CN101393008B - Tapping type high-sensitivity SPM feeler based on PVDF and measurement method - Google Patents
Tapping type high-sensitivity SPM feeler based on PVDF and measurement method Download PDFInfo
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- CN101393008B CN101393008B CN2008101568219A CN200810156821A CN101393008B CN 101393008 B CN101393008 B CN 101393008B CN 2008101568219 A CN2008101568219 A CN 2008101568219A CN 200810156821 A CN200810156821 A CN 200810156821A CN 101393008 B CN101393008 B CN 101393008B
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Abstract
The invention relates to a PVDF-based tapping-mode high-sensitivity SPM measuring head and a measuring method thereof. The PVDF-based tapping-mode high-sensitivity SPM measuring head is characterized in that a PVDF piezoelectric membrane is taken as a vibrating beam and a tungsten probe is taken as scanning probe; the vibrating beam is set to be a simply supported beam with bended radian; the left end and the right end of the vibrating beam are fixed on front ends of oppositely arranged piezoelectric drivers on both sides through clamping structures respectively; rear ends of the piezoelectric drivers on both sides are fixed on respective cantilever beams respectively; one end of each of the cantilever beams is suspended on a measuring head holder; and the scanning probe is fixed on a center position on the lower surface of the vibrating beam. The measuring method takes the variation of electric charges outputted by the vibrating beam to represent the amplitude variation of the vibrating beam caused by a micrometering force, and performs multipoint micrometering force tapping scanning on a surface to be measured to realize measurement of the surface of a sample. The PVDF-based tapping-mode high-sensitivity SPM measuring head and the measuring method can realize high spatial resolution and low measuring force, are suitable for various materials, and can measure under air environment.
Description
Technical field
The present invention relates to nanometer measuring device, a kind of scan-probe microscopic system gauge head that can be used for constituting of more specifically saying so, make system realize the nanometer microscopic appearance measure in the FEEDBACK CONTROL of nano-resolution power on the vertical direction; Can constitute the nanometer positioning probe of micro-nano three coordinate measuring machine, realize the nanometer positioning of three coordinate measuring machine probe; Can be used for constituting the scan-probe microscopic system to realize the frangible sample of softness (as biomaterial surfaces such as protein molecules), sample (as semiconductor silicon micro element, micro-electromechanical device etc.) with precipitous ledge surface feature are carried out the non-destructive microcosmic surface topography measurement of nanometer resolution; And be used to constitute micro-nano three coordinate measuring machine probe to realize the measurement of micro electro mechanical device (MEMS), micromechanical parts.
Background technology
Over past ten years, along with the high-precision requirement to the surface microscopic topographic measurement such as micro semiconductor device, MEMS, nano-device, and biomaterial surfaces such as DNA, the protein molecule non-destructive requirement of measuring, require surveying instrument not only to have nano level resolution, also will have as far as possible little ergometry.
Contact pin type contourgraph commonly used is a kind ofly to be widely used in that mechanical surface is measured, simple and reliable fine measuring instrument, its measurement range can reach tens of millimeters, but its vertical resolution can only reach tens nanometer, and contact pilotage and measured surface Continuous Contact in the measuring process, laterally dynamometry is big, easily cause scuffing, the surface measurement that is not suitable for soft material and has precipitous micromechanism to the surface.Optical measuring systems such as confocal microscope, though have the advantage of non-cpntact measurement, and its highest vertical resolution is near the level of 10 nanometers, but its lateral resolution is subjected to the restriction of focal beam spot diameter and can't improves, and is not suitable for the measurement of non-reflective material.Scanning tunnel microscope (STM) is although have the advantage of vertical resolution and the non-cpntact measurement of Ya Nami, but be subjected to the influence of measured material electric conductivity very big owing to measure electric current, can not directly apply to the easily material of oxidation of insulating material and surface, and the vacuum tightness to measurement environment also has very high requirement, so its usable range has been received very big restriction.Atomic force microscope (AFM) is though be suitable for various materials, the measurement of multiple parameter, and ergometry with vertical resolution and nN level of Subnano-class, but the probe that is adopted is most is silicon micro-cantilever type, its effective length is short, the tip curvature radius is big, coning angle is usually about 30 °, be not suitable for the measurement of big step microcosmic surface, and the control of used silicon cantilever need adopt additional position detection systems such as optical lever method or optical interferometry to realize in the gauge head, the leak light that the optical detection system is produced not only influences the measurement of semiconductor devices electrical quantity, also may bring the interference error to surface measurement.Therefore, complex structure and be difficult to realize to adjust and detect.Therefore, the ubiquity that does not have use in the existing system for measuring surface appearance.
Summary of the invention
The present invention is for avoiding above-mentioned existing in prior technology weak point, provide a kind of tapping type high-sensitivity SPM feeler and measuring method, to realize high spatial resolution, low ergometry, be fit to various materials, satisfy the measurement of the surface topography of submillimeter microcosmic difference in height based on PVDF.
Technical solution problem of the present invention adopts following technical scheme:
The design feature that the present invention is based on the tapping type high-sensitivity SPM feeler of PVDF is to be walking beam, to be scan-probe with the tungsten tipped probe with the PVDF piezoelectric membrane; Described walking beam is set to have the free beam of crooked radian, the two ends, the left and right sides of walking beam are separately fixed at the front end of the both sides piezoelectric actuator that is oppositely arranged by clamp structure, the rear end of both sides piezoelectric actuator is separately fixed on separately the semi-girder, and semi-girder is single-ended suspending and is arranged on the head-measuring rack; Scan-probe is fixedly installed on the center of walking beam lower surface.
The characteristics of measuring method that the present invention is based on the tapping type high-sensitivity SPM feeler of PVDF are to apply the AC sinusoidal voltage signal of amplitude and frequency adjustable as drive signal on the piezoelectric actuator of both sides, under drive signal, both sides piezoelectric actuator along continuous straight runs produces and comes and goes displacement, and by walking beam scan-probe is vertically vibrated; Adjust driving signal frequency, make walking beam be in the Near resonance oscillating state; In the scanning process, when scan-probe did not touch specimen surface as yet, walking beam was operated in the Near resonance oscillating state, produced free amplitude A
0, free amplitude A
0Under walking beam be output as free amplitude quantity of electric charge C
0Contact with moment that sample takes place on a bit at certain for scan-probe, walking beam produces the amplitude A that decays
1, the decay amplitude A
1Under walking beam be output as decay quantity of electric charge C
1, characterize the variation of walking beam amplitude with the change of the quantity of electric charge of walking beam output, on tested surface, carry out multiple spot micrometering power and rap scanning and realize measurement specimen surface.
The PVDF that is adopted among the present invention (Polyvinylidene Fluoride) piezoelectric membrane has another name called polyvinylidene difluoride film, is the piezoelectric membrane of being made by high polymer piezoelectric material, has good piezoelectric property, along the electric constant g perpendicular to the plane of polarization direction
31Can reach 0.26Vm/N.The density of PVDF piezoelectric membrane is at 1.76～1.80g/cm
3Between, frivolous softness, and have certain elasticity, serviceability temperature is-40～150 ℃; SPM is scanning probe microscopy (Scanning Probe Microscope).Scanning head is the tungsten tip by the big L/D ratio of electrochemical milling method acquisition among the present invention.
The present invention replaces rapping silicon materials cantilever in the mode atomic force microscopy with poly meta fluoroethylene piezoelectric film PVDF, constitute the scan-probe gauge head in conjunction with the tungsten tipped probe in the scanning tunnel microscope, in this structure, piezoelectric membrane PVDF with piezoelectric effect both uses as the micro-cantilever of band probe among the similar atomic force microscope AFM, again as the force-sensing sensor among the similar scanning force microscopy SFM to detect the variation of small power or displacement.Gauge head of the present invention is combined with the atomic force microscope measuring system, can realize that the sample (as biomaterial surfaces such as protein molecules) that various materials are constituted, the sample (as semiconductor silicon micro element, micro-electromechanical device etc.) with precipitous ledge surface feature etc. carry out the non-destructive microcosmic surface topography measurement of nanometer resolution.
Compared with the prior art, beneficial effect of the present invention is embodied in:
1, encourages the PVDF piezoelectric membrane walking beam that shakes with piezoelectric actuator among the present invention, PVDF piezoelectric membrane walking beam is both as the cantilever of scanning constant probe, also, avoided numerous and diverse additional position pick-up unit well as the sensor that detects PVDF piezoelectric membrane walking beam amplitude variations;
2, the PVDF walking beam works in resonant condition during measuring process of the present invention, and scan-probe contacted with the surperficial moment of tested sample, and ergometry can be reduced to receives ox (10
-9Newton) magnitude can realize the silicon micro element of the cracked damage of commute and the high-acruracy survey of nano-device, and is more great for the high precision non-destroyed measurement meaning of the Biosample of frivolous soft cracky;
3, the present invention adopt have big L/D ratio, most advanced and sophisticated coning angle is that tungsten tipped probe about 10 ° is a scan-probe, therefore is particularly suitable for the high precision of soft material surface and big ledge surface etc., the measurement that micrometering is measured one's own ability.
Description of drawings
Fig. 1 is the schematic diagram of PVDF vibration of thin membrane beam of the present invention.
Fig. 2 is the invention structural representation.
Fig. 3 is the plan structure synoptic diagram of Fig. 2.
Number in the figure: 1 head-measuring rack, 2 regulating tanks, 3 semi-girders, 4 piezoelectric actuators, 5 left side piezoelectric actuator drive wires, 6 walking beams, 7 scan-probes, 8 film charge signal extension lines, 9 right side piezoelectric actuator drive wires, 10 clamp structures.
Below pass through embodiment, and in conjunction with the accompanying drawings the present invention done an into explanation:
Embodiment:
Referring to Fig. 1, Fig. 2, this example is to be walking beam 6, to be scan-probe 7 with the tungsten tipped probe with the PVDF piezoelectric membrane; Walking beam 6 is set to have the free beam of crooked radian, the two ends, the left and right sides of walking beam 6 are separately fixed at the front end of the both sides piezoelectric actuator 4 that is oppositely arranged by clamp structure 10, the rear end of both sides piezoelectric actuator 4 is separately fixed on separately the semi-girder 3, and semi-girder 3 is single-ended suspending and is arranged on the head-measuring rack 1; Scan-probe 7 is fixedly installed on the center of walking beam 6 lower surfaces.
Measuring method is to apply the AC sinusoidal voltage signal of amplitude and frequency adjustable as drive signal on both sides piezoelectric actuator 4, under drive signal, piezoelectric actuator 4 along continuous straight runs in both sides produce and come and go displacement, and by walking beam 6 scan-probe 7 are vertically vibrated; Adjust driving signal frequency, make walking beam 6 be in the Near resonance oscillating state; In the scanning process, when scan-probe 7 did not touch specimen surface as yet, walking beam 6 was operated in the Near resonance oscillating state, produced free amplitude A
0, free amplitude A
0Under walking beam 6 be output as free amplitude quantity of electric charge C
0Contact with moment that sample takes place on a bit at certain for scan-probe 7, walking beam 6 produces the amplitude A that decay
1, the decay amplitude A
1Under walking beam be output as decay quantity of electric charge C
1, characterize the variation of walking beam amplitude with the change of the quantity of electric charge of walking beam output, on tested surface, carry out multiple spot micrometering power and rap scanning and realize measurement specimen surface.
Regulating tank 2 shown in Fig. 2 can be used to adjust the distance between the both sides piezoelectric actuator 4, reach and adjust the purpose that PVDF vibration of thin membrane beam is the radian size, left side piezoelectric actuator lead-in wire 5 and right side piezoelectric actuator lead-in wire 9 input leads as the piezoelectric actuator drive signal, film charge signal extension line 8 is as the leading-out end line of charge signal.
About the gauge head vibration frequency:
In the formula of the rapping scanning feeler based on the PVDF walking beam, the principle of its walking beam structure as shown in Figure 1, among the figure, one deck PVDF piezoelectric membrane constitutes the walking beam structure, length is l.When two ends are squeezed and stretch the power F that draws, will produce forced vibration along directions X.Got by correlation analysis, this two ends fixedly walking beam structural vibrations frequency can have following formula to express:
Wherein, A is the cross-sectional area of PVDF piezoelectric membrane; F is the acting force that is carried in two ends, the piezoelectric membrane left and right sides; L, b, h are respectively length, width and the thickness of piezoelectric membrane; E is a Young's modulus of elasticity, and I is the moment of inertia of piezoelectric membrane.
Can express by following formula and be carried in two ends, piezoelectric membrane left and right sides directed force F:
F＝4πEI/l
2
So, the walking beam structure that constitutes of PVDF piezoelectric membrane is just can be by estimating that following formula is similar to along the vibration frequency of directions X:
As from the foregoing, the factor that influences the walking beam vibration frequency mainly comprises: the length l of piezoelectric membrane, width b, thickness h and moment of inertia I, other are the constant relevant with material.Therefore, the dimensional parameters of change piezoelectric membrane has also just changed the vibration frequency of walking beam.
Influence the parameter of gauge head performance:
Two important parameters weighing SPM gauge head performance are the resolution that gauge head can reach in vertical direction, and gauge head in the scanned sample process to the ergometry of specimen surface.And the parameter that characterizes these two performance index height mainly is raise one's arm elastic constant k and quality factor q.
The mechanical elasticity constant k is meant the suffered power of PVDF piezoelectric membrane walking beam 6 (ergometry when just probe contacted with specimen surface moment under the pattern of rapping) and the elastic deformation amount's who produces ratio on vibration of thin membrane beam 6, unit is " Newton/meter ".What of the height of the sensitivity of gauge head, the size of ergometry and the piezoelectric signal charge number that produces this ratio be directly connected to.That is to say when probe is being measured when contacting with surperficial moment, mechanical elasticity constant k value is more little, very little ergometry just can make piezoelectric membrane walking beam 6 produce very big distortion, the variation that piezoelectric membrane also just can produce enough quantities of electric charge is used for detecting, therefore such walking beam sensitivity is very high, required ergometry is very little, the charge signal vary within wide limits; Otherwise, mechanical elasticity constant k value is big more, need very big ergometry just can make piezoelectric membrane walking beam 6 produce enough deflections, the variation that could produce enough quantities of electric charge is used for detecting, the walking beam sensitivity that is constituted is lower, and the ergometry to sample is very big, and the variation of charge signal is also not obvious.
Quality factor q is a basic parameter of reflection dynamic performance.In vibrational system, quality factor q is defined as follows formula:
Wherein, E is the gross energy of vibrational system; Δ E is the energy of vibrational system vibration one-period loss; F0 is the resonance frequency of amplitude when reaching maximum; And f
1＜f
0＜f
2, f
1, f
2Be respectively f
0The vibration frequency value of 0.707 times of peak swing place, both sides correspondence.This that is to say that in a vibrational system quality factor have characterized what of system vibration one-period internal loss energy, the size of system damping and the height of vibration peak.
For above-mentioned gauge head, following three the aspect performances of the main influence of the size of quality factor q: promptly rap the resonance amplitude size that 6 on PVDF vibration of thin membrane beam can reach in the scanning process; Moment takes place and contact front and back, the size of walking beam 6 amplitude change amounts in probe and surface; Walking beam 6 is returned to the length of stable oscillation state required time.Just quality factor are high more, and under the situation of identical contact force, the change amount of vibration of thin membrane beam 6 amplitudes is big more, and force sensitivity is high more, but it is long more to be returned to the required time of steady state (SS); Otherwise then the change amount of amplitude is less, and force sensitivity is lower, but more easily keeps stable vibrational state.
Therefore, have higher resolution and less dynamometry, will rationally adjust each structural parameters that Q and k are exerted an influence in order to make system.
After having determined the good total system of each structural parameters of PVDF film and framework, just can actually test the sensitivity that this gauge head structure can reach.Test is to realize in the following manner: control nanometer displacement platform moves in the vertical direction, constantly approach with certain stepping amount (as 1nm) to tungsten tipped probe 7, when probe 7 moment takes place when contacting with the nanometer displacement platform at certain on a bit, the amplitude of vibration of thin membrane beam 6 will be decayed.Because reducing of membrane oscillation amplitudes, the quantity of electric charge that the PVDF piezoelectric membrane is produced also can reduce accordingly, and the amplitude of the detected voltage signal of testing circuit also can reduce thereupon.Stepping amount during generation touching by noting and the decrease of voltage signal, just can calculate the sensitivity of this gauge head structure, its unit is V/ μ m.Sensitivity is high more, and the spatial resolution that is characterizing the vertical direction that the SPM scanning probe microscope system built by this gauge head structure can reach is high more; Otherwise then the resolution that can reach is just lower.In addition, sensitivity test can be used to also verify whether each parameter of selected film is appropriate.
Experimental data:
In measuring, length I, width b by changing PVDF vibration of thin membrane beam 6 structural parameters such as film and thickness h and walking beam 6 be radian and survey the performance that this novel gauge head can reach, the radian that walking beam 6 is can be realized by the distance D between the regulating tank 2 adjustment both sides piezoelectric actuators 4.
The physical dimension of the piezoelectric membrane of being determined by experimental result is: I=10mm, and b=2.5mm, h=40 μ m, radian that walking beam is are the best when clamp structure 10 space D=9.5mm.The quality factor q of gauge head is 24.3, and elastic constant k is 35N/m.
Wherein, quality factor q will be far below the quality factor (being generally thousands of) of AFM gauge head, and this is relevant with the structure and the working environment under the atmosphere of this novel gauge head, has caused the damping of vibrational system bigger, and the energy of system vibration loss is also big.But under the situation that has guaranteed enough sensitivity, lower Q value but can guarantee the stable of system vibration, shortens the time of replying steady state (SS), so just can improve sweep velocity and work efficiency; And the mechanical elasticity constant k of walking beam is 35N/m, also just improve the sensitivity of this novel gauge head much smaller than the elastic constant of the hundreds of Newton/meter of silicon micro-cantilever, and specimen surface is had slighter ergometry.
Through measuring, the scan-probe microscopic system that constitutes of gauge head thus, sensitivity is 1.98V/ μ m, and the amplitude of free vibration is 150～200nm, and vertical resolution reaches 1.6nm, and scanning survey power is the nN level.
Claims (2)
1. based on the tapping type high-sensitivity SPM feeler of PVDF, it is characterized in that being walking beam (6), being scan-probe (7) with the tungsten tipped probe with the PVDF piezoelectric membrane; Described walking beam (6) is set to have the free beam of crooked radian, the two ends, the left and right sides of walking beam (6) are separately fixed at the front end of the both sides piezoelectric actuator (4) that is oppositely arranged by clamp structure (10), the rear end of both sides piezoelectric actuator (4) is separately fixed on separately the semi-girder (3), and semi-girder (3) is single-ended suspending and is arranged on the head-measuring rack (1); Described scan-probe (7) is fixedly installed on the center of walking beam (6) lower surface.
2. the measuring method of the described tapping type high-sensitivity SPM feeler based on PVDF of a claim 1, it is characterized in that on described both sides piezoelectric actuators (4), applying the AC sinusoidal voltage signal of amplitude and frequency adjustable as drive signal, under described drive signal, both sides piezoelectric actuator (4) along continuous straight runs produces and comes and goes displacement, and by walking beam (6) scan-probe (7) is vertically vibrated; Adjust driving signal frequency, make walking beam (6) be in the Near resonance oscillating state; In the scanning process, when not touching specimen surface as yet, walking beam (6) is operated in the Near resonance oscillating state, produces free amplitude A at scan-probe (7)
0, free amplitude A
0Under walking beam (6) be output as free amplitude quantity of electric charge C
0Contact with moment that sample takes place on a bit at certain for scan-probe (7), walking beam (6) produces the amplitude A that decays
1, the decay amplitude A
1Under walking beam (6) be output as decay quantity of electric charge C
1, characterize the variation of walking beam amplitude with the change of the quantity of electric charge of described walking beam (6) output, on tested surface, carry out multiple spot micrometering power and rap scanning and realize measurement specimen surface.
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| CN2008101568219A CN101393008B (en) | 2008-09-26 | 2008-09-26 | Tapping type high-sensitivity SPM feeler based on PVDF and measurement method |
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| CN2008101568219A CN101393008B (en) | 2008-09-26 | 2008-09-26 | Tapping type high-sensitivity SPM feeler based on PVDF and measurement method |
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| CN101393008B true CN101393008B (en) | 2011-09-28 |
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| CN102538657B (en) * | 2011-12-30 | 2014-12-03 | 合肥工业大学 | Three-dimensional resonance trigger measuring head based on PVDF (polyvinylidene fluoride) and three-dimensional resonance trigger positioning method |
| CN109555006B (en) * | 2018-10-29 | 2020-10-02 | 山东理工大学 | Beam spring vibration damper |
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