CN104393164B - Manufacturing method of 1-1-3 piezoelectric composite material - Google Patents
Manufacturing method of 1-1-3 piezoelectric composite material Download PDFInfo
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- CN104393164B CN104393164B CN201410573671.7A CN201410573671A CN104393164B CN 104393164 B CN104393164 B CN 104393164B CN 201410573671 A CN201410573671 A CN 201410573671A CN 104393164 B CN104393164 B CN 104393164B
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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 its device arts, and in particular to one kind is used for the underwater sound, supersonic sounding
The piezo-electricity composite material with electromechanical coupling factor high preparation method.
Background technology
Piezo-electricity composite material is mainly used in two aspects of underwater acoustic transducer and ultrasonic transducer.Underwater acoustic transducer is by sound
The device of mutual conversion can be carried out with electric energy, is the Primary Component for launching and receiving sound wave under water, be mainly used under water
Exploitation of detection, identification, communication, and marine environmental monitoring and marine resources etc..And ultrasonic transducer is mainly used in medical treatment and surpasses
The aspects such as acoustic imaging, Ultrasonic NDT.
At present, the sensing element mainly piezoelectric element that transducer is used, accounts for more than the 80% of total transducer material.Pressure
Electric device is broadly divided into piezoelectric ceramics, piezoelectric monocrystal, piezo-electricity composite material and the class of piezopolymer four.Because its feature difference exists
The underwater sound, ultrasound and sensory field have different applications.Wherein, piezo-electricity composite material be by piezoelectric ceramics or monocrystalline be polymerized
Thing is composited, and it mainly improves the combination property of material by adding polymer phase.Its thickness electromechanical coupling coefficient can be compared with
Piezoelectric ceramics improves 20%, and Characteristic impedance and density significantly reduce, and the nearly half of mechanical quality factor reduction, bandwidth is more ceramic
2 times of extension.
Current existing piezo-electricity composite material, mainly 1-3 types, 2-2 type composites, although by the electromechanics of piezoelectric
The coefficient of coup improves 20% or so, but according to current document report, the thickness electromechanical coupling coefficient of flaky material only up to
0.85 is reached, how further to be improved in key of the thickness electromechanical coupling coefficient as current piezo-electricity composite material research field
Hold.
The content of the invention
The present invention regarding to the issue above, by using relaxor ferroelectric monocrystal as active material, there is provided one kind have height
The 1-1-3 types piezo-electricity composite material of electromechanical coupling factor with and preparation method thereof, the material has that electromechanical coupling factor is high, primitive
Between the features such as vibration coupling is low, acoustic impedance is low, temperature stability is high.
1-1-3 types piezo-electricity composite material of the invention, including piezoelectric monocrystal crystal column, flexible polymer and rigid polymer,
Wherein, piezoelectric monocrystal crystal column is in periodic arrangement, flexible polymer and rigid polymer be filled in adj acent piezoelectric monocrystalline crystal column it
Between, piezoelectric monocrystal crystal column is connected in one-dimensional square (such as z directions), and flexible polymer is around piezoelectric monocrystal crystal column and same
One-dimensional square (such as z directions) connection, rigid polymer and flexible polymer are tight adjacent and in three-dimensional (x, y, z three
Direction) connect.
In above-mentioned piezo-electricity composite material, rigid polymer is connected in three-dimensional and can play cross-brace effect,
Hydrostatic pressing characteristic, temperature and the mechanical stability of composite be ensure that while transverse coupling between primitive can also be reduced.
Further, the 1-1-3 types piezo-electricity composite material also includes Top electrode, bottom electrode, respectively positioned at Piezoelectric anisotropy
The upper and lower surface of material, it is deposited by the easily welding metal easy welding metal such as gold, silver, copper or sintering is made.
Further, the piezoelectric monocrystal crystal column is relaxation ferro-electricity single crystal crystal column, is passed through using a monoblock relaxation ferro-electricity single crystal
Accurate cutting is crossed to be made, and the arrangement of periodic law ground.Preferably, the positioning precision between piezoelectric monocrystal crystal column reaches
0.001mm, the quantity of crystal column is more than 100, and the length of side of crystal column is usually 0.2~5mm, and every height of crystal column is 0.5~
15mm, the size of all crystal columns is identical.
Further, the flexible polymer is using the relatively low polymer of hardness, flexible polymer such as polyurethane, silicon rubber
Width is 0.02~3mm after solidification；The rigid polymer can use the polymer such as modified hardness epoxy resin higher,
Width is 0.02~2mm after rigid polymer solidification.
1-1-3 types piezo-electricity composite material of the invention has two kinds of preparation methods, is respectively described below：
The first prepares the method for above-mentioned 1-1-3 types piezo-electricity composite material, and its step includes：
1) piezoelectric monocrystal is cut, evenly distributed piezoelectric monocrystal crystal column skeleton is formed；
2) by certain weight than preparing flexible polymer, and bubble therein is discharged；
3) flexible polymer is poured into a mould in piezoelectric monocrystal crystal column array, and is solidified；
4) secondary cut piezo-electricity composite material, removes the monocrystalline between flexible polymer and forms grooving, is poured into a mould in grooving
Rigid polymer, and solidify, form 1-1-3 type piezo-electricity composite materials.
Further, step 1) before piezoelectric monocrystal is cut, piezoelectric monocrystal and polymer are chosen, according to composite
Performance requirement, calculates the when width of grooving in length and breadth of the percent by volume of piezoelectric monocrystal, appearance and size, post, it is determined that cutting ginseng
Number.
Further, step 1) after piezoelectric monocrystal is cut, detect the size of crystal column and the uniformity of arrangement.
Further, step 2) it is typically single group locellus than preparing flexible polymer, such as silicon rubber by certain weight
Temperature solidification, polyurethane be usually according to curing agent 10:1 mass ratio；The step is discharged by the mode such as stirring, vacuumizing
Bubble in flexible polymer, and visual inspection has bubble-free with glue (polymer not solidified also).
Further, step 4) after the rigid polymer solidification of cast, the piezo-electricity composite material blank after polishing solidification
Surface, cuts blank surrounding, is made the material sample of required size.
Further, in step 4) after, using sputtering method prepare piezo-electricity composite material sample surfaces Top electrode and under
Electrode.Then piezoelectricity, dielectric and the impedance operator test of piezo-electricity composite material can also be carried out.
The method for preparing above-mentioned 1-1-3 types piezo-electricity composite material for second, its step includes：
1) piezoelectric monocrystal is cut, evenly distributed piezoelectric monocrystal crystal column skeleton is formed；
2) rigid polymer framework is prepared, and this framework is positioned between piezoelectric monocrystal crystal column skeleton；
3) by certain weight than preparing flexible polymer, and bubble therein is discharged；
4) flexible polymer is poured into a mould in the gap of piezoelectric monocrystal crystal column and rigid polymer framework, and is solidified, form 1-
1-3 type piezo-electricity composite materials.
Further, step 2) prepare rigid polymer framework using perfusion ejection technique.
Further, second preparation method can also be used and refine measure with the first preparation method identical, such as：Cutting
Before cutting piezoelectric monocrystal, piezoelectric monocrystal and polymer are chosen, according to the performance requirement of composite, calculate the volume of piezoelectric monocrystal
Percentage, appearance and size, the when width of grooving in length and breadth of post, determine cutting parameter；Crystal column is detected after piezoelectric monocrystal is cut
Size and arrangement uniformity；Bubble in flexible polymer is discharged by the mode such as stirring, vacuumizing, and glue is matched somebody with somebody in visual inspection
There is bubble-free；Piezo-electricity composite material blank surface after polishing solidification, cuts blank surrounding, is made the material sample of required size
Product；Piezo-electricity composite material sample surfaces electrode is prepared with sputtering method；Carry out piezoelectricity, dielectric and the impedance operator of piezo-electricity composite material
Test etc..
Compared with prior art, beneficial effects of the present invention are as follows：
The present invention constitutes piezo-electricity composite material using 1-1-3 types structure, can apply to underwater acoustic transducer and ultrasonic transduction
Device.The piezo-electricity composite material wraps up monocrystalline buttress shaft, with rigid polymer using piezoelectric monocrystal as initiative material with flexible polymer
Thing constitutes three dimensional network structure and plays a supporting role so that the piezo-electricity composite material is the strong piezoelectricity energy for keeping monocrystalline, is subtracted again
Transverse coupling between small primitive, while acoustic impedance can also be reduced, make itself and meanwhile have electromechanical coupling factor high (>=0.9),
Vibration coupling is small between array element and mechanical and temperature stability advantage high, and it is hard and crisp to overcome relaxor ferroelectric monocrystal, mechanical resistance
Low intensity, acoustic impedance is high, is difficult match with empty gas and water and tissue, is a kind of preferably preparation greatly the shortcomings of narrow bandwidth
The sensing element of power underwater acoustic transducer battle array, can improve the operating distance and detection accuracy of underwater acoustic transducer battle array.
Brief description of the drawings
Fig. 1 is 1-1-3 type structures of piezoelectric composite schematic diagrames in embodiment.
Fig. 2 is 1-1-3 type piezo-electricity composite material primitive post explosion views in embodiment.
Fig. 3 is the preparation technology flow chart of 1-1-3 type piezo-electricity composite materials in embodiment.
Fig. 4 is 1-1-3 type composite admittance result of finite element figures in embodiment.
Fig. 5 is 1-1-3 type composite mechanical admittance curves experimental measurements figures in embodiment.
Fig. 6 is 1-1-3 type piezo-electricity composite material mode of oscillation result of finite element figures in embodiment, wherein (a) figure is
Three phase material z directions vibration displacements compare, and (b) figure is the mode of oscillation of primitive under resonant frequency.
Wherein, 1-piezo-electric crystal；2-flexible polymer；3-rigid polymer；4-upper surface electrode layer；5-following table
Face electrode layer.
Specific embodiment
To enable the above objects, features and advantages of the present invention more obvious understandable, below by specific embodiment and
Accompanying drawing, the present invention will be further described.
Fig. 1 is 1-1-3 types structures of piezoelectric composite schematic diagram of the invention.As illustrated, the 1-1-3 type Piezoelectric anisotropies
Material includes：Piezoelectric monocrystal crystal column 1, flexible polymer 2, rigid polymer 3 and upper surface electrode layer 4, lower surface electrode layer 5
(what " 5 " were pointed in figure is bottom).Fig. 2 gives the explosion views of specific single primitive (single piezoelectric monocrystal crystal column).This reality
Apply in example, piezoelectric monocrystal crystal column uses relaxation ferro-electricity single crystal crystal column, single relaxation ferro-electricity single crystal crystal column periodic regularity arrangement, one
As for 10 × 10,15 × 15,20 × 20 grade various ways quadrate array arrange, each crystal column quilt before being not filled by polymer
Gap after cutting is generally 0.2-0.8mm.Relaxation ferro-electricity single crystal is a kind of most significant piezoelectric monocrystal of piezo-electric effect, and electromechanical
The coefficient of coup is higher, can reach 0.95, and composite mechanical-electric coupling of the invention can be further improved using this piezoelectric monocrystal
Coefficient, lifts material property.
As shown in Figure 1 and Figure 2, piezoelectric monocrystal crystal column 1 is around only connected around one layer in the one-dimensional connection in z directions in z directions
Flexible polymer 2.The periphery of flexible polymer 2 is surrounded by rigid polymer 3, and rigid polymer 3 is equal in three directions of x, y, z
Connection, plays cross-brace effect.Flexible polymer is wrapped in each relaxation ferro-electricity single crystal crystal column, and rigid polymer support is inlayed
In flexible polymer so that total has the support of rigid support, stability is stronger.This structure ensure that composite
Hydrostatic pressing characteristic, temperature and mechanical stability can also reduce transverse coupling between primitive simultaneously.Can by introducing flexible polymer
To reduce the load of monocrystalline so that monocrystalline crystal column is similar to free vibration, and then improves the electromechanical coupling factor of composite.It is soft
Property polymer generally uses polyurethane, silicon rubber etc..Rigid polymer generally uses the stronger polymer of the hardness such as epoxy resin.
It is upper surface electrode layer 4, lower surface electrode layer 5 in the upper and lower surface of monoblock composite, electrode can be conducting resinl, sheet metal
Or the metal conducting layer of the surface attachment such as sputtered metal film, the easily welding metal such as gold, silver, copper may be selected.
Fig. 3 gives the preparation technology flow chart of relaxation ferro-electricity single crystal 1-1-3 type piezo-electricity composite materials, gives two sets not
Same cutting, preparation scheme.Scheme one, first along x, y direction parallel to relaxation ferro-electricity single crystal polaxis, uses automatic gas cutting machine
Cutting relaxation ferro-electricity single crystal, forms the gap of foursquare periodic law arrangement, and the flexible polymer through processing is poured into a mould in gap
Thing.Secondly, according to the design size of primitive, in x directions and y directions, the monocrystalline between flexible polymer is cut away, and formation is cut
Groove, notes rigid polymer, spraying plating upper/lower electrode layer in grooving.Scheme two, first along parallel to relaxation ferro-electricity single crystal polaxis
X, y direction, cut relaxation ferro-electricity single crystal with automatic gas cutting machine, form the gap of foursquare periodic law arrangement.Secondly, should
Rigid polymer framework is prepared with perfusion ejection technique so that composite has rigidity poly- being parallel and perpendicular to polarised direction
Compound is supported, and this rigid polymer framework is positioned in relaxation ferro-electricity single crystal skeleton.Finally, after cast treatment in gap
Flexible polymer.
The present invention establishes FEM model to 1-1-3 type composites, as shown in Fig. 2 and having carried out analysis verification.Its
In, piezoelectric monocrystal crystal column uses PMNT monocrystalline (relaxation ferro-electricity single crystal), flexible polymer to use silicon rubber, rigid polymer to use
Epoxy resin.Fig. 4 gives the 1-1-3 type composite mechanical admittance curves result of finite element, by can be seen that composite wood in figure
Material series resonance frequency fs is 465kHz, parallel resonance frequency fpIt is 1206kHz, is calculated effective electro-mechanical couple factor
Keff is 0.923.Further to verify effectiveness of the invention, the compound unit's meter sample of a 1-1-3 type is prepared for.Fig. 5 is given
The 1-1-3 type composite mechanical admittance curves experimental measurements, by can be seen that composite series resonance frequency f in figuresFor
324kHz, parallel resonance frequency fpIt is 681kHz, is calculated effective electro-mechanical couple factor keffIt is 0.9.Due to FEM model
Thickness is different from actual sample thickness, so resonant frequency value difference is larger.Due to electromechanical coupling factor and the correlation of thickness
Smaller, its experimental measurements is coupled preferably with result of finite element.
For analysis 1-1-3 type composite constructions in by two kinds of polymer reduce primitive between oscillation crosswise coupling effect, this hair
The bright 1-1-3 type piezo-electricity composite material vibration displacements that analyze are with vibration of element mould under resonant frequency change curve and resonant frequency
State.Fig. 6 is 1-1-3 type piezo-electricity composite material mode of oscillation result of finite element figures, wherein (a) figure is three phase material z directions
Vibration displacement compares, and (b) figure is the mode of oscillation of primitive under resonant frequency.As seen from Figure 6, PMNT monocrystalline is initiative material
Material, under 1000V voltage drives, vibration displacement maximum can reach 0.132mm.Silicon rubber is forced vibration, and its displacement is relatively
Greatly, 5.914 μm are reached, the displacement compared to PMNT monocrystalline declines 13.49dB, and oscillation crosswise is excited near resonant frequency
Mode.And the z directions displacement of asphalt mixtures modified by epoxy resin lipid phase is then relatively low, only 0.448 μm, the displacement compared to PMNT monocrystalline declines
24.7dB.Thus, it is possible to find out 1-1-3 type composite constructions, the oscillation crosswise coupling of composite can be effectively reduced.
The 1-1-3 types piezo-electricity composite material based on relaxation ferro-electricity single crystal of the invention that is described above by embodiment and its
Preparation method, is not intended to limit the present invention, and any those skilled in the art is not departing from spirit and substance of the present invention model
In enclosing, various changes and retouching can be done, therefore protection scope of the present invention is defined depending on claims.
Claims (4)
1. a kind of method for preparing 1-1-3 type piezo-electricity composite materials, the 1-1-3 types piezo-electricity composite material includes that piezoelectric monocrystal is brilliant
Post, flexible polymer and rigid polymer, wherein, piezoelectric monocrystal crystal column is in periodic arrangement, flexible polymer and rigid polymer
Thing is filled between adj acent piezoelectric monocrystalline crystal column, and piezoelectric monocrystal crystal column is connected in one-dimensional square, and flexible polymer is around piezoelectricity list
Jingjing post is simultaneously connected in same one-dimensional square, and rigid polymer is closely adjacent and equal in three-dimensional with flexible polymer
The step of connection, the method, includes：
1) piezoelectric monocrystal is cut, evenly distributed piezoelectric monocrystal crystal column skeleton is formed；
2) rigid polymer framework is prepared, and this framework is positioned between piezoelectric monocrystal crystal column skeleton；
3) flexible polymer is prepared, and discharges bubble therein；
4) flexible polymer is poured into a mould in the gap of piezoelectric monocrystal crystal column and rigid polymer framework, and is solidified, form 1-1-3 types
Piezo-electricity composite material.
2. the method for claim 1, it is characterised in that：Step 2) prepare rigid polymer frame using perfusion ejection technique
Frame.
3. the method for claim 1, it is characterised in that：Also include being prepared using sputtering method the step of Top electrode and bottom electrode
Suddenly.
4. the method for claim 1, it is characterised in that：Before piezoelectric monocrystal is cut, piezoelectric monocrystal and polymerization are chosen
Thing, according to the performance requirement of composite, calculates the when grooving in length and breadth of the percent by volume of piezoelectric monocrystal, appearance and size, post
Width, determine cutting parameter；The size of crystal column and the uniformity of arrangement are detected after piezoelectric monocrystal is cut；By stirring or taking out
The mode of vacuum discharges the bubble in flexible polymer, and visual inspection has bubble-free with glue；Piezoelectric anisotropy material after polishing solidification
Material blank surface, cuts blank surrounding, is made the material sample of required size.
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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 |
| 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 |
| CN107170882B (en) * | 2017-05-09 | 2019-12-20 | 北京信息科技大学 | 1-3 type piezoelectric composite material based on improved polymer phase and preparation method thereof |
| CN108903975B (en) * | 2018-05-07 | 2020-09-08 | 华中科技大学 | High-frequency ultrasonic phased array for ophthalmology and preparation method thereof |
| CN110176433B (en) * | 2019-04-30 | 2020-12-18 | 杭州电子科技大学 | Flexible base composite substrate and preparation method thereof |
| 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 |
| CN112152308B (en) * | 2020-09-04 | 2022-12-09 | 北京信息科技大学 | Underwater wireless charging method and device covering full sea depth based on sound waves |
| CN112221917B (en) * | 2020-09-04 | 2022-02-18 | 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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