CN115069524A - 1-3 composite piezoelectric material for high-frequency ultrasonic transducer and preparation method thereof - Google Patents
1-3 composite piezoelectric material for high-frequency ultrasonic transducer and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a piezoelectric material, in particular to a 1-3 composite piezoelectric material for a high-frequency ultrasonic transducer and a preparation method thereof, which comprises the following steps: s1: preparing a soft template containing micropores by an etching technology; s2: filling the micropores in the soft template obtained in the step S1 with piezoelectric ceramic powder; s3: sintering the product obtained in the step S2 at high temperature to remove the soft template, so as to obtain a piezoelectric ceramic column array; s4: filling and curing the piezoelectric ceramic column array obtained in the step S3 by using a high molecular polymer to obtain a semi-finished product; s5: and grinding and thinning the semi-finished product obtained in the step S4, plating electrodes and polarizing to obtain the 1-3 composite piezoelectric material. Compared with the prior art, the preparation method realizes simplification and high efficiency of the preparation process, and the prepared 1-3 composite piezoelectric material has excellent piezoelectric performance in a high-frequency ultrasonic range (30-50 MHz).
Description
Technical Field
The invention relates to a piezoelectric material, in particular to a 1-3 composite piezoelectric material for a high-frequency ultrasonic transducer and a preparation method thereof.
Background
High-frequency medical ultrasonic imaging and industrial nondestructive testing can carry out micro-structure ultrasonic imaging and detection with micron-scale resolution on human tissues and important micro industrial parts through an ultrasonic transducer, and the technology belongs to next-generation high-end medical and industrial equipment and is one of the key points of technical research. The ultra-high spatial resolution of a high-frequency ultrasonic transducer requires high sensitivity and bandwidth, but the higher the frequency of ultrasonic transmission and reception, the lower the electromechanical coupling coefficient determining the electromechanical conversion efficiency thereof. Therefore, there is a need for ultrasonic imaging, detection and identification using a piezoelectric material that has a high electromechanical coupling coefficient in the high frequency ultrasonic band.
Compared with the traditional single-phase piezoelectric material (such as PZT ceramic, PMNT single crystal and the like), the 1-3 composite material has higher electromechanical coupling coefficient on one hand, and can greatly increase the sensitivity of echo signals of the ultrasonic transducer. On the other hand, the high-frequency ultrasonic transducer has lower acoustic impedance than a single-phase material, is easy to realize impedance matching with human tissues and plastic parts, and can increase the sensitivity of the high-frequency ultrasonic transducer and simultaneously reduce the difficulty of the preparation process of the transducer. Particularly, in a high-frequency ultrasonic stage of 30-50MHz, the 1-3 composite material still has a high electromechanical coupling coefficient, and is a necessary material for high-performance medical high-frequency ultrasonic imaging and high-frequency nondestructive testing.
The 1-3 composite material for high-frequency ultrasonic imaging is different from a common piezoelectric material used at medium and low frequencies, and the piezoelectric phase microstructure of the composite material is required to have large length-diameter ratio, small column spacing and high piezoelectric performance on a micron scale due to the requirement of a longitudinal vibration mode. However, for a piezoelectric microstructure of dozens of micrometers applied to high-frequency ultrasound, the conventional 1-3 composite material preparation methods such as a mechanical cutting-filling method, a plasma etching method and the like require large-scale precision equipment, consume much time, have a small piezoelectric filling proportion, and cannot meet the industrial production of high-frequency composite materials. In addition, the traditional silicon template method adopts a photoetching silicon wafer as a template, PZT nano powder is injected into micropores, and a piezoelectric column array is prepared by hot isostatic pressing sintering, but the incompressibility of the silicon template ensures that the sintering density of the ceramic microcolumns is low, and higher piezoelectric performance is difficult to obtain.
Disclosure of Invention
The present invention has been made to solve at least one of the above problems, and an object of the present invention is to provide a 1-3 composite piezoelectric material for a high-frequency ultrasonic transducer and a method for manufacturing the same, which can simplify and improve the efficiency of a manufacturing process, and can obtain a 1-3 composite piezoelectric material having excellent piezoelectric properties in a high-frequency ultrasonic range (30 to 50 MHz).
The purpose of the invention is realized by the following technical scheme:
the invention discloses a preparation method of a 1-3 composite piezoelectric material for a high-frequency ultrasonic transducer, which comprises the following steps:
s1: preparing a soft template containing micropores by an etching technology;
s2: filling the micropores in the soft template obtained in the step S1 with piezoelectric ceramic powder;
s3: sintering the product obtained in the step S2 at high temperature to remove the soft template, so as to obtain a piezoelectric ceramic column array;
s4: filling and curing the piezoelectric ceramic column array obtained in the step S3 by using a high molecular polymer to obtain a semi-finished product;
s5: and grinding and thinning the semi-finished product obtained in the step S4, plating electrodes and polarizing to obtain the 1-3 composite piezoelectric material.
Preferably, in step S1, the etching technique is one of laser etching, plasma etching and chemical etching; the soft template is made of rosin; the diameter of the micropores is 25-150 μm, and the length is not more than 200 μm; the density of the micropores on the soft template is 400- 2 . Through the design of the template micropores, the diameter, the spacing and the arrangement mode of the piezoelectric columns (microcolumns) in the prepared product can be controlled, and the microstructure regulation and control are realized; and the use of the template enables the product to be prepared and produced in large-scale batch.
Preferably, in step S2, the piezoelectric ceramic powder is a perovskite-structured ferroelectric powder.
Preferably, the piezoelectric ceramic powder is one or more of lead zirconate titanate (PZT), lead magnesium niobate titanate (PMN-PT), lead indium magnesium niobate titanate (PIN-PMN-PT, i.e., lead indium niobate-lead magnesium niobate-lead titanate), potassium sodium niobate (KNN), and bismuth sodium titanate-barium titanate (NBT-BT).
Preferably, in step S2, the filling includes the following steps:
s21: dispersing piezoelectric ceramic powder in a binder to form slurry;
s22: vacuum-filling the slurry obtained in the step S21 into the micropores in the soft template obtained in the step S1, and then drying the slurry under normal pressure to form a microcolumn precursor with high density;
s23: a pressure perpendicular to the surface is applied to the microcolumn precursor obtained in step S22.
Preferably, in step S21, the binder is acrylamide.
Preferably, in step S23, the pressure is 6.0MPa and the maintaining time is 30 min.
Preferably, in step S3, the high-temperature sintering is unidirectional hot-pressing sintering, which includes the following steps: the soft template is heated to 500-1200 ℃ at the heating rate of 50 ℃/h and is kept for 2-3h, and then is heated to 1150-1200 ℃ at the same heating rate and is kept for 1.5-2 h. The main advantages of the unidirectional hot-pressing sintering adopted in the invention are that firstly, the equipment requirement is not as high as that of isostatic hot-pressing sintering (another hot-pressing sintering mode), the technological process is simple, the cost is low, and meanwhile, the sintering densification effect can be achieved. In addition, because the soft template is pressurized, the unidirectional hot-pressing sintering can enable the sample to be burnt out and kept flat, and the template can be pressed into an irregular shape by isostatic pressing and cannot be used.
The high-temperature sintering in step S3 has three functions: firstly, removing the soft template; secondly, the sintered piezoelectric microcolumns are erected on a substrate to form a piezoelectric ceramic microcolumn array; and thirdly, the substrate can shrink in the sintering process, so that the spacing between the piezoelectric micro-columns is reduced, the arrangement is tighter, and the filling proportion of the piezoelectric phase is increased.
Preferably, in step S4, the high molecular polymer is an epoxy resin; the filling and curing are carried out under vacuum conditions. The epoxy curing is carried out under the vacuum-pumping condition, so that air bubbles in gaps of the ceramic microcolumns can be eliminated.
Preferably, in step S5, the upper and lower surfaces of the cured composite material are thinned by grinding to maintain parallelism, and the substrate is also removed by grinding; grinding and thinning the composite material to a required thickness according to the frequency requirement of the transducer, and plating electrodes on the upper surface and the lower surface by utilizing magnetron sputtering; and (3) polarizing the sample, wherein the polarization is performed under the conditions of silicone oil and room temperature, the applied electric field is 3kV/mm, and the polarization time is 30 minutes.
The invention discloses a 1-3 composite piezoelectric material for a high-frequency ultrasonic transducer in a second aspect, which is prepared by the preparation method of the 1-3 composite piezoelectric material for the high-frequency ultrasonic transducer.
Compared with the prior art, the invention has the following beneficial effects:
1. in the aspect of preparation, the method is an effective novel method for preparing the high-frequency 1-3 composite piezoelectric material, has high preparation efficiency and low cost, and is beneficial to industrial preparation and application of the 1-3 composite piezoelectric material in the technical field of high-frequency ultrasound.
2. The piezoelectric ceramic microcolumn prepared by the invention has the advantages of uniform radial distribution of element content, simple phase structure and complete crystal lattice. Comprehensive performance tests show that the high-frequency 1-3 composite piezoelectric material prepared by the invention has excellent piezoelectric performance in a high-frequency ultrasonic range (30-50MHz), particularly the electromechanical coupling coefficient can reach more than 61.5 percent, and the piezoelectric performance is greatly improved compared with single-phase PZT ceramics with the same component.
3. The composite piezoelectric material provided by the invention is composed of two parts, and plays a main role in a piezoelectric phase (piezoelectric column), so that 1) the higher the piezoelectric performance of the piezoelectric column material is, the larger the piezoelectric response of the composite material is. Piezoelectric constant d of commonly used piezoelectric materials 33 600 to 1300 pC/N. 2) The length-diameter ratio (cylindrical), namely the common width-height ratio (strip shape), of the invention is between 1.2 and 5Belonging to a longitudinal vibration mode and having a high electromechanical coupling coefficient (>60%) instead of composite aspect ratio 0.1, the electromechanical coupling coefficient is only 50% for monolithic PZT ceramics. 3) The distance between the composite material columns prepared by the cut-and-fill method is general>12 μm, the preparation method of the invention can realize>3 μm, the column spacing is smaller, and compared with the two, the piezoelectric constant of the composite material can be improved by 30 percent.
4. The invention uses the soft template to prepare, so that the prepared composite piezoelectric material has the following advantages:
1) diameter: the diameter can be made very small, minimum 25 microns. Under the condition of keeping the long diameter to be larger (1.2-5), the smaller the diameter is, the smaller the column length (the thickness of the composite material) is, the smaller the thickness is, the high frequency is, and the higher the resonant frequency of the composite material is, so that the frequency of the material and the ultrasonic transducer can be improved, and the high frequency (30-50MHz) is achieved. Only when the diameter is small enough, high frequency can be achieved, for example, when the traditional cutting and filling method is adopted, the pillar is too thin and falls down, and only 10MHz at most can be achieved, so that the high frequency requirement cannot be met.
2) Spacing: when the distance is small, the proportion of the piezoelectric phase can be increased, the piezoelectric response of the whole composite material is large, or the piezoelectric performance is good, and the piezoelectric coefficient is large. The minimum distance obtained by the traditional method is 12 microns, while the minimum distance obtained by the method is 3 microns, so that the piezoelectric constant of the composite material can be improved by 30-40% compared with that obtained by the traditional method.
3) The arrangement mode is as follows: the uniform random arrangement can inhibit the vibration mode between the pillars, so that the vibration mode of the whole composite material is purer, and the signal of the piezoelectric response is purer.
Drawings
FIG. 1 is a schematic flow diagram of a production process of the present invention;
FIG. 2 is a microscopic structural view of a 1-3 composite piezoelectric material obtained in example 1;
fig. 3 is a graph of impedance properties versus resonant/antiresonant frequencies for 1-3 composite piezoelectric materials prepared in example 1.
Detailed Description
The invention is described in detail below with reference to the figures and specific embodiments.
In the following examples, if the reagents used are not specifically described, commercially available products that can be obtained conventionally by those skilled in the art can be used. In the following examples, methods that can be conventionally known and used by those skilled in the art can be used unless otherwise specified.
A preparation method of a 1-3 composite piezoelectric material for a high-frequency ultrasonic transducer is shown in figure 1 and comprises the following steps:
s1: preparing a soft template containing micropores through laser etching;
s2: filling the micropores in the soft template obtained in the step S1 with piezoelectric ceramic powder;
s3: sintering the product obtained in the step S2 at high temperature to remove the soft template, so as to obtain a piezoelectric ceramic column array;
s4: filling and curing the piezoelectric ceramic column array obtained in the step S3 by using a high molecular polymer to obtain a semi-finished product;
s5: and grinding and thinning the semi-finished product obtained in the step S4, plating electrodes and polarizing to obtain the 1-3 composite piezoelectric material.
In step S1, the soft template is made of rosin and has a thickness of 0.5 +/-0.2 mm; the diameter of the micropores is 25-70 μm, and the length is not more than 200 μm; the density of the micropores on the soft template is 400- 2 。
In step S2, the piezoelectric ceramic powder is a perovskite-structured ferroelectric powder, and may specifically be one or more of lead zirconate titanate (PZT), lead magnesium niobate titanate (PMN-PT), lead indium magnesium niobate titanate (PIN-PMN-PT), potassium sodium niobate (KNN), and sodium bismuth titanate-barium titanate (NBBT).
Wherein, the filling in step S2 includes the following sub-steps:
s21: dispersing piezoelectric ceramic powder with the granularity of 1-3 mu m in an adhesive to form slurry;
s22: vacuum-filling the slurry obtained in the step S21 into the micropores in the soft template obtained in the step S1, and then drying the slurry under normal pressure to form a microcolumn precursor with high density;
s23: a pressure of 6.0MPa perpendicular to the surface was applied to the microcolumn precursor obtained in step S22, and maintained for 30 minutes.
In step S3, the high-temperature sintering is unidirectional hot-pressed sintering, which includes the following steps: the soft template is heated to 500-1200 ℃ at the heating rate of 50 ℃/h and is kept for 2-3h, and then is heated to 1150-1200 ℃ at the same heating rate and is kept for 1.5-2 h.
In step S4, the high molecular polymer is epoxy resin; the filling and curing are carried out under vacuum conditions.
In step S5, the upper and lower surfaces of the cured composite material are thinned by grinding to maintain parallelism, and the substrate is also removed by grinding; grinding and thinning the composite material to a required thickness according to the frequency requirement of the transducer, and plating electrodes on the upper surface and the lower surface by utilizing magnetron sputtering; and (3) polarizing the sample, wherein the polarization is performed under the conditions of silicone oil and room temperature, the applied electric field is 3kV/mm, and the polarization time is 30 minutes.
Example 1
Preparing a 1-3 composite piezoelectric material with high uniformity and a microcolumn diameter of 25 mu m:
in the embodiment, lead zirconate titanate (PZT) nano powder with a homogeneous phase boundary component is selected as a piezoelectric phase, and the average grain size of PZT is 500 nm; and epoxy resin (Epo-Tek 301-2) was chosen as the polymer matrix.
S1: a flexible template was prepared by laser etching a plastic sheet as shown in fig. 1. The thickness of the soft template is 0.5 +/-0.2 mm, and the diameter of the micropore is 25 mu m.
S2, filling the micropores of the template by adopting powder of PZT-5H component.
1) And dispersing PZT powder with the granularity within the range of 1-3 mu m into the adhesive solution to form PZT slurry.
2) And pouring the slurry into micropores of the plastic sheet in a vacuum environment, and drying at normal pressure to volatilize the flux so as to form a microcolumn precursor with high density.
3) The template filled with PZT powder was maintained under a pressure of 6.0MPa perpendicular to the surface for 30 minutes.
S3: and heating the soft template to 500 ℃ at the heating rate of 50 ℃/h, preserving heat for 3h, continuously heating to 1200 ℃ at the same heating rate, preserving heat for 2h, and sintering the PZT ceramic microcolumn.
S4: and filling and curing by using an epoxy resin polymer (Epo-Tek 301-2) to obtain the 1-3 type piezoelectric composite material, as shown in figure 1. Selecting a PZT powder tablet as a micro-column array substrate, wherein the density of the tablet is 3.52g/cm 3 The diameter of the tablet is 10mm and the thickness is 1 mm. The pressing sheet shrinks in the sintering process, so that the space between the PZT piezoelectric micro-columns on the pressing sheet can be obviously reduced, and the arrangement of the PZT piezoelectric micro-columns is more compact. As shown in fig. 2.
S5: grinding and thinning the sample by a cutting machine, specifically, thinning the 1-3 composite piezoelectric material obtained by curing by a mechanical grinding machine, roughly grinding by a 1000-mesh diamond grinding disc, and finely grinding by an alumina template to finally obtain a 1-3 composite piezoelectric material sheet with the thickness of 50 microns. The upper and lower surfaces of the sample were then plated with gold electrodes using magnetron sputtering, as shown in FIG. 1. The specific operation is as follows: and (3) carrying out ultrasonic cleaning on the wafer in alcohol, acetone and deionized water respectively for 15 minutes by using an ultrasonic cleaning machine, and then drying at 50 ℃. And then carrying out multilayer composite electrode coating on the upper surface and the lower surface of the sample by utilizing magnetron sputtering. In this example, a Ni electrode is sputtered first, then a Cr electrode is sputtered as a transition electrode with a thickness controlled between 900-1500nm, and then a Au electrode is sputtered with a thickness controlled between 1-2 μm. The sputtering time of each layer of electrode was 10 minutes, and the surface temperature of the sample was kept below 80 ℃.
S6: and (3) polarizing the sample, wherein the polarization is performed under the conditions of silicone oil and room temperature, the applied electric field is 3kV/mm, and the polarization time is 30 minutes.
Microstructure observation was performed on the prepared 1-3 composite material using an optical microscope at a magnification of 1000 times, as shown in fig. 2. The piezoelectric columns are arranged neatly and uniformly, and the diameter of each piezoelectric column is smaller and reaches 25 mu m. The average spacing between the ceramic micro-pillars is small, reaching 3 μm.
The shape and size of the piezoelectric column directly determine the piezoelectric constant of the material and determine the vibration mode of the material, and the vibration mode determines the electromechanical coupling performance. Therefore, the piezoelectric columns are tidy and uniform, vibration mode interference among the columns can be consistent, the vibration mode is pure, and the purity of generating and receiving piezoelectric signals is improved. In addition, the diameter of the column is small, so that the sample can be made thinner under the condition of maintaining a certain length-diameter ratio (determining the size of electromechanical coupling performance), and then the frequency is made higher, so that high frequency is realized. The average distance is smaller, so that the proportion of the piezoelectric phase can be improved, and a larger piezoelectric constant, namely a higher piezoelectric response, can be obtained.
And (3) impedance spectrum testing, namely measuring an impedance-frequency spectrum and a loss-frequency spectrum of the product by using a precision LCR analyzer HP4284A according to a piezoceramic material performance testing method-performance parameter determination (GB/T3389-2008). The measurement temperature was room temperature and the test frequency was in the range of 20-60MHz as shown in FIG. 3.
As can be seen from FIG. 3, the resonant frequency of the high-frequency 1-3 composite piezoelectric material of this embodiment is 37.4MHz, the anti-resonant frequency is 46.1MHz, and the electromechanical coupling coefficient reaches 62.4% and is significantly higher than that of a PZT single-phase ceramic plate (k is significantly higher than that of a PZT single-phase ceramic plate) calculated according to the method for testing the performance of piezoelectric ceramic materials-determination of performance parameters (GB/T3389- t ～50％)。
Examples 2 to 5
The preparation process was substantially the same as in example 1 except that the design size of the micropores was changed in step S1, and the specific data are shown in Table 1.
The performance test method was the same as in example 1.
Example 6
S1, preparing soft templates with different thicknesses and different micropore diameters by adopting a method of laser etching plastic sheets with different thicknesses, as shown in figure 1. The thickness of the soft template is 0.5 +/-0.2 mm, and the diameter of the micropore is 120 mu m.
S2, filling the micropores of the template by adopting powder of PZT-5H component.
1) And dispersing PZT powder with the granularity of 1-3 mu m into the adhesive solution to form PZT slurry.
2) And pouring the slurry into micropores of the plastic sheet in a vacuum environment, and drying at normal pressure to volatilize the flux so as to form the microcolumn precursor with high density.
3) The template filled with PZT powder was maintained under a pressure of 6MPa perpendicular to the surface for 30 minutes.
And S3, heating the soft template to 530 ℃ at a heating rate of 50 ℃/h, preserving heat for 2h, continuously heating to 1200 ℃ at the same heating rate, preserving heat for 2h, and sintering the PZT ceramic microcolumn.
S4, filling and curing by using epoxy resin polymer (Epo-Tek 301-2) to obtain the 1-3 type piezoelectric composite material, as shown in figure 1. Selecting a PZT powder tablet as a micro-column array substrate, wherein the density of the tablet is 3.52g/cm 3 The diameter of the tablet is 10mm and the thickness is 1 mm.
And S5, cutting the sample into different thicknesses by a cutting machine, and plating gold electrodes on the upper surface and the lower surface of the sample by magnetron sputtering, as shown in figure 1. This process corresponds to step S5 in embodiment 1.
And S6, polarizing the sample, wherein the polarization is carried out under the conditions of silicone oil and room temperature, the applied electric field is 3kV/mm, and the polarization time is 30 minutes.
The performance test method was the same as in example 1, and the results are shown in Table 1.
Table 1 examples 1-6 data summary table
In Table 1, sample number 1# corresponds to the sample prepared in example 1, sample number 2# corresponds to the sample prepared in example 2, and so on.
And further observing the microstructures of the prepared 6 1-3 composite piezoelectric material samples by using a scanning electron microscope SEM. For example, microstructure information such as a microcolumn diameter d, a microcolumn pitch s, a microcolumn length h, etc. is obtained as shown in table 1. Therefore, the preparation method can prepare samples with any microcolumn diameter from 25 μm to 120 μm; the range of the space between the obtained ceramic micro-columns is 3-10 mu m; the length range of the obtained PZT ceramic microcolumn is 40-100 mu m; the proportion range of the available 1-3 composite piezoelectric material ceramic phase is 43-55%; the resonance frequency that can be achieved can be higher than 35MHz, and the maximum anti-resonance frequency in the sample reaches 46.1 MHz. When the composite material is used to make an ultrasonic transducer, an important parameter of the transducer is the center frequency, which is determined by the resonant frequency and the anti-resonant frequency of the composite material. The higher the resonant, anti-resonant frequency of the material, the higher the center frequency of the transducer. As can be seen by combining the detection data in Table 1, the center frequency of the material prepared by the method provided by the invention can reach high frequency after the material is further prepared into an ultrasonic transducer.
In addition, as shown in Table 1, the electromechanical coupling coefficient is distributed between 61% and 71% at high frequency (40 MHz) and is much higher than 50% to 55% of that of a PZT ceramic single chip, so that the electromechanical coupling performance advantage is relatively high, and the performance of the high-frequency ultrasonic transducer is favorably improved.
The embodiments described above are described to facilitate an understanding and use of the invention by those skilled in the art. It will be readily apparent to those skilled in the art that various modifications to these embodiments may be made, and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the above embodiments, and those skilled in the art should make improvements and modifications within the scope of the present invention based on the disclosure of the present invention.
Claims (10)
1. A preparation method of a 1-3 composite piezoelectric material for a high-frequency ultrasonic transducer is characterized by comprising the following steps:
s1: preparing a soft template containing micropores by an etching technology;
s2: filling the micropores in the soft template obtained in the step S1 with piezoelectric ceramic powder;
s3: sintering the product obtained in the step S2 at high temperature to remove the soft template, so as to obtain a piezoelectric ceramic column array;
s4: filling and curing the piezoelectric ceramic column array obtained in the step S3 by using a high molecular polymer to obtain a semi-finished product;
s5: and grinding and thinning the semi-finished product obtained in the step S4, plating electrodes and polarizing to obtain the 1-3 composite piezoelectric material.
2. The method for preparing a 1-3 composite piezoelectric material for a high-frequency ultrasonic transducer according to claim 1, wherein in step S1, the etching technique is one of laser etching, plasma etching and chemical etching; the soft template is made of rosin; the diameter of the micropores is 25-150 μm, and the length is not more than 200 μm; the density of the micropores on the soft template is 400- 2 。
3. The method for preparing a 1-3 composite piezoelectric material for a high-frequency ultrasonic transducer according to claim 1, wherein in step S2, the piezoelectric ceramic powder is a perovskite structure ferroelectric powder.
4. The method for preparing a 1-3 composite piezoelectric material for a high-frequency ultrasonic transducer according to claim 3, wherein the piezoelectric ceramic powder is one or more of lead zirconate titanate, lead magnesium niobate titanate, lead indium magnesium niobate titanate, potassium sodium niobate and sodium bismuth titanate-barium titanate.
5. The method for preparing a 1-3 composite piezoelectric material for a high-frequency ultrasonic transducer according to claim 1, wherein the filling in step S2 comprises the steps of:
s21: dispersing piezoelectric ceramic powder in a binder to form slurry;
s22: vacuum-filling the slurry obtained in the step S21 into the micropores in the soft template obtained in the step S1, and then drying under normal pressure to form a microcolumn precursor;
s23: a pressure perpendicular to the surface is applied to the microcolumn precursor obtained in step S22.
6. The method for preparing a 1-3 composite piezoelectric material for a high-frequency ultrasonic transducer according to claim 5, wherein in step S21, the binder is acrylamide.
7. The method for preparing a 1-3 composite piezoelectric material for a high-frequency ultrasonic transducer according to claim 5, wherein in step S23, the pressure is 6.0MPa and the holding time is 30 min.
8. The method for preparing a 1-3 composite piezoelectric material for a high-frequency ultrasonic transducer according to claim 1, wherein in step S3, the high-temperature sintering is unidirectional hot-pressing sintering, comprising the following steps: the soft template is heated to 500-1200 ℃ at the heating rate of 50 ℃/h and is kept for 2-3h, and then is heated to 1150-1200 ℃ at the same heating rate and is kept for 1.5-2 h.
9. The method for preparing a 1-3 composite piezoelectric material for a high-frequency ultrasonic transducer according to claim 1, wherein in step S4, the high molecular polymer is an epoxy resin; the filling and curing are carried out under vacuum conditions.
10. A 1-3 composite piezoelectric material for a high-frequency ultrasonic transducer, characterized by being prepared by the method for preparing a 1-3 composite piezoelectric material for a high-frequency ultrasonic transducer according to any one of claims 1 to 9.
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