CN103465576B - A kind of high dielectric composite film and preparation method thereof - Google Patents
A kind of high dielectric composite film and preparation method thereof Download PDFInfo
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- CN103465576B CN103465576B CN201310426421.6A CN201310426421A CN103465576B CN 103465576 B CN103465576 B CN 103465576B CN 201310426421 A CN201310426421 A CN 201310426421A CN 103465576 B CN103465576 B CN 103465576B
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Abstract
The invention discloses a kind of high dielectric composite film and preparation method thereof, it belongs to electric thin Material Field, this high dielectric composite film is alternately composited by polymer and inorganic nano-particle, the method, based on LB embrane method deposited polymer and inorganic nano-particle composite construction, obtains the high dielectric property of laminated film by the good cooperative effect between polymer and inorganic nano-particle.The present invention is based on ripe LB membrane technology, overcome defect existing in prior art, be easy to prepare large area, self-supported membrane, preparation method rationally simple, be easy to operation.
Description
Technical field
The present invention relates to electric thin material in electronic material and components and parts field, be specifically related to a kind of high dielectric composite film based on polymer and inorganic nano-particle and preparation method thereof.
Background technology
High density capacitors is widely used in guided missile and space field, is mainly used in the new concept weapon such as electromagnet pulse weapon and electromagnetic energy weapon, PRK weapon, particle beam accelerator, high-power microwave source, x-ray source and strategic ballistic missile, electromagnetic installing is first-class.Because the states such as the high density capacitors U.S. implement embargo to China, the development of China's Novel electric magnetic energy weapon is restricted.
In high density capacitors, the form of the dielectric material used and performance determine the usefulness of capacitor greatly.Accelerate the research and development to novel medium material during the nearly last ten years abroad greatly, promote the development of various high-end energy storage electronic component.Based on the core that novel medium material technology is high-performance energy-storage capacitor, for the progress of the novel medium material of high energy-storage capacitor, the technical development of new concept weapon and non-nuclear weapon can be promoted greatly.
The dielectric properties of high density capacitors to dielectric material propose more and more higher requirement, it is desirable to obtain the having superior novel electron material of the combination property such as high-dielectric coefficient, low-loss, easily processing.All the time, inorganic high-dielectric material receives very large concern, but pursues along with to the good toughness of high dielectric material, high dielectric constant and good film forming in recent years, and the focus of research has transferred to the composite based on inorganic/polymer gradually.
Energy-storage travelling wave tube is as the parts occupying maximum ratio weight and volume in energy resource system, and the raising of its energy storage density is significant.And dielectric material is as the core material of energy storage device, the development of novel medium material technology supports energy resource system in pulse power weapon and develops to miniaturized, lightweight.In numerous dielectric materials, high dielectric polymer particularly Intrinsical height dielectric polymer has the advantages such as dielectric constant is large, Heat stability is good, therefore becomes the focus of extensively research both at home and abroad.Be that the thin film capacitor of energy-accumulating medium has the highest energy storage density with dielectric polymer, the room for promotion of energy storage density is very large, its good processing characteristics simultaneously.
The dielectric properties of high density capacitors to dielectric material propose more and more higher requirement, it is desirable to obtain the having superior novel electron material of the combination property such as high-dielectric coefficient, low-loss, easily processing.All the time, inorganic high-dielectric material receives very large concern, but pursues along with to the good toughness of high dielectric material, high dielectric constant and good film forming in recent years, and the focus of research has transferred to the composite based on inorganic/polymer gradually.
At present, for high dielectric property inorganic/polymer thin-film material, the high dielectric material of new structure is obtained on the one hand by different MOLECULE DESIGN and synthetic technology, but while the high dielectric property obtaining polymer, how to ensure that the matched well between inorganic material and organic material remains letter problem to be solved.
Summary of the invention
For existing technical problem, the object of the invention is to how to provide a kind of high dielectric composite film and preparation method thereof, this high dielectric composite film, based on the inorganic nano-particle of polymer and coupling agent, assembles the matched well that can realize between inorganic material and organic material by LB film.
For achieving the above object, the present invention adopts following technical scheme:
A kind of high dielectric composite film, it is characterized in that, comprise the inorganic nano-particle thin layer of polymer film layer and the coupling agent prepared by LB film method, described polymeric layer forms through the vertical alternating deposit of LB film method the membrane structure that polymer/inorganic nanometer particle replaces compound with the inorganic nano-particle sublayer of coupling agent on a substrate.
The preparation method of high dielectric composite film provided by the invention, is characterized in that, specifically comprise the following steps:
1. polymer is dissolved in organic solvent, forms polymer dispersed solution, for the deposition of Polymer LB Films;
2. the nano particle of coupling agent is dissolved in n-butanol, forms coupling agent inorganic nano-particle molecular disperse solution, for the deposition of inorganic nano-particle LB film;
3. the polymer dispersed solution 1. obtained and the coupling agent inorganic nano-particle molecular disperse solution that 2. obtains are dripped respectively the deionized water surface in Different L B film groove, polymer and the dispersion of coupling agent inorganic nano-particle spread in deionized water surface;
4. comperession polymer and coupling agent inorganic nano-particle, to film forming mould, form polymer and the inorganic nano-particle membrane structure of high-density array to the sliding barrier of control LB film device respectively respectively;
5. the mode of vertical film forming is adopted to be transferred on substrate by polymer film and inorganic nano-particle film successively;
6. repeat step 1.-5., obtain the polymer/inorganic nanometer particle composite film structure of different-thickness.
In the preparation method of high dielectric composite film provided by the invention, described step 1. in polymer be Kynoar, poly-titanium cyanines copper, poly-titanium cyanines zinc height dielectric polymer material, organic solvent is DMF.
In the preparation method of high dielectric composite film provided by the invention, step 2. described in coupling agent inorganic nano-particle be barium titanate, strontium titanates, the zirconia titanate nano particle of silane coupler, it has higher dielectric constant.
In the preparation method of high dielectric composite film provided by the invention, it is characterized in that, its more specifically step be:
1. be dissolved in by Kynoar in DMF solvent, the concentration of Kynoar is 10-15mg/ml, forms the Kynoar dispersion liquid being used for LB film preparation;
2. silane coupler barium titanate is dissolved in n-butanol solvent, the concentration of silane coupler barium titanate is 8-12mg/ml, forms the nanoparticle dispersion liquid being used for LB film preparation;
3. solution that 1. and 2. 500-800 μ l obtain drips the deionized water solution surface in Different L B film groove to adopt microsyringe to extract respectively, starts press mold, now form polymer and film of nanoparticles at gas/liquid interface after solvent volatilization 30-40min;
4. the sliding barrier of control LB film device is with the speed compression polymer film of 0.2-0.5mm/min to mould 30-35mN/m, and the mould of nano particle is 15-20mN/m;
5. adopt the mode of vertical film forming to be first transferred on substrate by polymer film, rate of film build is 0.2-0.4mm/min, then is transferred on polymer film by film of nanoparticles, and rate of film build is 0.2-0.4mN/m;
6. the high dielectric composite film structure that 5. step repeatedly just obtains a kind of Polymer/nano particle is repeated.
Compared with prior art, the present invention has following beneficial effect:
One, high dielectric composite film provided by the invention is based on the inorganic nano-particle of polymer and coupling agent, is assembled the matched well that can realize between inorganic material and organic material by LB film;
Two, the present invention can realize combination good between organic polymer and inorganic nano-particle by the assembling of LB film, forms good cooperative effect, makes film have higher dielectric constant, and can peel off from substrate the feature realizing self-supporting.
Accompanying drawing explanation
Fig. 1 is structural representation of the present invention;
Reference numeral is: 1 be substrate, 2 be high dielectric polymer film layer, 3 for coupling agent inorganic nano-particle thin layer.
Detailed description of the invention
Below in conjunction with the drawings and the specific embodiments, the invention will be further described
A kind of high dielectric composite film, comprise the inorganic nano-particle thin layer of polymer film layer and the coupling agent prepared by LB film method, described polymeric layer forms through the vertical alternating deposit of LB film method the membrane structure that polymer/inorganic nanometer particle replaces compound with the inorganic nano-particle sublayer of coupling agent on a substrate.
The present invention selects the polymer of high dielectric and the inorganic nano-particle material of coupling agent, by the alternating structure of LB film method assembling even compact, and obtains different alternating structures and the thickness of film by control LB film film forming order.
Rely on ripe LB film film build method, the inorganic nano-particle of the polymer based on high dielectric prepared by the present invention and coupling agent can be prepared on multiple substrate and (comprise flexible substrates), obtains the high dielectric composite film of large area, self-supporting.
Some the high dielectric composite film structure example adopting the present invention to prepare are as follows:
1. Kynoar/barium titanate nano particle composite film;
2. titan bronze/strontium titanates Nanocomposites film;
3. Kynoar/zirconia titanate Nanocomposites film;
Below specific embodiments of the invention:
embodiment 1
Preparation method is as follows:
1. be dissolved in by Kynoar in DMF solvent, the concentration of Kynoar is 10-15mg/ml, forms the Kynoar dispersion liquid being used for LB film preparation;
2. silane coupler barium titanate is dissolved in n-butanol solvent, the concentration of silane coupler barium titanate is 8-12mg/ml, forms the nanoparticle dispersion liquid being used for LB film preparation;
3. solution that 1. and 2. 500-800 μ l obtain drips the deionized water solution surface in Different L B film groove to adopt microsyringe to extract respectively, starts press mold, now form polymer and film of nanoparticles at gas/liquid interface after solvent volatilization 30-40min;
4. the sliding barrier of control LB film device is with the speed compression polymer film of 0.2-0.5mm/min to mould 30-35mN/m, and the mould of nano particle is 15-20mN/m;
5. adopt the mode of vertical film forming to be first transferred on substrate by polymer film, rate of film build is 0.2-0.4mm/min, then is transferred on polymer film by film of nanoparticles, and rate of film build is 0.2-0.4mN/m;
6. the high dielectric composite film structure that 5. step repeatedly just obtains Kynoar/barium titanate nano particle is repeated.
embodiment 2
As Fig. 1, polymer is Kynoar, and nano particle is strontium titanates.
The preparation flow of complex thin film structure is similar to embodiment 1.
Thus obtain the high dielectric composite film structure of Kynoar/strontium titanates nano particle.
embodiment 3
As Fig. 1, polymer is poly-titanium cyanines copper.Nano particle is barium titanate.
The preparation flow of complex thin film structure is similar to embodiment 1.
Thus obtain the high dielectric composite film structure of poly-titanium cyanines copper/barium titanate nano particle.
embodiment 4
As Fig. 1, polymer is poly-titanium cyanines copper.Nano particle is zirconia titanate.
The preparation flow of complex thin film structure is similar to embodiment 1.
Thus obtain the high dielectric composite film structure of poly-titanium cyanines copper/zirconia titanate nano particle.
Claims (1)
1. the preparation method of high dielectric composite film, is characterized in that, concrete steps are:
1. be dissolved in by Kynoar in DMF solvent, the concentration of Kynoar is 10-15mg/ml, forms the Kynoar dispersion liquid being used for LB film preparation;
2. silane coupler barium titanate is dissolved in n-butanol solvent, the concentration of silane coupler barium titanate is 8-12mg/ml, forms the nanoparticle dispersion liquid being used for LB film preparation;
3. adopt microsyringe to extract respectively dispersant liquid drop that 1. and 2. 500-800 μ l obtain is added on the deionized water solution surface in Different L B film groove, starts press mold, now form polymer and film of nanoparticles at gas/liquid interface after solvent volatilization 30-40min;
4. the sliding barrier of control LB film device is with the speed compression polymer film of 0.2-0.5mm/min to mould 30-35mN/m, and the mould of nano particle is 15-20mN/m;
5. adopt the mode of vertical film forming to be first transferred on substrate by polymer film, rate of film build is 0.2-0.4mm/min, then is transferred on polymer film by film of nanoparticles, and rate of film build is 0.2-0.4mN/m;
6. the high dielectric composite film structure that 5. step repeatedly just obtains a kind of Polymer/nano particle is repeated.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101919080A (en) * | 2007-12-11 | 2010-12-15 | 韩国食品研究院 | Substrate manufacturing method for sensor applications using optical characteristics and the substrate therefrom |
| CN102173155A (en) * | 2011-01-14 | 2011-09-07 | 北京化工大学 | Polymer-base ceramic composite dielectric material 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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| US9390857B2 (en) * | 2008-09-30 | 2016-07-12 | General Electric Company | Film capacitor |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101919080A (en) * | 2007-12-11 | 2010-12-15 | 韩国食品研究院 | Substrate manufacturing method for sensor applications using optical characteristics and the substrate therefrom |
| CN102173155A (en) * | 2011-01-14 | 2011-09-07 | 北京化工大学 | Polymer-base ceramic composite dielectric material and preparation method thereof |
| CN102632675A (en) * | 2012-04-17 | 2012-08-15 | 电子科技大学 | Method for preparing nanocomposite dielectric film |
Non-Patent Citations (1)
| Title |
|---|
| LB技术在纳米粒子组装中的应用;高书燕等;《应用化学》;20050731;第22卷(第7期);第697-702页 * |
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