CN101266236B - Method for real time measurement for nano material photostrictive performance - Google Patents
Method for real time measurement for nano material photostrictive performance Download PDFInfo
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- CN101266236B CN101266236B CN2008100305733A CN200810030573A CN101266236B CN 101266236 B CN101266236 B CN 101266236B CN 2008100305733 A CN2008100305733 A CN 2008100305733A CN 200810030573 A CN200810030573 A CN 200810030573A CN 101266236 B CN101266236 B CN 101266236B
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01Q—SCANNING-PROBE TECHNIQUES OR APPARATUS; APPLICATIONS OF SCANNING-PROBE TECHNIQUES, e.g. SCANNING PROBE MICROSCOPY [SPM]
- G01Q60/00—Particular types of SPM [Scanning Probe Microscopy] or microscopes; Essential components thereof
- G01Q60/24—AFM [Atomic Force Microscopy] or apparatus therefor, e.g. AFM probes
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- G01Q60/366—Nanoindenters, i.e. wherein the indenting force is measured
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Abstract
The invention discloses a method for real-time measuring the photo retractility of nm material, comprising: (1) the nm material is positioned and imaged using three chip capacitor plate sensing nm probe to find the nm material smooth and flat surface to determine the thickness of the nm material along the indenting direction. (2) the incident beam with power density of 0.2-0.8mW/cm<2> is introduced into the nm probe at the contact area of the diamond nm probe and the nm material to perform the home position indenting and load holding experiment on the nm material. During prolonging the load holding time, the wave and power density of the incident beam is changed and the probe indentation displacement-time variation curve of the probe is recorded. The difference of the displacement from the illumination starting to illumination ending is calculated on the curve, namely amount of photo deformation of the nm material along the indenting direction. (3) The percentage ratio of the amount of photo deformation and the thickness thereof is photo strain, namely photo retractility of the nm material. The invention can solve the problem that it is difficult to test the photo retractility of the nm material under photoirradiation. The method is simple and easy to operate, and prevents the infection of the inhere laser in traditional atomic force microscope technique and can accurately and reliability measure the photo retractility of nm material.
Description
Technical field
The invention belongs to the material properties test field, particularly a kind of method of real time measurement for nano material photostrictive performance.
Background technology
Utilize the photo-induced telescopic performance of material, people have designed and have produced various microstructure opto-mechanical devices.For example: utilize the photo-induced telescopic performance to make photic motor type relay, photic moving stepper, photic moving SAW device and optical tracking transducer etc.In the index evaluation system of these devices, the photo-induced telescopic measurer of accurately measuring material has crucial meaning.The method of measuring the material photo-induced telescopic on the traditional sense can be divided into two kinds: a kind of is the displacement sensing measuring method, measures the method for mixing the photoinduced strain of lanthanum ferroelectric ceramic material like report in (Mechatronics 10 (2000) 467-487).Owing to can not accurately locate nano material, this method only is fit to the measuring body material, and can't be used to measure nano material such as nano belt, the isostructural photoinduced strain of nano wire.Another kind is to nano material with the atomic force microscope probe technology; Realize that nano-precision location and original position are pressed into, as having reported the photo-induced telescopic that utilizes atomic force microscope probe commercial measurement sulfuration glass film in the science magazine (Science 277 (1997) 1799-1803).But; Atomic force microscope utilizes light pickup probe technology to survey; Its intrinsic laser possibly interact with incident beam; Its measurement result also possibly exert an influence, so possibly be inaccurate during with the photic performance of traditional atomic force microscope technology exosyndrome material to nano material.
At present, it is more to utilize capacitance sensing probe original position to be pressed into both at home and abroad to protect support method to measure the report of conventional mechanical properties such as creep and plastic yield of nano material.For example: Chinese patent (patent No. 200510124587.8) has been reported the nano impress method testing room temperature press-in creeping performance of metal film that adopts three chip capacitor plate sensing technologies; Materials Science and Engineering (MaterialsScience and Engineering:A, 449-451 (2007) 962-965) has been reported with the plastic yield of nano impress method research cerium base metal glass.But, up to now, do not see as yet and utilize original position to be pressed into guarantor's year pattern, go into condition at the maintenance load phasic change light beam that prolongs, measure the photo-induced telescopic of nano material and the report of observing its restorability degree.
Because needs highly microminiaturized, Highgrade integration, the photo-induced telescopic performance of nano material has potential wide application prospect in the micro-nano mechanical system.But receive the restriction of low yardstick characterization technique, the measurement of nano material photo-induced telescopicing performance is difficult.Therefore, demand developing a kind of new method of measuring nano material photo-induced telescopicing performance urgently.
Summary of the invention
The method that the purpose of this invention is to provide a kind of real time measurement for nano material photostrictive performance.
The objective of the invention is to realize through following mode: a kind of method of real time measurement for nano material photostrictive performance may further comprise the steps:
(1) adopts three chip capacitor plate sensing nano-probe technology to nano material location and imaging, find the nano material smooth planar surface, confirm that nano material is along the thickness that is pressed into direction.
(2) be 0.2-0.8mW/cm with power density
2Incident beam is introduced the nano-probe device, and light beam incides the diamond nano probe zone that contacts with nano material, nano material is implemented original position be pressed into to protect to carry and test.In the wavelength and the power density of the hold time of prolongation phasic change incident beam, record probe impression displacement-time changing curve.Calculate the poor of the shift value of illumination when beginning and finishing from this curve, be pressed into the photic deflection of direction for the nano material edge.
(3) number percent of the photic deflection of nano material and its thickness is the photo-induced telescopic strain, and this photo-induced telescopic strain is the photo-induced telescopic performance of nano material.
Nano material comprises quantum dot, nano belt, nano wire, nanometer rods, nanotube, nano-rings and nano thin-film.
The incident beam wavelength is modulated through filter plate.
Light beam incides the diamond nano probe zone that contacts with nano material after the reflection of the bimirror window of piezoelectric sensor.
Nano-probe can be Vickers or Nu Shi probe.
The nano-probe original position is pressed into protects the stage of carrying, and hold time is 10-100s.
The present invention has following beneficial effect, and it can solve the technical barrier of test nano material photo-induced telescopic performance under photoirradiation.This method is simple, has avoided the influence of intrinsic laser in the traditional atomic force microscope technology, can measure the photo-induced telescopic performance of nano material accurately and reliably.
Description of drawings
Fig. 1 is that incident beam of the present invention connects three chip capacitor plate sensing nano-probe device synoptic diagram;
Fig. 2 is the single nano belt shape appearance figure of zinc paste in the embodiment of the invention 1;
Fig. 3 be in the embodiment of the invention 1 under unglazed photograph, utilize original position to be pressed into and protect indentation load-time curve that support method obtains single zinc oxide nano-belt;
Fig. 4 be in the embodiment of the invention 1 the control beam of white light " open " 15 seconds with " passs " 15 seconds alternate under, utilize original position to be pressed into indentation load-time curve that guarantor's support method obtains single zinc oxide nano-belt;
Fig. 5 be in the embodiment of the invention 1 the control beam of white light " open " 15 seconds with " passs " 15 seconds alternate under, utilize original position to be pressed into the impression displacement-time curve that guarantor's support method obtains single zinc oxide nano-belt;
Fig. 6 is the single nano belt shape appearance figure of zinc sulphide in the embodiment of the invention 2;
Fig. 7 be in the embodiment of the invention 2 under unglazed photograph, utilize original position to be pressed into and protect indentation load-time curve that support method obtains single zinc sulfide nano-belt;
Fig. 8 be in the embodiment of the invention 2 the control ultraviolet light beam " open " 15 seconds with " passs " 15 seconds alternate under, utilize original position to be pressed into indentation load-time curve that guarantor's support method obtains single zinc sulfide nano-belt;
Fig. 9 be in the embodiment of the invention 2 the control ultraviolet light beam " open " 15 seconds with " passs " 15 seconds alternate under, utilize original position to be pressed into the impression displacement-time curve that guarantor's support method obtains single zinc sulfide nano-belt;
Indicate among the figure:
1-light source 2-incident beam 3-is flat
The face catoptron
4-plane mirror 5-three chip capacitor plate converter 6-press
Electric transducer
7-controller 8-controller 9-letter
Number processor
10-microcomputer 11-adamas probe 12-behaviour
Vertical platform
13-nano material to be measured is placed the 14-substrate
Embodiment
Embodiment 1:
Measure the method for single zinc oxide nano-belt photo-induced telescopic performance among the embodiment 1 in real time, specifically may further comprise the steps:
(1) incident light source is connected with the nano-probe device by requirement shown in Figure 1.Light source 1 sends incident beam 2, and after parallel plane mirror 3 and 4 reflections, irradiation is on the nano material rest area 13 to be measured in the substrate 14.Microcomputer 10 control signal processors 9 and manoeuvring platform 11 input signals.Signal processor 9 is exported signals to three chip capacitor plate converters 5 through controller 8, and then converts the load input signal of nano-probe 11 to.On the other hand, signal processor 9 is exported signals to piezoelectric sensor 6 through controller 7, and then the displacement of control nano-probe 11.
(2) light source mechanism (Ocean Optics Inc.USA) produces beam of white light among Fig. 1, and its power is 0.8mW/cm
2Through the "on" and "off" of light path switch control incident beam, thereby obtain the periodically incident beam of "on" and "off".
(3) select the monocrystalline silicon piece substrate, this silicon chip is (001) single-sided polishing.
(4) the zinc oxide nano-belt floccus is dissolved in acetone soln, adopt the ultrasonic cleaning appearance that its solution is disperseed, duration of oscillation is 30-40 minute, the dispersion liquid of the countless single nano belt that obtain suspending.Dispersant liquid drop volatilizing more than 1 hour naturally behind the substrate surface, is obtained being randomly distributed in the single nano belt on the substrate surface, and the adhesion layer that acetone soln volatilization back forms is fixed on single nano belt on the substrate surface.
(5) (imaging pattern USA) is carried out to picture to single nano belt for Hysitron Triboindenter, HysitronInc., obtains the single nano belt pattern of zinc paste shown in Figure 2 to adopt nano-hardness tester.Sweep speed is set to 15nm/s, and contact force is set to 1 μ N, and the picture size size is set to 3 μ m, and feedback gain setting is 600.Know that by Fig. 2 the xsect of single zinc oxide nano-belt is a rectangle, thickness is 500nm, and smooth surface is smooth, is beneficial to implement original position and is pressed into.
(6) carry the stage the guarantor who prolongs, adopt the described method of step (2) to change light beam and go into condition, carry out original position and be pressed into guarantor's year experiment.Its parameter is provided with as follows: the load time is 10s, and loading speed is 4 μ N/s, and hold time is extended for 90s, and keeping indentation load is 40 μ N, and discharge time is set to 10s, and rate of debarkation is 4 μ N/s.Indentation load-the time curve of real time record nano-probe under unglazed photograph, as shown in Figure 3.The real time record nano-probe the control beam of white light " open " 15 seconds with " pass " 15 seconds alternate under indentation load-time curve, as shown in Figure 4.The real time record nano-probe the control beam of white light " open " 15 seconds with " pass " 15 seconds alternate under the impression displacement-time curve, as shown in Figure 5.
(7) under the effect of incident beam of white light, the displacement variable of nano-probe can be analyzed acquisition from Fig. 5.Keeping the indentation load stage, when the incident beam of white light was opened 15s, 16.5nm moved to the 12.5nm place to nano-probe vertically upward from the equilibrium position, and displacement variable is 4nm.When the incident white light was closed 15s, nano-probe turned back to 16.5nm place, equilibrium position downwards from 12.5nm.During incident beam of white light periodicity irradiation, the variation of nano-probe displacement generating period property.The photic deflection of single zinc oxide semi-conductor nano belt under the incident beam of white light that then records is 4nm.
(8) analyze to such an extent that the thickness of single zinc oxide nano-belt is 500 nm by step (5); Analyze to such an extent that the photic deflection of single zinc oxide nano-belt under the incident white light is 4 nm by step (7); The photic deflection of nano belt and the number percent of its thickness are 0.8%; Therefore, the photo-induced telescopic performance of single zinc oxide nano-belt under the incident white light is 0.8%.
Embodiment 2:
Measure the method for single zinc sulfide nano-belt photo-induced telescopic performance among the embodiment 2 in real time, specifically may further comprise the steps:
(1) with embodiment 1 in step (1) identical.
(2) light source mechanism (Ocean Optics Inc.USA) produces ultraviolet light beam among Fig. 1, and its wavelength is 340nm, and power is 0.2mW/cm
2Through the "on" and "off" of light path switch control incident beam, thereby obtain the periodically incident beam of "on" and "off".
(3) with embodiment 1 in step (3) identical with (4).
(4) with embodiment 1 in step (5) identical, obtain single zinc sulfide nano-belt pattern shown in Figure 6.The picture size size is set to 3.93 μ m, and all the other parameters are provided with said identical with step (5).From Fig. 6 analysis, the xsect of single zinc sulfide nano-belt is a rectangle, and thickness is 310nm, and smooth surface is smooth, is beneficial to implement original position and is pressed into.
(5) carry the stage the guarantor who prolongs, adopt the described method of step (2) to change light beam and go into condition, carry out original position and be pressed into experiment.Load time is 10s, and loading speed is 0.5 μ N/s, and hold time is extended for 60s, and keeping indentation load is 5 μ N, and discharge time is set to 10s, and rate of debarkation is 0.5 μ N/s.Indentation load-the time curve of real time record nano-probe under unglazed photograph; As shown in Figure 7; The real time record nano-probe the control ultraviolet light beam " open " 15 seconds with " pass " 15 seconds alternate under indentation load-time curve; As shown in Figure 8, the real time record nano-probe the control ultraviolet light beam " open " 15 seconds with " pass " 15 seconds alternate under the impression displacement-time curve, as shown in Figure 9.
(6) under incident uv Shu Zuoyong, the change in displacement analytical approach of nano-probe is identical with step (7) among the embodiment 1.As shown in Figure 9, keeping the indentation load stage, when incident uv Shu Kaiqi 15s, 2nm moves to nano-probe vertically upward from the equilibrium position-the 6nm place, change in displacement is 8nm.When the incident uv bundle was closed 15s, nano-probe turned back to 2nm place, equilibrium position downwards from-6nm.During incident uv bundle periodicity irradiation, the variation of nano-probe displacement generating period property.The photic deflection of then single zinc sulfide nano-belt under incident uv Shu Zuoyong is 8nm.
(7) analyze to such an extent that the thickness of single zinc sulfide nano-belt is 310nm by step (4); Analyze to such an extent that the photic deflection of single zinc sulfide nano-belt under incident uv is 8nm by step (6); The photic deflection of nano belt and the number percent of its thickness are 2.5%; Therefore, the photo-induced telescopic performance of single zinc sulfide nano-belt under incident uv is 2.5%.
Claims (3)
1. the method for a real time measurement for nano material photostrictive performance is characterized in that, comprises the steps:
(1) adopts three chip capacitor plate sensing nano-probe technology to nano material location and imaging, find the nano material smooth planar surface, confirm that nano material is along the thickness that is pressed into direction;
(2) to single zinc oxide nano-belt nano material, to implement original position and be pressed into guarantor's year experiment, the load time is 10s, and loading speed is 4 μ N/s, and hold time is extended for 90s, and keeping indentation load is 40 μ N, and discharge time is set to 10s, and rate of debarkation is 4 μ N/s; Wherein, be 0.8mW/cm in stage hold time that prolongs with power density
2The incident beam of white light is introduced the nano-probe device, and light beam incides the diamond nano probe zone that contacts with nano material;
To single zinc sulfide nano-belt nano material, to implement original position and be pressed into guarantor's year experiment, the load time is 10s, and loading speed is 0.5 μ N/s, and hold time is extended for 60s, and keeping indentation load is 5 μ N, and discharge time is set to 10s, and rate of debarkation is 0.5 μ N/s; Wherein, be 0.2mW/cm in stage hold time that prolongs with power density
2The incident uv bundle is introduced the nano-probe device, and light beam incides the diamond nano probe zone that contacts with nano material;
Stage hold time control incident beam prolonging " was opened " 15 seconds and " pass " 15 seconds alternate, record probe impression displacement-time changing curve; Calculate the poor of the shift value of illumination when beginning and finishing from this curve, be pressed into the photic deflection of direction for the nano material edge;
(3) obtain the photo-induced telescopic strain by the photic deflection of nano material and the number percent of its thickness, this photo-induced telescopic strain is the photo-induced telescopic performance of nano material.
2. the method for a kind of real time measurement for nano material photostrictive performance as claimed in claim 1 is characterized in that, light beam incides the diamond nano probe zone that contacts with nano material after the reflection of the bimirror window of piezoelectric sensor.
3. the method for a kind of real time measurement for nano material photostrictive performance as claimed in claim 1 is characterized in that, nano-probe is Vickers or Nu Shi probe.
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| CN110207868A (en) * | 2019-06-19 | 2019-09-06 | 安徽理工大学 | The preparation and detection method of a kind of light-operated actuator of micro-nano based on micro-cantilever array sensing technology |
| CN113405471B (en) * | 2021-07-14 | 2023-02-10 | 西安电子科技大学 | Optical displacement sensor and optical displacement detection system |
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| CN1793824A (en) * | 2005-12-20 | 2006-06-28 | 西安交通大学 | Method of testing room temperature press-in creeping performance of metal film |
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| CN1793824A (en) * | 2005-12-20 | 2006-06-28 | 西安交通大学 | Method of testing room temperature press-in creeping performance of metal film |
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