CN114674875A - Method for measuring longitudinal effective piezoelectric coefficient of piezoelectric film - Google Patents

Method for measuring longitudinal effective piezoelectric coefficient of piezoelectric film Download PDF

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CN114674875A
CN114674875A CN202210244668.5A CN202210244668A CN114674875A CN 114674875 A CN114674875 A CN 114674875A CN 202210244668 A CN202210244668 A CN 202210244668A CN 114674875 A CN114674875 A CN 114674875A
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彭斌
孟奔阳
曾慧中
王韬
张万里
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University of Electronic Science and Technology of China
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Abstract

The invention belongs to the technical field of material testing, and particularly relates to a method for measuring a longitudinal effective piezoelectric coefficient of a piezoelectric film. The invention is based on the piezoelectric response obtained by fiber laser interference type PFM measurement under different voltage excitations, uses a simple harmonic vibration model to describe the probe-sample vibration behavior so as to reduce the interference and frequency dependence of thermal noise, uses the simple harmonic vibration model to fit the piezoelectric response for multiple times, extracts the effective piezoelectric deformation of the measured film under different excitations, calculates and obtains the longitudinal effective piezoelectric coefficient of the film by combining the effective piezoelectric deformation under different excitations, eliminates the interference of the piezoelectric response signal frequency dependence and background noise of the PFM, and improves the signal-to-noise ratio. Compared with the traditional piezoelectric coefficient measuring method, the method can realize accurate local measurement and draw a piezoelectric coefficient map, and has stable result and no frequency dependence.

Description

Method for measuring longitudinal effective piezoelectric coefficient of piezoelectric film
Technical Field
The invention belongs to the technical field of material testing, and particularly relates to a longitudinal effective piezoelectric coefficient (d) of a piezoelectric filmzz) The method of measuring (1).
Background
The piezoelectric coefficient testing method is generally based on the inverse piezoelectric effect, when an electric field is applied to the polarization direction of a piezoelectric material, the material can deform, and the effective piezoelectric coefficient can be obtained by measuring the ratio of the deformation to the applied voltage. Among the parameters for measuring the piezoelectric characteristics, the longitudinal piezoelectric coefficient d 33And transverse piezoelectric coefficient d31It is important. The piezoelectric coefficients measured are all effective values due to the substrate clamping effect of the film-substrate structure.
In recent years, many advances have been made in the measurement of the piezoelectric coefficient of a thin film material, such as a vertical pressure loading method based on a direct piezoelectric effect, a capacitance method, a PFM method, and an X-ray diffraction method, and also a bulk acoustic wave and surface acoustic wave method using indirect measurement, a complex resonance method, and the like. The more common vertical pressure loading method is a standard method for measuring piezoelectric coefficients, but is only suitable for bulk and bulk materials and cannot be used for thin-film piezoelectric materials. The principle of the capacitance method is to measure the change in capacitance when piezoelectric is deformed. The capacitive method is not suitable for certain piezoelectric thin film materials due to the influence of capacitance measurement accuracy and thin film/electrode interface capacitance.
The PFM method is a Microscope developed on the basis of an Atomic Force Microscope (AFM), which detects effective piezoelectric vibration of a sample under an applied excitation voltage by using a conductive probe, and is widely applied to an effective piezoelectric coefficient test in recent years. Most current commercial AFMs use beam deflection to measure cantilever deflection, i.e., piezoelectric response, using a four quadrant photoelectric position sensor to detect the position of the reflected spot. However, the beam deflection method is essentially converted into the displacement of the cantilever by measuring the deflection angle of the cantilever, and is only an indirect measurement of the displacement of the cantilever. Secondly, due to process variations in the conductive probes used, a rigorous calibration procedure is required for quantitative measurements. The other detection method is an optical fiber laser interferometry, which can realize the direct measurement of the piezoelectric response of the sample surface by utilizing the linear approximation between the interference intensity of the optical fiber laser and the cantilever displacement, and does not need to be calibrated before use. Compared with a light beam deflection method, the piezoelectric response obtained by using the optical fiber laser interferometry has higher accuracy and repeatability.
To measure the PFM piezoelectric response signal, the conductive probe is usually biased with an ac voltage at a fixed frequency, and the PFM piezoelectric response signal is extracted by a lock-in amplifier. However, the PFM piezoelectric response signal obtained in the method is very weak and almost equivalent to the thermal noise of a probe, and the frequency dependence of the piezoelectric response is measured, and the method measures dzz distribution of the longitudinal effective piezoelectric coefficient of the periodically polarized lithium niobate in the range of 10-100 pm/V. However, the effective piezoelectric deformation obtained by fitting in single measurement is directly used for representing the longitudinal effective piezoelectric coefficient dzz, so that the influence of background noise cannot be avoided, and the error range of dzz obtained by single measurement calculation is large, so that the method is difficult to be applied practically.
Disclosure of Invention
Aiming at the problems or the defects, and aiming at realizing the problems of frequency dependence and thermal noise in the accurate local measurement of the longitudinal effective piezoelectric coefficient dzz of the piezoelectric film and PFM measurement, the invention provides a longitudinal effective piezoelectric coefficient d of the piezoelectric filmzzThe method of measuring (1). Based on piezoelectric response obtained by fiber laser interference type PFM measurement under different voltage excitations, effective piezoelectric deformation of a measured film under different excitations is extracted by fitting the piezoelectric response for multiple times by using a simple harmonic vibration model, and the effective piezoelectric deformation under different excitations is combined to calculate to obtain a longitudinal effective piezoelectric coefficient d of the film zz。
A method for measuring the longitudinal effective piezoelectric coefficient of a piezoelectric film comprises the following specific steps:
step 1, fixing a film to be detected on a sample table positioned above a scanning tube, and calculating a sensitivity factor according to the working principle of a fiber laser instrument and laser wavelength lambda
Figure BDA0003544652030000021
Step 2, enabling the conductive probe to reach the position with a distance of 10-100um from the surface of the film to be detected, and enabling V to be arrangedAC1V, sweeping the free resonant frequency of the probe + -10 kHz, and measuring the free resonant frequency f of the probe0。
Step 3, scanning an F-D curve, and measuring the surface adhesion force F of the film to be measuredadTo make the piezoelectric force displayThe micromirror operates in a contact mode. Further, the step is carried out by maintaining the contact force F between the needle point and the film to be measuredN＝5FadConstant to reduce the effect of surface adsorption force on the measurement.
Step 4, enabling the alternating voltage V applied to the probeAC1V, sweep frequency in 0-2MHz under contact mode, and determine first-order resonance peak position
Figure BDA0003544652030000022
Step 5, applying an alternating current power supply V between the probe and the film to be detectedACInitial value V00.1-0.3V, with V0Linearly increasing to 10V for a fixed step size0At each VACFor first order formant
Figure BDA0003544652030000023
A frequency sweep is performed and the amplitude V signal is detected using a lock-in amplifier to calculate the cantilever amplitude a ═ s × V. The scanning tube remains stationary during the measurement.
Step 6, using simple harmonic vibration model to the different V obtained in the step 5ACSubstituting amplitude A of the cantilever under excitation into a simple harmonic vibration model
Figure BDA0003544652030000024
Carrying out nonlinear fitting to calculate the effective piezoelectric deformation A0Obtaining a relation curve VAC-A0。
Step 7, comparing the relation curve V obtained in the step 6AC-A0Performing first-order linear fitting, and calculating the slope to obtain the effective longitudinal piezoelectric coefficient dzzAnd finishing the measurement.
The invention provides a piezoelectric film with a longitudinal effective piezoelectric coefficient dzzIn the measuring method, based on the piezoelectric response obtained by measuring the fiber laser interference type PFM under different voltage excitations, a simple harmonic vibration model is used for describing the vibration behavior of the probe-sample, namely, the elastic modulus and the effective piezoelectric deformation of the sample are extracted from the resonance frequency spectrum data of the probe-sample so as to reduce the interference of thermal noise and the frequency dependence, and the simple harmonic vibration model is used for carrying out multiple times on the piezoelectric responseFitting, extracting effective piezoelectric deformation of the measured film under different excitations, and calculating by combining the effective piezoelectric deformation under different excitations to obtain a longitudinal effective piezoelectric coefficient d of the filmzz. Compared with the traditional piezoelectric coefficient measuring method, the method can realize accurate local measurement and draw a piezoelectric coefficient map due to the extremely high transverse resolution (10-20 nm) and sensitivity (0.1 pm/V) of the PFM. Compared with periodically polarized lithium niobate dzz which is measured at a fixed frequency based on PFM and is 10-100pm/V, dzz of the periodically polarized lithium niobate is measured to be 13 +/-1 pm/V by using the method of the invention, and the result is stable and has no frequency dependence.
In conclusion, the invention can accurately and locally measure the longitudinal effective piezoelectric coefficient dzz of the piezoelectric film, eliminates the frequency dependence of the piezoelectric response signal of the PFM and the interference of background noise, improves the signal-to-noise ratio, and has stable result and no frequency dependence.
Drawings
FIG. 1 is a schematic diagram of a system structure of a fiber laser interference type piezoelectric microscope according to the present invention;
FIG. 2 is a graph showing the relationship between the first-order amplitude A of the cantilever and the frequency of the AC bias when the AC bias is applied;
FIG. 3 is a curve fitted by sweep data and a simple harmonic vibration model under different AC biases in example 1;
FIG. 4 shows the final effective piezoelectric deformation A of the film to be measured in example 10With an applied AC bias voltage VACAnd (5) a relational graph.
FIG. 5 is a plot of sweep data versus simple harmonic vibration model fitting for lithium niobate samples under different AC biases for example 2;
FIG. 6 is a schematic diagram of the effective piezoelectric deformation A of lithium niobate calculated by simple harmonic vibration model fitting0With an applied AC bias voltage VACAnd (4) relationship.
Reference numerals: 1-scanning tube, 2-sample stage, 3-film to be measured, 4-probe tip, 5-probe cantilever, 6-piezoelectric plate, 7-optical fiber, 8-optical fiber laser generator and detector, 9-phase-locked amplifier, 10-computer and 11-function generator.
Detailed Description
The present invention will be described in further detail with reference to the drawings and examples.
Fig. 1 is a schematic structural diagram of a system for measuring a longitudinal effective piezoelectric coefficient of a piezoelectric film of the fiber laser interference type piezoelectric microscope used in this embodiment. The length of the actual probe is in the order of micrometers to millimeters, and the probe is enlarged in order to explain the relationship between the probe and the sample to be measured. In this embodiment, the conductive probe is CDT-FMR produced by Nanosensors, with elastic coefficient kc＝18N/m。
This example is to measure the effective piezoelectric coefficient d of the aluminum nitride film in the longitudinal directionzzFor example, the test system shown in fig. 1 is connected to an instrument, wherein the single-direction arrows represent voltage signal transmission directions, and the double-direction arrows represent incidence and reflection directions of the fiber laser. The measurement is performed by the flowchart shown in FIG. 2, and FIG. 2 shows the relationship between the first order amplitude A of the cantilever and the frequency of the AC bias voltage when the AC bias voltage is applied, along the arrow direction VACAnd gradually increases. The specific measurement steps are as follows: step 1, fixing the AlN thin film to be detected on a sample table positioned above the scanning tube, and realizing electrical connection by using silver paste. The sensitivity factor s is 55.64pm/V calculated according to the working principle of the fiber laser instrument and the laser wavelength lambda is 1330 nm.
Step 2, enabling the piezoelectric force microscope probe to reach the position of 20 microns on the surface of the AlN thin film sample, and enabling V to be arrangedDC＝0V，VACThe free resonant frequency f of the probe is measured by sweeping the frequency within 90 kHz-130 kHz which is the free resonant frequency of the probe at 1V0＝110kHz。
Step 3, scanning an F-D curve, and measuring the surface adhesion force F of the AlN thin filmad30 nN. The piezoelectric force microscope is operated in a contact mode, and the contact force F of the needle tip and the AlN film is maintainedN150nN constant.
Step 4, enabling the alternating voltage V applied to the probeACScanning in contact mode at 0-2MHz to determine the first-order resonance peak position, and measuring
Figure BDA0003544652030000041
Step 5, making the alternating voltage V applied between the probe and the AlN thin filmACInitial value V0Step length is fixed at 0.2VLinear increase, i.e. 0.2V, 0.4V, 0.6V, … 1.8.8V, 2V, at each VACFor first order formant
Figure BDA0003544652030000042
The frequency is swept between 550kHz and 610kHz, a frequency doubling amplitude V signal is detected by using a phase lock amplifier, and a frequency doubling amplitude A-s-V signal is calculated. The scanning tube remains stationary during the measurement.
Step 6, using simple harmonic vibration model to process different V received by the computerACSubstitution of a frequency multiplication amplitude A of the cantilever under excitation
Figure BDA0003544652030000043
Carrying out nonlinear fitting and recording the effective piezoelectric deformation A of the AlN film0＝0.23pm、0.46pm、0.72pm、…2.10pm、2.24pm。
Step 7, the relation curve V is matchedAC-A0Linear fitting was performed, and the slope was calculated to be 1.2, so d was measured zz＝1.2pm/V。
FIG. 3 is a graph of the frequency sweep data under different AC biases according to the present embodiment fitting to a simple harmonic vibration model. FIG. 4 is a diagram illustrating effective piezoelectric deformation A of the thin film to be measured according to the simple harmonic vibration model fitting calculation in this embodiment0With an applied AC bias voltage VACAnd (4) relationship.
Example 2
In this example, the conductive probe used was NSC18/Pt manufactured by Mikromasch, elastic modulus kc2.8N/m. To measure the lithium niobate thin film dzzFor example, according to the test system connection instrument shown in fig. 1, the measurement is performed through the flowchart shown in fig. 2, and the specific measurement steps are as follows:
step 1, fixing the LNO film to be detected on a sample table above the scanning tube, and realizing electrical connection by using silver paste. The sensitivity factor s is 55.64pm/V calculated according to the working principle of the fiber laser instrument and the laser wavelength lambda is 1330 nm.
Step 2, enabling the probe of the piezoelectric force microscope to reach the position with a distance of 20um from the surface of the sample, and enabling V to be arrangedDC＝0V，VACThe frequency is swept within 50 kHz-90 kHz as the free resonance frequency of the probe, and the probe is measuredFree resonance frequency f0＝67kHz。
Step 3, scanning an F-D curve, and measuring the surface adhesion F of the LNO filmad100 nN. The piezoelectric force microscope is enabled to work in a contact mode, and the contact force F of the needle point-LNO film is keptN300nN constant.
Step 4, enabling the alternating voltage V applied to the probe ACScanning in contact mode at 0-2MHz to determine the first-order resonance peak position, and measuring
Figure BDA0003544652030000051
Step 5, enabling an alternating voltage V applied between the probe and the LNO filmACInitial value V00.2V and linearly increased in fixed steps of 0.2V, i.e. 0.2V, 0.4V, 0.6V, … 1.8.8V, 2V, at each VACFor first order formant
Figure BDA0003544652030000052
I.e., 355kHz to 415kHz, and the amplitude V signal is detected by a lock-in amplifier, and the cantilever amplitude a is calculated as s V. The scanning tube remains stationary during the measurement.
Step 6, using simple harmonic vibration model to process different V received by the computerACSubstitution of cantilever amplitude A under excitation
Figure BDA0003544652030000053
Carrying out nonlinear fitting and recording the effective piezoelectric deformation A of the LNO film0＝3.7pm、7.3pm、10.5pm、…22.5pm、26.3pm。
Step 7, the relation curve V is matchedAC-A0A linear fit was performed, and the slope was calculated to be 13.1, so d was measuredzz＝13.1pm/V。
Compared with the periodically polarized lithium niobate dzz measured at a fixed frequency based on PFM, which is 10-100pm/V, dzz measured in this example is 13 + -1 pm/V, and the result is stable and has no frequency dependence.
As can be seen from the above examples, the present invention enables accurate local measurement of the effective piezoelectric coefficient dzz in the longitudinal direction of the piezoelectric thin film, with stable results and no frequency dependence. The invention provides a piezoelectric film with a longitudinal effective piezoelectric coefficient dzzIn the measuring method, based on the piezoelectric response obtained by fiber laser interference type PFM measurement under different voltage excitations, the simple harmonic vibration model is utilized to fit the piezoelectric response for multiple times, the effective piezoelectric deformation of the measured film under different excitations is extracted, and the effective piezoelectric deformation under different excitations is combined to calculate to obtain the longitudinal effective piezoelectric coefficient d of the film zz. Compared with the traditional piezoelectric coefficient measuring method, the method can realize accurate local measurement and draw a piezoelectric coefficient map due to the extremely high transverse resolution (10-20 nm) and sensitivity (0.1 pm/V) of the PFM.

Claims (3)

1. A method for measuring the longitudinal effective piezoelectric coefficient of a piezoelectric film is characterized by comprising the following specific steps:
step 1, fixing a film to be detected on a sample table above a scanning tube, and calculating a sensitivity factor according to the working principle of a fiber laser instrument and the laser wavelength lambda
Figure FDA0003544652020000011
Step 2, enabling the conductive probe to be 10-100um away from the surface of the film to be detected, and enabling V to beACSweep at probe free resonance frequency + -10 kHz, measuring free resonance frequency f of probe0；
Step 3, scanning an F-D curve, and measuring the surface adhesion force F of the film to be measuredadOperating the piezoelectric force microscope in a contact mode;
step 4, enabling the alternating voltage V applied to the probeAC1V, sweep frequency in 0-2MHz under contact mode, and determine first-order resonance peak position
Figure FDA0003544652020000012
Step 5, applying an alternating current power supply V between the probe and the film to be detectedACInitial value V00.1-0.3V, with V0Linearly increasing to 10V for a fixed step size0At each VACFor first order formant
Figure FDA0003544652020000013
Carrying out frequency sweeping, and detecting an amplitude V signal by using a lock-in amplifier, thereby calculating the cantilever amplitude A ═ s × V; the scanning tube is kept static in the measuring process;
Step 6, using a simple harmonic vibration model to the different V obtained in the step 5ACSubstituting amplitude A of the cantilever under excitation into a simple harmonic vibration model
Figure FDA0003544652020000014
Carrying out nonlinear fitting to calculate the effective piezoelectric deformation A0Obtaining a relation curve VAC-A0；
Step 7, comparing the relation curve V obtained in the step 6AC-A0Performing first-order linear fitting, and calculating the slope to obtain the longitudinal effective piezoelectric coefficient dzzAnd finishing the measurement.
2. The method for measuring a longitudinal effective piezoelectric coefficient of a piezoelectric thin film according to claim 1, wherein: keeping the contact force F of the needle point and the film to be measured in the step 3N＝5FadIs constant.
3. The method for measuring the effective piezoelectric coefficient in the longitudinal direction of the piezoelectric thin film according to claim 1, wherein: the film to be detected is an aluminum nitride film or a lithium niobate film.
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