CN104496491A - Piezoelectric composite material and preparation method thereof - Google Patents
Piezoelectric composite material and preparation method thereof Download PDFInfo
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- CN104496491A CN104496491A CN201510006138.7A CN201510006138A CN104496491A CN 104496491 A CN104496491 A CN 104496491A CN 201510006138 A CN201510006138 A CN 201510006138A CN 104496491 A CN104496491 A CN 104496491A
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Abstract
The invention provides a piezoelectric ceramic, polyvinylidene fluoride (PVDF) and pressure-sensitive material three-phase composite material with high piezoelectric property. The pressure-sensitive material is added to a piezoelectric ceramic/PVDF piezoelectric composite material as an intermediate layer, so as to play a bridging role; the interfacial bonding properties of the piezoelectric ceramic and the PVDF are improved; coupling between the piezoelectric ceramic and the PVDF is increased; electron migration between ceramic particles is promoted; and the polarization voltage of a ceramic phase is improved. In addition, due to the nonlinear current-voltage characteristics of the pressure-sensitive material, when the pressure-sensitive material is added to the piezoelectric ceramic and PVDF composite material, the polarization-resistant voltage of the piezoelectric composite material is improved; and the overall piezoelectric property of the composite material is improved. Therefore, the piezoelectric composite material is simple in process, and low in cost; the piezoelectric composite film with excellent overall performance and large size can be prepared; and the piezoelectric composite material is expected to be applied to a piezoelectric touchpad, thus industrialized production is achieved.
Description
Technical field
The present invention relates to a kind of piezo-electricity composite material, particularly the material of a kind of piezoelectric ceramics, poly(vinylidene fluoride) (PVDF) and voltage-sensitive ceramic three-phase composite.
Technical background
Piezo-electricity composite material is a kind of type material consisted of recombining process piezoelectric ceramics phase (as PZT) and high molecular polymer (PVDF, other multipolymers).Piezoceramic material has that piezoelectric property is excellent, dielectric loss is low and the advantage such as electromechanical coupling factor is large, but its one-tenth is hard and crisp, not easily forming process, and impact resistance is poor.And although piezopolymer has that density is low, snappiness good, can be prepared into large and uniform film, but its piezoelectric property is poor.Piezo-electricity composite material has the advantage of pottery and polymkeric substance concurrently, and can suppress respective shortcoming, and cost is low, is suitable for commercially producing and being studied widely.
In current piezo-electricity composite material system, because the specific inductivity (ε) of piezoelectric ceramics is generally greater than 1000, and the specific inductivity of PVDF (ε) is about 10, the electric property difference of two phase material is too large, piezoelectric ceramics in system is polarized mutually very difficult, and then cause overall piezoelectric property undesirable, therefore by carrying out modification to piezo-electricity composite material, as improved interfacial bonding property to improve or to improve electric property.In document, report adds third phase conductive phase as silver powder, Graphene etc., increase matrix conductance, improve the polarizing voltage be distributed on ceramic phase, improve macroscopic polarization performance, improve specific inductivity and piezoelectric constant, but along with conductive phase content be increased to a certain threshold value (percolation threshold) time, the specific conductivity of matrix material sharply increases, conducting particles forms connection circuit, and leakage current sharply increases, and easily punctures during polarization.
Voltage-sensitive ceramic is a kind of resistance value along with impressed voltage change has the semiconductor material of a significant nonlinearities change, there is nonlinear wind vibration, under a certain critical voltage, resistance value is very high, does not almost have electric current, but when exceeding this critical voltage, resistance will sharply change, and have electric current to pass through, with a little increase of voltage, electric current can increase very soon.Utilize the nonlinear resistance property of voltage-sensitive ceramic to can be made into varistor, it is large that it has nonlinear factor, and temperature conefficient of voltage is little, resistance to heavy current impact, and the advantages such as Surge handling capability is strong, can play the effect of overvoltage protection, anti-lightning, suppression momentary pulse.
Summary of the invention
The object of the invention is to solve piezo-electricity composite material piezoelectric property difference and the low shortcoming such as easily to puncture of the resistance to polarizing voltage of piezo-electricity composite material after adding conductive phase, and provide that a kind of piezoelectric property is good, the simple piezo-electricity composite material of preparation technology.
To achieve these goals, the technical solution adopted in the present invention is: a kind of piezo-electricity composite material, it is characterized in that: comprise piezoelectric ceramics and poly(vinylidene fluoride) (PVDF), its mass percent consists of: piezoelectric ceramics 50% ~ 98%, poly(vinylidene fluoride) 2% ~ 50%; Also be added with pressure sensitive, described pressure sensitive accounts for 0.1% ~ 10% of piezoelectric ceramics and poly(vinylidene fluoride) gross weight.
As a further improvement on the present invention, described piezoelectric ceramics is for containing lead piezoelectric ceramics Pb-based lanthanumdoped zirconate titanates (PZT) or leadless piezoelectric ceramics.
As a further improvement on the present invention, described voltage-sensitive ceramic is ZnO, SnO
2, TiO
2, SrTiO
3etc. one or more in the material of system.
As a further improvement on the present invention, the preparation method of described piezo-electricity composite material is as follows:
One, described piezoelectric ceramics and voltage-sensitive ceramic are again finely ground into powder after burning till;
Two, piezoelectric ceramic powder, PVDF powder are mixed with into mixed powder with voltage-sensitive ceramic powder three-phase, and the dry-pressing formed diameter of preparing of pressure adopting 5 ~ 10 Mpa is 10 ~ 20 mm, and thickness is the disk of 1 ~ 3 mm;
Three, disk is hot-forming on vulcanizing press is prepared into Piezoelectric anisotropy sheet, and hot-forming condition is: hot pressing temperature 180 ~ 200 DEG C, pressure 5 ~ 20 Mpa, dwell time 30 ~ 120 min;
Four, Piezoelectric anisotropy sheet top and bottom are by electrode, and described electrode slurry is conductive resin or low-temperature silver slurry, adopt the method preparation of silk screen printing or magnetron sputtering;
Five, Piezoelectric anisotropy sheet polarizes in silicone oil/transformer oil, and polarization condition is: polarizing voltage is 3kV/mm ~ 10kV/mm, and poling temperature 110 DEG C ~ 130 DEG C, the polarization time is 20 ~ 90 min.
As a further improvement on the present invention, adopt flow casting molding to prepare after described piezoelectric ceramic powder, PVDF powder and voltage-sensitive ceramic powder three-phase are mixed with form slurry film that thickness is 0.05 ~ 0.5 mm, which floor pellicular cascade is hot-forming prepares composite membrane, and circular piezoelectric composite sheet is made in punching.
The invention has the beneficial effects as follows:
1, voltage-sensitive ceramic is joined in piezoelectric ceramics/PVDF piezo-electricity composite material as middle layer, serve as a connection, improve piezoelectric ceramics and PVDF interfacial bonding property, increase piezoelectric ceramics and being coupled between PVDF, promote the migration of electronics between ceramic particle, improve effective polarizing voltage of ceramic phase;
2, utilize the nonlinear wind vibration of voltage-sensitive ceramic, improve the resistance to polarizing voltage of piezo-electricity composite material, improve the overall piezoelectric property of matrix material;
Present invention process is simple, with low cost, can prepare the piezo-electricity composite material of excellent combination property, can prepare large size Piezoelectric anisotropy film, be expected to be applied to piezoelectricity Trackpad, realizes industrialization and produces.
Embodiment
In order to deepen the understanding of the present invention, below in conjunction with embodiment, the invention will be further described, and all embodiments only for explaining the present invention, do not form limiting the scope of the present invention.
Below with the piezoelectric ceramics (Pb of low-k, low Curie temperature
1-xla
x) (Zr
1-yti
y)
1-4/xo
3(being denoted as PLZT, x=0.01 ~ 0.09, y=0.4 ~ 0.6), PVDF and voltage-sensitive ceramic three-phase piezo-electricity composite material are example, are described in detail the present invention.
Embodiment 1:
Adopt conventional solid-state method to prepare PLZT, according to stoichiometric, through batch mixing, pre-burning, rolling formation, punching, binder removal, burn till and prepare piezoelectric ceramic piece, its performance is: ε
33 t/ ε
0=2000 ± 250, tan δ=1.5% ~ 3.0%, d
33> 300 pC/N, by ceramic plate vibration in vibrating ball mill, crosses the mesh screen of different meshes, is prepared into varigrained PLZT ceramics powder stand-by.
By account for PLZT and PVDF compound gross weight 1.5% TiO
2voltage-sensitive ceramic powder joins in stainless steel cup, add the PVDF powder ultrasonic disperse 15min that massfraction is 4.7% after adding alcohol ultrasonic disperse 5min, after add massfraction be 95.3% 250 ~ 300 object piezoelectric ceramic powder electric stirrings evaporation alcohols for three-phase powder mix.Adopt the dry-pressing formed diameter of preparing of the pressure of 10 Mpa to be 17.6mm, thickness is the disk of 2 mm, and disk is hot-forming on vulcanizing press is prepared into Piezoelectric anisotropy sheet, and hot-forming condition is: hot pressing temperature 180 DEG C, pressure 10 Mpa, dwell time 30 min.Piezoelectric anisotropy sheet top and bottom Screen-printed conductive glue; Piezoelectric anisotropy sheet polarizes in transformer oil, and polarization condition is: polarizing voltage is 8kV/mm, poling temperature 120 DEG C, and the polarization time is 30 min.The performance and characteristic of adding pressure sensitive and blank group are tested, specifically in table 1 and table 2.
The piezoelectric property of table 1 piezo-electricity composite material
Embodiment 2:
The preparation method of PLZT ceramics powder is with embodiment 1.
The ZnO voltage-sensitive ceramic powder of account for PLZT and PVDF compound gross weight 0.5% is joined in stainless steel cup, add a certain amount of dispersion agent, after ultrasonic disperse 1h, add the PVDF that massfraction is 4.7%, dissolve completely until PVDF, add the PLZT ceramics powder that massfraction is 95.3%, pour in homemade casting device after rotary evaporation to required viscosity after electric stirring 4h, strike off and dry the thick film of obtained 0.2 ~ 0.4 mm, double-layer films is superimposed upon hot-formingly on vulcanizing press prepares composite membrane, diameter 8.9 mm is made in composite membrane punching, thickness is 0.4 ~ 0.6mm circular piezoelectric composite sheet, wherein hot-forming condition is: hot pressing temperature 180 DEG C, pressure 10 Mpa, dwell time 30 min.Piezoelectric anisotropy sheet top and bottom Screen-printed conductive glue, polarize in transformer oil, polarization condition is: polarizing voltage is 8 kV/mm, poling temperature 120 DEG C, and the polarization time is 30 min, tests its piezoelectric property: ε=186, d after placing 24h
33=75 pC/N, insulation resistance is 62.3 G Ω.The performance and characteristic of adding pressure sensitive and blank group are tested, specifically in table 3 and table 4.
The piezoelectric property of table 2 piezo-electricity composite material
Claims (5)
1. a piezo-electricity composite material, is characterized in that: comprise piezoelectric ceramics and poly(vinylidene fluoride) (PVDF), its mass percent consists of: piezoelectric ceramics 50% ~ 98%, poly(vinylidene fluoride) 2% ~ 50%; Also be added with pressure sensitive, described pressure sensitive accounts for 0.1% ~ 10% of piezoelectric ceramics and poly(vinylidene fluoride) gross weight.
2. piezo-electricity composite material according to claim 1, is characterized in that: described piezoelectric ceramics is for containing lead piezoelectric ceramics Pb-based lanthanumdoped zirconate titanates (PZT) being or leadless piezoelectric ceramics.
3. piezo-electricity composite material according to claim 1, is characterized in that: described voltage-sensitive ceramic is ZnO, SnO
2, TiO
2, SrTiO
3etc. one or several in system.
4., according to the preparation method of the piezo-electricity composite material in claim 1 ~ 3 described in any one, it is characterized in that:
One, described piezoelectric ceramics and voltage-sensitive ceramic are again finely ground into powder after burning till;
Two, piezoelectric ceramic powder, PVDF powder are mixed with into mixed powder with voltage-sensitive ceramic powder three-phase, and the dry-pressing formed diameter of preparing of pressure adopting 5 ~ 10 Mpa is 10 ~ 20 mm, and thickness is the disk of 1 ~ 3 mm;
Three, disk is hot-forming on vulcanizing press is prepared into Piezoelectric anisotropy sheet, and hot-forming condition is: hot pressing temperature 180 ~ 200 DEG C, pressure 5 ~ 20 Mpa, dwell time 30 ~ 120 min;
Four, Piezoelectric anisotropy sheet top and bottom are by electrode, and described electrode slurry is conductive resin or low-temperature silver slurry, adopt the method preparation of silk screen printing or magnetron sputtering;
Five, Piezoelectric anisotropy sheet polarizes in silicone oil/transformer oil, and polarization condition is: polarizing voltage is 3kV/mm ~ 10kV/mm, and poling temperature 110 DEG C ~ 130 DEG C, the polarization time is 20 ~ 90 min.
5. the preparation method of piezo-electricity composite material according to claim 4, it is characterized in that: in described step 2 and step 3, adopt flow casting molding to prepare after piezoelectric ceramic powder, PVDF powder and voltage-sensitive ceramic powder three-phase are mixed with form slurry film that thickness is 0.05 ~ 0.5 mm, hot-formingly after which floor pellicular cascade prepare composite membrane, circular piezoelectric composite sheet is made in punching.
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Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105449095A (en) * | 2015-12-31 | 2016-03-30 | 长安大学 | Piezoelectric composite material for road construction and preparation method of piezoelectric composite material |
| CN106278263A (en) * | 2016-08-10 | 2017-01-04 | 湖南文理学院 | The preparation method of leadless piezoelectric ceramic thin film |
| CN106549100A (en) * | 2016-10-27 | 2017-03-29 | 北京航空航天大学 | A kind of preparation method of new Piezoelectric anisotropy thin film sensor |
| CN106571423A (en) * | 2016-10-27 | 2017-04-19 | 北京航空航天大学 | Preparation method for preparing novel piezoelectric composite film in acicular underwater acoustic transducer |
| CN107262172A (en) * | 2017-08-03 | 2017-10-20 | 江苏大学 | A kind of design and preparation method of lubricating oil fine particle separating device |
| CN108749015A (en) * | 2018-05-11 | 2018-11-06 | 横店集团东磁股份有限公司 | A kind of high magnetic permeability inhales the preparation method of thickness of convolution piece |
| CN109369144A (en) * | 2018-12-07 | 2019-02-22 | 武汉理工大学 | A kind of 0-3 type PZT- steel slag piezo-electricity composite material |
| KR101971797B1 (en) * | 2017-10-27 | 2019-04-23 | 한국과학기술연구원 | Membrane for water treatment and manufacturing method for the same |
| CN111460935A (en) * | 2020-03-18 | 2020-07-28 | 南昌欧菲生物识别技术有限公司 | Ultrasonic fingerprint identification module, preparation method and electronic equipment |
| CN112226867A (en) * | 2020-08-19 | 2021-01-15 | 西安工程大学 | Method for preparing super-soft piezoelectric PVDF yarn |
| CN112239327A (en) * | 2020-10-14 | 2021-01-19 | 北京化工大学 | Piezoelectric intelligent material for active control of structural vibration |
| CN112646296A (en) * | 2020-12-21 | 2021-04-13 | 之江实验室 | Preparation method of 0-0-3 type flexible piezoelectric composite film |
| CN113512261A (en) * | 2021-04-23 | 2021-10-19 | 苏州攀特电陶科技股份有限公司 | High-sensitivity piezoelectric composite material for touch feedback and preparation method thereof |
| CN113624370A (en) * | 2021-07-28 | 2021-11-09 | 东莞市万科建筑技术研究有限公司 | Building outer wall monitoring module and building |
| CN115240796A (en) * | 2022-07-15 | 2022-10-25 | 北京航空航天大学 | Method for constructing dielectric constant model of graphene-doped piezoelectric polymer matrix composite material |
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Cited By (19)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105449095A (en) * | 2015-12-31 | 2016-03-30 | 长安大学 | Piezoelectric composite material for road construction and preparation method of piezoelectric composite material |
| CN106278263B (en) * | 2016-08-10 | 2019-02-19 | 湖南文理学院 | The preparation method of leadless piezoelectric ceramic thin film |
| CN106278263A (en) * | 2016-08-10 | 2017-01-04 | 湖南文理学院 | The preparation method of leadless piezoelectric ceramic thin film |
| CN106549100A (en) * | 2016-10-27 | 2017-03-29 | 北京航空航天大学 | A kind of preparation method of new Piezoelectric anisotropy thin film sensor |
| CN106571423A (en) * | 2016-10-27 | 2017-04-19 | 北京航空航天大学 | Preparation method for preparing novel piezoelectric composite film in acicular underwater acoustic transducer |
| CN107262172A (en) * | 2017-08-03 | 2017-10-20 | 江苏大学 | A kind of design and preparation method of lubricating oil fine particle separating device |
| KR101971797B1 (en) * | 2017-10-27 | 2019-04-23 | 한국과학기술연구원 | Membrane for water treatment and manufacturing method for the same |
| CN108749015A (en) * | 2018-05-11 | 2018-11-06 | 横店集团东磁股份有限公司 | A kind of high magnetic permeability inhales the preparation method of thickness of convolution piece |
| CN108749015B (en) * | 2018-05-11 | 2020-06-19 | 横店集团东磁股份有限公司 | Preparation method of high-permeability wave-absorbing thick sheet |
| CN109369144A (en) * | 2018-12-07 | 2019-02-22 | 武汉理工大学 | A kind of 0-3 type PZT- steel slag piezo-electricity composite material |
| CN111460935A (en) * | 2020-03-18 | 2020-07-28 | 南昌欧菲生物识别技术有限公司 | Ultrasonic fingerprint identification module, preparation method and electronic equipment |
| CN112226867A (en) * | 2020-08-19 | 2021-01-15 | 西安工程大学 | Method for preparing super-soft piezoelectric PVDF yarn |
| CN112239327A (en) * | 2020-10-14 | 2021-01-19 | 北京化工大学 | Piezoelectric intelligent material for active control of structural vibration |
| CN112646296A (en) * | 2020-12-21 | 2021-04-13 | 之江实验室 | Preparation method of 0-0-3 type flexible piezoelectric composite film |
| CN113512261A (en) * | 2021-04-23 | 2021-10-19 | 苏州攀特电陶科技股份有限公司 | High-sensitivity piezoelectric composite material for touch feedback and preparation method thereof |
| CN113624370A (en) * | 2021-07-28 | 2021-11-09 | 东莞市万科建筑技术研究有限公司 | Building outer wall monitoring module and building |
| CN113624370B (en) * | 2021-07-28 | 2023-08-04 | 东莞市万科建筑技术研究有限公司 | Building outer wall monitoring module and building |
| CN115240796A (en) * | 2022-07-15 | 2022-10-25 | 北京航空航天大学 | Method for constructing dielectric constant model of graphene-doped piezoelectric polymer matrix composite material |
| CN115240796B (en) * | 2022-07-15 | 2023-08-04 | 北京航空航天大学 | Construction method of dielectric constant model of graphene doped piezoelectric polymer matrix composite material |
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