CN105803602A - Method for preparing graphene fiber through graphene film twisting forming method - Google Patents
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Abstract
The invention discloses a method for preparing a graphene fiber through a graphene film twisting forming method. The method comprises the steps that a copper foil-loaded graphene film roll material is prepared on the surface of copper foil through a chemical vapor deposition method or a copper foil vacuum heating method; the copper foil-loaded graphene film roll material is guided into 60-90-DEG C water, a graphene film is separated from the copper foil, and the graphene film is obtained; the copper foil is rolled up to be recycled, the graphene film is twisted into the graphene fiber through a gathering and twisting device and simultaneously output to a winding forming device to be directly made into a graphene fiber bobbin with the twist. According to the method, the operation process is simple and convenient, preparation of the graphene fiber is directly achieved through existing textile equipment, the cost is low, and massive and continuous production can be achieved; the graphene fiber prepared through the method has the twist and are close in combination among layers, uniform in appearance and internal structure, excellent in mechanical performance, good in flexibility and capable of being bent, and the oxidized graphene film can be coated with a nanometer functional material before being slit to obtain a composite graphene fiber with a nanometer function.
Description
Technical field
The invention belongs to grapheme material preparing technical field, be specifically related to the method that a kind of graphene film twisting method of forming prepares graphene fiber, described method is dry spinning method.
Background technology
Graphene is as the most basic construction unit of all material with carbon elements, there is real monoatomic layer thickness and strict two-dimensional structure, there is significantly high mechanical strength, elasticity, heat conductivity, electron mobility (100,000cm2 V-1 s-1) and quantum hall effect etc..Since British scientist An Delie Jim in 2010 and Ke Siteyanuowosainuo find that Graphene obtains Nobel Prize, Graphene research reaches unprecedented research climax, more and more studying discovery, Graphene can be used for field-effect transistor, high-frequency element, super microprocessor and single-molecule detection device etc..And be the three dimensional structure material that elementary cell is constituted by Graphene, such as thin film and bulk material, can be applicable to the field of functional materials such as controlled Breathable films, anisotropy ion-conducting material, ultracapacitor, lithium ion battery and energy catalysis.
Consider from practical application angle, nano-graphene material is changed in macrostructure material and is undoubtedly very valuable research direction.A main bugbear in Graphene research and application is effective assembling of Graphene macrostructure, and relatively successfully assembling at present is the thin film and the bulk that obtain three dimensional structure.In assembling the Graphene that macrostructure is one-dimentional structure；Graphene fiber is prepared although existing at present, but, owing to the dissolubility of Graphene itself is low and viscosity is poor, so being difficult to preparation high strength graphite alkene fiber.
At present, domestic and international researcher has prepared graphene fiber respectively through diverse ways.Zhejiang University is superb et al. and Chinese University of Science and Technology's Yu's book is grand et al. selects different precipitant to obtain graphene fiber by wet spinning-reduction two-step method.Beijing Institute of Technology Qu Liangti et al. obtains graphene fiber by high-temperature water thermal response in glass tubing.The bibliographical information of Qu Liangti etc., the open inside that graphene oxide solution is injected into of the document is equipped with in the capillary tube of copper wire, carry out the fiber of Hydrothermal Synthesis Graphene/copper wire, after cooling, copper wire is removed the Graphene micro-nano mitron obtaining hollow, Graphene micro-nano mitron prepared by the method has certain suppleness, but can not continuous prodution, can only obtain Graphene micro-nano mitron, graphene oxide doughnut can not be obtained, and the method subsequent treatment and remove impurity operation are all consuming time very long, have much room for improvement or develop new method.
In recent years, patent CN201180020978.9, for spinning the technique of graphene ribbon fiber, disclosed the method that CNT expands into graphene ribbon；201410016557.4, the method that CN201210001537.0(is prepared high-strength conductive graphene fiber by large-size graphene oxide sheet), CN201210001524.3(high-strength graphene ordered porous fibers and preparation method thereof), the preparation method of a CN201210017773.1(graphene fiber), CN201210001536.6(ion-enhanced graphene fiber and preparation method thereof), the preparation method of a CN201110441254.3(high strength macro graphene conductive fiber) etc. disclose different wet laid fiber preparation methoies；The preparation method of CN201310064816.6(Graphene/TiO2 fiber) disclose the technique that wet-layer preparation mixes titanium oxide；The method of CN201110098809.9(preparing grapheme/ceramic nanocrystalline particle composite material with electrospinning-hydrothemal method) method that discloses wet electrostatic spinning；CN200580000581.8(has the fine carbon fiber of various structures) disclose the performance of axially vertical fine carbon fiber；Therefore one can efficiently utilize existing, ripe, Traditional Industrialization equipment, and easy one-step method and low temperature, the method leniently preparing graphene fiber have to be developed, in order to better large-scale application.
Summary of the invention
The technical problem to be solved is in that to overcome the preparation method adopting wet-layer preparation graphene fiber in prior art to need drying to consume energy greatly, the defect of complex process, it is provided that a kind of method of dry process graphene fiber.The preparation method of the present invention is simple to operate, mild condition, and the cost of raw material is low；Utilizing the graphene fiber that method of the present invention prepares, even structure, mechanical performance is excellent, easy functionalization.
For solving above-mentioned technical problem, the present invention by the following technical solutions: a kind of rubbing method prepares the method for graphene fiber, and step is as follows:
The method that a kind of graphene film twisting method of forming prepares graphene fiber, step is as follows:
(1) Copper Foil load graphene film coiled material is prepared by the method for chemical vapour deposition technique or heating in vacuum Copper Foil at copper foil surface；
(2) Copper Foil load graphene film coiled material is imported in the water that temperature is 60-90 DEG C, due to ordering about of temperature, power between the Graphene of copper foil surface appendix and Copper Foil is not enough so that Graphene is retained in copper foil surface, and graphene film separates with Copper Foil, obtains graphene film；
(3) Copper Foil rolling is reclaimed, and the aggregated twister of graphene film adds and is twisted graphene fiber or silk or yarn or line, is simultaneously outputting to coiling and molding device, is directly prepared into the graphene fiber/silk/yarn with the twist/spool of certain package capacity.
The technique preparing Copper Foil load graphene film coiled material by the method for heating in vacuum Copper Foil at copper foil surface in described step (1) is: with Copper Foil for catalyst, and when 1020-1069 DEG C, heatable catalyst makes carbon source vapor form the graphene film needing thickness at catalyst surface.
Described step (3) is assembled twister and adopts ring ingot method, looping method, air-flow spinning or jet spinning, it is preferred to jet spinning.Through twisting, Free water squeezing out fiber, twisting synchronizes to increase the binding strength of graphene sheet layer, solves additive method and prepares the problem that the raising of graphene fiber intensity is little.
It is coated with plus nano functional particulate, nano functional solution/emulsion, nano material presoma emulsion/solution to the graphene film top layer in step (2), prepares graphene oxide and the graphene fiber of functionalization.
Beneficial effects of the present invention: 1. the invention provides the dry-forming method of a kind of graphene oxide fiber, the method operating process is easy, existing Weaving device is utilized to be directly realized by the preparation of graphene fiber, through the corresponding ripe accessory of reasonably design and coupling, graphene fiber can be directly obtained, it is not necessary to subsequent treatment and remove impurity with pure graphene composite thin film；Graphene fiber can be obtained in a large number, in the scope of equipment license, it is possible to quickly prepare the graphene fiber up to a few myriametre length, and form specific package, it is simple to next step industrial applications；2. the construction material graphene oxide wide material sources utilized, cost is low, it is possible to a large amount of productions continuously；3. the graphene fiber that the present invention prepares has the twist, and graphene film interlayer is tightly combined, graphene fiber appearance and consistent internal structure, and mechanical performance is outstanding, flexible, flexible；4. the invention provides the graphene film twisting method of forming method of preparing graphene fiber, can before graphene oxide film is cut coating nanometer functional material, obtain the composite graphite alkene fiber of in-situ modification containing equally distributed nano functional.
Figure of description
Fig. 1 is the process chart that the graphene film of the present invention twisting method of forming prepares graphene fiber.
Detailed description of the invention
For being best understood from the present invention, below in conjunction with specific embodiment, the present invention is described in further detail.
Embodiment 1
Copper Foil load graphene film coiled material 1 is prepared at the copper foil surface of fabric width 50 centimetres through CVD, this Copper Foil coiled material is imported in the pond 5 that temperature is 90 DEG C, graphene film will separate with Copper Foil, Copper Foil 2 is reclaimed with the speed rolling of 0.1 m/min, the aggregated twisting of graphene film fills 3 and adds that to be twisted the twist be 1000 sth. made by twisting/10 centimetre, the graphene fiber 4 that diameter is 70 μm, twisting synchronizes to increase the binding strength of graphene sheet layer, solve additive method and prepare the problem that the raising of graphene fiber intensity is little, it is simultaneously outputting to coiling and molding device, it is directly prepared into the graphene fiber bobbin with the twist of certain package capacity.
Embodiment 2
The method utilizing CVD device heating Copper Foil to 1060 degree prepares Copper Foil load graphene film coiled material at the copper foil surface of fabric width 100 centimetres, this Copper Foil coiled material is imported in the water that temperature is 80 DEG C, graphene film will separate with Copper Foil, Copper Foil is reclaimed with the speed rolling of 0.01 m/min, graphene film is assembled twister through RING SPINNING and is added that to be twisted the twist be 2000 sth. made by twisting/10 centimetre, the silk that diameter is 120 μm.Twisting synchronizes to increase the binding strength of graphene sheet layer, solves additive method and prepares the problem that the raising of graphene fiber intensity is little；It is simultaneously outputting to coiling and molding device, is directly prepared into the graphene fiber bobbin with the twist of certain package capacity.
Embodiment 3
Copper Foil load graphene film coiled material is prepared at the copper foil surface of fabric width 120 centimetres through the method for heating in vacuum Copper Foil to 1060 degree, this Copper Foil coiled material is imported in the water that temperature is 90 DEG C, graphene film will separate with Copper Foil, Copper Foil is reclaimed with the speed rolling of 0.01 m/min, graphene film is assembled twister through Air-Jet Spinning and is added that to be twisted the twist be 2000 sth. made by twisting/10 centimetre, diameter 150 μm silk, three rhizoids are also twisted the line of 210 μm.Twisting synchronizes to increase the binding strength of graphene sheet layer, solves additive method and prepares the problem that the raising of graphene fiber intensity is little；It is simultaneously outputting to coiling and molding device, is directly prepared into the graphene fiber bobbin with the twist of certain package capacity.
Embodiment 4
The method that the graphene film twisting method of forming of the present embodiment prepares graphene fiber, step is as follows:
(1) with Copper Foil for catalyst, when 1020 DEG C, heatable catalyst Copper Foil makes carbon source vapor form the graphene film needing thickness at catalyst copper foil surface, prepares Copper Foil load graphene film coiled material at copper foil surface；
(2) Copper Foil load graphene film coiled material is imported in the water that temperature is 60 DEG C, due to ordering about of temperature, power between the Graphene of copper foil surface appendix and Copper Foil is not enough so that Graphene is retained in copper foil surface, and graphene film separates with Copper Foil, obtains graphene film；
(3) it is coated with plus nano functional particulate to the graphene film top layer in step (2), Copper Foil rolling is reclaimed, graphene film adds through ring ingot method and is twisted graphene fiber, is simultaneously outputting to coiling and molding device, is directly prepared into the graphene fiber bobbin with the twist of certain package capacity.
Embodiment 5
The method that the graphene film twisting method of forming of the present embodiment prepares graphene fiber, step is as follows:
(1) by the method for chemical vapour deposition technique or heating in vacuum Copper Foil with Copper Foil for catalyst, when 1069 DEG C, heatable catalyst makes carbon source vapor form the graphene film needing thickness at catalyst surface, prepares Copper Foil load graphene film coiled material at copper foil surface；
(2) Copper Foil load graphene film coiled material is imported in the water that temperature is 90 DEG C, due to ordering about of temperature, power between the Graphene of copper foil surface appendix and Copper Foil is not enough so that Graphene is retained in copper foil surface, and graphene film separates with Copper Foil, obtains graphene film；
(3) Copper Foil rolling is reclaimed, and graphene film twists into graphene fiber or long filament through air-flow spinning, or yarn or line, is simultaneously outputting to coiling and molding device, 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 is as follows:
(1) by the method for chemical vapour deposition technique or heating in vacuum Copper Foil with Copper Foil for catalyst, when 1050 DEG C, heatable catalyst makes carbon source vapor form the graphene film needing thickness at catalyst surface, prepares Copper Foil load graphene film coiled material at copper foil surface；
(2) Copper Foil load graphene film coiled material is imported in the water that temperature is 80 DEG C, due to ordering about of temperature, power between the Graphene of copper foil surface appendix and Copper Foil is not enough so that Graphene is retained in copper foil surface, and graphene film separates with Copper Foil, obtains graphene film；
(3) Copper Foil rolling is reclaimed, and graphene film twists into graphene fiber or silk or yarn or line through jet spinning, is simultaneously outputting to coiling and molding device, is directly prepared into the graphene fiber/silk/yarn with the twist/spool of certain package capacity.
Claims (4)
1. the method that a graphene film twisting method of forming prepares graphene fiber, it is characterised in that step is as follows:
(1) Copper Foil load graphene film coiled material is prepared by the method for chemical vapour deposition technique or heating in vacuum Copper Foil at copper foil surface；
(2) being imported in the water that temperature is 60-90 DEG C by Copper Foil load graphene film coiled material, graphene film separates with Copper Foil, obtains graphene film；
(3) Copper Foil rolling is reclaimed, and the aggregated twister of graphene film adds and is twisted graphene fiber, is simultaneously outputting to coiling and molding device, is directly prepared into the graphene fiber bobbin with the twist.
2. the method that the graphene film according to claim 1 twisting method of forming prepares graphene fiber, it is characterized in that: the technique preparing Copper Foil load graphene film coiled material by the method for heating in vacuum Copper Foil at copper foil surface in described step (1) is: with Copper Foil for catalyst, when 1020-1069 DEG C, heatable catalyst makes carbon source vapor form the graphene film needing thickness at catalyst surface.
3. the method that the graphene film according to claim 1 twisting method of forming prepares graphene fiber, it is characterised in that: described step (3) is assembled twister and adopts ring ingot method, looping method, air-flow spinning or jet spinning.
4. the method that the graphene film twisting method of forming according to any one in claims 1 to 3 prepares graphene fiber, it is characterized in that: be coated with plus nano functional particulate, nano functional solution/emulsion to the graphene film top layer in step (2), nano material presoma emulsion/solution, prepares graphene oxide and the graphene fiber of functionalization.
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Cited By (7)
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| CN107034552A (en) * | 2016-12-05 | 2017-08-11 | 信阳师范学院 | Graphene fiber and preparation method thereof |
| CN108035140A (en) * | 2017-11-22 | 2018-05-15 | 东莞市明骏智能科技有限公司 | A kind of production technology 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 |
| WO2018210027A1 (en) * | 2017-05-19 | 2018-11-22 | 杭州高烯科技有限公司 | Flexible graphene fibers and continuous preparation method therefor |
| CN108910870A (en) * | 2018-07-20 | 2018-11-30 | 西安交通大学 | A kind of pollution-free shifting process of CVD graphene obtains the laminated film and method of graphene oxide and graphene composite structure |
| 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 |
| CN111439746A (en) * | 2020-05-20 | 2020-07-24 | 东华大学 | Preparation method of single-layer graphene folding structure with controllable torsion angle |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107034552A (en) * | 2016-12-05 | 2017-08-11 | 信阳师范学院 | Graphene fiber and preparation method thereof |
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| 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 |
| CN108910870A (en) * | 2018-07-20 | 2018-11-30 | 西安交通大学 | A kind of pollution-free shifting process of CVD graphene obtains the laminated film and method of graphene oxide and graphene composite structure |
| 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 |
| CN111439746A (en) * | 2020-05-20 | 2020-07-24 | 东华大学 | Preparation method of single-layer graphene folding structure with controllable torsion angle |
| 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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