is another
End is connected with sample stage.
2. the transmission electron microscope double shaft tilting in-situ mechanical sample according to claim 1 based on Piezoelectric Ceramic
Bar, it is characterised in that：Sample stage is molded using body silicon etching technology integration.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610237986.3A CN105758711B (en) | 2016-04-17 | 2016-04-17 | Transmission electron microscope double shaft tilting in-situ mechanical specimen holder based on Piezoelectric Ceramic |
| US15/387,534 US10103001B2 (en) | 2016-04-17 | 2016-12-21 | Double-tilt in-situ mechanical sample holder for TEM based on piezoelectric ceramic drive |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610237986.3A CN105758711B (en) | 2016-04-17 | 2016-04-17 | Transmission electron microscope double shaft tilting in-situ mechanical specimen holder based on Piezoelectric Ceramic |
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| CN105758711B true CN105758711B (en) | 2018-04-06 |
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| CN107576823A (en) * | 2017-09-05 | 2018-01-12 | 浙江大学 | Nanopositioner for transmission electron microscope sample bar |
| CN109725005B (en) * | 2017-10-27 | 2021-07-27 | 北京纳米能源与系统研究所 | Transmission electron microscope sample rod head and transmission electron microscope sample rod applying same |
| CN108169003B (en) * | 2017-12-23 | 2020-10-27 | 西安交通大学 | Ampere force-based micro-nano material in-situ mechanical property testing device and method |
| CN108550513B (en) * | 2018-05-25 | 2024-05-28 | 兰州大学 | Three-dimensional force transmission electron microscope in-situ sample rod |
| CN109883828B (en) * | 2019-02-28 | 2024-06-25 | 北京工业大学 | Transmission electron microscope in-situ high-temperature quantitative mechanical experiment table |
| CN110006740B (en) * | 2019-03-21 | 2024-06-25 | 北京工业大学 | In-situ heating mechanical sample rod |
| CN111261480B (en) * | 2020-01-31 | 2021-03-23 | 浙江大学 | Transmission electron microscope in-situ sample rod with double-inclination function |
| CN113125475B (en) * | 2021-03-19 | 2022-04-01 | 复旦大学 | Method for in-situ stress application in transmission electron microscope |
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