CN104393164A - 1-1-3 piezoelectric composite material and manufacturing method thereof - Google Patents
1-1-3 piezoelectric composite material and manufacturing method thereof Download PDFInfo
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- CN104393164A CN104393164A CN201410573671.7A CN201410573671A CN104393164A CN 104393164 A CN104393164 A CN 104393164A CN 201410573671 A CN201410573671 A CN 201410573671A CN 104393164 A CN104393164 A CN 104393164A
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Abstract
The invention relates to a 1-1-3 piezoelectric composite material and a manufacturing method thereof, and belongs to the technical field of piezoelectric composite material. The piezoelectric composite material comprises piezoelectric single-crystal crystalline columns, flexible polymers and rigid polymers, wherein the piezoelectric single-crystal crystalline columns are arranged periodically and regularly, the flexible polymers tightly coat the single-crystal crystalline columns, the rigid polymers are arranged inside the flexible polymers, and thus a three-dimensional grid structure is formed to play a supporting role so as to enable stability and impact resistance to be stronger. Through the above structure, the composite material can maintain the strong piezoelectric performance of the single crystal, can reduce transverse coupling among primitives and reduce acoustic impedance, and thus the 1-1-3 piezoelectric composite material has the advantages of high electromechanical coupling factor (>/=0.9), small vibration coupling between array elements and high mechanical and temperature stability, and is an ideal sensitive element for manufacturing a high-power underwater sound transducer array.
Description
Technical field
The invention belongs to piezo-electricity composite material and device arts thereof, be specifically related to a kind of for the underwater sound, supersonic sounding there is piezo-electricity composite material of high electromechanical coupling factor and preparation method thereof.
Background technology
Piezo-electricity composite material is mainly used in underwater acoustic transducer and ultrasonic transducer two aspects.Underwater acoustic transducer is device acoustic energy and electric energy being carried out conversion mutually, is the Primary Component transmitting and receiving sound wave under water, is mainly used in detection under water, identification, communication, and the exploitation etc. of marine environmental monitoring and marine resources.And ultrasonic transducer is mainly used in the aspect such as medical ultrasound imaging, Ultrasonic NDT.
At present, the senser mainly piezoelectric element that transducer uses, accounts for more than 80% of total transducer material.Piezoelectric element is mainly divided into piezoelectric ceramic, piezoelectric monocrystal, piezo-electricity composite material and piezopolymer four class.Because the do not coexist underwater sound, ultrasonic and sensory field of its feature has different application.Wherein, piezo-electricity composite material is composited by piezoelectric ceramic or monocrystalline and polymer, and it improves the combination property of material mutually mainly through adding polymer.Its thickness electromechanical coupling coefficient comparatively can improve 20% by piezoelectric ceramic, and Characteristic impedance and density significantly reduce, and mechanical quality factor reduces nearly half, the more ceramic expansion of bandwidth 2 times.
Current existing piezo-electricity composite material, mainly 1-3 type, 2-2 type composite material, although the electromechanical coupling factor of piezoelectric is improve about 20%, but according to current bibliographical information, the thickness electromechanical coupling coefficient of flaky material is the highest can only reach 0.85, how to improve the key content that thickness electromechanical coupling coefficient becomes current piezo-electricity composite material research field further.
Summary of the invention
The present invention is directed to the problems referred to above, by using relaxor ferroelectric monocrystal as active material, provide a kind of 1-1-3 type piezo-electricity composite material with high electromechanical coupling factor with and preparation method thereof, this material has that electromechanical coupling factor is high, vibration coupling is low between primitive, acoustic impedance is low, temperature stability high.
1-1-3 type piezo-electricity composite material of the present invention, comprise piezoelectric monocrystal crystal column, flexible polymer and rigid polymer, wherein, piezoelectric monocrystal crystal column is periodic arrangement, flexible polymer and rigid polymer are filled between adj acent piezoelectric monocrystalline crystal column, piezoelectric monocrystal crystal column is communicated with to (as z direction) at one-dimensional square, flexible polymer is around piezoelectric monocrystal crystal column and be communicated with to (as z direction) at the one-dimensional square identical with it, and rigid polymer and flexible polymer are closely adjacent and be all communicated with at three-dimensional (x, y, z three directions).
In above-mentioned piezo-electricity composite material, rigid polymer is all communicated with at three-dimensional can play cross-brace effect, ensure that the hydrostatic pressing characteristic of composite material, temperature and mechanical stability can also reduce transverse coupling between primitive simultaneously.
Further, described 1-1-3 type piezo-electricity composite material also comprises top electrode, bottom electrode, lays respectively at the upper and lower surface of piezo-electricity composite material, is made up through deposition or sintering of the easy easy weld metal of weld metal such as gold, silver, copper.
Further, described piezoelectric monocrystal crystal column is relaxation ferro-electricity single crystal crystal column, adopts a monoblock relaxation ferro-electricity single crystal to be made through accurate cutting, and the arrangement of periodic law ground.Preferably, the positioning precision between piezoelectric monocrystal crystal column reaches 0.001mm, and the quantity of crystal column is greater than 100, and the length of side of crystal column is generally 0.2 ~ 5mm, and the height of every sheet crystal column is 0.5 ~ 15mm, all crystal columns measure-alike.
Further, described flexible polymer adopts the polymer that the hardness such as polyurethane, silicon rubber is lower, and after flexible polymer solidification, width is 0.02 ~ 3mm; Described rigid polymer can adopt the polymer such as the epoxy resin that the hardness of modification is higher, and after rigid polymer solidification, width is 0.02 ~ 2mm.
1-1-3 type piezo-electricity composite material of the present invention has two kinds of preparation methods, is respectively described below:
The first prepares the method for above-mentioned 1-1-3 type piezo-electricity composite material, and its step comprises:
1) cut piezoelectric monocrystal, form evenly distributed piezoelectric monocrystal crystal column skeleton;
2) by certain weight ratio preparation flexible polymer, and bubble is wherein discharged;
3) in piezoelectric monocrystal crystal column array, pour into a mould flexible polymer, and solidify;
4) secondary cut piezo-electricity composite material, removes the monocrystalline between flexible polymer and forms grooving, pouring into a mould rigid polymer, and solidify in grooving, forms 1-1-3 type piezo-electricity composite material.
Further, step 1) before cutting piezoelectric monocrystal, choose piezoelectric monocrystal and polymer, according to the performance requirement of composite material, calculate the width of when grooving in length and breadth of the percent by volume of piezoelectric monocrystal, overall dimension, post, determine cutting parameter.
Further, step 1) after cutting piezoelectric monocrystal, detect the size of crystal column and the uniformity of arrangement.
Further, step 2) by certain weight ratio preparation flexible polymer, such as silicon rubber is normally monocomponent room-temperature cured, and polyurethane is generally according to the mass ratio with curing agent 10:1; This step by stirring, the mode such as to vacuumize discharges bubble in flexible polymer, and visual inspection is joined glue (polymer also do not solidified) and is had bubble-free.
Further, step 4) after the rigid polymer solidification of cast, the piezo-electricity composite material blank surface after polishing solidification, cutting blank surrounding, makes the material sample of required size.
Further, in step 4) after, adopt sputtering method to prepare top electrode and the bottom electrode of piezo-electricity composite material sample surfaces.Then the test of the piezoelectricity of piezo-electricity composite material, dielectric and impedance operator can also be carried out.
The second prepares the method for above-mentioned 1-1-3 type piezo-electricity composite material, and its step comprises:
1) cut piezoelectric monocrystal, form evenly distributed piezoelectric monocrystal crystal column skeleton;
2) prepare rigid polymer framework, and this framework is positioned between piezoelectric monocrystal crystal column skeleton;
3) by certain weight ratio preparation flexible polymer, and bubble is wherein discharged;
4) in the gap of piezoelectric monocrystal crystal column and rigid polymer framework, pour into a mould flexible polymer, and solidify, form 1-1-3 type piezo-electricity composite material.
Further, step 2) application perfusion ejection technique prepare rigid polymer framework.
Further, the second preparation method also can adopt the refinement measure identical with the first preparation method, as: before cutting piezoelectric monocrystal, choose piezoelectric monocrystal and polymer, according to the performance requirement of composite material, calculate the width of when grooving in length and breadth of the percent by volume of piezoelectric monocrystal, overall dimension, post, determine cutting parameter; The size of crystal column and the uniformity of arrangement is detected after cutting piezoelectric monocrystal; Discharged the bubble in flexible polymer by modes such as stirring, vacuumize, and visual inspection is joined glue and is had bubble-free; Piezo-electricity composite material blank surface after polishing solidification, cutting blank surrounding, makes the material sample of required size; Piezo-electricity composite material sample surfaces electrode is prepared with sputtering method; Carry out the piezoelectricity of piezo-electricity composite material, dielectric and impedance operator test etc.
Compared with prior art, beneficial effect of the present invention is as follows:
The present invention adopts 1-1-3 type Structure composing piezo-electricity composite material, can be applied to underwater acoustic transducer and ultrasonic transducer.This piezo-electricity composite material is using piezoelectric monocrystal as initiative material, with flexible polymer parcel monocrystalline buttress shaft, formed three dimensional network structure with rigid polymer to play a supporting role, this piezo-electricity composite material is made namely to keep the strong piezoelectricity energy of monocrystalline, turn reduce the transverse coupling between primitive, acoustic impedance can also be reduced simultaneously, make it have high electromechanical coupling factor (>=0.9) simultaneously, the advantage that between array element, vibration coupling is little and mechanical and temperature stability is high, overcome relaxor ferroelectric monocrystal hard and crisp, mechanical tensile strength is low, acoustic impedance is high, not easily with air, water and tissue coupling, the shortcomings such as narrow bandwidth, it is the senser of the high-power underwater acoustic transducer battle array of a kind of desirable preparation, operating distance and the detection accuracy of underwater acoustic transducer battle array can be improved.
Accompanying drawing explanation
Fig. 1 is 1-1-3 type structures of piezoelectric composite schematic diagram in embodiment.
Fig. 2 is 1-1-3 type piezo-electricity composite material primitive post explosion views in embodiment.
Fig. 3 is preparation technology's flow chart of 1-1-3 type piezo-electricity composite material in embodiment.
Fig. 4 is 1-1-3 type composite material admittance result of finite element figure in embodiment.
Fig. 5 is 1-1-3 type composite material mechanical admittance curves experimental measurements figure in embodiment.
Fig. 6 is 1-1-3 type piezo-electricity composite material mode of oscillation result of finite element figure in embodiment, and wherein (a) figure is that three phase material z direction vibration displacements compare, and (b) figure is the mode of oscillation of primitive under resonance frequency.
Wherein, 1-piezoelectric crystal; 2-flexible polymer; 3-rigid polymer; 4-upper surface electrode layer; 5-lower surface electrode layer.
Embodiment
For enabling above-mentioned purpose of the present invention, feature and advantage become apparent more, and below by specific embodiments and the drawings, the present invention will be further described.
Fig. 1 is 1-1-3 type structures of piezoelectric composite schematic diagram of the present invention.As shown in the figure, this 1-1-3 type piezo-electricity composite material comprises: piezoelectric monocrystal crystal column 1, flexible polymer 2, rigid polymer 3 and upper surface electrode layer 4, lower surface electrode layer 5 (what in figure, " 5 " were pointed to is bottom).Fig. 2 gives the explosion views of concrete single primitive (single piezoelectric monocrystal crystal column).In the present embodiment, piezoelectric monocrystal crystal column adopts relaxation ferro-electricity single crystal crystal column, single relaxation ferro-electricity single crystal crystal column periodic regularity arrangement, be generally 10 × 10,15 × 15,20 × 20 various ways such as grade quadrate array arrangement, before non-filled polymer each crystal column be cut after gap be generally 0.2-0.8mm.Relaxation ferro-electricity single crystal is the most significant a kind of piezoelectric monocrystal of piezoelectric effect, and electromechanical coupling factor is higher, can reach 0.95, adopts this piezoelectric monocrystal can improve composite material electromechanical coupling factor of the present invention further, promotes material property.
As shown in Figure 1 and Figure 2, piezoelectric monocrystal crystal column 1 is at z direction one dimension connect, and surrounding is around one deck flexible polymer 2 be communicated with in z direction.Flexible polymer 2 periphery is surrounded by rigid polymer 3, and rigid polymer 3 is all communicated with in x, y, z three directions, plays cross-brace effect.Flexible polymer is wrapped in each relaxation ferro-electricity single crystal crystal column, and rigid polymer support is embedded in flexible polymer, and make total have the support of rigid support, stability is stronger.This structure ensure that the hydrostatic pressing characteristic of composite material, temperature and mechanical stability can also reduce transverse coupling between primitive simultaneously.The load of monocrystalline can be reduced by introducing flexible polymer, making monocrystalline crystal column be similar to free vibration, and then improve the electromechanical coupling factor of composite material.Flexible polymer generally uses polyurethane, silicon rubber etc.Rigid polymer generally uses the polymer that the hardness such as epoxy resin are stronger.Be upper surface electrode layer 4, lower surface electrode layer 5 in the upper and lower surface of monoblock composite material, electrode can be the metal conducting layer of the surface attachment such as conducting resinl, sheet metal or sputtered metal film, can select the easily weld metal such as gold, silver, copper.
Fig. 3 gives preparation technology's flow chart of relaxation ferro-electricity single crystal 1-1-3 type piezo-electricity composite material, gives the different cutting of two covers, preparation scheme.Scheme one, first along x, y direction being parallel to relaxation ferro-electricity single crystal polaxis, with automatic gas cutting machine cutting relaxation ferro-electricity single crystal, forms the gap of foursquare periodic law arrangement, pours into a mould treated flexible polymer in gap.Secondly, according to the design size of primitive, in x direction and y direction, the monocrystalline between flexible polymer is cut away, and forms grooving, in grooving, note rigid polymer, spraying plating upper/lower electrode layer.Scheme two, first along x, y direction being parallel to relaxation ferro-electricity single crystal polaxis, with automatic gas cutting machine cutting relaxation ferro-electricity single crystal, forms the gap of foursquare periodic law arrangement.Secondly, application perfusion ejection technique prepares rigid polymer framework, makes composite material all have rigid polymer to support being parallel and perpendicular to polarised direction, and is positioned in relaxation ferro-electricity single crystal skeleton by this rigid polymer framework.Finally, the flexible polymer in gap after cast process.
The present invention establishes FEM (finite element) model to 1-1-3 type composite material, as shown in Figure 2, and has carried out analysis verification.Wherein, piezoelectric monocrystal crystal column adopts PMNT monocrystalline (relaxation ferro-electricity single crystal), and flexible polymer adopts silicon rubber, and rigid polymer adopts epoxy resin.Fig. 4 gives this 1-1-3 type composite material mechanical admittance curves result of finite element, by finding out in figure that composite material series resonance frequency fs is 465kHz, parallel resonance frequency f
pfor 1206kHz, calculating effective electro-mechanical couple factor keff is 0.923.For verifying validity of the present invention further, prepare a 1-1-3 type compound unit meter sample.Fig. 5 gives this 1-1-3 type composite material mechanical admittance curves experimental measurements, can find out composite material series resonance frequency f by figure
sfor 324kHz, parallel resonance frequency f
pfor 681kHz, calculate effective electro-mechanical couple factor k
effbe 0.9.Because FEM (finite element) model thickness is different from actual sample thickness, so resonant frequency value difference is larger.Because the correlation of electromechanical coupling factor and thickness is less, its experimental measurements is coupled better with result of finite element.
Reduce transverse vibration coupling effect between primitive for analyzing in 1-1-3 type composite construction by two kinds of polymer, the present invention analyzes 1-1-3 type piezo-electricity composite material vibration displacement with vibration of element mode under resonance frequency change curve and resonance frequency.Fig. 6 is 1-1-3 type piezo-electricity composite material mode of oscillation result of finite element figure, and wherein (a) figure is that three phase material z direction vibration displacements compare, and (b) figure is the mode of oscillation of primitive under resonance frequency.As seen from Figure 6, PMNT monocrystalline is initiative material, and under 1000V voltage drive, vibration displacement is maximum reaches 0.132mm.Silicon rubber is forced vibration, and its displacement is relatively large, reaches 5.914 μm, compares the displacement decline 13.49dB of PMNT monocrystalline, and excite Lateral Vibration Modal near resonance frequency.The z direction displacement of epoxy resin phase is then relatively low, only has 0.448 μm, compares the displacement decline 24.7dB of PMNT monocrystalline.Thus, 1-1-3 type composite construction can be found out, effectively can reduce the transverse vibration coupling of composite material.
1-1-3 type piezo-electricity composite material based on relaxation ferro-electricity single crystal of the present invention described by embodiment above and preparation method thereof; be not intended to limit the present invention; any those skilled in the art; not departing from spirit of the present invention and essential scope; can do various changes and retouching, therefore protection scope of the present invention defined depending on claims.
Claims (10)
1. a 1-1-3 type piezo-electricity composite material, it is characterized in that, comprise piezoelectric monocrystal crystal column, flexible polymer and rigid polymer, wherein, piezoelectric monocrystal crystal column is periodic arrangement, and flexible polymer and rigid polymer are filled between adj acent piezoelectric monocrystalline crystal column, piezoelectric monocrystal crystal column at one-dimensional square to connection, flexible polymer is around piezoelectric monocrystal crystal column and at the one-dimensional square identical with it to connection, and rigid polymer and flexible polymer are closely adjacent and be all communicated with at three-dimensional.
2. 1-1-3 type piezo-electricity composite material as claimed in claim 1, is characterized in that: described 1-1-3 type piezo-electricity composite material also comprises top electrode and bottom electrode, lays respectively at the upper and lower surface of piezo-electricity composite material.
3. 1-1-3 type piezo-electricity composite material as claimed in claim 1 or 2, is characterized in that: described piezoelectric monocrystal crystal column is relaxation ferro-electricity single crystal crystal column.
4. 1-1-3 type piezo-electricity composite material as claimed in claim 1 or 2, it is characterized in that: the positioning precision between described piezoelectric monocrystal crystal column reaches 0.001mm, the quantity of crystal column is greater than 100, and the length of side of crystal column is 0.5 ~ 5mm, and the height of every sheet crystal column is 1.5 ~ 15mm.
5. 1-1-3 type piezo-electricity composite material as claimed in claim 1 or 2, it is characterized in that: described flexible polymer is polyurethane or silicon rubber, described rigid polymer is epoxy resin.
6. prepare a method for 1-1-3 type piezo-electricity composite material described in claim 1, its step comprises:
1) cut piezoelectric monocrystal, form evenly distributed piezoelectric monocrystal crystal column skeleton;
2) prepare flexible polymer, and discharge bubble wherein;
3) in piezoelectric monocrystal crystal column array, pour into a mould flexible polymer, and solidify;
4) secondary cut piezo-electricity composite material, removes the monocrystalline between flexible polymer and forms grooving, pouring into a mould rigid polymer, and solidify in grooving, forms 1-1-3 type piezo-electricity composite material.
7. prepare a method for 1-1-3 type piezo-electricity composite material described in claim 1, its step comprises:
1) cut piezoelectric monocrystal, form evenly distributed piezoelectric monocrystal crystal column skeleton;
2) prepare rigid polymer framework, and this framework is positioned between piezoelectric monocrystal crystal column skeleton;
3) prepare flexible polymer, and discharge bubble wherein;
4) in the gap of piezoelectric monocrystal crystal column and rigid polymer framework, pour into a mould flexible polymer, and solidify, form 1-1-3 type piezo-electricity composite material.
8. method as claimed in claim 7, is characterized in that: step 2) application perfusion ejection technique prepares rigid polymer framework.
9. method as claimed in claims 6 or 7, is characterized in that: also comprise the step that employing sputtering method prepares top electrode and bottom electrode.
10. method as claimed in claims 6 or 7, it is characterized in that: before cutting piezoelectric monocrystal, choose piezoelectric monocrystal and polymer, according to the performance requirement of composite material, calculate the width of when grooving in length and breadth of the percent by volume of piezoelectric monocrystal, overall dimension, post, determine cutting parameter; The size of crystal column and the uniformity of arrangement is detected after cutting piezoelectric monocrystal; Discharged the bubble in flexible polymer by modes such as stirring, vacuumize, and visual inspection is joined glue and is had bubble-free; Piezo-electricity composite material blank surface after polishing solidification, cutting blank surrounding, makes the material sample of required size.
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| CN107068852A (en) * | 2017-02-09 | 2017-08-18 | 湖北工程学院 | It is a kind of applied to magnetic electric compound material of energy acquisition and preparation method thereof |
| CN107170882A (en) * | 2017-05-09 | 2017-09-15 | 北京信息科技大学 | Based on 13 type piezo-electricity composite materials for improving polymer phase and preparation method thereof |
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| CN110176433A (en) * | 2019-04-30 | 2019-08-27 | 杭州电子科技大学 | A kind of flexibility base compound substrate and preparation method thereof |
| CN110828655A (en) * | 2019-11-15 | 2020-02-21 | 飞依诺科技(苏州)有限公司 | Ultrasonic probe, piezoelectric composite material wafer and preparation method thereof |
| CN112221917A (en) * | 2020-09-04 | 2021-01-15 | 北京信息科技大学 | High-power high-frequency directional emission underwater acoustic transducer and preparation method thereof |
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| CN106856401B (en) * | 2015-12-08 | 2020-10-23 | 中国科学院上海硅酸盐研究所 | Piezoelectric vibrator and preparation method and application thereof |
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| CN110828655B (en) * | 2019-11-15 | 2021-11-30 | 飞依诺科技(苏州)有限公司 | Ultrasonic probe, piezoelectric composite material wafer and preparation method thereof |
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Effective date of registration: 20230925 Address after: 213100 a1-701-3-2, Changzhou science and Education City Zhongke entrepreneurship center, No. 18, Changwu Middle Road, Wujin District, Changzhou City, Jiangsu Province Patentee after: Changzhou deep sea echo Acoustics Technology Co.,Ltd. Address before: 100101 No. 35 middle Fourth Ring Road, Chaoyang District, Beijing Patentee before: BEIJING INFORMATION SCIENCE AND TECHNOLOGY University |