CN105732038A - Highly conductive flexible self-supported graphene film and preparation method thereof - Google Patents
Highly conductive flexible self-supported graphene film and preparation method thereof Download PDFInfo
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- CN105732038A CN105732038A CN201610028929.4A CN201610028929A CN105732038A CN 105732038 A CN105732038 A CN 105732038A CN 201610028929 A CN201610028929 A CN 201610028929A CN 105732038 A CN105732038 A CN 105732038A
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/52—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbon, e.g. graphite
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- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/04—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of carbon-silicon compounds, carbon or silicon
Abstract
The invention discloses a highly conductive flexible self-supported graphene film and a preparation method thereof. The preparation method comprises the following steps: by using graphite as a raw material, preparing uniformly dispersed graphene oxide aqueous solution according to an improved Hummers method; firstly performing plasms surface treatment on a solid substrate, and titrating the graphene oxide solution on the solid substrate to dry to form a film; placing the obtained graphene oxide film in a hydroiodic acid aqueous solution to heat and reduce, and automatically separating the obtained graphene film from the solid substrate so as to obtain the highly conductive flexible self-supported graphene film. The method disclosed by the invention is simple in preparation, convenient for operation, simple to device and process requirement, cheap in raw material, low in cost, and capable of realizing large-scale industrial production. The prepared self-supported graphene is controllable in thickness, good in flexibility, and high in electrical conductivity, and is expected to be applied to the flexible electronics, super capacitors, wearable sensors and the like aspects.
Description
Technical field
The invention belongs to grapheme material preparing technical field, particularly to the preparation method of the flexible self-supporting graphene film of a kind of high connductivity.
Background technology
Grapheme material is the carbon simple substance of a kind of two-dimensional layer, monoatomic thickness, by sp2The carbon atom of hydridization ordered arrangement on two dimensional surface forms.Graphene, since within 2004, being found, has caused the extensive concern of scientist and great interest with its peculiar process based prediction model, and have a very wide range of applications field.The predominantly organic tool stripping method of preparation method of current Graphene, chemical vapour deposition technique, solvent stripping method and chemical oxidization method etc..Wherein chemical oxidization method is due to advantages such as technique are simple, reliable, with low cost, is considered as the effective way being capable of large-scale production Graphene always.Graphene oxide prepared by the method introduces many oxygen-containing functional groups on graphene edge dough-making powder, efficiently solves dissolution dispersity and the machinability problem of current Graphene, it has also become the focus of Graphene research at present.
For realizing the graphene oxide practical application in fields such as energy storage, electronic device, chemical filterings, the self-supporting graphene film that graphene oxide dispersion is further processed into high connductivity is its key issue needing to solve.The method preparing self-supporting graphene film at present mainly has Langmuir-Blodgett technology (J.Am.Chem.Soc., 2009,131:1043-1049), vacuum filtration method (Nature, 2007,448:457-460) and solvent volatilization self assembly (Adv.Mater.2009,21,3,007 3011).LB construction from part can realize the preparation of large-area smooth graphene film, but shortcoming to be it consuming time longer.Vacuum filtration method is a kind of method of relatively common preparation self-supporting graphene film and composite membrane thereof, detailed process is: first prepare graphene oxide membrane with suction method, and by organic solvent, filter membrane is dissolved the graphene oxide film obtaining self-supporting, carry out high-temperature calcination reduction again and obtain self-supporting graphene film (Naturenanotechnology, 2008,3:270-274);Suction method needs to first pass through organic solvent and removes filter membrane substrate, retransfers and carries out thermal reduction, complicated operation, and prepared self-supporting graphene film is subject to the restriction of filter core size, is unfavorable for realizing the preparation of large area controllable material.Solvent volatilization self-assembly method is to make solvent volatilize by heating, and obtains the graphene oxide membrane of self-supporting at solvent/air interfacial assembly, then carries out reducing the graphene film obtaining self-supporting.The self-supporting substantial amounts of graphene oxide solution of graphene film needs prepared by solvent evaporation method, stock utilization is low, is unfavorable for batch production.
Summary of the invention
The present invention overcomes the graphene film Problems existing preparing self-supporting in prior art, it is provided that flexible self-supporting graphene film of a kind of high conductivity and preparation method thereof.The method preparation is simple, easy to operate, and to equipment, technological requirement simply, raw material availability is high, and cost is low, it may be achieved large-scale industrial production.Preparation self-supporting graphene film size, thickness is controlled, pliability good, electric conductivity is high.
The technical scheme is that the flexible self-supporting graphene film of a kind of high conductivity, solid substrate is first carried out plasma surface treatment, by graphene oxide solution titration drying and forming-film in solid substrate, the graphene oxide film obtained is put into heat reduction in hydriodic acid aqueous solution, the flexible self-supporting graphene film obtaining high conductivity separates automatically solid substrate, the flexible self-supporting graphene film thickness of described high conductivity is 50nm-10 μm, and electrical conductivity is 1x104~1x105S/m, it is possible to 0~180 degree of bending.
Described solid substrate includes in glass, piezoid, silicon chip any one.
The method of the flexible self-supporting graphene film of the high conductivity that preparation is described, specifically includes following steps:
(1) first solid substrate is carried out plasma surface treatment, and by graphene oxide solution titration in the solid substrate processed, vacuum drying obtains graphene oxide film;
(2) putting in hydriodic acid aqueous solution by the graphene oxide film in solid substrate, then airtight when, heating carries out reduction reaction, obtains being suspended in the self-supporting graphene film of hydroiodic acid solution surface, cleans and dries, gets product.
Described graphene oxide water solution is that with graphite for raw material, the graphene oxide water solution prepared, the concentration of described graphene oxide water solution is 0.2~3mg/ml according to the Hummers method improved.
In step (1), vacuum drying temperature is 50~100 DEG C, and the time is 2~6h.
Described hydriodic acid aqueous solution concentration is 47~80wt.%.
Step (2) reduction reaction temperature is 50~200, time 1~5h, and the mass ratio of hydroiodic acid and graphite oxide film is 5~30:1.
Beneficial effect:
(1) present invention achieves that the preparation of graphene oxide film by simple titration, and achieves that the separation of graphene film and substrate in the reduction process of graphene oxide film.Simple to operate, experimental procedure is few, not high to equipment, technological requirement, cost is low, it may be achieved batch production.(2) using filter membrane as substrate, and filter membrane must be dissolved removal to prepare self-supporting graphene film relative to vacuum filtration method, present invention can be implemented in and many kinds of solids substrate is prepared graphene film, and solid substrate can repeatedly use.(3) size of self-supporting graphene film, thickness are controlled.The present invention can control the size of graphene film by controlling the size of solid substrate, can control the thickness of graphene film by controlling the consumption of graphene oxide, and the thickness of the self-supporting graphene film of preparation is at 50nm-10 μm;(4) the self-supporting graphene film pliability good (can realize the bending of graphene film 0~180 degree) prepared, electric conductivity are high, and (electrical conductivity of graphene film is 1x104~1x105S/m), it is expected to for aspects such as flexible electronic, super capacitor, wearable sensings.
Accompanying drawing explanation
The scanning electron microscope diagram of Fig. 1 flexible self-supporting graphene film plane.
The scanning electron microscope diagram in Fig. 2 flexible self-supporting graphene film cross section.
The IV curve of Fig. 3 flexible self-supporting graphene film.
Fig. 4 flexible self-supporting graphene film bends the photo of 180 degree.
The scanning electron microscope diagram in Fig. 5 flexible self-supporting graphene film cross section.
Detailed description of the invention
The feature that the invention is further illustrated by the following examples, but the invention is not limited in following example.According to technology disclosed by the invention, it will be clear to the skilled person that the preparation of the flexible self-supporting graphene film of high connductivity can be realized completely in conjunction with prior art.
The preparation method of the flexible self-supporting paper-like graphene film of a kind of high connductivity, comprises the steps:
(1) according to the Hummers method improved, with graphite for raw material, preparation concentration is the graphene oxide water solution of 0.2~3mg/ml;
(2) first solid substrate is carried out plasma surface treatment, and by graphene oxide solution titration in the solid substrate processed, and further at 50~100 degrees Celsius of lower vacuum drying 2~6h, obtain graphene oxide film;
(3) graphene oxide film in solid substrate is put in the hydriodic acid aqueous solution that concentration is 47~80wt.%, then airtight when, 50~200 degrees Celsius of oil baths react 1~5h, obtain being suspended in the self-supporting graphene film on hydriodic acid aqueous solution surface.The mass ratio of hydroiodic acid and graphite oxide film is 5~30:1.
(4) repeatedly soaking with water, rinse, room temperature is dried, and namely obtains the flexible self-supporting graphene film of high connductivity.
Embodiment 1: the preparation of the flexible self-supporting graphene film of high connductivity
(1) according to the Hummers method (document ACSNano4 (8): 4806 (2010) improved, Improvedsynthesisofgrapheneoxide), with graphite for raw material, preparation concentration is the graphene oxide water solution of 1.5mg/ml;
(2) substrate of glass is carried out plasma surface treatment, and by uniform for graphene oxide water solution titration on the glass substrate, and further at 65 degrees Celsius of lower vacuum drying 3h, obtain graphene oxide film;
(3) graphene oxide film in substrate of glass is put in the hydriodic acid aqueous solution that concentration is 55wt.%, airtight when, 100 degrees Celsius of oil baths react 2h, obtain being suspended in the self-supporting graphene film of hydroiodic acid solution surface.The mass ratio of hydroiodic acid and graphite oxide film is 5:1.
(4) self-supporting graphene film being transferred to pure water soak, rinse, room temperature is dried, and namely prepares the self-supporting graphene film of high connductivity.Performance and Electronic Speculum figure are shown in accompanying drawing 1~5.
Embodiment 2: the preparation of the flexible self-supporting graphene film of high connductivity
(1) according to the Hummers method improved, with graphite for raw material, preparation concentration is the graphene oxide water solution of 0.5mg/ml;
(2) substrate of glass is carried out plasma surface treatment, and by uniform for graphene oxide water solution titration on the glass substrate, and further at 100 degrees Celsius of lower vacuum drying 2h, obtain graphene oxide film;
(3) graphene oxide film in substrate of glass is put in the hydriodic acid aqueous solution that concentration is 80wt.%, airtight when, 50 degrees Celsius of oil baths react 5h, obtain being suspended in the self-supporting graphene film of hydroiodic acid solution surface.The mass ratio of hydroiodic acid and graphite oxide film is 15:1.
(4) self-supporting graphene film being transferred to pure water soak, rinse, room temperature is dried, and namely prepares the self-supporting graphene film of high connductivity.
Embodiment 3: the preparation of the flexible self-supporting graphene film of high connductivity
(1) according to the Hummers method improved, with graphite for raw material, preparation concentration is the graphene oxide water solution of 3mg/ml;Substrate of glass is carried out plasma surface treatment, and by uniform for graphene oxide water solution titration on the glass substrate, and vacuum drying 6h at 50 c further, obtain graphene oxide film;
(2) graphene oxide film in substrate of glass is put in the hydriodic acid aqueous solution that concentration is 47wt.%, airtight when, 200 degrees Celsius of oil baths react 1h, obtain being suspended in the self-supporting graphene film of hydroiodic acid solution surface.The mass ratio of hydroiodic acid and graphite oxide film is 30:1.
(3) self-supporting graphene film being transferred to pure water soak, rinse, room temperature is dried, and namely prepares the self-supporting graphene film of high connductivity.
Claims (7)
1. the flexible self-supporting graphene film of a high conductivity, it is characterized in that, solid substrate is first carried out plasma surface treatment, by graphene oxide solution titration drying and forming-film in solid substrate, the graphene oxide film obtained is put into heat reduction in hydriodic acid aqueous solution, the flexible self-supporting graphene film obtaining high conductivity separates automatically solid substrate, and the flexible self-supporting graphene film thickness of described high conductivity is 50nm-10 μm, and electrical conductivity is 1x104~1x105S/m, it is possible to 0~180 degree of bending.
2. the flexible self-supporting graphene film of high conductivity according to claim 1, it is characterised in that described solid substrate includes in glass, piezoid, silicon chip any one.
3. the method for the flexible self-supporting graphene film of preparation high conductivity described in claim 1 or 2, it is characterised in that specifically include following steps:
(1) first solid substrate is carried out plasma surface treatment, and by graphene oxide solution titration in the solid substrate processed, vacuum drying obtains graphene oxide film;
(2) putting in hydriodic acid aqueous solution by the graphene oxide film in solid substrate, then airtight when, heating carries out reduction reaction, obtains being suspended in the self-supporting graphene film of hydroiodic acid solution surface, cleans and dries, gets product.
4. the method for the flexible self-supporting graphene film preparing high conductivity according to claim 3, it is characterized in that, described graphene oxide water solution is according to the Hummers method improved, with graphite for raw material, the graphene oxide water solution prepared, the concentration of described graphene oxide water solution is 0.2~3mg/ml.
5. the method for the flexible self-supporting graphene film preparing high conductivity according to claim 3, it is characterised in that in step (1), vacuum drying temperature is 50~100 DEG C, and the time is 2~6h.
6. the method for the flexible self-supporting graphene film preparing high conductivity according to claim 3, it is characterised in that described hydriodic acid aqueous solution concentration is 47~80wt.%.
7. the method for the flexible self-supporting graphene film preparing high conductivity according to claim 3, it is characterised in that: step (2) reduction reaction temperature is 50~200, time 1~5h, and the mass ratio of hydroiodic acid and graphite oxide film is 5~30:1.
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CN106698402A (en) * | 2017-01-05 | 2017-05-24 | 东南大学 | Production method of metal nano-particle doped flexible self-supporting graphene film |
CN106698405A (en) * | 2017-01-12 | 2017-05-24 | 东南大学 | Method for preparing large-area graphene paper by utilizing hydroiodic acid |
CN106835082A (en) * | 2017-01-11 | 2017-06-13 | 东南大学 | The preparation method of the flexible self-supporting graphene film of metal nanoparticle doping |
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CN106835082A (en) * | 2017-01-11 | 2017-06-13 | 东南大学 | The preparation method of the flexible self-supporting graphene film of metal nanoparticle doping |
CN106698405A (en) * | 2017-01-12 | 2017-05-24 | 东南大学 | Method for preparing large-area graphene paper by utilizing hydroiodic acid |
CN107324316A (en) * | 2017-06-30 | 2017-11-07 | 杭州高烯科技有限公司 | A kind of preparation method of graphene film positive electrode and its application in aluminium ion battery |
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CN108975316B (en) * | 2018-09-26 | 2020-02-04 | 西北有色金属研究院 | Preparation method of graphene film |
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WO2022141180A1 (en) * | 2020-12-30 | 2022-07-07 | 杭州高烯科技有限公司 | Method for stripping graphene oxide nano membrane from substrate |
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