CN103289113B - A kind of method manufacturing organic composite dielectric film - Google Patents
A kind of method manufacturing organic composite dielectric film Download PDFInfo
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- CN103289113B CN103289113B CN201310234935.1A CN201310234935A CN103289113B CN 103289113 B CN103289113 B CN 103289113B CN 201310234935 A CN201310234935 A CN 201310234935A CN 103289113 B CN103289113 B CN 103289113B
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Abstract
The embodiment of the invention discloses a kind of method manufacturing organic composite dielectric film, comprising: by polyvinylidene difluoride (PVDF) and Polythiophene Homogeneous phase mixing, obtain mixing material powder; Mixing material powder is dissolved in organic solvent, obtains organic mixing solutions; By organic mixing solutions at room temperature vacuum standing and defoaming; Heating this organic mixing solutions makes organic solvent volatilize, and obtains Polythiophene-polyvinylidene difluoride (PVDF) organic composite dielectric film.Organic composite dielectric film prepared by the method for embodiments of the invention had both had higher specific inductivity, be again fexible film, have excellent machinability, simultaneously the method that provides of embodiments of the invention is easy and simple to handle, with low cost, be applicable to the production of film capacitor.
Description
Technical field
The present invention relates to electronic functional material technical field, especially relate to a kind of method manufacturing organic composite dielectric film.
Background technology
Film capacitor, since appearance, has been used widely because of its superior high frequency performance.Film capacitor has the advantages such as nonpolarity, high insulation resistance, broadband response, minimum dielectric loss, be widely used in electronics, electric power, electrically, communication, household electrical appliances, the every field such as space flight and aviation, become and promote above-mentioned industry and to update one of indispensable electronic component.
But the lower principal element becoming the application of restriction film capacitor of capacity, the parts affecting film capacitor electric capacity most critical are that the specific inductivity of organic film is lower, the organic film that present stage adopts is poly-ethyl ester, polypropylene, polystyrene and poly-carbonic acid mainly, the specific inductivity of this several film, all between 1 ~ 2, seriously constrains the growth of film capacitor capacity.
Therefore, there is the demand for the organic composite dielectric film with higher specific inductivity.
Summary of the invention
An object of the present invention is to provide a kind of method manufacturing the organic composite dielectric film that specific inductivity is greatly improved.
Technical scheme disclosed by the invention comprises:
Provide a kind of method manufacturing organic composite dielectric film, it is characterized in that, comprising: by polyvinylidene difluoride (PVDF) and Polythiophene Homogeneous phase mixing, obtain mixing material powder; Described mixing material powder is dissolved in organic solvent, obtains organic mixing solutions; By described organic mixing solutions at room temperature vacuum standing and defoaming; Heating described organic mixing solutions makes described organic solvent volatilize from described organic mixing solutions, obtains Polythiophene-polyvinylidene difluoride (PVDF) organic composite dielectric film.
Further, described polyvinylidene difluoride (PVDF) and Polythiophene are pulverized and are mixed comprise: described polyvinylidene difluoride (PVDF) is mixed 8 to 12 hours with described Polythiophene ball-grinding machine ball milling.
Further, the weight ratio of described polyvinylidene difluoride (PVDF) and described Polythiophene is 100:1 to 100:5.
Further, described organic solvent is DMF, N,N-dimethylacetamide, dimethyl sulfoxide (DMSO), chloroform, tetrahydrofuran (THF), triethyl phosphate or N-Methyl pyrrolidone.
Further, describedly described mixing material powder is dissolved in organic solvent comprises: described mixing material powder to be added in described organic solvent and at agitated under sonication, until described mixing material powder dissolves completely, the weight of wherein said organic solvent is 10 to 50 times of the weight of described polyvinylidene difluoride (PVDF).
Further, by described organic mixing solutions at room temperature vacuum standing and defoaming comprise: by described organic mixing solutions down in dull and stereotyped groove, the degree of depth controlling described organic mixing solutions is 0.2 to 1 millimeter, and vacuum suction bubble leave standstill 4 to 5 hours.
Further, the described organic mixing solutions of described heating makes described organic solvent volatilize from described organic mixing solutions to comprise: by described organic mixing solutions heating under vacuum to 60 to 80 degrees Celsius, and keep described 60 to 80 degrees Celsius of constant temperature under vacuum 8 to 24 hours.
In the method for embodiments of the invention, make use of the seep effect of conductive polymers Polythiophene (PEDOT) in dielectric polymer based composites polyvinylidene difluoride (PVDF) (PVDF), by the even filler of the conductive polymers of lower aq in dielectric polymer matrix, define Polythiophene-polyvinylidene difluoride (PVDF) (PEDOT-PVDF) organic composite dielectric film, the specific inductivity of this organic composite dielectric film is greatly improved, and adopt organic filler and matrix, make organic film have good processing characteristics.
Organic composite dielectric film prepared by the method for embodiments of the invention had both had higher specific inductivity, be again fexible film, have excellent machinability, simultaneously the method that provides of the embodiment of the present invention is easy and simple to handle, with low cost, be applicable to the production of film capacitor.
Accompanying drawing explanation
Fig. 1 is the schematic flow sheet of the method for the manufacture organic composite dielectric film of one embodiment of the invention.
Embodiment
The method of the manufacture organic composite dielectric film of embodiments of the invention is described in detail below in conjunction with accompanying drawing.
As shown in Figure 1, in embodiments of the invention, a kind of method manufacturing organic composite dielectric film comprises step 10, step 12, step 14 and step 16.
Step 10: mixing polyvinylidene difluoride (PVDF) and Polythiophene.
In embodiments of the invention, first by a certain amount of polyvinylidene difluoride (PVDF) and a certain amount of Polythiophene Homogeneous phase mixing, mixing material powder can be obtained.
In embodiments of the invention, any applicable method can be used polyvinylidene difluoride (PVDF) and Polythiophene Homogeneous phase mixing.Such as, in an embodiment, can ball-grinding machine be used, add in ball-grinding machine by a certain amount of polyvinylidene difluoride (PVDF) and a certain amount of Polythiophene, with ball-grinding machine, the polyvinylidene difluoride (PVDF) added and Polythiophene ball milling be mixed, obtain mixing material powder.Wherein, can determine according to the needs of practical situation with the time of ball-grinding machine ball milling mixing polyvinylidene difluoride (PVDF) and Polythiophene, such as, in an embodiment, polyvinylidene difluoride (PVDF) and Polythiophene ball-grinding machine can be ground mixing 8 to 12 hours.
Polyvinylidene difluoride (PVDF) and Polythiophene are powdery substances, but the two particle diameter is different, there is certain agglomeration simultaneously.Therefore, in embodiments of the invention, adopt method mixing polyvinylidene difluoride (PVDF) and the Polythiophene of ball milling mixing, the two mixing can be made more even, and ensure that the mixing material powder obtained is below micron level
Through such process, polyvinylidene difluoride (PVDF) and Polythiophene are uniformly mixed.
In embodiments of the invention, in aforesaid step, the weight ratio of polyvinylidene difluoride (PVDF) and Polythiophene is 100:1 to 100:5.
In embodiments of the invention, pulverize and the concrete quantity of mixed uniformly polyvinylidene difluoride (PVDF) and Polythiophene can determine according to practical situation, as long as make the weight ratio of polyvinylidene difluoride (PVDF) and Polythiophene be 100:1 to 100:5.
Step 12: mixing material powder is dissolved in the first solvent.
After obtaining mixing material powder, in step 12, this mixing material powder is dissolved in organic solvent, obtains organic mixing solutions.
In embodiments of the invention, organic solvent used herein can be have volatility and polyvinylidene difluoride (PVDF) and Polythiophene can be dissolved in organic solvent wherein.Such as, in an embodiment, organic solvent here can be DMF, N,N-dimethylacetamide, dimethyl sulfoxide (DMSO), chloroform, tetrahydrofuran (THF), triethyl phosphate or N-Methyl pyrrolidone.
In embodiments of the invention, this mixing material powder can be added in this organic solvent and at agitated under sonication, until mixing material powder dissolves completely, wherein, the weight of organic solvent used herein is 10 to 50 times of the weight of the polyvinylidene difluoride (PVDF) in step 10.
In embodiments of the invention, " at agitated under sonication " mentioned here refers to and to stir with ultrasonic irradiation solution simultaneously, to promote the dissolving of mixing material powder.
Step 14: by organic mixing solutions vacuum standing and defoaming.
After obtaining organic mixing solutions, at step 14, by this organic mixing solutions at room temperature vacuum standing and defoaming, the bubble in organic mixing solutions is departed from from organic mixing solutions.
Such as, in an embodiment, the detailed process of organic mixing solutions at room temperature vacuum standing and defoaming can be comprised: by organic mixing solutions down in dull and stereotyped groove, the degree of depth controlling this organic mixing solutions is 0.2 to 1 millimeter, and vacuum suction steeps, leave standstill 4 to 5 hours.
Through such process, the bubble in organic mixing solutions is discharged, with the formation avoiding these bubbles to affect required organic composite dielectric film in subsequent step.
Step 16: heat organic mixing solutions and organic solvent is volatilized.
Organic mixing solutions, after the vacuum standing and defoaming process of step 14, heats this organic mixing solutions, and the organic solvent in this organic mixing solutions is volatilized from this organic mixing solutions.In the process of organic solvent volatilization, previously be dissolved in polyvinylidene difluoride (PVDF) in this organic solvent and Polythiophene composition will be separated out, in this process, due to the seep effect of conductive polymers Polythiophene (PEDOT) in dielectric polymer based composites polyvinylidene difluoride (PVDF) (PVDF), even filler in polyvinylidene difluoride (PVDF) matrix, thus is defined Polythiophene-polyvinylidene difluoride (PVDF) (PEDOT-PVDF) organic composite dielectric film by the Polythiophene of lower aq.
In embodiments of the invention, heat the concrete steps that organic mixing solutions makes organic solvent volatilize from organic mixing solutions can comprise: by organic mixing solutions heating under vacuum to 60 to 80 degrees Celsius, and keep these 60 to 80 degrees Celsius of constant temperature under vacuum 8 to 24 hours.
Through the process of step 16, namely obtain required Polythiophene-polyvinylidene difluoride (PVDF) (PEDOT-PVDF) organic composite dielectric film.
Illustrate several specific exampless of method of the present invention below.
Example one:
(1) take 10g polyvinylidene difluoride (PVDF) and 0.2g Polythiophene ball milling mixing 12h, obtain organic mixed material powders A 1;
(2), in the 200ml DMF organic mixed material powders A 1 of polyvinylidene difluoride (PVDF) and Polythiophene joined, ultrasonic lower abundant stirring 3h, until organic dust dissolves completely or disperses, obtains organic mixing solutions B1;
(3) by mixing solutions B1 down in Special horizontal board slot, control solution deep is 0.5mm, and vacuum suction bubble leaves standstill 4 ~ 5 hours, obtains bubble-free mixed solution C 1;
(4) by bubble-free mixed solution C 1 heating under vacuum to 60 DEG C, vacuum constant temperature 24h, drives away organic solvent, and obtain Polythiophene-polyvinylidene difluoride (PVDF) (PEDOT-PVDF) full stress-strain compound dielectric film sample 1, recording specific inductivity is 13.5.
Example two:
(1) take 10g polyvinylidene difluoride (PVDF) and 0.3g Polythiophene ball milling mixing 12h, obtain organic mixed material powders A 2;
(2), in 200ml DMF polyvinylidene difluoride (PVDF) and the organic mixed powder A2 of Polythiophene joined, ultrasonic lower abundant stirring 3h, until organic dust dissolves completely or disperses, obtains organic mixing solutions B2;
(3) by mixing solutions B2 down in Special horizontal board slot, control solution deep is 0.5mm, and vacuum suction bubble leaves standstill 4 ~ 5 hours, obtains bubble-free mixed solution C 2;
(4) by bubble-free mixed solution C 2 heating under vacuum to 60 DEG C, vacuum constant temperature 24h, drives away organic solvent, and obtain Polythiophene-polyvinylidene difluoride (PVDF) (PEDOT-PVDF) full stress-strain compound dielectric film sample 2, recording specific inductivity is 15.8.
Example three:
(1) take 10g polyvinylidene difluoride (PVDF) and 0.4g Polythiophene ball milling mixing 12h, obtain organic mixed material powders A 3;
(2), in 200ml DMF polyvinylidene difluoride (PVDF) and Polythiophene organic mixed material powders A 3 joined, ultrasonic lower abundant stirring 3h, until organic dust dissolves completely or disperses, obtains organic mixing solutions B3;
(3) by mixing solutions B3 down in Special horizontal board slot, control solution deep is 0.5mm, and vacuum suction bubble leaves standstill 4 ~ 5 hours, obtains bubble-free mixed solution C 3;
(4) by bubble-free mixed solution C 3 heating under vacuum to 60 DEG C, vacuum constant temperature 24h, drives away organic solvent, and obtain Polythiophene-polyvinylidene difluoride (PVDF) (PEDOT-PVDF) full stress-strain compound dielectric film sample 3, recording specific inductivity is 17.4.
Example four:
(1) take 10g polyvinylidene difluoride (PVDF) and 0.2g Polythiophene ball milling mixing 12h, obtain organic mixed material powders A 4;
(2), in 200ml DMF polyvinylidene difluoride (PVDF) and the organic mixed powder A4 of Polythiophene joined, ultrasonic lower abundant stirring 3h, until organic dust dissolves completely or disperses, obtains organic mixing solutions B4;
(3) by mixing solutions B4 down in Special horizontal board slot, control solution deep is 0.5mm, and vacuum suction bubble leaves standstill 4 ~ 5 hours, obtains bubble-free mixed solution C 4;
(4) by bubble-free mixed solution C 4 heating under vacuum to 60 DEG C, vacuum constant temperature 24h, drives away organic solvent, and obtain Polythiophene-polyvinylidene difluoride (PVDF) (PEDOT-PVDF) full stress-strain compound dielectric film sample 4, recording specific inductivity is 16.7.
In the method for embodiments of the invention, make use of the seep effect of conductive polymers Polythiophene (PEDOT) in dielectric polymer based composites polyvinylidene difluoride (PVDF) (PVDF), by the even filler of the conductive polymers of lower aq in dielectric polymer matrix, define Polythiophene-polyvinylidene difluoride (PVDF) (PEDOT-PVDF) organic composite dielectric film, the specific inductivity of this organic composite dielectric film is greatly improved, and adopt organic filler and matrix, make organic film have good processing characteristics.
Organic composite dielectric film prepared by the method for embodiments of the invention had both had higher specific inductivity, be again fexible film, have excellent machinability, simultaneously the method that provides of the embodiment of the present invention is easy and simple to handle, with low cost, be applicable to the production of film capacitor.
Described the present invention by specific embodiment above, but the present invention is not limited to these specific embodiments.It will be understood by those skilled in the art that and can also make various amendment, equivalent replacement, change etc. to the present invention, as long as these conversion do not deviate from spirit of the present invention, all should within protection scope of the present invention.In addition, " embodiment " described in above many places represents different embodiments, can certainly by its all or part of combination in one embodiment.
Claims (6)
1. manufacture a method for organic composite dielectric film, it is characterized in that, comprising:
By polyvinylidene difluoride (PVDF) and Polythiophene Homogeneous phase mixing, obtain mixing material powder, the weight ratio of wherein said polyvinylidene difluoride (PVDF) and described Polythiophene is 100:1 to 100:5;
Described mixing material powder is dissolved in organic solvent, obtains organic mixing solutions;
By described organic mixing solutions at room temperature vacuum standing and defoaming;
Heating described organic mixing solutions makes described organic solvent volatilize from described organic mixing solutions, obtain Polythiophene-polyvinylidene difluoride (PVDF) organic composite dielectric film, wherein in described Polythiophene-polyvinylidene difluoride (PVDF) organic composite dielectric film, the even filler of Polythiophene is in polyvinylidene difluoride (PVDF) matrix.
2. the method for claim 1, is characterized in that, describedly polyvinylidene difluoride (PVDF) and Polythiophene Homogeneous phase mixing is comprised: described polyvinylidene difluoride (PVDF) is mixed 8 to 12 hours with described Polythiophene ball-grinding machine ball milling.
3. the method for claim 1, is characterized in that: described organic solvent is DMF, N,N-dimethylacetamide, dimethyl sulfoxide (DMSO), chloroform, tetrahydrofuran (THF), triethyl phosphate or N-Methyl pyrrolidone.
4. the method for claim 1, it is characterized in that: describedly described mixing material powder is dissolved in organic solvent comprises: described mixing material powder to be added in described organic solvent and at agitated under sonication, until described mixing material powder dissolves completely, the weight of wherein said organic solvent is 10 to 50 times of the weight of described polyvinylidene difluoride (PVDF).
5. the method for claim 1, it is characterized in that: by described organic mixing solutions at room temperature vacuum standing and defoaming comprise: by described organic mixing solutions down in dull and stereotyped groove, the degree of depth controlling described organic mixing solutions is 0.2 to 1 millimeter, and vacuum suction bubble leaves standstill 4 to 5 hours.
6. the method for claim 1, it is characterized in that: the described organic mixing solutions of described heating makes described organic solvent volatilize from described organic mixing solutions to comprise: by described organic mixing solutions heating under vacuum to 60 to 80 degrees Celsius, and keep described 60 to 80 degrees Celsius of constant temperature under vacuum 8 to 24 hours.
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| CN101230149A (en) * | 2007-12-29 | 2008-07-30 | 中国科学院化学研究所 | Two-dimensional ordered organic semiconductor composite nano membrane as well as special substrate and preparation method thereof |
| CN102632675A (en) * | 2012-04-17 | 2012-08-15 | 电子科技大学 | Method for preparing nanocomposite dielectric film |
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| CN102632675A (en) * | 2012-04-17 | 2012-08-15 | 电子科技大学 | Method for preparing nanocomposite dielectric film |
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