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CN108362913B - Ferroelectric domain polarization direction discrimination method of laser interference type piezoelectric power microscope - Google Patents

Ferroelectric domain polarization direction discrimination method of laser interference type piezoelectric power microscope Download PDF

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CN108362913B
CN108362913B CN201810126877.3A CN201810126877A CN108362913B CN 108362913 B CN108362913 B CN 108362913B CN 201810126877 A CN201810126877 A CN 201810126877A CN 108362913 B CN108362913 B CN 108362913B
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曾慧中
葛宛兵
张佳玉
何月
张万里
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University of Electronic Science and Technology of China
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Abstract

本发明提供的一种激光干涉式压电力显微镜的铁电畴极化方向判别方法，属于材料测试技术领域。本发明通过设定探针悬臂与样品的夹角，仅需一次测量，分析一组幅度图和相位图，即可准确判别样品的铁电畴面内极化与面外极化的方向，进而得到实际的极化分布。同时，由于激光干涉式压电力显微镜的便利性，使得该方法可以在超高真空、超低温度下进行测试，拓展了铁电材料的研究范围。

Figure 201810126877

The invention provides a method for judging the polarization direction of a ferroelectric domain of a laser interference type piezoelectric force microscope, which belongs to the technical field of material testing. By setting the included angle between the probe cantilever and the sample, the present invention can accurately determine the in-plane polarization and out-plane polarization directions of the ferroelectric domain of the sample by only one measurement and analyzing a set of amplitude maps and phase maps. Get the actual polarization distribution. At the same time, due to the convenience of the laser interferometric piezoelectric force microscope, the method can be tested in ultra-high vacuum and ultra-low temperature, which expands the research scope of ferroelectric materials.

Figure 201810126877

Description

Ferroelectric domain polarization direction discrimination method of laser interference type piezoelectric power microscope
Technical Field
The invention belongs to the technical field of material testing, and particularly relates to a ferroelectric domain polarization direction discrimination method based on a laser interference type piezoelectric power microscope.
Background
The ferroelectric material has properties such as large dielectric constant, unique photoelectric effect, piezoelectric effect, pyroelectric effect and the like, is often used as a capacitance medium, an imaging unit or a storage unit, and is widely applied to electronic devices. In ferroelectric materials, the phenomenon of electric dipole moment due to misalignment of the centers of positive and negative charges in cells is called spontaneous polarization. Ferroelectric materials have two or more spontaneous polarization directions that can be reversed by external forces. In order to minimize the total free energy, the interior of the ferroelectric material is divided into several small regions, each region having the same polarization direction and being called a ferroelectric domain, and the boundary regions of different domains being called domain walls. For samples with relatively small thicknesses, such as thin films, polarization perpendicular to the upper surface of the sample (i.e., parallel to the thickness direction) is generally referred to as out-of-plane polarization, and polarization parallel to the upper surface of the sample is generally referred to as in-plane polarization. The polarization direction of the ferroelectric domain is controlled by an external electric field, which is the basic principle of the working of the ferroelectric memory; meanwhile, the enhancement of domain wall conductivity in some directions is also a hot spot in the current research on ferroelectric materials.
The ferroelectric domain is strained by an electric field in the polarization direction, and this phenomenon is called inverse piezoelectric effect. A Piezoelectric Force Microscopy (PFM) technique utilizing inverse piezoelectric effect is a method for observing the electric domain structure of ferroelectric materials, which has been developed gradually in the last two decades. Compared with the traditional observation methods such as a liquid crystal method, a chemical corrosion method, a powder precipitation method and the like, the piezoelectric force microscopy has the advantages of high resolution, small destructiveness on a sample, no requirement on a vacuum environment, capability of observing the change of the sample under an electric field, strong expansibility and the like. The piezoelectric force Microscopy is based on Scanning Probe Microscopy (SPM), utilizes a microprobe to contact with the surface of a sample to be measured, applies an alternating voltage between a needle tip and the sample, and uses a lock-in amplifier to analyze a vibration signal of the needle tip, thereby observing the inverse piezoelectric effect of a ferroelectric domain below the needle tip. With the progress of probe manufacturing and signal processing technology, the current PFM spatial resolution can reach nanometer level, and the signal-to-noise ratio can be larger than 106Magnitude.
The conventional piezoelectric force microscope detects the inverse piezoelectric deformation by adopting a Beam cantilever Beam Deflection (OBD) mode, a group of amplitude diagrams and phase diagrams of out-of-plane polarization and a group of amplitude diagrams and phase diagrams of in-plane polarization are obtained by each measurement, and ferroelectric domain distribution of a test area can be obtained by comparing and analyzing the four diagrams. The commonly adopted 3D-PFM method needs the same measuring area to carry out two times of measurement before and after rotation, and the complete ferroelectric domain direction distribution can be obtained by analyzing and comparing eight test charts. Analyzing in principle, the light beam cantilever beam deflection structure is limited by the arrangement of a light path, only the deflection angle of the cantilever can be actually measured, and the magnitude of the inverse piezoelectric deformation of a sample cannot be quantitatively measured; meanwhile, the optical path structure is complex, high integration is difficult to achieve, the temperature drift is easy to influence, and measurement in a low-temperature environment is difficult to achieve. These disadvantages limit the wider application of beam cantilever deflected piezoelectric force microscopes.
The novel piezoelectric force microscope adopts a laser interference method (OFI), a beam of laser is vertically irradiated on a probe cantilever, then a reflected beam returns along an original light path and interferes with an incident beam to form interference fringes with light and shade at intervals. The space between the cantilever and the laser is changed by the vibration of the needle tip along with the sample, and the photoelectric detector at the fixed position can detect the change of the interference optical signal and output corresponding voltage, namely an inverse piezoelectric effect signal. Compared with a beam cantilever beam deflection type piezoelectric force microscope, the laser interference type piezoelectric force microscope can quantitatively measure the piezoelectric deformation of a sample, needs a short optical path, can miniaturize a measuring main body, and can work under high vacuum and ultralow temperature.
However, the laser interference piezoelectric microscope is generally considered to be limited by its working principle, and is only sensitive to the inverse piezoelectric deformation parallel to the optical path propagation direction of the laser, i.e. perpendicular to the upper surface of the sample, so that only the out-of-plane piezoelectric signal can be detected. For common samples with multiple polarization directions, such as bismuth ferrite (BiFeO)3) And bismuth titanate (BiTiO)3) And the laser interference piezoelectric power microscope cannot be used for acquiring in-plane piezoelectric signals parallel to the upper surface of the sample. These one-sided insights have limited the large-scale application of laser interference piezoelectric microscopes.
Disclosure of Invention
The invention aims to provide a method for judging the polarization direction of a ferroelectric domain of a laser interference type piezoelectric power microscope.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a method for judging the polarization direction of a ferroelectric domain of a laser interference type piezoelectric power microscope specifically comprises the following steps:
step 1, establishing a space rectangular coordinate system, wherein an axis a and an axis b are parallel to the upper surface of a habitual primitive cell of a sample to be detected, and an axis c is perpendicular to the upper surface of the habitual primitive cell; then decomposing the polarization direction existing in the sample to be tested into an established space rectangular coordinate system, wherein the polarization along the c axis is called out-of-plane polarization, and the polarization along the a axis and the b axis is called in-plane polarization;
step 2, placing a sample to be detected on a sample table, and adjusting the included angle between the a axis and the probe cantilever in the spatial rectangular coordinate system in the step 1
Figure BDA0001573752140000031
Making the angle of the probe tip less than 45 degrees, and then inserting the probe until the probe tip contacts with the surface of a sample to be detected;
step 3, applying alternating voltage between the probe tip and a sample to be detected, and then scanning the sample to be detected once to obtain an amplitude diagram and a phase diagram;
in the phase diagram obtained in the step 4 and the step 3, areas with phase difference of 180 degrees respectively have out-of-plane polarization along the positive direction or the negative direction of the c axis; for the areas with the same phase value, according to the amplitude diagram obtained in the step 3, obtaining the area with the strongest signal and the area with the same phase value, wherein the area with the strongest signal has the in-plane polarization along the positive direction of the a axis, the area with the second strongest signal has the in-plane polarization along the positive direction of the b axis, the area with the second weakest signal has the in-plane polarization along the negative direction of the b axis, and the area with the weakest signal has the in-plane polarization along the negative direction of the a;
and 5, reducing and combining the polarization intensities decomposed to the axis a, the axis b and the axis c obtained in the step 4 according to the inverse operation of the decomposition in the step 1, so as to obtain the complete ferroelectric domain polarization direction distribution of the test area of the sample to be tested.
Preferably, the angle between the a axis and the cantilever of the probe in step 2
Figure BDA0001573752140000032
At this time
Figure BDA0001573752140000033
Figure BDA0001573752140000034
Is an arithmetic progression.
Further, step 3 is performed on the probe tip and the probe to be testedFixed frequency f of alternating voltage applied between samples0And a fixed amplitude VacAnd setting according to the type of the probe, the measurement environment temperature and the components and the appearance of the sample to be measured.
The invention has the beneficial effects that:
in the method for judging the polarization direction of the ferroelectric domain of the laser interference type piezoelectric microscope, the included angle between a probe cantilever and a sample is set, and only one-time measurement is needed to analyze a group of amplitude diagrams and phase diagrams, so that the directions of the in-plane polarization and the out-of-plane polarization of the ferroelectric domain of the sample can be accurately judged, and further the actual polarization distribution is obtained. Meanwhile, due to the convenience of the laser interference type piezoelectric power microscope, the method can be used for testing under ultrahigh vacuum and ultralow temperature, and the research range of the ferroelectric material is expanded.
Drawings
FIG. 1 is a schematic diagram of a system structure of a method for determining a polarization direction of a ferroelectric domain of a laser interference type piezoelectric microscope according to the present invention; the device comprises a scanning tube 1, a sample table 2, a sample to be detected 3, a probe tip 4, a probe cantilever 5, a piezoelectric plate 6, an optical fiber 7, a laser generator and a detector 8, a phase-locked amplifier 9, a computer 10 and a function generator 11, wherein the scanning tube 1 is a scanning tube; in the figure, a single-direction arrow represents a voltage signal transmission direction, and a double-direction arrow represents an incidence and reflection direction of laser;
FIG. 2 shows BiFeO used in the embodiment of the present invention3A graph of the measured piezoelectric response amplitude of a film sample; wherein, U1、U2、U3And U4Respectively representing the areas corresponding to four voltage values from the strongest to the weakest;
FIG. 3 is a phase diagram of the piezoelectric response corresponding to FIG. 2;
fig. 4 is a graph of voltage signal amplitude values at the dashed line locations in fig. 2.
Detailed Description
The technical scheme of the invention is detailed below by combining the accompanying drawings and the embodiment.
As shown in fig. 1, it is a schematic diagram of a system structure of the method for determining the polarization direction of a ferroelectric domain of a laser interference type piezoelectric microscope according to the present invention; 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.
The invention provides a method for judging the polarization direction of a ferroelectric domain of a laser interference type piezoelectric power microscope, which comprises the following steps:
step 1, analyzing the relative displacement of positive and negative charge centers in a conventional cell for a sample to be tested with known crystal orientation to obtain all possible polarization directions. However, the crystal lattice can be divided into seven crystal systems such as triclinic, orthogonal, triangular and hexagonal crystal systems according to different symmetries, the corresponding conventional cells have different shapes, and the orientations of the polarization directions in the conventional cells are different, which increases the analysis difficulty. In order to simplify analysis, a set of space rectangular coordinate system is established, wherein the axis a and the axis b are parallel to the upper surface of the habitual primitive cell of the sample to be detected, and the axis c is perpendicular to the upper surface of the habitual primitive cell; and then decomposing all possible polarization directions in the sample to be detected into an established space rectangular coordinate system, wherein the polarization along the c axis is called out-of-plane polarization, and the polarization along the a axis and the b axis is called in-plane polarization. Through the operation, the original polarization directions with different symmetries are decomposed into a relatively simple rectangular coordinate system, and then the sample is tested and analyzed.
Step 2, placing a sample to be detected on a sample table, and adjusting the included angle between the axis a and the probe cantilever 5 in the spatial rectangular coordinate system in the step 1
Figure BDA0001573752140000041
The needle is inserted until the point of the probe is contacted with the surface of the sample to be measured after the angle is less than 45 degrees.
Step 3, applying fixed frequency f between the probe tip and the sample to be detected0And a fixed amplitude VacThe alternating voltage of the laser interference type piezoelectric microscope obtains a clear inverse piezoelectric effect image; wherein, the frequency f0Sum amplitude VacThe selection needs to consider the influence of factors such as the type of the probe, the measurement environment temperature, the components and the morphology of the sample to be measured and the like.
Step 4, carrying out the detection on the sample to be detectedAnd scanning once to obtain an amplitude diagram and a phase diagram, namely an inverse piezoelectric effect image. During scanning, strain induced strain of out-of-plane polarization in either the positive or negative direction of the c-axis produces opposing piezoelectric signals 180 ° out of phase. The strain polarized in the plane along the axis a or the axis b drives the needle point to move, so that the probe cantilever deforms, and the deformation comprises twisting in the front-back direction parallel to the probe cantilever and twisting in the left-right direction perpendicular to the probe cantilever; wherein the forward twist reduces the separation of the laser from the probe cantilever, the backward twist increases the separation, and the left-right twist has no effect on the separation. Because the laser interference principle is very sensitive to the change of the spacing, the influence of the deformation on the spacing can cause signals with different contrasts to be generated in an amplitude diagram, and the method is specifically divided into four types: polarization in the positive a-axis and the positive b-axis directions produces enhanced signals due to
Figure BDA0001573752140000051
Therefore, the signal along the positive direction of the axis a is strongest, and the signal along the positive direction of the axis b is strongest; similarly, the signal along the negative a-axis direction is weakest, and the signal along the negative b-axis direction is second weakest.
And 5, analyzing the measured inverse piezoelectric effect image: firstly, analyzing a phase diagram, wherein in the phase diagram obtained in the step 4, areas with phase difference of 180 degrees respectively have out-of-plane polarization along the positive direction or the negative direction of the c axis; for the areas with the same phase value, the amplitude diagram needs to be analyzed, and according to the amplitude diagram obtained in the step 4, the area with the strongest signal has the in-plane polarization along the positive direction of the a axis, the area with the second strongest signal has the in-plane polarization along the positive direction of the b axis, the area with the second weakest signal has the in-plane polarization along the negative direction of the b axis, and the area with the weakest signal has the in-plane polarization along the negative direction of the a axis;
and 6, reducing and combining the polarization intensities decomposed to the axis a, the axis b and the axis c obtained in the step 5 according to the inverse operation of the decomposition operation in the step 1, and thus obtaining the complete ferroelectric domain polarization direction distribution of the test area of the sample to be tested.
Preferably, the angle between the a axis and the cantilever of the probe in step 2
Figure BDA0001573752140000052
At this time
Figure BDA0001573752140000053
Figure BDA0001573752140000054
Is an arithmetic progression.
Examples
In the laser interference type piezoelectric power microscope adopted in the embodiment, the wavelength of a laser source is 1330 nm; the conductive probe used was NSC18/Pt type probe manufactured by Mikromasch, the cantilever length of the probe was about 200 μm, the tip length was about 15 μm, the elastic coefficient was 2.8N/m, and the resonance frequency was 75 kHz. To measure the ferroelectric material bismuth ferrite (BiFeO)3) Taking the polarization direction of ferroelectric domain of a thin film (thickness 100nm, crystal orientation 100) as an example, according to the test system shown in fig. 1, the specific test steps are as follows:
step 1, BiFeO3The conventional primitive cell of (1) is a cube, the edge of which<111>The axis has 8 possible polarization directions, and has strong symmetry. When a rectangular coordinate system is established, the positive directions of the a axis, the b axis and the c axis are respectively along BiFeO3Idiocytic [100 ] -]、[010]And [001 ]]The direction is the same; then 8 possible polarization directions are decomposed into an established rectangular coordinate system, wherein 4 polarization directions have components along the positive direction of the c axis, 4 polarization directions have components along the negative direction of the c axis, and in-plane polarization components along the positive direction of the a axis, the positive direction of the b axis, the negative direction of the a axis and the negative direction of the b axis;
step 2, placing a sample to be detected on a sample table, and adjusting the included angle between the sample a axis and the probe cantilever
Figure BDA0001573752140000063
Setting the working point of the z loop of the instrument to be 1.52V, and then inserting the probe until the probe tip is contacted with the surface of the sample to be detected. The wavelength of incident infrared light of the test instrument is 1330nm, the voltage change corresponding to the interference signal is about 1.48V, and the sensitivity of the detection signal is about 200 nm/V;
step 3, applying f between the probe tip and the sample to be detected0365kHz, amplitude Vac2V ac voltage;
step 4, scanning the sample to be detected once, wherein the scanning range is 4 x 4 mu m2The scanning pixel array is 256 × 256, the size of each pixel point is 15.62nm, the staying time of each pixel point is 3ms, and an amplitude diagram and a phase diagram are obtained, namely, an inverse piezoelectric effect image is obtained;
step 5, analyzing the measured inverse piezoelectric effect image by adopting Gwyddion software: first, the phase diagram is analyzed, as shown in fig. 3, in which the different out-of-plane polarization directions can be clearly distinguished. Then, adjusting the color scale of the amplitude diagram, and seeing that the image is divided into four color contrasts, wherein the brighter the color, the larger the corresponding voltage value is; the brightest region (voltage value U)1About 2.5mV) has a positive direction along the a-axis of [100 ]]Directional in-plane polarization, sub-bright region (voltage value U)2About 2.1mV) has a positive direction along the b-axis of [010]Directional in-plane polarization, sub-dark region (voltage value U)3About 1.1mV) has a negative direction along the b-axis, i.e.
Figure BDA0001573752140000062
Directional in-plane polarization, darkest region (voltage value U)4About 0.6mV) has a negative direction along the a-axis, i.e.
Figure BDA0001573752140000061
Directional in-plane polarization. At the same time, U1+U4≈U2+U3The previous analysis can be verified.
And 6, combining the polarization direction obtained in the step 5 with the <111> direction of the conventional primitive cell of the sample to be tested, and obtaining the complete ferroelectric domain polarization direction distribution of the test area. Withdrawing the needle, taking out the sample and finishing the measurement.
The present invention is not limited to the above-described embodiments. The foregoing description of the specific embodiments is intended to describe and illustrate the technical solutions of the present invention, and the above specific embodiments are merely illustrative and not restrictive. Those skilled in the art can make many specific changes in form and detail without departing from the spirit and scope of the invention as defined in the appended claims.

Claims (2)

1.一种激光干涉式压电力显微镜的铁电畴极化方向判别方法，包括以下步骤：1. A method for judging the polarization direction of a ferroelectric domain of a laser interferometric piezoelectric force microscope, comprising the following steps: 步骤1、建立空间直角坐标系，其中，a轴和b轴平行于待测样品惯用原胞的上表面，c轴垂直于惯用原胞的上表面；然后将待测样品中存在的极化方向分解到建立的空间直角坐标系中，沿c轴的极化称为面外极化，沿a轴和b轴的极化称为面内极化；Step 1. Establish a spatial Cartesian coordinate system, in which the a-axis and b-axis are parallel to the upper surface of the conventional primary cell of the sample to be tested, and the c-axis is perpendicular to the upper surface of the conventional primary cell; then the polarization direction existing in the sample to be tested is determined. Decomposed into the established space rectangular coordinate system, the polarization along the c-axis is called out-of-plane polarization, and the polarization along the a-axis and b-axis is called in-plane polarization; 步骤2、将待测样品放置于样品台上，调整步骤1空间直角坐标系中的a轴与探针悬臂的夹角φ，使其小于45°，然后进针至探针针尖与待测样品表面接触；Step 2. Place the sample to be tested on the sample stage, adjust the angle φ between the a-axis in the spatial Cartesian coordinate system and the probe cantilever in step 1, so that it is less than 45°, and then insert the needle to the probe tip and the sample to be tested. surface contact; 步骤3、在探针针尖与待测样品之间施加固定频率f0和固定幅值Vac的交流电压，使激光干涉式压电力显微镜得到清晰的逆压电效应图像，其中，频率f0和幅值Vac根据探针型号、测量环境温度、待测样品的成分与形貌进行选取；然后对待测样品进行一次扫描，得到一张幅度图和一张相位图；Step 3. Apply an alternating voltage with a fixed frequency f 0 and a fixed amplitude V ac between the probe tip and the sample to be tested, so that the laser interferometric piezoelectric force microscope can obtain a clear inverse piezoelectric effect image, wherein the frequency f 0 and The amplitude V ac is selected according to the probe model, the measurement environment temperature, and the composition and morphology of the sample to be tested; then the sample to be tested is scanned once to obtain an amplitude map and a phase map; 步骤4、步骤3得到的相位图中，相位相差180°的区域分别具有沿c轴正方向或负方向的面外极化；而对于相位值相同的区域，根据步骤3得到的幅度图，得到具有最强信号的区域具有沿a轴正方向的面内极化，次强信号区域具有沿b轴正方向的面内极化，次弱信号区域具有沿b轴负方向的面内极化，最弱信号区域具有沿a轴负方向的面内极化；In the phase diagrams obtained in step 4 and step 3, the regions with a phase difference of 180° have out-of-plane polarization along the positive or negative direction of the c-axis respectively; and for regions with the same phase value, according to the amplitude diagram obtained in step 3, we can obtain The region with the strongest signal has an in-plane polarization along the positive a-axis, the second-strongest signal region has an in-plane polarization along the positive b-axis, and the second-weakest signal region has an in-plane polarization along the negative b-axis, The weakest signal region has in-plane polarization along the negative a-axis; 步骤5、将步骤4得到的分解到a轴、b轴和c轴上的极化强度按步骤1中分解的逆操作进行还原与合并，即可得到待测样品测试区域的铁电畴极化方向分布。Step 5. Reduce and combine the polarizations obtained in step 4 on the a-axis, b-axis and c-axis according to the inverse operation of the decomposition in step 1, and then the ferroelectric domain polarization of the test area of the sample to be tested can be obtained. directional distribution. 2.根据权利要求1所述的激光干涉式压电力显微镜的铁电畴极化方向判别方法，其特征在于，步骤2中a轴与探针悬臂的夹角φ=26.6°。2 . The method for judging the ferroelectric domain polarization direction of a laser interferometric piezoelectric force microscope according to claim 1 , wherein the angle φ=26.6° between the a-axis and the probe cantilever in step 2. 3 .
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