CN106521719A - Graphene-based carbon nanofiber preparation method - Google Patents
Graphene-based carbon nanofiber preparation method Download PDFInfo
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- CN106521719A CN106521719A CN201610989772.1A CN201610989772A CN106521719A CN 106521719 A CN106521719 A CN 106521719A CN 201610989772 A CN201610989772 A CN 201610989772A CN 106521719 A CN106521719 A CN 106521719A
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
- D01F9/12—Carbon filaments; Apparatus specially adapted for the manufacture thereof
- D01F9/14—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments
- D01F9/20—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products
- D01F9/21—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products from macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D01F9/22—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products from macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds from polyacrylonitriles
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
- D01F9/12—Carbon filaments; Apparatus specially adapted for the manufacture thereof
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
Abstract
The invention provides a graphene-based carbon nanofiber preparation method, characterized in that polyacrylonitrile is taken as a carbon source, oxidized graphene prepared by an improved method provided by the invention is added, then an electrospinning technique is used for preparing and obtaining oxidized graphene/polypropylene nanofiber, then pre-oxidation and carbonization steps are adopted to prepare and obtain graphene-based carbon nanofiber. The graphene-based carbon nano material prepared by the method provided by the invention is very easily dispersed, the overlapping of sheets is reduced, and the removal of a functional group at high temperature is facilitated, so that the conductivity and specific surface area of nanofiber are improved. Under the condition that the current density is 1A/g, the specific capacitance is 468F/g.
Description
Technical field
The present invention relates to new material technology field, more particularly to a kind of preparation method of graphene-based carbon nano-fiber.
Background technology
So far, due to highly stable physics and chemical property, very big specific surface area and controllable
The porous carbon of pore structure, various patterns and texture is considered as the wide variety of electrode material of ultracapacitor energy always, and
In business ultracapacitor, the capacitance of a unit may be up to 5000F.Additionally, nearest nano science and nanotechnology research
In progress, numerous researchers all concentrate the material with carbon element such as CNT (CNTs) of research nanostructured, carbon nano-fiber
(CNFs), the ideal electrode material of the ultracapacitor such as Graphene, and find that they have very high specific capacitance value.
In recent years in various nano-carbon materials, Graphene and continuous carbon nano-fiber (CNFs) are used as super
Capacitor electrode material is subject to what is continued to increase to pay close attention to.Wherein Graphene itself has very many good characteristics, as excellent
Electric conductivity, outstanding mechanical performance and superhigh specific surface area, the specific surface area of single-layer graphene film are up to 3100m2/g.But
As the key-key for having powerful between graphene sheet layer interacts, inevasible presence in prepared grapheme material
The graphene film of stacking, so that its specific surface area is reduced.In order to solve the phenomenon of graphene sheet layer stacking, using Graphene
It is combined with porous material, the discrete nature having yet with Graphene and graphite nano plate in itself makes which in porous material
In loose arrangement, cause contact resistance increase so that super capacitor energy and power density are reduced.In sum, wish
Hope that a kind of emerging technology can solve the problem that drawbacks described above, and while superhigh specific surface area being obtained, keep graphene film interlayer
Conductivity.
Electrostatic spinning technique is to prepare continuous one-dimensional polymer, polymer derived carbon, metal, metal-oxide and ceramics
Deng the effective ways of nano wire.Which has low cost, controllability strong a little.In addition electrostatic spinning can provide number of ways system
Standby low cost, directly and the adjustable porous nano line of component, and commercial production is scalable to for ultracapacitor and can
Storage battery.The continuous CNFs prepared after electrostatic spinning polymer carbonization there is fabulous electric conductivity, heat stability with
And to electric charge and the high connectivity of heat.According to the literature, several carbon nano-fibers (CNFs) conduct for being prepared by electrostatic spinning
Electrode material for super capacitor shows very high specific capacitance and excellent stability.
But relative to CNTs and Graphene, generally than relatively low, this just limits for the specific surface area of CNFs prepared by electrostatic spinning
Its application in ultracapacitor is made.
The content of the invention
It is an object of the invention to a kind of preparation method of graphene-based carbon nano-fiber is proposed, being capable of its specific surface area
Greatly, it is adaptable to the application in ultracapacitor.
It is that, up to this purpose, the present invention is employed the following technical solutions：
A kind of preparation method of graphene-based carbon nano-fiber, including：
(1) by the crystalline flake graphite of 2-5 weight portions, the phosphoric acid mixing of the concentrated sulphuric acid and 30-60 weight portions of 300-500 weight portions
Uniformly, the potassium permanganate of 15-20 weight portions is slowly added to, 9-18 hours is stirred at 45-55 DEG C；
(2) deionized water of 300-500 weight portions, and the 10- of 20-50 weight portions at 0-5 DEG C, are added in mixture
The hydrogen peroxide of 30wt% concentration, and stir 5-10 minutes；
(3) separate and priority deionized water, the hydrochloric acid of 10-30wt% concentration and absolute ethanol washing product, vacuum is done
It is dry to obtain graphene oxide；
(4) graphene oxide of 0.01-0.1 weight portions is added into the N,N-dimethylformamide of 5-20 weight portions
In, ultrasonic disperse is to being completely dispersed；
(5) while stirring, the polyacrylonitrile of 0.5-1.5 weight portions is added, 40-50 DEG C is heated to and is persistently stirred,
Until polyacrylonitrile is completely dissolved, mixed liquor is obtained；
(6) by the mixed liquor electrostatic spinning, using aluminium foil as receiving screen, obtain spinning thin film；
(7) pre-oxidize at 250-300 DEG C in the strong film-air, then in protective atmosphere at 750-850 DEG C
Carbonization 30-120 minutes, obtain the graphene-based carbon nano-fiber.
The present invention with polyacrylonitrile as carbon source, the graphene oxide for adding improved method of the invention to prepare, then
Graphene oxide/polyacrylic nanofiber is prepared by electrostatic spinning technique, then using pre-oxidation and carbonization
Prepare graphene-based carbon nano-fiber.
The product that the present invention is prepared is characterized using CO2 absorption, SEM, elementary analysiss and FT-IR, find to change
Graphene oxide hydrophilic after entering substantially preferably, is better than the graphene oxide that Hummers methods are prepared.The method of the present invention
The graphene-based carbon nanomaterial for preparing, easily disperses and reduces the stacking of lamella, is conducive to functional group in high temperature
Removing so that the electrical conductivity and specific surface area of nanofiber is improved.Under conditions of electric current density is 1A/g, which is than electricity
Hold and be at least 468F/g.
Specific embodiment
Technical scheme is further illustrated below by specific embodiment.
Embodiment 1
A kind of preparation method of graphene-based carbon nano-fiber, including：
(1) by the phosphoric acid mix homogeneously of the crystalline flake graphite of 2 weight portions, the concentrated sulphuric acid of 300 weight portions and 30 weight portions, slowly
The potassium permanganate of 15 weight portions is added, is stirred 9 hours at 45 DEG C；
(2) at 0 DEG C, add the deionized water of 300 weight portions in mixture, and the 30wt% concentration of 20 weight portions
Hydrogen peroxide, and stir 5 minutes；
(3) separate and priority deionized water, the hydrochloric acid of 10wt% concentration and absolute ethanol washing product, be vacuum dried
To graphene oxide；
(4) graphene oxide of 0.01 weight portion is added in the DMF of 5 weight portions, ultrasound point
It is dissipated to and is completely dispersed；
(5) while stirring, the polyacrylonitrile of 0.5 weight portion is added, 40 DEG C is heated to and is persistently stirred, until poly- third
Alkene nitrile is completely dissolved, and obtains mixed liquor；
(6) by the mixed liquor electrostatic spinning, using aluminium foil as receiving screen, obtain spinning thin film；
(7) pre-oxidize at 250 DEG C in the strong film-air, then in protective atmosphere at 750 DEG C 30 points of carbonization
Clock, obtains the graphene-based carbon nano-fiber.
Embodiment 2
A kind of preparation method of graphene-based carbon nano-fiber, including：
(1) by the phosphoric acid mix homogeneously of the crystalline flake graphite of 5 weight portions, the concentrated sulphuric acid of 500 weight portions and 60 weight portions, slowly
The potassium permanganate of 20 weight portions is added, is stirred 18 hours at 55 DEG C；
(2) at 5 DEG C, add the deionized water of 500 weight portions in mixture, and the 30wt% concentration of 50 weight portions
Hydrogen peroxide, and stir 10 minutes；
(3) separate and priority deionized water, the hydrochloric acid of 30wt% concentration and absolute ethanol washing product, be vacuum dried
To graphene oxide；
(4) graphene oxide of 0.1 weight portion is added in the DMF of 20 weight portions, ultrasound point
It is dissipated to and is completely dispersed；
(5) while stirring, the polyacrylonitrile of 1.5 weight portions is added, 50 DEG C is heated to and is persistently stirred, until poly- third
Alkene nitrile is completely dissolved, and obtains mixed liquor；
(6) by the mixed liquor electrostatic spinning, using aluminium foil as receiving screen, obtain spinning thin film；
(7) pre-oxidize at 300 DEG C in the strong film-air, then in protective atmosphere at 850 DEG C 120 points of carbonization
Clock, obtains the graphene-based carbon nano-fiber.
Embodiment 3
A kind of preparation method of graphene-based carbon nano-fiber, including：
(1) by the phosphoric acid mix homogeneously of the crystalline flake graphite of 3 weight portions, the concentrated sulphuric acid of 400 weight portions and 40 weight portions, slowly
The potassium permanganate of 16 weight portions is added, is stirred 12 hours at 50 DEG C；
(2) at 2 DEG C, add the deionized water of 400 weight portions in mixture, and the 10wt% concentration of 30 weight portions
Hydrogen peroxide, and stir 6 minutes；
(3) separate and priority deionized water, the hydrochloric acid of 20wt% concentration and absolute ethanol washing product, be vacuum dried
To graphene oxide；
(4) graphene oxide of 0.05 weight portion is added in the DMF of 10 weight portions, ultrasound
It is dispersed to and is completely dispersed；
(5) while stirring, the polyacrylonitrile of 1.0 weight portions is added, 45 DEG C is heated to and is persistently stirred, until poly- third
Alkene nitrile is completely dissolved, and obtains mixed liquor；
(6) by the mixed liquor electrostatic spinning, using aluminium foil as receiving screen, obtain spinning thin film；
(7) pre-oxidize at 280 DEG C in the strong film-air, then in protective atmosphere at 800 DEG C 60 points of carbonization
Clock, obtains the graphene-based carbon nano-fiber.
The product that the present invention is prepared is characterized using CO2 absorption, SEM, elementary analysiss and FT-IR, find this
Graphene oxide hydrophilic after inventive embodiments 1-3 are improved is substantially preferable, is better than the graphite oxide that Hummers methods are prepared
Alkene.The graphene-based carbon nanomaterial that the method for the present invention is prepared, easily disperses and reduces the stacking of lamella, be conducive to
Removing of the functional group in high temperature so that the electrical conductivity and specific surface area of nanofiber is improved.It is 1A/g in electric current density
Under conditions of, its specific capacitance is at least 468F/g.
Claims (1)
1. a kind of preparation method of graphene-based carbon nano-fiber, including：
(1) by the crystalline flake graphite of 2-5 weight portions, the phosphoric acid mixing of the concentrated sulphuric acid and 30-60 weight portions of 300-500 weight portions is equal
It is even, the potassium permanganate of 15-20 weight portions is slowly added to, 9-18 hours are stirred at 45-55 DEG C；
(2) deionized water of 300-500 weight portions, and the 10- of 20-50 weight portions at 0-5 DEG C, are added in mixture
The hydrogen peroxide of 30wt% concentration, and stir 5-10 minutes；
(3) separate and priority deionized water, the hydrochloric acid of 10-30wt% concentration and absolute ethanol washing product, be vacuum dried
To graphene oxide；
(4) graphene oxide of 0.01-0.1 weight portions is added in the DMF of 5-20 weight portions, is surpassed
Sound is dispersed to and is completely dispersed；
(5) while stirring, the polyacrylonitrile of 0.5-1.5 weight portions is added, 40-50 DEG C is heated to and is persistently stirred, until
Polyacrylonitrile is completely dissolved, and obtains mixed liquor；
(6) by the mixed liquor electrostatic spinning, using aluminium foil as receiving screen, obtain spinning thin film；
(7) pre-oxidize at 250-300 DEG C in the strong film-air, the then carbonization at 750-850 DEG C in protective atmosphere
30-120 minutes, obtain the graphene-based carbon nano-fiber.
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107021549A (en) * | 2017-04-06 | 2017-08-08 | 上海电力学院 | The preparation method of graphene/carbon nano-tube/carbon nanofiber membrane tri compound structure capacitance desalination electrode |
| CN108315834A (en) * | 2018-01-26 | 2018-07-24 | 渤海大学 | A kind of preparation method of array magnetizing reduction graphene oxide-carbon nanofibers |
| CN108589025A (en) * | 2018-04-23 | 2018-09-28 | 中国石油大学(华东) | A kind of preparation method of graphene-carbon composite nano-fiber |
| CN108998892A (en) * | 2017-06-07 | 2018-12-14 | 南京理工大学 | A kind of preparation method of chitosan-graphene oxide/polyacrylonitrile double-layer nanometer tunica fibrosa |
| CN109440231A (en) * | 2018-11-14 | 2019-03-08 | 中国地质大学（北京） | A kind of graphene/carbon composite micro-nano rice fiber and preparation method thereof |
| CN109989127A (en) * | 2017-12-31 | 2019-07-09 | 福建恒安集团有限公司 | A kind of hot-wind nonwoven cloth material |
| CN110284263A (en) * | 2019-06-13 | 2019-09-27 | 上海交通大学 | The preparation method of lamination composite nano fiber |
| CN110760946A (en) * | 2019-11-07 | 2020-02-07 | 黑龙江黑大生物质新材料科技有限公司 | Graphene-based composite fiber, and preparation method and application thereof |
| CN111013540A (en) * | 2019-12-30 | 2020-04-17 | 西北工业大学 | Preparation method of graphene magnetic aerogel with high adsorption performance |
| RU2765294C1 (en) * | 2018-07-17 | 2022-01-28 | Графенано Медикал Кеа, С.Л. | Graphene product and its therapeutic applications |
| CN114792779A (en) * | 2021-11-19 | 2022-07-26 | 广东一纳科技有限公司 | Flexible battery pole piece and battery |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107021549A (en) * | 2017-04-06 | 2017-08-08 | 上海电力学院 | The preparation method of graphene/carbon nano-tube/carbon nanofiber membrane tri compound structure capacitance desalination electrode |
| CN108998892A (en) * | 2017-06-07 | 2018-12-14 | 南京理工大学 | A kind of preparation method of chitosan-graphene oxide/polyacrylonitrile double-layer nanometer tunica fibrosa |
| CN109989127A (en) * | 2017-12-31 | 2019-07-09 | 福建恒安集团有限公司 | A kind of hot-wind nonwoven cloth material |
| CN108315834A (en) * | 2018-01-26 | 2018-07-24 | 渤海大学 | A kind of preparation method of array magnetizing reduction graphene oxide-carbon nanofibers |
| CN108315834B (en) * | 2018-01-26 | 2020-04-10 | 渤海大学 | Preparation method of array type magnetic reduced graphene oxide-carbon nanofiber |
| CN108589025A (en) * | 2018-04-23 | 2018-09-28 | 中国石油大学(华东) | A kind of preparation method of graphene-carbon composite nano-fiber |
| RU2765294C1 (en) * | 2018-07-17 | 2022-01-28 | Графенано Медикал Кеа, С.Л. | Graphene product and its therapeutic applications |
| CN109440231A (en) * | 2018-11-14 | 2019-03-08 | 中国地质大学（北京） | A kind of graphene/carbon composite micro-nano rice fiber and preparation method thereof |
| CN110284263A (en) * | 2019-06-13 | 2019-09-27 | 上海交通大学 | The preparation method of lamination composite nano fiber |
| CN110760946A (en) * | 2019-11-07 | 2020-02-07 | 黑龙江黑大生物质新材料科技有限公司 | Graphene-based composite fiber, and preparation method and application thereof |
| CN111013540A (en) * | 2019-12-30 | 2020-04-17 | 西北工业大学 | Preparation method of graphene magnetic aerogel with high adsorption performance |
| CN114792779A (en) * | 2021-11-19 | 2022-07-26 | 广东一纳科技有限公司 | Flexible battery pole piece and battery |
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