CN108589025A - A kind of preparation method of graphene-carbon composite nano-fiber - Google Patents
A kind of preparation method of graphene-carbon composite nano-fiber Download PDFInfo
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Abstract
The invention discloses a kind of preparation methods of graphene carbon composite nano fiber comprising：Crystalline flake graphite and acid are sequentially added into container, after stirring evenly, is slowly added to potassium permanganate thereto, are opened stirring and are reacted；Deionized water and hydrogen peroxide is added into reaction gained mixture, continues to stir；By centrifuging, drying and obtaining graphite oxide；Then the graphite oxide is added to N, in N dimethylformamides, ultrasonic disperse；Polyacrylonitrile is added during magnetic agitation so that PAN is uniformly dissolved in DMF, obtains spinning solution；Spinning solution is transferred to relevant device and carries out spinning；The placement of obtained film is pre-oxidized in air, is then carbonized in nitrogen to get graphene carbon composite nano fiber.The high-specific surface area of graphene, the excellent electric conductivity of excellent conductivity and CNFs and continuity can be combined the common capacitive property for improving electrode material by the present invention.
Description
Technical field
The present invention relates to carbon fibre composite preparing technical fields, and in particular to a kind of graphene-carbon composite nano is fine
The preparation method of dimension.
Background technology
In recent years in various nano-carbon materials, graphene and continuous carbon nano-fiber (CNFs) are as super
Capacitor electrode material is paid close attention to by sustainable growth.Wherein the self-contained very more good characteristic of graphene is for example excellent leads
Electrically, outstanding mechanical performance and superhigh specific surface area etc., however since there are powerful key is mutual between graphene sheet layer
Effect, in prepared grapheme material it is inevasible there is the graphene sheet layer stacked so that its specific surface area not
It is high.It is numerous to be reported as the phenomenon that solution graphene sheet layer stacks, it is compound using graphene and porous material progress, however due to
The discrete nature that graphene and graphite nano plate itself have makes its loose arrangement in the porous material, and contact resistance is caused to increase
Greatly so that super capacitor energy and power density reduce.In summary, it is desirable to have a kind of emerging technology can solve
The conductivity of graphene film interlayer is kept while stating situation and superhigh specific surface area can be obtained.
Electrostatic spinning technique is preparing continuous one-dimensional polymer, polymer derived carbon, metal, metal oxide and ceramics
The effective ways of equal nano wires and it is at low cost, controllability is strong.In addition it is inexpensive, straight can to provide number of ways preparation for electrostatic spinning
Diameter and the adjustable porous nano line of component are simultaneously scalable to industrial production for ultracapacitor and rechargeable battery.Its
In by the continuous CNFs that is prepared after electrostatic spinning polymer carbonization there is fabulous electric conductivity, thermal stability and to charge and
The high connectivity of heat.The research report for preparing graphene-carbon composite nano-fiber using method of electrostatic spinning in the prior art is seldom,
And wherein there is also the specific surface areas of the CNFs of preparation to lead to the technical problems such as low, conductivity is low, which limits it in super electricity
Performance in container.
Invention content
The purpose of the present invention is to provide a kind of preparation methods of graphene-carbon composite nano-fiber, utilize Static Spinning
Silk method, which combines graphene and CNFs, prepares graphene-charcoal composite nano fiber, passes through Optimizing Technical and technique
Parameter can combine the high-specific surface area of graphene, the excellent electric conductivity of excellent conductivity and CNFs and continuity
The common capacitive property for improving electrode material.
Its technical solution includes：
A kind of preparation method of graphene-carbon composite nano-fiber, includes the following steps successively：
A prepares graphite oxide,
Crystalline flake graphite and acid are sequentially added into container, after stirring evenly, are slowly added to potassium permanganate thereto, unlatching is stirred
It mixes and is reacted；
Deionized water and hydrogen peroxide is added into reaction gained mixture, continues to stir；
By centrifuging, drying and obtaining graphite oxide；
B prepares graphene-carbon composite nano-fiber by method of electrostatic spinning,
Graphite oxide obtained by step a is added in n,N-Dimethylformamide, ultrasound is to being completely dispersed；
Polyacrylonitrile is added during magnetic agitation, stirring makes PAN uniformly be dissolved in DMF, obtains spinning solution；
The spinning solution is transferred in plastics needle tubing, is mounted on electrostatic spinning machine, using aluminium foil as receiving screen,
Under 25KV high voltages, spinning is carried out with the speed of 1ml/h；
The placement of obtained film is pre-oxidized in air, is then carbonized in nitrogen to get graphene-carbon
Composite nano fiber；
In step a, the acid is the concentrated sulfuric acid and phosphoric acid, and the two volume ratio is 9:1；The crystalline flake graphite with it is described
The concentrated sulfuric acid bulking value proportioning be 1:The quality proportioning of 120g/mL, the crystalline flake graphite and potassium permanganate is 1:6.
As a preferred solution of the present invention, it is first 50 DEG C of water-baths in temperature after potassium permanganate is added in step a
In reacted, after reacting 12h, be placed in ice-water bath and deionized water and hydrogen peroxide be added.
As another preferred embodiment of the present invention, the volume proportion of above-mentioned deionized water and hydrogen peroxide is 40:3.
Further, it in step a, between centrifugation and drying steps, is carried out successively with deionized water, hydrochloric acid and absolute ethyl alcohol
Cleaning.
Further, in step b, above-mentioned graphite oxide and the bulking value of above-mentioned n,N-Dimethylformamide match
It is 0.005:The quality proportioning of 1g/mL, above-mentioned graphite oxide and above-mentioned polyacrylonitrile is 1:16, after polyacrylonitrile is added,
Stirring 4h in 45 DEG C makes PAN uniformly be dissolved in DMF.
Further, in step b, obtained film is placed into 280 DEG C of pre-oxidation 60min in air, then in nitrogen
It is middle to carry out 800 DEG C of carbonization 1h.
Advantageous effects caused by the present invention are：
(1) that the present invention uses is simple for process, operation is simple, be readily synthesized, is suitable for producing in enormous quantities, thus has
Important application value.
(2) excellent electric conductivity and continuity of the invention by the high-specific surface area of graphene, excellent conductivity and CNFs
Combine, is 1A g in current density-1Under the conditions of its specific capacitance be 670F g-1。
The specific advantageous effect of the present invention can further be embodied by following embodiments 2.
Description of the drawings
The present invention will be further described for explanation below in conjunction with the accompanying drawings：
(a) is the SEM pictures of HCG in Fig. 1, is (b) the SEM pictures of ICG；
Fig. 2 is the infrared spectrum of HCG and ICG.
Specific implementation mode
The present invention proposes a kind of preparation method of graphene-carbon composite nano-fiber, in order to make advantages of the present invention, skill
Art scheme is clearer, clear, elaborates to the present invention with reference to specific embodiment.
Raw material needed for the present invention can be bought by commercial channel and be obtained.
Embodiment 1：
(1) preparation of graphite oxide
Hummers methods prepare graphite oxide：250ml reaction bulbs are equipped in ice-water bath, by 2g crystalline flake graphites and 1g nitre
Sour sodium is placed in a reaction flask, and the 46ml concentrated sulfuric acids are added and continue stirring until uniform mixing；It is slowly added to 6g potassium permanganate by several times, in temperature
Degree reacts 2h in the case of being no more than 20 DEG C, transfers in 35 DEG C of waters bath with thermostatic control and reacts 30min；Reaction bulb is taken from water-bath
Go out, 70 DEG C of deionized waters of 92ml are added dropwise, it is highly exothermic so that solution rises to 98 DEG C and keeps 15min；Directly into solution
70 DEG C of deionized waters of 280ml are poured into, the hydrogen peroxide of 20ml 30% is added, neutralizes unreacted potassium permanganate；It centrifuges while hot
Filtering, and be washed with deionized repeatedly, 50 DEG C of vacuum drying obtain graphite oxide (GO).
(2) preparation of graphene-charcoal composite nano fiber：
The GO of 0.05g Hummers methods preparation is respectively adopted, is added in the n,N-Dimethylformamide (DMF) of 10ml,
Ultrasound is to being completely dispersed；Then 0.8g polyacrylonitrile (PAN), 45 DEG C of stirring 4h so that PAN are added during magnetic agitation
Uniformly it is dissolved in DMF.Above-mentioned solution is transferred in plastics needle tubing, is mounted on electrostatic spinning machine, using aluminium foil as receiving screen,
The distance between syringe needle and receiving screen are maintained at 15cm, and under 25KV high voltages, spinning is carried out with the speed of 1ml/h；It will obtain
Film place in air carry out 280 DEG C pre-oxidation 60min, then in nitrogen carry out 800 DEG C carbonization 1h, obtained graphite
Alkene-charcoal composite nano fiber is named as HCG, and (H represents what the GO being added was prepared as Hummers methods, and C represents carbon material, and G represents stone
Black alkene).
(3) structure of graphene-charcoal composite nano fiber and capacitance characteristic characterization：
Fig. 1 is the SEM figures of HCG, as can clearly see from the figure carbon fiber surface rule.Fig. 2 is the FT-IR figures of HCG,
In wave number 3407cm-1The broad peak at place belongs to the stretching vibration of O-H keys (deriving from hydroxyl)；In 1457,2851,2925 and of wave number
2962cm-1Place, they correspond to methylene functional group (- (CH2)n) bending vibration, symmetrical and asymmetrical stretching vibration；
Peak at wave number 1620cm-1 belongs to stretching vibration and the graphene bone of the C=C double bonds in unoxidized graphite-like region
Frame vibrates；Wave number 1275cm-1Be attributed to the fact that the bending vibration of C-OH keys in the peak at place；Peak at wave number 1092 and 1052cm-1
Be attributed to the fact that the stretching vibration of C-O keys (from epoxy-ester and and epoxy group).
It is 730m to adsorb measuring and calculation to obtain the accumulation micropore specific area of HCG by CO22g-1.It is 1A in current density
g-1Under the conditions of, the specific capacitance of HCG is 520F g-1。
Embodiment 2：
(1) preparation of graphite oxide
Improved Hummers methods prepare graphite oxide.It is equipped with the beaker of 1000ml first, sequentially adds 3g scale stones
Ink, the 360ml concentrated sulfuric acids and 40ml phosphoric acid after stirring evenly, are slowly added to 18g potassium permanganate (being steeply risen to avoid temperature),
Beaker is put into 50 DEG C of water-baths, 12h is stirred；Then beaker is put into ice-water bath, 400ml is slowly added into mixture goes
The hydrogen peroxide of ionized water and 30ml 30% continues to stir；Centrifugation obtains product while hot, uses 200ml deionized waters, 200ml respectively
30% hydrochloric acid and the cleaning of 200ml sewage ethyl alcohol, freeze-drying obtain graphite oxide (GO).
(2) preparation of graphene-charcoal composite nano fiber：
GO prepared by the improved Hummers methods of 0.05g is respectively adopted, is added to the n,N-Dimethylformamide of 10ml
(DMF) in, ultrasound is to being completely dispersed；Then 0.8g polyacrylonitrile (PAN), 45 DEG C of stirrings are added during magnetic agitation
4h so that PAN is uniformly dissolved in DMF.Above-mentioned solution is transferred in plastics needle tubing, is mounted on electrostatic spinning machine, with aluminium foil
As receiving screen, the distance between syringe needle and receiving screen are maintained at 15cm, under 25KV high voltages, are carried out with the speed of 1ml/h
Spinning；Obtained film is placed and carries out 280 DEG C of pre-oxidation 60min in air, 800 DEG C of carbonizations are then carried out in nitrogen
1h, obtained graphene-charcoal composite nano fiber is named as ICG, and (I represents what the GO being added was prepared to improve rear method, and C is represented
Carbon material, G represent graphene).
(3) structure of graphene-charcoal composite nano fiber and capacitance characteristic characterization：
Fig. 1 is the SEM figures of ICG, and carbon fiber surface is fairly regular as can clearly see from the figure.Fig. 2 is the FT- of ICG
IR schemes, in wave number 3407cm-1The broad peak at place belongs to the stretching vibration of O-H keys (deriving from hydroxyl)；Wave number 1457,2851,
2925 and 2962cm-1Place, they correspond to methylene functional group (- (CH2)n) bending vibration, symmetrical and asymmetrical flexible
Vibration；In wave number 1620cm-1The peak at place belongs to stretching vibration and the graphite of the C=C double bonds in unoxidized graphite-like region
Alkene skeletal vibration；Be attributed to the fact that the bending vibration of C-OH keys in peak at wave number 1275cm-1.
Pass through CO2The accumulation micropore specific area that absorption measuring and calculation obtains HCG is 860m2g-1.It is 1A in current density
g-1Under the conditions of, the specific capacitance of HCG is 670F g-1。
It should be noted that any equivalent way that those skilled in the art are made under the introduction of this specification, or
Obvious variant should all be within the scope of the present invention.
Claims (6)
1. a kind of preparation method of graphene-carbon composite nano-fiber, which is characterized in that include the following steps successively：
A prepares graphite oxide,
Sequentially add crystalline flake graphite and acid into container, after stirring evenly, be slowly added to potassium permanganate thereto, unlatching stir into
Row reaction；
Deionized water and hydrogen peroxide is added into reaction gained mixture, continues to stir；
By centrifuging, drying and obtaining graphite oxide；
B prepares graphene-carbon composite nano-fiber by method of electrostatic spinning,
Graphite oxide obtained by step a is added in n,N-Dimethylformamide, ultrasound is to being completely dispersed；
Polyacrylonitrile is added during magnetic agitation, stirring makes PAN uniformly be dissolved in DMF, obtains spinning solution；
The spinning solution is transferred in plastics needle tubing, is mounted on electrostatic spinning machine, using aluminium foil as receiving screen,
Under 25KV high voltages, spinning is carried out with the speed of 1ml/h；
The placement of obtained film is pre-oxidized in air, is then carbonized in nitrogen compound to get graphene-carbon
Nanofiber；
In step a, the acid is the concentrated sulfuric acid and phosphoric acid, and the two volume ratio is 9:1；The crystalline flake graphite with it is described dense
The bulking value proportioning of sulfuric acid is 1:The quality proportioning of 120g/mL, the crystalline flake graphite and potassium permanganate is 1:6.
2. a kind of preparation method of graphene-carbon composite nano-fiber according to claim 1, it is characterised in that：Step a
In, it after potassium permanganate is added, is reacted in temperature is 50 DEG C of water-baths first, after reacting 12h, is placed in be added in ice-water bath and go
Ionized water and hydrogen peroxide.
3. a kind of preparation method of graphene-carbon composite nano-fiber according to claim 2, it is characterised in that：It is described
Deionized water and hydrogen peroxide volume proportion be 40:3.
4. a kind of preparation method of graphene-carbon composite nano-fiber according to claim 1, it is characterised in that：Step a
In, between centrifugation and drying steps, cleaned successively with deionized water, hydrochloric acid and absolute ethyl alcohol.
5. a kind of preparation method of graphene-carbon composite nano-fiber according to claim 1, it is characterised in that：Step b
In, the graphite oxide and the bulking value proportioning of the n,N-Dimethylformamide are 0.005:1g/mL, the oxygen
Graphite and the quality proportioning of the polyacrylonitrile are 1:16, after polyacrylonitrile is added, stirs 4h in 45 DEG C and so that PAN is uniform
It is dissolved in DMF.
6. a kind of preparation method of graphene-carbon composite nano-fiber according to claim 1, it is characterised in that：Step b
In, obtained film is placed into 280 DEG C of pre-oxidation 60min in air, 800 DEG C of carbonization 1h are then carried out in nitrogen.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109322040A (en) * | 2018-11-07 | 2019-02-12 | 湖州通益环保纤维股份有限公司 | A kind of graphene radiation resistant fiber fabric |
| 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 |
| CN109914037A (en) * | 2019-03-29 | 2019-06-21 | 中原工学院 | A kind of preparation method of non-woven nano-graphene/polyacrylonitrile non-woven fabrics |
| 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 |
| CN117568968A (en) * | 2024-01-15 | 2024-02-20 | 苏州扬越高新材料有限公司 | Production process of polyester fine denier yarn |
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| CN102658108A (en) * | 2012-05-04 | 2012-09-12 | 东南大学 | Method for preparing photocatalytic filtering membrane based on graphene/semiconductor by an electrospinning method |
| CN103741259A (en) * | 2014-01-16 | 2014-04-23 | 齐齐哈尔大学 | Fluorene-triphenylamine copolymer/graphene composite nano-fiber material with shell-core structure |
| CN104947227A (en) * | 2015-07-13 | 2015-09-30 | 黑龙江大学 | Polyvinylpyrrolidone/graphene composite nanofiber material and preparation method thereof |
| CN106521719A (en) * | 2016-11-10 | 2017-03-22 | 过冬 | Graphene-based carbon nanofiber preparation method |
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| CN102658108A (en) * | 2012-05-04 | 2012-09-12 | 东南大学 | Method for preparing photocatalytic filtering membrane based on graphene/semiconductor by an electrospinning method |
| CN103741259A (en) * | 2014-01-16 | 2014-04-23 | 齐齐哈尔大学 | Fluorene-triphenylamine copolymer/graphene composite nano-fiber material with shell-core structure |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109322040A (en) * | 2018-11-07 | 2019-02-12 | 湖州通益环保纤维股份有限公司 | A kind of graphene radiation resistant fiber fabric |
| 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 |
| CN109914037A (en) * | 2019-03-29 | 2019-06-21 | 中原工学院 | A kind of preparation method of non-woven nano-graphene/polyacrylonitrile non-woven fabrics |
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| CN117568968A (en) * | 2024-01-15 | 2024-02-20 | 苏州扬越高新材料有限公司 | Production process of polyester fine denier yarn |
| CN117568968B (en) * | 2024-01-15 | 2024-03-22 | 苏州扬越高新材料有限公司 | Production process of polyester fine denier yarn |
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Application publication date: 20180928 |