CN104634660A - Device and method for performing in-situ double-tilting single-axis stretching on nanowire and two-dimensional laminar thin film in transmission electron microscope - Google Patents
Device and method for performing in-situ double-tilting single-axis stretching on nanowire and two-dimensional laminar thin film in transmission electron microscope Download PDFInfo
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Abstract
The invention relates to a device and a method for performing in-situ double-tilting single-axis stretching on a nanowire and a two-dimensional laminar thin film in a transmission electron microscope, belonging to the field of in-situ mechanical performance measurement research of transmission electron microscope accessories and a nanomaterial. The device comprises a supporting part, a power part and a carrying network part. The supporting part is a metal ring; the driving part is a thermal double-metal sheet, one end of the double-metal sheet is fixedly arranged on the metal ring, the other end of the double-metal sheet generates driving force through bending and moving caused by heat expansion; the carrying network can carry a nanomaterial and is adhered onto the free end of the double-metal sheet, the heated bent double-metal sheet stretches the carrying network, so that the stretching effect of the nanomaterial can be achieved. According to the device, the axial stretching of a single nanowire, and stretching of single-layer/multilayer two-dimensional thin films can be realized conveniently, the problems that the nanowire and the thin film in the original double-metal sheet technology are difficult to fix and poor in stability can be solved, and the structure evolution of the material during deformation can be observed.
Description
Technical field
The present invention relates to a kind of device in transmission electron microscope situ atomic scale research nano wire, the mechanical property of two-dimensional layer film in uniaxial tension process and drawing process.The invention belongs to nano material microstructure in-situ characterization instrument and equipment technical field.
Background technology
Along with the development of nano-device and the exploitation of micro mechanical system, the research of single nano-wire and two-dimensional film mechanical property under external force seems particularly important.Because the structure of nano material is tiny, transmission electron microscope (hereinafter referred to as transmission electron microscope) is made to become the important tool of research nano material.But the pole shoe of transmission electron microscope is very little, generally in a few millimeter, want be fixed nano material in narrow space like this and apply stress, and the atomic scale deformation mechanism observing nano material is in situ very difficult.
Beijing University of Technology Han Xiao east seminar started to have developed a series of deformation device (patent No.: 200910086803.2 based on carbon support membrane and thermo bimetal from 2006, ZL200610057989.5, ZL200610144031.X, ZL200710122092.0,200810056836.8, ZL200820078706.X, 200810103494.0 etc.), make nano material can be captured deformation mechanism (the Nano Letters 7 of atomic size in situ under stretching, bending, compression deformation condition, 452-457,2007; Advanced Materials 19,2112-2118,2007; Nature Communications 1,24:1-8,2010; Nano Letters13,3812-3816,2013).
Wherein based on the deformation technology of carbon support membrane, its principle of work is that metal nano wire being randomly dispersed in carbon support membrane carries on the net (carbon film is scratched in advance), and a part of nano wire is just distributed in the crack place of carbon film.When sample is subject to the radiation of electronics in transmission electron microscope, the position that carbon film breaks can occur curling, thus the stretching realized nano wire or flexural deformation.Because nano wire is distributed on carbon film randomly, the draw direction of nano wire and draw speed are difficult to control, and success ratio is low.In addition, be connected between nano wire with carbon film by Van der Waals force, this just requires that the diameter of nano wire is 30nm ~ 80nm, and length-diameter ratio is greater than 100.Therefore, based on the deformation technology restricted application (nano wire that longer and diameter is less is difficult to preparation) of carbon support membrane.
For the deformation device based on thrermostatic bimetal-plate, its principle of work is by the heating of transmission electron microscope heated sample bar, and because bimetallic thermal expansivity difference causes its swell increment different, when heating in order to coordinate this species diversity, thermometal can produce flexural deformation.Two panels thermometal symmetric offset spread, one end is fixed on the becket that external diameter is 3mm, and the other end fixes nano material, and after being heated, the bimetallic free end of two panels bends to different directions, thus applies to stretch or compression stress to material.This device can be used for the stretching experiment of one-dimensional nano line and the two-dimensional nano-film material be prepared from through nanoprocessing from massive material, but due to the preparation condition of sample harsh, the manufacturing cycle of one-dimensional nano line is long, and the probability gone wrong is large; And for membraneous material, be applicable to the membraneous material prepared by magnetically controlled sputter method, the research of their deformation mechanism substantially can not be realized to the single or multiple lift membraneous material (as Graphene, platelike molybdenumdisulfide etc.) with layer structure.And, due to the limitation of technology, be bonded at two the bimetallic strip spacing comparatively large (more than 20 μm) on becket, make the nano material of lift-launch unsettled more, easily shake in drawing process, thus be difficult to the observation realizing stable pulling and atomic scale.
In addition, U.S. Hysitron company develops a kind of PTP device (US8434370B2) stretched for nano wire of business.Principle of operation is the outshot of pushing PTP device, by four springs of device surrounding, compression is changed into stretching.The shortcoming of this device is that utilization factor is low, not reproducible utilization, and needs to coordinate special specimen holder to use, and expensive, cost is very high.
Therefore develop one can stretch nano wire and two-dimensional layer film again can restrained stretching direction, and the pervasive device not high to sample requirement, is still this area problem demanding prompt solution.
Summary of the invention
For prior art Problems existing, the invention provides a kind of method of transmission electron microscope situ two incline single-axle units and stretching nano wire, two-dimensional layer film.This device combines primarily of thrermostatic bimetal-plate and a year net, may be used for realizing, to nano wire and two-dimensional layer film original position uniaxial tension, also not losing the wide-angle double shaft tilting function of transmission electron microscope in transmission electron microscope simultaneously.This device can be applicable to the research of nano wire and two-dimensional layer thin film mechanical performance-microstructure integration under atomic scale.
To achieve these goals, the present invention realizes by the following technical solutions:
The two uniaxial stretching device that inclines of transmission electron microscope situ, is characterized in that, it comprises support section, drive part and carries net three part, support section (1) is metal ring, and the inner side of metal ring is provided with a horizontal support platform, drive part (2) for two panels parallel and have the bimetallic strip of spacing, bimetallic strip is by nonmagnetic, the different two panels metal of thermal expansivity is overlayed by weldering and is combined formation, the thickness of two panels bimetallic strip is equal, symmetrically arrange, two relative metals of inner side are that thermal expansivity is relatively large, two relative metals of outside are that thermal expansivity is relatively little, wherein one end of two panels bimetallic strip is all vertically fixed on the brace table of becket (1) inner side, the other end is free end, carry net (3) for having ductility, wire netting with holes, be fixed on the free end of drive part (2), carry net (3) parallel with drive part (2).
Described support section external diameter is preferably 3mm, internal diameter is 2mm, and the brace table inside metal ring and ring forms horse-hof shape, and " water chestnut platform " is for one end of fixing bimetallic strip, the material of becket is the metal or alloy of copper, molybdenum or other heat conduction, and thickness is between 25 μm ~ 30 μm.
Thrermostatic bimetal-plate one end is fixed on becket, and the other end can move freely, the thrermostatic bimetal-plate free end length of preferred drive part is greater than 1000 μm, the spacing of two thrermostatic bimetal-plates 100 μm ~ 200 μm, symmetrically arrange, the thermal expansivity difference of two metals is more large more obvious, as copper and titanium, the large metal of thermal expansivity is in inner side, the little metal of thermal expansivity is in outside, when this device is heated, two panels bimetallic strip is respectively to outer lateral bend, (deformation displacement can according to thermal expansion coefficient difference as being less than 1 μm for deformation displacement, any condition of the conditions such as temperature regulates), uniaxial tension distortion can be equal to by approximate for the distortion of material.Carry net (3) and be fixed on one end that thrermostatic bimetal-plate can move freely, the described net (3) that carries is prepared by wet etch techniques.When thrermostatic bimetal-plate is respectively towards outer lateral bend, stretches and carry net (3), and then the nano wire/film carrying and carry on the net that stretches.
Within foregoing year, net (3) preferred overall length is 400 μm, wide 80 μm, 2 μm, aperture, and material used is the metal (as aluminium) that ductility is good, is prepared from by wet etch techniques.Utilize the aluminium film that the method for magnetron sputtering spraying plating 500nm on the silicon chip designing figure is thick, soak in acetone, dissolving photoresist can obtain aluminum and carry net.
Adopt the method for said apparatus stretching nano wire, it is characterized in that, comprise the following steps:
(1), nano wire is put into organic solvent nonreactive with it (such as ethanol), utilize ultrasound wave vibration dispersion (10 ~ 30 minutes, determine according to the cluster degree of nano wire) become suspending liquid, hanging drop is inclined on the surface of uniaxial stretching device transmission electron microscope situ is two;
(2), in room temperature after abundant drying, focused ion beam Scanning election microscope is utilized to carry the distribution situation of the nano wire on net 3 surface, select radial parallel in draw direction and the nano wire ridden on hole, make it fix at the two ends platinum gas aggradation of nano wire;
(3) on the heated sample bar, two for the transmission electron microscope situ carrying nano wire uniaxial stretching device that inclines loaded in transmission electron microscope, control heating platen temperature, two panels bimetallic strip is heated bending respectively to both sides, thus year net that stretches, and drive nano wire to stretch, measure displacement and strain by the length variations measuring nano wire in transmission electron microscope.
Adopt the method for said apparatus stretching two-dimensional layer film, it is characterized in that, comprise the following steps:
(1), by two-dimensional layer film (such as Graphene) transferring to transmission electron microscope situ pair inclines on the surface of uniaxial stretching device, and fully dry at room temperature, two-dimensional layer membraneous material can utilize the legal systems such as chemical vapor deposition standby;
(2), two for the transmission electron microscope situ carrying two-dimensional layer film uniaxial stretching device that inclines is loaded heated sample bar, control heating platen temperature, two panels bimetallic strip is heated bending respectively to both sides, thus year net that stretches, and drive two-dimensional layer film stretching.Film and carry a Netcom and cross Van der Waals force and be combined and just can well realize stretching, without the need to extra process.
This device and transmission electron microscope heated sample bar match, and can be implemented in high-resolution-ration transmission electric-lens and stretch to carried monoatomic layer membraneous material, meanwhile, can also observe material plasticity deformation process and structural evolution under atomic scale.The method makes to be easy to fix by the nano material two ends of carrying, sample stability is good, less demanding to sample size, and can control the rate of extension of nano wire/film by convenience and high-efficiency, has more universality.
The present invention has the following advantages:
1, the present invention is to the design driving the device of nano material to innovate in transmission electron microscope, utilize thrermostatic bimetal-plate and carry net and realize nano wire and the distortion of two-dimensional layered structure membraneous material under transmission electron microscope situ atomic scale, for the deformation mechanism disclosing nano wire and two-dimensional layered structure membraneous material provides convenient, efficient method.This technology effectively can control the draw direction of nano wire, realizes the stretching of two-dimensional layer film, and sample size only need reach more than 2 μm.
2, the present invention utilizes heated sample bar, manually can regulate the degree of crook of thrermostatic bimetal-plate by control temperature, can control rate of deformation.
3, thrermostatic bimetal-plate of the present invention can reuse, and each stretching experiment terminates rear available sand paper and grinds off a year net, uses new year net, cost and price cost of saving time.
4, the present invention makes to be easy to fix by the nano material two ends of carrying, sample stability is good, less demanding to sample size, has more universality.
Accompanying drawing illustrates:
The two uniaxial stretching device vertical view that inclines of Fig. 1 transmission electron microscope situ;
Fig. 2 bimetallic strip bends schematic diagram;
Fig. 3 nano silver wire original position stretching transmission electron microscope picture group.Wherein, (a) is the transmission electron microscope picture before nano wire stretches; (b, c) be transmission electron microscope picture in nano wire drawing process, nano wire is elongated and then occurs constriction.
Fig. 4 Graphene original position stretching transmission electron microscope picture group;
Wherein, (a) is the transmission electron microscope picture before Graphene stretches; B () is that Graphene is stretched the transmission electron microscope picture after splitting.
Accompanying drawing is described as follows:
1, becket 2, thrermostatic bimetal-plate 3, year net.
Embodiment:
Do specific descriptions below in conjunction with accompanying drawing to the present invention to illustrate, but the present invention is not limited to following examples.
Transmission electron microscope situ two incline uniaxial tension nano wire, two-dimensional layer membrane unit, is characterized in that it comprises support section, drive part and carries net three part.Described support section is the becket 1 of external diameter 3mm, internal diameter 2mm, and inside structure is horse-hof shape, and " water chestnut platform " is for one end of stationary heat bimetallic strip.The material of becket is the copper that thermal conductivity is good, and thickness is between 25 μm ~ 30 μm.Drive part is thrermostatic bimetal-plate 2, and material used is the metal (as copper and titanium) that nonmagnetic, thermal expansivity differs greatly, and free end length is greater than 1mm, and the spacing of two panels thrermostatic bimetal-plate is 100 μm ~ 200 μm.Thrermostatic bimetal-plate symmetrically arranges, and the large metal of thermal expansivity is in inner side, and the little metal of thermal expansivity is in outside, and one end is fixed on becket, and the other end can move freely.Carry net 3 and be fixed on one end that thrermostatic bimetal-plate can move freely, be adhesive in the free end of thrermostatic bimetal-plate 2 with AB, when thrermostatic bimetal-plate 2 is respectively towards outer lateral bend, pulls and carry a net 3, and then stretch and carry the online nano wire/film carried.The described net 3 that carries is prepared by wet etch techniques, and total length is 400 μm, wide 80 μm, 2 μm, aperture.
For nano wire, the present invention is utilized to realize the step of stretcher strain as follows:
1, nano wire is put into organic solvent nonreactive with it (such as ethanol), (determining according to the cluster degree of nano wire) becomes suspending liquid to utilize ultrasound wave vibration dispersion 10 ~ 30 minutes, is inclined on the surface of uniaxial stretching device transmission electron microscope situ is two by hanging drop.
2, in room temperature after abundant drying, utilize focused ion beam Scanning election microscope to carry the distribution situation of the nano wire on net 3 surface, select radial parallel in draw direction and the nano wire ridden on hole, make it fix at the two ends platinum gas aggradation of nano wire;
3, two for the transmission electron microscope original position of carrying nano wire uniaxial stretching device that inclines is loaded heated sample bar.Controlling warm table makes bimetallic strip bend respectively to both sides, thus stretch year net and a nano wire, and the speed of restrained stretching can be carried out by control temperature.Displacement and strain can be measured by the length variations measuring nano wire in transmission electron microscope.
Accompanying drawing 3 is shown in the stretching of nano wire.
For two-dimensional layer membraneous material, the present invention is utilized to realize the step of stretcher strain as follows:
1, the two-dimensional layer membraneous material (such as Graphene) utilizing the legal systems such as chemical vapor deposition standby being transferred to transmission electron microscope situ pair inclines on uniaxial stretching device, fully dry at room temperature;
2, two for the transmission electron microscope situ carrying two-dimensional layer film uniaxial stretching device that inclines is loaded heated sample bar, by warm table control temperature, make thermo bimetal's bending tablet, stretch and carry net and film.Film and carry a Netcom and cross Van der Waals force and be combined and just can well realize stretching, without the need to extra process.
Accompanying drawing 4 is shown in the stretching of two-dimensional layer film.
Claims (5)
1. the two uniaxial stretching device that inclines of transmission electron microscope situ, is characterized in that, it comprises support section, drive part and carries net three part, support section (1) is metal ring, and the inner side of metal ring is provided with a horizontal support platform, drive part (2) for two panels parallel and have the bimetallic strip of spacing, bimetallic strip is by nonmagnetic, the different two panels metal of thermal expansivity is overlayed by weldering and is combined formation, the thickness of two panels bimetallic strip is equal, symmetrically arrange, two relative metals of inner side are that thermal expansivity is relatively large, two relative metals of outside are that thermal expansivity is relatively little, wherein one end of two panels bimetallic strip is all vertically fixed on the brace table of becket (1) inner side, the other end is free end, carry net (3) for having ductility, wire netting with holes, be fixed on the free end of drive part (2), carry net (3) parallel with drive part (2).
2., according to the two uniaxial stretching device that inclines of the transmission electron microscope situ of claim 1, it is characterized in that, support section becket external diameter is 3mm, and internal diameter is 2mm, and thickness is between 25 μm ~ 30 μm; Bimetallic strip length is greater than 1000 μm, the spacing of two panels bimetallic strip 100 μm ~ 200 μm; Carrying net (3) length is 400 μm, wide 80 μm, 2 μm, aperture.
3., according to the two uniaxial stretching device that inclines of the transmission electron microscope situ of claim 1, it is characterized in that, the material of support section becket is the metal or alloy of heat conduction, and two metals of bimetallic strip are respectively copper and titanium, and the material of carrying net (3) is aluminium.
4. adopt the two uniaxial stretching device stretching nano wire that inclines of arbitrary transmission electron microscope situ of claim 1-3, comprise the following steps:
(1), by nano wire put into organic solvent nonreactive with it, utilize ultrasound wave vibration dispersion to become suspending liquid, hanging drop is inclined on the surface of uniaxial stretching device at transmission electron microscope situ pair;
(2), in room temperature after abundant drying, focused ion beam Scanning election microscope is utilized to carry the distribution situation of the nano wire on net (3) surface, select radial parallel in draw direction and the nano wire ridden on hole, make it fix at the two ends platinum gas aggradation of nano wire;
(3) on the heated sample bar that the two uniaxial stretching device that inclines of transmission electron microscope situ, step (2) being carried nano wire loads in transmission electron microscope, control warm table, it is bending respectively to both sides that heating makes two panels bimetallic strip be heated, thus year net that stretches, and drive nano wire to stretch, measure displacement and strain by the length variations measuring nano wire in transmission electron microscope.
5. adopt the two uniaxial stretching device stretching two-dimensional layer film that inclines of arbitrary transmission electron microscope situ of claim 1-3, comprise the following steps:
(1), two-dimensional layer film transfer is inclined on the surface of uniaxial stretching device to transmission electron microscope situ is two, fully dry at room temperature;
(2), two for the transmission electron microscope situ carrying two-dimensional layer film uniaxial stretching device that inclines is loaded heated sample bar, control warm table, it is bending respectively to both sides that heating makes two panels bimetallic strip be heated, thus year net that stretches, and drive two-dimensional layer film stretching.
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