CN201034884Y - Nano lines in-situ stretching device in scanning electron microscope - Google Patents
Nano lines in-situ stretching device in scanning electron microscope Download PDFInfo
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- CN201034884Y CN201034884Y CNU2006201728144U CN200620172814U CN201034884Y CN 201034884 Y CN201034884 Y CN 201034884Y CN U2006201728144 U CNU2006201728144 U CN U2006201728144U CN 200620172814 U CN200620172814 U CN 200620172814U CN 201034884 Y CN201034884 Y CN 201034884Y
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Abstract
A nanowire in-situ stretching device in scanning electron microscope of the utility model belongs to nanometer material mechanical performance in-situ measurement field. The utility model is characterized in comprising a base (1) and a heater (2) fixed thereon. A stent (3) with grooves is fixed on the heater (2), one end of the two bimetallic tablets (7) is respectively fixed by fastening screws (9) in the two grooves of the stent, and the other end of the two bimetallic tablets (7) is respectively connected with a pair of sliding blocks (5). A guide rail (4) is fixed on the base (1); the guide rail (4) is parallel to the stent (3) and perpendicular to the bimetallic tablets (7). A pair of sliding blocks (5) is arranged on the guide rail (4), and the two sliding blocks (5) are respectively provided with a sample stage (6), the horizontal position of which is adjustable. The utility model has advantages of simple structure, convenient control; and the strain rate is controllable. The utility model can be conveniently used to work in scanning electron microscope, realizing the function of in-situ and online measurement of mechanical performance of nanowire.
Description
The technical field is as follows:
the utility model relates to a device of tensile nano wire in situ in scanning electron microscope utilizes scanning electron microscope can survey the structural change of nano wire tensile deformation in-process in real time, reveals the deformation mechanism of nano wire under tensile load, and brittle-tough transition mode belongs to nano-material mechanical properties normal position measurement field.
Background art:
with the development of nanotechnology and the development of nano devices, nanowires are the basic units of nano devices, and not only nanowires have good electrical, magnetic, optical properties, but also are required to bear mechanical loads, transfer forces, execute motions, and the like in the devices. The mechanical response mode and failure mode of the nanowire under the action of external force, such as brittle fracture or ductile fracture, and the maximum fracture strain necessarily influence the reliability of the device, so that the mechanical response and the service behavior of a single nanowire under the action of external force are researched, the mechanical property data of the nanowire are accumulated, and the method is a basic material criterion for currently designing and developing nano devices. At present, the main methods for in-situ testing the mechanical properties of a single nanowire include an in-situ high-frequency electric field excitation resonance method in a transmission electron microscope and a scanning electron microscope, an in-situ bending method, a stretching method and the like. The stretching is the most direct mechanical property testing means, the scanning electron microscope is convenient to operate, the space of a sample chamber is large, and the scanning electron microscope is a powerful tool for researching the structure and the performance of a nano material, but the nano material is small in structure and difficult to operate, how to fix and uniaxially stretch and deform a single nano wire sample in the scanning electron microscope, and the problem of disclosing the mechanical property and the deformation mechanism of the nano wire in situ is the current nano mechanical research. At present, due to the limitation of experimental means, it is very difficult to directly measure the tensile deformation of a single nanowire/tube, and a literature reports an experimental measurement method for the mechanical properties of a one-dimensional carbon nanotube under the action of uniaxial tensile stress.
The method is reported in Science, 287 and 637-640, 2000, and comprises the steps of installing two sets of Atomic Force Microscope (AFM) probes in a Scanning Electron Microscope (SEM), fixing the carbon nanotubes adsorbed on the AFM tip in the SEM by in-situ chemical vapor deposition, adjusting the AFM probes to be vertically opposite, moving one AFM probe by applying a load to stretch a single carbon nanotube and observing the single carbon nanotube in situ under the SEM, calculating the tensile strength of the single multi-walled carbon nanotube and the single-walled carbon nanotube according to the magnitude of the tensile force and the degree of the elongation, and directly observing the fracture process of the nanotube. The method integrates the simultaneous working of a plurality of kinds of precision equipment, has complex control and operation systems, can obtain reliable experimental data only by higher experimental technology, and is not beneficial to popularization and promotion. Meanwhile, the AFM tip is thin, so that the nanowire is difficult to fix on the tip, and the method is difficult to be applied to thick nanowires or nanowires with high strength.
The utility model has the following contents:
the utility model aims at providing an install the tensile deformation device of nano wire in scanning electron microscope, utilize scanning electron microscope normal position real-time recording nano wire elastoplasticity deformation process and the mode that the fracture became invalid under the tensile action, the biggest fracture dependent variable of the nano wire of different diameters and material, change the direct correspondence of fracture mechanical properties and the microstructure of nano wire and play, reveal the mechanical properties of one-dimensional nano wire from the nanometer yardstick.
In order to achieve the above object, the present invention provides a device and a method for stretching a single nanowire in situ in a middle-scanning electron microscope, which is characterized in that: the heating device comprises a base 1 and a heater 2 fixed on the base, wherein a bracket 3 with grooves is fixed on the heater 2, two bimetallic strips 7 are respectively fixed in the two grooves on the bracket by fastening screws 9, and the bimetallic strips 7 are respectively connected with a pair of sliding blocks 5. The guide rail 4 is fixed on the base 1, and the guide rail 4 is parallel to the bracket 3 and is vertical to the bimetallic strip 7. A pair of slide blocks 5 are arranged on the guide rail 4, a pair of sample tables 6 with adjustable horizontal positions are respectively arranged on the two slide blocks 5, and a gap between the two sample tables is adjusted to be several micrometers at room temperature, so that a longer nanowire can be ensured to cross between the two sample tables.
A top cover 8 which can play a role of heat preservation is arranged on the bracket 3 and the bimetallic strip 7. The heater 2 heats the support 3, heat conducted to the bimetallic strip 7 causes the bimetallic strip 7 to generate bending deformation, the bimetallic strip drives the sliding block 5 to linearly move towards two sides along the guide rail 4, the sample table 6 fixed on the sliding block can stretch the nanowires fixed at two ends of the sample table, the nanowires are subjected to biaxial stretching deformation, and the scanning electronic microscope imaging system is used for simultaneously and sequentially recording the deformation process of the nanowires and the structural and morphological changes of the micro-regions.
The utility model discloses also can use a bimetallic strip 7, make a slider motion, another slider is fixed motionless, realizes the unidirectional stretching deformation to the nano wire.
Furthermore, the bimetallic strip is formed by overlaying metal sheets with different linear expansion coefficients, and when the temperature changes, the bimetallic strip expands and contracts differently due to the difference of the linear expansion coefficients of two different materials of the bimetallic strip, so that the bimetallic strip bends and deforms to one side with a small linear expansion coefficient. The utility model discloses well bimetallic strip's installation is guaranteed to the both sides motion of guide rail when being heated, and bimetallic strip is heated back drive slider motion, fixes the sample platform on the slider and realizes the tensile deformation to the nano wire. In the utility model, in order to ensure the realization of larger bending deformation at lower temperature, the recommended use ratio is more than 10/10 of bending -6 ·℃ -1 Of the double metal sheet
Further, the heater be resistance heater, including direct current controllable power to and temperature indicator, the linear programming range of heater 0-350 ℃, can be according to the strain rate who sets for, the programming rate of adjustment heater.
Furthermore, the gap between the two sample stages can be finely adjusted on the slide block, the end face and the upper surface of the sample stage are smooth, the roughness is less than 100nm, the two sample stages are adjusted to be in close contact at room temperature (20-30 ℃), and the contact gap is less than 3 μm.
Furthermore, the stretching device is fixed in a scanning electron microscope sample chamber, an assembled sample stretching table heater is placed on a scanning electron microscope sample table, the heating rate of the heater is set, the sample table is heated, the motion of the stretching table is observed under the imaging state of a scanning electron microscope, the stretching deformation and the fracture process of the nanowires fixed on the stretching table are observed in situ, the maximum strain variable before the fracture of the nanowires is directly calculated from images recorded in the in situ sequence, and the brittle-tough transition mode and the size effect of the nanowires are revealed from the appearance images of fractures. The rate of the tensile strain of the nanowires is changed by changing the rate of temperature rise.
The utility model discloses the application method of device is implemented through following step:
1. the nanowires are placed in an organic solvent (e.g., ethanol, acetone, etc.) that does not react with the sample, dispersed for 10-30 minutes by ultrasonic waves, and the suspension is dropped on a sample stage so that the nanowires are randomly distributed and attached on the sample stage.
2. And (3) overlapping and fixing the nanowires picked and distributed on the sample stages on the two sample stages by using a micro manipulator under an optical microscope to ensure that the axes of the nanowires are consistent with the stretching direction. The stretching apparatus was placed in a scanning electron microscope.
3. Maintaining the vacuum degree of the scanning electron microscope at 2 × 10 -4 In a high vacuum state of Pa or more, a voltage is applied to the heater according to a set temperature rise rate to start the operation of the heater.
4. The deformation process of the nanowire pulled by the sample stage is recorded in situ by using a scanning electron microscope, and the length of the nanowire before and after deformation is recorded by using a formula
Calculating the maximum fracture strain of the nanowire, wherein 0 Is the length of the nanowire before stretching and l is the length of the nanowire after stretching deformation.
5. The tensile fracture of the nanowire is observed with different magnifications through a high-resolution scanning electron microscope, and the deformation mechanism, the fracture mechanism and the size effect of the nanowire are revealed from the comparison of the microstructure changes of the nanowire before and after fracture. Or the temperature rise rate is controlled, the tensile strain rate of the nanowire is changed, and the influence of the strain rate on the breaking process and the failure mode of the nanowire is observed in situ.
Compared with the prior art, the utility model discloses simple structure, control is convenient, advantages such as rate of meeting an emergency is controllable, can conveniently work in scanning electron microscope, can observe the elastic deformation that many nanowires take place under tensile state simultaneously in an experiment, plastic deformation and unstability fracture process, can realize the mechanical properties measurement of nanowire under the different rate of meeting an emergency through control rate of rising temperature, because bimetallic strip drive power is great, can be applicable to all draw ratios and be greater than 5 one-dimensional nano-material, the diameter is the fibre and the whisker also can the normal position measurement of micron order even. The method utilizes the in-situ sequential imaging of a scanning electron microscope to directly correspond the mechanical properties and the microstructure of the nanowire, can explain the elastoplastic deformation mechanism and the fracture failure mode of different materials and one-dimensional nanomaterials with different diameters from the micro, and discloses the singular mechanical properties of the one-dimensional nanomaterials by using the brittle-tough transition mechanism.
Drawings
Fig. 1 is a schematic diagram of a principle structure of a nano stretching table provided by the present invention, and nanowires are dispersed on two sliders capable of moving relatively.
Wherein: the device comprises a base 1, a heater 3 2, a support 4, a guide rail 5, a slide block 6, a sample table 7, a bimetallic strip 8 and a top cover 9.
The specific implementation mode is as follows:
the present invention will be further described with reference to the accompanying drawings and the detailed description.
The utility model discloses well device characterized in that: the heating device comprises a base 1 and a heater 2 fixed on the base, wherein a bracket 3 with grooves is fixed on the upper surface of the heater 2, two bimetallic strips 7 are respectively fixed in the two grooves on the bracket by fastening screws 9, and the bimetallic strips 7 are respectively connected with a pair of sliding blocks 5. The guide rail 4 is fixed on the base 1, and the guide rail 4 is parallel to the bracket 3 and is vertical to the bimetallic strip 7. The pair of slide blocks 5 are arranged on the guide rail 4, the pair of sample tables 6 with adjustable horizontal positions are respectively arranged on the two slide blocks 5, and a gap between the two sample tables is adjusted to be several micrometers at room temperature, so that a longer nanowire can span between the two sample tables.
The nanowire in-situ stretching device in the scanning electron microscope is designed according to a FEIQuanta200 environment scanning electron microscope and a JEOLJSM6500F field emission scanning electron microscope, the length, the width and the height of the device are 30mm multiplied by 20mm multiplied by 10mm, the device can be conveniently installed in a sample chamber of the scanning electron microscope, the grade of a bimetallic strip is 5J20110, and the specific bending is 20.8/10 -6 ·℃ -1 The linear temperature rise range of the heater is 0-350 ℃, the control precision is 0.1 ℃, the adjusting distance of the two sample tables is kept to be less than or equal to 2 mu m at room temperature, the maximum linear displacement measuring range is 5mm, and the displacement precision is 0.2 mu m. The prepared SiC nanowires are placed in acetone for ultrasonic dispersion for 60min, the nanowires suspended in the acetone are randomly dispersed on two sample tables of a stretching device, nanowires picked and distributed on the sample tables are lapped and fixed on the two sample tables by utilizing a micro-manipulator under an optical microscope, the axis of the nanowires is consistent with the stretching direction, then the device with the nanowires fixed is integrally placed in a scanning electron microscope, a sample chamber door of the scanning electron microscope is closed, and the device is vacuumized to reach the working range of the scanning electron microscope. And adjusting the scanning parameters of an electron beam microscopic imaging system of the scanning electron microscope to focus the electron beam on the surface of the tested nanowire and receive a secondary electron image. Adjusting a heating power supply, heating a bimetallic strip to make a bimetallic drive sample stage stretch the SiC nanowire, placing the stretching device in a JEOLJSM6500F field emission scanning electron microscope, fixing two ends of one stretching device, and stretching the SiC nanowireSiC nanowires, the average diameter of the nanowires being 85nm. By measuring the elongation before the fracture of the nanowire, the average fracture strain of the two SiC nanowires is calculated to be 11 percent and 25.6 percent respectively, and the strain rate is calculated to be 3.2 multiplied by 10 -9 m/s and 6.6X 10 -9 m/s, the two SiC nanowires are subjected to large elastic and plastic deformation before fracture, the fracture strain of SiC of the bulk material is between 0.1 and 0.2 percent at low temperature and is represented as brittle fracture, and the unusual mechanical property of the material at the nanoscale is revealed by scanning an in-situ nanowire stretching device in an electron microscope.
Claims (2)
1. The utility model provides a nanowire normal position stretching device in scanning electron microscope which characterized in that: the heating device comprises a base (1) and a heater (2) fixed on the base, wherein a bracket (3) with grooves is fixed on the heater (2), one ends of two bimetallic strips (7) are respectively fixed in the two grooves on the bracket by fastening screws (9), and the other ends of the two bimetallic strips (7) are respectively connected with a pair of sliding blocks (5);
the guide rail (4) is fixed on the base (1), and the guide rail (4) is parallel to the bracket (3) and is vertical to the bimetallic strip (7); the pair of sliding blocks (5) are arranged on the guide rail (4), and the two sliding blocks (5) are respectively provided with a pair of sample tables (6) with adjustable horizontal positions.
2. The in-situ stretching device for the nanowires in the scanning electron microscope of claim 1, wherein: a top cover (8) is added on the support (3) and the bimetallic strip (7).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNU2006201728144U CN201034884Y (en) | 2006-12-29 | 2006-12-29 | Nano lines in-situ stretching device in scanning electron microscope |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNU2006201728144U CN201034884Y (en) | 2006-12-29 | 2006-12-29 | Nano lines in-situ stretching device in scanning electron microscope |
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| CN201034884Y true CN201034884Y (en) | 2008-03-12 |
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| CNU2006201728144U Expired - Fee Related CN201034884Y (en) | 2006-12-29 | 2006-12-29 | Nano lines in-situ stretching device in scanning electron microscope |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103217445A (en) * | 2013-04-08 | 2013-07-24 | 中国科学技术大学 | Extruding and drawing device for in-situ structure detection in combination with scattering of X rays and experimental method thereof |
| CN103471922A (en) * | 2013-09-30 | 2013-12-25 | 重庆大学 | Device and method for observing shape memory alloy tension-torsion experiment |
| CN105301027A (en) * | 2015-11-22 | 2016-02-03 | 北京工业大学 | Transmission/scanning electron microscope mechanical-thermal coupling field loaded in-situ experimental platform |
| CN109946161A (en) * | 2019-05-05 | 2019-06-28 | 中国人民解放军陆军装甲兵学院 | Original position stretching machine for coating material original position stretching observation system |
| CN110006755A (en) * | 2019-05-05 | 2019-07-12 | 中国人民解放军陆军装甲兵学院 | Original position stretching machine for coating material original position stretching observation system |
-
2006
- 2006-12-29 CN CNU2006201728144U patent/CN201034884Y/en not_active Expired - Fee Related
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103217445A (en) * | 2013-04-08 | 2013-07-24 | 中国科学技术大学 | Extruding and drawing device for in-situ structure detection in combination with scattering of X rays and experimental method thereof |
| CN103217445B (en) * | 2013-04-08 | 2015-06-17 | 中国科学技术大学 | Extruding and drawing device for in-situ structure detection in combination with scattering of X rays and experimental method thereof |
| CN103471922A (en) * | 2013-09-30 | 2013-12-25 | 重庆大学 | Device and method for observing shape memory alloy tension-torsion experiment |
| CN103471922B (en) * | 2013-09-30 | 2015-12-02 | 重庆大学 | Marmem tension-torsion experimental observation device and method |
| CN105301027A (en) * | 2015-11-22 | 2016-02-03 | 北京工业大学 | Transmission/scanning electron microscope mechanical-thermal coupling field loaded in-situ experimental platform |
| CN105301027B (en) * | 2015-11-22 | 2017-11-14 | 北京工业大学 | A kind of transmission/ESEM power, the experiment porch in situ of thermal coupling field loading |
| CN109946161A (en) * | 2019-05-05 | 2019-06-28 | 中国人民解放军陆军装甲兵学院 | Original position stretching machine for coating material original position stretching observation system |
| CN110006755A (en) * | 2019-05-05 | 2019-07-12 | 中国人民解放军陆军装甲兵学院 | Original position stretching machine for coating material original position stretching observation system |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20080312 Termination date: 20141229 |
|
| EXPY | Termination of patent right or utility model |