CN103289113A - Method for manufacturing organic composite dielectric film - Google Patents
Method for manufacturing organic composite dielectric film Download PDFInfo
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- CN103289113A CN103289113A CN2013102349351A CN201310234935A CN103289113A CN 103289113 A CN103289113 A CN 103289113A CN 2013102349351 A CN2013102349351 A CN 2013102349351A CN 201310234935 A CN201310234935 A CN 201310234935A CN 103289113 A CN103289113 A CN 103289113A
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Abstract
The embodiment of the invention discloses a method for manufacturing an organic composite dielectric film, which comprises the following steps: evenly mixing polyvinylidene fluoride and polythiophene to obtain mixed powder; dissolving the mixed powder in an organic solvent to obtain an organic mixed solution; standing the organic mixed solution at room temperature in a vacuum for deaeration; and heating the organic mixed solution to volatilize the organic solvent, thereby obtaining the polythiophene-polyvinylidene fluoride organic composite dielectric film. The organic composite dielectric film prepared by the method disclosed by the embodiment of the invention has the advantages of higher dielectric constant, high flexibility and favorable working properties; and the method disclosed by the embodiment of the invention is simple to operate and low in cost, and is suitable for producing film capacitors.
Description
Technical field
The present invention relates to the electronic functional material technical field, especially relate to a kind of method of making organic compound dielectric film.
Background technology
Film capacitor has been used widely because of its superior high frequency performance since coming out.Film capacitor has nonpolarity, high insulation resistance, broadband response, minimum advantages such as dielectric loss, be widely used in every field such as electronics, electric power, electric, communication, household electrical appliances, space flight and aviation, become and promote above-mentioned industry one of the indispensable electronic component that updates.
Yet the low principal element that becomes the application of restriction film capacitor of capacity, the parts that influence film capacitor electric capacity most critical are that the specific inductivity of organic film is lower, the organic film that present stage adopts mainly is poly-ethyl ester, polypropylene, polystyrene and poly-carbonic acid, the specific inductivity of these several films all between 1 ~ 2, has seriously restricted the growth of film capacitor capacity.
Therefore, existence is for the demand of the organic compound dielectric film with higher dielectric constant.
Summary of the invention
One of purpose of the present invention provides a kind of method of making organic compound dielectric film that specific inductivity is greatly improved.
Technical scheme disclosed by the invention comprises:
A kind of method of making organic compound dielectric film is provided, has it is characterized in that, having comprised: polyvinylidene difluoride (PVDF) and Polythiophene have evenly been mixed, obtain the mixing material powder; Described mixing material powder is dissolved in the organic solvent, obtains organic mixing solutions; With described organic mixing solutions vacuum standing and defoaming at room temperature; Heat described organic mixing solutions described organic solvent is volatilized from described organic mixing solutions, obtain the organic compound dielectric film of Polythiophene-polyvinylidene difluoride (PVDF).
Further, described polyvinylidene difluoride (PVDF) and Polythiophene are pulverized and are mixed comprise: described polyvinylidene difluoride (PVDF) was mixed 8 to 12 hours with the ball-grinding machine ball milling with described Polythiophene.
Further, the weight ratio of described polyvinylidene difluoride (PVDF) and described Polythiophene is 100:1 to 100:5.
Further, described organic solvent is N, dinethylformamide, N,N-dimethylacetamide, dimethyl sulfoxide (DMSO), chloroform, tetrahydrofuran (THF), triethyl phosphate or N-Methyl pyrrolidone.
Further, described described mixing material powder is dissolved in the organic solvent comprises: described mixing material powder is added in the described organic solvent and ultrasonic stir down, dissolve fully until described mixing material powder, the weight of wherein said organic solvent is 10 to 50 times of weight of described polyvinylidene difluoride (PVDF).
Further, with described organic mixing solutions at room temperature the vacuum standing and defoaming comprise: to the dull and stereotyped groove, the degree of depth of controlling described organic mixing solutions is 0.2 to 1 millimeter, and the vacuum suction bubble left standstill 4 to 5 hours with described organic mixing solutions.
Further, the described organic mixing solutions of described heating volatilizees described organic solvent to comprise from described organic mixing solutions: described organic mixing solutions heating under vacuum to 60 to 80 degrees centigrade, and was kept described 60 to 80 degrees centigrade of constant temperature 8 to 24 hours under vacuum condition.
In the method for embodiments of the invention, utilized 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 the dielectric polymer matrix, formed the organic compound dielectric film of Polythiophene-polyvinylidene difluoride (PVDF) (PEDOT-PVDF), the specific inductivity of this organic compound dielectric film is greatly improved, and adopt organic filler and matrix, make organic film have good processing properties.
Organic compound dielectric film of the method preparation of embodiments of the invention had both had higher dielectric constant, be again fexible film, have excellent machinability, the method that the while embodiment of the invention provides is easy and simple to handle, with low cost, be applicable to the production of film capacitor.
Description of drawings
Fig. 1 is the schematic flow sheet of method of the organic compound dielectric film of manufacturing of one embodiment of the invention.
Embodiment
Describe the method for the organic compound dielectric film of manufacturing of embodiments of the invention in detail below in conjunction with accompanying drawing.
As shown in Figure 1, in the embodiments of the invention, a kind of method of making organic compound dielectric film comprises step 10, step 12, step 14 and step 16.
Step 10: mix polyvinylidene difluoride (PVDF) and Polythiophene.
In the embodiments of the invention, can at first a certain amount of polyvinylidene difluoride (PVDF) and a certain amount of Polythiophene evenly be mixed, obtain the mixing material powder.
In the embodiments of the invention, can use any suitable method that polyvinylidene difluoride (PVDF) and Polythiophene are evenly mixed.For example, among the embodiment, can use ball-grinding machine, be about to a certain amount of polyvinylidene difluoride (PVDF) and a certain amount of Polythiophene and add in the ball-grinding machine, with ball-grinding machine polyvinylidene difluoride (PVDF) and the Polythiophene ball milling that adds be mixed, obtain the mixing material powder.Wherein, use the time of ball-grinding machine ball milling mixing polyvinylidene difluoride (PVDF) and Polythiophene to decide according to the needs of practical situation, for example, among the embodiment, polyvinylidene difluoride (PVDF) and Polythiophene can be ground mixing 8 to 12 hours with ball-grinding machine.
Polyvinylidene difluoride (PVDF) and Polythiophene are powdery substances, but there is certain agglomeration simultaneously in the two particle diameter difference.Therefore in the embodiments of the invention, the method that adopts ball milling to mix is mixed polyvinylidene difluoride (PVDF) and Polythiophene, can make the two mixing more even, and the mixing material powder that guarantees to obtain is below micron level
Through such processing, polyvinylidene difluoride (PVDF) and Polythiophene are mixed equably.
In the embodiments of the invention, in the aforesaid step, the weight ratio of polyvinylidene difluoride (PVDF) and Polythiophene is 100:1 to 100:5.
In the embodiments of the invention, the concrete quantity of pulverizing and mixed uniformly polyvinylidene difluoride (PVDF) and Polythiophene can be determined according to practical situation, be 100:1 to 100:5 as long as make the weight ratio of polyvinylidene difluoride (PVDF) and Polythiophene.
Step 12: the mixing material powder is dissolved in first solvent.
Obtained after the mixing material powder, in step 12, this mixing material powder has been dissolved in the organic solvent, obtained organic mixing solutions.
In the embodiments of the invention, organic solvent used herein can be to have volatility and polyvinylidene difluoride (PVDF) and Polythiophene can be dissolved in wherein organic solvent.For example, among the embodiment, the organic solvent here can be N, dinethylformamide, N,N-dimethylacetamide, dimethyl sulfoxide (DMSO), chloroform, tetrahydrofuran (THF), triethyl phosphate or N-Methyl pyrrolidone.
In the embodiments of the invention, this mixing material powder can be added in this organic solvent and ultrasonic and stir down, dissolve fully until the mixing material powder, wherein, the weight of organic solvent used herein is 10 to 50 times of weight of the polyvinylidene difluoride (PVDF) in the step 10.
In the embodiments of the invention, said " stirring down ultrasonic " refers to stir simultaneously with ultrasonic irradiation solution here, to promote the dissolving of mixing material powder.
Step 14: with organic mixing solutions vacuum standing and defoaming.
Obtained after organic mixing solutions, in step 14, should organic mixing solutions vacuum standing and defoaming at room temperature, the bubble in organic mixing solutions is broken away from from organic mixing solutions.
For example, among the embodiment, with organic mixing solutions at room temperature the detailed process of vacuum standing and defoaming can comprise: to the dull and stereotyped groove, the degree of depth of controlling this organic mixing solutions is 0.2 to 1 millimeter with organic mixing solutions, and the vacuum suction bubble left standstill 4 to 5 hours.
Through such processing, the bubble in organic mixing solutions is discharged from, and influences the formation of needed organic compound dielectric film to avoid these bubbles in subsequent step.
Step 16: heat organic mixing solutions and make the organic solvent volatilization.
Organic mixing solutions heats this organic mixing solutions after handling through the vacuum standing and defoaming of step 14, makes that the organic solvent in this organic mixing solutions volatilizees from this organic mixing solutions.In the process of organic solvent volatilization, the polyvinylidene difluoride (PVDF) and the Polythiophene composition that before be dissolved in this organic solvent will be separated out, in this process, because the seep effect of conductive polymers Polythiophene (PEDOT) in dielectric polymer based composites polyvinylidene difluoride (PVDF) (PVDF), the Polythiophene of lower aq with even filler in the polyvinylidene difluoride (PVDF) matrix, thereby formed the organic compound dielectric film of Polythiophene-polyvinylidene difluoride (PVDF) (PEDOT-PVDF).
In the embodiments of the invention, heating organic mixing solutions volatilizees organic solvent from organic mixing solutions concrete steps can comprise: organic mixing solutions heating under vacuum to 60 to 80 degrees centigrade, and was kept these 60 to 80 degrees centigrade of constant temperature 8 to 24 hours under vacuum condition.
Processing through step 16 has namely obtained the organic compound dielectric film of needed Polythiophene-polyvinylidene difluoride (PVDF) (PEDOT-PVDF).
Specify several specific exampless of method of the present invention below.
Example one:
(1) takes by weighing 10g polyvinylidene difluoride (PVDF) and 0.2g Polythiophene ball milling mixing 12h, obtain organic mixed material powders A 1;
(2) the 200ml N that the organic mixed material powders A 1 of polyvinylidene difluoride (PVDF) and Polythiophene is joined, in the dinethylformamide, the ultrasonic 3h that fully stirs down dissolves fully or disperses until organic dust, obtains organic mixing solutions B1;
(3) with mixing solutions B1 to the special-purpose dull and stereotyped groove, control solution deep is 0.5mm, and vacuum suction steeps and left standstill 4～5 hours, obtains no bubble mixed solution C 1;
(4) will not have bubble mixed solution C 1 heating under vacuum to 60 ℃, vacuum constant temperature 24h drives away organic solvent, obtains the complete organic compound dielectric film sample 1 of Polythiophene-polyvinylidene difluoride (PVDF) (PEDOT-PVDF), and recording specific inductivity is 13.5.
Example two:
(1) takes by weighing 10g polyvinylidene difluoride (PVDF) and 0.3g Polythiophene ball milling mixing 12h, obtain organic mixed material powders A 2;
(2) the 200ml N that polyvinylidene difluoride (PVDF) and the organic mixed powder A2 of Polythiophene are joined, in the dinethylformamide, the ultrasonic 3h that fully stirs down dissolves fully or disperses until organic dust, obtains organic mixing solutions B2;
(3) with mixing solutions B2 to the special-purpose dull and stereotyped groove, control solution deep is 0.5mm, and vacuum suction steeps and left standstill 4～5 hours, obtains no bubble mixed solution C 2;
(4) will not have bubble mixed solution C 2 heating under vacuum to 60 ℃, vacuum constant temperature 24h drives away organic solvent, obtains the complete organic compound dielectric film sample 2 of Polythiophene-polyvinylidene difluoride (PVDF) (PEDOT-PVDF), and recording specific inductivity is 15.8.
Example three:
(1) takes by weighing 10g polyvinylidene difluoride (PVDF) and 0.4g Polythiophene ball milling mixing 12h, obtain organic mixed material powders A 3;
(2) the 200ml N that polyvinylidene difluoride (PVDF) and Polythiophene organic mixed material powders A 3 are joined, in the dinethylformamide, the ultrasonic 3h that fully stirs down dissolves fully or disperses until organic dust, obtains organic mixing solutions B3;
(3) with mixing solutions B3 to the special-purpose dull and stereotyped groove, control solution deep is 0.5mm, and vacuum suction steeps and left standstill 4～5 hours, obtains no bubble mixed solution C 3;
(4) will not have bubble mixed solution C 3 heating under vacuum to 60 ℃, vacuum constant temperature 24h drives away organic solvent, obtains the complete organic compound dielectric film sample 3 of Polythiophene-polyvinylidene difluoride (PVDF) (PEDOT-PVDF), and recording specific inductivity is 17.4.
Example four:
(1) takes by weighing 10g polyvinylidene difluoride (PVDF) and 0.2g Polythiophene ball milling mixing 12h, obtain organic mixed material powders A 4;
(2) the 200ml N that polyvinylidene difluoride (PVDF) and the organic mixed powder A4 of Polythiophene are joined, in the dinethylformamide, the ultrasonic 3h that fully stirs down dissolves fully or disperses until organic dust, obtains organic mixing solutions B4;
(3) with mixing solutions B4 to the special-purpose dull and stereotyped groove, control solution deep is 0.5mm, and vacuum suction steeps and left standstill 4～5 hours, obtains no bubble mixed solution C 4;
(4) will not have bubble mixed solution C 4 heating under vacuum to 60 ℃, vacuum constant temperature 24h drives away organic solvent, obtains the complete organic compound dielectric film sample 4 of Polythiophene-polyvinylidene difluoride (PVDF) (PEDOT-PVDF), and recording specific inductivity is 16.7.
In the method for embodiments of the invention, utilized 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 the dielectric polymer matrix, formed the organic compound dielectric film of Polythiophene-polyvinylidene difluoride (PVDF) (PEDOT-PVDF), the specific inductivity of this organic compound dielectric film is greatly improved, and adopt organic filler and matrix, make organic film have good processing properties.
Organic compound dielectric film of the method preparation of embodiments of the invention had both had higher dielectric constant, be again fexible film, have excellent machinability, the method that the while embodiment of the invention provides is easy and simple to handle, with low cost, be applicable to the production of film capacitor.
More than describe the present invention by specific embodiment, but the present invention is not limited to these specific embodiments.It will be understood by those skilled in the art that and to make various modifications to the present invention, be equal to replacement, change etc. that these conversion all should be within protection scope of the present invention as long as do not deviate from spirit of the present invention.In addition, the different embodiment of above many places described " embodiment " expression can certainly be with its all or part of combination in one embodiment.
Claims (7)
1. a method of making organic compound dielectric film is characterized in that, comprising:
Polyvinylidene difluoride (PVDF) and Polythiophene are evenly mixed, obtain the mixing material powder;
Described mixing material powder is dissolved in the organic solvent, obtains organic mixing solutions;
With described organic mixing solutions vacuum standing and defoaming at room temperature;
Heat described organic mixing solutions described organic solvent is volatilized from described organic mixing solutions, obtain the organic compound dielectric film of Polythiophene-polyvinylidene difluoride (PVDF).
2. the method for claim 1 is characterized in that, described polyvinylidene difluoride (PVDF) and Polythiophene are evenly mixed comprises: described polyvinylidene difluoride (PVDF) was mixed 8 to 12 hours with the ball-grinding machine ball milling with described Polythiophene.
3. as claim 1 or 2 described methods, it is characterized in that: the weight ratio of described polyvinylidene difluoride (PVDF) and described Polythiophene is 100:1 to 100:5.
4. as any described method in the claim 1 to 3, it is characterized in that: described organic solvent is N, dinethylformamide, N,N-dimethylacetamide, dimethyl sulfoxide (DMSO), chloroform, tetrahydrofuran (THF), triethyl phosphate or N-Methyl pyrrolidone.
5. as any described method in the claim 1 to 3, it is characterized in that: described described mixing material powder is dissolved in the organic solvent comprises: described mixing material powder is added in the described organic solvent and ultrasonic stir down, dissolve fully until described mixing material powder, the weight of wherein said organic solvent is 10 to 50 times of weight of described polyvinylidene difluoride (PVDF).
6. as any described method in the claim 1 to 3, it is characterized in that: with described organic mixing solutions at room temperature the vacuum standing and defoaming comprise: with described organic mixing solutions to the dull and stereotyped groove, the degree of depth of controlling described organic mixing solutions is 0.2 to 1 millimeter, and the vacuum suction bubble left standstill 4 to 5 hours.
7. as any described method in the claim 1 to 3, it is characterized in that: the described organic mixing solutions of described heating volatilizees described organic solvent to comprise from described organic mixing solutions: described organic mixing solutions heating under vacuum to 60 to 80 degrees centigrade, and was kept described 60 to 80 degrees centigrade of constant temperature 8 to 24 hours under vacuum condition.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN117727937A (en) * | 2024-02-07 | 2024-03-19 | 紫金矿业新能源新材料科技(长沙)有限公司 | Composite lithium-rich lithium nickelate material and preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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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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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117727937A (en) * | 2024-02-07 | 2024-03-19 | 紫金矿业新能源新材料科技(长沙)有限公司 | Composite lithium-rich lithium nickelate material and preparation method and application thereof |
| CN117727937B (en) * | 2024-02-07 | 2024-05-28 | 紫金矿业新能源新材料科技(长沙)有限公司 | Composite lithium-rich lithium nickelate material and preparation method and application thereof |
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