CN100370263C - Method and apparatus for measuring material piezoelectric coefficient by using scanning near-field microwave microscopy - Google Patents
Method and apparatus for measuring material piezoelectric coefficient by using scanning near-field microwave microscopy Download PDFInfo
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- CN100370263C CN100370263C CNB2005100407875A CN200510040787A CN100370263C CN 100370263 C CN100370263 C CN 100370263C CN B2005100407875 A CNB2005100407875 A CN B2005100407875A CN 200510040787 A CN200510040787 A CN 200510040787A CN 100370263 C CN100370263 C CN 100370263C
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Abstract
The present invention relates to the measurement technology of the piezoelectric property of materials, more particularly to a method and an apparatus for measuring piezoelectric coefficients by using a near-field scanning microwave microscope by a converse piezoelectric effect. The present invention is characterized in that a sample to be tested is produced, and a dielectric constant epsilon of the sample is measured; then, the output end of a signal generator is connected with an electrode of the sample, and is divided into a circuit to be connected to the input end of a reference signal of a phase-locking amplifier, so that a cycle modulation signal is added on the electrode of the sample; the input end of the phase-locking amplifier is communicated with the output end of a frequency signal of a microscope controller, the output end of the phase-locking amplifier is connected to a data collection and processing system to probe the same cycle modulation signal v of the sample in a micro signal caused by the cyclomorphosis of a piezoelectricity effect; a piezoelectric coefficient d<ij> is equal to-1/(5.80 b<2> minus 9.09 bplus 3.77) gL/ASf<0>l v/V. The method of the present invention has the advantages of high precision, high scanning speed and micro region distinguishing. The present realizes and large range and fast scan for the sample, and accordingly, conveniently and swiftly obtain large area of distribution situation of the piezoelectric property of materials.
Description
Technical field
The present invention relates to the measuring technique of material piezoelectric property, be specifically related to utilize inverse piezoelectric effect to measure the method and the device of material piezoelectric coefficient.
Background technology
Piezoelectric effect is meant and produces the phenomenon that produces mechanical deformation (being called inverse piezoelectric effect) under electric charge (being called direct piezo electric effect) or the alive outside effect under the stressed outside effect of material that both are different expression forms of same essence.Material with obvious piezoelectric effect is called as piezoelectric.Piezoelectric is called as piezoelectric modulus at electric charge that produces under the unit pressure effect or the deformation quantity that produces under the unit voltage effect, be used for weighing the size of piezoelectric effect.Owing to realized machine one electric coupling, piezoelectric is widely used in fields such as precision optical machinery, sensor, microelectronics, MEMS (micro electro mechanical system).
In the prior art, the method for measuring material piezoelectric coefficient can be divided into two big classes, utilizes direct piezo electric effect and inverse piezoelectric effect respectively.
When utilizing direct piezo electric effect to measure piezoelectric modulus, with tested piezoelectric material slabbing, make electrode at two end face, exert pressure on material then, the electric charge on the potential electrode obtains piezoelectric modulus.According to the technology difference of exerting pressure, they can be divided into again: vertical loading method, air pressure platform method etc.These methods are comparatively simple, but precision is not high, and piezoelectric property that can not the exosyndrome material microcell, use seldom at present.
When utilizing inverse piezoelectric effect to measure piezoelectric modulus, also need on measured material, to make electrode, apply voltage by electrode to material then, measure the deformation of material, obtain piezoelectric modulus.According to the method difference of measuring deformation, they can be divided into again: laser interferance method and atomic force microscopy etc.These methods have the high advantage of measuring accuracy, are the main measuring methods of present piezoelectric modulus.
The deformation that laser interferance method utilizes the principle of laser interference range finding to measure piezoelectric effect, but be subjected to the restriction of optical diffraction effect, its spatial resolving power can only reach the magnitude of sub-micron, can't check the small piezoelectricity deformation of film, and the microscopic uniformity of observing material also has certain restriction.
The principle of work of atomic force microscope is: when a superfine needle point and object were close to atomic scale, the atom at needle point tip and the atom on the object interacted, and this acting force can change the intrinsic mechanical resonance frequency of needle point.Excite the vibrations of needle point with an electronic system, survey the frequency or the amplitude of needle point resonance, and the distance of regulating probe and sample by feedback system, make resonant frequency or amplitude constant on a setting value, can obtain the height of this sample, by the relative scanning of sample and probe, can obtain the feature image of sample surfaces again.The method of measuring piezoelectric modulus with atomic force microscope is: apply an alternating voltage with conducting probe (can make or plate conductive layer on probe with conductive material) contact top electrode to material, because piezoelectric effect, material can produce the deformation with adding alternating voltage same frequency, this deformation will atomic force microscope apart from feedback system in produce the feedback signal of a same frequency.This signal can be surveyed with a lock-in amplifier.Because feedback signal is proportional to deformation quantity, and deformation quantity is proportional to piezoelectric modulus, and therefore, through suitable calibration, as by the measurement of known piezoelectric modulus material sample is demarcated, available the method is measured the piezoelectric modulus of material.Because the spatial resolution of atomic force microscope is high, the measuring accuracy of this method is also very high and have an ability of measuring each regional piezoelectric modulus of material.But because the probe of atomic force microscope and measured material sample are at a distance of too closely (distance of having only atomic scale), measure and be very easy to the damage needle point when big piezoelectricity deformation and mobile example are measured each regional piezoelectric modulus of material, thereby be difficult to realize the quick scanning in each zone of large tracts of land sample.
Scanning near-field microwave microscopy is a new developing technology in recent years.It is contained in probe on the center conductor of a quarter-wave coaxial microwave resonant cavity, with probe load microwave, as sample during near needle point, interaction by sample and needle point microwave field, comprise contact and contactless, the electric charge and near the microwave field the needle point that change on the probe distribute, and then change the resonant frequency and the quality factor of resonant cavity.By surveying this variation, can infer many character of sample, as the specific inductive capacity of sample microcell, dielectric loss etc.The spatial resolving power of scanning near-field microwave microscopy has reached 100 nanometers.
Still find no at present the report that utilizes scanning near-field microwave microscopy that material piezoelectric coefficient is measured.Its reason is: the frequency shift signal of scanning near-field microwave microscopy depends on the specific inductive capacity of sample and the distance between sample and the probe, and when sample is the specific inductive capacity of metal material or known materials, then signal only depends on the distance of probe and sample room.Though in theory, the deformation that piezoelectric effect causes can change acquisition by the distance of above-mentioned relation measuring samples probe, but in fact because piezoelectricity deformation very small (less than 1 nanometer sometimes), therefore the feeble signal that is caused by this deformation can be flooded by the intrinsic noise of system, cause and to obtain the deformation data, that is to say that existing scanning near-field microwave microscopy still can not directly be measured piezoelectricity deformation, also just can't obtain piezoelectric modulus naturally.
Summary of the invention:
The objective of the invention is to, overcome the deficiencies in the prior art, a kind of method of utilizing scanning near-field microwave microscopy to measure material piezoelectric coefficient is provided.This technology has the precision height, speed is fast and the microcell measurement capability, can realize on a large scale scanning fast, thereby can obtain the large tracts of land distribution situation of material piezoelectric property easily.
Purpose of the present invention realizes in the following manner.
The present invention utilizes scanning near-field microwave microscopy that material is carried out the method that piezoelectric modulus is measured, comprise and at first make the measured material sample that has electrode, and measure the DIELECTRIC CONSTANT of this material sample or obtain the DIELECTRIC CONSTANT (to the situation of electrode of metal, this goes on foot omission) of this material sample by inspection information; Then the measured material sample is fixed on the sample stage of scanning near-field microwave microscopy, and makes the axis direction of deformation direction along probe, set the probe of scanning near-field microwave microscopy and sample room apart from g; It is characterized in that operation steps after this is:
(1) the ac cycle modulation signal that signal generator is sent is added on the electrode of measured material sample.
(2) utilize lock-in amplifier to survey the measured material sample because the same periodic modulation signal v in the scanning near-field microwave microscopic signal that the deformation of piezoelectric effect generating period is caused.
(3) calculate the piezoelectric coefficient d of measured material sample according to following formula
Ij:
Wherein: A is the scanning near-field microwave microscopy calibration constants, and S is the frequency response coefficient of scanning near-field microwave microscopy microwave system, f
0Be near the resonant frequency of the microwave resonance cavity during n.s. probe, L is the distance between two parallel poles, and l is the measured material sample thickness, and V is the modulation voltage that signal generator provides, b=(ε-ε
0)/(ε+ε
0), ε
0It is permittivity of vacuum.
In the said method, the probe of described setting scanning near-field microwave microscopy and measured material sample room apart from g be: when measuring horizontal piezoelectric coefficient d
Ij(during i ≠ j), the probe of scanning near-field microwave microscopy is controlled at from measured material sample 0.01R
0To 0.1R
0Distance, R wherein
0Be the needle point radius-of-curvature; When measuring vertical piezoelectric coefficient d
IiThe time, make the probe of scanning near-field microwave microscopy be controlled at distance from 0.1 micron to 10 microns in measured material sample.
In above-mentioned measuring method, at measuring vertical piezoelectric modulus (being that the deformation direction is consistent with the applied field direction) and horizontal two kinds of situations of piezoelectric modulus (being that the deformation direction is vertical with the applied field direction), two kinds of different electrode allocation plans are arranged: for measuring horizontal piezoelectric coefficient d
Ij(i ≠ j) makes in electrode or the upper surface at membraneous material in two sides of measured material sample and to make electrode, makes the applied field direction vertical with the deformation direction of measurement; To measuring vertical piezoelectric coefficient d
Ii, make electrode in the upper and lower surface of measured material sample, make the applied field direction consistent with the direction of the deformation of measurement, calculate piezoelectric coefficient d this moment
IjSimplified formula be
The present invention utilizes scanning near-field microwave microscopy to measure the device of material piezoelectric coefficient, the scan table, probe, controller and the data Collection ﹠ Processing System that comprise scanning near-field microwave microscopy of the prior art, and signal generator, lock-in amplifier, the signal output part of described signal generator is used for linking to each other with the electrode of sample, tells one road reference signal input end that is connected to lock-in amplifier simultaneously; The input end of described lock-in amplifier is communicated with the frequency signal output terminal of scanning near-field microwave microscopy controller, and the output terminal of this lock-in amplifier is connected in the data Collection ﹠ Processing System.When being provided with the built-in signal generator in the lock-in amplifier, can be without the outer signal generator, but directly the output of lock-in amplifier built-in signal generator is received on the electrode of measured material sample.Signal generator, lock-in amplifier and near-field microwave microscopy common ground.
The present invention is directed to the not deficiency of energy measurement material micro-zone piezoelectric coefficient of scanning near-field microwave microscopy, creatively will modulate---phase lock amplifying technology is integrated in the scanning near-field microwave microscopy, and obtained the quantitative relationship of modulation signal and material micro-zone piezoelectric coefficient by theoretical analysis, produced a kind of new method of utilizing scanning near-field microwave microscopy to measure the material micro-zone piezoelectric coefficient.Because in the prior art, scanning near-field microwave microscopy can have been measured microcell specific inductive capacity, dielectric loss, the nonlinear dielectric constant of material, behind the present invention, these piezoelectric property correlation parameters that need originally to measure respectively can be measured simultaneously, therefore, the present invention has expanded the range of application of scanning near-field microwave microscopy.
Compare with laser interferance method, distance resolution of the present invention is greatly improved, and brings up to the level (referring to embodiment 1) of several micromicrons from sub-micron.Because signal of the present invention is from scanning near-field microwave microscopy, therefore have the horizontal space resolution characteristic identical with scanning near-field microwave microscopy, 100 nanometers just, this also is better than the horizontal space resolution characteristic of laser interferance method.
Compare with the atomic force microscope method, probe of the inventive method and sample room have the gap of a micron dimension, and the sample that the injustice because of the vibrations of sample stage in the scanning process or sample surfaces causes and the collision of needle point have been avoided in the existence in this gap effectively.Because in the atomic force microscope, probe and sample have been close to the yardstick of atom size, any small vibrations all can cause the collision of sample and needle point and then damage probe.For fear of this collision, must reserve time enough and when sample is further close, have enough time to return by needle point.Therefore, atomic force microscope generally can only reach the image scanning speed of about 1000 of per seconds, and sweep limit also can only arrive about 100 microns.And in the present invention, the existence in micron dimension gap makes probe have time enough to return probe before sample is run into needle point, so speed image and sweep limit are all unrestricted.Speed image depends primarily on electronic technology in the prior art, can reach per second 100,000 points, and sweep limit then depends on the size of platform.This technical breakthrough has important application prospects in investigation of materials.For example, in the screening of environment-friendly type lead-free piezoelectric ceramics, people estimate theoretically, variation along with material constituent element composition, the piezoelectric property of material is also along with changing, near the accurate similar shape phase boundary that the material crystals structure changes, the structure of material is subjected to having the greatest impact of outfield, and corresponding piezoelectric effect also can reach maximum value.For seek accurate similar shape phase boundary, traditional method need be synthesized a series of sample, the piezoelectric properties of composition Study material one by one, such need of work expends a large amount of man power and materials, can finish just change long time.Adopt combined method, the mode of all compositions with material chip can be made on the same substrate, disposable structure and the performance study of finishing all the components in the system.Because the size of material chip is in a centimetre magnitude, when its piezoelectric properties are characterized, need be with the mode scanning fast on a large scale of microcell, atomic force microscope method (sweep limit and sweep velocity) and laser interferance method (sensitivity and spatial resolving power) all can not satisfy this requirement, have only the present invention of employing could satisfy this demand.
Be described further below by embodiment and accompanying drawing thereof.
Description of drawings
Fig. 1 is the structural representation that utilizes scanning near-field microwave microscopy to measure the material piezoelectric coefficient device of the present invention.
Electrode configuration schematic diagram when Fig. 2 is the vertical piezoelectric modulus of measurement of the present invention.
Electrode configuration schematic diagram when Fig. 3 is the horizontal piezoelectric modulus of measurement of the present invention.
Fig. 4 is of the present invention to the measurement curve of the vertical piezoelectric signal of PZT piezoelectric ceramics with the probe sample variable in distance.
Fig. 5 is the measurement curve that the vertical piezoelectric signal of PZT piezoelectric membrane is changed with modulation voltage of the present invention.
Referring to Fig. 1, will be fixed on the material sample 3 of electrode on the scan table 2 of scanning near-field microwave microscopy; The 5th, sweep Retouch the support of near-field microwave microscopy, 6 is the microwave probe of scanning near-field microwave microscopy, and the signal of signal generator 1 is defeated Go out end and link to each other with two electrodes of material sample 3 and tell one tunnel reference signal input that is input to lock-in amplifier 9, The frequency signal output of scanning near-field microwave microscopy controller 7 is told the input of one tunnel input lock-in amplifier, should The output of lock-in amplifier is connected with data Collection ﹠ Processing System 8. Signal generator 1, lock-in amplifier 9 and near field The microwave microscopy common ground. After the ac cycle modulation signal that signal generator 1 produces is added on the sample by electrode, Because the cause of piezo-electric effect, sample 3, cause sample 3 and scanning near-field microwave microscopy with the deformation of generating period Distance between the probe 4 also generating period sexually revises, and then causes scanning near-field microwave microscopy controller 7 output signals The periodic modulation of (resonant frequency), this synperiodic modulation signal will be carried from background noise by lock-in amplifier 9 Take out, enter in the data Collection ﹠ Processing System 8.
Electrode configuration mode among Fig. 2 is used for the measurement of vertical piezoelectric modulus. Wherein, 4 is scanning near-field microwave microscopy Probe, 3 is sample. 10, the 11st, be connected two electrodes on the sample upper and lower surface, they are sent out with signal respectively Giving birth to device 1 connects. Arrow among the figure represents the applied field direction. As seen from the figure, the deformation direction of sample and institute power up Field direction is consistent, all along the axis direction of probe.
Fig. 3 is for measuring the electrode configuring condition of the horizontal piezoelectric modulus of film, and 4 is the probe of scanning near-field microwave microscopy, quilt Test sample product 3 are film, and two electrodes 12 all are arranged on the upper surface of sample thin film, and they are connected with signal generator 1 respectively. Arrow among the figure represents the applied field direction. As seen from the figure, the deformation direction of sample (along the axis direction of probe) Mutually vertical with applied field direction (axis direction of Vertrical probe).
Embodiment
Embodiment 1: measure the vertical piezoelectric modulus of PZT piezoelectric ceramics
(1) by the lead titanate-zirconate at a 5mm * 5mm * 4mm shown in Figure 2 (Pb (ZrTi) O
3Be called for short: PZT) on the upper and lower surface of piezoelectric ceramics block sample electrode is set, be fixed in near-field microwave microscopy (EMP2001, U.S. ArielTechnology, Inc.) on the scan table, and press Fig. 1, connection device therefor shown in Figure 2 and energized: with signal generator (SG1643, Jiangsu flood Zerit Electronics Equipment Co., Ltd) the sinusoidal alternating voltage that produces is received on two electrodes of piezoelectric ceramics sample, and the signal of near-field microwave microscopy output is received lock-in amplifier, and (SR 830, U.S. Stanford Research Systems, Inc.) input end, the modulation signal that signal generator produces is told one the tunnel and is linked to each other with lock-in amplifier reference signal input end, and described power supply is the 220V AC mains.
When being provided with the built-in signal generator in the lock-in amplifier, can be without the outer signal generator, the electrode of directly output of lock-in amplifier built-in signal generator being received piezoelectric ceramics gets final product.
(2) adjusting the probe location of scanning near-field microwave microscopy, make probe from afar continuously near sample, is 45 microns up to the distance of needle point and sample;
(3) continue to make probe near sample, during less than 45 microns, read value from data Collection ﹠ Processing System with periodic modulation signal v every 0.1 micron in needle point and sample distance, up to both apart from the 0-0.1 micrometer range;
(4) with various data (scanning near-field microwave microscopy calibration constants A, the frequency response coefficient S of scanning near-field microwave microscopy microwave system, the resonant frequency f of microwave resonance cavity during n.s.
0, the distance L between two parallel poles, the modulation voltage V that sample thickness l, signal generator provide is with periodic modulation signal v value) be input in the data Collection ﹠ Processing System, according to piezoelectric coefficient d of the present invention
IjComputing formula is calculated the piezoelectric coefficient d that records on the different probe sample distance
IjValue is tested to computing formula of the present invention.
Fig. 4 is the measurement result of above-mentioned ceramic block sample.Inverted triangle symbol wherein is the output signal (all measurement points not being drawn among the figure) of actual measurement lock-in amplifier, solid line is the result with computing formula match of the present invention, and its ordinate is the v in left side, and the modulation voltage during measurement is 5V, modulating frequency is 1kHz, and remains unchanged.Block symbol among the figure is the piezoelectric modulus that calculates with the present invention, and dotted line is the mean value that calculates, and its ordinate is the d on right side
33From calculating, when distance was close to below 10 microns, the value of modulation signal v reached more than 3 times of noise, satisfied the requirement of calculating piezoelectric modulus with the present invention.The difference of vertical piezoelectric modulus of measuring on the different distance is in the scope of noise, and its best-fit values is 650pm/V, and this numerical value is in the reasonable error scope with other method measurement result.The measuring accuracy that is calculated by background noise is 5pm.This shows, when the distance of probe and sample when 10 μ m are following, the signal of measurement all enough provides result accurately.Show that thus measuring method of the present invention has practicality, and higher degree of accuracy is arranged.
Embodiment 2: vertical piezoelectric modulus of measuring pzt thin film
Sample is one the 1 thick PZT piezoelectric membrane of μ m, and by the electrode of making on sample shown in Figure 2, the near-field microwave microscopy of selecting for use, signal generator, lock-in amplifier are identical with embodiment 1, and circuit connecting mode is also identical.Near-field microwave microscopy is chosen 1.24 microns with the distance of probe and sample top electrode, and remains unchanged.The resonant frequency f of microwave resonance cavity when the frequency response coefficient S of scanning near-field microwave microscopy calibration constants A, scanning near-field microwave microscopy microwave system, n.s.
0All identical with embodiment 1.Represented the situation of change (block symbol, modulating frequency stuck-at-kHz) of the output of lock-in amplifier among Fig. 5, also provided non-piezoelectric material---the measurement result (solid garden circle) of glass among the figure as the test of back of the body end noise with modulation voltage.As can be seen from the figure the output of lock-in amplifier and modulation voltage satisfy good linear relationship, its slope of match v/V, the i.e. piezoelectric coefficient d that calculates with formula of the present invention
33Be 82.2pm/V.
Claims (5)
1. one kind is utilized scanning near-field microwave microscopy that material is carried out the method that piezoelectric modulus is measured, comprise at first making having the measured material sample of electrode, and measure the DIELECTRIC CONSTANT of this material sample or obtain the DIELECTRIC CONSTANT of this material sample by inspection information; Then the measured material sample is fixed on the sample stage of scanning near-field microwave microscopy, and makes the axis direction of deformation direction along probe, set the probe of scanning near-field microwave microscopy and sample room apart from g; It is characterized in that operation steps after this is:
(1) the ac cycle modulation signal that signal generator is sent is added on the electrode of measured material sample,
(2) utilize lock-in amplifier to survey the measured material sample because the same periodic modulation signal v in the scanning near-field microwave microscopic signal that the deformation of piezoelectric effect generating period is caused,
(3) calculate the piezoelectric coefficient d of measured material sample according to following formula
Ij
Wherein: A is the scanning near-field microwave microscopy calibration constants, and S is the frequency response coefficient of scanning near-field microwave microscopy microwave system, f
0Be near the resonant frequency of the microwave resonance cavity during n.s. probe, L is the distance between two parallel poles, and l is the measured material sample thickness, and V is the modulation voltage that signal generator provides,
B=(ε-ε
0)/(ε+ε
0), ε
0It is permittivity of vacuum.
2. the scanning near-field microwave microscopy that utilizes as claimed in claim 1 carries out the method that piezoelectric modulus is measured to material, it is characterized in that, when measuring horizontal piezoelectric coefficient d
Ij(during i ≠ j), the probe of described setting scanning near-field microwave microscopy and measured material sample room apart from g at 0.01R
0To 0.1R
0Between, R wherein
0Be the needle point radius-of-curvature.
3. the scanning near-field microwave microscopy that utilizes as claimed in claim 1 carries out the measuring method of piezoelectric modulus to material, it is characterized in that, when measuring vertical piezoelectric coefficient d
IjThe time, the probe of described setting scanning near-field microwave microscopy and measured material sample room apart from g between 0.1 micron to 10 microns.
4. the scanning near-field microwave microscopy that utilizes as claimed in claim 1 or 2 carries out the measuring method of piezoelectric modulus to material, it is characterized in that, when measuring horizontal piezoelectric coefficient d
Ij(during i ≠ j), its electrode layout method is to make in electrode or the upper surface at membraneous material in two sides of measured material sample to make electrode, makes the applied field direction vertical with the deformation direction of measurement.
5. as claim 1 or the 3 described scanning near-field microwave microscopies that utilize material is carried out the method that piezoelectric modulus is measured, it is characterized in that, when measuring vertical piezoelectric coefficient d
IjThe time, its electrode layout method is to make electrode in the upper and lower surface of measured material sample, makes the applied field direction consistent with the direction of the deformation of measurement, calculates piezoelectric coefficient d this moment
IjSimplified formula be
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| CN110579651A (en) * | 2019-09-05 | 2019-12-17 | 佛山市卓膜科技有限公司 | Piezoelectric coefficient measuring device |
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