CN115069524B - 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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- CN115069524B CN115069524B CN202210772291.0A CN202210772291A CN115069524B CN 115069524 B CN115069524 B CN 115069524B CN 202210772291 A CN202210772291 A CN 202210772291A CN 115069524 B CN115069524 B CN 115069524B
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- B06B1/00—Methods or apparatus for generating mechanical vibrations of infrasonic, sonic, or ultrasonic frequency
- B06B1/02—Methods or apparatus for generating mechanical vibrations of infrasonic, sonic, or ultrasonic frequency making use of electrical energy
- B06B1/06—Methods or apparatus for generating mechanical vibrations of infrasonic, sonic, or ultrasonic frequency making use of electrical energy operating with piezoelectric effect or with electrostriction
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- B06B2201/00—Indexing scheme associated with B06B1/0207 for details covered by B06B1/0207 but not provided for in any of its subgroups
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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, comprising the following steps: s1: preparing a soft template containing micropores by an etching technology; s2: filling micropores in the soft template obtained in the step S1 with piezoelectric ceramic powder; s3: performing high-temperature sintering on the product obtained in the step S2 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 polymer to obtain a semi-finished product; s5: and (3) 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 provided by the invention has the advantages that the preparation process is simplified and efficient, and meanwhile, 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
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 high frequency ultrasonic transducers requires higher sensitivity and bandwidth, but the higher the frequency of ultrasonic transmission and reception, the lower the electromechanical coupling coefficient that determines their electromechanical conversion efficiency. Accordingly, there is a need for ultrasound imaging, detection and identification using a piezoelectric material that still has a high electromechanical coupling coefficient at high frequency ultrasound bands.
Compared with the traditional single-phase piezoelectric material (such as PZT ceramics, PMNT single crystals and the like), the 1-3 composite material has higher electromechanical coupling coefficient on one hand and can greatly increase the sensitivity of the echo signal of the ultrasonic transducer. On the other hand, the high-frequency ultrasonic transducer has lower acoustic impedance than that of 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 reduce the preparation process difficulty of the transducer. In particular, in the high-frequency ultrasonic stage of 30-50 MHz, the 1-3 composite material still has higher electromechanical coupling coefficient, and is a necessary material for high-performance medical high-frequency ultrasonic imaging and high-frequency nondestructive detection.
The 1-3 composite material for high-frequency ultrasonic imaging is different from the piezoelectric material used in common medium-low frequency, 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 the micrometer scale due to the requirement of a longitudinal vibration mode. However, for the piezoelectric microstructure of several tens micrometers applied by high-frequency ultrasound, the traditional 1-3 composite material preparation methods such as a mechanical cutting-filling method, a plasma etching method and the like need large-scale precise equipment, are time-consuming and have small piezoelectric filling proportion, and cannot meet the industrial production of the high-frequency composite material. In addition, the traditional silicon template method adopts a photoetching silicon wafer as a template, PZT nano powder is injected into micropores and hot isostatic pressing sintering is used for preparing the piezoelectric column array, but the incompressibility of the silicon template leads the sintering density of the ceramic micro column to be low, and higher piezoelectric performance is difficult to obtain.
Disclosure of Invention
The invention aims to solve at least one of the problems and provide a 1-3 composite piezoelectric material for a high-frequency ultrasonic transducer and a preparation method thereof, which realize simplification and high efficiency of the preparation process, and meanwhile, the prepared 1-3 composite piezoelectric material has excellent piezoelectric performance in a high-frequency ultrasonic range (30-50 MHz).
The aim of the invention is achieved 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 micropores in the soft template obtained in the step S1 with piezoelectric ceramic powder;
s3: performing high-temperature sintering on the product obtained in the step S2 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 polymer to obtain a semi-finished product;
S5: and (3) 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 technology 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 micropores on the soft template is 400-1000 micropores/mm 2. The diameter, the spacing and the arrangement mode of piezoelectric columns (micro columns) in the prepared product can be controlled by the design of template micropores, so that microstructure regulation and control are realized; and the use of the template enables the product to realize large-scale batch preparation and production.
Preferably, in step S2, the piezoelectric ceramic powder is perovskite structure ferroelectric powder.
Preferably, the piezoelectric ceramic powder is one or more of lead zirconate titanate (PZT), lead magnesium niobate titanate (PMN-PT), lead indium niobate titanate (PIN-PMN-PT), i.e., lead indium niobate-lead magnesium niobate-lead titanate), potassium sodium niobate (KNN), and sodium bismuth titanate-barium titanate (NBT-BT).
Preferably, in step S2, the filling includes the following steps:
S21: dispersing piezoelectric ceramic powder in an adhesive to form slurry;
S22: vacuum pouring the slurry obtained in the step S21 into micropores in the soft template obtained in the step S1, and then drying under normal pressure to form a microcolumn precursor with higher density;
s23: and (2) applying pressure vertical to the surface to the micro-column precursor obtained in the step S22.
Preferably, in step S21, the adhesive is acrylamide.
Preferably, in step S23, the pressure is 6.0MPa and the holding time is 30min.
Preferably, in step S3, the high-temperature sintering is unidirectional hot-pressed sintering, and includes the following steps: the soft template is heated to 500-530 ℃ at the heating rate of 50 ℃/h and is kept for 2-3h, and then heated to 1150-1200 ℃ at the same heating rate and is kept for 1.5-2h. The method has the main advantages that firstly, equipment requirements are not as high as that of isostatic pressing hot pressing sintering (another hot pressing sintering mode), the process is simple, the cost is low, and meanwhile, the effect of sintering densification can be achieved. In addition, because the soft template is pressurized, the sample can be burned out to be flat by unidirectional hot-pressing sintering, and the template can be pressed into an irregular shape by isostatic pressing, so that the template cannot be used.
The high temperature sintering in step S3 has three roles: firstly, removing the soft template; erecting the sintered piezoelectric microcolumn on a substrate to form a piezoelectric ceramic microcolumn array; and thirdly, the substrate is contracted in the sintering process, so that the distance between the piezoelectric micropillars is reduced, the arrangement is more compact, and the filling proportion of the piezoelectric phase is increased.
Preferably, in step S4, the high molecular polymer is epoxy resin; the filling and curing are carried out under vacuum. Epoxy curing is carried out under the condition of vacuumizing, so that 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 required to be 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; the sample was polarized under silicone oil and room temperature conditions with an applied electric field of 3kV/mm for 30 minutes.
The invention discloses a 1-3 composite piezoelectric material for a high-frequency ultrasonic transducer, 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 a novel method for effectively preparing the high-frequency 1-3 composite piezoelectric material, has high preparation efficiency and low cost, and is beneficial to the industrial preparation and application of the 1-3 composite piezoelectric material in the technical field of high-frequency ultrasound.
2. The element content in the piezoelectric ceramic microcolumn prepared by the method is radially distributed uniformly, and the piezoelectric ceramic microcolumn has simple phase structure and complete crystal lattice. The comprehensive performance test shows that the high-frequency 1-3 composite piezoelectric material prepared by the invention has excellent piezoelectric performance in a high-frequency ultrasonic range (30-50 MHz), particularly has an electromechanical coupling coefficient of more than 61.5 percent, and is greatly improved compared with the homocomponent single-phase PZT ceramic.
3. The composite piezoelectric material provided by the invention consists of two parts, and plays a main role in 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. The piezoelectric constant d 33 of the common piezoelectric material is 600-1300 pC/N. 2) The aspect ratio (cylindrical shape), namely the common aspect ratio (long strip shape), is between 1.2 and 5, belongs to the longitudinal vibration mode, has higher electromechanical coupling coefficient (> 60%), and is not the aspect ratio of composite materials to 0.1, such as monolithic PZT ceramics, and has the electromechanical coupling coefficient of only 50%. 3) And the column spacing of the composite material prepared by a cutting filling method is generally more than 12 mu m, the preparation method can achieve more than 3 mu m, the column spacing is smaller, and compared with the column spacing, the piezoelectric constant of the composite material can be improved by 30%.
4. The invention is prepared by utilizing the soft template, so that the prepared composite piezoelectric material has the following advantages:
1) Diameter: the diameter can be made very small, at least 25 microns. Under the condition of maintaining the larger length-diameter ratio (1.2-5), the smaller the diameter, the smaller the thickness of the column (the thickness of the composite material), and the higher the frequency, the higher the resonant frequency of the composite material, namely the frequency of the material and the ultrasonic transducer can be improved, and the high frequency (30-50 MHz) can be achieved. The high frequency can be achieved only when the diameter is small enough, for example, when the traditional cutting filling method is adopted, the column is too thin and can fall down, and the high frequency requirement cannot be met only by at most 10 MHz.
2) Spacing: when the distance is small, the proportion of piezoelectric phase can be high, the piezoelectric response of the whole composite material is large, or the piezoelectric performance is good, and the piezoelectric coefficient is large. The distance which can be obtained by the traditional method is minimum of 12 microns, and the method is minimum of 3 microns, so that the piezoelectric constant of the composite material can be improved by 30% -40% compared with that of the traditional method.
3) The arrangement mode is as follows: the vibration modes among the columns can be restrained by uniform random arrangement, so that the vibration mode of the whole composite material is purer, and the signal of piezoelectric response is purer.
Drawings
FIG. 1 is a schematic flow chart of the preparation method of the present invention;
FIG. 2 is a microstructure of the 1-3 composite piezoelectric material prepared in example 1;
FIG. 3 is a graph of impedance performance versus resonant/antiresonant frequency for the 1-3 composite piezoelectric material prepared in example 1.
Detailed Description
The invention will now be described in detail with reference to the drawings and specific examples.
In the following examples, if the reagents used are not specifically described, commercially available products which can be conventionally obtained by those skilled in the art can be used. In the following examples, methods which can be conventionally understood and used by those skilled in the art may be employed if the methods used are not specifically described.
A preparation method of a 1-3 composite piezoelectric material for a high-frequency ultrasonic transducer, as shown in figure 1, comprises the following steps:
s1: preparing a soft template containing micropores through laser etching;
s2: filling micropores in the soft template obtained in the step S1 with piezoelectric ceramic powder;
s3: performing high-temperature sintering on the product obtained in the step S2 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 polymer to obtain a semi-finished product;
S5: and (3) 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 the step S1, the soft template is made of rosin, and the thickness of the soft template is 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 micropores on the soft template is 400-1000 micropores/mm 2.
In step S2, the piezoelectric ceramic powder is a perovskite 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 comprises the following sub-steps:
s21: dispersing piezoelectric ceramic powder with granularity of 1-3 mu m in an adhesive to form slurry;
S22: vacuum pouring the slurry obtained in the step S21 into micropores in the soft template obtained in the step S1, and then drying under normal pressure to form a microcolumn precursor with higher 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 500-530 ℃ at the heating rate of 50 ℃/h and is kept for 2-3h, and then heated to 1150-1200 ℃ at the same heating rate and is kept for 1.5-2h.
In the step S4, the high molecular polymer is epoxy resin; the filling curing is carried out under vacuum.
In step S5, the upper and lower surfaces of the cured composite material are thinned by grinding to keep parallel, and the substrate is also required to be 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; the sample was polarized under silicone oil and room temperature conditions with an applied electric field of 3kV/mm for 30 minutes.
Example 1
Preparing a high-uniformity 1-3 composite piezoelectric material with a microcolumn diameter of 25 mu m:
In the embodiment, lead zirconate titanate (PZT) nano powder with a quasi-homotype phase boundary component is selected as a piezoelectric phase, and the average grain diameter of the PZT is 500nm; and epoxy (Epo-Tek 301-2) was chosen as the polymer matrix.
S1: a soft template was prepared by laser etching a plastic sheet as shown in fig. 1. The thickness of the soft template was 0.5.+ -. 0.2mm and the diameter of the microwells was 25. Mu.m.
S2, filling micropores of the template by adopting powder of the PZT-5H component.
1) PZT powder having a particle size in the range of 1 to 3 μm is dispersed in a binder solution to form a PZT slurry.
2) And pouring the slurry into micropores of the plastic sheet in a vacuum environment, and drying the slurry under normal pressure to volatilize the flux, thereby forming the microcolumn precursor with higher density.
3) The template filled with PZT powder was maintained under a pressure of 6.0MPa perpendicular to the surface for 30 minutes.
S3: heating the soft template to 500 ℃ at a 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 adopting an epoxy resin polymer (Epo-Tek 301-2) to obtain the 1-3 piezoelectric composite material, as shown in figure 1. PZT powder tablets are selected as a micro-column array substrate, the density of the tablets is 3.52g/cm 3, the diameter of the tablets is 10mm, and the thickness of the tablets is 1mm. The compression of the pressed sheet in the sintering process can obviously reduce the interval between the PZT piezoelectric microposts on the pressed sheet, so that the arrangement of the PZT piezoelectric microposts is more compact. As shown in fig. 2.
S5: and (3) grinding and thinning the sample by a cutting machine, namely thinning the 1-3 composite piezoelectric material obtained by curing by a mechanical grinding machine, coarsely grinding by a 1000-mesh diamond grinding disc, and finely grinding by an alumina template to finally obtain the 1-3 composite piezoelectric material sheet with the thickness of 50 mu m. 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: the wafer was ultrasonically cleaned in alcohol, acetone, deionized water for 15 minutes, respectively, using an ultrasonic cleaner, and then dried at 50 ℃. And then coating the upper and lower surfaces of the sample with multiple layers of composite electrodes by utilizing magnetron sputtering. In this example, a nickel electrode is sputtered, then a chromium electrode is sputtered, and the thickness of the chromium electrode is controlled to be 900-1500nm as a transition electrode, and then a gold electrode is sputtered, and the thickness of the gold electrode is controlled to be 1-2 μm. The sputtering time of each layer of electrode is 10 minutes, and the surface temperature of the sample is kept below 80 ℃.
S6: the sample was polarized under silicone oil and room temperature conditions with an applied electric field of 3kV/mm for 30 minutes.
The 1-3 composites prepared were microstructural observed using an optical microscope at 1000 x magnification, as shown in fig. 2. The piezoelectric columns are arranged in order and distributed uniformly, and the diameter of each piezoelectric column is smaller and reaches 25 mu m. The average spacing between ceramic micropillars 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, which determines the electromechanical coupling performance. Therefore, the piezoelectric columns are neat and uniform, and the vibration mode interference among the columns can be consistent, so that the vibration mode is purer, and the purity of the piezoelectric signals generated and received by the piezoelectric columns is enhanced. In addition, the diameter of the column is smaller, so that the sample can be made thinner under the condition of maintaining a certain length-diameter ratio (determining the size of the electromechanical coupling performance), and then the frequency is made higher, thereby realizing high frequency. The average spacing is smaller, the proportion of the piezoelectric phase can be increased, and a larger piezoelectric constant, namely a higher piezoelectric response, is obtained.
Impedance spectrum test, according to the method for testing the performance of the piezoelectric ceramic material, namely the determination of the performance parameters (GB/T3389-2008), a precise LCR analyzer HP4284A is adopted to measure the impedance-frequency spectrum and the loss-frequency spectrum of the product. The measurement temperature was room temperature and the test frequency range was 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 the embodiment is 37.4MHz, the antiresonance frequency is 46.1MHz, and the electromechanical coupling coefficient of the high-frequency 1-3 composite piezoelectric material is 62.4% which is obviously higher than that of a PZT single-phase ceramic sheet (k t -50%) according to the "test method for the performance of piezoelectric ceramic material" measurement of performance parameters (GB/T3389-2008).
Examples 2 to 5
The preparation process was substantially the same as in example 1, except that the design dimensions of the micropores in step S1 were as 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 micropores is 120 μm.
S2, filling micropores of the template by adopting powder of the PZT-5H component.
1) PZT powder having a grain size of 1-3 μm is dispersed in a binder solution to form a PZT slurry.
2) And pouring the slurry into micropores of the plastic sheet in a vacuum environment, and drying the slurry under normal pressure to volatilize the flux, thereby forming the microcolumn precursor with higher 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 an epoxy resin polymer (Epo-Tek 301-2) to obtain the 1-3 piezoelectric composite material, as shown in figure 1. PZT powder tablets are selected as a micro-column array substrate, the density of the tablets is 3.52g/cm 3, the diameter of the tablets is 10mm, and the thickness of the tablets is 1mm.
S5, cutting the sample into different thicknesses by a cutting machine, and plating gold electrodes on the upper and lower surfaces of the sample by utilizing magnetron sputtering, as shown in figure 1. This procedure corresponds to step S5 in example 1.
S6, polarizing the sample, wherein the polarizing is performed under the conditions of silicone oil and room temperature, an applied electric field is 3kV/mm, and the polarizing 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 No. 1 corresponds to the sample prepared in example 1, sample No. 2 corresponds to the sample prepared in example 2, and so on.
The microstructure of the prepared 6 1-3 composite piezoelectric material samples is further observed 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, and the like is obtained as shown in table 1. It can be seen that the preparation method can prepare samples with any microcolumn diameter ranging from 25 μm to 120 μm for PZT ceramic microcolumn diameter; the distance range of the ceramic microcolumn which can be obtained is 3-10 mu m; the length range of the obtained PZT ceramic micro-column is 40-100 mu m; the proportion range of the ceramic phase of the 1-3 composite piezoelectric material is 43-55%; the resonance frequency that can be achieved can be higher than 35MHz, and the maximum antiresonance frequency in the sample reaches 46.1MHz. After the composite material is used to fabricate an ultrasonic transducer, one important parameter of the transducer is the center frequency, which is determined by both the resonant and anti-resonant frequencies of the composite material. The higher the resonant, antiresonant frequency of the material, the higher the center frequency of the transducer. In combination with the test data in table 1, it can be seen that the center frequency of the material prepared by the method provided by the invention can reach high frequency after the ultrasonic transducer is further prepared.
In addition, the electromechanical coupling coefficient is distributed between 61-71% at high frequency (-40 MHz) and is far higher than 50-55% of that of a PZT ceramic single chip, so that the method has the advantages of larger electromechanical coupling performance and is beneficial to improving the performance of the high-frequency ultrasonic transducer.
The previous description of the embodiments is provided to facilitate a person of ordinary skill in the art in order to make and use the present invention. It will be apparent to those skilled in the art that various modifications can be readily made to these embodiments 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-described embodiments, and those skilled in the art, based on the present disclosure, should make improvements and modifications without departing from the scope of the present invention.
Claims (8)
1. The preparation method of the 1-3 composite piezoelectric material for the high-frequency ultrasonic transducer is characterized by comprising the following steps of:
s1: preparing a soft template containing micropores by an etching technology;
s2: filling micropores in the soft template obtained in the step S1 with piezoelectric ceramic powder;
s3: performing high-temperature sintering on the product obtained in the step S2 to remove the soft template, so as to obtain a piezoelectric ceramic column array; the high-temperature sintering is unidirectional hot-pressing sintering, and the product obtained in the step S2 is pressed and sintered to shrink in the sintering process;
S4: filling and curing the piezoelectric ceramic column array obtained in the step S3 by using a high polymer to obtain a semi-finished product;
S5: 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 the step S1, the etching technology 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 micropores on the soft template is 400-1000 micropores/mm 2;
In step S3, the high temperature sintering includes the following steps: the soft template is heated to 500-530 ℃ at the heating rate of 50 ℃/h and is kept for 2-3h, and then heated to 1150-1200 ℃ at the same heating rate and is kept for 1.5-2h.
2. 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 perovskite structure ferroelectric powder.
3. The method for preparing a 1-3 composite piezoelectric material for a high-frequency ultrasonic transducer according to claim 2, 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 bismuth sodium titanate-barium titanate.
4. 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 filling comprises the steps of:
S21: dispersing piezoelectric ceramic powder in an adhesive to form slurry;
s22: vacuum pouring the slurry obtained in the step S21 into micropores in the soft template obtained in the step S1, and then drying under normal pressure to form a microcolumn precursor;
s23: and (2) applying pressure vertical to the surface to the micro-column precursor obtained in the step S22.
5. The method of manufacturing a 1-3 composite piezoelectric material for a high frequency ultrasonic transducer according to claim 4, wherein in step S21, the adhesive is acrylamide.
6. The method of manufacturing a 1-3 composite piezoelectric material for a high frequency ultrasonic transducer according to claim 4, wherein in step S23, the pressure is 6.0MPa and the holding time is 30min.
7. 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 epoxy resin; the filling and curing are carried out under vacuum.
8. A 1-3 composite piezoelectric material for a high-frequency ultrasonic transducer, which is prepared by the preparation method of the 1-3 composite piezoelectric material for the high-frequency ultrasonic transducer according to any one of claims 1-7.
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| CN101255265A (en) * | 2008-04-11 | 2008-09-03 | 清华大学 | Leadless piezoelectric ceramics/polymer 1-3 structure composite material and method for processing same |
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