CN100590412C - Nano-wire in-situ stretching device in scanning electron microscope and method therefor - Google Patents
Nano-wire in-situ stretching device in scanning electron microscope and method therefor Download PDFInfo
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- CN100590412C CN100590412C CN200610169839A CN200610169839A CN100590412C CN 100590412 C CN100590412 C CN 100590412C CN 200610169839 A CN200610169839 A CN 200610169839A CN 200610169839 A CN200610169839 A CN 200610169839A CN 100590412 C CN100590412 C CN 100590412C
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Abstract
The invention relates to a scanning electron microscope nanometer line original tensile device and method. It controls the heater to make the dual metal plate bending, drive slide of dual metal platemoving linearly along the track to both sides, tensile the nanometer line fastened on the sample bench, recording the tensile acted plastic tensile deformation and fracture failure, matching the dynamic performance of the nanometer line and the microstructure change, revealing the tensile deformation mechanism, fracture failure mode, brittle-ductile transition and so on of one dimension nanometerdynamic performance. It is simple, easy to control, realizing the original position one line measurement of the nanometer line dynamic feature.
Description
Technical field:
The present invention relates to a kind of in scanning electron microscope the device and method of original position stretching nano wire, utilize the structural change of scanning electron microscope in can real-time monitored nano wire stretcher strain process, disclose the deformation mechanism of nano wire under tensile load, the brittle-ductile transition mode belongs to nano material mechanics performance in-situ fields of measurement.
Background technology:
Along with the development of nanometer technology and the exploitation of nano-device, nano wire is the elementary cell of nano-device, and nano wire not only has character such as good electricity, magnetic, light, also will require to carry in device mechanical load, and transmission power is carried out motion etc.Nano wire mechanical response mode and failure mode under external force, for example brittle fracture or ductile rupture, maximum breaking strain amount, will influence the reliability of device, therefore study single nano-wire mechanical response and military service behavior under external force, the mechanical performance data of accumulation nano wire is the stock criterion of current design and exploitation nano-device.The main method of single nano-wire mechanical property in-situ test has at present, the original position high-frequency electric field excitation resonance method in transmission electron microscope and scanning electron microscope, original position bending method, pulling method etc.Wherein stretching is the most direct Mechanics Performance Testing means, scanning electron microscope is because easy to operate, the space, sample chamber is bigger, it is the strong instrument of research nanometer material structure and performance, but because nanometer material structure is tiny, be difficult to handle, how the single nano-wire sample fixed and the uniaxial tension distortion in scanning electron microscope, mechanical property and deformation mechanism that original position discloses nano wire are the difficult problems of current nanometer mechanics research.At present owing to be subjected to the restriction of laboratory facilities, directly measure very difficultly for the stretcher strain of single nano-wire/pipe, wherein bibliographical information has been arranged for the experimental measurement method of the mechanical property of one dimension carbon nano-tube under the uniaxial tension stress.
This method is reported in " Science " 2000 287 volumes 637-640 page or leaf, be that two cover atomic force microscope (AFM) probes are installed in the scanning electron microscope (SEM), the carbon nano-tube that will be adsorbed on the afm tip by in-situ chemical vapor deposition in SEM is fixed, it is vertically opposite to adjust the AFM probe, move one of them AFM probe stretching single-root carbon nano-tube and home position observation under SEM by imposed load, according to the size of the pulling force that is subjected to and the degree of elongation, calculate the pulling strengrth of single multi-walled carbon nano-tubes and Single Walled Carbon Nanotube, and can directly observe the fracture process of nanotube.This method is integrated, and several precision equipments are worked simultaneously, control and operating system complexity, and the higher experimental technique of needs just can obtain reliable experimental, is unfavorable for penetration and promotion.Because afm tip is thinner, the fixing relatively difficulty of nano wire on needle point is difficult to be suitable for for thicker nano wire or the bigger this method of nano wire of intensity simultaneously.
Summary of the invention:
Problem at the prior art existence, the purpose of this invention is to provide a kind of nano wire stretcher strain device that is installed in the scanning electron microscope, utilize the mode of scanning electron microscope original position real time record nano wire elastic and plastic deformation process and fracture failure under stretching action, the maximum breaking strain amount of the nano wire of different-diameter and material, the fracture mechanical property and the microstructure change of nano wire directly are mapped, disclose the mechanical property of one-dimensional nano line from nanoscale.
In order to realize top purpose, single-nano-thread in-situ stretching device and method in the scanning electron microscope among the present invention, it is characterized in that: comprise base 1 and the well heater 2 that is fixed on the base, the reeded support 3 of fixed band above the well heater 2, two groove the insides on the support utilize trip bolt 9 to fix two bimetallic strips 7 respectively, and bimetallic strip 7 is connected with a pair of slide block 5 respectively.Guide rail 4 is fixed on above the base 1, and guide rail 4 is parallel with support 3, and is vertical with bimetallic strip 7.A pair of slide block 5 is arranged on above the guide rail 4, and the adjustable sample stage 6 of a pair of horizontal level is set respectively above two slide blocks 5, regulates slit between two sample stage when room temperature between several microns, guarantees that long nano wire can be across between two sample stage.
Support 3 and add the top cover 8 that can play insulation effect above the bimetallic strip 7.By well heater 2 heated holder 3, the heat that is transmitted on the bimetallic strip 7 occurs bending and deformation bimetallic strip 7, bimetallic strip drive slide block 5 along guide rail 4 to the both sides rectilinear motion, the sample stage 6 that is fixed on above the slide block is understood the nano wire that stretching is fixed on the sample stage two ends, make nano wire generation two-way stretch distortion, utilize the scanning electron microscope imaging system to write down the deformation process of nano wire and the structure and the morphology change of microcell simultaneously successively.
The present invention also can use a bimetallic strip 7, makes a slide block movement, and another slide block maintains static, and realizes the unilateral stretching distortion to nano wire.
Further, described bimetallic strip is that the different metal film stack of linear expansion coefficient is welded together, when temperature variation,, cause bimetallic strip to the bent distortion of the little lateral bending of linear expansion coefficient because of two kinds of different materials linear expansion coefficient differences of bimetallic strip produce different expansions and contraction.The installation of bimetallic strip guarantees when being heated two lateral movements to guide rail among the present invention, and the bimetallic strip rear drive slide block movement that is heated is fixed on sample stage on the slide block and realizes stretcher strain to nano wire.Among the present invention,, recommend to use than crooked greater than 10/10 in order to guarantee to realize at a lower temperature bigger flexural deformation
-6℃
-1Bimetallic strip
Further, well heater of the present invention is an electric resistance heater, comprises controlled power of direct current, and temperature indicator (TI), and 0-350 ℃ of the linear temperature increase scope of well heater can be adjusted the heating rate of well heater according to the strain rate of setting.
Further, the slit between two sample stage can be finely tuned on slide block, and the end face and the upper surface of sample stage are level and smooth, and roughness is less than 100nm, and (20-30 ℃) adjustment two sample stage closely contact when room temperature, and contact gap is less than 3 μ m.
Further, described stretching device is fixed in the scanning electron microscope sample chamber, the sample drawing stand well heater that assembles is placed on the sample platform of scanning electronic microscope, set the heating rate of well heater, sample stage is heated, under the scanning electron microscope image formation state, observe the motion of drawing stand, home position observation is fixed on the process of the stretcher strain and the fracture of the nano wire on the drawing stand, directly calculate the preceding maximum strain variable of nano wire fracture from the image of original position order record, disclose the mode of the brittle-ductile transition of nano wire, size effect from the feature image of fracture.By changing heating rate, change the nano wire tensile strain rate.
The using method of apparatus of the present invention is implemented as follows:
1. nano wire is put in the organic solvent (for example, ethanol, acetone etc.) that does not react with sample, ultrasonic dispersing 10-30 divides kind, and hanging drop on sample stage, is made the nano wire stochastic distribution and attached on the sample stage.
2. the nano wire overlap joint that utilizes mechanical arm to pick up under optical microscope to be distributed on the sample stage also is fixed on two sample stage, makes the axis of nano wire consistent with draw direction.Stretching device is placed in the scanning electron microscope.
3. make scanning electron microscope keep vacuum tightness 2 * 10
-4The high vacuum state that Pa is above, the heating rate according to setting applies voltage to well heater well heater is started working.
4. utilize the deformation process of scanning electron microscope original position record sample stage pulling nano wire, utilize formula by the length of nano wire before and after the distortion of scanning electron microscope record
Calculate the maximum breaking strain amount of nano wire, wherein l0 is the length of nano wire before stretching, and l is the length of nano wire after the stretcher strain.
5. the nano wire to tension failure carries out the observation of different amplification by high resolution scanning electron microscope to the pattern of fracture, and the microstructure change contrast of nano wire discloses the deformation mechanism and the mechanism of fracture of nano wire, size effect before and after the fracture.Perhaps by the control heating rate, change the nano wire tensile strain rate, the in-situ observation strain rate is to the influence of nano wire fracture process and failure mode.
Compared with prior art, the present invention is simple in structure, control is convenient, advantages such as strain rate is controlled, can in scanning electron microscope, work easily, can once observe the elastic deformation that many nano wires take place simultaneously in the experiment under extended state, plastic yield and unstable fracture process, can realize the mechanical property measurement of nano wire under the differently strained speed by the control heating rate, because the bimetallic strip driving force is bigger, go for all length-diameter ratios greater than 5 monodimension nanometer material, even diameter is that micron-sized fiber and whisker also can in site measurements.This method is utilized the imaging of scanning electron microscope original position order, the mechanical property and the micromechanism of nano wire directly are mapped, can explain the elastic-plastic deformation mechanism of monodimension nanometer material of different materials and different-diameter and the form of fracture failure from microcosmic, brittle-ductile transition mechanism discloses the unusual mechanical property of monodimension nanometer material.
Description of drawings
Fig. 1 is the theory structure synoptic diagram of nanometer stretching platform provided by the invention, nano wire be dispersed in two can the slide block of relative motion on.
Wherein: 1 base, 2 well heaters, 3 supports, 4 guide rails, 5 slide blocks, 6 sample stage, 7 bimetallic strips, 8 top covers, 9 trip bolts.
The SiC nano wire that one of Fig. 2 is stretching
SiC nano wire (b) the SiC nano wire that two of Fig. 3 (a) are stretched is simultaneously broken
Embodiment:
Further describe the present invention below in conjunction with the drawings and the specific embodiments.
Nano-thread in-situ stretching device in the scanning electron microscope, according to FEI Quanta 200 environmental scanning electron microscopes and the design of JEOL JSM 6500F field emission scanning electron microscope, the length and width height of this device is 30mm * 20mm * 10mm, can be installed in the scanning electron microscope sample chamber easily, the trade mark that bimetallic strip is selected for use is 5J20110, than crooked 20.8/10
-6℃
-1, 0-350 ℃ of the linear intensification scope of well heater, 0.1 ℃ of control accuracy, two sample stage adjustable range when room temperature keeps≤2 μ m, and maximum linear displacement range is 5mm, displacement accuracy 0.2 μ m.The nano wire of SiC will be prepared, be placed on ultrasonic dispersion 60min in the acetone, to be suspended in nano wire random dispersion in the acetone on two sample stage of stretching device, the nano wire overlap joint that utilizes mechanical arm to pick up under optical microscope to be distributed on the sample stage also is fixed on two sample stage, make the axis of nano wire consistent with draw direction, the device integral body that will fix nano wire is then put into scanning electron microscope, shut scanning electron microscope sample chamber door, be evacuated down to the scanning electron microscope working range.Adjust scanning electron microscope electron beam micro imaging system, sweep parameter makes electron beam focus on tested nanowire surface, receives secondary electron image.Adjust heating power supply, add thrermostatic bimetal-plate, make thermometal drive sample stage stretching SiC nano wire, Fig. 2 is placed on stretching device in the JEOL JSM6500F field emission scanning electron microscope, two ends fix, the SiC nano wire that is being stretched, and the mean diameter of nano wire is 85nm.Fig. 3 (a) is placed on two SiC nano wires that are stretched simultaneously of FEI Quanta 200 environmental scanning electron microscopes with stretching device, mean diameter is respectively 88nm and 100nm, two SiC nano wires that show among Fig. 3 (b) are all broken, graphical analysis from the original position record, bigger elastic deformation and plastic yield have all taken place in two SiC before fracture, wherein Fig. 3 (b) SiC nano wire is stretched, and fracture back one end is rapid to jump, the other end is seen tangible necking, shown the feature of ductile rupture, by measuring the preceding elongation of nano wire fracture, the average breaking strain that calculates two SiC nano wires is respectively 11% and 25.6%, and strain rate is respectively 3.2 * 10
-9M/s and 6.6 * 10
-9M/s, big elasticity and plastic yield have all taken place in two SiC nano wires before fracture, and the SiC of body material at low temperatures breaking strain between 0.1%-0.2%, and show as brittle fracture, by nano-thread in-situ stretching device and method in the scanning electron microscope, disclosed material unusual mechanical property under nanoscale.
Claims (3)
1, nano-thread in-situ stretching device in a kind of scanning electron microscope, it is characterized in that: comprise base (1) and be fixed on well heater (2) on the base, the reeded support of fixed band (3) above the well heater (2), fix an end of two bimetallic strips (7) inside two grooves on the support respectively with trip bolt (9), the other end of two bimetallic strips (7) is connected with a pair of slide block (5) respectively;
Guide rail (4) is fixed on above the base (1), and guide rail (4) is parallel with support (3), and is vertical with bimetallic strip (7); A pair of slide block (5) is arranged on above the guide rail (4), and the adjustable sample stage of a pair of horizontal level (6) is set respectively above two slide blocks (5), when bimetallic strip (7) guarantees to be heated when mounted to guide rail (4) two lateral movements.
2, nano-thread in-situ stretching device in a kind of scanning electron microscope according to claim 1 is characterized in that: described support (3) and add a top cover (8) above the bimetallic strip (7).
3, a kind of use stretching device as claimed in claim 1 carries out nano-thread in-situ drawing process in the scanning electron microscope, it is characterized in that, may further comprise the steps:
1) nano wire is put into the organic solvent that does not react with sample, ultrasonic dispersing 10-30 divides kind, and hanging drop on sample stage, is made the nano wire stochastic distribution and attached on the sample stage;
2) nano wire that utilizes mechanical arm will be randomly dispersed on the sample stage under optical microscope overlaps and is fixed on two sample stage, makes the axis of nano wire consistent with draw direction, and stretching device is placed in the scanning electron microscope;
3) make scanning electron microscope keep vacuum tightness 2 * 10
-4The high vacuum state that Pa is above applies voltage to well heater well heater is started working;
4) utilize scanning electron microscope original position record sample stage to spur the deformation process of nano wire,, utilize formula by the length of nano wire before and after the distortion of scanning electron microscope record
Calculate the maximum breaking strain amount of nano wire, wherein l0 is the length of nano wire before stretching, and l is the length of nano wire after the stretcher strain;
5) nano wire to tension failure carries out the observation of different amplification by scanning electron microscope to the pattern of fracture, and the microstructure change contrast of nano wire discloses the deformation mechanism and the mechanism of fracture of nano wire, size effect before and after the fracture; Perhaps change the nano wire tensile strain rate, the in-situ observation strain rate is to the influence of nano wire fracture process and failure mode.
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| CN100590412C true CN100590412C (en) | 2010-02-17 |
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Families Citing this family (11)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101158629B (en) * | 2007-10-26 | 2010-06-02 | 北京工业大学 | Scanning electron microscope electron back scattering diffraction in-situ stretching device and measuring method |
| CN101819109B (en) * | 2010-06-02 | 2012-02-15 | 哈尔滨工业大学 | Method for measuring nano monofilament tensile strength |
| CN104634660B (en) * | 2015-02-04 | 2017-05-10 | 北京工业大学 | Device and method for performing in-situ double-tilting single-axis stretching on nanowire and two-dimensional laminar thin film in transmission electron microscope |
| CN104764660A (en) * | 2015-03-29 | 2015-07-08 | 北京工业大学 | Thermal-driving uniaxial drawing/compressive deformation device for scanning/transmission electron microscope |
| CN106645806A (en) * | 2016-11-09 | 2017-05-10 | 深圳烯湾科技有限公司 | Mechanical property testing method based on atomic force microscope probe |
| CN108225865A (en) * | 2018-01-19 | 2018-06-29 | 扬州大学 | A kind of test specimen production method of the fixed cement concrete tension test for the bundle fiber that is chopped |
| CN108535296B (en) | 2018-04-18 | 2020-08-14 | 大连理工大学 | One-dimensional material transmission electron microscope force-electric coupling in-situ test method |
| CN109030208B (en) * | 2018-07-31 | 2020-12-29 | 内蒙古工业大学 | In-situ stretching experimental device for scanning electron microscope |
| CN109946160A (en) * | 2019-05-05 | 2019-06-28 | 中国人民解放军陆军装甲兵学院 | Coating material original position stretching observation system |
| CN113138125B (en) * | 2021-04-21 | 2023-03-14 | 北京工业大学 | In-situ double-inclination single-shaft stretching nanowire device and manufacturing method thereof |
| CN113324836B (en) * | 2021-05-28 | 2023-11-10 | 北京工业大学 | Damping device and method for in-situ deformation micro-nano sample in microscope |
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Non-Patent Citations (2)
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| An electromechanical material testing system for in situ electron microscopy and applications. Yong Zhu et al.PNAS,Vol.102 No.41. 2005 |
| An electromechanical material testing system for in situ electron microscopy and applications. Yong Zhu et al.PNAS,Vol.102 No.41. 2005 * |
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