CN105038228A - Polyimide high-dielectric composite film mixed with nano-boron carbide-loaded graphene and used for capacitor and preparation method thereof - Google Patents

Polyimide high-dielectric composite film mixed with nano-boron carbide-loaded graphene and used for capacitor and preparation method thereof Download PDF

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Publication number
CN105038228A
CN105038228A CN201510478674.7A CN201510478674A CN105038228A CN 105038228 A CN105038228 A CN 105038228A CN 201510478674 A CN201510478674 A CN 201510478674A CN 105038228 A CN105038228 A CN 105038228A
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graphene
boron carbide
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composite
preparation
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唐彬
唐发根
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Tongling Sheng Da Electronics Technology Co Ltd
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Tongling Sheng Da Electronics Technology Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K9/00—Use of pretreated ingredients
    • C08K9/12—Adsorbed ingredients, e.g. ingredients on carriers
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
    • C08G73/06—Polycondensates having nitrogen-containing heterocyclic rings in the main chain of the macromolecule
    • C08G73/10—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
    • C08G73/1003—Preparatory processes
    • C08G73/1007—Preparatory processes from tetracarboxylic acids or derivatives and diamines
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
    • C08J5/18—Manufacture of films or sheets
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/02—Elements
    • C08K3/04—Carbon
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/38—Boron-containing compounds
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K9/00—Use of pretreated ingredients
    • C08K9/04—Ingredients treated with organic substances
    • C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K9/00—Use of pretreated ingredients
    • C08K9/10—Encapsulated ingredients
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2379/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen with or without oxygen, or carbon only, not provided for in groups C08J2361/00 - C08J2377/00
    • C08J2379/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
    • C08J2379/08—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00—Specific properties of additives
    • C08K2201/011—Nanostructured additives
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2203/00—Applications
    • C08L2203/16—Applications used for films
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2203/00—Applications
    • C08L2203/20—Applications use in electrical or conductive gadgets

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  • Polymers & Plastics (AREA)
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  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
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Abstract

The invention discloses a polyimide high-dielectric composite film mixed with nano-boron carbide-loaded graphene and used for a capacitor. Packing such as nano-boron carbide and graphene is mixed in the polyimide film preparation process and graphene is loaded in the pre-treated nano-boron carbide so as to improve the dispersity and utilization rate of the graphene; coating processing is performed on powder by utilizing a polyvinyl alcohol film having good stability in an organic solvent; and composite powder having undergone silane coupling agent surface modification treatment and organic glue solution are good in interfacial compatibility and are liable to be scattered evenly. The compound packing can improve dielectric properties of the material stably and efficiently and have a high dielectric constant and a low dielectric loss. Compared with a pure polyimide film, the finally prepared composite film material is greatly improved in dielectric properties, still maintains good mechanical properties and processing performance and is good in application prospect.

Description

Polyimide high dielectric composite film of a kind of electrical condenser blending nano boron carbide load Graphene and preparation method thereof
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 boron carbide load Graphene 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 boron carbide load Graphene 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 boron carbide load Graphene, 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, N,N-dimethylacetamide 20-25, nano boron carbide 2-3, Graphene 0.01-0.02, dehydrated alcohol 3-5, silane coupling agent 0.1-0.2, hydroxyethyl methylacrylate 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 boron carbide load Graphene, described preparation method is:
(1) preparation of surface-modified nano norbide load graphene solution: first nano boron carbide is dried to neutral through acid treatment after washing, again polyvinyl alcohol dissolution is mixed with solution in water, by the drying nano norbide after acid treatment above, Graphene 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 norbide load graphene composite powder, 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 200-250 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 boron carbide in Kapton preparation process, the fillers such as Graphene, and by graphene-supported on nano boron carbide after pretreatment, to improve its dispersed and utilization ratio, the polyvinyl alcohol film that recycling has good stability in organic solvent carries out coated process to powder, and 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 raising material of this compounded mix energy stability and high efficiency, have high specific inductivity and low dielectric loss concurrently, the more simple Kapton of the composite film material finally prepared obtains and greatly improves in dielectric properties, and still keep excellent mechanical property and processing characteristics, application prospect is good.
Embodiment
Embodiment:
A polyimide high dielectric composite film for electrical condenser blending nano boron carbide load Graphene, 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, N,N-dimethylacetamide 20, nano boron carbide 2, Graphene 0.01, dehydrated alcohol 3, silane coupling agent 0.1, hydroxyethyl methylacrylate 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 boron carbide load Graphene, described preparation method is:
(1) preparation of surface-modified nano norbide load graphene solution: first nano boron carbide is dried to neutral through acid treatment after washing, again polyvinyl alcohol dissolution is mixed with solution in water, by the drying nano norbide after acid treatment above, Graphene 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 norbide load graphene composite powder, 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 200 DEG C, in the treatment time: 2h, obtain described laminated film.
The performance index of the laminated film obtained by the present embodiment are as follows:
Tensile strength is: 121MPa; Elongation at break: 16%; Breaking down field strength: 155KV/mm; Under room temperature condition 100Hz frequency, specific inductivity is: 58; Dielectric loss≤0.12% under equal conditions.

Claims (2)

1. an electrical condenser polyimide high dielectric composite film for blending nano boron carbide load Graphene, 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, N,N-dimethylacetamide 20-25, nano boron carbide 2-3, Graphene 0.01-0.02, dehydrated alcohol 3-5, silane coupling agent 0.1-0.2, hydroxyethyl methylacrylate 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 boron carbide load Graphene as claimed in claim 1, it is characterized in that, described preparation method is:
(1) preparation of surface-modified nano norbide load graphene solution: first nano boron carbide is dried to neutral through acid treatment after washing, again polyvinyl alcohol dissolution is mixed with solution in water, by the drying nano norbide after acid treatment above, Graphene 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 norbide load graphene composite powder, 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 200-250 DEG C, the treatment time: 1.5-2h, obtain described laminated film.
CN201510478674.7A 2015-08-03 2015-08-03 Polyimide high-dielectric composite film mixed with nano-boron carbide-loaded graphene and used for capacitor and preparation method thereof Pending CN105038228A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109545415A (en) * 2018-11-12 2019-03-29 东莞理工学院 A kind of radiation protection material
CN111944331A (en) * 2020-08-04 2020-11-17 上海核工程研究设计院有限公司 Surface modification treatment method of anti-settling boron carbide powder
CN112358693A (en) * 2020-11-13 2021-02-12 湖南华菱线缆股份有限公司 Interface modified chlorinated polyethylene rubber based on novel reinforcing agent and preparation method thereof

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104211962A (en) * 2014-09-10 2014-12-17 北京化工大学常州先进材料研究院 High dielectric polyimide composite material and preparation method thereof

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104211962A (en) * 2014-09-10 2014-12-17 北京化工大学常州先进材料研究院 High dielectric polyimide composite material and preparation method thereof

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
屈凌波主编: "《新型功能材料设计及应用》", 31 May 2014, 郑州：郑州大学出版社 *
朱洪法、朱玉霞: "《工业助剂手册》", 30 June 2007, 金盾出版社 *

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109545415A (en) * 2018-11-12 2019-03-29 东莞理工学院 A kind of radiation protection material
CN111944331A (en) * 2020-08-04 2020-11-17 上海核工程研究设计院有限公司 Surface modification treatment method of anti-settling boron carbide powder
CN112358693A (en) * 2020-11-13 2021-02-12 湖南华菱线缆股份有限公司 Interface modified chlorinated polyethylene rubber based on novel reinforcing agent and preparation method thereof

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