CN117560986A - 1-3 type texture piezoelectric ceramic composite material, preparation method and application thereof - Google Patents
1-3 type texture piezoelectric ceramic composite material, preparation method and application thereof Download PDFInfo
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- CN117560986A CN117560986A CN202311528815.2A CN202311528815A CN117560986A CN 117560986 A CN117560986 A CN 117560986A CN 202311528815 A CN202311528815 A CN 202311528815A CN 117560986 A CN117560986 A CN 117560986A
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- 239000000919 ceramic Substances 0.000 title claims abstract description 238
- 239000002131 composite material Substances 0.000 title claims abstract description 128
- 238000002360 preparation method Methods 0.000 title abstract description 15
- 229910052451 lead zirconate titanate Inorganic materials 0.000 claims abstract description 112
- 238000005520 cutting process Methods 0.000 claims abstract description 57
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims abstract description 46
- 229910052749 magnesium Inorganic materials 0.000 claims abstract description 46
- 239000011777 magnesium Substances 0.000 claims abstract description 46
- 238000000034 method Methods 0.000 claims abstract description 44
- 239000003822 epoxy resin Substances 0.000 claims abstract description 43
- 229920000647 polyepoxide Polymers 0.000 claims abstract description 43
- 229920000642 polymer Polymers 0.000 claims abstract description 21
- 238000004140 cleaning Methods 0.000 claims abstract description 13
- 238000001035 drying Methods 0.000 claims abstract description 13
- 239000000084 colloidal system Substances 0.000 claims abstract description 11
- 238000005498 polishing Methods 0.000 claims abstract description 9
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000011248 coating agent Substances 0.000 claims abstract description 7
- 238000000576 coating method Methods 0.000 claims abstract description 7
- 238000001755 magnetron sputter deposition Methods 0.000 claims abstract description 7
- 238000004519 manufacturing process Methods 0.000 claims abstract description 7
- 229910052709 silver Inorganic materials 0.000 claims abstract description 7
- 239000004332 silver Substances 0.000 claims abstract description 7
- 229910010293 ceramic material Inorganic materials 0.000 claims description 21
- 239000000758 substrate Substances 0.000 claims description 19
- 229910052738 indium Inorganic materials 0.000 claims description 15
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 claims description 15
- 229910052727 yttrium Inorganic materials 0.000 claims description 15
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 claims description 15
- JQJCSZOEVBFDKO-UHFFFAOYSA-N lead zinc Chemical compound [Zn].[Pb] JQJCSZOEVBFDKO-UHFFFAOYSA-N 0.000 claims description 11
- 229920005989 resin Polymers 0.000 claims description 8
- 239000011347 resin Substances 0.000 claims description 8
- 238000003491 array Methods 0.000 claims description 6
- 238000011049 filling Methods 0.000 claims description 5
- 239000004593 Epoxy Substances 0.000 claims description 2
- 230000008878 coupling Effects 0.000 abstract description 24
- 238000010168 coupling process Methods 0.000 abstract description 24
- 238000005859 coupling reaction Methods 0.000 abstract description 24
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 8
- 239000013078 crystal Substances 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- 238000003756 stirring Methods 0.000 description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- 230000001276 controlling effect Effects 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000000741 silica gel Substances 0.000 description 3
- 229910002027 silica gel Inorganic materials 0.000 description 3
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 238000003475 lamination Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
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- H10N—ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N30/00—Piezoelectric or electrostrictive devices
- H10N30/80—Constructional details
- H10N30/85—Piezoelectric or electrostrictive active materials
- H10N30/852—Composite materials, e.g. having 1-3 or 2-2 type connectivity
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01H—MEASUREMENT OF MECHANICAL VIBRATIONS OR ULTRASONIC, SONIC OR INFRASONIC WAVES
- G01H11/00—Measuring mechanical vibrations or ultrasonic, sonic or infrasonic waves by detecting changes in electric or magnetic properties
- G01H11/06—Measuring mechanical vibrations or ultrasonic, sonic or infrasonic waves by detecting changes in electric or magnetic properties by electric means
- G01H11/08—Measuring mechanical vibrations or ultrasonic, sonic or infrasonic waves by detecting changes in electric or magnetic properties by electric means using piezoelectric devices
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N—ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N30/00—Piezoelectric or electrostrictive devices
- H10N30/01—Manufacture or treatment
- H10N30/09—Forming piezoelectric or electrostrictive materials
- H10N30/092—Forming composite materials
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N—ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N30/00—Piezoelectric or electrostrictive devices
- H10N30/30—Piezoelectric or electrostrictive devices with mechanical input and electrical output, e.g. functioning as generators or sensors
- H10N30/302—Sensors
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Abstract
A1-3 texture piezoelectric ceramic composite material, a preparation method and application thereof, comprises a textured piezoelectric ceramic phase of lead magnesium niobate-lead zirconate titanate with perovskite structure which is communicated in one dimension and an epoxy resin polymer phase which is arranged in parallel in three dimension; the preparation method comprises the following steps: firstly, obtaining a ceramic strip array, then cutting to obtain a lead magnesium niobate-lead zirconate titanate texture piezoelectric ceramic column array, injecting epoxy resin colloid for treatment to obtain a lead magnesium niobate-lead zirconate titanate texture piezoelectric ceramic epoxy resin composite material, polishing, ultrasonically cleaning and drying, and preparing a conductive layer on the surface of the texture piezoelectric ceramic composite material by adopting silver paste coating or rotary magnetron sputtering to obtain a 1-3 texture piezoelectric ceramic composite material; application of 1-3 type texture piezoelectric ceramic composite material for preparing underwater acoustic transducer; the invention has the characteristics of high piezoelectric performance, high coupling coefficient, small dielectric loss, simple process, mass production and low cost.
Description
Technical Field
The invention relates to the technical field of composite materials, in particular to a 1-3 type texture piezoelectric ceramic composite material, a preparation method and application thereof.
Background
The 1-3 type piezoelectric composite material consists of one-dimensional communicated piezoelectric ceramic phase and three-dimensional communicated polymer phase arranged in parallel. The piezoelectric phase of the common 1-3 type piezoelectric composite material is PZT ceramic and single crystal, the common preparation technology comprises an arrangement pouring method, a cutting filling method, a demolding method, an injection method, a casting lamination method, a dielectric medium method, an extrusion method, a laser ultrasonic cutting method and the like, and the piezoelectric constant of the 1-3 type composite material made of PZT ceramic is generally lower than 500pC/N and the electromechanical coupling coefficient k t Less than 0.6, the PZT is difficult to meet along with the improvement of the sensitivity and resolution requirements of the transducer, so the piezoelectric transducer has low piezoelectric performance and low electromechanical coupling coefficient; for high-performance monocrystalline materials, the utilization rate of the monocrystalline rod is less than 40%, the price is high, and meanwhile, the cutting loss exists in the process of manufacturing the 1-3 type composite material, so that the cost is high, and mass production is difficult.
In recent years, with the rapid development of the textured piezoelectric ceramics, the piezoelectric performance and the electromechanical coupling performance of the textured piezoelectric ceramics have great advantages (such as longitudinal piezoelectric coefficient d) 33 The thickness of the ceramic composite material is 2-3 times of that of the common ceramic composite material, and the electromechanical coupling k is thick t The improvement is about 10% -30%), and the textured piezoelectric ceramic is formed by arranging ceramic grains in an oriented way through a specific process.
However, the above prior art has the following disadvantages: 1) The piezoelectric phase is mostly made of common ceramics, and the comprehensive performance of the random oriented common ceramics is generally low; 2) The single crystal has excellent piezoelectric performance, is subject to the growth size and the in-chip uniformity of the single crystal material, has high cost and is difficult to realize mass production.
Bulletin No. CN 116744769A]The patent application of (1-3) type piezoelectric ceramic composite material, a preparation method and application thereof are disclosed, wherein the composite material comprises an array formed by ceramic columns and polymers, namely, the periphery of the ceramic columns is sequentially provided with an epoxy resin layer and a silica gel layer, the epoxy resin layer and the silica gel layer form soft and hard polymers, and the thickness vibration mode and the transverse vibration mode are regulated and controlled by the soft and hard polymers so as to couple the ceramic columns and promote the electromechanical coupling coefficient; the preparation method adopts a cutting filling method: firstly, cutting ceramic into a ceramic skeleton once, pouring epoxy resin into a primary cutting gap, performing secondary cutting in the primary cutting gap, pouring silica gel into the secondary cutting gap, curing, and polishing to expose a ceramic phase; the composite material can be applied to underwater acoustic transducers, and can expand the bandwidth and improve the performance parameters of resolution. Due to the electromechanical coupling coefficient k of the common piezoelectric ceramics 33 Low, typically about 0.7, and the electromechanical coupling coefficient of the composite material of 1-3 will be higher than k 33 Low, and therefore has the disadvantage that the electromechanical coupling coefficient of the composite material thus produced is not higher than 0.7.
Disclosure of Invention
In order to overcome the disadvantages of the prior art, the present invention aims to provide a 1-3 type texture piezoelectric ceramic composite material, a preparation method and application thereof, which is prepared by combining a ceramic material with a high electromechanical coupling coefficient (k 33 About 0.9) and a high piezoelectric constant (d) 33 1008 pC/N) to prepare 1-3 type texture piezoelectric ceramic composite material, the piezoelectric performance is about twice higher than that of the common piezoelectric ceramic composite material, the cost is only half of that of the single crystal composite material, and the electromechanical coupling coefficient k t Greater than 0.8; therefore, the piezoelectric ceramic has the characteristics of high piezoelectric performance, high electromechanical coupling coefficient, small dielectric loss, simple process, mass production and low cost.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
a1-3 texture piezoelectric ceramic composite material comprises a textured piezoelectric ceramic phase 3 of lead magnesium niobate-lead zirconate titanate with a perovskite structure which is communicated in one dimension and an epoxy resin polymer phase 4 which is communicated in three dimensions in parallel.
The textured piezoelectric ceramic phase 3 of the lead magnesium niobate-lead zirconate titanate accounts for 10-90% of the volume fraction of the textured piezoelectric ceramic composite material, and the epoxy resin polymer phase 4 accounts for 90-10% of the volume fraction of the textured piezoelectric ceramic composite material.
The textured piezoelectric ceramic phase of the lead magnesium niobate-lead zirconate titanate accounts for 56% of the volume of the textured piezoelectric ceramic composite material, and the epoxy resin polymer phase accounts for 44% of the volume of the textured piezoelectric ceramic composite material.
The textured piezoelectric ceramic phase of lead magnesium niobate-lead zirconate titanate with perovskite structure can also be textured piezoelectric ceramic of lead zinc niobate-lead zirconate titanate (PZN-PZT) or textured piezoelectric ceramic of lead indium niobate-lead zirconate titanate (PIN-PZT) or textured piezoelectric ceramic of lead yttrium niobate-lead zirconate titanate (PYN-PZT).
A preparation method of a 1-3 type texture piezoelectric ceramic composite material comprises the following steps:
step 1, cutting a lead magnesium niobate-lead zirconate titanate textured piezoelectric ceramic material block along a first direction, and reserving the lead magnesium niobate-lead zirconate titanate textured piezoelectric ceramic material with required thickness as a substrate 1 to obtain a ceramic strip array 2;
step 2, cutting the ceramic strip array obtained in the step 1 along a second direction, ultrasonically cleaning the array after cutting, and drying to obtain a plurality of mutually independent lead magnesium niobate-lead zirconate titanate texture piezoelectric ceramic column arrays 3; the second direction is on the same plane as the first direction, and the second direction is perpendicular to the first direction;
step 3, injecting epoxy resin colloid into the lead magnesium niobate-lead zirconate titanate texture piezoelectric ceramic column array 3 prepared in the step 2, filling cutting gaps, and curing at room temperature after removing bubbles in vacuum to obtain a lead magnesium niobate-lead zirconate titanate texture piezoelectric ceramic epoxy resin composite material;
polishing the lead magnesium niobate-lead zirconate titanate textured piezoelectric ceramic epoxy resin composite material prepared in the step 3, and removing redundant resin on the upper surface and the lower surface and the lead magnesium niobate-lead zirconate titanate textured piezoelectric ceramic substrate 1 to expose ceramic columns;
and 5, ultrasonically cleaning and drying the ceramic piezoelectric composite material prepared in the step 4, and preparing a conductive layer on the surface of the textured piezoelectric ceramic composite material by adopting 80-150 ℃ curing silver paste coating or rotary magnetron sputtering to obtain the 1-3 textured piezoelectric ceramic composite material.
And in the step 1, the cutting step length is the width of the ceramic column plus the width of the kerf.
The thickness of the substrate 1 in the step 1 is 1/3-1/5 of the cutting depth.
The cutting depth in the step 2 is the same as that in the step 1, and the cutting depth is 0.3-0.6 mm higher than that of the final 1-3 type texture piezoelectric ceramic composite material.
In the step 4, the sum of the width of the ceramic column and the width of the cutting gap in the step 1 is the transverse period size of the composite material, and the ratio of the final thickness of the polished ceramic composite material to the transverse period size is 2.5-3.5.
An application of a 1-3 type texture piezoelectric ceramic composite material is used for preparing an underwater acoustic transducer.
Compared with the prior art, the invention has the beneficial effects that:
1. the 1-3 texture piezoelectric ceramic composite material prepared by the invention has high piezoelectric performance (d) due to the adoption of the lead magnesium niobate-lead zirconate titanate texture piezoelectric ceramic 33 About 1000 pC/N/-1200 pC/N) and electromechanical coupling coefficient (k) t 0.9), high electromechanical conversion efficiency; the invention improves the electromechanical coupling coefficient of the thickness to the longitudinal electromechanical coupling coefficient k by the ratio of the final thickness of the polished ceramic composite material to the transverse period size being approximately equal to 2.5-3.5 33 Compared with the traditional piezoelectric ceramic composite material, the performance of the piezoelectric ceramic composite material is improved by about 2 times, and a new opportunity is provided for the next-generation piezoelectric transducer.
2. The invention adopts the electromechanical coupling coefficient (k) with high thickness vibration mode 33 0.9) and high voltage electrical constant ((d) 33 1008 pC/N) texture piezoelectric ceramic, preparing a 1-3 texture piezoelectric ceramic composite material, reasonably designing the aspect ratio of the ceramic column, and obtaining pure thickness vibration mode and polymer phaseThe acoustic impedance is low, so that the electromechanical coupling performance can be effectively improved, the energy conversion efficiency is improved, the range of the resonant frequency and the antiresonant frequency is widened, the acoustic impedance is reduced, and the acoustic impedance has advantages when the acoustic impedance is applied to devices such as an underwater acoustic transducer; the invention overcomes the defects that the traditional common ceramic composite material has low performance, the piezoelectric monocrystal composite material is difficult to achieve consistency and the price is high.
3. The 1-3 type texture piezoelectric ceramic composite material is prepared by adopting a cutting filling method, the working procedure is simple, the cutting parameters can be accurately controlled, the process stability is high, and the repeatability of a finished product is good.
In summary, the present invention is achieved by providing a high electromechanical coupling coefficient (k 33 0.9) and high voltage electrical constant ((d) 33 1008 pC/N) to prepare 1-3 type texture piezoelectric ceramic composite material, the piezoelectric performance is about twice higher than that of the common piezoelectric ceramic composite material, the cost is only half of that of the single crystal composite material, and the electromechanical coupling coefficient k t Greater than 0.8; therefore, the piezoelectric ceramic has the characteristics of high piezoelectric performance, high coupling coefficient, small dielectric loss, simple process, mass production and low cost.
Drawings
FIG. 1 is a flow chart of the preparation method of the invention.
In the figure, 1 is a base, 2 is a ceramic strip array, 3 is a textured piezoelectric ceramic phase, and 4 is an epoxy polymer phase.
Detailed Description
The invention will be described in detail with reference to the accompanying drawings.
Example 1
A1-3 texture piezoelectric ceramic composite material comprises a textured piezoelectric ceramic phase 3 of lead magnesium niobate-lead zirconate titanate with a perovskite structure which is communicated in one dimension and an epoxy resin polymer phase 4 which is communicated in three dimensions in parallel.
The textured piezoelectric ceramic phase 3 of lead magnesium niobate-lead zirconate titanate with perovskite structure is a textured piezoelectric ceramic with high orientation degree prepared by a template grain growth method of ceramics and devices, and the preferential orientation growth of grains is controlled to obviously improve the hardness ceramicPiezoelectric and electromechanical properties, while maintaining low loss of hard ceramics, piezoelectric constants up to 1000pC/N, relative dielectric constants 2100, k 33 Up to 0.9.
The textured piezoelectric ceramic phase 3 of the lead magnesium niobate-lead zirconate titanate accounts for 56% of the volume of the textured piezoelectric ceramic composite material, and the epoxy resin polymer phase 4 accounts for 44% of the volume of the textured piezoelectric ceramic composite material.
Referring to fig. 1, a preparation method of a 1-3 type texture piezoelectric ceramic composite material comprises the following steps:
step 1, cutting a lead magnesium niobate-lead zirconate titanate texture piezoelectric ceramic material block along a first direction, and reserving the lead magnesium niobate-lead zirconate titanate texture piezoelectric ceramic material with the thickness of 0.7mm, namely 1/4 of the cutting depth as a substrate 1 to obtain a ceramic strip array 2, wherein the actual required height of the 1-3 type texture piezoelectric ceramic composite material based on the lead magnesium niobate-lead zirconate titanate texture piezoelectric ceramic material is 2.2mm, the cutting depth of the ceramic strip array is 2.8mm, the section width is 0.54 x 0.54, and the ceramic substrate with the thickness of 0.7mm is reserved, so that the texture piezoelectric ceramic strip can be prevented from being broken; the kerf width is 0.18mm, and the cutting speed is about 1.5mm/min so as to ensure the integrity of the cut lead magnesium niobate-lead zirconate titanate texture piezoelectric ceramic array;
step 2, cutting the ceramic strip array 2 obtained in the step 1 along a second direction, ultrasonically cleaning the array after cutting, and drying to obtain a plurality of mutually independent lead magnesium niobate-lead zirconate titanate texture piezoelectric ceramic column arrays 3; the second direction is on the same plane as the first direction, and the second direction is perpendicular to the first direction;
step 3, pouring epoxy resin colloid into the lead magnesium niobate-lead zirconate titanate texture piezoelectric ceramic column array 3 prepared in the step 2, and pouring from the same position of a die and slowing down the resin pouring speed in the pouring process, so that the generation of bubbles in the pouring process can be effectively reduced, cutting gaps are filled, and the lead magnesium niobate-lead zirconate titanate texture piezoelectric ceramic epoxy resin composite material is obtained after the bubbles are removed in vacuum and solidified at room temperature; the epoxy resin colloid added during pouring is required to be stirred firstly, and is placed into a vacuum box for vacuumizing after being stirred uniformly so as to remove bubbles generated in the stirring process;
polishing the lead magnesium niobate-lead zirconate titanate textured piezoelectric ceramic epoxy resin composite material prepared in the step 3, and removing redundant epoxy resin and lead magnesium niobate-lead zirconate titanate textured piezoelectric ceramic substrate 1 on the upper surface and the lower surface to expose ceramic columns;
and 5, cleaning the lead magnesium niobate-lead zirconate titanate ceramic piezoelectric composite material prepared in the step 4 with ethanol under the condition of ultrasonic vibration for 3min, drying, and preparing a conductive layer on the surface of the textured piezoelectric ceramic composite material by adopting a 80 ℃ curing silver paste coating or rotary magnetron sputtering method to obtain the 1-3 hard textured piezoelectric ceramic composite material.
An application of a 1-3 type texture piezoelectric ceramic composite material is used for preparing an underwater acoustic transducer.
Example 2
A1-3 texture piezoelectric ceramic composite material comprises a one-dimensional communicated textured piezoelectric ceramic phase 3 of lead zincate niobate-lead zirconate titanate with perovskite structure and an epoxy resin polymer phase 4 which is arranged in parallel in three-dimensional communication.
The textured piezoelectric ceramic phase 3 of lead zinc niobate-lead zirconate titanate with perovskite structure is a textured piezoelectric ceramic with high orientation degree prepared by a template grain growth method of ceramic and device, the piezoelectric and electromechanical properties of the hard ceramic are obviously improved by controlling the preferred orientation growth of grains, meanwhile, the low loss of the hard ceramic is maintained, the piezoelectric constant is as high as 900pC/N, and the relative dielectric constant is 2500, k 33 Up to 0.9.
The textured piezoelectric ceramic phase 3 of the lead zinc niobate-lead zirconate titanate accounts for 10 percent of the volume fraction of the textured piezoelectric ceramic composite material, and the epoxy resin polymer phase 4 accounts for 90 percent of the volume fraction of the textured piezoelectric ceramic composite material.
A preparation method of a 1-3 type texture piezoelectric ceramic composite material comprises the following steps:
step 1, cutting a lead zinc niobate-lead zirconate titanate texture piezoelectric ceramic material block along a first direction, reserving a lead zinc niobate-lead zirconate titanate texture piezoelectric ceramic material with the thickness of 0.6mm as a substrate 1 to obtain a ceramic strip array 2, wherein the actual required height of the 1-3 type texture piezoelectric ceramic composite material based on the lead zinc niobate-lead zirconate titanate texture piezoelectric ceramic is 2.0mm, and the cutting depth of the ceramic strip array is 2.4mm, the section width is 0.22 x 0.22, and reserving a ceramic substrate with the thickness of the lead zinc niobate-lead zirconate titanate texture piezoelectric ceramic material with the thickness of 0.6mm to prevent the texture piezoelectric ceramic strip from being broken; the kerf width is 0.44mm, and the cutting speed is about 1.5mm/min so as to ensure the integrity of the cut lead magnesium niobate-lead zirconate titanate texture piezoelectric ceramic array;
step 2, cutting the ceramic strip array 2 obtained in the step 1 along a second direction, ultrasonically cleaning the array after cutting, and drying to obtain a plurality of mutually independent lead zinc niobate-lead zirconate titanate texture piezoelectric ceramic column arrays 3; the second direction is on the same plane as the first direction, and the second direction is perpendicular to the first direction;
step 3, pouring epoxy resin colloid into the lead zinc niobate-lead zirconate titanate texture piezoelectric ceramic column array 3 prepared in the step 2, and pouring from the same position of a die and slowing down the resin pouring speed in the pouring process, so that the generation of bubbles in the pouring process can be effectively reduced, cutting gaps are filled, and the lead zinc niobate-lead zirconate titanate texture piezoelectric ceramic epoxy resin composite material is obtained after the bubbles are removed in vacuum and solidified at room temperature; the epoxy resin colloid added during pouring is required to be stirred firstly, and is placed into a vacuum box for vacuumizing after being stirred uniformly so as to remove bubbles generated in the stirring process;
polishing the lead zincate niobate-lead zirconate titanate textured piezoelectric ceramic epoxy resin composite material prepared in the step 3, and removing redundant epoxy resin and lead zincate niobate-lead zirconate titanate textured piezoelectric ceramic substrate 1 on the upper surface and the lower surface to expose ceramic columns;
and 5, cleaning the lead niobate zincate-lead zirconate titanate ceramic piezoelectric composite material prepared in the step 4 with ethanol under the condition of ultrasonic vibration for 5min, drying, and preparing a conductive layer on the surface of the textured piezoelectric ceramic composite material by adopting a 150 ℃ curing silver paste coating or rotating magnetron sputtering method to obtain the 1-3 hard textured piezoelectric ceramic composite material.
An application of a 1-3 type texture piezoelectric ceramic composite material is used for preparing an underwater acoustic transducer.
Example 3
A1-3 texture piezoelectric ceramic composite material comprises a textured piezoelectric ceramic phase 3 of lead indium niobate-lead zirconate titanate with a perovskite structure which is communicated in one dimension and an epoxy resin polymer phase 4 which is arranged in parallel in three dimensions.
The textured piezoelectric ceramic phase 3 of the lead indium niobate-lead zirconate titanate with perovskite structure is textured piezoelectric ceramic with high orientation degree prepared by a template grain growth method of ceramics and devices, the piezoelectric and electromechanical properties of the hard ceramic are obviously improved by controlling the preferred orientation growth of grains, meanwhile, the low loss of the hard ceramic is maintained, the piezoelectric constant is as high as 1200pC/N, and the relative dielectric constant is 3000, k 33 Up to 0.92.
The textured piezoelectric ceramic phase 3 of the lead indium niobate-lead zirconate titanate accounts for 30% of the volume of the textured piezoelectric ceramic composite material, and the epoxy resin polymer phase 4 accounts for 70% of the volume of the textured piezoelectric ceramic composite material.
A preparation method of a 1-3 type texture piezoelectric ceramic composite material comprises the following steps:
step 1, cutting a lead indium niobate-lead zirconate titanate texture piezoelectric ceramic material block along a first direction, reserving the lead indium niobate-lead zirconate titanate texture piezoelectric ceramic material with the thickness of 0.6mm as a substrate 1 to obtain a ceramic strip array 2, wherein the actual required height of the 1-3 type texture piezoelectric ceramic composite material based on the lead indium niobate-lead zirconate titanate texture piezoelectric ceramic material is 1.8mm, and the cutting depth of the ceramic strip array is 2.3mm, the section width is 0.33 x 0.33, and reserving the lead indium niobate-lead zirconate titanate texture piezoelectric ceramic material with the thickness of 0.6mm as the substrate to prevent the texture piezoelectric ceramic strip from being broken; the kerf width is 0.27mm, and the cutting speed is about 1.5mm/min so as to ensure the integrity of the cut lead magnesium niobate-lead zirconate titanate texture piezoelectric ceramic array;
step 2, cutting the ceramic strip array 2 obtained in the step 1 along a second direction, ultrasonically cleaning the array after cutting, and drying to obtain a plurality of mutually independent lead indium niobate-lead zirconate titanate texture piezoelectric ceramic column arrays 3; the second direction is on the same plane as the first direction, and is vertical to the first direction, and after cutting is completed, the array is ultrasonically cleaned and dried;
step 3, pouring epoxy resin colloid into the lead indium niobate-lead zirconate titanate texture piezoelectric ceramic column array 3 prepared in the step 2, and pouring from the same position of a die and slowing down the resin pouring speed in the pouring process, so that the generation of bubbles in the pouring process can be effectively reduced, cutting gaps are filled, and the lead indium niobate-lead zirconate titanate texture piezoelectric ceramic epoxy resin composite material is obtained after the bubbles are removed in vacuum and solidified at room temperature; the epoxy resin colloid added during pouring is required to be stirred firstly, and is placed into a vacuum box for vacuumizing after being stirred uniformly so as to remove bubbles generated in the stirring process;
polishing the lead indium niobate-lead zirconate titanate textured piezoelectric ceramic epoxy resin composite material prepared in the step 3, and removing redundant resin on the upper surface and the lower surface and the lead indium niobate-lead zirconate titanate textured piezoelectric ceramic substrate 1 to expose ceramic columns;
and 5, cleaning the lead indium niobate-lead zirconate titanate textured piezoelectric ceramic composite material prepared in the step 4 with ethanol under the condition of ultrasonic vibration for 4min, drying, and preparing a conductive layer on the surface of the textured piezoelectric ceramic composite material by adopting a 100 ℃ curing silver paste coating or rotating magnetron sputtering method to obtain the 1-3 hard textured piezoelectric ceramic composite material.
An application of a 1-3 type texture piezoelectric ceramic composite material is used for preparing an underwater acoustic transducer.
Example 4
A1-3 texture piezoelectric ceramic composite material comprises a textured piezoelectric ceramic phase 3 of lead yttrium niobate-lead zirconate titanate with a perovskite structure which is communicated in one dimension and an epoxy resin polymer phase 4 which is communicated in three dimensions in parallel.
The textured piezoelectric ceramic phase 3 of lead yttrium niobate-lead zirconate titanate with perovskite structure is a textured piezoelectric ceramic with high orientation degree prepared by a template grain growth method of ceramics and devices, the piezoelectric and electromechanical properties of hard ceramics are obviously improved by controlling the preferred orientation growth of grains, and meanwhile, the hardness is also maintainedLow loss, piezoelectric constant up to 800pC/N, relative dielectric constant 2100, k of ceramic 33 Up to 0.89.
The textured piezoelectric ceramic phase 3 of the lead yttrium niobate-lead zirconate titanate accounts for 64% of the volume of the textured piezoelectric ceramic composite material, and the epoxy resin polymer phase 4 accounts for 36% of the volume of the textured piezoelectric ceramic composite material.
A preparation method of a 1-3 type texture piezoelectric ceramic composite material comprises the following steps:
step 1, cutting a lead yttrium niobate-lead zirconate titanate texture piezoelectric ceramic material block along a first direction, reserving a lead yttrium niobate-lead zirconate titanate texture piezoelectric ceramic material with the thickness of 0.5mm as a substrate 1 to obtain a ceramic strip array 2, wherein the actual required height of the 1-3 type texture piezoelectric ceramic composite material based on the lead yttrium niobate-lead zirconate titanate texture piezoelectric ceramic material is 1.8mm, and the cutting depth of the ceramic strip array is 2.0mm and the section width is 0.36 x 0.36, and reserving a ceramic substrate with a certain thickness to prevent the texture piezoelectric ceramic strip from being broken; the kerf width is 0.24mm, and the cutting speed is about 1.5mm/min so as to ensure the integrity of the cut lead yttrium niobate-lead zirconate titanate texture piezoelectric ceramic array;
step 2, cutting the ceramic strip array 2 obtained in the step 1 along a second direction, ultrasonically cleaning the array after cutting, and drying to obtain a plurality of mutually independent lead yttrium niobate-lead zirconate titanate texture piezoelectric ceramic column arrays 3; the second direction is on the same plane as the first direction, and is vertical to the first direction, and after cutting is completed, the array is ultrasonically cleaned and dried;
step 3, pouring epoxy resin colloid into the lead yttrium niobate-lead zirconate titanate texture piezoelectric ceramic column array prepared in the step 2, and pouring from the same position of a die and slowing down the resin pouring speed in the pouring process, so that the generation of bubbles in the pouring process can be effectively reduced, cutting gaps are filled, and the lead yttrium niobate-lead zirconate titanate texture piezoelectric ceramic epoxy resin composite material is obtained after the bubbles are removed in vacuum and solidified at room temperature; the epoxy resin colloid added during pouring is required to be stirred firstly, and is placed into a vacuum box for vacuumizing after being stirred uniformly so as to remove bubbles generated in the stirring process;
polishing the lead yttrium niobate-lead zirconate titanate textured piezoelectric ceramic epoxy resin composite material prepared in the step 3, and polishing redundant resin and lead yttrium niobate-lead zirconate titanate ceramic substrates on the upper surface and the lower surface to expose ceramic columns;
and 5, cleaning the lead yttrium niobate-lead zirconate titanate ceramic piezoelectric composite material prepared in the step 4 with ethanol under the condition of ultrasonic vibration for 4.5min, drying, and preparing a conductive layer on the surface of the textured piezoelectric ceramic composite material by adopting a 120 ℃ curing silver paste coating or rotating magnetron sputtering method to obtain the 1-3 hard textured piezoelectric ceramic composite material.
An application of a 1-3 type texture piezoelectric ceramic composite material is used for preparing an underwater acoustic transducer.
The main properties of the hard textured piezoelectric ceramic used in the present invention and the 1-3 type piezoelectric composite material prepared were measured by the following methods.
The relative dielectric constant and dielectric loss of the lead magnesium niobate-lead zirconate titanate PMN-PZT hard texture piezoelectric ceramic and the prepared 1-3 piezoelectric composite material are measured 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 tester (E4980 AL, keysight, USA) is adopted, the dielectric constant is obtained through measurement by the capacitance of the product, the test frequency is 1kHz, the PMN-PZT texture piezoelectric ceramic and the piezoelectric constant of the prepared 1-3 piezoelectric composite material are tested according to the method for testing the performance parameters of the piezoelectric ceramic material, namely the determination of the performance parameters (GB/T3389-2008), a quasi-static d is adopted, and a testing instrument is ZJ-3A type of the acoustic development of China academy of sciences 33 A tester; the PMN-PZT hard texture piezoelectric ceramic and the resonance frequency and anti-resonance frequency of the prepared 1-3 piezoelectric composite material are measured by a precision impedance analyzer (E4990A, keysight, USA), and the thickness mechanical coefficient (k) can be calculated according to the method for testing the performance of the piezoelectric ceramic material, the measurement of the performance parameters (GB/T3389-2008) t ) The calculation formula is as follows:
the results of the performance test of the lead magnesium niobate-lead zirconate titanate PMN-PZT hard texture material and the 1-3 type piezoelectric composite material prepared by using the same as a piezoelectric substrate are shown in Table 1.
TABLE 1
As can be seen from Table 1, when the volume fraction of the lead magnesium niobate-lead zirconate titanate PMN-PZT textured piezoelectric ceramic is 1,1-3 textured piezoelectric composite material, the volume fraction of the lead magnesium niobate-lead zirconate titanate PMN-PZT textured piezoelectric ceramic is 0.55, and the piezoelectric constant d of the PMN-PZT textured piezoelectric ceramic is the same 33 Piezoelectric constant d of 1008,1-3 texture piezoelectric composite material 33 730, the electromechanical coupling coefficient of the PMN-PZT textured piezoelectric ceramic is 0.9 (k) 33 ) The electromechanical coupling coefficient of the 1-3 type texture piezoelectric composite material is 0.8 (k) t ) Relative dielectric constant epsilon of PMN-PZT textured piezoelectric ceramic r Relative dielectric constant epsilon of 2100,1-3 texture piezoelectric composite material r For 1122, the dielectric loss tan delta of the PMN-PZT textured piezoelectric ceramic was 0.25% and the dielectric loss tan delta of the 1-3 textured piezoelectric composite material was 1.07%, it can be seen that the lead magnesium niobate-lead zirconate titanate PMN-PZT textured piezoelectric ceramic has high piezoelectric performance and high longitudinal electromechanical coupling coefficient, and the 1-3 textured piezoelectric composite material based on the PMN-PZT textured piezoelectric ceramic has high piezoelectric constant d 33 And a high electromechanical coupling coefficient k t Is far higher than 1-3 type piezoelectric composite materials prepared by common ceramics.
Claims (10)
1. The 1-3 texture piezoelectric ceramic composite material is characterized by comprising a textured piezoelectric ceramic phase (3) of lead magnesium niobate-lead zirconate titanate with a perovskite structure which is communicated in one dimension and an epoxy resin polymer phase (4) which is communicated in three dimensions and is arranged in parallel.
2. The 1-3 textured piezoelectric ceramic composite material according to claim 1, wherein the textured piezoelectric ceramic phase (3) of lead magnesium niobate-lead zirconate titanate accounts for 10-90% of the volume of the textured piezoelectric ceramic composite material, and the epoxy resin polymer phase (4) accounts for 90-10% of the volume of the textured piezoelectric ceramic composite material.
3. The 1-3 textured piezoelectric ceramic composite material according to claim 2, wherein the textured piezoelectric ceramic phase of lead magnesium niobate-lead zirconate titanate is 56% by volume of the textured piezoelectric ceramic composite material, and the epoxy polymer phase is 44% by volume of the textured piezoelectric ceramic composite material.
4. The 1-3 type textured piezoelectric ceramic composite material according to claim 1, wherein the textured piezoelectric ceramic phase of lead magnesium niobate-lead zirconate titanate having a perovskite structure may be a textured piezoelectric ceramic of lead zinc niobate-lead zirconate titanate (PZN-PZT) or a textured piezoelectric ceramic of lead indium niobate-lead zirconate titanate (PIN-PZT) or a textured piezoelectric ceramic of lead yttrium niobate-lead zirconate titanate (PYN-PZT).
5. A method for preparing a 1-3 type texture piezoelectric ceramic composite material according to any one of claims 1 to 4, comprising the steps of:
step 1, cutting a lead magnesium niobate-lead zirconate titanate textured piezoelectric ceramic material block along a first direction, and reserving the lead magnesium niobate-lead zirconate titanate textured piezoelectric ceramic material with required thickness as a substrate (1) to obtain a ceramic strip array (2);
step 2, cutting the ceramic strip array obtained in the step 1 along a second direction, ultrasonically cleaning the array after cutting, and drying to obtain a plurality of mutually independent lead magnesium niobate-lead zirconate titanate texture piezoelectric ceramic column arrays (3); the second direction is on the same plane as the first direction, and the second direction is perpendicular to the first direction;
step 3, injecting epoxy resin colloid into the lead magnesium niobate-lead zirconate titanate texture piezoelectric ceramic column array (3) prepared in the step 2, filling cutting gaps, and curing at room temperature after removing bubbles in vacuum to obtain a lead magnesium niobate-lead zirconate titanate texture piezoelectric ceramic epoxy resin composite material;
polishing the lead magnesium niobate-lead zirconate titanate textured piezoelectric ceramic epoxy resin composite material prepared in the step 3, and removing redundant resin on the upper surface and the lower surface and the lead magnesium niobate-lead zirconate titanate textured piezoelectric ceramic substrate (1) to expose ceramic columns;
and 5, ultrasonically cleaning and drying the ceramic piezoelectric composite material prepared in the step 4, and preparing a conductive layer on the surface of the textured piezoelectric ceramic composite material by adopting 80-150 ℃ curing silver paste coating or rotary magnetron sputtering to obtain the 1-3 textured piezoelectric ceramic composite material.
6. The method for preparing a 1-3 type textured piezoelectric ceramic composite material according to claim 5, wherein the cutting step in the step 1 is a ceramic column width plus a kerf width.
7. The method for producing a type 1-3 textured piezoelectric ceramic composite material according to claim 5, wherein the thickness of the substrate (1) in the step 1 is 1/3-1/5 of the depth of cut.
8. The method for preparing a 1-3 type textured piezoelectric ceramic composite material according to claim 5, wherein the cutting depth in the step 2 is the same as the cutting depth in the step 1, and the cutting depth is 0.3-0.6 mm higher than the final 1-3 type textured piezoelectric ceramic composite material.
9. The method for preparing a 1-3 type textured piezoelectric ceramic composite material according to claim 5, wherein in the step 4, the sum of the width of the ceramic column and the width of the cutting gap in the step 1 is the transverse period size of the composite material, and the ratio of the final thickness of the polished ceramic composite material to the transverse period size is 2.5-3.5.
10. The application of the 1-3 type texture piezoelectric ceramic composite material is characterized by being used for preparing an underwater acoustic transducer.
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