CN103500654A - Nitrogen-doped graphene/PVDF (Polyvinylidene Fluoride) composite dielectric film and preparation method thereof - Google Patents
Nitrogen-doped graphene/PVDF (Polyvinylidene Fluoride) composite dielectric film and preparation method thereof Download PDFInfo
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- CN103500654A CN103500654A CN201310481158.0A CN201310481158A CN103500654A CN 103500654 A CN103500654 A CN 103500654A CN 201310481158 A CN201310481158 A CN 201310481158A CN 103500654 A CN103500654 A CN 103500654A
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- nitrogen
- doped graphene
- dielectric film
- pvdf
- graphene
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 40
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 38
- 239000002033 PVDF binder Substances 0.000 title claims abstract description 20
- 239000002131 composite material Substances 0.000 title claims abstract description 12
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- 229920002981 polyvinylidene fluoride Polymers 0.000 claims abstract description 19
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000000034 method Methods 0.000 claims abstract description 8
- 238000005266 casting Methods 0.000 claims abstract description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 4
- 125000004433 nitrogen atom Chemical group N* 0.000 claims abstract description 4
- 150000001875 compounds Chemical class 0.000 claims description 18
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- 238000005516 engineering process Methods 0.000 claims description 6
- 239000011521 glass Substances 0.000 claims description 6
- 239000000758 substrate Substances 0.000 claims description 6
- 229920000877 Melamine resin Polymers 0.000 claims description 3
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 3
- 238000013019 agitation Methods 0.000 claims description 3
- 230000015572 biosynthetic process Effects 0.000 claims description 3
- 210000000988 bone and bone Anatomy 0.000 claims description 3
- 238000006243 chemical reaction Methods 0.000 claims description 3
- 239000007789 gas Substances 0.000 claims description 3
- 239000003292 glue Substances 0.000 claims description 3
- 229910002804 graphite Inorganic materials 0.000 claims description 3
- 239000010439 graphite Substances 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 238000009413 insulation Methods 0.000 claims description 3
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims description 3
- 239000012528 membrane Substances 0.000 claims description 3
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 3
- 230000001681 protective effect Effects 0.000 claims description 3
- 239000004065 semiconductor Substances 0.000 claims description 3
- 229910052709 silver Inorganic materials 0.000 claims description 3
- 239000004332 silver Substances 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- 239000000725 suspension Substances 0.000 claims description 3
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 2
- 229920000642 polymer Polymers 0.000 abstract description 4
- 239000002861 polymer material Substances 0.000 abstract description 3
- 239000004020 conductor Substances 0.000 abstract 2
- 230000001105 regulatory effect Effects 0.000 abstract 1
- 239000010408 film Substances 0.000 description 12
- 239000003989 dielectric material Substances 0.000 description 7
- 239000003990 capacitor Substances 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 239000013528 metallic particle Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229920013657 polymer matrix composite Polymers 0.000 description 1
- 239000011160 polymer matrix composite Substances 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
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- Carbon And Carbon Compounds (AREA)
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Abstract
The invention discloses a nitrogen-doped graphene/PVDF composite dielectric film and a preparation method thereof. The nitrogen-doped graphene/PVDF composite dielectric film (thereinafter referred to as composite dielectric film) is characterized in that nitrogen atoms are introduced into a graphene lattice, so that nitrogen-doped graphene is obtained, the nitrogen-doped graphene has a structure and properties different from grapheme, and the nitrogen-doped graphene/PVDF composite dielectric film can be transformed between a p-type conductor and an n-type conductor by regulating the doping amount of nitrogen, and is prepared by adopting the solution casting method. The invention has the advantages that because the nitrogen-doped graphene has high strength, high conductivity and large specific surface area, when the nitrogen-doped graphene is used for modifying polymer materials, high-performance polymer-based composite materials can be obtained, so the nitrogen-doped graphene/PVDF composite dielectric film has high conductivity, high strength, high heat stability and certain fire resistance.
Description
Technical field
The present invention relates to a kind of dielectric material, relate in particular to a kind of high dielectric material.
Background technology
Traditional dielectric material is generally ceramics polymer material and dielectric polymer based composites, and the ceramics polymer material dielectric constant is high, but machining property is poor, complex process, difficulty or ease are prepared into flexible material, the polymer matrix composite that the metallic particles of take is filler is the excellent performance high dielectric material of flexibility again, but, fast development along with modern science and technology and human society, polymer thin film capacitor is widely used in mobile electronic device, electric power system, hybrid vehicle, the pulse energy instrument, this capacitor deposited energy structure is to small size, high energy storage density, the high power density future development, dielectric material has been proposed to higher specification requirement, require the dielectric material high conductivity, high strength, high thermal stability also has certain anti-flammability, existing dielectric material just can not adapt to.
Summary of the invention
Purpose of the present invention is exactly in order to overcome above-mentioned weak point of the prior art, provides a kind of and has high conductivity, high strength, high thermal stability and have high performance compound dielectric film of certain anti-flammability and preparation method thereof.
The present invention solves the problems of the technologies described above adopted technical scheme: a kind of nitrogen-doped graphene/PVDF compound dielectric film and preparation method thereof, it is characterized in that: described nitrogen-doped graphene/PVDF compound dielectric film (hereinafter to be referred as compound dielectric film) is to introduce nitrogen-atoms in the Graphene lattice, obtain nitrogen-doped graphene, described nitrogen-doped graphene and Graphene have totally different structure and character, and the present invention realizes that by adjusting the nitrogen doping its conversion between p-type and N-shaped semiconductor realizes.
The present invention adopts solution casting method to be prepared, and the concrete technology flow process of sample is as follows:
(1) graphite oxide is mixed according to mass ratio 4:1 with melamine, join after mixing in the acetone soln of 100mL, stir 5h; Heating is boiled solution and is removed acetone, in drying box, after drying, sample is placed in to tube furnace, under N2 gas protective condition, is heated to 950 ℃, and insulation 0.5h, obtain nitrogen-doped graphene.
(2) the proper N doped graphene adds in quantitative ethanol, and ultrasonic dispersion 30min is to nitrogen-doped graphene formation stable homogeneous suspension;
(3) appropriate PVDF is added in above-mentioned mixed liquor, be heated to that 60 degree are following to be stirred, dissolve fully to PVDF;
(4) above-mentioned mixed liquor continuation is ultrasonic, and mechanical agitation 5min;
(5) above-mentioned mixed liquor is watered and casts from glass substrate, be placed in bone dry in baking oven, composite membrane is peeled from glass substrate, folding being placed in mould, be hot pressed into compound dielectric film;
(6) be coated with high-purity conductive silver glue as the electrode for test on described compound dielectric film.
The invention has the beneficial effects as follows: because nitrogen-doped graphene has high strength, high conductivity, high-specific surface area, with it, polymeric material is carried out to modification and can obtain the high performance polymer based composites, so nitrogen-doped graphene/PVDF compound dielectric film has high conductivity, high strength, high thermal stability and has certain anti-flammability.
Embodiment
Below with an embodiment, the invention will be further described:
A kind of nitrogen-doped graphene/PVDF compound dielectric film and preparation method thereof, described nitrogen-doped graphene/PVDF compound dielectric film is to introduce nitrogen-atoms in the Graphene lattice, obtain nitrogen-doped graphene, described nitrogen-doped graphene and Graphene have totally different structure and character, and the present invention realizes that by adjusting the nitrogen doping its conversion between p-type and N-shaped semiconductor realizes.
The present invention adopts solution casting method to be prepared, and the concrete technology flow process of sample is as follows:
(1) join in the acetone soln of 100mL after graphite oxide is mixed according to mass ratio 4:1 with melamine, stir 5h; Heating is boiled solution and is removed acetone, in drying box, after drying, sample is placed in to tube furnace, under N2 gas protective condition, is heated to 950 ℃, and insulation 0.5h, obtain nitrogen-doped graphene.
(2) the proper N doped graphene adds in quantitative ethanol, and ultrasonic dispersion 30min is to nitrogen-doped graphene formation stable homogeneous suspension;
(3) appropriate PVDF is added in above-mentioned mixed liquor, be heated to that 60 degree are following to be stirred, dissolve fully to PVDF;
(4) above-mentioned mixed liquor continuation is ultrasonic, and mechanical agitation 5min;
(5) above-mentioned mixed liquor is watered and casts from glass substrate, be placed in bone dry in baking oven, composite membrane is peeled from glass substrate, folding being placed in mould, be hot pressed into compound dielectric film;
(6) be coated with high-purity conductive silver glue as the electrode for test on described compound dielectric film.
Above-described embodiment, just an example of the present invention, be not for limiting enforcement of the present invention and interest field, all or technical schemes of being equal to identical with the described content of the claims in the present invention, all should be included in protection range of the present invention.
Claims (2)
1. nitrogen-doped graphene/PVDF compound dielectric film and preparation method thereof, it is characterized in that: described nitrogen-doped graphene/PVDF compound dielectric film (hereinafter to be referred as compound dielectric film) is to introduce nitrogen-atoms in the Graphene lattice, obtain nitrogen-doped graphene, described nitrogen-doped graphene and Graphene have totally different structure and character, and the present invention realizes that by adjusting the nitrogen doping its conversion between p-type and N-shaped semiconductor realizes.
2. a kind of nitrogen-doped graphene according to claim 1/PVDF compound dielectric film and preparation method thereof is characterized in that: the present invention adopts solution casting method to be prepared, and the concrete technology flow process of sample is as follows:
(1) graphite oxide is mixed according to mass ratio 4:1 with melamine, join after mixing in the acetone soln of 100mL, stir 5h; Heating is boiled solution and is removed acetone, in drying box, after drying, sample is placed in to tube furnace, under N2 gas protective condition, is heated to 950 ℃, and insulation 0.5h, obtain N-graphene;
(2) the proper N doped graphene adds in quantitative ethanol, and ultrasonic dispersion 30min is to nitrogen-doped graphene formation stable homogeneous suspension;
(3) appropriate PVDF is added in above-mentioned mixed liquor, be heated to that 60 degree are following to be stirred, dissolve fully to PVDF;
(4) above-mentioned mixed liquor continuation is ultrasonic, and mechanical agitation 5min;
(5) above-mentioned mixed liquor is watered and casts from glass substrate, be placed in bone dry in baking oven, composite membrane is peeled from glass substrate, folding being placed in mould, be hot pressed into compound dielectric film;
(6) be coated with high-purity conductive silver glue as the electrode for test on described compound dielectric film.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201310481158.0A CN103500654A (en) | 2013-10-11 | 2013-10-11 | Nitrogen-doped graphene/PVDF (Polyvinylidene Fluoride) composite dielectric film and preparation method thereof |
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| CN201310481158.0A Pending CN103500654A (en) | 2013-10-11 | 2013-10-11 | Nitrogen-doped graphene/PVDF (Polyvinylidene Fluoride) composite dielectric film and preparation method thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104860312A (en) * | 2015-05-27 | 2015-08-26 | 上海理工大学 | Preparation method for corrugated nitrogen-doped graphene |
| CN109390149A (en) * | 2017-08-11 | 2019-02-26 | 钰邦科技股份有限公司 | The production method of the making apparatus and thin film capacitor of multiple field stacked structure |
| CN109671577A (en) * | 2017-10-13 | 2019-04-23 | 钰邦科技股份有限公司 | The production method of the making apparatus and thin film capacitor of multiple field stacked structure |
| CN114621540A (en) * | 2022-03-16 | 2022-06-14 | 广州特种承压设备检测研究院 | Nitrided graphene/PVDF (polyvinylidene fluoride) nanocomposite and preparation method and application thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102120572A (en) * | 2011-01-24 | 2011-07-13 | 南京大学 | Method for preparing nitrogen-doped graphene |
| CN102964754A (en) * | 2012-11-29 | 2013-03-13 | 哈尔滨师范大学 | High-dielectric-constant polyvinylidene fluoride composite material and preparation method thereof |
| KR101274991B1 (en) * | 2011-09-28 | 2013-07-30 | 재단법인 포항산업과학연구원 | The method for manufacturing nitrogen doped graphene electrode for capacitor, electrode and electric double layer capacitor using the same |
-
2013
- 2013-10-11 CN CN201310481158.0A patent/CN103500654A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102120572A (en) * | 2011-01-24 | 2011-07-13 | 南京大学 | Method for preparing nitrogen-doped graphene |
| KR101274991B1 (en) * | 2011-09-28 | 2013-07-30 | 재단법인 포항산업과학연구원 | The method for manufacturing nitrogen doped graphene electrode for capacitor, electrode and electric double layer capacitor using the same |
| CN102964754A (en) * | 2012-11-29 | 2013-03-13 | 哈尔滨师范大学 | High-dielectric-constant polyvinylidene fluoride composite material and preparation method thereof |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104860312A (en) * | 2015-05-27 | 2015-08-26 | 上海理工大学 | Preparation method for corrugated nitrogen-doped graphene |
| CN109390149A (en) * | 2017-08-11 | 2019-02-26 | 钰邦科技股份有限公司 | The production method of the making apparatus and thin film capacitor of multiple field stacked structure |
| CN109390149B (en) * | 2017-08-11 | 2020-08-11 | 钰邦科技股份有限公司 | Manufacturing equipment of multilayer stacked structure and manufacturing method of thin film capacitor |
| CN109671577A (en) * | 2017-10-13 | 2019-04-23 | 钰邦科技股份有限公司 | The production method of the making apparatus and thin film capacitor of multiple field stacked structure |
| CN114621540A (en) * | 2022-03-16 | 2022-06-14 | 广州特种承压设备检测研究院 | Nitrided graphene/PVDF (polyvinylidene fluoride) nanocomposite and preparation method and application thereof |
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Effective date of registration: 20140528 Address after: 315010, room 23, Shuguang Road, Jiangdong District, Zhejiang, Ningbo 502, China Applicant after: Zhang Xiaobin Applicant after: Ningbo Yicheng Electronic Technology Co., Ltd. Applicant after: ZHEJIANG DONGCHI SWITCH CO., LTD. Address before: 315040, room 23, Shuguang Road, Jiangdong District, Zhejiang, Ningbo 502, China Applicant before: Zhang Xiaobin |
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Application publication date: 20140108 |