CN104409626A - Preparation method for polyvinylidene fluoride (PVDF)-based high voltage coefficient thin film - Google Patents
Preparation method for polyvinylidene fluoride (PVDF)-based high voltage coefficient thin film Download PDFInfo
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Abstract
The invention discloses a preparation method for a polyvinylidene fluoride (PVDF)-based high voltage coefficient thin film. The preparation method is characterized in that PVDF-based organic ferroelectric polymers are dissolved in a dimethyl sulfoxide solution; through a Langmuir-Blodgett method, different PVDF-based organic ferroelectric polymers are transferred to a substrate alternately layer by layer; and annealing treatment is performed to remove interface residual solvent and guarantee good crystalline characteristic of the thin film, so as to form a PVDF-based organic polymer compound structure. The preparation method for the PVDF-based high voltage coefficient thin film is simple, can control the thickness of a single layer of thin film precisely, and provides guarantee for research of piezoelectric property of the PVDF-based organic ferroelectric polymer compound structure. Experiments prove that the piezoelectric coefficient of the PVDF-based organic ferroelectric polymer compound structure is remarkably improved.
Description
Technical field
The present invention relates to the technology of preparing of high tension electricity coefficient organic polymer laminated film, specifically refer to a kind of preparation method based on polyvinylidene fluoride Organic Iron electric polymer multi-layer film structure.
Background technology
Ferroelectric material is that a class has spontaneous polarization in certain temperature range, and spontaneous polarization strength with external electric field change, one class material of change is a class focus material of Recent study.In recent years, based on polyvinylidene fluoride (referred to as PVDF), the copolymer (being called for short P (VDF-TrFE)) of polyvinylidene fluoride and trifluoro-ethylene is a kind of ferroelectric, polymeric piezoelectric material of function admirable, energy conduction can be widely used in, the functional material of information storage and infrared acquisition.Its piezoelectric property is mainly used in mechanical energy-electric energy conversion, militarily utilize the feature of piezopolymer, development uses other current art to be difficult to device that is that realize and that have special electroacoustic function, as antioise telephone, broadband ultrasonic signal emission system etc.Piezopolymer, due to nontoxic, can also apply to biomedical sensory field, especially in ultrasonic imaging, obtains successful application the most.
Zhang etc. find that ferroelectric polymers P (VDF-TrFE) has relaxation behavior after electron irradiation, and its piezoelectric property obtains lifting (Science 280,2101-2104 (1998) .).Subsequently, a kind of novel organic relaxor ferroelectric polymer Kynoar-trifluoro-ethylene-chlorine PVF trimer P (VDF-TrFE-CFE) is successfully developed.Compared to ferroelectric polymers P (VDF-TrFE), relaxor ferroelectric polymer shows a series of premium properties, as (Science 321,821-823 (2008) .) such as high electric card coefficients under high-k, high tension electricity coefficient, room temperature.Room temperature refrigerator, piezoelectric transducer etc. can be applied to.
Because some beyond thought unusual performances can appear in different types of ferroelectric material stratiform composite construction, as dielectric property enhancing, ferroelectric properties strengthen, occur anti-ferroelectricity etc., people are in an active state to the research of the composite construction of ferroelectric material always.In recent years, along with the development of film preparing technology, the report of different types of ferroelectric material stratiform composite construction is also more and more many.As ferroelectric material BaTiO
3with ferroelectric material SrTiO
3the composite construction (Nature 433,395 – 399 (2005) .) formed can strengthen iron electric polarization characteristic.At ferroelectric PbTiO
3with relaxation ferroelectric Pb (Mg
1/3nb
2/3) O
3in the layered composite film formed, there is antiferroelectric behavior (Phys.Rev.B 74,184104 (2006)).Ferroelectric PbTiO
3and PbZrO
3the dielectric constant of the layered composite film formed is enhanced (Jpn.J.Appl.Phys.33,5272-5276 (1994)).But report is rarely had for the correlated performance of the composite construction of Organic Iron electric material.
Along with the development of transducer and micro electro mechanical device, now the performance of device is had higher requirement.Based on preparation and the physical property of ferroelectric material straticulate structure, and the development of related device, be more and more subject to extensive concern.The present invention based on material based on PVDF base ferroelectric polymers, will invent a kind of technical process being prepared in PVDF base ferroelectric polymers straticulate structure based on LB technology.Experimental result shows, and polymer composite layer shape structure prepared by the method has more excellent piezoelectric property, its piezoelectric coefficient d
33up to 81.6pC/N, be far longer than the 51.6pC/N of 41pC/N and P (VDF-TrFE-CFE) of P (VDF-TrFE).This method preparation technology is simple, can room temperature preparation.
Summary of the invention
The present invention proposes a kind of preparation method of PVDF base high tension electricity coefficient film, achieves the preparation of high tension electricity coefficient Organic Iron electric polymer film composite structure.
1. the preparation method of a PVDF base high tension electricity coefficient film.Its feature comprises the following steps:
(1) backing material is cleaned up the evenness ensureing its surface, and do surface hydrophobicity process;
(2) different PVDF base Organic Iron electric polymer solution is dripped uniform spreading and enter the ad hoc standby liquid tank having injected standing ultra-pure water of Langmuir-Brocchi, treat that PVDF base Organic Iron electric polymer is evenly distributed on liquid level, and by extruding the liquid level of film forming, make forming thin film continuous by controlling fluid level gauge surface pressure;
(3) by continuous film by horizontal transfer Langmuir-Brocchi special formula method is transferred on substrate, by alternately shifting the organic ferroelectric polymer film of different PVDF bases, repeat some cycles, and by the annealed process of alternate thin films of growth, the annealing temperature of film is 110-135 DEG C, maintain after 4 hours, be cooled to room temperature, just form PVDF base high tension electricity coefficient film.
Described backing material is quartz glass, oxide monocrystal, silicon chip or organic film material, and the surface roughness of substrate is lower than 3 nanometers.
Described PVDF base Organic Iron electric polymer is: Kynoar list polymers, Kynoar-trifluoro-ethylene copolymer P (VDF-TrFE) or Kynoar-trifluoro-ethylene-chlorine PVF trimer P (VDF-TrFE-CFE).
The solvent of described PVDF base Organic Iron electric polymer solution is dimethyl sulfoxide (DMSO), and the mass percentage of its solution concentration is 0.01%.
The resistance of described ultra-pure water is 18.2 megohms, and liquid level surface pressure-controlled is in 5 milli newton every meter.
Feature of the present invention is to prepare a kind of high tension electricity coefficient film based on Kynoar (PVDF), the PVDF base high tension electricity coefficient film utilizing the method to prepare, its technique is simple, and cost is low, is easy to the organic ferroelectric polymer film of high tension electricity coefficient preparing different cycles structure.
Accompanying drawing illustrates:
Fig. 1 be PVDF based polyalcohol laminated film prepare schematic diagram;
Fig. 2 is the piezoelectric property phenogram of the PVDF based polyalcohol laminated film adopting this method to prepare; In Fig. 2, No. 1 curve is the piezoelectricity curve of PVDF based polyalcohol laminated film, and No. 2 and No. 3 curves are respectively the piezoelectricity curve of P (VDF-TrFE-CFE) film and P (VDF-TrFE) film.
Embodiment:
To be by reference to the accompanying drawings 1 below, statement specific embodiment of the invention method, be divided into three embodiments specifically to state.Concrete steps are followed successively by:
A, embodiment 1:
Backing material is cleaned up the evenness ensureing its surface, and do surface hydrophobicity process; Backing material can be quartz glass.Use ferric stearate in the wiping repeatedly of its surface, the ferric stearate wiping surface attachment with absorbent cotton remains, and quartz glass substrate is rinsed well by rear deionized water.
PVDF based polyalcohol P (VDF-TrFE) and PVDF based polyalcohol P (VDF-TrFE-CFE) Organic Iron electric polymer are dissolved in respectively in dimethyl sulphoxide solution, its solution concentration is mass percentage is 0.01%.
Respectively P (VDF-TrFE) and P (VDF-TrFE-CFE) Organic Iron electric polymer dimethyl sulphoxide solution uniform spreading are entered two ad hoc standby liquid tanks having injected standing ultra-pure water of Langmuir-Brocchi, ultra-pure water resistance is 18.2 megohms, treat that Organic Iron electric polymer is evenly distributed on liquid level, and by extruding the liquid level of film forming, by controlling fluid level gauge surface pressure to 5 milli ox every meter, make forming thin film continuous;
Wherein said ultra-pure water resistance is 18.2 megohms.
By continuous film by horizontal transfer Langmuir-Brocchi special formula method is transferred in quartz substrate, by alternately shifting P (VDF-TrFE) and P (VDF-TrFE-CFE) organic ferroelectric polymer film, and repeat some cycles, certain thickness alternate thin films can be obtained, and by the annealed process of alternate thin films 4 hours of growth, annealing temperature is 110 DEG C, is cooled to room temperature, can form PVDF base Organic Iron electric polymer superlattice structure.B, embodiment 2:
Backing material is cleaned up the evenness ensureing its surface, and do surface hydrophobicity process; Backing material can be quartz glass.Use ferric stearate in the wiping repeatedly of its surface, the ferric stearate wiping surface attachment with absorbent cotton remains, and quartz glass substrate is rinsed well by rear deionized water.
PVDF based polyalcohol P (VDF-TrFE) and PVDF based polyalcohol P (VDF-TrFE-CFE) Organic Iron electric polymer are dissolved in respectively in dimethyl sulphoxide solution, its solution concentration is mass percentage is 0.01%.
Respectively P (VDF-TrFE) and P (VDF-TrFE-CFE) Organic Iron electric polymer dimethyl sulphoxide solution uniform spreading are entered two ad hoc standby liquid tanks having injected standing ultra-pure water of Langmuir-Brocchi, ultra-pure water resistance is 18.2 megohms, treat that Organic Iron electric polymer is evenly distributed on liquid level, and by extruding the liquid level of film forming, by controlling fluid level gauge surface pressure to 5 milli ox every meter, make forming thin film continuous;
Wherein said ultra-pure water resistance is 18.2 megohms.
By continuous film by horizontal transfer Langmuir-Brocchi special formula method is transferred in quartz substrate, by alternately shifting P (VDF-TrFE) and P (VDF-TrFE-CFE) organic ferroelectric polymer film, and repeat some cycles, certain thickness alternate thin films can be obtained, and by the annealed process of alternate thin films 4 hours of growth, annealing temperature is 135 DEG C, is cooled to room temperature, can form PVDF base Organic Iron electric polymer superlattice structure.C, embodiment 3:
Backing material is cleaned up the evenness ensureing its surface, and do surface hydrophobicity process; Backing material can be quartz glass.Use ferric stearate in the wiping repeatedly of its surface, the ferric stearate wiping surface attachment with absorbent cotton remains, and quartz glass substrate is rinsed well by rear deionized water.
PVDF based polyalcohol P (VDF-TrFE) and PVDF based polyalcohol P (VDF-TrFE-CFE) Organic Iron electric polymer are dissolved in respectively in dimethyl sulphoxide solution, its solution concentration is mass percentage is 0.01%.
Respectively P (VDF-TrFE) and P (VDF-TrFE-CFE) Organic Iron electric polymer dimethyl sulphoxide solution uniform spreading are entered two ad hoc standby liquid tanks having injected standing ultra-pure water of Langmuir-Brocchi, ultra-pure water resistance is 18.2 megohms, treat that Organic Iron electric polymer is evenly distributed on liquid level, and by extruding the liquid level of film forming, by controlling fluid level gauge surface pressure to 5 milli ox every meter, make forming thin film continuous;
Wherein said ultra-pure water resistance is 18.2 megohms.
By continuous film by horizontal transfer Langmuir-Brocchi special formula method is transferred in quartz substrate, by alternately shifting P (VDF-TrFE) and P (VDF-TrFE-CFE) organic ferroelectric polymer film, and repeat some cycles, certain thickness alternate thin films can be obtained, and by the annealed process of alternate thin films 4 hours of growth, annealing temperature is 120 DEG C, is cooled to room temperature, can form PVDF base Organic Iron electric polymer superlattice structure.
Claims (5)
1. a preparation method for PVDF base high tension electricity coefficient film, its feature comprises the following steps:
(1) backing material is cleaned up the evenness ensureing its surface, and do surface hydrophobicity process;
(2) different PVDF base Organic Iron electric polymer solution is dripped uniform spreading and enter the ad hoc standby liquid tank having injected standing ultra-pure water of Langmuir-Brocchi, treat that PVDF base Organic Iron electric polymer is evenly distributed on liquid level, and by extruding the liquid level of film forming, make forming thin film continuous by controlling fluid level gauge surface pressure;
(3) by continuous film by horizontal transfer Langmuir-Brocchi special formula method is transferred on substrate, by alternately shifting the organic ferroelectric polymer film of different PVDF bases, repeat some cycles, and by the annealed process of alternate thin films of growth, the annealing temperature 110-135 DEG C of film, maintain after 4 hours, be cooled to room temperature, just form PVDF base high tension electricity coefficient film.
2. the preparation method of a kind of PVDF base high tension electricity coefficient film according to claim 1, it is characterized in that, described backing material is quartz glass, oxide monocrystal, silicon chip or organic film material, and the surface roughness of substrate is lower than 3 nanometers.
3. the preparation method of a kind of PVDF base high tension electricity coefficient film according to claim 1, it is characterized in that, described PVDF base Organic Iron electric polymer is: Kynoar list polymers, Kynoar-trifluoro-ethylene copolymer P (VDF-TrFE) or Kynoar-trifluoro-ethylene-chlorine PVF trimer P (VDF-TrFE-CFE).
4. the preparation method of a kind of PVDF base high tension electricity coefficient film according to claim 1, is characterized in that, the solvent of described PVDF base Organic Iron electric polymer solution is dimethyl sulfoxide (DMSO), and the mass percentage of its solution concentration is 0.01%.
5. the preparation method of a kind of PVDF base high tension electricity coefficient film according to claim 1, it is characterized in that, the resistance of described ultra-pure water is 18.2 megohms, and liquid level surface pressure-controlled is in 5 milli newton every meter.
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| CN105529397A (en) * | 2016-01-15 | 2016-04-27 | 电子科技大学 | Composite flexible nanometer power generator and fabrication method thereof |
| CN106863859A (en) * | 2017-01-04 | 2017-06-20 | 复旦大学 | It is a kind of to prepare the height-oriented method for gathering inclined difluoro trifluoro-ethylene copolymer film |
| CN108428622A (en) * | 2018-03-30 | 2018-08-21 | 湖南工程学院 | A kind of preparation method of Quito high pyroelectric coefficient PVDF tunic |
| CN109400929A (en) * | 2018-10-30 | 2019-03-01 | 郭和俊 | A kind of P(VDF-TrFE) ferroelectric thin-flim materials preparation method |
| CN109453431A (en) * | 2018-10-23 | 2019-03-12 | 北京大学口腔医学院 | Membrane material and preparation method thereof is repaired in a kind of electrification that surface potential is controllable |
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| CN111938867A (en) * | 2020-07-22 | 2020-11-17 | 南开大学 | Artificial blood vessel capable of simulating natural blood vessel to release electric signal and preparation method thereof |
| CN111938867B (en) * | 2020-07-22 | 2023-07-04 | 南开大学 | Artificial blood vessel capable of simulating natural blood vessel to release electric signals and preparation method thereof |
| CN112480451A (en) * | 2020-10-26 | 2021-03-12 | 清华大学 | Polymer-based terahertz spatial light modulator and preparation method thereof |
| CN112480451B (en) * | 2020-10-26 | 2022-03-18 | 清华大学 | Polymer-based terahertz spatial light modulator and preparation method thereof |
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