CN104877278B - A kind of Vinalac 5920/polyvinylidene fluoride compound dielectric film and preparation method thereof - Google Patents
A kind of Vinalac 5920/polyvinylidene fluoride compound dielectric film and preparation method thereof Download PDFInfo
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- CN104877278B CN104877278B CN201510365809.9A CN201510365809A CN104877278B CN 104877278 B CN104877278 B CN 104877278B CN 201510365809 A CN201510365809 A CN 201510365809A CN 104877278 B CN104877278 B CN 104877278B
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L27/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers
- C08L27/02—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L27/12—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
- C08L27/16—Homopolymers or copolymers or vinylidene fluoride
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2327/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers
- C08J2327/02—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment
- C08J2327/12—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
- C08J2327/16—Homopolymers or copolymers of vinylidene fluoride
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2433/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
- C08J2433/04—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers esters
- C08J2433/06—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers esters of esters containing only carbon, hydrogen, and oxygen, the oxygen atom being present only as part of the carboxyl radical
- C08J2433/10—Homopolymers or copolymers of methacrylic acid esters
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/16—Applications used for films
Abstract
The invention discloses a kind of Vinalac 5920（PBMA）/ polyvinylidene fluoride compound dielectric film, the film is with fluoropolymer and organic PBMA mixing casting film-forming.Wherein compound dielectric film mass percent, which is constituted, is：Organic PBMA is 10% 30%, and fluoropolymer is 70% 90%.This compound dielectric film is that have higher dielectric constant, the new dielectric material of relatively low dielectric loss.The compound dielectric film of dielectric constant needed for being prepared by controlling filler adding proportion.The composite film preparation technology is simple, combined temp is low and environmentally friendly, is with a wide range of applications.
Description
Technical field
The invention belongs to compound dielectric film field, more particularly to a kind of Vinalac 5920（PBMA）/ poly- inclined
Fluoride-based compound dielectric film.
Background technology
Possess the polymer-based dielectric material of high-k, low-dielectric loss because it has huge in terms of electric energy is stored
Potential and be widely used, such as communication equipment, charge storage capacitance system, artificial-muscle, brake and space flight military affairs
Aspect.Traditional dielectric substance includes inorganic ceramic material and high-molecular organic material.Common inorganic ceramic material, such as titanium
Sour barium (BaTiO3), CaCu 3 Ti 4 O（CCTO）, lead zirconate titanate (PZT) etc., with very high dielectric constant, but they make
For complex process, brittle and dielectric loss is larger.The machine high polymer material of common are have polyethylene, polypropylene, poly- trifluoro-ethylene,
Epoxy resin etc., their flexible, dielectric losses are low, film forming easy to process, but their dielectric constant is relatively low.It is single
Dielectric substance be difficult to meet industrialized needs, therefore prepare the polymer matrix composite tool of high dielectric property
There is very important meaning at present, polymer-based dielectric material is broadly divided into following three types：（1）Inorganic ceramic material：
Such as barium titanate（BaTiO3）, its electric capacity is larger, and dielectric constant is up to 6300, but the material sintering temperature is high, preparation process is complicated,
Brittle, processing request is high, and poor with polymer compatibility, is difficult film forming, bad mechanical property.（2）Conductive material：By graphite
Alkene is added in PVDF as filler and forms composite, is 3 times of PVDF matrixes in the dielectric constant of 1000Hz composites
More than, but composite can be influenceed by percolation threshold, can be improved a lot close to dielectric loss during percolation threshold, simultaneously
Dielectric material sports conductive material, has a strong impact on its production application.（3）Organic composite material：Such as polystyrene（PS）, lead to
The method for crossing solution coating is prepared for PSAN films, and the dielectric constant of film is 4, dielectric loss 0.027, and energy storage density reaches
6.8J/cm3, pliability is good, and dielectric loss is low, but dielectric constant is too small.
The content of the invention
It is a primary object of the present invention to provide a kind of Vinalac 5920（PBMA）/ polyvinylidene fluoride is combined
Dielectric film.The laminated film has preferable dielectric properties.The Vinalac 5920（PBMA）/ polyvinylidene fluoride
Compound dielectric film is made up of PBMA and fluoropolymer.Its mass percent is constituted：
PBMA 10%-30%
Fluoropolymer 70%-90%
Described Vinalac 5920（PBMA）/ polyvinylidene fluoride compound dielectric film, it is characterised in that institute
Organic PBMA is stated for commercial goods;
The fluoropolymer is Kynoar-trifluoro-ethylene copolymer [P (VDF-TrFE)], Kynoar-three
One kind in PVF-fluorine vinyl chloride copolymer [P (VDF-TrFE-CFE)].
It is a further object of the present invention to provide a kind of Vinalac 5920（PBMA）/ polyvinylidene fluoride is compound to be situated between
The preparation method of conductive film：
1. after PBMA, fluoropolymer and solvent DMF (DMF) are mixed, ultrasonic agitation is scattered equal
It is even, form stable colloidal sol；Its mass percent is constituted：
PBMA 10%-30%
Fluoropolymer 70%-90%
Organic PBMA and fluoropolymer gross mass and DMF mass ratio are 1:7-10
2nd, the colloidal sol for preparing step 1 80 ± 1 DEG C of casting film-formings on mould, dry 18 ± 1h, then by natural cooling,
120 ± 1 DEG C of 8 ± 1h of annealing, remove residual solvent, that is, obtain organic filler/polymer matrix composite dielectric of 110-150 μm of thickness
Film.
According to above-mentioned preparation method, in described organic PBMA mass ratio ranges, its mass ratio is adjusted, that is, is made
The compound dielectric film of required differing dielectric constant.
The invention has the advantages that：
A. organic PBMA fillers overcome problems present in background technology, and it has the polarizability of middle rank, table
Reveal higher dielectric constant, relatively low dielectric loss, the transparency is good, and pliability is preferable, with higher mechanical performance.
B. the filler and matrix dielectric constants are smaller, and have good compatibility with polymeric substrates, therefore are combined and are situated between
Conductive film has preferable dielectric properties, and its dielectric loss is not obviously improved, and is still maintained at a relatively low position,
It is a kind of new high-dielectric composite material.
C. the film can significantly change the dielectric properties of material by adjusting organic filler PBMA mass ratio,
So as to prepare required high dielectric constant film.
D. the preparation technology of the film is simple, combined temp is low and environmentally friendly, can change mould as requested
Shape size so that suitable for different electronic equipments, energy storage material.
The laminated film of the present invention, dielectric properties are stablized relatively with the change of frequency, occur without very big mutation.It is multiple
45 or so can be brought up to by closing the dielectric constant of film.
Specific embodiment
Below by product and preparation method in the specific embodiment narration present invention.Unless stated otherwise, it is of the invention
In used technological means be method known in those skilled in the art.In addition, embodiment be interpreted as it is illustrative,
The scope being not intended to limit the present invention, the spirit and scope of the invention are limited only by the claims that follow.For people in the art
For member, on the premise of without prejudice to spirit and scope of the present invention, the conditions such as the ratio and solvent in these embodiments are entered
Capable various changes or change fall within the protection category of the present invention.
Below in conjunction with specific embodiment, the present invention is further illustrated, but does not mean that to the scope of the present invention
Limitation.
Embodiment 1：
A. by the organic PBMA of 0.0100g, 0.1000g Kynoar-trifluoro-ethylene copolymer [P (VDF-TrFE)] and
After the mixing of 1.0005g solvent DMFs, ultrasonic agitation is uniformly dispersed, and forms stable colloidal sol, and charge ratio composition is：Organic PBMA
For 10%, polymer is 90%；
B. the colloidal sol prepared by step a 80 DEG C of casting film-formings on mould, dry 18h；Again by natural cooling, 120 DEG C
Anneal 8h, that is, prepares PBMA/ P (VDF-TrFE) compound dielectric film.In 1000Hz, dielectric constant can reach 16, dielectric
It is lost as 0.21, disruptive field intensity is 322MV/m.
Embodiment 2：
A. by the organic PBMA of 0.0200g, 0.1000g Kynoar-trifluoro-ethylene copolymer [P (VDF-TrFE)] and
After the mixing of 1.0005g solvent DMFs, ultrasonic agitation is uniformly dispersed, and forms stable colloidal sol, and charge ratio composition is：Organic PBMA
For 20%, polymer is 80%；
B. the colloidal sol prepared by step a 80 DEG C of casting film-formings on mould, dry 18h；Again by natural cooling, 120 DEG C
Anneal 8h, that is, prepares PBMA/ P (VDF-TrFE) compound dielectric film.In 1000Hz, dielectric constant can reach 23, dielectric
It is lost as 0.29, disruptive field intensity is 243 MV/m.
Embodiment 3：
A. by the organic PBMA of 0.0300g, 0.1000g Kynoar-trifluoro-ethylene copolymer [P (VDF-TrFE)] and
After the mixing of 1.0005g solvent DMFs, ultrasonic agitation is uniformly dispersed, and forms stable colloidal sol, and charge ratio composition is：Organic PBMA
For 30%, polymer is 70%；
B. the colloidal sol prepared by step a 80 DEG C of casting film-formings on mould, dry 18h；Again by natural cooling, 120 DEG C
Anneal 8h, that is, prepares PBMA/ P (VDF-TrFE) compound dielectric film.In 1000Hz, dielectric constant can reach 21, dielectric
It is lost as 0.30, disruptive field intensity is 259MV/m.
Embodiment 4：
This group of embodiment is comparative example.0.1000g Kynoar-trifluoro-ethylene copolymer [P (VDF-TrFE)]
After the mixing of 1.0005g solvent DMFs, ultrasonic agitation is uniformly dispersed, and stable colloidal sol is formed, by the colloidal sol of preparation 80 on mould
DEG C casting film-forming, dries 18h；Again by natural cooling, 120 DEG C of annealing 8h, that is, prepare P (VDF-TrFE) composite dielectric thin
Film.In 1000Hz, dielectric constant can reach 15, and dielectric loss is 0.23, and disruptive field intensity is 300 MV/m.
Embodiment 5：
A. by the organic PBMA of 0.0100g, 0.1000g Kynoar-trifluoro-ethylene-chlorine fluoride copolymers [P (VDF-
TrFE-CFE)] and after the mixing of 1.0005g solvent DMFs, ultrasonic agitation is uniformly dispersed, and forms stable colloidal sol, charge ratio composition
For：Organic PBMA is 10%, and polymer is 90%；
B. the colloidal sol prepared by step a 80 DEG C of casting film-formings on mould, dry 18h；Again by natural cooling, 120 DEG C
Anneal 8h, that is, prepares PBMA/ P (VDF-TrFE-CFE) compound dielectric film.In 1000Hz, dielectric constant can reach 45,
Dielectric loss is 2.5, and disruptive field intensity is 322 MV/m.
Embodiment 6：
A. by the organic PBMA of 0.0200g, 0.1000g Kynoar-trifluoro-ethylene-chlorine fluoride copolymers [P (VDF-
TrFE-CFE)] and after the mixing of 1.0005g solvent DMFs, ultrasonic agitation is uniformly dispersed, and forms stable colloidal sol, charge ratio composition
For：Organic PBMA is 20%, and polymer is 80%；
B. the colloidal sol prepared by step a 80 DEG C of casting film-formings on mould, dry 18h；Again by natural cooling, 120 DEG C
Anneal 8h, that is, prepares PBMA/ P (VDF-TrFE-CFE) compound dielectric film.In 1000Hz, dielectric constant can reach 34,
Dielectric loss is 1.6, and disruptive field intensity is 203 MV/m.
Embodiment 7：
A. by the organic PBMA of 0.0300g, 0.1000g Kynoar-trifluoro-ethylene-chlorine fluoride copolymers [P (VDF-
TrFE-CFE)] and after the mixing of 1.0005g solvent DMFs, ultrasonic agitation is uniformly dispersed, and forms stable colloidal sol, charge ratio composition
For：Organic PBMA is 30%, and polymer is 70%；
B. the colloidal sol prepared by step a 80 DEG C of casting film-formings on mould, dry 18h；Again by natural cooling, 120 DEG C
Anneal 8h, that is, prepares PBMA/ P (VDF-TrFE-CFE) compound dielectric film.In 1000Hz, dielectric constant can reach 40,
Dielectric loss is 1.2, and disruptive field intensity is 202 MV/m.
Embodiment 8：
This group of embodiment is comparative example.0.1000g Kynoar-trifluoro-ethylene-chlorine fluoride copolymers [P
(VDF-TrFE-CFE)] and after the mixing of 1.0005g solvent DMFs, ultrasonic agitation is uniformly dispersed, and forms stable colloidal sol, will prepare
Colloidal sol on mould 80 DEG C of casting film-formings, dry 18h；Again by natural cooling, 120 DEG C of annealing 8h, that is, prepare P (VDF-
TrFE-CFE) compound dielectric film.In 1000Hz, dielectric constant can reach 35, and dielectric loss is 2.0, and disruptive field intensity is 294
MV/m。
Embodiments of the invention are explained in detail above, all embodiments are under premised on technical solution of the present invention
Implemented, give detailed embodiment and specific operating process, but protection scope of the present invention be not limited to it is above-mentioned
Embodiment.
Claims (3)
1. a kind of Vinalac 5920（PBMA）/ polyvinylidene fluoride compound dielectric film, it is characterised in that described multiple
Close dielectric film to be made up of fluoropolymer and organic filler PBMA, its mass percent is：Organic filler PBMA10%-30%,
Fluoropolymer 70%-90%；The fluoropolymer is Kynoar-trifluoro-ethylene [P (VDF-TrFE)], polyvinylidene fluoride
One kind in alkene-trifluoro-ethylene-chlorine PVF [P (VDF-TrFE-CFE)] copolymer；The preparation method of compound dielectric film is：
By PBMA, after Kynoar based polyalcohol and solvent DMF mixing, ultrasonic agitation is uniformly dispersed, and forms stable colloidal sol, will make
Standby colloidal sol 80 DEG C of casting film-formings on mould, dry 18h；Again by natural cooling, 120 DEG C of annealing 8h, that is, prepare poly- first
Base n-butyl acrylate（PBMA）/ polyvinylidene fluoride compound dielectric film.
2. Vinalac 5920 according to claim 1（PBMA）/ polyvinylidene fluoride compound dielectric film, its
It is characterised by, organic PBMA is commercial goods.
3. Vinalac 5920 according to claim 2（PBMA）/ polyvinylidene fluoride compound dielectric film, its
It is characterised by, PBMA and the fluoropolymer gross mass and DMF mass ratio are 1:7-10.
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| CN109961952A (en) * | 2019-03-27 | 2019-07-02 | 哈尔滨理工大学 | A kind of multiple layer polymer base composite energy-storage material of heterojunction structure and preparation method thereof |
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| DE102007029263A1 (en) * | 2007-06-22 | 2008-12-24 | Evonik Röhm Gmbh | PMMA / PVDF film with particularly high weather resistance and high UV protection |
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