A high-throughput thin film piezoelectric performance comprehensive characterization device and method

Abstract

The present invention provides a high-throughput thin film piezoelectric performance comprehensive characterization device and method, the device includes: a synchrotron radiation light source beam emitter, a light receiver, a sample stage, a power supply and an electrode selector, and a heating and temperature measuring device. The present invention realizes high-throughput characterization of thin film piezoelectric performance by moving and positioning the piezoelectric film on the same substrate; at the same time, the uniqueness of the X-ray spectrum collected under the irradiation of the synchrotron radiation light source for a specific material is utilized to avoid the interference of the substrate; in addition, the ultra-high resolution of the lattice constant of the object by the synchrotron radiation light source is utilized to effectively improve the measurement accuracy of the piezoelectric coefficient; finally, in conjunction with the in-situ heating and temperature measuring device, after measuring the piezoelectric coefficient, the Curie temperature of the same piezoelectric film area can be measured in real time in the same experiment, thereby improving the efficiency of comprehensive characterization of the piezoelectric performance of the piezoelectric film.

Description

Technical Field

[0001] The present invention belongs to the technical field of thin film piezoelectric performance characterization, and in particular relates to a high-throughput thin film piezoelectric performance comprehensive characterization device and method. Background Art

[0002] In recent years, various MEMS devices that utilize the electromechanical conversion and coupling effects of piezoelectric films, such as microphones, ultrasonic transducers, resonators, filters, etc., have been widely used. The piezoelectric coefficient and Curie temperature are two important parameters of piezoelectric materials. Improving the piezoelectric coefficient helps to improve the electromechanical coupling coefficient, sensitivity and driving ability of the device, while the Curie temperature determines the maximum operating temperature of the piezoelectric film. When it is higher than the Curie temperature, the piezoelectric film will lose its piezoelectricity and the device will fail. The operating environment of piezoelectric devices is complex, especially in harsh environments such as high power and high temperature. Therefore, the development of piezoelectric films with high piezoelectric coefficients and high Curie temperatures has become a research focus.

[0003] High-throughput experiments are an experimental method to accelerate material research and development. For thin film research and development, it is usually based on a substrate. Through reasonable design, dozens or hundreds of material sample libraries with certain changes in composition, structure and / or thickness parameters are formed, and the material parameters are characterized by high-throughput characterization methods to screen out suitable materials. In view of the wide variety and complex composition of piezoelectric materials, it is suitable to use high-throughput characterization methods to achieve rapid screening of piezoelectric thin film materials.

[0004] At present, the characterization methods for the piezoelectric properties of thin films are mainly based on the direct piezoelectric effect and the inverse piezoelectric effect. The former obtains the piezoelectric coefficient by applying an alternating load to the sample and measuring the electrical signal fed back by the sample, mainly including a piezoelectric coefficient meter, and the latter obtains the piezoelectric coefficient by applying an electrical signal to the sample and measuring the deformation, including piezoelectric force microscopy (PFM), double-beam laser interferometry (DBLI), etc. However, the existing test methods cannot eliminate the interference of the substrate under the film on the test during the measurement process, resulting in low measurement accuracy of the piezoelectric coefficient of the piezoelectric film material. In addition, most of the existing piezoelectric coefficient measurement equipment can only characterize one sample at a time, and its function is relatively single. If other parameters other than the piezoelectric coefficient are to be measured, additional experiments are required, which is inefficient. Summary of the invention

[0005] In view of the above-mentioned shortcomings of the prior art, the object of the present invention is to provide a high-throughput thin film piezoelectric performance comprehensive characterization device and method for solving the problem of the efficiency of screening piezoelectric thin film materials for multiple performance indicators including piezoelectric coefficient and Curie temperature in the prior art.

[0006] To achieve the above-mentioned and other related purposes, the present invention provides a high-throughput thin-film piezoelectric performance comprehensive characterization device, the device comprising: a shielding chamber and a measuring mechanism located in the shielding chamber, the measuring mechanism comprising:

[0007] A synchrotron radiation light source beam emitter, used to emit X-rays to a piezoelectric structure, wherein the piezoelectric structure includes a lower electrode composed of two or more independent first electrodes, a piezoelectric film located on the lower electrode, and an upper electrode located on the piezoelectric film, wherein the piezoelectric film is divided into two or more test areas based on different first electrodes;

[0008] An optical receiver, used for receiving X-rays returned by the piezoelectric film to obtain an X-ray spectrum of the piezoelectric film;

[0009] A sample stage, used to carry the piezoelectric structure and realize the movement and / or rotation of the piezoelectric structure to detect different test areas;

[0010] A power supply and an electrode selector, wherein the electrode selector is connected to the lower electrode and the upper electrode of the piezoelectric film and is used to select the test area to which voltage needs to be applied for testing by selecting different first electrodes;

[0011] The heating and temperature measuring device is used to heat the test area and perform temperature detection to obtain the Curie temperature of the test area in conjunction with the X-ray spectrum.

[0012] Optionally, the piezoelectric film includes at least two different components, or / and, the piezoelectric film includes at least two different structures, or / and, the piezoelectric film includes at least two different thicknesses.

[0013] Optionally, the upper electrode is composed of two or more independent second electrodes, the projections of the first electrode and the second electrode on the piezoelectric film have an overlapping area, and a voltage is applied to the corresponding test area by selecting the first electrode and the second electrode with the overlapping area.

[0014] Optionally, the material of the lower electrode includes one of Ti, Au, Pt, Mo and W, and the material of the upper electrode includes one of Ti, Au, Pt, Mo and W.

[0015] Optionally, the sample stage includes a rotating base, a Y-axis plane translation stage located on the rotating base, and an X-axis plane translation stage located on the Y-axis plane translation stage, which are used to align the test area selected by the electrode selector with the synchrotron radiation light source beam emitter to measure and characterize the piezoelectric properties of different test areas.

[0016] Optionally, the mechanism also includes a controller for controlling the actions of the synchrotron radiation light source beam emitter, the light receiver, the sample stage, the electrode selector, and the heating and temperature measuring device and collecting data.

[0017] Optionally, the mechanism further includes a calculator for processing and analyzing the X-ray spectrum information obtained by the optical receiver and the data collected by the controller to at least obtain the piezoelectric coefficient and Curie temperature of the piezoelectric film.

[0018] The present invention also provides a high-throughput thin film piezoelectric performance comprehensive characterization method, wherein the method preferably uses the comprehensive characterization device of the present invention for comprehensive characterization, and of course, other devices can also be used for comprehensive characterization. The comprehensive characterization method comprises the following steps:

[0019] Providing the high-throughput thin film piezoelectric performance comprehensive characterization device;

[0020] Moving the sample stage so that the X-ray beam emitted by the synchrotron radiation light source beam emitter is aimed at the test area;

[0021] The piezoelectric film is measured for the first time without applying an electric field, the sample stage is rotated by a preset angle, the light receiver obtains an X-ray spectrum signal, and the Bragg formula λ=2d·sinθ is substituted according to the measured diffraction peak θ and the wavelength λ of the light source to obtain the lattice constant d0 of the piezoelectric film in the test area at this time;

[0022] Apply an electric field E1 to the piezoelectric film for a second measurement, repeat the first measurement step, when the diffraction peak of the applied electric field is offset by a preset value from the diffraction peak of the first measurement without an electric field, the lattice constant of the piezoelectric film is obtained to be d1, the strain of the test area is S = (d1-d0) / d0, and the piezoelectric coefficient of the piezoelectric film in the test area is obtained to be d xy =S / E1;

[0023] During the second measurement, when the preset offset is generated, the heating and temperature measuring device is used to heat and measure the temperature of the test area;

[0024] When the diffraction peak position of the piezoelectric film in the test area changes after heating to a value greater than a preset threshold, the heating and temperature measuring device records the temperature of the test area at this time as the Curie temperature.

[0025] Optionally, different electric field strengths are applied to the piezoelectric film, and the second measurement is repeated n times, where n is an integer greater than or equal to 2, to obtain strains S1 to S2 of the test area under n electric field strengths. n , and the obtained strain-electric field (SE) curve was linearly fitted, and the slope after fitting was obtained as the piezoelectric coefficient

[0026] Optionally, the comprehensive characterization method further comprises the step of preparing a piezoelectric structure, and the preparation of the piezoelectric structure comprises the following steps:

[0027] forming a lower electrode on a substrate;

[0028] Patterning the lower electrode to form two or more mutually independent first electrodes;

[0029] Sequentially preparing various test areas of the piezoelectric film on the first electrode by selective area deposition;

[0030] An upper electrode is formed over the piezoelectric film.

[0031] Optionally, the substrate material includes one of sapphire, silicon, and silicon carbide.

[0032] Optionally, the preparation method of the piezoelectric film includes one of PVD, CVD, MBE, and ALD.

[0033] Optionally, the method further includes the step of patterning the upper electrode to form two or more independent second electrodes, wherein projections of the first electrode and the second electrode on the piezoelectric film have an overlapping area.

[0034] As described above, the high-throughput thin film piezoelectric performance comprehensive characterization device and method of the present invention have the following beneficial effects:

[0035] The present invention realizes high-throughput characterization of piezoelectric properties of thin films by partitioning and moving the piezoelectric films on the same substrate;

[0036] The present invention utilizes the ultra-high resolution of the lattice constant of an object by a synchrotron radiation source, and can observe the slight deformation of the piezoelectric film under an electric field, thereby effectively improving the measurement accuracy of the piezoelectric coefficient.

[0037] The present invention utilizes the uniqueness of X-ray spectra for specific materials to avoid interference of the substrate in measuring the deformation of the piezoelectric film;

[0038] The present invention can also simultaneously characterize the physical phase and structure of the film by using the X-ray spectrum, which can further improve the application scope of the characterization device and method of the present invention;

[0039] The present invention uses an in-situ heating and temperature measurement device to measure and characterize the Curie temperature of the piezoelectric film while characterizing the piezoelectric coefficient, thereby improving the comprehensive characterization efficiency of the piezoelectric performance of the piezoelectric film. BRIEF DESCRIPTION OF THE DRAWINGS

[0040] Figure 1Shown is a schematic diagram of the structure of a high-throughput thin-film piezoelectric performance comprehensive characterization device in one example of the present invention.

[0041] Figure 2 Shown is a schematic diagram of a piezoelectric structure in an example of the present invention.

[0042] Figure 3 to Figure 5 Shown is a schematic structural diagram of various steps of a method for preparing a piezoelectric structure in an example of the present invention.

[0043] Figure 6 Shown is a schematic flow chart of a high-throughput thin-film piezoelectric performance comprehensive characterization method in an example of the present invention.

[0044] Figure 7 It is a schematic diagram showing the diffraction peak shift of the piezoelectric film of the present invention (in the prior art) under different electric field intensities.

[0045] Figure 8 Shown is a schematic diagram of the strain-electric field (SE) function relationship and piezoelectric coefficient of the piezoelectric film of the present invention (in the prior art).

[0046] Component number description

[0047] 101 Synchrotron Radiation Source Beam Launcher

[0048] 102 Piezoelectric structure

[0049] 103 X-axis plane translation stage

[0050] 104 Y-axis plane translation stage

[0051] 105 Rotating Base

[0052] 106 Electrode Selector

[0053] 107 Power Supply

[0054] 108 Heating and temperature measuring device

[0055] 109 Controller

[0056] 110 Optical Receiver

[0057] 111 Calculator

[0058] 112 Shielded Room

[0059] 113 Sample stage

[0060] 201 Substrate

[0061] 202 Lower electrode

[0062] 203 Piezoelectric film

[0063] 204 Upper electrode

[0064] 205 Test Area

[0065] 206 first electrode

[0066] 207 Second Electrode

[0067] S101~S114 Example steps DETAILED DESCRIPTION

[0068] The following describes the embodiments of the present invention through specific examples, and those skilled in the art can easily understand other advantages and effects of the present invention from the contents disclosed in this specification. The present invention can also be implemented or applied through other different specific embodiments, and the details in this specification can also be modified or changed in various ways based on different viewpoints and applications without departing from the spirit of the present invention.

[0069] For example, when describing the embodiments of the present invention in detail, for the sake of convenience, the schematic diagrams showing the device structure will not be partially enlarged according to the general scale, and the schematic diagrams are only examples, which should not limit the scope of protection of the present invention. In addition, in actual production, the three-dimensional dimensions of length, width and depth should be included.

[0070] For convenience of description, spatially relative terms such as "under", "below", "below", "below", "above", "on", etc. may be used herein to describe the relationship of one element or feature shown in the drawings to other elements or features. It will be understood that these spatially relative terms are intended to encompass other orientations of the device in use or operation in addition to the orientation depicted in the drawings.

[0071] In the context of the present application, a structure in which a first feature is described as being "above" a second feature may include embodiments in which the first and second features are formed in direct contact, and may also include embodiments in which additional features are formed between the first and second features, such that the first and second features may not be in direct contact.

[0072] It should be noted that the illustrations provided in this embodiment are only used to illustrate the basic concept of the present invention in a schematic manner, and therefore the illustrations only show components related to the present invention rather than being drawn according to the number, shape and size of components in actual implementation. In actual implementation, the type, quantity and proportion of each component may be changed arbitrarily, and the component layout may also be more complicated.

[0073] In the existing piezoelectric performance characterization technology, the measurement results will be disturbed by the substrate. Taking the piezoelectric force microscope (PFM) as an example, it applies an electric field to the film through a probe in contact with the film, and measures the degree of deformation of the film through the probe to obtain the piezoelectric coefficient. However, when the film is deformed, it will also cause the substrate to warp. The total deformation includes the contribution of the substrate and the film, which will cause deviations in the measurement results. Although dual-beam laser interferometry (DBLI) can eliminate the interference caused by substrate warping, it is difficult to avoid the measurement deviation caused by the expansion or contraction of the substrate during the measurement process. In addition, most of the existing piezoelectric coefficient measurement equipment can only characterize one sample at a time, and has a single function. It is impossible to obtain other piezoelectric performance parameters such as Curie temperature, and the characterization efficiency is low.

[0074] To solve the above technical problems, Figure 1 As shown, and see Figures 2 to 5 The present invention provides a high-throughput thin film piezoelectric performance comprehensive characterization device, the comprehensive characterization device comprising:

[0075] A shielding room 112 and a measuring mechanism located in the shielding room 112, wherein the measuring mechanism comprises:

[0076] A synchrotron radiation light source beam emitter 101, used to emit X-rays to a piezoelectric structure 102, wherein the piezoelectric structure 102 includes a lower electrode 202 composed of two or more independent first electrodes 206, a piezoelectric film 203 located on the lower electrode 202, and an upper electrode 204 located on the piezoelectric film 203, wherein the piezoelectric film 203 is divided into two or more test areas 205 based on different first electrodes 206;

[0077] The optical receiver 110 is used to receive the X-rays returned by the piezoelectric film 203 to obtain the X-ray spectrum of the piezoelectric film 203;

[0078] A sample stage 113, used for carrying the piezoelectric structure 102 and realizing the movement and / or rotation of the piezoelectric structure 102, so as to detect different test areas 205;

[0079] A power supply 107 and an electrode selector 106, wherein the electrode selector 106 is connected to the lower electrode 202 and the upper electrode 204 of the piezoelectric film 203, and is used to select the test area 205 to which voltage needs to be applied for testing by selecting different first electrodes 206;

[0080] The heating and temperature measuring device 108 is used to heat the test area 205 and perform temperature detection to obtain the Curie temperature of the test area 205 in conjunction with the X-ray spectrum.

[0081] As an example, the piezoelectric film 203 includes at least two different components, or / and, the piezoelectric film 203 includes at least two different structures, or / and, the piezoelectric film 203 includes at least two different thicknesses.

[0082] As an example, the upper electrode 204 is composed of two or more independent second electrodes 207, and the projections of the first electrode 206 and the second electrode 207 on the piezoelectric film 203 have an overlapping area. A voltage is applied to the corresponding test area 205 by selecting the first electrode 206 and the second electrode 207 with the overlapping area.

[0083] As an example, the material of the lower electrode 202 includes one of Ti, Au, Pt, Mo and W, and the material of the upper electrode 204 includes one of Ti, Au, Pt, Mo and W. Preferably, one of the high temperature resistant metals W, Mo and Pt is used. Specifically, an alloy composed of two or more of the above electrode materials is used to make the electrode performances of various metals complement each other, so that the electrode can be made into an electrode with better performance than the original single metal material, such as more corrosion resistance and better conductivity.

[0084] As an example, the sample stage 113 includes a rotating base 105, a Y-axis plane translation stage 104 located on the rotating base 105, and an X-axis plane translation stage 103 located on the Y-axis plane translation stage 104, which is used to align the test area 205 selected by the electrode selector 106 with the synchrotron radiation light source beam emitter 101 to measure and characterize the piezoelectric properties of different test areas 205.

[0085] As an example, the device also includes a controller 109 for controlling the actions of the synchrotron radiation light source beam emitter 101, the light receiver 110, the sample stage 113, the electrode selector 106, and the heating and temperature measuring device 108 and collecting data.

[0086] As an example, the device further includes a calculator 111 for processing and analyzing the X-ray spectrum information obtained by the optical receiver 110 and the data collected by the controller 109 to at least obtain the piezoelectric coefficient and Curie temperature of the piezoelectric film 203 .

[0087] In addition, the present invention also provides a high-throughput thin film piezoelectric performance comprehensive characterization method, wherein the method preferably uses the comprehensive characterization device of the present invention for comprehensive characterization, and of course, other devices can also be used for comprehensive characterization. The comprehensive characterization method in this embodiment includes the following steps:

[0088] Step 1): providing the high-throughput thin film piezoelectric performance comprehensive characterization device;

[0089] Step 2): Move the sample stage 113 so that the X-ray beam emitted by the synchrotron radiation light source beam emitter 101 is aligned with the test area 205;

[0090] Step 3): The piezoelectric film 203 is measured for the first time without applying an electric field, the sample stage 113 is rotated by a preset angle, and the light receiver 110 obtains an X-ray spectrum signal. According to the measured diffraction peak θ and the wavelength λ of the light source, the Bragg formula λ=2d·sinθ is substituted to obtain the lattice constant d0 of the piezoelectric film 203 in the test area 205 at this time;

[0091] Step 4): Apply an electric field E1 to the piezoelectric film 203 for a second measurement, repeat the first measurement step, when the diffraction peak of the applied electric field is offset by a preset value from the diffraction peak of the first measurement without an electric field, the lattice constant of the piezoelectric film 203 is obtained to be d1, and the strain of the test area 205 is S=(d1-d0) / d0, and the piezoelectric coefficient of the piezoelectric film 203 in the test area 205 is obtained to be d xy =S / E1;

[0092] Step 5): During the second measurement, when the preset offset is generated, the heating and temperature measuring device 108 is used to heat and measure the temperature of the test area 205;

[0093] Step 6): When the change in the diffraction peak position of the piezoelectric film 203 in the test area 205 is greater than a preset threshold, the heating and temperature measuring device 108 records the temperature of the test area 205 at this time as the Curie temperature.

[0094] The high-throughput thin-film piezoelectric performance comprehensive characterization method of the present invention will be described in detail below in conjunction with the accompanying drawings. It should be noted that the above sequence does not strictly represent the sequence of the high-throughput thin-film piezoelectric performance comprehensive characterization method protected by the present invention, and those skilled in the art may change it according to the actual measurement steps. Figure 6 Only the steps of a high-throughput thin film piezoelectric performance comprehensive characterization method in one example are shown.

[0095] First, if Figure 6 As shown, step S101 is performed to move the X-axis plane translation stage 103 and the Y-axis plane translation stage so that the X-ray beam is aligned with the area to be tested of the piezoelectric structure 102. Specifically, as Figure 2 to Figure 5 As shown, the preparation of the piezoelectric structure 102 includes the following steps:

[0096] A lower electrode 202 is formed on a substrate 201;

[0097] The lower electrode 202 is patterned to form two or more independent first electrodes 206, such as Figure 3As shown;

[0098] The test areas 205 of the piezoelectric film 203 are sequentially prepared on the first electrode 206 by selective deposition. Figure 2 and Figure 4 As shown;

[0099] An upper electrode 204 is formed on the piezoelectric film 203. Figure 5 shown.

[0100] Specifically, the number of the test areas 205 prepared for high-throughput testing may be in the order of thousands or tens of thousands.

[0101] The present invention prepares a large number of test areas 205 on the same substrate 201, and moves the piezoelectric structure 102 by means of the X-axis plane translation stage 103 and the Y-axis plane translation stage, thereby realizing high-throughput piezoelectric performance characterization of the piezoelectric film 203, greatly saving the cost of screening piezoelectric materials. The automated operation device realizes the scale of piezoelectric material screening, while reducing the occurrence of operational errors and improving measurement speed, sensitivity and accuracy.

[0102] As an example, the substrate 201 material includes one of sapphire, silicon, and silicon carbide. Preferably, silicon material is used, which has high thermal conductivity and low cost, and is more suitable for the method of the present invention.

[0103] As an example, the preparation method of the piezoelectric film 203 includes one of PVD, CVD, MBE, and ALD.

[0104] As an example, the preparation of the piezoelectric structure 102 further includes the step of patterning the upper electrode 204 to form two or more independent second electrodes 207. Preferably, the projection angle range is 60° to 120°. The projections of the first electrode 206 and the second electrode 207 on the piezoelectric film 203 have an overlapping area.

[0105] Preferably, if Figure 2 As shown, each first electrode 206 is a strip electrode parallel to each other, and each second electrode 207 is a strip electrode parallel to each other, which is convenient for moving and positioning the sample stage 113 and transmitting and receiving X-rays.

[0106] Preferably, the projection angle between the first electrode 206 and the second electrode 207 on the film is 90°, so as to improve the area utilization rate of the piezoelectric structure 102 and facilitate the selection of the corresponding test area 205 by the electrode selector.

[0107] As an example, the patterning method of the lower electrode 202 and the upper electrode 204 includes one of optical exposure and development technology, micro-contact pattern transfer technology, and stripping technology. Preferably, the stripping technology is used to ensure the accuracy of the pattern size and avoid the problem of accidental contact of the electrode edge affecting the electrode selection function of the high-flux piezoelectric structure 102.

[0108] Then, if Figure 6 As shown, step S102 is performed to determine whether the piezoelectric film 203 needs to be subjected to an electric field. If it is the first measurement, the determination result is "no".

[0109] Then, if Figure 6 As shown, step S104 is performed to perform the first measurement on the piezoelectric film 203 without applying an electric field. Specifically, the rotating base 105 rotates by a preset angle, and the receiver obtains an X-ray spectrum signal. According to the measured diffraction peak θ and the wavelength λ of the light source, the Bragg formula λ=2d·sinθ is substituted to obtain the lattice constant d0 of the piezoelectric film 203 in the test area 205 at this time. Specifically, as Figure 7 The diagram shows the diffraction peak shift of the piezoelectric film 203 of the present invention under different electric field strengths. The horizontal axis represents the angle 2θ between the incident light and the diffracted light when the X-ray enters the lattice of the piezoelectric film 203. The vertical axis represents the intensity of the diffracted light collected at the angle corresponding to the horizontal axis. Different curves represent the corresponding angles and diffracted light intensities under different electric field strengths. The diffraction peak refers to the ray incident at a grazing angle of θ onto a crystal plane with a lattice lattice constant of a certain point of the measured material and a d. When the grazing angle satisfies the Bragg formula, the diffraction line enhanced by the superposition of the diffraction waves is reflected from the crystal plane of the measured material, and the diffraction peak of the measured material is defined as 2θ. Applying different electric field strengths to the material will cause the material to produce a slight deformation, and the lattice constant will change, thereby producing different diffraction peaks. According to the Bragg formula, the lattice constant of the measured material can be obtained by the known wavelength of the ray and the measured diffraction peak. The present invention utilizes the uniqueness of the X-ray spectrum collected under the irradiation of a synchrotron radiation light source for a specific material, thereby avoiding the interference of the substrate 201 in measuring the deformation of the piezoelectric film 203; in addition, utilizing the ultra-high resolution capability of the synchrotron radiation light source for the lattice constant of the object, the slight deformation of the piezoelectric film 203 under the electric field can be observed, thereby effectively improving the measurement accuracy of the piezoelectric coefficient.

[0110] Preferably, the rotation angle range of the rotating base 105 should be between θ and 2θ to ensure that the diffraction peak of the piezoelectric film 203 can be measured. Specifically, the rotation angle of the rotating base 105 is set to be between 10° and 80°.

[0111] Then, if Figure 6As shown, proceed to step S105 to determine whether the data is sufficient. If the determination result is "no", return to step S102 to step S105 again until the determination result is "yes", then proceed to step S106;

[0112] Specifically, it is determined whether the number of measurements is 2n according to the preset number of times n of measuring different electric fields. If the determination result is "no", the process returns to step S102 to step S105 again, which is the same as the above-mentioned process of steps S102 to S105. Specifically, n is an integer greater than or equal to 2.

[0113] As an example, the preset electric field is 1 kV / cm, 0 kV / cm, and -1 kV / cm.

[0114] As an example, n is 3, and when step S105 determines that the number of measurements is 6, the determination result is "yes".

[0115] Then, if Figure 6 As shown, step S106 is performed, according to the strains S1 to S5 of the test area 205 under five electric field strengths, and the obtained strain-electric field (SE) curve is linearly fitted to obtain the slope of the fitted curve as the piezoelectric coefficient Specifically, Figure 8 The strain-electric field (SE) function relationship and piezoelectric coefficient of the piezoelectric film 203 of the present invention (in the prior art) are shown as follows: Schematic diagram, as described above, the piezoelectric coefficient d xy =S / E1, the piezoelectric coefficient of a specific material is determined, so the strain of the material and the applied electric field strength are linearly related, and the slope of the linear fit is the piezoelectric coefficient after eliminating the accidental error in a single measurement to the greatest extent.

[0116] Among them, in an optional example, according to the collected X-ray spectrum signal, the physical phase and structure of the piezoelectric film 203 can also be characterized. The present invention adopts a high-throughput piezoelectric material measurement method, and practitioners may not know the specific values ​​of parameters such as the structure and composition of the material. The function of characterizing the physical phase and structure of the piezoelectric film 203 facilitates practitioners to study material parameters with ideal piezoelectric properties, which is conducive to further theoretical and practical research on the screening of piezoelectric materials.

[0117] Then, if Figure 6 As shown, step S107 is performed to determine whether to measure the Curie temperature according to a preset requirement. If the determination result is "yes", step S108 is performed to control the power supply 107 to apply a preset electric field to the piezoelectric film 203.

[0118] As an example, the preset electric field is 1 kV / cm.

[0119] Then, if Figure 6As shown, proceed to step S109, which is specifically implemented in the same process as the above step S104.

[0120] Then, if Figure 6 As shown, step S110 is performed to turn on the heating and temperature measuring device 108 and simultaneously observe the receiver to obtain an X-ray spectrum signal.

[0121] Then, if Figure 6 As shown, step S111 is performed to determine whether the change in the diffraction peak position of the film area reaches a preset threshold. Specifically, step S111 is performed alternately with step S110, that is, in the process of heating and measuring temperature and observing the X-ray spectrum signal in step S110, step S111 is performed at every preset time interval to determine whether the change in the diffraction peak position of the film area reaches a preset threshold. When the judgment result is "no", return to step S110, and when the judgment result is "yes", step S112 is performed to record the current temperature of the piezoelectric film 203, that is, the Curie temperature. The heating and temperature measuring device 108 records that the temperature of the test area 205 at this time is the Curie temperature. The preset time is determined according to the speed of the temperature rise of the piezoelectric film 203 and the Curie temperature accuracy expected by the practitioners. The present invention realizes the simultaneous measurement and characterization of the piezoelectric coefficient and the Curie temperature of the piezoelectric film 203 by combining the use of the synchrotron radiation light source and the heating and temperature measuring device 108, which greatly improves the efficiency of the practitioners in screening piezoelectric materials.

[0122] Then, if Figure 6 As shown, step S113 is performed to determine whether to measure other positions according to the preset measurement area. If the judgment result of step S107 is "no", step S113 is directly performed. If the judgment result is "yes", return to step S101. If the judgment result is "no", step S114 is performed to end the measurement.

[0123] In summary, the high-throughput thin film piezoelectric performance comprehensive characterization device and method of the present invention can achieve high-throughput characterization of thin film piezoelectric performance by moving and positioning the piezoelectric film on the same substrate, thereby reducing measurement costs and improving measurement speed and accuracy; at the same time, the uniqueness of the X-ray spectrum collected under the irradiation of a synchrotron radiation light source for a specific material is utilized to avoid interference caused by the substrate in measuring the deformation of the piezoelectric film; in addition, the ultra-high resolution of the lattice constant of the object by the synchrotron radiation light source can be used to observe the slight deformation of the piezoelectric film under the electric field, thereby effectively improving the measurement accuracy of the piezoelectric coefficient; at the same time, the collected X-ray spectrum can also characterize the physical phase and structure of the piezoelectric film, which is convenient for practitioners to further study the material characteristics of excellent piezoelectric performance; finally, in conjunction with the in-situ heating and temperature measuring device, after measuring the piezoelectric coefficient, the Curie temperature of the same piezoelectric film area can be measured in real time in situ in the same experiment, thereby improving the efficiency of comprehensive characterization of the piezoelectric performance of the piezoelectric film.

[0124] Therefore, the present invention effectively overcomes various shortcomings in the prior art and has high industrial utilization value.

[0125] The above embodiments are merely illustrative of the principles and effects of the present invention, and are not intended to limit the present invention. Anyone familiar with the art may modify or alter the above embodiments without departing from the spirit and scope of the present invention. Therefore, all equivalent modifications or alterations made by a person of ordinary skill in the art without departing from the spirit and technical concept disclosed by the present invention shall still be covered by the claims of the present invention.

Claims

1. A high-throughput thin film piezoelectric performance comprehensive characterization device, characterized in that: The device comprises: a shielding room and a measuring mechanism located in the shielding room, wherein the measuring mechanism comprises: A synchrotron radiation light source beam emitter, used for emitting X-rays to a piezoelectric structure, wherein the piezoelectric structure comprises a lower electrode composed of two or more independent first electrodes, a piezoelectric film located on the lower electrode, and an upper electrode located on the piezoelectric film, wherein the piezoelectric film is divided into two or more test areas based on different first electrodes; the upper electrode comprises two or more independent second electrodes, and the projections of the first electrode and the second electrode on the piezoelectric film have an overlapping area, and a voltage is applied to the corresponding test area by selecting the first electrode and the second electrode having the overlapping area; An optical receiver, used for receiving X-rays returned by the piezoelectric film to obtain an X-ray spectrum of the piezoelectric film; A sample stage, used for carrying the piezoelectric structure and realizing the movement and / or rotation of the piezoelectric structure, so as to detect different test areas; A power supply and an electrode selector, wherein the electrode selector is connected to the lower electrode and the upper electrode of the piezoelectric film and is used to select the test area to which voltage needs to be applied for testing by selecting different first electrodes; The heating and temperature measuring device is used to heat the test area and perform temperature detection to obtain the Curie temperature of the test area in conjunction with the X-ray spectrum.

2. The high-throughput thin film piezoelectric performance comprehensive characterization device according to claim 1, characterized in that: The piezoelectric film includes at least two different components, or / and, the piezoelectric film includes at least two different structures, or / and, the piezoelectric film includes at least two different thicknesses.

3. The high-throughput thin film piezoelectric performance comprehensive characterization device according to claim 1, characterized in that: The material of the lower electrode includes one of Ti, Au, Pt, Mo and W, and the material of the upper electrode includes one of Ti, Au, Pt, Mo and W.

4. The high-throughput thin film piezoelectric performance comprehensive characterization device according to claim 1, characterized in that: The sample stage includes a rotating base, a Y-axis plane translation stage located on the rotating base, and an X-axis plane translation stage located on the Y-axis plane translation stage, which are used to align the test area selected by the electrode selector with the synchrotron radiation light source beam emitter to measure and characterize the piezoelectric properties of different test areas.

5. The high-throughput thin film piezoelectric performance comprehensive characterization device according to claim 1, characterized in that: It also includes a controller for controlling the actions of the synchrotron radiation light source beam emitter, the light receiver, the sample stage, the electrode selector, and the heating and temperature measuring device and collecting data.

6. The high-throughput thin-film piezoelectric performance comprehensive characterization device according to claim 5, characterized in that: It also includes a calculator for processing and analyzing the X-ray spectrum information obtained by the optical receiver and the data collected by the controller to at least obtain the piezoelectric coefficient and Curie temperature of the piezoelectric film.

7. A high-throughput thin film piezoelectric performance comprehensive characterization method, characterized in that: The method comprises at least the following steps: Providing a high-throughput thin film piezoelectric performance comprehensive characterization device as described in any one of claims 1 to 6; Moving the sample stage so that the X-ray beam emitted by the synchrotron radiation light source beam emitter is aimed at the test area; The piezoelectric film is measured for the first time without applying an electric field, the sample stage is rotated by a preset angle, the light receiver obtains an X-ray spectrum signal, and the Bragg formula λ=2d·sinθ is substituted according to the measured diffraction peak θ and the wavelength λ of the light source to obtain the lattice constant d0 of the piezoelectric film in the test area at this time; Apply an electric field E1 to the piezoelectric film for a second measurement, repeat the first measurement step, when the diffraction peak of the applied electric field is offset by a preset value from the diffraction peak of the first measurement without an electric field, the lattice constant of the piezoelectric film is obtained to be d1, the strain of the test area is S=(d1-d0) / d0, and the piezoelectric coefficient of the piezoelectric film in the test area is obtained to be dxy=S / E1; During the second measurement, when the preset offset is generated, the heating and temperature measuring device is used to heat and measure the temperature of the test area; When the diffraction peak position of the piezoelectric film in the test area changes after heating to a value greater than a preset threshold, the heating and temperature measuring device records the temperature of the test area at this time as the Curie temperature.

8. The high-throughput thin film piezoelectric performance comprehensive characterization method according to claim 7, characterized in that: Apply different electric field strengths to the piezoelectric film, repeat the second measurement n times, where n is an integer greater than or equal to 2, to obtain the strains S1 to S2 of the test area under n electric field strengths. n , and the obtained strain-electric field (SE) curve was linearly fitted, and the slope after fitting was obtained as the piezoelectric coefficient 9. The high-throughput thin film piezoelectric performance comprehensive characterization method according to claim 7, characterized in that: The method also includes the step of preparing a piezoelectric structure, wherein the preparation of the piezoelectric structure includes the following steps: forming a lower electrode on a substrate; Patterning the lower electrode to form two or more mutually independent first electrodes; Sequentially preparing various test areas of the piezoelectric film on the first electrode by selective area deposition; An upper electrode is formed over the piezoelectric film.

10. The high-throughput thin film piezoelectric performance comprehensive characterization method according to claim 9, characterized in that: The preparation method of the piezoelectric film includes one of PVD, CVD, MBE and ALD.

11. The high-throughput thin film piezoelectric performance comprehensive characterization method according to claim 9, characterized in that: The method further includes the step of patterning the upper electrode to form two or more independent second electrodes, wherein the projections of the first electrode and the second electrode on the piezoelectric film have an overlapping area.

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