CN100520351C - Single-nano-thread in-situ mechanical characteristic detection and structure analysis method and apparatus - Google Patents
Single-nano-thread in-situ mechanical characteristic detection and structure analysis method and apparatus Download PDFInfo
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- CN100520351C CN100520351C CNB2006100579895A CN200610057989A CN100520351C CN 100520351 C CN100520351 C CN 100520351C CN B2006100579895 A CNB2006100579895 A CN B2006100579895A CN 200610057989 A CN200610057989 A CN 200610057989A CN 100520351 C CN100520351 C CN 100520351C
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Abstract
Said invented belongs to nano material in situ characterization field. Said invented method contains putting nano line in organic solvent organic solvent, after ultrasonic dispersion 10-30 minute becoming suspension, dropping on metal grid coated with 60-120 nm collodion supporting film to make nano attached at supporting film, fixing metal grid on sample holder and putting in transmission electron microscope, measuring nano line unstretched length and diameter, adjusting transmission electron microscope beam voltage beam voltage as 80 KV to 400 KV and beam density as 20th power of 10 to 8X30th power of 10 electron/square centimeter second, to make collodion supporting film and nano line generating deformation, real time in situ recording nano line structural changes in deformation process, measuring nano line length line length and diameter after deformation, calculating nano length and diameter ratio and maximum strain quantity. Said invented has low cost and simple technology, capable of revealling one dimension nano line mechanical property from nano and atom level.
Description
Technical field:
The present invention relates to the diastrophic method of a kind of single nano-wire original position in transmission electron microscope, utilize the variation that transmission electron microscope can real-time monitored distorted area atomic structure, disclose the deformation mechanism of single nano-wire, belong to the nano material in-situ representational field.
Background technology:
Along with the development of nano-device and the exploitation of micro mechanical system, for the research of mechanical property under external force of single nano-wire show particularly urgent, transmission electron microscope is the strong instrument of research nano material microstructure, but because nanometer material structure is tiny, be difficult to handle, in transmission electron microscope, how the single nano-wire sample is fixed and the original position distortion, disclose nano wire deformation mechanism under external force from nanoscale and atom level, become the difficult problem of pendulum in face of the researchist.At present owing to be subjected to the restriction of laboratory facilities, for the unusual difficulty of the direct measurement of the mechanical property of single nano-wire, and data are more discrete, for example to the measurement of the elastic modulus of carbon nano-tube, diverse ways may differ one to two order of magnitude, and the experiment measuring for the monodimension nanometer material mechanical property mainly contains two kinds of methods at present.
Wherein a kind of is to utilize atomic force microscope that nano wire or pipe are carried out flexural deformation, see " Science " 1997 277 volumes 1971-1975 page or leaf for details, " mechanical property of nanometer bundle; the elasticity of nanometer rods and nanotube; intensity and toughness " (nanobeam mechanics:Elasticity, Strength, and Toughness of Nanorods and Nanotubes), utilize atomic force microscope (AFM) to measure the bending modulus of independent multi-walled carbon nano-tubes and silicon carbide nano bar under the side force pattern, they adopt lithographic printing SiO to be covered and pushes down at low friction MoS
2An end of the multi-walled carbon nano-tubes of deposition on the surface, use AFM to position and measure the size of multi-walled carbon nano-tubes and silicon carbide nano bar then, applying side force along the carbon nano-tube contact point place different again with the silicon carbide nano bar length direction, side force promotes multi-walled carbon nano-tubes, notes the data of side force to amount of deflection.According to the continuous model of considering friction force, side direction concentrated force and beam rigidity data are analyzed at last, match power-sag curve just can obtain the bending modulus of multi-walled carbon nano-tubes.Utilize this model to make beam deflection surpass critical yield point and also obtained carbon nano-tube and silicon carbide nano bar bending strength, this method operating process is complicated, it is bigger that measurement result is received artifical influence factor, though can measure the elastic modulus of nano wire or pipe preferably in the nano material elastic deformation stage, but when surrender takes place material, can not provide the structural change of offset procedure nano wire, can not fundamentally understand its deformation mechanism.
Another kind is the experiment that utilizes the combination stretching single-root carbon nano-tube of scanning electron microscope (SEM) and atomic force microscope, be reported in " Science " 2000 287 volumes 637-640 page or leaf, in their scanning electron microscope two atomic force microscope probes have been installed, two atomic force microscope probes all outwards stretch and parallel to each other, they are bonded at two of single nanotube respectively on the needle point of two probes earlier, then in two ends imposed load and nervous observation under SEM, size according to the pulling force that extends and be subjected to, by calculating the pulling strengrth of single multi-walled carbon nano-tubes and Single Walled Carbon Nanotube, and observed the fracture process that plays nanotube, this method system complex, need higher experimental technique just can obtain reliable experimental, though can utilize the scanning electron microscope in-situ observation to stretch until fracture process, because the restriction of the resolution of scanning electron microscope, still need to put into its fracture behaviour of transmission electron microscope kind observational study after utilizing the last nanotube fracture of this method, can not disclose its deformation mechanism from original position on the atom level, this method complex process, use several different microscopy apparatus just can finish, be unfavorable for penetration and promotion.
Summary of the invention:
Performance test and structure analysis are separately carried out in above-mentioned all nano material mechanics performance tests, problem at the prior art existence, the purpose of this invention is to provide a kind of transmission electron microscope original position real time record the nano wire atomic structure of microcell and method of deformation process under external force utilized, microcell mechanical property and micromechanism directly are mapped, from the mechanical property of nanoscale and atom level announcement one-dimensional nano line.
In order to realize top purpose, the method for single-nano-thread in-situ mechanical test and structure analysis and device thereof comprise transmission electron microscope and can apply the sample supporting film of external force to single nano-wire among the present invention.This sample supporting film is placed on that to utilize electron beam irradiation to take place in the transmission electron microscope Texturized, the nano wire that distributes in the above also can occur bending and deformation along with the distortion of supporting film, utilizes transmission electron microscope to carry out the micro area structure analysis of distorted area simultaneously.
The invention provides the method for a kind of single-nano-thread in-situ mechanical test and structure analysis, it is characterized in that, may further comprise the steps:
1) (for example nano wire is put into the organic solvent that do not react with nano wire, ethanol, acetone) in, ultrasonic dispersing 10-30 minute, be dispersed into suspending liquid, this hanging drop is carried on the net at the metal that scribbles 60-120nm collodion supporting film, make nano wire attached to above the supporting film; The aperture that this metal carries net is 100 order to 1000 orders;
2) metal is carried on the sample holder that net is fixed on standard example of transmission electron microscope bar and put into transmission electron microscope;
3) the original length l of measurement nano wire
0And diameter d
0, the operating parameter of adjusting transmission electron microscope makes the generation of collodion supporting film Texturized; The nano wire that is distributed on the supporting film occurs bending and deformation along with the distortion of supporting film; The transmission electron microscope range of operating parameters is: beam voltage is 80KV to 400KV, and the electron beam beam current density is 10
20To 8 * 10
30Electronics/square centimeter is between second;
4) change by maximum strain regional structure in the deformation process of transmission electron microscope real-time in-situ record nano wire;
5) distortion stops length l and the diameter d that distortion back nano wire is measured in the back, utilizes formula
Calculate the length and the diameter ratio of nano wire,
Calculate the maximum strain amount of nano wire.
By comparative analysis to the real-time full resolution pricture of maximum strain zone reflection nano material microstructure change before and after the distortion, can on nanoscale and atom level, disclose the generation of nano material dislocation in deformation process, and reflection such as the expansion change of crackle material Micromechanics performance institutional framework.
Described sample supporting film is the collodion film, and the material of the nano wire that the thickness of film is measured as required, diameter and length are generally 60-120nm, and is suitable nano wire can be bent into.
Described transmission electron microscope range of operating parameters is: beam voltage is 80KV to 400KV, and the electron beam beam current density is 10
20To 10
30Texturized being advisable takes place with the collodion film irradiation that 60-120nm is thick between second in electronics/square centimeter, and general thicker film needs bigger accelerating potential and electron beam beam current density.
Further, it is that electric conductivity is good that metal carries net, and processing is copper mesh easily, nickel screen and golden net, and the aperture of net is 100 order to 1000 orders, drops in the mesh with the length that is dispersed in the most of single nano-wire on the supporting film to be as the criterion.
Equipment therefor of the present invention comprises transmission electron microscope, and associated example of transmission electron microscope bar and sample holder, and the metal that fixedly scribbles 60-120nm collodion supporting film on this sample holder carries net, and the aperture that this metal carries net is 100 order to 1000 orders.
The method of single nano-wire mechanical property provided by the present invention in site measurement and structure analysis is applicable to diameter at 30-200nm, and length-diameter ratio is greater than 20 nano wire.The smaller nano wire of general length and diameter needs thicker collodion film.
Compare with existing nanometer mechanics measuring method, ingenious sample for use in transmitted electron microscope supporting film and the electron beam-induced collodion deformation of thin membrane of utilizing realized nano wire original position flexural deformation in transmission electron microscope, disclose the microstructure of nano material and the relation of mechanical property from nanoscale and atom level, simultaneously can the home position observation nano wire at the evolution process of deformation process kind structure, and nano wire initial configuration and size are to the influence of its mechanical property.This method does not need to purchase special equipment, having common transmission electron microscope just can implement, having the low technology characteristic of simple of cost, the structure and the mechanical property of nano wire are contacted directly, is a kind of method of testing of single nano-wire mechanical property original position of flexibility and reliability.
Description of drawings
The Si nano wire curls and the flexural deformation feature with collodion among Fig. 1: the embodiment 1, and nano wire along with collodion curls tangible flexural deformation has taken place, and has shown that the Si nano wire has big bending strength
High-resolution atomic diagram picture during the flexural deformation of SiC nano wire has shown the flexural deformation of upper surface lattice among Fig. 2: the embodiment 2 among the figure.
High-resolution atomic diagram picture among Fig. 3: the embodiment 3 after the distortion of SiC nano wire has shown regional area and has begun decrystallized feature among the figure.
High-resolution atomic diagram picture among Fig. 4: the embodiment 4 after the distortion of SiC nano wire has shown lattice stretcher strain feature among the figure
Embodiment 1
Si nano wire powder was placed in the acetone ultrasonic dispersing 20 minutes, is that 100 orders are coated with the golden online of the thick collodion supporting film of 60nm with hanging drop carrying net, golden net is fixed on the sample holder of example of transmission electron microscope bar and puts into transmission electron microscope, at accelerating potential 200KV, adjust the electron beam beam current density and remain on 2 * 10
20Electronics/square centimeter second, irradiation collodion supporting film, supporting film has taken place Texturized, flexural deformation has taken place in the Si nano wire, the diameter of distortion nano wire is 30nm, length is about 3 μ m, the maximum strain amount of nano wire is 2.5%, nano wire still keeps original structure, fracture and plastic yield do not take place, disclosed the Si nano wire and had big bending strength, Fig. 1 has provided crooked transmission electron microscope photo when maximum, Texturized as can be seen collodion supporting film and diastrophic Si nano wire in the photo.
Embodiment 2
SiC nano wire powder is placed in the ethanol, through ultrasonic dispersing 30 minutes, be coated with the hanging drop that disperses on the copper mesh of collodion supporting film in 1000 purposes, collodion supporting film thickness is 80nm, copper mesh is fixed on the sample holder of example of transmission electron microscope bar and puts into transmission electron microscope, at accelerating potential 80KV, adjust the electron beam beam current density and remain on 1 * 10
20Electronics/square centimeter second, irradiation collodion supporting film, supporting film has taken place Texturized, drive distributes thereon and SiC nano wire on every side moves or flexural deformation, wherein a diameter is 200nm, length is that the deformation process of the SiC nano wire of 4.3 μ m has been carried out in site measurement, wherein a SiC nano wire reaches 2% in strain and still keeps the perfect elasticity behavior, Fig. 2 has provided the high-resolution atomic lattice image when maximum flexibility, obvious bending has taken place in crystal display cell, and the electron beam beam current density is risen to 2 * 10
24Electronics/square centimeter second, supporting film continues distortion, stretches fully again after the end unloading of SiC nano wire to be original linearity, and original position has disclosed the super-elasticity behavior of SiC nano wire.
Embodiment 3
The SiC nanometer powder is placed in the ethanol, through ultrasonic dispersing 10 minutes, the hanging drop that disperses is coated with in 300 purposes on the nickel screen of supporting film of collodion, collodion supporting film thickness is 100nm, nickel screen is fixed on the sample holder of example of transmission electron microscope bar and puts into transmission electron microscope, at accelerating potential 300KV, adjust the electron beam beam current density and remain on 8 * 10
25Electronics/square centimeter, irradiation collodion supporting film, supporting film has taken place Texturized, a diameter is 150nm, length is that 15 μ mSiC nano wires are along with flexural deformation has taken place in the supporting film distortion, plastic yield after reaching 2.0%, the maximum deflection elastic strain has taken place, by the full resolution pricture real time record process of SiC nano wire generation plastic yield, Fig. 3 high-resolution atomic lattice image has provided in the compressive stress maximum region and has just begun decrystallized deformation behaviour, last SiC nano wire has been realized plastic yield and necking by decrystallized process progressively, the maximum plastic strain amount has reached 60%, disclose the plastic yield feature and the process of nano grade Sic stupalith in real time by high-resolution atomic diagram picture, the structural change and the plastic yield feature of SiC nano wire are contacted directly, on the atom level, disclosed the superplastic behavior of SiC nano wire.
Embodiment 4
The SiC nanometer powder is placed in the acetone, through ultrasonic dispersing 25 minutes, be coated with the hanging drop that disperses on the copper mesh of collodion supporting film in 400 purposes, collodion supporting film thickness is 120nm, put into transmission electron microscope on the sample holder with copper mesh fixed transmittance electron microscope sample bar, at accelerating potential 400KV, adjust the electron beam beam current density and remain on 8 * 10
30Electronics/square centimeter, irradiation collodion supporting film, supporting film has taken place Texturized, a diameter is that the 40nmSiC nano wire reaches 3% along with stretcher strain has taken place in the supporting film distortion in maximum strain, by the full resolution pricture real time record process of SiC nano wire distortion, find that tangible stretcher strain feature takes place SiC nano wire lattice, and the high-resolution atomic lattice image after the generation of dislocation, Fig. 4 have provided the last stretcher strain of SiC nano wire is arranged.
Claims (3)
1, the method for a kind of single-nano-thread in-situ mechanical test and structure analysis is characterized in that, may further comprise the steps:
1) nano wire is put into the organic solvent that does not react with nano wire, ultrasonic dispersing 10-30 minute, being dispersed into suspending liquid, is that the metal of 60-120nm collodion supporting film carries on the net with this hanging drop scribbling thickness, makes nano wire attached to above the collodion supporting film; The aperture that this metal carries net is 100 order to 1000 orders;
2) metal is carried on the sample holder that net is fixed on the example of transmission electron microscope bar and put into transmission electron microscope;
3) the original length l of measurement nano wire
0And diameter d
0, the operating parameter of adjusting transmission electron microscope makes the generation of collodion supporting film Texturized; The nano wire that is distributed on the collodion supporting film occurs bending and deformation along with the distortion of collodion supporting film; The transmission electron microscope range of operating parameters is: beam voltage is 80KV to 400KV, and the electron beam beam current density is 10
20To 8 * 10
30Electronics/square centimeter is between second;
4) change by maximum strain regional structure in the deformation process of transmission electron microscope real-time in-situ record nano wire;
5) distortion stops length l and the diameter d that distortion back nano wire is measured in the back, utilizes formula
Calculate the length and the diameter ratio of nano wire,
Calculate the maximum strain amount of nano wire.
2, the method for single-nano-thread in-situ mechanical test according to claim 1 and structure analysis is characterized in that it is copper mesh, nickel screen or golden net that described metal carries net.
3, the method equipment therefor of single-nano-thread in-situ mechanical test according to claim 1 and structure analysis, it is characterized in that, this device comprises transmission electron microscope, and associated example of transmission electron microscope bar and sample holder, the metal that fixedly scribbles thickness on this sample holder and be 60-120nm collodion supporting film carries net, and the aperture that this metal carries net is 100 order to 1000 orders.
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| CN101113946B (en) * | 2007-07-20 | 2010-08-04 | 北京工业大学 | Force and electrical behavior testing device under Nanometer lines in-situ compressing in transmission electron microscope |
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