CN101419150B - Performance test device under stress condition for low-dimensional material - Google Patents

Performance test device under stress condition for low-dimensional material Download PDF

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Publication number
CN101419150B
CN101419150B CN2008102392346A CN200810239234A CN101419150B CN 101419150 B CN101419150 B CN 101419150B CN 2008102392346 A CN2008102392346 A CN 2008102392346A CN 200810239234 A CN200810239234 A CN 200810239234A CN 101419150 B CN101419150 B CN 101419150B
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piezoelectric ceramics
girder
base
stress
low
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CN101419150A (en
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韩晓东
岳永海
张跃飞
张泽
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Beijing University of Technology
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Beijing University of Technology
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Abstract

The invention relates to a performance testing device under the stress state of a low-dimensional material, and belongs to the field of testing comprehensive performances under the stress state of the low-dimensional material. The performance testing device is characterized by comprising a base and piezoelectric ceramics of which one end is fixed on the base while the other end is a free end. A three-axle displacement adjusting device is arranged on the base and is used for adjusting a soft cantilever beam and a hard cantilever beam to be in the same level and the distance between the soft cantilever beam and the hard cantilever beam to between 2 and 50 mu m; a precise laser positioning system is used to obtain accurate deformation amount of the soft cantilever beam in the stretching and deforming process, thereby measuring the stress value applied on the material, disclosing the relation between the stress born by the material and a deformation mechanism and simultaneously being engaged in the research of optical and electrical performance of the material under the action of stress. The performance testing device has a simple structure, low price and reliable performance and can realize the test of the optical and electrical performance and other comprehensive performances of the low-dimensional material under the action of the stress.

Description

Performance test device under stress condition for low-dimensional material
Technical field
The present invention relates to a kind of stretching device of under optical microscope (hereinafter to be referred as light microscopic) and scanning electron microscope (hereinafter to be referred as scanning electron microscope), testing low-dimensional materials optics, electrical properties under stress state.The present invention utilizes the real-time monitoring of double cantilever beam (hard semi-girder and soft semi-girder) that is equipped with to be applied to the stress signal on the material when utilizing the accurate deflection of piezoelectric ceramics to realize low-dimensional materials stretching or compression deformation.In addition, can utilize this device to carry out the research of low-dimensional materials optical properties such as Raman spectrum, photoluminescence spectra under stress state, belong to all-round property testing field under the stress condition for low-dimensional material.
Background technology
In recent years, continuous development along with science and technology, low-dimensional materials are (as nano wire, nano belt, nano thin-film, nanometer rods etc.) more and more be subjected to people's attention, but because the restriction of size, make and equally to operate low-dimension nano material to the operation macroscopic material, therefore, research for low-dimensional materials variation of character under stress state is backward relatively, yet, as the status material of the primary element military service situation and the fiduciary level performance that but affects material greatly under stress of nano-device in future, the method for the character of development test low-dimensional materials under stress state just seems particularly important.
At present, the method that is used for testing the performance of low-dimension nano material under stress roughly has following several.
One, utilizes scanning probe microscopy (SPM, comprise AFM, STM etc.) realize the research of character under the low-dimension nano material stress, " Resonant Raman Spectroscopy of Individual Strained Single-Wall CarbonNanotubes " that Xiaojie Duan in 2007 etc. are published on " Nano letters " utilizes the atomic force probe of atomic force microscope to apply a torsional moment and uniaxial strain for respectively single overlength Single Walled Carbon Nanotube, finds that the frequency displacement of different modes has appearred in the raman spectra of carbon nano-tube.And the variation of passing through Raman peaks intensity discloses the influence of strain to electronic band structure.But this method can't be accurately real-time provides the strain that material takes place, and can't provide the corresponding relation between strain and the Raman spectrum frequency displacement simultaneously in real time.
Two, transmission electron microscope is realized the test of the electric property of nano material under stress in conjunction with scanning probe microscopy.Xuedong Bai etc. is published in being entitled as on " Nano letters " " Deformation-DrivenElectrical Transport of Individual Boron Nitride Nanotubes " and has just studied the variation of single BN nanotube conduction property under stress state.Discovery originally is that BN nanotube electric conductivity after being subjected to stress flexural deformation of insulator has become semi-conductive conductive characteristic, and can also be returned to the conductive characteristic of insulator after stress removes.This method also just provides the relation between acting force and the material electric conductivity qualitatively, can not be quantitative provide the great power that applies, the variation that great strain can cause the material conduction property perhaps takes place.
Summary of the invention
At the prior art problem, this invention provides a kind of stretching device and method of simple and effective nano material, utilize this installation method can realize stretching and squeeze operation, and real-time observation is applied to the signal of the power on the nano material when carrying out aforesaid operations for one dimension, two dimension nano materials.Accurately control the rate of deformation of nano material by piezoelectric ceramics, can control the stress that is applied on the material accurately, thereby obtain institute's stress application and material electricity, the optical property relation between changing.
To achieve these goals, this performance test device under stress condition for low-dimensional material, it is characterized in that: comprise that a base 1 and an end are fixed on that the other end is free-ended piezoelectric ceramics 2 on the base 1, be supported on the base 1 to guarantee piezoelectric ceramics 2 piezoelectric ceramics 2 stressed evenly with support column 3.Base 1 fixedly a side of piezoelectric ceramics 2 also installed three (X simultaneously additional, Y, Z) displacement adjustment device 4, the free end of three-shaft displacement regulating device 4 is positioned at the top of piezoelectric ceramics 2 and is fixing brace table I5 thereon, soft semi-girder 6 is fixed on the brace table I5, fixing on the free end of piezoelectric ceramics 2 and supporting seat 7, support that seat 7 is that a side is fixed on the piezoelectric ceramics 2, opposite side is positioned at the top of piezoelectric ceramics 2, and place with three-shaft displacement regulating device 4 free end opposing parallel, support fixing brace table II8 on the seat 7, hard semi-girder 9 is fixed on the brace table II8.Piezoelectric ceramics 2 is connected to by external lead wire 10 and adds on the driving power 11.
Precise laser positioning system 12 also can be installed in the plane on the base 1 of this device, and laser orientation system 12 is external to outer computer disposal system 13, can obtain the accurate deflection that soft semi-girder 6 takes place by analysis software.
Under optical microscope, make soft semi-girder 6 and hard semi-girder 9 on same plane by the locus of regulating the soft semi-girder 6 of three-shaft displacement regulating device 4 changes, relative distance is between 2~50 μ m.Respectively the both positive and negative polarity of piezoelectric ceramics 2 is connected with the both positive and negative polarity that adds driving power 11 by external lead wire 10, adjusting is applied to the dc voltage value on the piezoelectric ceramics 2, the free end of piezoelectric ceramics 2 will deviate from the displacement of stiff end, drive is fixed on piezoelectric ceramics 2 free-ended support seats 7 corresponding displacement takes place, be fixed on the brace table of supporting on the seat 78 and can drive the corresponding displacement of hard semi-girder 9 generations, thereby realize being fixed on the stretcher strain operation of the sample on soft semi-girder 6 and the hard semi-girder 9.Because sample is subjected to the acting force of two semi-girders, makes soft semi-girder 6 to occur bending and deformation, thereby can record the value that is applied to the power on the sample.
Utilize laser orientation system 12 can record the displacement that soft semi-girder 6 is taken place accurately, can obtain the strain-stress relation of material, thereby disclose distortion of materials mechanism by computer processing system 13.
Further described three-shaft displacement regulating device can adopt traditional screw rod to regulate stepper motor, piezoelectric ceramics micrometric displacement system etc.
Further the described driving power that adds can adopt ac-dc dual power supply, if select for use direct current can realize the stretcher strain operation of nano material, if select interchange for use then can realize the fatigue property test of nano material by setting suitable alternative frequency.
Further, can be on two semi-girders external electrode, be used for measuring the electric charge transport mechanism of nano material in the stretcher strain process, but the also variation of test material other character such as optics in adding electric process.
The present invention has following advantage:
It is low, easy and simple to handle that the present invention compared with prior art has a cost, dependable performance, the advantage of applied range.Simultaneously, owing to adopted piezoelectric ceramics as driving element, made and adopt double cantilever beam can well measure the stress that is applied on the material by the displacement that accurately to control sample stage easily, obtain more accurate strain-stress relation, disclose material elastoplasticity modification mechanism.Simultaneously, also can utilize this stretching device to measure electric charge transport characteristic and the performances such as Raman, fluorescence, photoluminescence of nano material under stress state, for nano material provides reliable data in the development and Design of numerous areas such as MEMS (micro electro mechanical system) and semiconductor devices, sensor.
Description of drawings:
Fig. 1, performance test device under stress condition for low-dimensional material front view
Fig. 2, performance test device under stress condition for low-dimensional material vertical view
Fig. 3, install the performance test device under stress condition for low-dimensional material vertical view of laser orientation system additional
Adjust the diatomic force probe semi-girder photo of locus under Fig. 4, the optical microscope
Fig. 5, single SiO 2The nano wire stress-strain diagram
Fig. 6, single SiO 2Raman frequency shift spectrogram under the nano wire stress state
Wherein description of drawings is as follows:
1, base 2, piezoelectric ceramics 3, support column 4, three-shaft displacement regulating device
5, brace table I 6, hard semi-girder 7, support seat 8 brace table II
9, soft semi-girder 10, external lead wire 11, add driving power
12, laser orientation system 13, computer processing system
Embodiment
The mensuration of stress-strain diagram
1, selecting stiffness factor for use is the hard semi-girder of AFM micro cantilever probe conduct of 4N/m, selecting stiffness factor for use is that the AFM micro cantilever probe of 0.2N/m is as soft semi-girder, by regulating the three-shaft displacement regulating device, make fixing soft semi-girder progressively approach hard semi-girder, and the upper surface of two stiff cantilevers beams is adjusted in the same plane, article two, cantilever tip is staggered relatively, and the spacing between two semi-girders is 10 μ m.
2, with SiO 2Nano wire is put in the organic solvent (for example, ethanol, acetone etc.) that does not react with sample, after 10 fens kinds of ultrasonic dispersing, hanging drop on the double cantilever beam position, is made the nano wire stochastic distribution and attached on the two stiff cantilevers beams.
3, under light microscopic, observe, find to meet the requirements and the nano wire two ends ride over single nano-wire on the two stiff cantilevers beams respectively, utilize the little manipulator robot in light microscopic or the scanning electron microscope or utilize methods such as EBSD, FIB will carry SiO on two stiff cantilevers beams 2The nano wire two ends are fixed, and make the axially consistent with draw direction of nano wire.
4, will be installed on the base of apparatus of the present invention after the repacking of the AFM MI-150 laser orientation system of prior art, adjusting light path, to make wavelength be that the laser of 632nm is beaten on soft cantilever tip, and external computer processing system.
5, utilize and to add the driving power regulation and control and be applied to the voltage at piezoelectric ceramics two ends (voltage range is that 0~250V is adjustable during experiment, step-length, 1V), make the piezoelectric ceramics free end that certain displacement take place, make hard semi-girder move, utilize light microscopic or scanning electron microscope imaging system original position record sample stage pulling SiO away from soft semi-girder 2The deformation process of nano wire is by SiO before and after distortion of scanning electron microscope record or the fracture 2The length of nano wire is calculated SiO 2The dependent variable that nano wire took place.
6, in the high resolution scanning Electronic Speculum, to the SiO of tension failure 2The fracture apperance of nano wire is observed, and discloses SiO by the pattern to nano wire fracture before and after the fracture 2The fracture mechanism of nano wire.
7, draw SiO at the deflection that each process took place that stress applies by the picture analyzing in the drawing process that imaging system is write down, and from the soft semi-girder that laser orientation system obtains 2The nano wire stress-strain curve can obtain SiO thus 2Nano wire is such as Young modulus, mechanical property information such as elastic strain range.
The test of the Raman spectrum frequency displacement under the stress
1, selecting stiffness factor for use is the hard semi-girder of AFM micro cantilever probe conduct of 4N/m, selecting stiffness factor for use is that the AFM micro cantilever probe of 0.2N/m is as soft semi-girder, by regulating the three-shaft displacement regulating device, two stiff cantilevers beams are adjusted into upper surface at semi-girder in same plane, article two, cantilever tip is existing to placing, and the spacing between two semi-girders is 10 μ m.
2, with SiO 2Nano wire is put in the organic solvent (for example, ethanol, acetone etc.) that does not react with sample, after 10 fens kinds of ultrasonic dispersing, hanging drop on the double cantilever beam position, is made the nano wire stochastic distribution and attached on the two stiff cantilevers beams.
3, under light microscopic, observe, find the single nano-wire at satisfactory lift-launch two stiff cantilevers beam two ends, utilize the little manipulator robot in light microscopic or the scanning electron microscope or utilize methods such as EBSD, FIB will carry SiO on two stiff cantilevers beams 2The nano wire two ends are fixed, and are the axially consistent with draw direction of nano wire.
4, will be installed on the base of apparatus of the present invention after the repacking of the AFM MI-150 laser orientation system of prior art, adjusting light path, to make wavelength be that the ruddiness of 632nm is beaten on soft cantilever tip, and external computer processing system.
5, device is installed on the objective table of French JYT6400 Raman spectrometer, used optical maser wavelength is the green glow of 514.5nm, laser power is 10mW, regulates the focusing system of Raman spectrometer, and hot spot is contracted to 1 micron and focus on the single SiO that rides on the double cantilever beam 2On the nano wire.
6, (voltage range is that 0~250V is adjustable during experiment, and step-length 1V), simultaneously, utilizes the register system of Raman spectrometer to obtain the Raman spectrum of nano wire at each deformation stage, by the mutation analysis SiO of Raman spectrum to adjust the magnitude of voltage that adds driving power 2The variation of nano wire structure under stress and the variation of inner suffered stress.
7, found through experiments along with being applied to single SiO 2The increase of the drawing stress on the nano wire, SiO 2Certain frequency displacement, SiO have taken place to high frequency direction in the Raman spectrum of nano wire 2Nano wire is not when being stretched, and the main peak position appears at 501.7cm -1When voltage was added to 80V, the frequency displacement of main peak position was to 505.8cm -1, along with the increase of voltage, at 140VSiO 2521.2cm had been arrived in the frequency displacement of main peak position when nano wire was broken -1, this illustrates that corresponding variation has taken place its inner structure.Can disclose the variation of its structure by the frequency displacement of analyzing its Raman spectrum.

Claims (3)

1. performance test device under stress condition for low-dimensional material, it is characterized in that: comprise that a base and an end are fixed on the base, the other end is free-ended piezoelectric ceramics, base fixedly a side of piezoelectric ceramics a three-shaft displacement regulating device has been installed, the free end of this three-shaft displacement regulating device is positioned at the top of piezoelectric ceramics and is fixing brace table on the three-shaft displacement regulating device, and soft semi-girder is fixed on the brace table; Fixing on the free end of piezoelectric ceramics and supporting seat, support seat one side to be fixed on the piezoelectric ceramics, opposite side is positioned at the top of piezoelectric ceramics, and places with three-shaft displacement regulating device free end opposing parallel, support fixing another brace table on the seat, hard semi-girder is fixed on described another brace table; Piezoelectric ceramics is connected to by external lead wire and adds on the driving power; Plane Installation laser orientation system on base, and laser orientation system is external to the outer computer disposal system; Between piezoelectric ceramics and base, install in order to guarantee the stressed uniform support column of piezoelectric ceramics.
2. device according to claim 1 is characterized in that: the described driving power that adds adopts interchange or direct supply.
3. device according to claim 1 is characterized in that: described hard semi-girder and soft semi-girder external electrode.
CN2008102392346A 2008-12-05 2008-12-05 Performance test device under stress condition for low-dimensional material Expired - Fee Related CN101419150B (en)

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CN108287034B (en) * 2018-01-25 2019-12-10 常州市利多合金材料有限公司 micro/nano-force-electric coupling characteristic measuring device and method based on AFM
CN114354726B (en) * 2022-01-18 2022-11-18 西北工业大学 Nano material single crystal stress field coupling electrochemical testing device and method

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101158629A (en) * 2007-10-26 2008-04-09 北京工业大学 Scanning electron microscope electron back scattering diffraction in-situ stretching device and measuring method
CN101221106A (en) * 2008-01-25 2008-07-16 北京工业大学 Nano material drawing device in scanning electron microscope driven by piezoelectric ceramic piece

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101158629A (en) * 2007-10-26 2008-04-09 北京工业大学 Scanning electron microscope electron back scattering diffraction in-situ stretching device and measuring method
CN101221106A (en) * 2008-01-25 2008-07-16 北京工业大学 Nano material drawing device in scanning electron microscope driven by piezoelectric ceramic piece

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
Xiaojie Duan et.al.Resonant Raman Spectroscopy of Individual Strained ....《Nano Letters》.2007,第7卷(第7期),2116-2121. *
Xuedong Bai et.al.Deformation-Driven Electrical Transport of Individual Boron Nitride Nanotubes.《Nano Letters》.2007,第7卷(第3期),632-637. *

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