CN104425705A - Polarization method of polyvinylidene fluoride thin film - Google Patents
Polarization method of polyvinylidene fluoride thin film Download PDFInfo
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- CN104425705A CN104425705A CN201310407026.3A CN201310407026A CN104425705A CN 104425705 A CN104425705 A CN 104425705A CN 201310407026 A CN201310407026 A CN 201310407026A CN 104425705 A CN104425705 A CN 104425705A
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- Prior art keywords
- polyvinylidene difluoride
- metal electrode
- thin film
- heater
- polyvinylidene fluoride
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- 229920002981 polyvinylidene fluoride Polymers 0.000 title claims abstract description 63
- 230000010287 polarization Effects 0.000 title claims abstract description 22
- 238000000034 method Methods 0.000 title claims abstract description 16
- 239000002033 PVDF binder Substances 0.000 title abstract description 14
- 239000010409 thin film Substances 0.000 title abstract description 11
- 229910052751 metal Inorganic materials 0.000 claims abstract description 29
- 239000002184 metal Substances 0.000 claims abstract description 29
- 238000001704 evaporation Methods 0.000 claims abstract description 9
- 229910052709 silver Inorganic materials 0.000 claims abstract description 6
- 239000004332 silver Substances 0.000 claims abstract description 6
- 229920002545 silicone oil Polymers 0.000 claims description 20
- 230000008020 evaporation Effects 0.000 claims description 8
- 239000010408 film Substances 0.000 abstract description 50
- 230000005616 pyroelectricity Effects 0.000 abstract description 6
- 230000005621 ferroelectricity Effects 0.000 abstract description 5
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 abstract 3
- 239000003921 oil Substances 0.000 abstract 3
- 229910052710 silicon Inorganic materials 0.000 abstract 3
- 239000010703 silicon Substances 0.000 abstract 3
- 238000001816 cooling Methods 0.000 abstract 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 5
- 239000002800 charge carrier Substances 0.000 description 3
- 230000015556 catabolic process Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- BQCIDUSAKPWEOX-UHFFFAOYSA-N 1,1-Difluoroethene Chemical compound FC(F)=C BQCIDUSAKPWEOX-UHFFFAOYSA-N 0.000 description 1
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 150000001338 aliphatic hydrocarbons Chemical class 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000007334 copolymerization reaction Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000005516 deep trap Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- NBVXSUQYWXRMNV-UHFFFAOYSA-N fluoromethane Chemical group FC NBVXSUQYWXRMNV-UHFFFAOYSA-N 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 239000007777 multifunctional material Substances 0.000 description 1
- 239000002798 polar solvent Substances 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 230000008961 swelling Effects 0.000 description 1
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- Treatments Of Macromolecular Shaped Articles (AREA)
Abstract
The invention discloses a polarization method of a polyvinylidene fluoride thin film. The polarization method comprises the following steps: S1. evaporating silver which is 90-100nm on the upper and lower planes of the polyvinylidene fluoride thin film as a metal electrode; S2. pouring silicon oil into a heater and putting the polyvinylidene fluoride thin film plated with the metal electrode into silicon oil of the heater; S3. adjusting the temperature of silicon oil in the heater to 80-90 DEG C and applying a voltage to the polyvinylidene fluoride thin film plated with the metal electrode, wherein the voltage applied to the polyvinylidene fluoride thin film plated with the metal electrode is 130-140MV/m for 50-60 minutes; and S4. taking out the polyvinylidene fluoride thin film in the heater and cooling at normal temperature to obtain the polarized polyvinylidene fluoride thin film. The polarized polyvinylidene fluoride thin film disclosed by the invention is good in piezoelectricity, ferroelectricity and pyroelectricity and low in film puncture rate, so that the manufacturing cost of the polyvinylidene fluoride thin film can be lowered, and the polarization method is convenient to popularize and apply.
Description
Technical field
The present invention relates to the manufacturing technology field of film, specifically the polarization method of polyvinylidene difluoride film.
Background technology
PVDF(Kynoar) be fluorine-containing multifunctional material by vinylidene fluoride monomers homopolymerization or copolymerization, be linear, crystalline polymer, its degree of crystallinity is generally between 50 ~ 70%.Because the combination of fluorocarbon chain can be high, there is good heat-resisting, decay resistance, the temperature range be suitable for is-40 ~ 150 DEG C, can antioxidant, acid, alkali, the corrosion of salt and halogen, aromatic hydrocarbons, aliphatic hydrocarbon and chlorinated solvent and swelling, there is excellent uvioresistant and ageing-resistant performance, and there is the features, particularly this material such as nonpolar, antipollution can be dissolved in polar solvent and be mixed with polymer solution.(as quartz, piezoelectric ceramic class) is compared compared with at present conventional inorganic matter piezoelectric, and Kynoar also has that acoustic impedance is little, frequency response is wide, dielectric constant is little, resistance to impact is strong, is convenient to be processed into the advantages such as arbitrary shape.
PVDF from solution or under molten condition crystallization not there is the characteristics such as piezoelectricity, ferroelectric, pyroelectricity.Polarization is an important step in PVDF material processed, main purpose allows the molecular dipole electric moment of mixed and disorderly orientation in ferroelectric along the consistent orientation of specific direction (polarized electric field direction), improves the piezoelectricity of PVDF thin film, ferroelectricity and pyroelectricity characteristic.In the process that polyvinylidene difluoride film is polarized, easily there is the phenomenon that film is breakdown now, this adds increased the manufacturing cost of polyvinylidene difluoride film.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, provide a kind of polarization method of polyvinylidene difluoride film, it by controlling to the process conditions of polarization the probability reducing film breakdown, and then can reduce the manufacturing cost of polyvinylidene difluoride film.
Object of the present invention is achieved through the following technical solutions:
The polarization method of polyvinylidene difluoride film, comprises the following steps:
Step one, be that the silver of 90 ~ 100nm is as metal electrode using equal for the lower planes of polyvinylidene difluoride film evaporation thickness;
Step 2, in heater, pour silicone oil into, and the polyvinylidene difluoride film being coated with metal electrode is put into the silicone oil of heater;
Step 3, silicone oil temperature in heater is adjusted to 80 ~ 90 DEG C, and apply voltage to the Kynoar being coated with metal electrode, wherein, the voltage of applying is 130 ~ 140MV/m on the polyvinylidene difluoride film being coated with metal electrode, and the duration is 50 ~ 60min;
Step 4, the polyvinylidene difluoride film taken out in heater cool at normal temperatures and obtain the polyvinylidene difluoride film after polarizing.
Wherein, polarizing voltage increases, deposited charge amount increases, the number of dipole deflection simultaneously also increases, and marshalling, also will make the piezoelectricity of composite membrane improve, but voltage is too high, leakage current increases, and easily punctured by film, therefore the voltage of applying is 130 ~ 140MV/m by the present invention on the polyvinylidene difluoride film being coated with metal electrode.Poling temperature raises, and electric dipole, ion and other charge carrier heat movement speeds are large on the one hand, are conducive to the migration of dipole orientation and charge carrier.On the other hand due to high temperature, charge carrier energy of thermal motion is large, be conducive to deep trap to catch, and be unfavorable for that shallow well is caught, the piezoelectricity ferro body of good stability can be formed, but temperature is too high, in film, leakage conductance increases, easily cause puncturing of film, therefore silicone oil temperature in heater is adjusted to 80 ~ 90 DEG C by the present invention, and namely poling temperature is 80 ~ 90 DEG C.Be not more then an independently factor as the polarization time, and by the restriction of polarizing voltage and poling temperature, when polarizing voltage and poling temperature limit, the present invention set the polarization time in 50 ~ 60min.
Further, the metal electrode thickness of the lower planes evaporation of described polyvinylidene difluoride film is 95nm.
Further, in described heater, silicone oil temperature is 85 DEG C, and being applied to the voltage be coated with on the polyvinylidene difluoride film of metal electrode in described step 3 is 135MV/m, and the duration of polarization is 55min.
Compared with prior art, the present invention has following beneficial effect: (1) the present invention is by the lower planes evaporation silver metal electrodes at polyvinylidene difluoride film, and in heater, add silicone oil as dielectric, and set poling temperature and polarizing voltage is come polyvinylidene difluoride film, integrated artistic is simple, and thoroughly, polarization rear stability is good in polarization, film occurs that the probability punctured is lower, and then can reduce the manufacturing cost of polyvinylidene difluoride film.
(2) dielectric of the present invention adopts silicone oil, and its good insulating, dielectric constant is high, can avoid high-tension edge arcing.
Embodiment
Below in conjunction with embodiment, the present invention is described in further detail, but embodiments of the present invention are not limited thereto.
Embodiment 1
The polarization method of polyvinylidene difluoride film, comprises the following steps: step one, be that the silver of 90nm is as metal electrode using equal for the lower planes of polyvinylidene difluoride film evaporation thickness; Step 2, in heater, pour silicone oil into, and the polyvinylidene difluoride film being coated with metal electrode is put into the silicone oil of heater; Step 3, silicone oil temperature in heater is adjusted to 80 DEG C, and applies voltage to the Kynoar being coated with metal electrode, wherein, the voltage of applying is 130MV/m on the polyvinylidene difluoride film being coated with metal electrode, and the duration is 60min; Step 4, the polyvinylidene difluoride film taken out in heater cool at normal temperatures and obtain the polyvinylidene difluoride film after polarizing.Adopt the present embodiment polarize the polyvinylidene difluoride film obtained, well, film punctures rate and is less than 0.1% for piezoelectricity, ferroelectricity and pyroelectricity characteristic.
Embodiment 2
The polarization method of polyvinylidene difluoride film, comprises the following steps: step one, be that the silver of 95nm is as metal electrode using equal for the lower planes of polyvinylidene difluoride film evaporation thickness; Step 2, in heater, pour silicone oil into, and the polyvinylidene difluoride film being coated with metal electrode is put into the silicone oil of heater; Step 3, silicone oil temperature in heater is adjusted to 85 DEG C, and applies voltage to the Kynoar being coated with metal electrode, wherein, the voltage of applying is 135MV/m on the polyvinylidene difluoride film being coated with metal electrode, and the duration is 55min; Step 4, the polyvinylidene difluoride film taken out in heater cool at normal temperatures and obtain the polyvinylidene difluoride film after polarizing.Adopt the present embodiment polarize the polyvinylidene difluoride film obtained, well, film punctures rate and is less than 0.13% for piezoelectricity, ferroelectricity and pyroelectricity characteristic.
Embodiment 3
The polarization method of polyvinylidene difluoride film, comprises the following steps: step one, be that the silver of 100nm is as metal electrode using equal for the lower planes of polyvinylidene difluoride film evaporation thickness; Step 2, in heater, pour silicone oil into, and the polyvinylidene difluoride film being coated with metal electrode is put into the silicone oil of heater; Step 3, silicone oil temperature in heater is adjusted to 90 DEG C, and applies voltage to the Kynoar being coated with metal electrode, wherein, the voltage of applying is 140MV/m on the polyvinylidene difluoride film being coated with metal electrode, and the duration is 50min; Step 4, the polyvinylidene difluoride film taken out in heater cool at normal temperatures and obtain the polyvinylidene difluoride film after polarizing.Adopt the present embodiment polarize the polyvinylidene difluoride film obtained, well, film punctures rate and is less than 0.15% for piezoelectricity, ferroelectricity and pyroelectricity characteristic.
Above content is the further description done the present invention in conjunction with concrete preferred implementation, can not assert that the specific embodiment of the present invention is confined to these explanations.For general technical staff of the technical field of the invention, not departing from other execution modes drawn under technical scheme of the present invention, all should be included in protection scope of the present invention.
Claims (3)
1. the polarization method of polyvinylidene difluoride film, is characterized in that, comprises the following steps:
Step one, be that the silver of 90 ~ 100nm is as metal electrode using equal for the lower planes of polyvinylidene difluoride film evaporation thickness;
Step 2, in heater, pour silicone oil into, and the polyvinylidene difluoride film being coated with metal electrode is put into the silicone oil of heater;
Step 3, silicone oil temperature in heater is adjusted to 80 ~ 90 DEG C, and apply voltage to the Kynoar being coated with metal electrode, wherein, the voltage of applying is 130 ~ 140MV/m on the polyvinylidene difluoride film being coated with metal electrode, and the duration is 50 ~ 60min;
Step 4, the polyvinylidene difluoride film taken out in heater cool at normal temperatures and obtain the polyvinylidene difluoride film after polarizing.
2. the polarization method of polyvinylidene difluoride film according to claim 1, is characterized in that, the metal electrode thickness of the lower planes evaporation of described polyvinylidene difluoride film is 95nm.
3. the polarization method of polyvinylidene difluoride film according to claim 1 and 2, it is characterized in that, in described heater, silicone oil temperature is 85 DEG C, and being applied to the voltage be coated with on the polyvinylidene difluoride film of metal electrode in described step 3 is 135MV/m, and the duration of polarization is 55min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201310407026.3A CN104425705A (en) | 2013-09-10 | 2013-09-10 | Polarization method of polyvinylidene fluoride thin film |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201310407026.3A CN104425705A (en) | 2013-09-10 | 2013-09-10 | Polarization method of polyvinylidene fluoride thin film |
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| CN104425705A true CN104425705A (en) | 2015-03-18 |
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| CN201310407026.3A Pending CN104425705A (en) | 2013-09-10 | 2013-09-10 | Polarization method of polyvinylidene fluoride thin film |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107261205A (en) * | 2017-06-13 | 2017-10-20 | 北京大学口腔医学院 | A kind of powered tissue repair film and preparation method thereof that prevents adhesion |
| CN108886090A (en) * | 2016-03-28 | 2018-11-23 | 大金工业株式会社 | Bimorph type piezoelectric film |
| CN110042481A (en) * | 2019-04-26 | 2019-07-23 | 西安工程大学 | A kind of device and method of continuous production piezoelectric fabric |
| CN110306248A (en) * | 2019-06-14 | 2019-10-08 | 西安工程大学 | A kind of continuous producing method and device of PVDF piezoelectric fabric |
| CN112606509A (en) * | 2020-12-16 | 2021-04-06 | 昆山微电子技术研究院 | Self-polarized composite electret-piezoelectric film, preparation method thereof and piezoelectric film sensor |
-
2013
- 2013-09-10 CN CN201310407026.3A patent/CN104425705A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108886090A (en) * | 2016-03-28 | 2018-11-23 | 大金工业株式会社 | Bimorph type piezoelectric film |
| CN108886090B (en) * | 2016-03-28 | 2022-10-18 | 大金工业株式会社 | Bimorph type piezoelectric film |
| CN107261205A (en) * | 2017-06-13 | 2017-10-20 | 北京大学口腔医学院 | A kind of powered tissue repair film and preparation method thereof that prevents adhesion |
| CN110042481A (en) * | 2019-04-26 | 2019-07-23 | 西安工程大学 | A kind of device and method of continuous production piezoelectric fabric |
| CN110306248A (en) * | 2019-06-14 | 2019-10-08 | 西安工程大学 | A kind of continuous producing method and device of PVDF piezoelectric fabric |
| CN112606509A (en) * | 2020-12-16 | 2021-04-06 | 昆山微电子技术研究院 | Self-polarized composite electret-piezoelectric film, preparation method thereof and piezoelectric film sensor |
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Application publication date: 20150318 |
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