CN102569641A - Method for producing piezoelectric electret functional films with piezoelectric coefficient d31 - Google Patents
Method for producing piezoelectric electret functional films with piezoelectric coefficient d31 Download PDFInfo
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- CN102569641A CN102569641A CN201210005276XA CN201210005276A CN102569641A CN 102569641 A CN102569641 A CN 102569641A CN 201210005276X A CN201210005276X A CN 201210005276XA CN 201210005276 A CN201210005276 A CN 201210005276A CN 102569641 A CN102569641 A CN 102569641A
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Abstract
The invention belongs to the technical field of piezoelectric function materials, and particularly relates to a method for producing piezoelectric electret functional films with piezoelectric coefficient d31. The method comprises the steps that non-polar polymer materials form thin polymer films on the surface of a template having grooves through impressing, spray-coating, lifting or spin-coating, the shape of the thin films is the same with that of the template structure, and the thickness of the thin films is between 1mu m and 200mu m; porous structure composite films on which grooves and dense portions are arranged alternately are obtained through hot-pressing bonding of two polymer films having the same structure; and finally the composite films are polarized via a corona charging process or a contact charging process so as to obtain the piezoelectric electret functional films. The piezoelectric electret having grooves obtained through the method has the high piezoelectric coefficient d31 (or d32). The piezoelectric electret functional films can be applied in the fields such as energy collectors, acoustoelectric sensors, robot skins, intelligent structures, opto-acoustic sensors and the like.
Description
Technical field
The invention belongs to the piezoelectricity technical field of function materials, be specifically related to a kind of piezoelectric modulus that has
d 31The preparation method of piezo-electric electret functional membrane.
Background technology
Piezo-electric electret piezoelectrets (being also referred to as ferroelectric electret ferroelectrets) is one type of novel artificial micro-structural piezoelectricity functional material.Do not have intrinsic electric dipole in the piezo-electric electret material, this is its key character that is different from traditional inorganic piezoelectric material (piezoelectric monocrystal or piezoelectric ceramic etc.) and organic piezoelectric polymer thin-film (Kynoar or its copolymer).Since the scientist of Finland found to suppress electrical effect in the polypropylene porous material before and after nineteen ninety, the piezo-electric electret functional material had received the extensive concern of domestic and international scientific circles and sensor technical field.Piezo-electric electret has the pliability of suppressing electrical effect and piezopolymer of piezoelectric ceramic concurrently; But and large tracts of land film forming; Cheap environmental protection, therefore acoustic impedance and human body and water coupling have boundless application prospect at aspects such as Based Intelligent Control, transducer and actuators.
But the prepared in laboratory of being reported so far only has strong ess-strain coefficient with commercial piezo-electric electret functional membrane
d 33, and its piezoelectric modulus
d 31Very little (between 1-3pC/N, therefore ignoring usually usually) is much smaller than the piezoelectric modulus of Kynoar
d 31(about 25pC/N).On the other hand, (for example bridge structure detection, suspension cable intelligent monitoring etc.) need piezoelectric to have stronger piezoelectric modulus in the middle of many application
d 31, existing piezo-electric electret film can not satisfy this requirement.
Summary of the invention
The object of the present invention is to provide a kind of preparation to have the electric stress of the suppressing coefficient of strain
d 31The method of piezo-electric electret functional membrane.Not only can make the piezo-electric electret functional membrane have piezoelectric modulus with this method
d 33, and have strong piezoelectric modulus
d 31(its piezoelectric modulus
d 31>25 pC/N).
In order to achieve the above object; The present invention is the non-polar polymer material, utilizes impress, spray, lift or technology such as spin coating, forms and the identical shaped thin polymer film of formwork structure at the template surface that is having groove structure; The thickness of film is between 1 μ m~200 μ m; With the polymer film heat pressure adhesive of two same structures, obtain groove and closely knit part pore space structure film alternately then, at last to the film processing that polarizes.
Among the present invention, said non-polar polymer material can be selected polypropylene (PP), polyester (PET and PEN), the rare copolymer of fluorinated ethylene-propylene (FEP), polytetrafluoroethylene (PTFE) or cyclic olefine copolymer (COC) etc.
Among the present invention, said polarization is handled can adopt corona charging technology or contact method charge technology.When adopting corona charging technology; Corona charging voltage is ± 2kV~± 100kV, gate control voltage is ± 50V~± 10kV, charging temperature is less than or equal to the melting temperature of film; Charging interval 5ms~2h; The spacing of electrode and film is 2cm~15cm, and the shape of corona electrode can be the array that needle-like, thread, edge of a knife shape or above-mentioned shape electrode are formed, and obtains to have the electric stress of the suppressing coefficient of strain behind the corona charging
d 31The piezo-electric electret film.When adopting the contact method charge technology; At first at film two sides vacuum evaporation that has the groove micro-structural or screen-printed metal electrode; Then Dc bias directly being loaded on two metal electrodes, the size of Dc bias is ± 100V~± 10kV, charging temperature is less than or equal to the melting temperature of film; Charging interval 5ms~2h obtains having and suppresses the electric coefficient of strain
d 31The piezo-electric electret film.
Advantage of the present invention is:
1, compare with existing piezo-electric electret functional membrane, the piezo-electric electret of the with groove structure that the present invention obtains has the electrostrictive coefficient of suppressing
d 31(or
d 32).
2, the present invention is used simple for process.
3, the piezo-electric electret functional membrane that utilizes the present invention to prepare can be applied in fields such as energy collecting device, acoustoelectric sensor, robot skin, intelligence structure, photoacoustic sensors.
Description of drawings
Fig. 1 is a film surface schematic diagram of the present invention.Wherein, 1 is functional membrane surface groove part, and 2 is functional membrane rat part.
Fig. 2 is the composite membrane generalized section.
Fig. 3 is the sem photograph of film of the present invention.
Fig. 4 be the piezo-electric electret film under 60Hz, be applied to the quantity of electric charge and time relation figure on the film.
Fig. 5 be the piezo-electric electret film under 60Hz, be applied to pressure and time relation figure on the film.
Fig. 6 be the piezo-electric electret film under 80Hz, be applied to the quantity of electric charge and time relation figure on the film.
Fig. 7 be the piezo-electric electret film under 80Hz, be applied to pressure and time relation figure on the film.
Fig. 8 be the piezo-electric electret film under 100Hz, be applied to the quantity of electric charge and time relation figure on the film.
Fig. 9 be the piezo-electric electret film under 100Hz, be applied to pressure and time relation figure on the film.
Embodiment
1, engraving groove structure as shown in Figure 1 on the metallic plate of 5cm*5cm, gash depth is 1mm, width 1mm, two groove pitch are 0.5mm, form the mould that has groove structure.
2, at first one of above-mentioned mould (mould 1) with groove structure is faced up; And be covered with the rubber membrane that commercially available FEP film covers, a slice 1mm is thick that a thickness is 12.5 um successively on the surface of mould 1; With a corrosion resistant plate that 3mm is thick; Then they are positioned on the heating plate of hot press together, are respectively 120 in temperature and pressure
oThe 1min that pressurizes under the condition of C and 11MPa removes corrosion resistant plate and rubber membrane at last, obtains attached to mould 1 surface, and has the fep film 1 of groove structure.
3, utilize the described method of step 2 to obtain, and have the fep film 2 of groove structure attached to mould 2 surfaces.
4, the mould 2 that surface attachment is had the mould 1 of fep film 1 and be attached with fep film 2 fastens (being that fep film 1 is relative with fep film 2) with the mirror image mode, uses metal fixture mold cramping then.
5, put into high temperature furnace to the mould of step 4/fep film system, under 320 ℃ temperature, carry out heat bonding, the time set of heat bonding is 15min.
6, take out mould/fep film system of process step 5 heat bonding, be cooled to room temperature, the demoulding obtains FEP composite membrane as shown in Figure 3, and its inside has the air hole structure of tubulose.
7, giving the two sides vacuum evaporation thickness of FEP composite membrane is the aluminium electrode of 100nm.
8, on the electrode on FEP composite membrane two sides, apply the Dc bias of 2000V, the making alive time is 5 mS, and ambient temperature is 20 ℃.
Through above-mentioned steps 1 to 8, obtain FEP composite membrane piezo-electric electret 1.
With the x direction of principal axis of the sinusoidal force signal excitation FEP composite membrane piezo-electric electret 1 of 60Hz, the change curve that obtains induction electric weight on the axial FEP composite membrane of Z piezo-electric electret 1 surface electrode is as shown in Figure 3.Through calculating,
d 31Be 83 pC/N.
With the x direction of principal axis of the sinusoidal force signal excitation FEP composite membrane piezo-electric electret 1 of 80Hz, the change curve that obtains induction electric weight on the axial FEP composite membrane of Z piezo-electric electret 1 surface electrode is as shown in Figure 4.Through calculating,
d 31Be 82 pC/N.
With the x direction of principal axis of the sinusoidal force signal excitation FEP composite membrane piezo-electric electret 1 of 100Hz, the change curve that obtains induction electric weight on the axial FEP composite membrane of Z piezo-electric electret 1 surface electrode is as shown in Figure 5.Through calculating,
d 31Be 71 pC/ N.
1, engraving groove structure as shown in Figure 1 on the metallic plate of 5cm*5cm, gash depth is 1mm, width 0.5mm, two groove pitch are 0.25mm, form the mould that has groove structure.
2, at first one of above-mentioned mould (mould 3) with groove structure is faced up; And be covered with the commercially available FEP film that a thickness is 12.5 um, the rubber membrane that a slice 1mm is thick successively on the surface of mould 3; With a corrosion resistant plate that 3mm is thick; Then they are positioned on the heating plate of hot press together, are respectively 100 in temperature and pressure
oThe 2min that pressurizes under the condition of C and 11MPa removes corrosion resistant plate and rubber membrane at last, obtains attached to mould 3 surfaces and has the fep film 3 of groove structure.
3, obtain attached to mould 4 surfaces with the described method of step 2, and have the fep film 4 of groove structure.
4, the mould 4 that surface attachment is had the mould 3 of fep film 3 and be attached with fep film 4 fastens (being that fep film 1 is relative with fep film 2) with the mirror image mode, uses metal fixture mold cramping then.
5, put into high temperature furnace to the mould of step 4/fep film system, under 320 ℃ temperature, carry out heat bonding, the time set of heat bonding is 30min.
6, take out mould/fep film system of process step 5 heat bonding, be cooled to room temperature, the demoulding obtains the FEP composite membrane that its inside has the air hole structure of tubulose.
7, giving the two sides vacuum evaporation thickness of FEP composite membrane is the aluminium electrode of 100nm.
8, on the electrode on FEP composite membrane two sides, apply the Dc bias of 2000V, the making alive time is 20 ms, and ambient temperature is 20 ℃.
Through above-mentioned steps 1 to 8, obtain FEP composite membrane piezo-electric electret 2, it is under the excitation of 100Hz sinusoidal force
d 31Be 60 pC/N.
Embodiment 3 can obtain to have piezoelectric modulus according to following steps
d 31FEP composite membrane piezo-electric electret 3.
1, utilizing pin-plate corona charging system that FEP composite membrane 1 is carried out corona charging handles.Corona pin is 4cm apart from the distance on FEP composite membrane 1 surface, corona voltage-20kV, charging interval 5min, ambient temperature 15
oC.
2, giving the two sides vacuum evaporation thickness of FEP composite membrane is the aluminium electrode of 100nm.
Obtain FEP composite membrane piezo-electric electret 3 through above-mentioned steps.
Obtain with the sinusoidal force signal excitation FEP composite membrane piezo-electric electret 3 of 100Hz
d 31Be 50 pC/N.
1, one of mould prepared among the embodiment 11 with groove structure is faced up; And be covered with the commercially available PTFE turning film that a thickness is 20 μ m, the rubber membrane that a slice 1mm is thick successively on the surface of mould 1; With a corrosion resistant plate that 3mm is thick; Then they are positioned on the heating plate of hot press together, are respectively 25 in temperature and pressure
oThe 10min that pressurizes under the condition of C and 5MPa removes corrosion resistant plate and rubber membrane at last, obtains attached to mould 1 surface, and has the PTFE film 1 of groove structure.
2, utilize the described method of step 1 to obtain, and have the PTFE film 2 of groove structure attached to mould 3 surfaces.
3, the mould 2 that surface attachment is had the mould 1 of PTFE film 1 and be attached with PTFE film 2 fastens (being that PTFE film 1 is relative with PTFE film 2) with the mirror image mode, steps up mould with metal fixture then.
4, put into high temperature furnace to the mould of step 3/PTFE film system, under 390 ℃ temperature, carry out sintering, the time set of sintering is 30min.
5, take out mould/PTFE film system of process step 4 sintering, be cooled to room temperature, the demoulding obtains the PTFE composite membrane that its inside has the air hole structure of tubulose.
6, giving the two sides vacuum evaporation thickness of PTFE composite membrane is the aluminium electrode of 100nm.
7, on the electrode on PTFE composite membrane two sides, apply the Dc bias of 5000V, the making alive time is 20 mS, and ambient temperature is 20 ℃.
Through above-mentioned steps 1 to 7, obtain PTFE composite membrane piezo-electric electret 1, it is under the excitation of 100Hz sinusoidal force
d 31Be 80 pC/N.
Embodiment 5 can obtain to have piezoelectric modulus according to following steps
d 31PP composite membrane piezo-electric electret.
1, one of mould prepared among the embodiment 11 with groove structure is faced up; And be covered with the commercially available PP film that a thickness is 10 μ m, the rubber membrane that a slice 1mm is thick successively on the surface of mould 1; With a corrosion resistant plate that 3mm is thick; Then they are positioned on the heating plate of hot press together, are respectively 95 in temperature and pressure
oThe 5min that pressurizes under the condition of C and 10MPa removes corrosion resistant plate and rubber membrane at last, obtains attached to mould 1 surface, and has the PP film 1 of groove structure.
2, utilize the described method of step 1 to obtain, and have the PP film 2 of groove structure attached to mould 3 surfaces.
3, the mould 2 that surface attachment is had the mould 1 of PP film 1 and be attached with PP film 2 fastens (being that PP film 1 is relative with PTFE film 2) with the mirror image mode, uses metal fixture mold cramping then.
4, put into high temperature furnace to the mould of step 3/PP film system, under 180 ℃ temperature, carry out heat bonding, the time set of heat bonding is 5min.
5, take out mould/PP film system of process step 4 sintering, be cooled to room temperature, the demoulding obtains the PP composite membrane that its inside has the air hole structure of tubulose.
6, utilizing pin-plate corona charging system that PP composite membrane 1 is carried out corona charging handles.The distance on corona pin distance P P composite membrane 1 surface is 4cm, corona voltage-25kV, charging interval 1min, ambient temperature 25
oC.
7, giving the two sides vacuum evaporation thickness of PP composite membrane is the aluminium electrode of 100nm.
Through above-mentioned steps 1 to 7, obtain PP composite membrane piezo-electric electret 1, it is under the excitation of 100Hz sinusoidal force
d 31Be 55 pC/N.
Claims (3)
1. one kind has piezoelectric modulus
d 31The preparation method of piezo-electric electret functional membrane; It is characterized in that concrete steps are: the non-polar polymer material; Utilize and impress, spray, lift or spin coating proceeding; Form and the identical shaped thin polymer film of formwork structure at the template surface that has groove structure, the thickness of film is between 1 μ m~200 μ m; With the polymer film heat pressure adhesive of two same structures, obtain groove and closely knit part pore space structure laminated film alternately then; At last to the laminated film processing that polarizes.
2. according to claim 1 have a piezoelectric modulus
d 31The preparation method of piezo-electric electret functional membrane, it is characterized in that said polarization is handled to adopt corona charging technology or contact method charge technology; Wherein, The step of said corona charging technology is: corona charging voltage for ± 2kV~± 100kV, gate control voltage is ± 50V~± 10kV, charging temperature is less than or equal to the melting temperature of film; Charging interval 5ms~2h; The spacing of electrode and film is 2cm~15cm, and the shape of corona electrode is the array that needle-like, thread, edge of a knife shape or above-mentioned shape electrode are formed, and obtains to have the electric stress of the suppressing coefficient of strain behind the corona charging
d 31The piezo-electric electret film; The step of said contact method charge technology is: at first at film two sides vacuum evaporation that has the groove micro-structural or screen-printed metal electrode; Then Dc bias directly is loaded on two metal electrodes; The size of Dc bias is ± 100V~± 10kV; Charging temperature is less than or equal to the melting temperature of film, and charging interval 5ms~2h obtains having and suppresses the electric coefficient of strain
d 31The piezo-electric electret film.
3. according to claim 1 have a piezoelectric modulus
d 31The preparation method of piezo-electric electret functional membrane, it is characterized in that said non-polar polymer material is polypropylene, polyester, the rare copolymer of fluorinated ethylene-propylene, polytetrafluoroethylene or cyclic olefine copolymer.
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Cited By (9)
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CN102856487A (en) * | 2012-09-25 | 2013-01-02 | 同济大学 | Preparation method of functional film of flexible piezoelectric electret |
CN103682083A (en) * | 2012-08-31 | 2014-03-26 | 纳米新能源(唐山)有限责任公司 | Piezoelectric electret film and preparation method thereof |
CN104022688A (en) * | 2014-06-20 | 2014-09-03 | 清华大学 | MEMS electric field energy collector based on electret |
CN104884942A (en) * | 2012-12-28 | 2015-09-02 | 大金工业株式会社 | Polarized resin film and process for producing same |
CN106025060A (en) * | 2016-07-15 | 2016-10-12 | 北京大学 | Wavy piezoelectric composite device and preparation method and application thereof |
CN106863994A (en) * | 2015-12-10 | 2017-06-20 | 华中科技大学 | A kind of preparation method of electric charge self- recoverage electret film |
CN110022087A (en) * | 2019-05-09 | 2019-07-16 | 同济大学 | The energy conversion unit and preparation method of beam type vibration energy collector |
CN111710778A (en) * | 2020-07-27 | 2020-09-25 | 西安交通大学 | Stretchable magnetoelectric electret and preparation method thereof |
CN113410377A (en) * | 2021-05-21 | 2021-09-17 | 同济大学 | Preparation method of flexible transparent electromechanical coupling functional film |
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CN103682083A (en) * | 2012-08-31 | 2014-03-26 | 纳米新能源(唐山)有限责任公司 | Piezoelectric electret film and preparation method thereof |
CN102856487A (en) * | 2012-09-25 | 2013-01-02 | 同济大学 | Preparation method of functional film of flexible piezoelectric electret |
CN104884942A (en) * | 2012-12-28 | 2015-09-02 | 大金工业株式会社 | Polarized resin film and process for producing same |
CN104884942B (en) * | 2012-12-28 | 2019-02-19 | 大金工业株式会社 | Polarize resin film and its manufacturing method |
CN104022688A (en) * | 2014-06-20 | 2014-09-03 | 清华大学 | MEMS electric field energy collector based on electret |
CN106863994A (en) * | 2015-12-10 | 2017-06-20 | 华中科技大学 | A kind of preparation method of electric charge self- recoverage electret film |
CN106863994B (en) * | 2015-12-10 | 2019-02-01 | 华中科技大学 | A kind of preparation method of charge self- recoverage electret film |
CN106025060A (en) * | 2016-07-15 | 2016-10-12 | 北京大学 | Wavy piezoelectric composite device and preparation method and application thereof |
CN110022087A (en) * | 2019-05-09 | 2019-07-16 | 同济大学 | The energy conversion unit and preparation method of beam type vibration energy collector |
CN111710778A (en) * | 2020-07-27 | 2020-09-25 | 西安交通大学 | Stretchable magnetoelectric electret and preparation method thereof |
CN113410377A (en) * | 2021-05-21 | 2021-09-17 | 同济大学 | Preparation method of flexible transparent electromechanical coupling functional film |
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Application publication date: 20120711 |