CN105803602B - The method that the graphene film twisting method of forming prepares graphene fiber - Google Patents
The method that the graphene film twisting method of forming prepares graphene fiber Download PDFInfo
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- CN105803602B CN105803602B CN201510000105.1A CN201510000105A CN105803602B CN 105803602 B CN105803602 B CN 105803602B CN 201510000105 A CN201510000105 A CN 201510000105A CN 105803602 B CN105803602 B CN 105803602B
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Abstract
The invention discloses the method that a kind of graphene film twisting method of forming prepares graphene fiber, and copper foil load graphene film coiled material is prepared in copper foil surface with the method for chemical vapour deposition technique or heating in vacuum copper foil；Copper foil load graphene film coiled material is imported in the water that temperature is 60 90 DEG C, graphene film separates with copper foil, obtains graphene film；Copper foil winding recovery, the aggregated twister twisting of graphene film are output to coiling and molding device into graphene fiber, are directly prepared into the graphene fiber bobbin with the twist.This method operating process is easy, the preparation of graphene fiber is directly realized by using existing Weaving device, cost is low, can a large amount of continuous productions；Graphene fiber produced by the present invention has the close twist, Coating combination, appearance and consistent internal structure, mechanical performance is outstanding, flexible, flexible, can graphene oxide film cutting before coating nanometer functional material, obtain the composite graphite alkene fiber of nano functional.
Description
Technical field
The invention belongs to grapheme material preparing technical field, and in particular to a kind of graphene film twisting method of forming prepares stone
The method of black alkene fiber, methods described are dry spinning method.
Background technology
Most basic construction unit of the graphene as all carbon materials, there is real monoatomic layer thickness and strict two
Structure is tieed up, there is very high mechanical strength, elasticity, thermal conductivity, electron mobility（100,000cm2· V-1·s-1）And amount
Sub- Hall effect etc..Obtained since British scientist An Delie Jim in 2010 and Ke Siteyanuowosainuo have found graphene
Since obtaining the Nobel Prize, graphene research reaches unprecedented research climax, and increasing research finds that graphene can use
In field-effect transistor, high-frequency element, super microprocessor and single-molecule detection device etc..And it is made up of graphene for elementary cell
Three-dimensional structure material, such as film and bulk material, can be applied to controllable Breathable filmses, anisotropy ion-conducting material, super
The field of functional materials such as capacitor, lithium ion battery and energy catalysis.
Consider from practical application angle, nano-graphene material is changed into macrostructure material undoubtedly very valuable
The research direction of value.A main bugbear in graphene research and application is effective assembling of graphene macrostructure, at present
Relatively successfully assembling is to obtain the film and bulk of three-dimensional structure.In the graphene side that assembling macrostructure is one-dimentional structure
Face；Although graphene fiber has been prepared at present, because the solubility of graphene in itself is low and sticky difference, institute
To be difficult to prepare high strength graphite alkene fiber.
At present, domestic and international researcher has prepared graphene fiber by different methods respectively.Zhejiang University is high
Superfine people and Chinese University of Science and Technology's Yu's book are grand et al. the different precipitating reagents of selection have obtained graphite by wet spinning-reduction two-step method
Alkene fiber.Beijing Institute of Technology Qu Liangti et al. in glass tube high temperature hydro-thermal reaction by having obtained graphene fiber.Qu Liang
The document report of body etc., the document, which discloses, is injected into graphene oxide solution in the internal capillary equipped with copper wire, enters water-filling
The fiber of thermal synthesis graphene/copper wire, removes to obtain hollow graphene micro-nano mitron after cooling by copper wire, prepared by this method
Graphene micro-nano mitron have certain suppleness, but be unable to continuous production, can only obtain graphene micro-nano mitron, it is impossible to
Obtain graphene oxide doughnut, and this method subsequent treatment and except miscellaneous operation is time-consuming very long, have much room for improvement or develop
New method.
In recent years, patent CN201180020978.9 was used for the technique for spinning graphene ribbon fiber, disclosed CNT
The method for expanding into graphene ribbon；201410016557.4、CN 201210001537.0（By large-size graphene oxide sheet system
The method of standby high-strength conductive graphene fiber）、CN201210001524.3（A kind of high-strength graphene ordered porous fibers and
Its preparation method）、CN201210017773.1（A kind of preparation method of graphene fiber）、CN201210001 536.6（It is a kind of
Ion-enhanced graphene fiber and preparation method thereof）、CN201110441254.3（A kind of high strength macro graphene conductive fiber
Preparation method）Etc. disclosing different wet laid fiber preparation methods；CN201310064 816.6（Graphene/TiO2 fibers
Preparation method）Disclose wet method and prepare the technique for mixing titanium oxide；CN2011 10098809.9（Electrospinning-hydro-thermal method prepares graphite
The method of alkene/ceramic nano crystalline substance particulate composite）The method for disclosing wet electrostatic spinning； CN200580000581.8（Tool
There is the fine carbon fiber of various structures）Disclose the performance of axially vertical fine carbon fiber；Therefore one kind can be efficiently using existing
Have, be ripe, Traditional Industrialization equipment, easy one-step method and low temperature, the method for leniently preparing graphene fiber need out
Hair, so as to more preferable large-scale application.
The content of the invention
The technical problems to be solved by the invention are to prepare graphene fiber using wet method in the prior art to overcome
Preparation method the defects of needing to dry power consumption big, complex process, there is provided a kind of method of dry process graphene fiber.This
The preparation method of invention is simple to operate, mild condition, and the cost of raw material is low；The stone being prepared using method of the present invention
Black alkene fiber, even structure, mechanical performance is excellent, easy functionalization.
In order to solve the above technical problems, the present invention uses following technical scheme：A kind of rubbing method prepares graphene fiber
Method, step are as follows：
A kind of method that graphene film twisting method of forming prepares graphene fiber, step are as follows：
（1）With the method for chemical vapour deposition technique or heating in vacuum copper foil copper foil surface prepare copper foil load graphene it is thin
Film coiled material；
（2）Copper foil load graphene film coiled material is imported in the water that temperature is 60-90 DEG C, due to driving for temperature, copper
Power between the graphene and copper foil of paper tinsel surface appendix is insufficient to allow graphene to be retained in copper foil surface, and graphene film is sent out with copper foil
It is estranged from obtaining graphene film；
（3）Copper foil winding recovery, the aggregated twister of graphene film are twisted into graphene fiber or silk or yarn or line,
Coiling and molding device is output to simultaneously, is directly prepared into graphene fiber/silk/yarn with the twist/spool of certain package capacity.
The step（1）The middle method with heating in vacuum copper foil prepares copper foil load graphene film coiled material in copper foil surface
Technique be：Using copper foil as catalyst, heatable catalyst makes carbon source vapor in catalyst surface under conditions of 1020-1069 DEG C
Being formed needs the graphene film of thickness.
The step（3）Middle aggregation twister uses ring ingot method, looping method, air-flow spinning or jet spinning, is preferably
Jet spinning.Through twisting, Free water is squeezed out into fiber, the binding strength of synchronous increase graphene sheet layer is twisted, solves it
Other party method prepares graphene fiber intensity and improves the problem of little.
To step（2）In graphene film top layer apply plus nano functional particulate, nano functional solution/emulsion, nanometer material
Material precursor emulsion/solution, the graphene oxide and graphene fiber of functionalization is prepared.
Beneficial effects of the present invention：1. the invention provides a kind of dry-forming method of graphene oxide fiber, the party
Method operating process is easy, and the preparation of graphene fiber is directly realized by using existing Weaving device, through rational design and matching phase
The ripe accessory answered, graphene fiber can be directly obtained with pure graphene composite thin film, it is not necessary to subsequent treatment
And removal of impurities；Graphene fiber can be largely obtained, in the range of equipment license, it is possible to quick to prepare up to several myriametres length
Graphene fiber, and specific package is formed, it is easy to the industrial applications of next step；2. the construction material graphene oxide utilized
Wide material sources, cost is low, can a large amount of continuous productions；3. graphene fiber produced by the present invention has the twist, graphene sheet layer
Between be tightly combined, graphene fiber appearance and consistent internal structure, mechanical performance is outstanding, flexible, flexible；4. the present invention carries
Supplied the graphene film twisting method of forming method for preparing graphene fiber, can before graphene oxide film cutting coating nanometer work(
Energy material, obtains the composite graphite alkene fiber of the in-situ modification containing equally distributed nano functional.
Figure of description
Fig. 1 is that graphene film of the present invention twists the process chart that the method for forming prepares graphene fiber.
Embodiment
To be best understood from the present invention, the present invention is described in further detail with reference to specific embodiment.
Embodiment 1
Copper foil load graphene film coiled material 1 is prepared in the copper foil surface of 50 centimetres of breadth through CVD, by the copper foil coiled material
Import in the pond 5 that temperature is 90 DEG C, graphene film will separate with copper foil, be wound back with 0.1 m/min of speed
Copper foil 2 is received, the aggregated twisting of graphene film fills 3 twisting and twists with the fingers/10 centimetres into the twist for 1000, the graphene fiber that 70 μm of diameter
4, twist the binding strength of synchronous increase graphene sheet layer, solve other method prepare graphene fiber intensity improve it is little
Problem, while coiling and molding device is output to, it is directly prepared into the graphene fiber bobbin with the twist of certain package capacity.
Embodiment 2
Copper foil is heated using CVD device prepare copper foil in the copper foil surface of 100 centimetres of breadth to 1060 degree of method load
Graphene film coiled material, the copper foil coiled material being imported in the water that temperature is 80 DEG C, graphene film will separate with copper foil, with
0.01 m/min of speed winding recovery copper foil, graphene film are into the twist through RING SPINNING aggregation twister twisting
2000 twist with the fingers/10 centimetres, the silk that 120 μm of diameter.The binding strength of the synchronous increase graphene sheet layer of twisting, solves other method system
Standby graphene fiber intensity improves the problem of little；Coiling and molding device is output to simultaneously, is directly prepared into certain package capacity
Graphene fiber bobbin with the twist.
Embodiment 3
Through heating in vacuum copper foil to 1060 degree of method copper foil load graphene is prepared in the copper foil surface of 120 centimetres of breadth
Film coil, the copper foil coiled material is imported in the water that temperature is 90 DEG C, graphene film will separate with copper foil, with 0.01
M/min speed winding recovery copper foil, graphene film through Air-Jet Spinning aggregation twister twisting into the twist be 2000 twist with the fingers/
10 centimetres, the silk that 150 μm of diameter, three silks are simultaneously twisted 210 μm of line.The combination jail of the synchronous increase graphene sheet layer of twisting
Degree, it is little to solve the problems, such as that other method prepares the raising of graphene fiber intensity；Coiling and molding device is output to simultaneously, directly
The graphene fiber bobbin with the twist of certain package capacity is made.
Embodiment 4
The method that the graphene film twisting method of forming of the present embodiment prepares graphene fiber, step are as follows：
（1）Using copper foil as catalyst, heatable catalyst copper foil makes carbon source vapor in catalyst copper under conditions of 1020 DEG C
Paper tinsel surface forms the graphene film for needing thickness, and copper foil load graphene film coiled material is prepared in copper foil surface；
（2）Copper foil load graphene film coiled material is imported in the water that temperature is 60 DEG C, due to driving for temperature, copper foil table
Power between the graphene and copper foil of face appendix is insufficient to allow graphene to be retained in copper foil surface, and graphene film occurs to divide with copper foil
From obtaining graphene film；
（3）To step（2）In graphene film top layer apply plus nano functional particulate, copper foil winding recovery, graphene is thin
Film is twisted into graphene fiber through ring ingot method, while is output to coiling and molding device, and the band for being directly prepared into certain package capacity is twisted with the fingers
The graphene fiber bobbin of degree.
Embodiment 5
The method that the graphene film twisting method of forming of the present embodiment prepares graphene fiber, step are as follows：
（1）With the method for chemical vapour deposition technique or heating in vacuum copper foil using copper foil as catalyst, in 1069 DEG C of condition
Lower heatable catalyst makes carbon source vapor form the graphene film for needing thickness in catalyst surface, and copper foil is prepared in copper foil surface
Load graphene film coiled material；
（2）Copper foil load graphene film coiled material is imported in the water that temperature is 90 DEG C, due to driving for temperature, copper foil table
Power between the graphene and copper foil of face appendix is insufficient to allow graphene to be retained in copper foil surface, and graphene film occurs to divide with copper foil
From obtaining graphene film；
（3）Copper foil winding recovery, graphene film are twisted into graphene fiber or long filament, or yarn or line through air-flow spinning,
Coiling and molding device is output to simultaneously, is directly prepared into the graphene fiber with the twist/silk bobbin of certain package capacity.
Embodiment 6
The method that the graphene film twisting method of forming of the present embodiment prepares graphene fiber, step are as follows：
（1）With the method for chemical vapour deposition technique or heating in vacuum copper foil using copper foil as catalyst, in 1050 DEG C of condition
Lower heatable catalyst makes carbon source vapor form the graphene film for needing thickness in catalyst surface, and copper foil is prepared in copper foil surface
Load graphene film coiled material；
（2）Copper foil load graphene film coiled material is imported in the water that temperature is 80 DEG C, due to driving for temperature, copper foil table
Power between the graphene and copper foil of face appendix is insufficient to allow graphene to be retained in copper foil surface, and graphene film occurs to divide with copper foil
From obtaining graphene film；
（3）Copper foil winding recovery, graphene film are twisted into graphene fiber or silk or yarn or line through jet spinning, simultaneously
Coiling and molding device is output to, is directly prepared into graphene fiber/silk/yarn with the twist/spool of certain package capacity.
Claims (4)
1. a kind of method that graphene film twisting method of forming prepares graphene fiber, it is characterised in that step is as follows：
（1）Copper foil load graphene film is prepared with the method for chemical vapour deposition technique or heating in vacuum copper foil in copper foil surface to roll up
Material；
（2）Copper foil load graphene film coiled material is imported in the water that temperature is 60-90 DEG C, graphene film occurs to divide with copper foil
From obtaining graphene film；
（3）Copper foil winding recovery, the aggregated twister twisting of graphene film are output to and are wound into graphene fiber
Type device, it is directly prepared into the graphene fiber bobbin with the twist.
2. the method that the graphene film twisting method of forming according to claim 1 prepares graphene fiber, it is characterised in that：
The step（1）The technique that the middle method with heating in vacuum copper foil prepares copper foil load graphene film coiled material in copper foil surface
For：Using copper foil as catalyst, heatable catalyst, which makes carbon source vapor be formed in catalyst surface, under conditions of 1020-1069 DEG C needs
Want the graphene film of thickness.
3. the method that the graphene film twisting method of forming according to claim 1 prepares graphene fiber, it is characterised in that：
The step（3）Middle aggregation twister uses ring ingot method, looping method, air-flow spinning or jet spinning.
4. the graphene film twisting method of forming according to any one in claim 1~3 prepares the side of graphene fiber
Method, it is characterised in that：To step（2）In graphene film top layer apply plus nano functional particulate, nano functional solution/emulsion,
Nano material presoma emulsion/solution, the graphene oxide and graphene fiber of functionalization is prepared.
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| CN107034552B (en) * | 2016-12-05 | 2019-04-02 | 信阳师范学院 | Graphene fiber and preparation method thereof |
| CN107151835B (en) * | 2017-05-19 | 2019-07-23 | 杭州高烯科技有限公司 | A kind of Flexible graphene fiber and its continuous preparation method |
| CN108035140B (en) * | 2017-11-22 | 2020-12-11 | 东莞市光钛科技有限公司 | Production process of graphene-based composite fiber fabric |
| CN108327359A (en) * | 2018-01-30 | 2018-07-27 | 四川省安德盖姆石墨烯科技有限公司 | A kind of graphene sleeping bag |
| CN108903560A (en) * | 2018-06-27 | 2018-11-30 | 四川省安德盖姆石墨烯科技有限公司 | A kind of preparation method of graphene far infrared heating carpet |
| CN108910870B (en) * | 2018-07-20 | 2020-10-27 | 西安交通大学 | Composite film with graphene oxide and graphene composite structure obtained by CVD graphene pollution-free transfer process and method |
| CN111439746B (en) * | 2020-05-20 | 2021-07-23 | 东华大学 | Preparation method of single-layer graphene folding structure with controllable torsion angle |
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| CN103086370A (en) * | 2013-01-22 | 2013-05-08 | 东北大学 | Method for preparing graphene strip by adopting low-temperature chemical vapour deposition |
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| EP0967423A2 (en) * | 1998-06-27 | 1999-12-29 | Sgl Technik Gmbh | Packing yarn of graphite and plastic sheet |
| CN103086370A (en) * | 2013-01-22 | 2013-05-08 | 东北大学 | Method for preparing graphene strip by adopting low-temperature chemical vapour deposition |
| CN103263860A (en) * | 2013-05-26 | 2013-08-28 | 北京工商大学 | Preparation method of polyvinyl fluoride separating membrane |
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