CN101477052A - Strain component lossless detection technology based on carbon nano-tube as sensing medium - Google Patents
Strain component lossless detection technology based on carbon nano-tube as sensing medium Download PDFInfo
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- CN101477052A CN101477052A CNA2009100676121A CN200910067612A CN101477052A CN 101477052 A CN101477052 A CN 101477052A CN A2009100676121 A CNA2009100676121 A CN A2009100676121A CN 200910067612 A CN200910067612 A CN 200910067612A CN 101477052 A CN101477052 A CN 101477052A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 26
- 239000002041 carbon nanotube Substances 0.000 title claims abstract description 26
- 229910021393 carbon nanotube Inorganic materials 0.000 title claims abstract description 26
- 238000005516 engineering process Methods 0.000 title claims abstract description 20
- 238000001514 detection method Methods 0.000 title claims abstract description 10
- 238000001069 Raman spectroscopy Methods 0.000 claims abstract description 47
- 230000010287 polarization Effects 0.000 claims abstract description 43
- 238000005259 measurement Methods 0.000 claims abstract description 31
- 230000003595 spectral effect Effects 0.000 claims abstract description 10
- 230000001066 destructive effect Effects 0.000 claims abstract 4
- 238000001530 Raman microscopy Methods 0.000 claims abstract 3
- 238000001237 Raman spectrum Methods 0.000 claims description 9
- 238000000691 measurement method Methods 0.000 claims description 8
- 238000009659 non-destructive testing Methods 0.000 claims 1
- 238000004458 analytical method Methods 0.000 abstract description 9
- 239000011149 active material Substances 0.000 abstract description 4
- 239000011343 solid material Substances 0.000 abstract description 3
- 238000002474 experimental method Methods 0.000 description 7
- 239000000463 material Substances 0.000 description 7
- 239000000523 sample Substances 0.000 description 7
- 238000000034 method Methods 0.000 description 6
- 238000010008 shearing Methods 0.000 description 6
- 238000006073 displacement reaction Methods 0.000 description 5
- 229920000915 polyvinyl chloride Polymers 0.000 description 5
- 239000004800 polyvinyl chloride Substances 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- 230000005540 biological transmission Effects 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000002109 single walled nanotube Substances 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- 238000013459 approach Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000001427 coherent effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- 238000001093 holography Methods 0.000 description 1
- 238000005305 interferometry Methods 0.000 description 1
- 239000006101 laboratory sample Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000001338 self-assembly Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000001132 ultrasonic dispersion Methods 0.000 description 1
- 230000004304 visual acuity Effects 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
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Abstract
本发明公开了一种基于碳纳米管为传感介质的应变分量无损检测技术。碳纳米管随机附着在被测物体的表面或掺杂其内部，偏振显微拉曼光谱系统将入射激光聚焦到被测物体表面并背向采集原始拉曼光谱信息，数据处理得出的拉曼频移增量与被测物体表面的平面应变分量之间的解析式为：ΔΩ(Φ)＝(1/6)ΨSensor·[(3+cos2φ)εX+(3－cos2φ)εY－2sin2φ·γXY]，给定三个不同的偏振方向，并将其频移增量测量结果代入上述方程组求解得出应变分量。本发明解决了拉曼应变测量中的非拉曼活性材料传感检测问题，可对固体材料表面的平面应变分量直接测量以及微区域应变场的实验分析，具有无损非破坏、高测量精度、高空间分辨率等特点，可用于微尺度力学行为的实验研究、MEMS微器件力学性能的分析等多个领域。
The invention discloses a strain component nondestructive detection technology based on carbon nanotube as a sensing medium. Carbon nanotubes are randomly attached to the surface of the measured object or doped inside. The polarization micro-Raman spectroscopy system focuses the incident laser light on the surface of the measured object and collects the original Raman spectral information. The analytical formula between the frequency shift increment and the plane strain component on the surface of the measured object is: ΔΩ (Φ) = (1/6)Ψ Sensor [(3+cos2φ)ε X +(3－cos2φ)ε Y － 2sin2φ·γ XY ], given three different polarization directions, and substituting the frequency shift incremental measurement results into the above equations to solve the strain component. The invention solves the problem of non-Raman active material sensing and detection in Raman strain measurement, can directly measure the plane strain component on the surface of solid materials and conduct experimental analysis of micro-area strain field, and has the advantages of non-destructive and non-destructive, high measurement accuracy, high Spatial resolution and other characteristics can be used in many fields such as experimental research on micro-scale mechanical behavior and analysis of mechanical properties of MEMS micro-devices.
Description
Technical field
The invention belongs to mechanics of materials field, be specifically related to the technology that a kind of the millimeter components of strain and the regularity of distribution thereof to the submicron-scale are measured.
Background technology
In recent years along with the fast development of material and message area science and technology, the fail-safe analysis that detects with micro devices about the mechanical property of material under macroscopic view and the micro-scale has become the multidisciplinary institute hot fields of concern jointly.In this field, Experimental Mechanics analysis and Performance Detection are being born important instrumental purpose, detect demand but present existing strain measurement technique has been difficult to satisfy new experiment.For example: the measuring point yardstick of existing strain gage testing technology is big, and the paster yardstick and belongs to the spot measurement of the contact that wiring is arranged at least on several mm-scales; In the existing optical deformation measurement technology, macroscopical photodynamics survey technology mainly is the measurement to the moderate finite deformation field, and the visual field is big and resolution is not enough.In the micrometering field, commercial high resolving power micro measurement instrument (for example atomic force microscope, scanning electron microscope, transmission electron microscope, nano-hardness tester etc.) can be realized the pattern observation of nanometer measured object to the micro-meter scale regional extent, but still unresolved under power or environmental load effect to the deformation field of measured object and the quantitative measurment problem of strain field; In addition, in the existing spectral class detection technique, the measuring point of x light diffraction techniques is big, and is restricted to material, and lack of resolution.Micro-Raman technology can realize Raman active materials such as silicon the micron zone stress and measurement, but be not suitable for non-Raman active material, and the measurement of still unresolved plane strain component (be stress and decomposition) problem is particularly with the closely-related shearing strain problems of measurement of intensity.
Therefore, detect detection demand with the fail-safe analysis of micro devices at the mechanical property of material under macroscopic view and the micro-scale, study new Experimental Mechanics measuring technique, realize having important scientific meaning and engineering background to the strain measurement of micron and sub-micron regions and to micro element key position intensity detection.Given this, the present invention's proposition is sensor information with the carbon nano-tube, is the components of strain Dynamic Non-Destruction Measurement of measurement means with micro-Raman technology, can be used for the quantitative measurment of the plane strain component (comprising normal strain and shearing strain) of material surface micron or submicron-scale measuring point, can realize the measurement of millimeter, and solve associated non-Raman active material strain detection problem to normal strain and the shearing strain component and the regularity of distribution thereof in submicron-scale zone.
Summary of the invention
The object of the present invention is to provide and a kind ofly be wireless noncontact sensor information, harmless, be used for the strain detecting technology of material mechanical performance and micro devices fail-safe analysis under macroscopic view and the micro-scale based on carbon nano-tube.
Based on carbon nano-tube is the components of strain Dynamic Non-Destruction Measurement of sensor information, has carbon nano-tube, testee, polarization micro Raman spectra system (as Fig. 1).The testee surface at random, is evenly disperseed and fixing carbon nano-tube adopts dual-polarization (incident light and scatter light polarization direction can be controlled and be consistent) or single polarization (only the incident light polarization direction can be controlled) Raman experimental system to carry out the resonance raman test, and Raman frequency shift increment that is obtained by experiment and the quantitative relationship between the testee plane strain component can be expressed by analytic expression.Wherein, the analytic expression between Raman frequency shift increment in the Raman spectral information and the testee plane strain component is under the dual-polarization resonance raman experiment model:
In the formula,
Represent the polarization direction to be
The time experimental system before and after distortion, gather the frequency displacement increment obtain Raman spectrum; ε
XAnd ε
YRepresent the normal strain component of testee surface X, Y direction respectively, γ
XYBe shearing strain component, Ψ
SensorBe the strain-frequency-shifting operator of carbon nano-tube strain sensing medium, i.e. Ψ
SensorBe the constant factor that characterizes as linear relationship between the Raman frequency shift of the axial strain of the carbon nano-tube of strain sensing medium and carbon nano-tube, given three different polarization directions
Be respectively
With
Set up system of equations with the analytic expression between Raman frequency shift increment in the Raman spectral information and the testee plane strain component, the frequency displacement increment measurement substitution system of equations as a result of three different polarization directions is found the solution drawn the components of strain.
As get the polarization direction
Be respectively 0 °, 45 ° and 90 °, bring Raman frequency shift increment in the Raman spectral information and the analytic expression between the testee plane strain component into, draw system of equations and be:
In three different polarization directions
Or
Or
When being all 45 °, be called 45 ° of Raman strain measurement methods with the angle of other two polarization directions; In three different polarization directions
Or
Or
When being all 60 °, be called 60 ° of Raman strain measurement methods with the angle of other two polarization directions; In three different polarization directions
Or
Or
When being all 120 °, be called 120 ° of Raman strain measurement methods with the angle of other two polarization directions.
Beneficial effect of the present invention and advantage are: the present invention has characteristics such as harmless, wireless noncontact, high-space resolution, can realize the components of strain ε of micro-meter scale measuring point
X, ε
YAnd γ
XYDirect measurement, and can adopt the point by point scanning mode to realize the full-field distribution measurement of each plane strain component in the film micro area, but thereby solved that microscale mechanics study and micro element fail-safe analysis needed badly existing experimental technique but is difficult to the problems of measurement, the particularly problems of measurement of shearing strain component and maximum principal strain and principal strain directions of the plane strain component of the micro-meter scale realized.The technology of the present invention compare with the resistance-strain chip technology outstanding characteristics be have wireless noncontact, measuring point yardstick little, can realize advantages such as whole audience components of strain distribution measuring; With classical photo-measuring experimental mechanics technology (for example holography method, moire method, cutting speckle method, Electronic Speckle Pattern Interferometry etc.) compare, outstanding feature of the present invention is to realize the direct measurement of strain, has experiment preparation, experimental implementation and the simple advantage of data processing in addition; Compare (based on commercial micro-platform mechanical parameter method of testings such as atomic force, scanning electron microscope, transmission electron microscope, nano-hardness testers) with the micro-photo-measuring experimental mechanics technology of high-resolution, outstanding advantage of the present invention is that laboratory sample is prepared simply, can realize the direct measurement of the plane strain component of measuring point, solve the problems of measurement of shearing strain component and maximum principal strain and principal strain directions.Compare with existing spectrum test technology, the present invention has broken through traditional Raman strain measurement technique, and requirement has the limitation of Raman active to tested object, can be in engineering be used by laminated film adhere to, chemical bonding is modified or mode such as molecule self assembly realizes the plane strain component of non-Raman active solid material surface is directly measured and the experimental analysis of film micro area strain field; Also can realize the strain of transparent inside of solid material is directly measured by means such as collosol and gel, blend doping, original position are compound.The present invention can be used for the related application occasion in a plurality of fields such as test of experimental study, the MEMS micro element mechanical property of microscale mechanical behavior.
Description of drawings
Fig. 1 is the technology of the present invention principle schematic, and wherein long broken line is an incident light, and short broken line is a scattered light.
Fig. 2 is the micro-Raman experimental system of dual-polarization, and wherein long broken line is an incident light, and short broken line is a scattered light.
Specific embodiment
Below by embodiment method of the present invention is described further.
Be the components of strain Dynamic Non-Destruction Measurement (as Fig. 1) of sensor information based on carbon nano-tube as previously mentioned, have carbon nano-tube 1, testee 2, polarization micro Raman spectra system 3.Carbon nano-tube 1 is at random attached to the surface of testee 2 or be doped in the inside of testee.Polarization micro Raman spectra system 3 (as Fig. 2) comprises LASER Light Source 4, half-wave plate 5, polaroid 6, microscope 7 and Raman spectrometer 8.The incident light of LASER Light Source 4 outgoing is incident on testee 2 surfaces through half-wave plate 5 and polaroid 6 backs by microscope 7 successively, and microscope 7 and the scattered light of collecting dorsad enter Raman spectrometer 8 through polaroid 6 and half-wave plate 4 successively and form Raman spectral information.Control the polarization angle of incident light and scattered light by the polarization axle of joint rotation half-wave plate 5 and polaroid 6.The Raman system of single polarization can not have polaroid or scattered light without polaroid in addition, only realizes polarization of incident light is controlled.
To measure " the strain regime analysis of Polyvinylchloride thin sheet surface " be embodiment, and employing is that the components of strain Dynamic Non-Destruction Measurement of sensor information is as follows to the implementation step that testee carries out strain testing based on carbon nano-tube:
The first step, specimen preparation: with purity is that 90% Single Walled Carbon Nanotube is mixed according to mass ratio 1:999 with liquid-state epoxy resin, after the ultrasonic dispersion mixed liquor press mold on the Polyvinylchloride thin plate is solidified, thereby make the thick coherent film of 30 μ m at the PVC thin sheet surface, carbon nano-tube evenly distributes at random in the film.With same approach obtain carbon nano-tube with content from the body film as calibration sample.
In second step, experimental system is prepared: the micro-Raman experimental system experiment of the polarization light path of adjusting dual-polarization with reference to Fig. 2; The 632.8nm laser that adopts the He-Ne laser instrument is as incident light, and Single Walled Carbon Nanotube is in the resonance raman state, is applicable to 45 ° of Raman strain measurement normal equation groups, i.e. formula under the dual-polarization system resonance Raman modes
In the 3rd step, demarcate sensor information strain-frequency-shifting operator Ψ
Sensor: calibration sample is in given strain regime, be placed on the micro-platform of Raman system, focus on incident light to sample surfaces, (as Fig. 2) controls the polarization direction of incident light and scattered light by the polarization axle of half-wave plate 5 and polaroid 6 in the joint rotation polarization micro Raman spectra system, with 0.04% strain is that step-length is carried out the uniaxial tension experiment to calibration sample, under each loaded-up condition, a plurality of measuring positions, calibration sample surface are gathered the Raman spectrum that the polarization direction is 0 ° and 90 ° respectively, handle experimental data and extract frequency displacement information (as table 1), bringing above-mentioned formula first formula into (is ε
X) find the solution, be averaged the result and draw Ψ
Sensor=1815cm
-1, the zero load frequency displacement is 2624cm
-1
Table 1 measurement data
| ε X(％) | 0 | 0.04 | 0.08 | 0.12 | 0.16 | 0.2 | 0.24 | 0.28 | 0.32 |
| Ω (0)(cm -1) | 2623.79 | 2623.62 | 2622.48 | 2622.44 | 2621.88 | 2621.53 | 2620.78 | 2620.67 | 2619.59 |
| Ω (90)(cm -1) | 2623.83 | 2624.27 | 2624.51 | 2624.49 | 2624.34 | 2624.52 | 2624.68 | 2625.54 | 2625.03 |
| ε X(‰) | 0.36 | 0.4 | 0.44 | 0.48 | 0.52 | 0.56 | 0.6 | 0.64 | 0.68 |
| Ω (0)(cm -1) | 2618.9 | 2618.83 | 2617.56 | 2616.98 | 2616.64 | 2615.88 | 2615.82 | 2615.23 | 2614.89 |
| Ω (90)(cm -1) | 2625.2 | 2625.24 | 2625.42 | 2625.77 | 2625.23 | 2625.31 | 2625.65 | 2626.1 | 2625.94 |
The 4th step, the formal measurement: the Polyvinylchloride thin sheet surface that will be under the loaded state places on the micro-platform of Raman system, focus on incident light to sample surfaces strain measurement position, (as Fig. 2) controls the polarization direction of incident light and scattered light by the polarization axle of half-wave plate 5 and polaroid 6 in the joint rotation polarization micro Raman spectra system, gather the polarization direction respectively and be the Raman spectrum of 0 °, 45 ° and 90 °, handle experimental data and extract frequency displacement information and draw respectively:
Δ Ω
(0)=-9.287cm
-1, Δ Ω
(45)=-9.226cm
-1With Δ Ω
(90)=-9.408cm
-1, the above-mentioned system of equations of substitution:
As seen ε
X≈ ε
YAnd γ
XY≈ 0, and therefore tested its measuring position of Polyvinylchloride thin plate sample is in " waiting biaxial stretch-formed loaded-up condition ".
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101929847A (en) * | 2010-06-01 | 2010-12-29 | 天津大学 | Strain Component Nondestructive Testing Technology Based on Carbon Nanotubes as Sensing Medium |
| CN102359764A (en) * | 2011-08-18 | 2012-02-22 | 天津大学 | Plane deformation non-destructive testing device on the basis of carbon nanotube as sensing medium |
| CN102564282A (en) * | 2010-12-15 | 2012-07-11 | 中国科学院金属研究所 | Strain measurement method |
| CN103743620A (en) * | 2013-12-27 | 2014-04-23 | 天津大学 | Method for carrying out non-contact measurement on plane transformation by using low-dimensional nano material |
| CN107478171A (en) * | 2017-08-31 | 2017-12-15 | 长江存储科技有限责任公司 | The monitoring method and monitoring device of a kind of buckling deformations |
| CN109443232A (en) * | 2018-12-29 | 2019-03-08 | 武汉华星光电技术有限公司 | Unimolecule substrate strain sensing device and preparation method thereof |
-
2009
- 2009-01-05 CN CNA2009100676121A patent/CN101477052A/en active Pending
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101929847A (en) * | 2010-06-01 | 2010-12-29 | 天津大学 | Strain Component Nondestructive Testing Technology Based on Carbon Nanotubes as Sensing Medium |
| CN102564282A (en) * | 2010-12-15 | 2012-07-11 | 中国科学院金属研究所 | Strain measurement method |
| CN102359764A (en) * | 2011-08-18 | 2012-02-22 | 天津大学 | Plane deformation non-destructive testing device on the basis of carbon nanotube as sensing medium |
| CN102359764B (en) * | 2011-08-18 | 2013-07-24 | 天津大学 | Plane deformation non-destructive testing device on the basis of carbon nanotube as sensing medium |
| CN103743620A (en) * | 2013-12-27 | 2014-04-23 | 天津大学 | Method for carrying out non-contact measurement on plane transformation by using low-dimensional nano material |
| CN107478171A (en) * | 2017-08-31 | 2017-12-15 | 长江存储科技有限责任公司 | The monitoring method and monitoring device of a kind of buckling deformations |
| CN107478171B (en) * | 2017-08-31 | 2019-10-18 | 长江存储科技有限责任公司 | A kind of monitoring method and monitoring device of buckling deformations |
| CN109443232A (en) * | 2018-12-29 | 2019-03-08 | 武汉华星光电技术有限公司 | Unimolecule substrate strain sensing device and preparation method thereof |
| CN109443232B (en) * | 2018-12-29 | 2020-10-13 | 武汉华星光电技术有限公司 | Single-molecule substrate strain sensing device and preparation method thereof |
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