CN102729562A - Composite medium film material based on polyvinylidene fluoride and graphene, and preparation method thereof - Google Patents
Composite medium film material based on polyvinylidene fluoride and graphene, and preparation method thereof Download PDFInfo
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- CN102729562A CN102729562A CN2012101797587A CN201210179758A CN102729562A CN 102729562 A CN102729562 A CN 102729562A CN 2012101797587 A CN2012101797587 A CN 2012101797587A CN 201210179758 A CN201210179758 A CN 201210179758A CN 102729562 A CN102729562 A CN 102729562A
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Abstract
The invention which discloses a composite medium film material based on polyvinylidene fluoride and graphene, and a preparation method thereof belongs to the technical field of electric functional materials. The composite medium film is obtained through compounding polyvinylidene fluoride and graphene, wherein the graphene mass percent content is 0.5-3% of the mass of the composite medium film. The preparation method comprises the following steps: preparing an organic solution (a system A) of polyvinylidene fluoride powder; adding graphene powder to the system A to obtain a system B; spraying the system B on the surface of a substrate through adopting an ultrasonic atomization technology; and drying the system B sprayed on the surface of the substrate to obtain the composite medium film material based on the polyvinylidene fluoride and the graphene. According to the invention, the graphene which approaches and does not exceed a percolation threshold is added to a polyvinylidene fluoride film to obtain the composite medium film material with the dielectric constant 100% higher than that of the pure polyvinylidene fluoride film material, and the original flexibility and the easy processability are maintained; and the preparation method has the advantages of simplicity, easy control and low cost.
Description
Technical field
The invention belongs to the electronic functional material technical field, relate to thin film dielectrics material and preparation method, especially high dielectric polymer thin-film material and high energy storage thin-film material.
Background technology
Dielectric substance has the function that stores electric charge and electric energy, so at all kinds of electron electric power devices, find broad application in space flight and aviation and the military weapon field.Along with the explosive growth of 21 century information industry, especially the intensification of (comprising device) of each class of electronic devices, microminiaturized requirement are improved constantly, so vigorous for increasing demand with high dielectric material (having high dielectric constant materials).Because the dielectric material that has no a kind of single component is at present taken into account good mechanicalness and processability having under the prerequisite of enough high-ks.Though for example the high-molecular organic material processing characteristics is excellent, and pliability is good, dielectric constant is lower usually; Though and ferroelectric ceramics has high dielectric constant, its processing temperature is too high, and very crisp; All be not suitable for independent application; So generally adopt complex technique, inorganic or organic high-dielectric constant particle and polymer are combined with each other through certain physical or chemical mode, obtain ideal material with the dielectric properties that improve composite.
Summary of the invention
The present invention provides a kind of composite dielectric film material based on Kynoar and Graphene and preparation method thereof.The present invention is matrix material with the Kynoar; Graphene-doped conductive material; Obtained the composite dielectric film material of high-k, characteristics such as have high-k, perfect heat-dissipating, density is low, cost is low are fit to apply to space flight military project device; The information technology electronic device, static storage and capacitors dielectrics.
Technical scheme of the present invention is following:
Based on the composite dielectric film material of Kynoar and Graphene, comprise that substrate is positioned at the composite dielectric film of substrate surface, said composite dielectric film is composited by Kynoar and Graphene; Wherein the mass percentage content of Graphene is 0.5% to 3% of a composite dielectric film quality.
Composite dielectric film preparation methods based on Kynoar and Graphene may further comprise the steps:
Step 1: the preparation mass percent concentration is no more than the organic solution of 5% Kynoar powder, is designated as system A.Organic solvent can be dimethyl sulfoxide (DMSO), dimethyl formamide, chloroform, dimethylacetylamide, oxolane, N-methyl pyrrolidone, triethyl phosphate or tetramethylurea isopolarity solvent among the system A.
Step 2: in system A, add graphene powder, ultrasonic being uniformly dispersed, the mixed system that obtains is designated as system B.Wherein among the system B mass percentage content of graphene powder be among the system B Kynoar and graphene powder quality and 0.5% to 3%.
Step 3: adopt ultrasonic atomizatio technology, B is sprayed at substrate surface with step 2 gained system.
Step 4: the system B to being sprayed at substrate surface is dried processing, removes organic solvent, obtains the composite dielectric film material based on Kynoar and Graphene.
Need to prove: when 1, preparing system A, can accompany by 20 ~ 100 ℃ sonicated, to quicken the dissolving of Kynoar powder; 2, bake out temperature is 40 ~ 100 ℃ in the step 4, and the time is 2 ~ 5 hours.
Essence of the present invention be in polyvinylidene difluoride film (thin polymer film), mix near but be no more than the Graphene (conducting particles) of percolation threshold; Obtain exceeding the composite dielectric film material of pure polyvinylidene difluoride film material dielectric constant more than 100%, and kept the pliability and the workability of polymer.Common pure polyvinylidene difluoride film material dielectric constant is 9, and the dielectric constant of composite dielectric film material provided by the invention reaches as high as 21.And simple, the easy control of composite dielectric film preparation methods provided by the invention, with low cost.
The specific embodiment
Embodiment one
At first get 1.99g Kynoar powder and be dissolved in the organic solvent (concentration is no more than 5%), make Kynoar fully be dissolved in the solvent, obtain system A temperature 20-100 ℃ of wide-ultra sound 1 hour; Get the 0.01g graphene powder then and slowly be dissolved among the system A, and constantly stir, continued under 20-100 ℃ condition ultrasonic 1-10 hour, obtain system B; Adopt ultrasonic atomizatio technology again, B is sprayed at substrate surface with system; (temperature is 40 ~ 100 ℃ at last the system B that is sprayed at substrate surface to be dried processing; Time is 2 ~ 5 hours); Remove organic solvent; Obtain the composite dielectric film material based on Kynoar and Graphene, wherein the mass percentage content of Graphene is 0.5% of a composite dielectric film quality, is designated as sample one.
Embodiment two
At first get 1.98g Kynoar powder and be dissolved in the organic solvent (concentration is no more than 5%), make Kynoar fully be dissolved in the solvent, obtain system A temperature 20-100 ℃ of wide-ultra sound 1 hour; Get the 0.02g graphene powder then and slowly be dissolved among the system A, and constantly stir, continued under 20-100 ℃ condition ultrasonic 1-10 hour, obtain system B; Adopt ultrasonic atomizatio technology again, B is sprayed at substrate surface with system; (temperature is 40 ~ 100 ℃ at last the system B that is sprayed at substrate surface to be dried processing; Time is 2 ~ 5 hours); Remove organic solvent; Obtain the composite dielectric film material based on Kynoar and Graphene, wherein the mass percentage content of Graphene is 1.0% of a composite dielectric film quality, is designated as sample two.
Embodiment three
At first get 1.97g Kynoar powder and be dissolved in the organic solvent (concentration is no more than 5%) in temperature 20-100 ℃ ultrasonic 1 hour, make Kynoar fully be dissolved in the solvent, obtain system A; Get the 0.03g graphene powder then and slowly be dissolved among the system A, and constantly stir, continued under 20-100 ℃ condition ultrasonic 1-10 hour, obtain system B; Adopt ultrasonic atomizatio technology again, B is sprayed at substrate surface with system; (temperature is 40 ~ 100 ℃ at last the system B that is sprayed at substrate surface to be dried processing; Time is 2 ~ 5 hours); Remove organic solvent; Obtain the composite dielectric film material based on Kynoar and Graphene, wherein the mass percentage content of Graphene is 1.5% of a composite dielectric film quality, is designated as sample three.
Embodiment four
At first get 1.96g Kynoar powder and be dissolved in the organic solvent (concentration is no more than 5%) in temperature 20-100 ℃ ultrasonic 1 hour, make Kynoar fully be dissolved in the solvent, obtain system A; Get the 0.04g graphene powder then and slowly be dissolved in the above-mentioned solution, and constantly stir, continued under 20-100 ℃ condition ultrasonic 1-10 hour, obtain system B; Adopt ultrasonic atomizatio technology again, B is sprayed at substrate surface with system; (temperature is 40 ~ 100 ℃ at last the system B that is sprayed at substrate surface to be dried processing; Time is 2 ~ 5 hours); Remove organic solvent; Obtain the composite dielectric film material based on Kynoar and Graphene, wherein the mass percentage content of Graphene is 2.0% of a composite dielectric film quality, is designated as sample four.
Embodiment five
At first get 1.95g Kynoar powder and be dissolved in the organic solvent (concentration is no more than 5%) in temperature 20-100 ℃ ultrasonic 1 hour, make Kynoar fully be dissolved in the solvent, obtain system A; Get the 0.05g graphene powder then and slowly be dissolved in the above-mentioned solution, and constantly stir, continued under 20-100 ℃ condition ultrasonic 1-10 hour, obtain system B; Adopt ultrasonic atomizatio technology again, B is sprayed at substrate surface with system; (temperature is 40 ~ 100 ℃ at last the system B that is sprayed at substrate surface to be dried processing; Time is 2 ~ 5 hours); Remove organic solvent; Obtain the composite dielectric film material based on Kynoar and Graphene, wherein the mass percentage content of Graphene is 2.5% of a composite dielectric film quality, is designated as sample five.
Embodiment six
At first get 1.94g Kynoar powder and be dissolved in the organic solvent (concentration is no more than 5%) in temperature 20-100 ℃ ultrasonic 1 hour, make Kynoar fully be dissolved in the solvent, obtain system A; Get the 0.06g graphene powder then and slowly be dissolved in the above-mentioned solution, and constantly stir, continued under 20-100 ℃ condition ultrasonic 1-10 hour, obtain system B; Adopt ultrasonic atomizatio technology again, B is sprayed at substrate surface with system; (temperature is 40 ~ 100 ℃ at last the system B that is sprayed at substrate surface to be dried processing; Time is 2 ~ 5 hours); Remove organic solvent; Obtain the composite dielectric film material based on Kynoar and Graphene, wherein the mass percentage content of Graphene is 3.0% of a composite dielectric film quality, is designated as sample six.
For the composite dielectric film of above-mentioned six kinds of different Graphene content, at 25 ° of C of probe temperature, under the test frequency 1000Hz condition, record the dielectric constant of six kinds of samples, as shown in table 1:
The dielectric properties of table 1 sample
| Specimen | Pure PVDF film | Sample 1 | Sample 2 | Sample 3 | Sample 4 | Sample 5 | Sample 6 |
| Dielectric constant | 8.9 | 9.5 | 10.1 | 12.3 | 15.6 | 21.2 | 18.7 |
Can find out from table 1; Of the present invention in polyvinylidene difluoride film (thin polymer film), mix near but be no more than the Graphene (conducting particles) of percolation threshold, obtain exceeding the composite dielectric film material of pure polyvinylidene difluoride film material dielectric constant more than 100%.Common pure polyvinylidene difluoride film material dielectric constant is 9, and the dielectric constant of composite dielectric film material provided by the invention reaches as high as 21.
Composite dielectric film material provided by the invention; The pliability and the workability that have kept pure polyvinylidene difluoride film when reentrying high dielectric constant; Can be applicable to space flight military project device, information technology electronic device, static storage and capacitors dielectrics.
Claims (5)
1. based on the composite dielectric film material of Kynoar and Graphene, comprise that substrate is positioned at the composite dielectric film of substrate surface, said composite dielectric film is composited by Kynoar and Graphene; Wherein the mass percentage content of Graphene is 0.5% to 3% of a composite dielectric film quality.
2. based on the composite dielectric film preparation methods of Kynoar and Graphene, may further comprise the steps:
Step 1: the preparation mass percent concentration is no more than the organic solution of 5% Kynoar powder, is designated as system A;
Step 2: in system A, add graphene powder, ultrasonic being uniformly dispersed, the mixed system that obtains is designated as system B; Wherein among the system B mass percentage content of graphene powder be among the system B Kynoar and graphene powder quality and 0.5% to 3%.
Step 3: adopt ultrasonic atomizatio technology, B is sprayed at substrate surface with step 2 gained system;
Step 4: the system B to being sprayed at substrate surface is dried processing, removes organic solvent, obtains the composite dielectric film material based on Kynoar and Graphene.
3. the composite dielectric film preparation methods based on Kynoar and Graphene according to claim 2; It is characterized in that organic solvent is dimethyl sulfoxide (DMSO), dimethyl formamide, chloroform, dimethylacetylamide, oxolane, N-methyl pyrrolidone, triethyl phosphate or tetramethylurea among the system A.
4. the composite dielectric film preparation methods based on Kynoar and Graphene according to claim 2 is characterized in that, during preparation system A, accompanies by 20 ~ 100 ℃ sonicated, to quicken the dissolving of Kynoar powder.
5. the composite dielectric film preparation methods based on Kynoar and Graphene according to claim 2 is characterized in that bake out temperature is 40 ~ 100 ℃ in the step 4, and the time is 2 ~ 5 hours.
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| CN2012101797587A CN102729562A (en) | 2012-06-04 | 2012-06-04 | Composite medium film material based on polyvinylidene fluoride and graphene, and preparation method thereof |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103319820A (en) * | 2013-06-24 | 2013-09-25 | 哈尔滨工程大学 | Preparation method of graphene and polymer conductive composite material |
| CN103538312A (en) * | 2013-09-10 | 2014-01-29 | 浙江工业大学 | Alternating layered graphene oxide/polyvinyl alcohol dielectric material and preparation method thereof |
| CN103951915A (en) * | 2014-04-29 | 2014-07-30 | 上海交通大学 | Lightweight flexible polymer-based high-energy-density material and preparation method thereof |
| CN105295265A (en) * | 2015-12-07 | 2016-02-03 | 郑州轻工业学院 | Modified polyvinylidene fluoride super-hydrophobic material and preparation method thereof |
| CN109485884A (en) * | 2018-11-02 | 2019-03-19 | 北京石油化工学院 | The preparation method of polyvinylidene difluoride film |
| CN109777009A (en) * | 2018-12-27 | 2019-05-21 | 佛山科学技术学院 | A kind of GR-TiO being used to prepare high density capacitors2- PVDF nanocomposite and preparation method thereof |
| CN110157346A (en) * | 2019-05-06 | 2019-08-23 | 费植煌 | A kind of decorating film of containing graphene |
| CN110951318A (en) * | 2019-12-18 | 2020-04-03 | 西北工业大学深圳研究院 | Method for inhibiting coffee ring effect of polymer-based ink, polymer solid film and polymer-based ink |
| CN111048659A (en) * | 2018-10-15 | 2020-04-21 | 电子科技大学 | Piezoelectric film and preparation method thereof |
| CN113651985A (en) * | 2021-08-18 | 2021-11-16 | 吉林大学重庆研究院 | Graphene-based ultra-smooth surface with photoresponse and preparation method thereof |
-
2012
- 2012-06-04 CN CN2012101797587A patent/CN102729562A/en active Pending
Non-Patent Citations (1)
| Title |
|---|
| JINHONG YU ET AL: "Permittivity, Thermal Conductivity and Thermal Stability of Poly(vinylidene fluoride)/Graphene Nanocomposites", 《IEEE TRANSACTIONS ON DIELECTRICS AND ELECTRICAL INSULATION》 * |
Cited By (17)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103319820A (en) * | 2013-06-24 | 2013-09-25 | 哈尔滨工程大学 | Preparation method of graphene and polymer conductive composite material |
| CN103319820B (en) * | 2013-06-24 | 2015-09-30 | 哈尔滨工程大学 | The preparation method of a kind of Graphene and composite conducting polymer material |
| CN103538312A (en) * | 2013-09-10 | 2014-01-29 | 浙江工业大学 | Alternating layered graphene oxide/polyvinyl alcohol dielectric material and preparation method thereof |
| CN103538312B (en) * | 2013-09-10 | 2016-05-18 | 浙江工业大学 | A kind of alternately stratiform graphene oxide/polyvinyl alcohol dielectric material and preparation method thereof |
| CN103951915A (en) * | 2014-04-29 | 2014-07-30 | 上海交通大学 | Lightweight flexible polymer-based high-energy-density material and preparation method thereof |
| CN103951915B (en) * | 2014-04-29 | 2016-06-01 | 上海交通大学 | Light flexible polymer-based high energy storage density material and its preparation method |
| CN105295265A (en) * | 2015-12-07 | 2016-02-03 | 郑州轻工业学院 | Modified polyvinylidene fluoride super-hydrophobic material and preparation method thereof |
| CN105295265B (en) * | 2015-12-07 | 2018-01-12 | 郑州轻工业学院 | A kind of modified polyvinilidene fluoride super hydrophobic material and preparation method thereof |
| CN111048659A (en) * | 2018-10-15 | 2020-04-21 | 电子科技大学 | Piezoelectric film and preparation method thereof |
| CN109485884A (en) * | 2018-11-02 | 2019-03-19 | 北京石油化工学院 | The preparation method of polyvinylidene difluoride film |
| CN109485884B (en) * | 2018-11-02 | 2021-07-09 | 北京石油化工学院 | Preparation method of polyvinylidene fluoride film |
| CN109777009A (en) * | 2018-12-27 | 2019-05-21 | 佛山科学技术学院 | A kind of GR-TiO being used to prepare high density capacitors2- PVDF nanocomposite and preparation method thereof |
| CN110157346A (en) * | 2019-05-06 | 2019-08-23 | 费植煌 | A kind of decorating film of containing graphene |
| CN110157346B (en) * | 2019-05-06 | 2021-05-07 | 费植煌 | Decoration film containing graphene |
| CN110951318A (en) * | 2019-12-18 | 2020-04-03 | 西北工业大学深圳研究院 | Method for inhibiting coffee ring effect of polymer-based ink, polymer solid film and polymer-based ink |
| CN113651985A (en) * | 2021-08-18 | 2021-11-16 | 吉林大学重庆研究院 | Graphene-based ultra-smooth surface with photoresponse and preparation method thereof |
| CN113651985B (en) * | 2021-08-18 | 2022-09-30 | 吉林大学重庆研究院 | Graphene-based ultra-smooth surface with photoresponse and preparation method thereof |
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Application publication date: 20121017 |