CN105085947A - Multiwalled-carbon-nanotube-loaded polyimide high-dielectric-permittivity composite film doped with nano titanium carbide and used for capacitor and preparing method of composite film - Google Patents
Multiwalled-carbon-nanotube-loaded polyimide high-dielectric-permittivity composite film doped with nano titanium carbide and used for capacitor and preparing method of composite film Download PDFInfo
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- CN105085947A CN105085947A CN201510466974.3A CN201510466974A CN105085947A CN 105085947 A CN105085947 A CN 105085947A CN 201510466974 A CN201510466974 A CN 201510466974A CN 105085947 A CN105085947 A CN 105085947A
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Abstract
The invention discloses a multiwalled-carbon-nanotube-loaded polyimide high-dielectric-permittivity composite film doped with nano titanium carbide and used for a capacitor. According to the composite film, the nano titanium carbide, multiwalled carbon nanotubes, nano aluminum and other filler are doped in the polyimide preparing process. The multiwalled carbon nanotubes are loaded in the nano filler so as to improve the dispersity and the utilization rate of the nano filler. A powder body is covered with a polyvinyl alcohol film good in stability in an organic solvent, and the composite powder body with the surface modified and processed by a silane coupling agent is good in compatibility with an organic glue solution interface and can be evenly dispersed more easily, so that the dielectric properties of a material are stably and efficiently improved. The dielectric properties of the finally prepared polyimide film pure in composite film material are greatly improved, good mechanical properties and processability are still maintained, and application prospects are good.
Description
Technical field
The present invention relates to high-dielectric composite material preparing technical field, particularly relate to polyimide high dielectric composite film of a kind of electrical condenser blending nano titanium carbide loading multi-wall carbon nanotubes and preparation method thereof.
Background technology
Along with the progress of electronic technology, more and more higher to the performance requriements such as dielectric properties, stored energy capacitance of electrical condenser, the dielectric material of development high-k, low-dielectric loss just seems particularly important, traditional film capacitor dielectric material mainly contains the material such as polyimide, polycarbonate of nonpolar polystyrene, polyethylene, polypropylene and polarity, wherein polyimide has the advantage such as good mechanical property and thermostability, workability, easy film forming good with substrate compatibility, has outstanding performance in the high performance dielectric film of preparation.Simple Kapton specific inductivity is too low, Production requirement can not be met, the method mainly using blending high dielectric material in polymkeric substance for the method improving thin-film dielectric constant common at present, however the general present film poor processability of defect map of these methods, specific inductivity improve while the aspect such as dielectric loss increase.
Summary of the invention
The object of the invention is exactly the defect in order to make up prior art, provides polyimide high dielectric composite film of a kind of electrical condenser blending nano titanium carbide loading multi-wall carbon nanotubes and preparation method thereof.
The present invention is achieved by the following technical solutions:
A polyimide high dielectric composite film for electrical condenser blending nano titanium carbide loading multi-wall carbon nanotubes, this laminated film is prepared by the raw material of following weight part: pyromellitic acid anhydride 10-12,4,4
,-diamino-diphenyl ether 8-10, NVP 3-5, nano titanium carbide 2-3, nanometer aluminium powder 0.01-0.02, N,N-dimethylacetamide 20-25, dehydrated alcohol 3-5, silane coupling agent 0.1-0.2, hydroxyethyl methylacrylate 0.4-0.5, multi-walled carbon nano-tubes 0.4-0.5, polyvinyl alcohol 0.1-0.2, water 4-5.
The preparation method of the polyimide high dielectric composite film of described a kind of electrical condenser blending nano titanium carbide loading multi-wall carbon nanotubes, described preparation method is:
(1) preparation of surface-modified nano titanium carbide loading multi-wall carbon nanotubes solution: first multi-walled carbon nano-tubes is dried to neutral through acid treatment after washing, again polyvinyl alcohol dissolution is mixed with solution in water, by the dry multi-walled carbon nano-tubes after acid treatment above, nano titanium carbide, nano aluminum drops in solution, after ultrasonic disperse 20-30min, mixed slurry is heated to 60-80 DEG C, constant temperature milled processed 30-40min, subsequently gained slurry is dried, remove moisture completely, gained powder and silane coupling agent mixing and stirring, obtain surface-modified nano titanium carbide loading multi-wall carbon nanotubes composite granule, finally gained composite granule is dropped in dehydrated alcohol, after ultrasonic disperse 20-30min, gained material is for subsequent use,
(2) by 4,4
,-diamino-diphenyl ether drops into N, in N-N,N-DIMETHYLACETAMIDE, after stirring, divide 5 steps to add the pyromellitic acid anhydride of equivalent, react 10-12h after interpolation, obtain polyamic acid glue, composite granule ethanol solution step (1) prepared subsequently drops in glue, add other leftover materials after being uniformly mixed 8-10h, continue stirring and make mixing of materials even, gained composite glue solution is for subsequent use;
(3) composite glue solution prepared by step (2) coated and sheet glass puts into convection oven carry out imidization process, treatment condition are: treatment temp 150-200 DEG C, the treatment time: 1.5-2h, obtain described laminated film.
Advantage of the present invention is: the present invention is by blending nano titanium carbide in Kapton preparation process, multi-walled carbon nano-tubes, the fillers such as nano aluminum, and by carbon multi-wall nano tube loaded in Nano filling, improve its dispersed and utilization ratio, the polyvinyl alcohol film in organic solvent with good stability is utilized to carry out coated process to powder, composite granule after silane coupling agent surface modification treatment and organic glue interface compatibility good, more easily be uniformly dispersed, the dielectric properties of the improvement material of stability and high efficiency, the more simple Kapton of the composite film material finally prepared obtains and greatly improves in dielectric properties, and still keep good mechanical property and processing characteristics, application prospect is good.
Embodiment
A polyimide high dielectric composite film for electrical condenser blending nano titanium carbide loading multi-wall carbon nanotubes, this laminated film is prepared by the raw material of following weight part: pyromellitic acid anhydride 10,4,4
,-diamino-diphenyl ether 8, NVP 3, nano titanium carbide 2, nanometer aluminium powder 0.01, N,N-dimethylacetamide 20, dehydrated alcohol 3, silane coupling agent 0.1, hydroxyethyl methylacrylate 0.4, multi-walled carbon nano-tubes 0.4, polyvinyl alcohol 0.1, water 4.
The preparation method of the polyimide high dielectric composite film of described a kind of electrical condenser blending nano titanium carbide loading multi-wall carbon nanotubes, described preparation method is:
(1) preparation of surface-modified nano titanium carbide loading multi-wall carbon nanotubes solution: first multi-walled carbon nano-tubes is dried to neutral through acid treatment after washing, again polyvinyl alcohol dissolution is mixed with solution in water, by the dry multi-walled carbon nano-tubes after acid treatment above, nano titanium carbide, nano aluminum drops in solution, after ultrasonic disperse 20min, mixed slurry is heated to 60 DEG C, constant temperature milled processed 30min, subsequently gained slurry is dried, remove moisture completely, gained powder and silane coupling agent mixing and stirring, obtain surface-modified nano titanium carbide loading multi-wall carbon nanotubes composite granule, finally gained composite granule is dropped in dehydrated alcohol, after ultrasonic disperse 20min, gained material is for subsequent use,
(2) by 4,4
,-diamino-diphenyl ether drops into N, in N-N,N-DIMETHYLACETAMIDE, after stirring, divide 5 steps to add the pyromellitic acid anhydride of equivalent, react 10h after interpolation, obtain polyamic acid glue, composite granule ethanol solution step (1) prepared subsequently drops in glue, add other leftover materials after being uniformly mixed 8h, continue stirring and make mixing of materials even, gained composite glue solution is for subsequent use;
(3) composite glue solution prepared by step (2) coated and sheet glass puts into convection oven carry out imidization process, treatment condition are: treatment temp 150 DEG C, in the treatment time: 1.5h, obtain described laminated film.
The performance index of the laminated film obtained by the present embodiment are as follows:
Tensile strength is: 115MPa; Elongation at break: 12%; Breaking down field strength: 172KV/mm; Under room temperature condition 100Hz frequency, specific inductivity is: 70; Dielectric loss≤0.12% under equal conditions.
Claims (2)
1. an electrical condenser polyimide high dielectric composite film for blending nano titanium carbide loading multi-wall carbon nanotubes, it is characterized in that, this laminated film is prepared by the raw material of following weight part: pyromellitic acid anhydride 10-12,4,4
,-diamino-diphenyl ether 8-10, NVP 3-5, nano titanium carbide 2-3, nanometer aluminium powder 0.01-0.02, N,N-dimethylacetamide 20-25, dehydrated alcohol 3-5, silane coupling agent 0.1-0.2, hydroxyethyl methylacrylate 0.4-0.5, multi-walled carbon nano-tubes 0.4-0.5, polyvinyl alcohol 0.1-0.2, water 4-5.
2. the preparation method of the polyimide high dielectric composite film of a kind of electrical condenser blending nano titanium carbide loading multi-wall carbon nanotubes as claimed in claim 1, it is characterized in that, described preparation method is:
(1) preparation of surface-modified nano titanium carbide loading multi-wall carbon nanotubes solution: first multi-walled carbon nano-tubes is dried to neutral through acid treatment after washing, again polyvinyl alcohol dissolution is mixed with solution in water, by the dry multi-walled carbon nano-tubes after acid treatment above, nano titanium carbide, nano aluminum drops in solution, after ultrasonic disperse 20-30min, mixed slurry is heated to 60-80 DEG C, constant temperature milled processed 30-40min, subsequently gained slurry is dried, remove moisture completely, gained powder and silane coupling agent mixing and stirring, obtain surface-modified nano titanium carbide loading multi-wall carbon nanotubes composite granule, finally gained composite granule is dropped in dehydrated alcohol, after ultrasonic disperse 20-30min, gained material is for subsequent use,
(2) by 4,4
,-diamino-diphenyl ether drops into N, in N-N,N-DIMETHYLACETAMIDE, after stirring, divide 5 steps to add the pyromellitic acid anhydride of equivalent, react 10-12h after interpolation, obtain polyamic acid glue, composite granule ethanol solution step (1) prepared subsequently drops in glue, add other leftover materials after being uniformly mixed 8-10h, continue stirring and make mixing of materials even, gained composite glue solution is for subsequent use;
(3) composite glue solution prepared by step (2) coated and sheet glass puts into convection oven carry out imidization process, treatment condition are: treatment temp 150-200 DEG C, the treatment time: 1.5-2h, obtain described laminated film.
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Cited By (5)
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| CN108912837A (en) * | 2018-08-13 | 2018-11-30 | 深圳市墨库图文技术有限公司 | A kind of new-type carbon black dispersion liquid and preparation method thereof, application |
| CN109103292A (en) * | 2018-07-31 | 2018-12-28 | 深圳众厉电力科技有限公司 | A kind of efficient photovoltaic component system |
| CN109167066A (en) * | 2018-09-03 | 2019-01-08 | 济南大学 | A kind of preparation method of few layer titanium carbide growth in situ nitrogen-doped carbon nanometer pipe three-dimensional composite material |
| US10767084B2 (en) | 2015-12-13 | 2020-09-08 | International Business Machines Corporation | Enhanced adhesive materials and processes for 3D applications |
| CN114410110A (en) * | 2022-01-26 | 2022-04-29 | 四川轻化工大学 | Preparation method of carbonized polyimide resin powder and composite film thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US10767084B2 (en) | 2015-12-13 | 2020-09-08 | International Business Machines Corporation | Enhanced adhesive materials and processes for 3D applications |
| US11168234B2 (en) | 2015-12-13 | 2021-11-09 | International Business Machines Corporation | Enhanced adhesive materials and processes for 3D applications |
| CN109103292A (en) * | 2018-07-31 | 2018-12-28 | 深圳众厉电力科技有限公司 | A kind of efficient photovoltaic component system |
| CN108912837A (en) * | 2018-08-13 | 2018-11-30 | 深圳市墨库图文技术有限公司 | A kind of new-type carbon black dispersion liquid and preparation method thereof, application |
| CN109167066A (en) * | 2018-09-03 | 2019-01-08 | 济南大学 | A kind of preparation method of few layer titanium carbide growth in situ nitrogen-doped carbon nanometer pipe three-dimensional composite material |
| CN114410110A (en) * | 2022-01-26 | 2022-04-29 | 四川轻化工大学 | Preparation method of carbonized polyimide resin powder and composite film thereof |
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Application publication date: 20151125 |