CN101252073A - Thermal drive deforming transmission electric mirror grid and one-dimensional nano material deforming method - Google Patents
Thermal drive deforming transmission electric mirror grid and one-dimensional nano material deforming method Download PDFInfo
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- CN101252073A CN101252073A CNA2008101034940A CN200810103494A CN101252073A CN 101252073 A CN101252073 A CN 101252073A CN A2008101034940 A CNA2008101034940 A CN A2008101034940A CN 200810103494 A CN200810103494 A CN 200810103494A CN 101252073 A CN101252073 A CN 101252073A
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Abstract
The invention relates to a thermally driven deforming transmission electron microscope grid and a one-dimensional nano material deformation method, belonging to the nano device and the transmission electron microscope original position nano material deformation method field. The prior grid can be deformed only through electron beam irradiation and the stress supplied is limited. The grid of the invention is as follows: a metallic film A and a metallic film B are vapor-plated on a supporting film of the prior grid, and the thermal expansion coefficient of the metallic film A is more than that of the metallic film B. The one-dimensional nano material deformation method by adoption of the grid is as follows: after the metallic film A and the metallic film B are cut open, one-dimensional nano materials are dispersed on the metallic film A and the metallic film B which are then placed into a transmission electron microscope for heating; the two cracked films are curled due to difference of the expansion coefficients, thereby the driving force for deformation of the one-dimensional nano materials is provided and deformation of the one-dimensional nano materials is realized. The grid can realize large-angle roll steer in two directions of X and Y and realize the original position deformation operation of the one-dimensional nano materials; moreover, the grid is characterized in reliable performance, convenient assembly and simple structure and expands the function of the transmission electron microscope.
Description
Technical field
The invention belongs to original position nano material deformation method field in nano-device and the transmission electron microscope, be specifically related to a kind of heat driving distortion transmission electron microscope and carry net and monodimension nanometer material deformation method.
Background technology
Because the high resolution capability of transmission electron microscope, the information of nanoscale even atomic scale can be provided, it is the strong instrument of research material microstructure, it is at physics, chemistry, material science, fields such as life science have a wide range of applications, particularly developing nano science and technical field rapidly at present, is one of powerful tool the most.It is to be used for supporting detected sample that transmission electron microscope carries net, and the skeleton that present the most frequently used transmission electron microscope carries net is generally copper mesh, and is furnished with the amorphous carbon supporting film on the copper mesh.Generally speaking, these years, net can only carry detected sample, and transmission electron microscope can only be observed the static tissue structure that is distributed in these years of online sample, can not utilize these years nets that sample is handled, and carried out dynamic in situ detection.Along with MEMS (micro electro mechanical system) (MEMS, micro electromechanical system) and receive Mechatronic Systems (NEMS, nano electromechanical systerm) development, for single nano-wire or film mechanical property research under external force show particularly urgent, but because single nano-wire or membrane structure are tiny, be difficult to handle, in transmission electron microscope, how single nano-wire or nano thin-film sample are fixed and the original position distortion, deformation mechanism and dimensional effect become the difficult problem of pendulum in face of the researcher under external force to disclose nano material from nanoscale and atom level.At present in transmission electron microscope owing to be subjected to sample stage and the extremely limited space of pole shoe, generally be 1～3mm, for the unusual difficulty of the direct measurement of the manipulation of single nano-wire or nano thin-film and mechanical property, that has reported in the document mainly contains three kinds of methods under atomic scale resolution.
A kind of is that method is reported in " Applied physics letters " 2002 80 the 21st phases of volume, its cardinal principle is to utilize the piezoceramics film of special deposition (PZT) as carrying net, with research thin film deposition on the piezoelectric ceramic surface, net will be carried and sample is put into transmission electron microscope with the sample for use in transmitted electron microscope bar that can switch on, realize stretching and squeeze operation in the distortion of effect of electric field lower piezoelectric pottery, utilize the fatigue fracture change procedure of transmission electron microscope imaging system recording sheet simultaneously film.This method sample making process is complicated, because the restriction of specimen holder tilt angle (generally can only single shaft vert or twin shaft vert ± 5 °), can not under the optimum resolution situation, (high-resolution atomic scale) carry out home position observation, can not fundamentally understand its deformation mechanism.
Another kind method is reported in 281 pages of 2006 439 volumes of 236802 pages of " Physics Review Letters " 2005 the 94th volumes and " Nature " respectively, its cardinal principle is that the scanning tunnel microscope probe is put into the transmission electron microscope kind, utilize outer connected control system control probe motion to handle single-root carbon nano-tube, realization is to the stretcher strain of carbon nano-tube, utilize the probe of conduction to realize in energising the carbon nano-tube behavior of high temperature superplastic deformation and fracture mechanism under the function of current have been found in the stretching of carbon nano-tube.Though this method can realize the atom resolution to well-designed sample, and stretch simultaneously and switch on measurement, but because comparatively complex mechanical construction is put into the sample for use in transmitted electron microscope chamber, sample stage can only low-angle be verted (± 5 °) or can only single shaft be verted (being no more than ± 20 °), still limit its range of application, be unfavorable for penetration and promotion.
281 pages of 2006 439 volumes of 236802 pages of 2007 the 94th volumes of the third method report and " Nano Letters " and " Advanced Materials ", it mainly is to utilize a kind of special carbon film, the carbon film that utilizes electron-beam-irradiation induced to break takes place to curl, thereby realize disperseing the crooked and stretching of the monodimension nanometer material on it, this method can realize that the wide-angle twin shaft verts, thereby can obtain the full resolution pricture of original position between deformation phases, and experimentation is simple, cost is not high.But utilize the curling controllability of electron-beam-irradiation induced carbon film relatively poor, the applying and the difficult control of strain rate of stress, and also the stress that provides is limited, and the bigger material of some intensity is difficult to be out of shape.
In the above-mentioned transmission electron microscope in-situ nano material mechanical performance test, preceding two kinds of sample manipulations platforms or carry a net and can not realize all that wide-angle is two and incline, for major part need Real Time Observation structural change under external force under positive tape spool nano material, its application is restricted.And the controllability of the third method is relatively poor, and the stress that provides is limited, and many materials are not suitable for this kind method.
Summary of the invention
The objective of the invention is to, solve the problems of the prior art, and provide a kind of wide-angle that can realize to vert, the heat that controllability is strong drives the method that the distortion transmission electron microscope carries net and monodimension nanometer material is out of shape.
Provided by the present invention year net comprises skeleton (1) and the evaporation supporting film (2) on skeleton (1), it is characterized in that, also comprises metallic film A (3) (claim not only active layers) and metallic film B (4) (but also claiming passive layer); Wherein, metallic film A (3) evaporation is on supporting film (2), and metallic film B (4) evaporation is on metallic film A (3), and the thermal coefficient of expansion of metallic film A (3) is greater than the thermal coefficient of expansion of metallic film B (4).
Wherein, the thickness of described metallic film A (3) and B (4) is 20～50nm.In order to guarantee to realize bigger flexural deformation at a lower temperature, the ratio bending of two kinds of metallic film A (3) and B (4) is greater than 10/10
-6℃
-1, as some commercial bimetal leaf materials, metallic film A (3) can be Mn75Ni15 or Ni20Mn6Fe74 or Mn72Ni10Cu18 etc.; Metallic film B (4) can be Ni36Fe64 or Ni42Fe58 etc.
Provided by the present invention year net, make as follows: adopt the physical evaporation coating process, (commonly used to carry a net generally be to be skeleton with the copper mesh to carry the upper surface of the supporting film (2) of net at conventional transmission electron microscope, evaporation carbon film on copper mesh), metallic film A (3) that the two-layer expansion coefficient difference of evaporation is bigger and B (4).
Provided by the present invention year net comprises the steps: the method that monodimension nanometer material is out of shape
1) will carry the metallic film A (3) and the prefabricated micro-crack of B (4) (5) (can draw gently by blade and split film or other appropriate methodology) of net;
2) monodimension nanometer material is carried out ultrasonic dispersion after, drip on the metallic film B (4) that transmission electron microscope carries net;
3) transmission electron microscope that heat is driven distortion carries net and is fixed on the heatable sample for use in transmitted electron microscope bar, puts into transmission electron microscope;
4) find metallic film B (4) micro-crack (5) to locate monodimension nanometer material and observe where, and carry out the fixing of sample, utilize heating pole to heat then carrying net by the method for electron beam welding;
5) the high-resolution atomic diagram by transmission electron microscope changes as deformation process and the lattice structure that real-time in-situ writes down nano wire.
Along with the rising of temperature, because metallic film A (3) is different with the thermal coefficient of expansion of B (4), micro-crack (5) is located to take place to curl, and then stretches or crooked monodimension nanometer material fixed thereon.By comparative analysis to the real-time full resolution pricture of monodimension nanometer material microstructure change before and after the distortion, can on the atom level, disclose the characteristics of monodimension nanometer material in elastic-plastic deformation, the dimensional effect of distortion, the generation of dislocation in the deformation process, and the heterogeneous microstructure of reflection such as the expansion change in crack material mechanical performance.
The present invention has following advantage:
1, heat provided by the present invention drives the distortion transmission electron microscope and carries net, can realize carrying the temperature distortion of mesh film, carry net overall dimension and prior art carry net in full accord, can pack into easily in the high-resolution-ration transmission electric-lens, can realize X, Y both direction wide-angle vert (the two heating stations that incline of commercialization at present can reach ± 30 °/± 60 °).
2, the present invention's heat drives the distortion transmission electron microscope and carries net to the monodimension nanometer material deformation method, has realized the original position deformation operation of monodimension nanometer material, has dependable performance, and is easy for installation, characteristic of simple structure, the function of having opened up transmission electron microscope.
Description of drawings
Fig. 1, heat drive the cross-sectional structure schematic diagram that the distortion transmission electron microscope carries net.
The transmission electron microscope that Fig. 2, heat drive distortion carries the net transmission electron microscope photo.
The transmission electron microscope photo of the curling stretching Si nano wire after Fig. 3, metallic film A (3) and B (4) are heated.
Embodiment
Embodiment
Adopt conventional physical evaporation coating process, make heat driving distortion transmission electron microscope and carry net, as shown in Figure 1, be furnished with supporting film (2) (carbon film) on the skeleton (1) (copper mesh), the upper surface of supporting film (2) evaporation successively has metallic film A (3) and metallic film B (4); Wherein, metallic film A (3) adopts the Mn72Ni10Cu18 alloy to make, and metallic film B (4) adopts the Ni36Fe64 alloy to make, and the thickness of metallic film A (3) is 30nm, and the degree of metallic film B (4) is 30nm.
Utilize heat to drive the distortion transmission electron microscope and carry the distortion of net monodimension nanometer material:
1) will carry the metallic film A (3) of net and B (4) with more prefabricated micro-cracks of blade (5), as shown in Figure 2, black region is a skeleton (1) (copper mesh), and grey circular hole zone is supporting film (2) (carbon film), metallic film A (3) and metallic film B (4), and blank space is micro-crack (5);
2) ultrasonic oscillation is scattered Si nano wire (in absolute ethyl alcohol) drips on year net metallic film B (4);
3) will carry net is fixed on the transmission electron microscope heated sample bar;
4) net is carried in heating, utilizes transmission electron microscope to observe the distortion of a nano wire and carries out nanoscale or the atomic scale recording process.
By observation, find that the Si nano wire shows big strain plasticity between deformation phases, this is different from the fragility of its body material, and Si shows under nanoscale and the big different mode of texturing of block materials, as shown in Figure 3.
It should be noted that at last: above embodiment only in order to the explanation the present invention and and unrestricted technical scheme described in the invention; Therefore, although this specification has been described in detail the present invention with reference to the above embodiments,, those of ordinary skill in the art should be appreciated that still and can make amendment or be equal to replacement the present invention; And all do not break away from the technical scheme and the improvement thereof of the spirit and scope of invention, and it all should be encompassed in the middle of the claim scope of the present invention.
Claims (5)
1. a heat drives the distortion transmission electron microscope and carries net, comprises skeleton (1) and the evaporation supporting film (2) on skeleton (1), it is characterized in that, also comprises metallic film A (3) and metallic film B (4); Wherein, metallic film A (3) evaporation is on supporting film (2), and metallic film B (4) evaporation is on metallic film A (3), and the thermal coefficient of expansion of metallic film A (3) is greater than the thermal coefficient of expansion of metallic film B (4).
2. year net according to claim 1 is characterized in that, the thickness of described metallic film A (3) is 20～50nm.
3. year net according to claim 1 is characterized in that, the thickness of described metallic film B (4) is 20～50nm.
4. year net according to claim 1 is characterized in that, the ratio bending of described metallic film A (3) and B (4) is greater than 10/10
-6℃
-1
5. a monodimension nanometer material deformation method is characterized in that, may further comprise the steps:
1) transmission electron microscope is carried the metallic film A (3) and the prefabricated micro-crack of B (4) (5) of net;
2) monodimension nanometer material being dispersed in the radio mirror carries on the metallic film B (4) of net;
3) the radio mirror that will be loaded with monodimension nanometer material again carries net and is fixed on the sample for use in transmitted electron microscope heating pole;
4) carry net by the heating pole heating, make metallic film A (3) and B (4) take place to curl, the distortion monodimension nanometer material.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2008101034940A CN101252073A (en) | 2008-04-07 | 2008-04-07 | Thermal drive deforming transmission electric mirror grid and one-dimensional nano material deforming method |
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| CNA2008101034940A CN101252073A (en) | 2008-04-07 | 2008-04-07 | Thermal drive deforming transmission electric mirror grid and one-dimensional nano material deforming method |
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| CN101252073A true CN101252073A (en) | 2008-08-27 |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102236160A (en) * | 2010-04-29 | 2011-11-09 | 武汉新芯集成电路制造有限公司 | Sample observation grid and manufacturing method thereof |
| CN103954487A (en) * | 2014-04-28 | 2014-07-30 | 浙江大学 | Method for preparing in-situ tensile sample for transmission electron microscope |
| CN105185679A (en) * | 2014-06-17 | 2015-12-23 | 清华大学 | TEM (transmission electron microscope) micro-grid |
| CN107132241A (en) * | 2017-04-24 | 2017-09-05 | 中国石油大学(北京) | A kind of method welded in Electronic Speculum in the original location to nano material |
| CN110632105A (en) * | 2019-09-17 | 2019-12-31 | 东南大学 | Liquid sample cavity for transmission electron microscope characterization and preparation method thereof |
| CN110729162A (en) * | 2019-09-17 | 2020-01-24 | 东南大学 | High-mesh-number micro grid loading net for transmission electron microscope characterization and preparation method thereof |
| CN113933325A (en) * | 2021-10-14 | 2022-01-14 | 思通检测技术有限公司 | Method for preparing transmission electron microscope sample from rubber in stretching state and performing transmission electron microscope characterization |
-
2008
- 2008-04-07 CN CNA2008101034940A patent/CN101252073A/en active Pending
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102236160A (en) * | 2010-04-29 | 2011-11-09 | 武汉新芯集成电路制造有限公司 | Sample observation grid and manufacturing method thereof |
| CN102236160B (en) * | 2010-04-29 | 2013-05-01 | 武汉新芯集成电路制造有限公司 | Sample observation grid and manufacturing method thereof |
| CN103954487A (en) * | 2014-04-28 | 2014-07-30 | 浙江大学 | Method for preparing in-situ tensile sample for transmission electron microscope |
| CN105185679A (en) * | 2014-06-17 | 2015-12-23 | 清华大学 | TEM (transmission electron microscope) micro-grid |
| CN105185679B (en) * | 2014-06-17 | 2017-04-12 | 清华大学 | TEM (transmission electron microscope) micro-grid |
| CN107132241A (en) * | 2017-04-24 | 2017-09-05 | 中国石油大学(北京) | A kind of method welded in Electronic Speculum in the original location to nano material |
| CN107132241B (en) * | 2017-04-24 | 2019-06-25 | 中国石油大学(北京) | A method of nano material is welded in Electronic Speculum in situ |
| CN110632105A (en) * | 2019-09-17 | 2019-12-31 | 东南大学 | Liquid sample cavity for transmission electron microscope characterization and preparation method thereof |
| CN110729162A (en) * | 2019-09-17 | 2020-01-24 | 东南大学 | High-mesh-number micro grid loading net for transmission electron microscope characterization and preparation method thereof |
| CN110729162B (en) * | 2019-09-17 | 2021-10-19 | 东南大学 | High-mesh-number micro grid loading net for transmission electron microscope characterization and preparation method thereof |
| CN113933325A (en) * | 2021-10-14 | 2022-01-14 | 思通检测技术有限公司 | Method for preparing transmission electron microscope sample from rubber in stretching state and performing transmission electron microscope characterization |
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Open date: 20080827 |