CN104764660A - Thermal-driving uniaxial drawing/compressive deformation device for scanning/transmission electron microscope - Google Patents
Thermal-driving uniaxial drawing/compressive deformation device for scanning/transmission electron microscope Download PDFInfo
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Abstract
The invention discloses a thermal-driving uniaxial drawing/compressive deformation device for a scanning/transmission electron microscope, and belongs to the field of material mechanical property-microscopic structure integrated in situ representation instrument equipment. The integral research on the micro-nano scale material deformation and microscopic structure and physical property evolution is realized. A scanning electron microscope warming table or a transmission electron heating sample rod is used for heating a metal V-shaped beam after corrosion processing, so that the V-shaped beam is thermally expanded. The V-shaped beam is composed of a plurality of thin beams in symmetric structures, the single beam is thermally expanded so as to be bent and deformed under the stress induction; the V-shaped beam can realize the uniaxial deformation of a sample due to the symmetric structure of the thin beams. The uniaxial drawing and uniaxial compressing of the sample can be realized through the change of a geometric structure of the V-shaped beam. The output force and the displacement of the V-shaped beam and the sample deformation rate are regulated through the controlling on the included angle of the V-shaped beam, the three-dimensional geometric size, the heating temperature and the rate. Moreover, the output force of the stress is regulated as drawing force or compressing force through the controlling on the positive and negative of the included angle of the V-shaped beam.
Description
Technical field:
The present invention relates to a kind of scanning/transmission electron microscope thermal drivers uniaxial tension/compression deformation device, can realize carrying out home position observation to the microstructural differentiation of nanometer/atomic scale in material deformation process in conjunction with scanning/transmission electron microscope, simultaneously by the real-time sampling strain information of scanning/transmission electron microscope observing, belong to material mechanical performance-microstructure integration in-situ characterization instrument and equipment field.
Background technology:
When the little extremely micro-nano magnitude of material characteristics yardstick, it is obviously different that strong size effect makes its mechanics, physical property and macroscopic material have.Understand the various mechanical property parameters of material physics as corresponding in Young modulus, tensile strength and Poisson ratio etc., microstructure mechanism, improve the mechanics of material, physical property, for assessing the reliability of various micro-nano device structural design and there is serviceable life important reference value, thus in the urgent need to developing corresponding micro/nano-scale mechanics, physical property-microstructure integration characterizing method, realize carrying out deep research to material behavior and inherent mechanism thereof under micro-nano-scale.
Scanning and transmission electron microscopy is the modernization large-scale instrument and equipment of research material microstructure, their resolution can reach 3-6nm and 0.2nm respectively at present, in fields such as physics, chemistry, material science and life sciences, particularly develop Nanometer scale science and technology field rapidly at present, having a wide range of applications, is one of the strongest research tool.Original position micro/nano-scale mechanics performance testing technology based on scanning or transmission electron microscope can while measurement material mechanical performance, the microscopic damage mechanism that real-time display material is out of shape under state under arms, for studying its failure mechanism, find new phenomenon, development new ideas, new theory and new opplication provide direct experimental basis.
Carry out uniaxial tension or uniaxial compression and carry out on-spot study to microstructural evolution being one of effective ways of research material deformation mechanism to sample at micro/nano-scale.During single shaft distortion, sample uniform force, test findings is explained easily, experimental data highly versatile, therefore carries out uniaxial tension or compression test is one of the most effective experimental technique disclosing material deformation mechanism at micro/nano-scale.At present, uniaxial tension platform that commercialization can be placed in scanning electron microscope is as the Microtest200 of Gatan company, and its displacement motor stepping rate is minimum is 500nm/s; The SEMTESTER100 of MTI instruments company, its displacement motor stepping rate is minimum is 400nm/s, and minimal sample is of a size of 44.5mm × 10mm.The drawing stand of above-mentioned two companies can realize in-situ mechanical in scanning electron microscope and test the function combined with displaing microstructure observing, but the step-wise displacement of these devices is comparatively large, for the material of micro-nano size as samples such as nano wires, can break sample instantaneously.The autograph that Han Xiaodong etc. are authorized to is propose the device that two kinds are placed in scanning electron microscope stretching/compressing micro/nano-scale sample in the patent of invention of " method of single-nano-thread in-situ mechanical test and structure analysis and device thereof " (number of patent application: CN200610057989.5) and " in scanning electron microscope nano-thread in-situ stretching device and method " (number of patent application: CN200610169839.3), two kinds of devices well solve the large difficult problem of commercialization drawing stand displacement stepping, achieve the stretching of micro/nano-scale sample and the combination of home position observation, but an extra acting force can be added in Sample Width direction, although this power is less, only can cause the lateral shift that sample is small, but still the single shaft power of collimation can not be provided, therefore they are devices of a kind of approximate uniaxial tension.
At present, based on the mechanics test device of transmission electron microscope, the PI 95 type specimen holder that the 654 and 671 type specimen holders produced as: Gatan company of the U.S. and Hysitron company of the U.S. produce all can realize stretching to micro/nano-scale sample or Compressive Mechanical test, but above-mentioned commercialization mechanical test specimen holder is owing to adopting Piezoelectric Driving mode, two function of inclining cannot be realized, limit the process that on-spot study material microstructure develops from atomic scale.For the problems referred to above, the nomination that Han Xiaodong etc. are authorized to is the stretching/compressing technology proposed in the patent of invention of " nano material in stress condition power electrical property and microstructure measurement apparatus and method " (number of patent application: CN200810240516.8) based on thermometal hot driver, achieves and apply uniaxially load and double shaft tilting in transmission electron microscope.But as previously mentioned, the uniaxial tension that this thermometal Driving technique cannot be realized ideal, thermometal driver wouldn't realize mass production on the other hand, in addition not enough with the assembling controllability of transmission electron microscope carrier net, have impact on controllability and the accuracy of driving force output.
At present, the type of drive of micro/nano-scale single shaft microdrive mainly contains Piezoelectric Driving, Electromagnetic Drive, electrostatic driving and electrothermal drive etc.Piezoelectric type driving is more difficult provides tensile force in face; Electromagnetic type drives and can produce stronger magnetic field in the course of work and affect Electron Beam Focusing; Electrostatic driving is higher to technological requirement, somewhat expensive and driving force and displacement less.Electrothermal drive is by being fixed on suprabasil semi-girder temperature distortion, and free end extends and is tied and produces driving force and displacement.Because electrothermal drive mode can provide face inner drive, its can with transmission electron microscope double shaft tilting specimen holder with the use of, carry out the mechanical stretch/compression verification of sample while realizing double shaft tilting.This type of drive is mainly applied in MEMS (micro electro mechanical system) based on silicon micromechanical structure at present.Gianchandani and Najafi is at " Journal ofMicroelectromechanical Systems " (VOL.5, NO.1,1996) autograph delivered on is the V-type girder construction that is prepared into of proposition polysilicon membrane first in the article of " Bent-Beam Strain Sensors ".Que etc. are at " Journal of Microelectromechanical Systems " (VOL.10, NO.2,2001) autograph delivered on is utilize V-type girder construction to make electric heating driver in the article of " Bent-Beam ElectrothermalActuators-Part I:Single Beam and Cascaded Devices ".The advantage of these V beams processed by body silicon etching is that after energising, response is fast, driving force and displacement comparatively large (driving compared to electrostatic), but the machining process of silicon micromechanical structure is complicated, and needs electrified regulation, has a certain impact to electron beam.
The present invention devise a kind of technique simple, without the need to energising, can the metal forming V-type beam hot driver of mass production, scanning electron microscope/transmission electron microscope can be placed in, microstructure in nanometer/atomic scale home position observation micro/nano-scale sample uniaxial tension or compression deformation process, simultaneously by the real-time sampling strain information of scanning/transmission electron microscope observing.
Summary of the invention:
The problem that the processing technology existed for prior art is complicated, cost is high, the invention provides a kind of preparation method simple, based on the scanning/used in transmission electron microscope micro/nano-scale thermal drivers original position stretching/compression deformation technology of V-type beam.At present, there is no the relevant report this technology being applied to micro/nano-scale sample uniaxial tension/compression in scanning/transmission electron microscope.
Utilize commercialization scanning electron microscope warm table or the heating of transmission electron microscope heated sample bar, occur bending and deformation after making V-type beam expanded by heating, owing to driving the symmetric geometry of beam, the stress that V-type beam produces is parallel to the axis of sample.Being equipped on the nano wire on sample stage, nanofiber, nano-pillar or nano thin-film etc. can by uniaxial tension or compression.Utilize scanning/transmission electron microscope can the Monte Carlo method process under external force such as original position real time record nano wire, nanofiber, nano-pillar or nano thin-film, microcell distortion is directly mapped with micromechanism, discloses mechanical property and the deformation mechanism of nano wire or film.
In order to realize object above, the present invention realizes by the following technical solutions:
A kind of scanning/used in transmission electron microscope micro/nano-scale thermal drivers original position uniaxial tension/compression deformation device, is characterized in that: comprise a frame support section, two central support portion and two drive parts; Wherein: frame support section is rectangular shaped rim, central support portion is rectangular beam, and without connecting between central support portion and frame support section; Drive part is many parallelogram beams; Each several part thickness is identical, and the upper and lower surface of each several part is in same plane respectively; Drive part one end is connected with frame support section, and the other end is connected with central support portion;
Described two central support portion alignment along its length; Two parts spacing is between 30 μm ~ 1mm; The two ends of sample are individually fixed on the adjacent end of two central support portion, and the part that sample is stretched/compresses is positioned at the gap between two central support portion;
One end of every root beam is connected with frame support section, one end is connected with central support portion, and every root beam all exists one in contrast in the beam that central support portion length direction becomes rotational symmetry to distribute, by central support portion, often pair of beam be symmetric forms the structure of " V " word shape.
Further, two described central support portion along its length spacing between 30 μm ~ 1mm.
Further, described drive part comprises many become 2 ~ 45 ° of angles inclined beams with central support portion length direction.
After drive part is heated, central support portion is driven to move along the tip direction of " V " word shape; When the opening direction of " V " word shape structure of two drive parts is relative, realize the stretch function to sample, when the tip direction of " V " word shape structure of two drive parts is relative, realize the compression function to sample.
Described frame support section, central support portion and drive part adopt wet etch techniques preparation, first spin coating photoresist on metal foil, utilize the reticle of processing, photoresist is exposed, then develop, and then immerse corrosive liquid, frame support section, central support portion and drive part described in release window obtains.
Further, described frame support section, central support portion and drive part are that thermal conductivity is good, and thermal expansivity is large, and the metal formings such as the aluminium of easily processing, copper and molybdenum.
Further, the photoetching in thermal drivers original position stretching/compression deformation device employing Micrometer-Nanometer Processing Technology and the method for wet corrosion technique, metal goes out V-structure by wet etching, and one-shot forming.
Scanning/used in transmission electron microscope thermal drivers original position stretching/compression deformation device, it is characterized in that the V-type beam of drive part is made up of multipair beam, one end of every root beam is connected with frame support section, and the other end is connected with central support portion.Then be fixed in scanning electron microscope focused ion beam double-beam system by thermal drivers original position stretching/compression deformation device, prepare micro/nano-scale drawn samples by focused ion beam, these sample two ends are fixed on two central support portion respectively.
When thermal drivers original position stretching/compression deformation device be fixed on scanning electron microscope warm table or on transmission electron microscope heated sample bar time, along with the rising of thermal station temperature, V-type fine strain of millet body produces thermal expansion, and then make V-type back point place generation acting force make central support portion produce displacement vertically, the sample be fixed on central support portion is stretched distortion, realizes micro-move device function.
Because V-type beam adopts the drives structure relative to central support portion symmetric design, under heating condition, two ends drive beam to produce identical thermal expansion, and therefore central support portion moves vertically, realizes uniaxial tension.
Be fixed on the nano wire of central connection part, nanofiber, nano-pillar or nano thin-film by two-way stretch/compression deformation, the strain rate of sample can regulate by controlling heating rate, and when the temperatures return to ambient conditions, V-type beam is returned to original position.Therefore, this V-type beam is adapted to the stretching/compressing fatigue experiment that driving sample carries out low week equally.
The material of the nano wire measured as required, nanofiber, nano-pillar or nano thin-film, size and mechanical characteristic performance (Young modulus, elastic strain, yield strength, fracture strength) thereof, can realize the driving force of different size by the logarithm adjusting the width of beam, thickness and beam; The drive displacement of different size is realized from the angle of central support portion length direction by the length and beam that adjust beam; For the sample of stretching nanoscale, the range of adjustment 0.5-5mm of V-type beam length, the range of adjustment of width is 0.03-0.1mm, and the range of adjustment of thickness is 0.03-0.1mm, and this range of size is much smaller than the size of sample platform of scanning electronic microscope; For the sample of stretching micron or mm size, corresponding increase in the scope that the three-dimensional dimension of V-type beam can allow at sample platform of scanning electronic microscope; The range of adjustment of beam and horizontal direction angle absolute value is 2 ~ 45 °, and experimental and theoretical computation shows, when angle absolute value is 2 ~ 5 °, can produce larger drive displacement.The type (stretch, compress) of V-type beam power output can regulate by regulating the angle between beam and horizontal direction, when angle is 2 ~ 45 °, exports drawing stress; When angle is-2 ~-45 °, output squeezing stress.
In material deformation process, utilize the in-situ dynamic observation that the systems such as scanning electron microscope imaging system, elemental analysis system, microstructure characterizations system (as: EBSD-EBSD, various spectrometer) or transmission electron microscope imaging, diffraction, constituent analysis can realize the pattern of material under stress-strain effect, composition, microstructural Evolution, disclose the deformation mechanism of material from nanometer/atomic scale.
Further, the present invention is based on semiconductor fine process technology, first utilize photoetching technique to be formed in metal foil surface to drive, the figure of frame and central support portion, then utilize metal wet etch techniques, release window, forms thermal drivers original position stretching/compression deformation device.
Thermal drivers original position stretching/compression deformation technology of the present invention is carried out original position dynamic tensile/compression verification to nano wire or film and is implemented as follows:
1. with conducting resinl, nano wire, nanofiber, nano-pillar or nano film are fixed on central support portion.
2. this thermal drivers original position stretching/compression deformation device is assembled in scanning/transmission electron microscope heating arrangement.
3. pair thermal drivers original position stretching/compression deformation device heats, along with the rising of temperature, V-type beam produces stretching or compressible drive power on central support portion, stretches, compresses nano wire fixed thereon, nanofiber, nano-pillar, nano-pillar or nano thin-film and deform.
4. by picture system, elemental analysis system, the microstructure analysis system of scanning electron microscope/transmission electron microscope, the pattern in real time record nano wire, nanofiber, nano-pillar or nano thin-film deformation process, composition, microstructural Evolution.
The present invention has the following advantages:
1. the present invention devises and a kind ofly provides and be out of shape micro/nano-scale material and match the hot actuating device of driving force, realize uniaxial tension/compression nano material in scanning/transmission electron microscope, provide a kind of novel nano material in-situ deformation technology, there is dependable performance, structure be simple, preparation method is simple, can the feature of mass production, expanded the function of scanning/transmission electron microscope.
2. expand after the thermal drivers original position stretching/compression deformation device in the present invention is heated and produce driving effect, control method is simple, is easy to realize in scanning/transmission electron microscope; Simultaneously compact, easy for installation, can load scanning/transmission electron microscope, easily not by its space constraint.
3. the thermal drivers original position stretching in the present invention/compression deformation device adopts two-step process to realize, process simplification compared with silicon technology, and significant cost reduces.
4. the thermal drivers original position stretching/compression deformation device in the present invention can regulate driving force and displacement by adjustment metal material kind or geometric parameter in a big way, can be widely used in the distortion of millimeter, micron and nanometer sized materials.
Accompanying drawing explanation
Fig. 1 (a) V-type beam stretching hot actuating device schematic diagram; (b) V-type beam compression heat drive unit schematic diagram.
In figure, each several part is described as follows:
1 frame support section 2 central support portion 3 drive part 4 is stretched/compression verification sample
Fig. 2 utilizes V-type beam drive unit Copper thin film to be carried out to the scanning electron microscope shape appearance figure of stretching experiment in scanning electron microscope: before (a) stretches; B () breaks after.
Fig. 3 utilizes V-type beam drive unit the Copper thin film of focused ion beam cutting preparation to be carried out to the transmission electron microscope shape appearance figure of stretching experiment in transmission electron microscope: before (a) stretches; B () breaks after.
Embodiment:
Below in conjunction with accompanying drawing, the present invention will be further described:
Choose 100 μm of thick aluminum foils of twin polishing, Copper Foil or molybdenum foil, after cleaning, drying, at the positive glue of its tow sides spin coating photoetching, then drying glue, the reticle prepared is aimed at Copper Foil face exposure, immerse developer solution and obtain drive part figure except after glue, the V-type beam width of drive part 3 is 100 μm, length is 700 μm, with the angle 15 ° of stretching vertical direction, frame support section 1 is of a size of 15mm × 8mm, the width on every limit is 1.5mm, central support portion 2 is 500 μm along the length of draw direction, width is 200 μm, central support portion 2 is 30 μm along the spacing of draw direction.Phosphoric acid, acetic acid and deionized water are made into etchant solution in the ratio of 1:1:2, metal forming immersed corrosive liquid after 65 seconds, window discharges, obtain the one-body molded drive unit of drive part 3, frame support section 1, central support portion 2, remove the residual photoresist of apparatus surface finally by the alcohol boiled and acetone.In scanning electron microscope focused ion beam double-beam system, utilize focused ion beam to prepare the nano thin-film drawn samples 4 be fixed on central support portion 2, then the drive unit carrying sample is fixed in scanning electron microscope warm table or transmission electron microscope heated sample bar.By warm table or the heating of heated sample pole pair drive unit, the V-type beam of drive part 3 drives central support portion 2 to move vertically, and the nano material distortion that stretches, utilize scanning/transmission electron microscope Real Time Observation record sample deformations process simultaneously.Fig. 2 and 3 is respectively and utilizes thermal drivers original position stretching deformation device in scanning electron microscope/transmission electron microscope to the shape appearance figure of the in-situ tensile test that Copper thin film sample carries out.(a) in Fig. 2 and 3 is the pattern of sample before stretching, and (b) is the pattern after breaking.Can find out, this thermal drivers original position stretching/compression deformation device can realize stretching or compression function to sample while scanning or transmission electron microscope in-situ observation.
Claims (6)
1. scanning/used in transmission electron microscope micro/nano-scale thermal drivers original position uniaxial tension/compression deformation device, is characterized in that: comprise a frame support section, two central support portion and two drive parts; Wherein: frame support section is rectangular shaped rim, central support portion is rectangular beam, and without connecting between central support portion and frame support section; Drive part is many parallelogram beams; Each several part thickness is identical, and the upper and lower surface of each several part is in same plane respectively; Drive part one end is connected with frame support section, and the other end is connected with central support portion; Described two central support portion alignment along its length; Two parts spacing is between 30 μm ~ 1mm; The two ends of sample are individually fixed on the adjacent end of two central support portion, and the part that sample is stretched/compresses is positioned at the gap between two central support portion; One end of every root beam is connected with frame support section, one end is connected with central support portion, and every root beam all exists one in contrast in the beam that central support portion length direction becomes rotational symmetry to distribute, by central support portion, often pair of beam be symmetric forms the structure of " V " word shape.
2. scanning according to claim 1/used in transmission electron microscope micro/nano-scale thermal drivers original position uniaxial tension/compression deformation device, is characterized in that: two described central support portion along its length spacing between 30 μm ~ 1mm.
3. scanning according to claim 1/used in transmission electron microscope micro/nano-scale thermal drivers original position uniaxial tension/compression deformation device, is characterized in that: described drive part comprises many become 2 ~ 45 ° of angles inclined beams with central support portion length direction.
4. scanning according to claim 1/used in transmission electron microscope micro/nano-scale thermal drivers original position uniaxial tension/compression deformation device, is characterized in that: after drive part is heated, and drives central support portion to move along the tip direction of " V " word shape; When the opening direction of " V " word shape structure of two drive parts is relative, realize the stretch function to sample, when the tip direction of " V " word shape structure of two drive parts is relative, realize the compression function to sample.
5. scanning according to claim 1/used in transmission electron microscope micro/nano-scale thermal drivers original position uniaxial tension/compression deformation device, is characterized in that: described frame support section, central support portion and drive part adopt the metal forming of aluminium, copper or molybdenum to process.
6. scanning according to claim 1/used in transmission electron microscope micro/nano-scale thermal drivers original position uniaxial tension/compression deformation device, it is characterized in that: described frame support section, central support portion and drive part adopt wet etch techniques preparation, first spin coating photoresist on metal foil, utilize the reticle of processing, photoresist is exposed, then develop, and then immerse corrosive liquid, frame support section, central support portion and drive part described in release window obtains.
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| CN110335801A (en) * | 2019-05-29 | 2019-10-15 | 北京工业大学 | A kind of pulling and pressing integrated formula driver of thermo bimetal and preparation method thereof |
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